Sample records for ultra-small-angle x-ray scattering

  1. Pinhole-type two-dimensional ultra-small-angle X-ray scattering on the micrometer scale

    PubMed Central

    Kishimoto, Hiroyuki; Shinohara, Yuya; Suzuki, Yoshio; Takeuchi, Akihisa; Yagi, Naoto; Amemiya, Yoshiyuki

    2014-01-01

    A pinhole-type two-dimensional ultra-small-angle X-ray scattering set-up at a so-called medium-length beamline at SPring-8 is reported. A long sample-to-detector distance, 160.5 m, can be used at this beamline and a small-angle resolution of 0.25 µm−1 was thereby achieved at an X-ray energy of 8 keV. PMID:24365910

  2. Small Angle X-Ray Scattering Detector

    DOEpatents

    Hessler, Jan P.

    2004-06-15

    A detector for time-resolved small-angle x-ray scattering includes a nearly constant diameter, evacuated linear tube having an end plate detector with a first fluorescent screen and concentric rings of first fiber optic bundles for low angle scattering detection and an annular detector having a second fluorescent screen and second fiber optic bundles concentrically disposed about the tube for higher angle scattering detection. With the scattering source, i.e., the specimen under investigation, located outside of the evacuated tube on the tube's longitudinal axis, scattered x-rays are detected by the fiber optic bundles, to each of which is coupled a respective photodetector, to provide a measurement resolution, i.e., dq/q, where q is the momentum transferred from an incident x-ray to an x-ray scattering specimen, of 2% over two (2) orders of magnitude in reciprocal space, i.e., q.sub.max /q.sub.min.congruent.100.

  3. An upgrade beamline for combined wide, small and ultra small-angle x-ray scattering at the ESRF

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

    Van Vaerenbergh, Pierre; Léonardon, Joachim; Sztucki, Michael

    2016-07-27

    This contribution presents the main design features of the upgraded beamline ID02 (TRUSAXS). The beamline combines different small-angle X-ray scattering techniques in one unique instrument. The key component of this instrument is an evacuated (5×10{sup −3} mbar) stainless steel detector tube of length 34 m and diameter 2 m. Three different detectors (Rayonix MX170, Pilatus 300 K and FReLoN 4M) are housed inside a motorized wagon which travels along a rail system with very low parasitic lateral movements (± 0.3 mm). This system allows automatically changing the sample-to-detector distance from about 1 m to 31 m and selecting the desiredmore » detector. In addition, a wide angle detector (Rayonix LX170) is installed just above the entrance cone of the tube for optional wide-angle X-ray scattering measurements. The beamstop system enables monitoring of the X-ray beam intensity in addition to blocking the primary beam, and automated insertion of selected masks behind the primary beamstop. The focusing optics and collimation system permit to cover a scattering vector (q) range of 0.002 nm{sup −1} ≤ q ≤ 50 nm{sup −1} with one unique setting using 0.1 nm X-ray wavelength for moderate flux (5×10{sup 12} photons/sec). However, for higher flux (6x10{sup 13} photons/sec) or higher resolution (minimum q < 0.001 nm{sup −1}), focusing and collimation, respectively need to be varied. For a sample-to-detector distance of 31 m and 0.1 nm wavelength, two dimensional ultra small-angle X-ray scattering patterns can be recorded down to q≈0.001 nm{sup −1} with far superior quality as compared to one dimensional profiles obtained with a Bonse-Hart instrument.« less

  4. NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

    DOE PAGES

    Allen, Andrew J.; Zhang, Fan; Kline, R. Joseph; ...

    2017-03-07

    The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008–0.25 Å –1, together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments thatmore » employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. As a result, the validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.« less

  5. NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

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

    Allen, Andrew J.; Zhang, Fan; Kline, R. Joseph

    The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008–0.25 Å –1, together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments thatmore » employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. As a result, the validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.« less

  6. NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering.

    PubMed

    Allen, Andrew J; Zhang, Fan; Kline, R Joseph; Guthrie, William F; Ilavsky, Jan

    2017-04-01

    The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008-0.25 Å -1 , together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments that employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. The validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.

  7. Dispersed SiC nanoparticles in Ni observed by ultra-small-angle X-ray scattering

    DOE PAGES

    Xie, R.; Ilavsky, J.; Huang, H. F.; ...

    2016-11-24

    In this paper, a metal-ceramic composite, nickel reinforced with SiC nanoparticles, was synthesized and characterized for its potential application in next-generation molten salt nuclear reactors. Synchrotron ultra-small-angle X-ray scattering (USAXS) measurements were conducted on the composite. The size distribution and number density of the SiC nanoparticles in the material were obtained through data modelling. Scanning and transmission electron microscopy characterization were performed to substantiate the results of the USAXS measurements. Tensile tests were performed on the samples to measure the change in their yield strength after doping with the nanoparticles. Finally, the average interparticle distance was calculated from the USAXSmore » results and is related to the increased yield strength of the composite.« less

  8. Probing the Complex Architecture of Multimodular Carbohydrate-Active Enzymes Using a Combination of Small Angle X-Ray Scattering and X-Ray Crystallography.

    PubMed

    Czjzek, Mirjam; Ficko-Blean, Elizabeth

    2017-01-01

    The various modules in multimodular carbohydrate-active enzymes (CAZymes) may function in catalysis, carbohydrate binding, protein-protein interactions or as linkers. Here, we describe how combining the biophysical techniques of Small Angle X-ray Scattering (SAXS) and macromolecular X-ray crystallography (XRC) provides a powerful tool for examination into questions related to overall structural organization of ultra multimodular CAZymes.

  9. Portable mini-chamber for temperature dependent studies using small angle and wide angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Dev, Arun Singh; Kumar, Dileep; Potdar, Satish; Pandit, Pallavi; Roth, Stephan V.; Gupta, Ajay

    2018-04-01

    The present work describes the design and performance of a vacuum compatible portable mini chamber for temperature dependent GISAXS and GIWAXS studies of thin films and multilayer structures. The water cooled body of the chamber allows sample annealing up to 900 K using ultra high vacuum compatible (UHV) pyrolytic boron nitride heater, thus making it possible to study the temperature dependent evolution of structure and morphology of two-dimensional nanostructured materials. Due to its light weight and small size, the chamber is portable and can be accommodated at synchrotron facilities worldwide. A systematic illustration of the versatility of the chamber has been demonstrated at beamline P03, PETRA-III, DESY, Hamburg, Germany. Temperature dependent grazing incidence small angle x-ray scattering (GISAXS) and grazing incidence wide angle x-ray scattering (GIWAXS) measurements were performed on oblique angle deposited Co/Ag multilayer structure, which jointly revealed that the surface diffusion in Co columns in Co/Ag multilayer enhances by increasing temperature from RT to ˜573 K. This results in a morphology change from columnar tilted structure to densely packed morphological isotropic multilayer.

  10. 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

  11. 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

  12. 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.

  13. Application of ultra-small-angle X-ray scattering / X-ray photon correlation spectroscopy to relate equilibrium or non-equilibrium dynamics to microstructure

    NASA Astrophysics Data System (ADS)

    Allen, Andrew; Zhang, Fan; Levine, Lyle; Ilavsky, Jan

    2013-03-01

    Ultra-small-angle X-ray scattering (USAXS) can probe microstructures over the nanometer-to-micrometer scale range. Through use of a small instrument entrance slit, X-ray photon correlation spectroscopy (XPCS) exploits the partial coherence of an X-ray synchrotron undulator beam to provide unprecedented sensitivity to the dynamics of microstructural change. In USAXS/XPCS studies, the dynamics of local structures in a scale range of 100 nm to 1000 nm can be related to an overall hierarchical microstructure extending from 1 nm to more than 1000 nm. Using a point-detection scintillator mode, the equilibrium dynamics at ambient temperature of small particles (which move more slowly than nanoparticles) in aqueous suspension have been quantified directly for the first time. Using a USAXS-XPCS scanning mode for non-equilibrium dynamics incipient processes within dental composites have been elucidated, prior to effects becoming detectable using any other technique. Use of the Advanced Photon Source, an Office of Science User Facility operated for the United States Department of Energy (U.S. DOE) Office of Science by Argonne National Laboratory, was supported by the U.S. DOE under Contract No. DE-AC02-06CH11357.

  14. Small-angle x-ray scattering investigations of extrudates

    NASA Astrophysics Data System (ADS)

    Pikus, Stanislaw; Jamroz, Jerzy

    1997-02-01

    The small-angle X-ray scattering investigations of the extrudes are presented. The investigations of the different samples of starch by means of the SAXS indicate the new possibilities for using this method for extrudates examination. Results obtained by SAXS method of close dependance between intensity SAXS scattering and characteristic parameters of the extrudates were shown.

  15. Complementary uses of small angle X-ray scattering and X-ray crystallography.

    PubMed

    Pillon, Monica C; Guarné, Alba

    2017-11-01

    Most proteins function within networks and, therefore, protein interactions are central to protein function. Although stable macromolecular machines have been extensively studied, dynamic protein interactions remain poorly understood. Small-angle X-ray scattering probes the size, shape and dynamics of proteins in solution at low resolution and can be used to study samples in a large range of molecular weights. Therefore, it has emerged as a powerful technique to study the structure and dynamics of biomolecular systems and bridge fragmented information obtained using high-resolution techniques. Here we review how small-angle X-ray scattering can be combined with other structural biology techniques to study protein dynamics. This article is part of a Special Issue entitled: Biophysics in Canada, edited by Lewis Kay, John Baenziger, Albert Berghuis and Peter Tieleman. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Measurements of droplet size in shear-driven atomization using ultra-small angle x-ray scattering

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

    Kastengren, A.; Ilavsky, J.; Viera, Juan Pablo

    Measurements of droplet size in optically-thick, non-evaporating, shear-driven sprays have been made using ultra-small angle x-ray scattering (USAXS). The sprays are produced by orifice-type nozzles coupled to diesel injectors, with measurements conducted from 1 – 24 mm from the orifice, spanning from the optically-dense near-nozzle region to more dilute regions where optical diagnostics are feasible. The influence of nozzle diameter, liquid injection pressure, and ambient density were examined. The USAXS measurements reveal few if any nanoscale droplets, in conflict with a popular computational model of diesel spray breakup. The average droplet diameter rapidly decreases with downstream distance from the nozzlemore » until a plateau value is reached, after which only small changes are seen in droplet diameter. This plateau droplet size is consistent with the droplets being small enough to be stable with respect to further breakup. As a result, liquid injection pressure and nozzle diameter have the biggest impact on droplet size, while ambient density has a smaller effect.« less

  17. Measurements of droplet size in shear-driven atomization using ultra-small angle x-ray scattering

    DOE PAGES

    Kastengren, A.; Ilavsky, J.; Viera, Juan Pablo; ...

    2017-03-16

    Measurements of droplet size in optically-thick, non-evaporating, shear-driven sprays have been made using ultra-small angle x-ray scattering (USAXS). The sprays are produced by orifice-type nozzles coupled to diesel injectors, with measurements conducted from 1 – 24 mm from the orifice, spanning from the optically-dense near-nozzle region to more dilute regions where optical diagnostics are feasible. The influence of nozzle diameter, liquid injection pressure, and ambient density were examined. The USAXS measurements reveal few if any nanoscale droplets, in conflict with a popular computational model of diesel spray breakup. The average droplet diameter rapidly decreases with downstream distance from the nozzlemore » until a plateau value is reached, after which only small changes are seen in droplet diameter. This plateau droplet size is consistent with the droplets being small enough to be stable with respect to further breakup. As a result, liquid injection pressure and nozzle diameter have the biggest impact on droplet size, while ambient density has a smaller effect.« less

  18. SMALL ANGLE SCATTERING OF X-RAYS BY PLASTICALLY DEFORMED SINGLE CRYSTALS

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

    Robinson, W.H.; Smoluchowski, R.

    1959-05-01

    The small-angle scattering of x rays from single crystals of magnesium plastically deformed by simple shear was measured in the angular range of 4' to 5 deg . The crystals were subjected to both unidirectional and cyclic shear stresses applied along the STAl 1 2-bar 0! direction. Thin slices of the deformed single crystals were prepared using strainfree cutting and polishing techniques. The thin slices had orientations such that the slip direction was either parallel or perpendicular to the incident x-ray beam in order to observe any anisotropy in the scattering that might be due to dislocations. It was foundmore » that those samples which contained deformation twins within the irradiated volume produced rather large scattered intensity. This scattered intensity is interpreted as being due to double Bragg scattering. The scattered intensity from other specimens was attributed to surface scattering. No evidence for small angle scattering by dislocations was found. (auth)« less

  19. Small angle x-ray scattering with edge-illumination

    NASA Astrophysics Data System (ADS)

    Modregger, Peter; Cremona, Tiziana P.; Benarafa, Charaf; Schittny, Johannes C.; Olivo, Alessandro; Endrizzi, Marco

    2016-08-01

    Sensitivity to sub-pixel sample features has been demonstrated as a valuable capability of phase contrast x-ray imaging. Here, we report on a method to obtain angular-resolved small angle x-ray scattering distributions with edge-illumination- based imaging utilizing incoherent illumination from an x-ray tube. Our approach provides both the three established image modalities (absorption, differential phase and scatter strength), plus a number of additional contrasts related to unresolved sample features. The complementarity of these contrasts is experimentally validated by using different materials in powder form. As a significant application example we show that the extended complementary contrasts could allow the diagnosis of pulmonary emphysema in a murine model. In support of this, we demonstrate that the properties of the retrieved scattering distributions are consistent with the expectation of increased feature sizes related to pulmonary emphysema. Combined with the simplicity of implementation of edge-illumination, these findings suggest a high potential for exploiting extended sub-pixel contrasts in the diagnosis of lung diseases and beyond.

  20. Characterization of zein assemblies by ultra-small-angle X-ray scattering

    DOE PAGES

    Uzun, Suzan; Ilavsky, Jan; Padua, Graciela Wild

    2017-03-23

    Zein, a protein of corn, has an amphiphilic molecule capable of self-assembly into distinctly different structures. In this work, ultra-small-angle X-ray scattering (USAXS) was applied to investigate the formation of self-assembled zein structures in binary solvent systems of ethanol and water. Our study included observing structural changes due to aging. Three hierarchical structures were identified in zein-solvent systems, molecular zein 2D films, believed to be formed by zein rods assembled first into one-dimensional fibers and then into two-dimensional films, and 3D spherical aggregates. Aging did not change the size or shape of primary units, but promoted their self-assembly into intermediatemore » 2D structures and shaped 3D structures into well19 defined spheres. We found that the rheological parameters, consistency index (K) and behavior index (n), storage and loss moduli (G’ and G”) were also measured. K and n, changed markedly with aging, from nearly Newtonian low consistency fresh samples to highly viscous pseudoplastic aged samples. G’ and G” increased with aging for all samples reflecting increased interactions among zein self-assembled structures. Furthermore, viscoelastic parameters indicated that zein dispersions formed gels upon aging. It was observed that USAX reported on molecular scale self-assembly processes, while rheological measurements reported on the macroscale interaction between self-assembled particles. Raman spectra suggested that α-helix to β-sheet transformations prompted zein self-assembly, which influenced the size and morphology of molecular assemblies and ultimately the rheological properties of zein dispersions.« less

  1. Ultra-Small-Angle X-ray ScatteringX-ray Photon Correlation Spectroscopy Studies of Incipient Structural Changes in Amorphous Calcium Phosphate Based Dental Composites

    PubMed Central

    Zhang, F.; Allen, A.J.; Levine, L.E.; Espinal, L.; Antonucci, J.M.; Skrtic, D.; O’Donnell, J.N.R.; Ilavsky, J.

    2012-01-01

    The local structural changes in amorphous calcium phosphate (ACP) based dental composites were studied under isothermal conditions using both static, bulk measurement techniques and a recently developed methodology based on combined ultra-small angle X-ray scatteringX-ray photon correlation spectroscopy (USAXS-XPCS), which permits a dynamic approach. While results from conventional bulk measurements do not show clear signs of structural change, USAXS-XPCS results reveal unambiguous evidence for local structural variations on a similar time scale to that of water loss in the ACP fillers. A thermal-expansion based simulation indicates that thermal behavior alone does not account for the observed dynamics. Together, these results suggest that changes in the water content of ACP affect the composite morphology due to changes in ACP structure that occur without an amorphous-to-crystalline conversion. It is also noted that biomedical materials research could benefit greatly from USAXS-XPCS, a dynamic approach. PMID:22374649

  2. Ultra small angle x-ray scattering in complex mixtures of triacylglycerols

    NASA Astrophysics Data System (ADS)

    Peyronel, Fernanda; Quinn, Bonnie; Marangoni, Alejandro G.; Pink, David A.

    2014-11-01

    Ultra-small angle x-ray scattering (USAXS) has been used to elucidate, in situ, the aggregation structure of unsheared model edible oils. Each system comprised one or two solid lipids and a combination of liquid lipids. The 3D nano- to micro-structures of each system were characterized. The length scale investigated, using the Bonse-Hart camera at beamline ID-15D at the Advanced Photon Source, ANL, ranged from 300 Å-10 µm. Using the Unified Fit model, level-1 analysis showed that the scatterers were 2D objects with either a smooth, a rough, or a diffuse surface. These 2D objects had an average radius of gyration Rg1 between 200-1500 Å. Level-2 analysis displayed a slope between -1 and -2. Use of the Guinier-Porod model gave s ≈ 1 thus showing that it was cylinders (TAGwoods) aggregating with fractal dimension 1 ≤ D2 ≤ 2. D2 = 1 is consistent with 1D structures formed from TAGwoods, while D2 = 2 implies that the TAGwoods had formed structures characteristic of diffusion or reaction limited cluster-cluster aggregation (DLCA/RLCA). These aggregates exhibited radii of gyration, Rg2, between 2500 and 6500 Å. Level-3 analyses showed diffuse surfaces, for most of the systems. These interpretations are in accord with theoretical models which studied crystalline nano-platelets (CNPs) coated with nano-scale layers arising from phase separation at the CNP surfaces. These layers could be due to either liquid-liquid phase separation with the CNPs coated, uniformly or non-uniformly, by a diffuse layer of TAGs, or solid-liquid phase separation with the CNPs coated by a rough layer of crystallites. A fundamental understanding of the self-organizing structures arising in these systems helps advance the characterization of fat crystal networks from nanometres to micrometres. This research can be used to design novel fat structures that use healthier fats via nano- and meso-scale structural engineering.

  3. 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

  4. Small-angle x-ray scattering in amorphous silicon: A computational study

    NASA Astrophysics Data System (ADS)

    Paudel, Durga; Atta-Fynn, Raymond; Drabold, David A.; Elliott, Stephen R.; Biswas, Parthapratim

    2018-05-01

    We present a computational study of small-angle x-ray scattering (SAXS) in amorphous silicon (a -Si) with particular emphasis on the morphology and microstructure of voids. The relationship between the scattering intensity in SAXS and the three-dimensional structure of nanoscale inhomogeneities or voids is addressed by generating large high-quality a -Si networks with 0.1%-0.3% volume concentration of voids, as observed in experiments using SAXS and positron annihilation spectroscopy. A systematic study of the variation of the scattering intensity in the small-angle scattering region with the size, shape, number density, and the spatial distribution of the voids in the networks is presented. Our results suggest that the scattering intensity in the small-angle region is particularly sensitive to the size and the total volume fraction of the voids, but the effect of the geometry or shape of the voids is less pronounced in the intensity profiles. A comparison of the average size of the voids obtained from the simulated values of the intensity, using the Guinier approximation and Kratky plots, with that of the same from the spatial distribution of the atoms in the vicinity of void surfaces is presented.

  5. Vesicle Adhesion and Fusion Studied by Small-Angle X-Ray Scattering.

    PubMed

    Komorowski, Karlo; Salditt, Annalena; Xu, Yihui; Yavuz, Halenur; Brennich, Martha; Jahn, Reinhard; Salditt, Tim

    2018-04-24

    We have studied the adhesion state (also denoted by docking state) of lipid vesicles as induced by the divalent ions Ca 2+ or Mg 2+ at well-controlled ion concentration, lipid composition, and charge density. The bilayer structure and the interbilayer distance in the docking state were analyzed by small-angle x-ray scattering. A strong adhesion state was observed for DOPC:DOPS vesicles, indicating like-charge attraction resulting from ion correlations. The observed interbilayer separations of ∼1.6 nm agree quantitatively with the predictions of electrostatics in the strong coupling regime. Although this phenomenon was observed when mixing anionic and zwitterionic (or neutral) lipids, pure anionic membranes (DOPS) with highest charge density σ resulted in a direct phase transition to a multilamellar state, which must be accompanied by rupture and fusion of vesicles. To extend the structural assay toward protein-controlled docking and fusion, we have characterized reconstituted N-ethylmaleimide-sensitive factor attachment protein receptors in controlled proteoliposome suspensions by small-angle x-ray scattering. Copyright © 2018 Biophysical Society. Published by Elsevier Inc. All rights reserved.

  6. Small angle x ray scattering studies of reverse micelles in supercritical fluids

    NASA Astrophysics Data System (ADS)

    Pfund, D. M.; Fulton, J. L.

    1994-10-01

    The nature of aggregates formed in a supercritical fluid determines its solvent power and selectivity. Small angle X ray scattering (SAXS) is a powerful tool for studying the properties of aggregates with sizes in the 10(angstrom) to 200(angstrom) range. It is also useful in studying those interparticle interactions which operate over a similar distance. The authors have used SAXS to examine the aggregates formed in pure fluids, in mixtures and in fluid/surfactant/water systems. The scattered intensity as a function of angle depends on the geometry, polydispersity, X ray contrast, and interaction strength of the particles as well as on the phase behavior of the system. In this paper the authors present the results of modeling the X-ray scattering from AOT/water reverse micelles in supercritical propane and in propane/carbon dioxide mixtures. They examine the effect of dilution with CO2 anti-solvent on the phase behavior of the system and on the strength of intermicellar attractions. A better understanding of these systems must be obtained before the applications of supercritical reverse micelle systems to extractions, reactions, and enhanced oil recovery can be fully developed.

  7. A small-angle x-ray scattering system with a vertical layout

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

    Wang, Zhen; Chen, Xiaowei; Meng, Lingpu

    A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range.more » With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.« less

  8. A small-angle x-ray scattering system with a vertical layout.

    PubMed

    Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

    2014-12-01

    A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

  9. The accurate assessment of small-angle X-ray scattering data

    DOE PAGES

    Grant, Thomas D.; Luft, Joseph R.; Carter, Lester G.; ...

    2015-01-23

    Small-angle X-ray scattering (SAXS) has grown in popularity in recent times with the advent of bright synchrotron X-ray sources, powerful computational resources and algorithms enabling the calculation of increasingly complex models. However, the lack of standardized data-quality metrics presents difficulties for the growing user community in accurately assessing the quality of experimental SAXS data. Here, a series of metrics to quantitatively describe SAXS data in an objective manner using statistical evaluations are defined. These metrics are applied to identify the effects of radiation damage, concentration dependence and interparticle interactions on SAXS data from a set of 27 previously described targetsmore » for which high-resolution structures have been determined via X-ray crystallography or nuclear magnetic resonance (NMR) spectroscopy. Studies show that these metrics are sufficient to characterize SAXS data quality on a small sample set with statistical rigor and sensitivity similar to or better than manual analysis. The development of data-quality analysis strategies such as these initial efforts is needed to enable the accurate and unbiased assessment of SAXS data quality.« less

  10. Difference structures from time-resolved small-angle and wide-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Nepal, Prakash; Saldin, D. K.

    2018-05-01

    Time-resolved small-angle x-ray scattering/wide-angle x-ray scattering (SAXS/WAXS) is capable of recovering difference structures directly from difference SAXS/WAXS curves. It does so by means of the theory described here because the structural changes in pump-probe detection in a typical time-resolved experiment are generally small enough to be confined to a single residue or group in close proximity which is identified by a method akin to the difference Fourier method of time-resolved crystallography. If it is assumed, as is usual with time-resolved structures, that the moved atoms lie within the residue, the 100-fold reduction in the search space (assuming a typical protein has about 100 residues) allows the exaction of the structure by a simulated annealing algorithm with a huge reduction in computing time and leads to a greater resolution by varying the positions of atoms only within that residue. This reduction in the number of potential moved atoms allows us to identify the actual motions of the individual atoms. In the case of a crystal, time-resolved calculations are normally performed using the difference Fourier method, which is, of course, not directly applicable to SAXS/WAXS. The method developed in this paper may be thought of as a substitute for that method which allows SAXS/WAXS (and hence disordered molecules) to also be used for time-resolved structural work.

  11. Small-Angle X-ray Scattering (SAXS) Instrument Performance and Validation Using Silver Nanoparticles

    DTIC Science & Technology

    2016-12-01

    Intercalibration of small-angle X- Ray and neutron-scattering data. Journal of Applied Crystallography . 1988;21:629–638. 7. Zhang F, Ilavsky J, Long GG...Materials Transactions A. 2009;41:1151–1158. 8. Kusz J, Bohm H. Performance of a confocal multilayer X-ray optic. Journal of Applied Crystallography ...Journal of Applied Crystallography . 2004;37:369–380. 10. Orthaber D, Bergmann A, Glatter O. SAXS experiments on absolute scale with Kratky systems using

  12. Small Angle X ray Scattering (SAXS) Instrument Performance and Validation Using Silver Nanoparticles

    DTIC Science & Technology

    2016-12-01

    Intercalibration of small-angle X- Ray and neutron-scattering data. Journal of Applied Crystallography . 1988;21:629–638. 7. Zhang F, Ilavsky J, Long GG...Materials Transactions A. 2009;41:1151–1158. 8. Kusz J, Bohm H. Performance of a confocal multilayer X-ray optic. Journal of Applied Crystallography ...Journal of Applied Crystallography . 2004;37:369–380. 10. Orthaber D, Bergmann A, Glatter O. SAXS experiments on absolute scale with Kratky systems using

  13. Simultaneous small- and wide-angle scattering at high X-ray energies.

    PubMed

    Daniels, J E; Pontoni, D; Hoo, Rui Ping; Honkimäki, V

    2010-07-01

    Combined small- and wide-angle X-ray scattering (SAXS/WAXS) is a powerful technique for the study of materials at length scales ranging from atomic/molecular sizes (a few angstroms) to the mesoscopic regime ( approximately 1 nm to approximately 1 microm). A set-up to apply this technique at high X-ray energies (E > 50 keV) has been developed. Hard X-rays permit the execution of at least three classes of investigations that are significantly more difficult to perform at standard X-ray energies (8-20 keV): (i) in situ strain analysis revealing anisotropic strain behaviour both at the atomic (WAXS) as well as at the mesoscopic (SAXS) length scales, (ii) acquisition of WAXS patterns to very large q (>20 A(-1)) thus allowing atomic pair distribution function analysis (SAXS/PDF) of micro- and nano-structured materials, and (iii) utilization of complex sample environments involving thick X-ray windows and/or samples that can be penetrated only by high-energy X-rays. Using the reported set-up a time resolution of approximately two seconds was demonstrated. It is planned to further improve this time resolution in the near future.

  14. Structural evolution of photocrosslinked silk fibroin and silk fibroin-based hybrid hydrogels: A small angle and ultra-small angle scattering investigation.

    PubMed

    Whittaker, Jasmin L; Balu, Rajkamal; Knott, Robert; de Campo, Liliana; Mata, Jitendra P; Rehm, Christine; Hill, Anita J; Dutta, Naba K; Roy Choudhury, Namita

    2018-07-15

    Regenerated Bombyx mori silk fibroin (RSF) is a widely recognized protein for biomedical applications; however, its hierarchical gel structure is poorly understood. In this paper, the hierarchical structure of photocrosslinked RSF and RSF-based hybrid hydrogel systems: (i) RSF/Rec1-resilin and (ii) RSF/poly(N-vinylcaprolactam (PVCL) is reported for the first time using small-angle scattering (SAS) techniques. The structure of RSF in dilute to concentrated solution to fabricated hydrogels were characterized using small angle X-ray scattering (SAXS), small angle neutron scattering (SANS) and ultra-small angle neutron scattering (USANS) techniques. The RSF hydrogel exhibited three distinctive structural characteristics: (i) a Porod region in the length scale of 2 to 3nm due to hydrophobic domains (containing β-sheets) which exhibits sharp interfaces with the amorphous matrix of the hydrogel and the solvent, (ii) a Guinier region in the length scale of 4 to 20nm due to hydrophilic domains (containing turns and random coil), and (iii) a Porod-like region in the length scale of few micrometers due to water pores/channels exhibiting fractal-like characteristics. Addition of Rec1-resilin or PVCL to RSF and subsequent crosslinking systematically increased the nanoscale size of hydrophobic and hydrophilic domains, whereas decreased the homogeneity of pore size distribution in the microscale. The presented results have implications on the fundamental understanding of the structure-property relationship of RSF-based hydrogels. Copyright © 2018. Published by Elsevier B.V.

  15. Planar small-angle x-ray scattering imaging of phantoms and biological samples

    NASA Astrophysics Data System (ADS)

    Choi, M.; Badano, A.

    2017-04-01

    Coherent small-angle x-ray scattering (SAXS) provides molecular and nanometer-scale structural information. By capturing SAXS data at multiple locations across a sample, we obtained planar images and observed improved contrast given by the difference in the material scattering cross sections. We use phantoms made with 3D printing techniques, with tissue-mimicking plastic (PMMA), and with a highly scattering reference material (AgBe), which were chosen because of their well characterized scattering cross section to demonstrate and characterize the planar imaging of a laboratory SAXS system. We measure 1.07 and 2.14 nm-1 angular intensity maps for AgBe, 9.5 nm-1 for PMMA, and 12.3 nm-1 for Veroclear. The planar SAXS images show material discrimination based on their cross sectional features. The image signal-to-noise ratio (SNR) of each q image was dependent on exposure time and x-ray flux. We observed a lower SNR (91 ± 48) at q angles where no characteristic peaks for either material exist. To improve the visualization of the acquired data by utilizing all q-binned data, we describe a weighted-sum presentation method with a priori knowledge of relevant cross sections to improve the SNR (10 000 ± 6400) over the SNR from a single q-image at 1.07 nm-1 (1100 ± 620). In addition, we describe planar SAXS imaging of a mouse brain slice showing differentiation of tissue types as compared to a conventional absorption-based x-ray imaging technique.

  16. A Microbeam Small-Angle X-ray Scattering Study on Enamel Crystallites in Subsurface Lesion

    NASA Astrophysics Data System (ADS)

    Yagi, N.; Ohta, N.; Matsuo, T.; Tanaka, T.; Terada, Y.; Kamasaka, H.; Kometani, T.

    2010-10-01

    The early caries lesion in bovine tooth enamel was studied by two different X-ray diffraction systems at the SPring-8 third generation synchrotron radiation facility. Both allowed us simultaneous measurement of the small and large angle regions. The beam size was 6μm at BL40XU and 50μm at BL45XU. The small-angle scattering from voids in the hydroxyapatite crystallites and the wide-angle diffraction from the hydroxyapatite crystals were observed simultaneously. At BL40XU an X-ray image intensifier was used for the small-angle and a CMOS flatpanel detector for the large-angle region. At BL45XU, a large-area CCD detector was used to cover both regions. A linear microbeam scan at BL40XU showed a detailed distribution of voids and crystals and made it possible to examine the structural details in the lesion. The two-dimensional scan at BL45XU showed distribution of voids and crystals in a wider region in the enamel. The simultaneous small- and wide-angle measurement with a microbeam is a powerful tool to elucidate the mechanisms of demineralization and remineralization in the early caries lesion.

  17. Grazing-incidence small angle x-ray scattering studies of nanoscale polymer gratings

    NASA Astrophysics Data System (ADS)

    Doxastakis, Manolis; Suh, Hyo Seon; Chen, Xuanxuan; Rincon Delgadillo, Paulina A.; Wan, Lingshu; Williamson, Lance; Jiang, Zhang; Strzalka, Joseph; Wang, Jin; Chen, Wei; Ferrier, Nicola; Ramirez-Hernandez, Abelardo; de Pablo, Juan J.; Gronheid, Roel; Nealey, Paul

    2015-03-01

    Grazing-Incidence Small Angle X-ray Scattering (GISAXS) offers the ability to probe large sample areas, providing three-dimensional structural information at high detail in a thin film geometry. In this study we exploit the application of GISAXS to structures formed at one step of the LiNe (Liu-Nealey) flow using chemical patterns for directed self-assembly of block copolymer films. Experiments conducted at the Argonne National Laboratory provided scattering patterns probing film characteristics at both parallel and normal directions to the surface. We demonstrate the application of new computational methods to construct models based on scattering measured. Such analysis allows for extraction of structural characteristics at unprecedented detail.

  18. A modified Rayleigh-Gans-Debye formula for small angle X-ray scattering by interstellar dust grains

    NASA Astrophysics Data System (ADS)

    Sharma, Subodh K.

    2015-05-01

    A widely used approximation in studies relating to small angle differential scattering cross-section of X-rays scattered by interstellar dust grains is the well known Rayleigh-Gans-Debye approximation (RGDA). The validity of this approximation, however, is limited only to X-ray energies greater than about 1 keV. At lower energies, this approximation overestimates the exact results. In this paper a modification to the RGDA is suggested. It is shown that a combination of the RGDA with Ramsauer approximation retains the formal simplicity of the RGDA and also yields good agreement with Mie computations at all X-ray energies.

  19. Long Periodic Structure of a Room-Temperature Ionic Liquid by High-Pressure Small-Angle X-Ray Scattering and Wide-Angle X-Ray Scattering: 1-Decyl-3-Methylimidazolium Chloride.

    PubMed

    Abe, Hiroshi; Hamaya, Nozomu; Koyama, Yoshihiro; Kishimura, Hiroaki; Takekiyo, Takahiro; Yoshimura, Yukihiro; Wakabayashi, Daisuke; Funamori, Nobumasa; Matsuishi, Kiyoto

    2018-04-23

    The Bragg reflections of 1-decyl-3-methylimidazolium chloride ([C 10 mim][Cl]), a room-temperature ionic liquid, are observed in a lowly scattered wavevector (q) region using high-pressure (HP) small-angle X-ray scattering methods. The HP crystal of [C 10 mim][Cl] was characterized by an extremely long periodic structure. The peak position at the lowest q (1.4 nm -1 ) was different from that of the prepeak observed in the liquid state (2.3 nm -1 ). Simultaneously, Bragg reflections at high-q were detected using HP wide-angle X-ray scattering. The longest lattice constant was estimated to be 4.3 nm using structural analysis. The crystal structure of HP differed from that of the low-temperature (LT) crystal and the LT liquid crystal. With increasing pressure, Bragg reflections in the high-q component became much broader, and were accompanied by phase transition, although those in the low-q component were observed to be relatively sharp. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Investigation of the structure of unilamellar dimyristoylphosphatidylcholine vesicles in aqueous sucrose solutions by small-angle neutron and X-ray scattering

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

    Kiselev, M. A., E-mail: elena@jinr.ru; Zemlyanaya, E. V.; Zhabitskaya, E. I.

    2015-01-15

    The structure of a polydispersed population of unilamellar dimyristoylphosphatidylcholine (DMPC) vesicles in sucrose solutions has been investigated by small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS). Calculations within the model of separated form factors (SFF) show that the structure of the vesicle system depends strongly on the sucrose concentration.

  1. Stoichiometry of Cd(S,Se) nanocrystals by anomalous small-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Ramos, Aline; Lyon, Olivier; Levelut, Claire

    1995-12-01

    In Cd(S,Se)-doped glasses the optical properties are strongly dependent on the size of the nanocrystals, but can be also largely modified by changes in the crystal stoichiometry; however, the information on both stoichiometry and size is difficult to obtain in crystals smaller than 10 nm. The intensity scattered at small angles is classically used to get information about nanoparticles sizes. Moreover the variation of amplitude of this intensity with the energy of the x ray—``the anomalous effect''—near the selenium edge is related to stoichiometry. Anomalous small-angle x-ray scattering has been used as a tentative method to get information about stoichiometry in nanocrystals with size lower than 10 nm. Experiments have been performed on samples treated for 2 days at temperatures in the range 540-650 °C. The samples treated at temperatures above 580 °C contain crystals with size larger than 4 nm. For all these samples the anomalous effect has nearly the same amplitude, and we found the stoichiometry x=0.4 for the CdSxSe1-x nanocrystals. This agrees with the previous results obtained by scanning electron microscopy and Raman spectroscopy. The results are also confirmed by measurements of the position of the optical absorption edge and by wide-angle x-ray scattering experiments. For the sample treated at 560 °C, the nanocrystal size is 3 nm and the stoichiometry x=0.6 is deduced from the anomalous effect. For samples treated at lower temperatures the anomalous effect is not observable, indicating an even lower selenium content in the nanocrystals (x≳0.7). We observed differences in the Se content of nanocrystals for different heat treatments of the same initial glass. These results may be very helpful to interpret the change in the optical properties when the temperature of the treatments decreases in the range 560-590 °C. In this temperature range, compositional effects seem to be of the same order of magnitude as the effects of the quantum confinement.

  2. Small-angle scattering of polychromatic X-rays: effects of bandwidth, spectral shape and high harmonics.

    PubMed

    Chen, Sen; Luo, Sheng Nian

    2018-03-01

    Polychromatic X-ray sources can be useful for photon-starved small-angle X-ray scattering given their high spectral fluxes. Their bandwidths, however, are 10-100 times larger than those using monochromators. To explore the feasibility, ideal scattering curves of homogeneous spherical particles for polychromatic X-rays are calculated and analyzed using the Guinier approach, maximum entropy and regularization methods. Monodisperse and polydisperse systems are explored. The influence of bandwidth and asymmetric spectra shape are explored via Gaussian and half-Gaussian spectra. Synchrotron undulator spectra represented by two undulator sources of the Advanced Photon Source are examined as an example, as regards the influence of asymmetric harmonic shape, fundamental harmonic bandwidth and high harmonics. The effects of bandwidth, spectral shape and high harmonics on particle size determination are evaluated quantitatively.

  3. Small-angle scattering of polychromatic X-rays: effects of bandwidth, spectral shape and high harmonics

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

    Chen, Sen; Luo, Sheng-Nian

    Polychromatic X-ray sources can be useful for photon-starved small-angle X-ray scattering given their high spectral fluxes. Their bandwidths, however, are 10–100 times larger than those using monochromators. To explore the feasibility, ideal scattering curves of homogeneous spherical particles for polychromatic X-rays are calculated and analyzed using the Guinier approach, maximum entropy and regularization methods. Monodisperse and polydisperse systems are explored. The influence of bandwidth and asymmetric spectra shape are exploredviaGaussian and half-Gaussian spectra. Synchrotron undulator spectra represented by two undulator sources of the Advanced Photon Source are examined as an example, as regards the influence of asymmetric harmonic shape, fundamentalmore » harmonic bandwidth and high harmonics. The effects of bandwidth, spectral shape and high harmonics on particle size determination are evaluated quantitatively.« less

  4. Effects of the environmental factors on the casein micelle structure studied by cryo transmission electron microscopy and small-angle x-ray scattering/ultrasmall-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Marchin, Stéphane; Putaux, Jean-Luc; Pignon, Frédéric; Léonil, Joëlle

    2007-01-01

    Casein micelles are colloidal protein-calcium-transport complexes whose structure has not been unequivocally elucidated. This study used small-angle x-ray scattering (SAXS) and ultrasmall angle x-ray scattering (USAXS) as well as cryo transmission electron microscopy (cryo-TEM) to provide fine structural details on their structure. Cryo-TEM observations of native casein micelles fractionated by differential centrifugation showed that colloidal calcium phosphate appeared as nanoclusters with a diameter of about 2.5nm. They were uniformly distributed in a homogeneous tangled web of caseins and were primarily responsible for the intensity distribution in the SAXS profiles at the highest q vectors corresponding to the internal structure of the casein micelles. A specific demineralization of casein micelles by decreasing the pH from 6.7 to 5.2 resulted in a reduced granular aspect of the micelles observed by cryo-TEM and the existence of a characteristic point of inflection in SAXS profiles. This supports the hypothesis that the smaller substructures detected by SAXS are colloidal calcium phosphate nanoclusters rather than putative submicelles.

  5. Imaging method based on attenuation, refraction and ultra-small-angle-scattering of x-rays

    DOEpatents

    Wernick, Miles N.; Chapman, Leroy Dean; Oltulu, Oral; Zhong, Zhong

    2005-09-20

    A method for detecting an image of an object by measuring the intensity at a plurality of positions of a transmitted beam of x-ray radiation emitted from the object as a function of angle within the transmitted beam. The intensity measurements of the transmitted beam are obtained by a crystal analyzer positioned at a plurality of angular positions. The plurality of intensity measurements are used to determine the angular intensity spectrum of the transmitted beam. One or more parameters, such as an attenuation property, a refraction property and a scatter property, can be obtained from the angular intensity spectrum and used to display an image of the object.

  6. Small Angle X-Ray Scattering from Lipid-Bound Myelin Basic Protein in Solution

    PubMed Central

    Haas, H.; Oliveira, C. L. P.; Torriani, I. L.; Polverini, E.; Fasano, A.; Carlone, G.; Cavatorta, P.; Riccio, P.

    2004-01-01

    The structure of myelin basic protein (MBP), purified from the myelin sheath in both lipid-free (LF-MBP) and lipid-bound (LB-MBP) forms, was investigated in solution by small angle x-ray scattering. The water-soluble LF-MBP, extracted at pH < 3.0 from defatted brain, is the classical preparation of MBP, commonly regarded as an intrinsically unfolded protein. LB-MBP is a lipoprotein-detergent complex extracted from myelin with its native lipidic environment at pH > 7.0. Under all conditions, the scattering from the two protein forms was different, indicating different molecular shapes. For the LB-MBP, well-defined scattering curves were obtained, suggesting that the protein had a unique, compact (but not globular) structure. Furthermore, these data were compatible with earlier results from molecular modeling calculations on the MBP structure which have been refined by us. In contrast, the LF-MBP data were in accordance with the expected open-coil conformation. The results represent the first direct structural information from x-ray scattering measurements on MBP in its native lipidic environment in solution. PMID:14695288

  7. Analysis of RNA structure using small-angle X-ray scattering

    PubMed Central

    Cantara, William A.; Olson, Erik D.; Musier-Forsyth, Karin

    2016-01-01

    In addition to their role in correctly attaching specific amino acids to cognate tRNAs, aminoacyl-tRNA synthetases (aaRS) have been found to possess many alternative functions and often bind to and act on other nucleic acids. In contrast to the well-defined 3D structure of tRNA, the structures of many of the other RNAs recognized by aaRSs have not been solved. Despite advances in the use of X-ray crystallography (XRC), nuclear magnetic resonance (NMR) spectroscopy and cryo-electron microscopy (cryo-EM) for structural characterization of biomolecules, significant challenges to solving RNA structures still exist. Recently, small-angle X-ray scattering (SAXS) has been increasingly employed to characterize the 3D structures of RNAs and RNA-protein complexes. SAXS is capable of providing low-resolution tertiary structure information under physiological conditions and with less intensive sample preparation and data analysis requirements than XRC, NMR and cryo-EM. In this article, we describe best practices involved in the process of RNA and RNA-protein sample preparation, SAXS data collection, data analysis, and structural model building. PMID:27777026

  8. Grazing-incidence small-angle X-ray scattering (GISAXS) on small periodic targets using large beams

    PubMed Central

    Soltwisch, Victor; Probst, Jürgen; Scholze, Frank; Krumrey, Michael

    2017-01-01

    Grazing-incidence small-angle X-ray scattering (GISAXS) is often used as a versatile tool for the contactless and destruction-free investigation of nano­structured surfaces. However, due to the shallow incidence angles, the footprint of the X-ray beam is significantly elongated, limiting GISAXS to samples with typical target lengths of several millimetres. For many potential applications, the production of large target areas is impractical, and the targets are surrounded by structured areas. Because the beam footprint is larger than the targets, the surrounding structures contribute parasitic scattering, burying the target signal. In this paper, GISAXS measurements of isolated as well as surrounded grating targets in Si substrates with line lengths from 50 µm down to 4 µm are presented. For the isolated grating targets, the changes in the scattering patterns due to the reduced target length are explained. For the surrounded grating targets, the scattering signal of a 15 µm × 15 µm target grating structure is separated from the scattering signal of 100 µm × 100 µm nanostructured surroundings by producing the target with a different orientation with respect to the predominant direction of the surrounding structures. As virtually all litho­graphically produced nanostructures have a predominant direction, the described technique allows GISAXS to be applied in a range of applications, e.g. for characterization of metrology fields in the semiconductor industry, where up to now it has been considered impossible to use this method due to the large beam footprint. PMID:28875030

  9. Grazing-incidence small-angle X-ray scattering (GISAXS) on small periodic targets using large beams.

    PubMed

    Pflüger, Mika; Soltwisch, Victor; Probst, Jürgen; Scholze, Frank; Krumrey, Michael

    2017-07-01

    Grazing-incidence small-angle X-ray scattering (GISAXS) is often used as a versatile tool for the contactless and destruction-free investigation of nano-structured surfaces. However, due to the shallow incidence angles, the footprint of the X-ray beam is significantly elongated, limiting GISAXS to samples with typical target lengths of several millimetres. For many potential applications, the production of large target areas is impractical, and the targets are surrounded by structured areas. Because the beam footprint is larger than the targets, the surrounding structures contribute parasitic scattering, burying the target signal. In this paper, GISAXS measurements of isolated as well as surrounded grating targets in Si substrates with line lengths from 50 µm down to 4 µm are presented. For the isolated grating targets, the changes in the scattering patterns due to the reduced target length are explained. For the surrounded grating targets, the scattering signal of a 15 µm × 15 µm target grating structure is separated from the scattering signal of 100 µm × 100 µm nanostructured surroundings by producing the target with a different orientation with respect to the predominant direction of the surrounding structures. As virtually all litho-graphically produced nanostructures have a predominant direction, the described technique allows GISAXS to be applied in a range of applications, e.g.  for characterization of metrology fields in the semiconductor industry, where up to now it has been considered impossible to use this method due to the large beam footprint.

  10. The effects of burial diagenesis on multiscale porosity in the St. Peter Sandstone: An imaging, small-angle, and ultra-small-angle neutron scattering analysis

    DOE PAGES

    Anovitz, Lawrence M.; Freiburg, Jared T.; Wasbrough, Matthew; ...

    2017-11-06

    To examine the effects of burial diagenesis on heirarchical pore structures in sandstone and compare those with the effects of overgrowth formation, we obtained samples of St. Peter Sandstone from drill cores obtained in the Illinois and Michigan Basins. The multiscale pore structure of rocks in sedimentary reservoirs and the mineralogy associated with those pores are critical factors for estimating reservoir properties, including fluid mass in place, permeability, and capillary pressures, as well as geochemical interactions between the rock and the fluid. The combination of small- and ultra-small-angle neutron scattering with backscattered electron or X ray-computed tomographic imaging, or both,more » provided a means by which pore structures were quantified at scales ranging from aproximately 1 nm to 1 cm—seven orders of magnitude. Larger scale (>10 µm) porosity showed the expected logarithmic decrease in porosity with depth, although there was significant variation in each sample group. However, small- and ultra-small-angle neutron scattering data showed that the proportion of small-scale porosity increased with depth. Porosity distributions were not continuous, but consisted of a series of log normal-like distributions at several distinct scales within these rocks. Fractal dimensions at larger scales decreased (surfaces smoothed) with increasing depth, and those at smaller scales increased (surfaces roughened) and pores become more isolated (higher lacunarity). Furthermore, data suggest that changes in pore-size distributions are controlled by both physical (compaction) and chemical effects (precipitation, cementation, dissolution).« less

  11. The effects of burial diagenesis on multiscale porosity in the St. Peter Sandstone: An imaging, small-angle, and ultra-small-angle neutron scattering analysis

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

    Anovitz, Lawrence M.; Freiburg, Jared T.; Wasbrough, Matthew

    To examine the effects of burial diagenesis on heirarchical pore structures in sandstone and compare those with the effects of overgrowth formation, we obtained samples of St. Peter Sandstone from drill cores obtained in the Illinois and Michigan Basins. The multiscale pore structure of rocks in sedimentary reservoirs and the mineralogy associated with those pores are critical factors for estimating reservoir properties, including fluid mass in place, permeability, and capillary pressures, as well as geochemical interactions between the rock and the fluid. The combination of small- and ultra-small-angle neutron scattering with backscattered electron or X ray-computed tomographic imaging, or both,more » provided a means by which pore structures were quantified at scales ranging from aproximately 1 nm to 1 cm—seven orders of magnitude. Larger scale (>10 µm) porosity showed the expected logarithmic decrease in porosity with depth, although there was significant variation in each sample group. However, small- and ultra-small-angle neutron scattering data showed that the proportion of small-scale porosity increased with depth. Porosity distributions were not continuous, but consisted of a series of log normal-like distributions at several distinct scales within these rocks. Fractal dimensions at larger scales decreased (surfaces smoothed) with increasing depth, and those at smaller scales increased (surfaces roughened) and pores become more isolated (higher lacunarity). Furthermore, data suggest that changes in pore-size distributions are controlled by both physical (compaction) and chemical effects (precipitation, cementation, dissolution).« less

  12. Analysis of small-angle X-ray scattering data in the presence of significant instrumental smearing

    PubMed Central

    Bergenholtz, Johan; Ulama, Jeanette; Zackrisson Oskolkova, Malin

    2016-01-01

    A laboratory-scale small-angle X-ray scattering instrument with pinhole collimation has been used to assess smearing effects due to instrumental resolution. A new, numerically efficient method to smear ideal model intensities is developed and presented. It allows for directly using measured profiles of isotropic but otherwise arbitrary beams in smearing calculations. Samples of low-polydispersity polymer spheres have been used to show that scattering data can in this way be quantitatively modeled even when there is substantial distortion due to instrumental resolution. PMID:26937235

  13. Structural dissection of human metapneumovirus phosphoprotein using small angle x-ray scattering.

    PubMed

    Renner, Max; Paesen, Guido C; Grison, Claire M; Granier, Sébastien; Grimes, Jonathan M; Leyrat, Cédric

    2017-11-01

    The phosphoprotein (P) is the main and essential cofactor of the RNA polymerase (L) of non-segmented, negative-strand RNA viruses. P positions the viral polymerase onto its nucleoprotein-RNA template and acts as a chaperone of the nucleoprotein (N), thereby preventing nonspecific encapsidation of cellular RNAs. The phosphoprotein of human metapneumovirus (HMPV) forms homotetramers composed of a stable oligomerization domain (P core ) flanked by large intrinsically disordered regions (IDRs). Here we combined x-ray crystallography of P core with small angle x-ray scattering (SAXS)-based ensemble modeling of the full-length P protein and several of its fragments to provide a structural description of P that captures its dynamic character, and highlights the presence of varyingly stable structural elements within the IDRs. We discuss the implications of the structural properties of HMPV P for the assembly and functioning of the viral transcription/replication machinery.

  14. Pressure-jump small-angle x-ray scattering detected kinetics of staphylococcal nuclease folding.

    PubMed Central

    Woenckhaus, J; Köhling, R; Thiyagarajan, P; Littrell, K C; Seifert, S; Royer, C A; Winter, R

    2001-01-01

    The kinetics of chain disruption and collapse of staphylococcal nuclease after positive or negative pressure jumps was monitored by real-time small-angle x-ray scattering under pressure. We used this method to probe the overall conformation of the protein by measuring its radius of gyration and pair-distance-distribution function p(r) which are sensitive to the spatial extent and shape of the particle. At all pressures and temperatures tested, the relaxation profiles were well described by a single exponential function. No fast collapse was observed, indicating that the rate limiting step for chain collapse is the same as that for secondary and tertiary structure formation. Whereas refolding at low pressures occurred in a few seconds, at high pressures the relaxation was quite slow, approximately 1 h, due to a large positive activation volume for the rate-limiting step for chain collapse. A large increase in the system volume upon folding implies significant dehydration of the transition state and a high degree of similarity in terms of the packing density between the native and transition states in this system. This study of the time-dependence of the tertiary structure in pressure-induced folding/unfolding reactions demonstrates that novel information about the nature of protein folding transitions and transition states can be obtained from a combination of small-angle x-ray scattering using high intensity synchrotron radiation with the high pressure perturbation technique. PMID:11222312

  15. Preliminary small-angle X-ray scattering and X-ray diffraction studies of the BTB domain of lola protein from Drosophila melanogaster

    NASA Astrophysics Data System (ADS)

    Boyko, K. M.; Nikolaeva, A. Yu.; Kachalova, G. S.; Bonchuk, A. N.; Dorovatovskii, P. V.; Popov, V. O.

    2017-11-01

    The Drosophila genome has several dozens of transcription factors (TTK group) containing BTB domains assembled into octamers. The LOLA protein belongs to this family. The purification, crystallization, and preliminary X-ray diffraction and small-angle X-ray scattering (SAXS) studies of the BTB domain of this protein are reported. The crystallization conditions were found by the vapor-diffusion technique. A very low diffraction resolution (8.7 Å resolution) of the crystals was insufficient for the determination of the threedimensional structure of the BTB domain. The SAXS study demonstrated that the BTB domain of the LOLA protein exists as an octamer in solution.

  16. Mineral crystal alignment in mineralized fracture callus determined by 3D small-angle X-ray scattering

    NASA Astrophysics Data System (ADS)

    Liu, Yifei; Manjubala, Inderchand; Roschger, Paul; Schell, Hanna; Duda, Georg N.; Fratzl, Peter

    2010-10-01

    Callus tissue formed during bone fracture healing is a mixture of different tissue types as revealed by histological analysis. But the structural characteristics of mineral crystals within the healing callus are not well known. Since two-dimensional (2D) scanning small-angle X-ray scattering (sSAXS) patterns showed that the size and orientation of callus crystals vary both spatially and temporally [1] and 2D electron microscopic analysis implies an anisotropic property of the callus morphology, the mineral crystals within the callus are also expected to vary in size and orientation in 3D. Three-dimensional small-angle X-ray scattering (3D SAXS), which combines 2D SAXS patterns collected at different angles of sample tilting, has been previously applied to investigate bone minerals in horse radius [2] and oim/oim mouse femur/tibia [3]. We implement a similar 3D SAXS method but with a different way of data analysis to gather information on the mineral alignment in fracture callus. With the proposed accurate yet fast assessment of 3D SAXS information, it was shown that the plate shaped mineral particles in the healing callus were aligned in groups with their predominant orientations occurring as a fiber texture.

  17. Beyond simple small-angle X-ray scattering: developments in online complementary techniques and sample environments.

    PubMed

    Bras, Wim; Koizumi, Satoshi; Terrill, Nicholas J

    2014-11-01

    Small- and wide-angle X-ray scattering (SAXS, WAXS) are standard tools in materials research. The simultaneous measurement of SAXS and WAXS data in time-resolved studies has gained popularity due to the complementary information obtained. Furthermore, the combination of these data with non X-ray based techniques, via either simultaneous or independent measurements, has advanced understanding of the driving forces that lead to the structures and morphologies of materials, which in turn give rise to their properties. The simultaneous measurement of different data regimes and types, using either X-rays or neutrons, and the desire to control parameters that initiate and control structural changes have led to greater demands on sample environments. Examples of developments in technique combinations and sample environment design are discussed, together with a brief speculation about promising future developments.

  18. Measurement of illite particle thickness using a direct Fourier transform of small-angle X-ray scattering data

    USGS Publications Warehouse

    Shang, Chao; Rice, James A.; Eberl, Dennis D.; Lin, Jar-Shyong

    2003-01-01

    It has been suggested that interstratified illite-smectite (I-S) minerals are composed of aggregates of fundamental particles. Many attempts have been made to measure the thickness of such fundamental particles, but each of the methods used suffers from its own limitations and uncertainties. Small-angle X-ray scattering (SAXS) can be used to measure the thickness of particles that scatter X-rays coherently. We used SAXS to study suspensions of Na-rectorite and other illites with varying proportions of smectite. The scattering intensity (I) was recorded as a function of the scattering vector, q = (4 /) sin(/2), where  is the X-ray wavelength and  is the scattering angle. The experimental data were treated with a direct Fourier transform to obtain the pair distance distribution function (PDDF) that was then used to determine the thickness of illite particles. The Guinier and Porod extrapolations were used to obtain the scattering intensity beyond the experimental q, and the effects of such extrapolations on the PDDF were examined. The thickness of independent rectorite particles (used as a reference mineral) is 18.3 Å. The SAXS results are compared with those obtained by X-ray diffraction peak broadening methods. It was found that the power-law exponent (α) obtained by fitting the data in the region of q = 0.1-0.6 nm-1 to the power law (I = I0q-α) is a linear function of illite particle thickness. Therefore, illite particle thickness could be predicted by the linear relationship as long as the thickness is within the limit where α <4.0.

  19. Accurate small and wide angle x-ray scattering profiles from atomic models of proteins and nucleic acids

    NASA Astrophysics Data System (ADS)

    Nguyen, Hung T.; Pabit, Suzette A.; Meisburger, Steve P.; Pollack, Lois; Case, David A.

    2014-12-01

    A new method is introduced to compute X-ray solution scattering profiles from atomic models of macromolecules. The three-dimensional version of the Reference Interaction Site Model (RISM) from liquid-state statistical mechanics is employed to compute the solvent distribution around the solute, including both water and ions. X-ray scattering profiles are computed from this distribution together with the solute geometry. We describe an efficient procedure for performing this calculation employing a Lebedev grid for the angular averaging. The intensity profiles (which involve no adjustable parameters) match experiment and molecular dynamics simulations up to wide angle for two proteins (lysozyme and myoglobin) in water, as well as the small-angle profiles for a dozen biomolecules taken from the BioIsis.net database. The RISM model is especially well-suited for studies of nucleic acids in salt solution. Use of fiber-diffraction models for the structure of duplex DNA in solution yields close agreement with the observed scattering profiles in both the small and wide angle scattering (SAXS and WAXS) regimes. In addition, computed profiles of anomalous SAXS signals (for Rb+ and Sr2+) emphasize the ionic contribution to scattering and are in reasonable agreement with experiment. In cases where an absolute calibration of the experimental data at q = 0 is available, one can extract a count of the excess number of waters and ions; computed values depend on the closure that is assumed in the solution of the Ornstein-Zernike equations, with results from the Kovalenko-Hirata closure being closest to experiment for the cases studied here.

  20. Small angle X-ray scattering analysis of the effect of cold compaction of Al/MoO3 thermite composites.

    PubMed

    Hammons, Joshua A; Wang, Wei; Ilavsky, Jan; Pantoya, Michelle L; Weeks, Brandon L; Vaughn, Mark W

    2008-01-07

    Nanothermites composed of aluminum and molybdenum trioxide (MoO(3)) have a high energy density and are attractive energetic materials. To enhance the surface contact between the spherical Al nanoparticles and the sheet-like MoO(3) particles, the mixture can be cold-pressed into a pelleted composite. However, it was found that the burn rate of the pellets decreased as the density of the pellets increased, contrary to expectation. Ultra-small angle X-ray scattering (USAXS) data and scanning electron microscopy (SEM) were used to elucidate the internal structure of the Al nanoparticles, and nanoparticle aggregate in the composite. Results from both SEM imaging and USAXS analysis indicate that as the density of the pellet increased, a fraction of the Al nanoparticles are compressed into sintered aggregates. The sintered Al nanoparticles lost contrast after forming the larger aggregates and no longer scattered X-rays as individual particles. The sintered aggregates hinder the burn rate, since the Al nanoparticles that make them up can no longer diffuse freely as individual particles during combustion. Results suggest a qualitative relationship for the probability that nanoparticles will sinter, based on the particle sizes and the initial structure of their respective agglomerates, as characterized by the mass fractal dimension.

  1. Quantitative evaluation of statistical errors in small-angle X-ray scattering measurements

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

    Sedlak, Steffen M.; Bruetzel, Linda K.; Lipfert, Jan

    A new model is proposed for the measurement errors incurred in typical small-angle X-ray scattering (SAXS) experiments, which takes into account the setup geometry and physics of the measurement process. The model accurately captures the experimentally determined errors from a large range of synchrotron and in-house anode-based measurements. Its most general formulation gives for the variance of the buffer-subtracted SAXS intensity σ 2(q) = [I(q) + const.]/(kq), whereI(q) is the scattering intensity as a function of the momentum transferq;kand const. are fitting parameters that are characteristic of the experimental setup. The model gives a concrete procedure for calculating realistic measurementmore » errors for simulated SAXS profiles. In addition, the results provide guidelines for optimizing SAXS measurements, which are in line with established procedures for SAXS experiments, and enable a quantitative evaluation of measurement errors.« less

  2. Beyond simple small-angle X-ray scattering: developments in online complementary techniques and sample environments

    PubMed Central

    Bras, Wim; Koizumi, Satoshi; Terrill, Nicholas J

    2014-01-01

    Small- and wide-angle X-ray scattering (SAXS, WAXS) are standard tools in materials research. The simultaneous measurement of SAXS and WAXS data in time-resolved studies has gained popularity due to the complementary information obtained. Furthermore, the combination of these data with non X-ray based techniques, via either simultaneous or independent measurements, has advanced understanding of the driving forces that lead to the structures and morphologies of materials, which in turn give rise to their properties. The simultaneous measurement of different data regimes and types, using either X-rays or neutrons, and the desire to control parameters that initiate and control structural changes have led to greater demands on sample environments. Examples of developments in technique combinations and sample environment design are discussed, together with a brief speculation about promising future developments. PMID:25485128

  3. Small-angle X-ray scattering probe of intermolecular interaction in red blood cells

    NASA Astrophysics Data System (ADS)

    Liu, Guan-Fen; Wang, We-Jia; Xu, Jia-Hua; Dong, Yu-Hui

    2015-03-01

    With high concentrations of hemoglobin (Hb) in red blood cells, self-interactions among these molecules could increase the propensities of their polymerization and aggregation. In the present work, high concentration Hb in solution and red blood cells were analyzed by small-angle X-ray scattering. Calculation of the effective structure factor indicates that the interaction of Hb molecules is the same when they are crowded together in both the cell and physiological saline. The Hb molecules stay individual without the formation of aggregates and clusters in cells. Supported by National Basic Research Program of China (2009CB918600) and National Natural Science Foundation of China (10979005)

  4. Structure of disordered gold-polymer thin films using small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Teixeira, F. S.; Salvadori, M. C.; Cattani, M.; Brown, I. G.

    2010-11-01

    We have investigated the structure of disordered gold-polymer thin films using small angle x-ray scattering and compared the results with the predictions of a theoretical model based on two approaches—a structure form factor approach and the generalized Porod law. The films are formed of polymer-embedded gold nanoclusters and were fabricated by very low energy gold ion implantation into polymethylmethacrylate (PMMA). The composite films span (with dose variation) the transition from electrically insulating to electrically conducting regimes, a range of interest fundamentally and technologically. We find excellent agreement with theory and show that the PMMA-Au films have monodispersive or polydispersive characteristics depending on the implanted ion dose.

  5. Thorough small-angle X-ray scattering analysis of the instability of liquid micro-jets in air.

    PubMed

    Marmiroli, Benedetta; Cacho-Nerin, Fernando; Sartori, Barbara; Pérez, Javier; Amenitsch, Heinz

    2014-01-01

    Liquid jets are of interest, both for their industrial relevance and for scientific applications (more important, in particular for X-rays, after the advent of free-electron lasers that require liquid jets as sample carrier). Instability mechanisms have been described theoretically and by numerical simulation, but confirmed by few experimental techniques. In fact, these are mainly based on cameras, which is limited by the imaging resolution, and on light scattering, which is hindered by absorption, reflection, Mie scattering and multiple scattering due to complex air/liquid interfaces during jet break-up. In this communication it is demonstrated that synchrotron small-angle X-ray scattering (SAXS) can give quantitative information on liquid jet dynamics at the nanoscale, by detecting time-dependent morphology and break-up length. Jets ejected from circular tubes of different diameters (100-450 µm) and speeds (0.7-21 m s(-1)) have been explored to cover the Rayleigh and first wind-induced regimes. Various solvents (water, ethanol, 2-propanol) and their mixtures have been examined. The determination of the liquid jet behaviour becomes essential, as it provides background data in subsequent studies of chemical and biological reactions using SAXS or X-ray diffraction based on synchrotron radiation and free-electron lasers.

  6. Probing He bubbles in naturally aged and annealed δ-Pu alloys using ultra-small-angle x-ray scattering

    DOE PAGES

    Jeffries, J. R.; Hammons, J. A.; Willey, T. M.; ...

    2017-10-31

    We report the self-irradiation of Pu alloys generates He that is trapped within the metal matrix in the form of He bubbles. The distribution of these He bubbles in δ-phase Pu-Ga alloys exhibits a peak near a radius of 0.7 nm, and this size is remarkably stable as function of time. When annealed, the He bubbles in δ-Pu alloys grow, coarsening the distribution. However, the magnitude of this coarsening is uncertain, as different experimental methods reveal bubbles that differ by at least one order of magnitude. Small-angle x-ray scattering results, which can probe a wide range of bubble sizes, implymore » only a mild coarsening of the He bubble distribution for an annealing treatment of 425 °C for 24 h, and analysis of the He bubble content suggests that He is actually lost from the bubbles with annealing.« less

  7. Carbon Condensation during High Explosive Detonation with Time Resolved Small Angle X-ray Scattering

    NASA Astrophysics Data System (ADS)

    Hammons, Joshua; Bagge-Hansen, Michael; Nielsen, Michael; Lauderbach, Lisa; Hodgin, Ralph; Bastea, Sorin; Fried, Larry; May, Chadd; Sinclair, Nicholas; Jensen, Brian; Gustavsen, Rick; Dattelbaum, Dana; Watkins, Erik; Firestone, Millicent; Ilavsky, Jan; van Buuren, Tony; Willey, Trevor; Lawrence Livermore National Lab Collaboration; Los Alamos National Laboratory Collaboration; Washington State University/Advanced Photon Source Team

    Carbon condensation during high-energy detonations occurs under extreme conditions and on very short time scales. Understanding and manipulating soot formation, particularly detonation nanodiamond, has attracted the attention of military, academic and industrial research. An in-situ characterization of these nanoscale phases, during detonation, is highly sought after and presents a formidable challenge even with today's instruments. Using the high flux available with synchrotron X-rays, pink beam small angle X-ray scattering is able to observe the carbon phases during detonation. This experimental approach, though powerful, requires careful consideration and support from other techniques, such as post-mortem TEM, EELS and USAXS. We present a comparative survey of carbon condensation from different CHNO high explosives. This work was performed under the auspices of the US DOE by LLNL under Contract DE-AC52-07NA27344.

  8. Six-dimensional real and reciprocal space small-angle X-ray scattering tomography

    NASA Astrophysics Data System (ADS)

    Schaff, Florian; Bech, Martin; Zaslansky, Paul; Jud, Christoph; Liebi, Marianne; Guizar-Sicairos, Manuel; Pfeiffer, Franz

    2015-11-01

    When used in combination with raster scanning, small-angle X-ray scattering (SAXS) has proven to be a valuable imaging technique of the nanoscale, for example of bone, teeth and brain matter. Although two-dimensional projection imaging has been used to characterize various materials successfully, its three-dimensional extension, SAXS computed tomography, poses substantial challenges, which have yet to be overcome. Previous work using SAXS computed tomography was unable to preserve oriented SAXS signals during reconstruction. Here we present a solution to this problem and obtain a complete SAXS computed tomography, which preserves oriented scattering information. By introducing virtual tomography axes, we take advantage of the two-dimensional SAXS information recorded on an area detector and use it to reconstruct the full three-dimensional scattering distribution in reciprocal space for each voxel of the three-dimensional object in real space. The presented method could be of interest for a combined six-dimensional real and reciprocal space characterization of mesoscopic materials with hierarchically structured features with length scales ranging from a few nanometres to a few millimetres—for example, biomaterials such as bone or teeth, or functional materials such as fuel-cell or battery components.

  9. Six-dimensional real and reciprocal space small-angle X-ray scattering tomography.

    PubMed

    Schaff, Florian; Bech, Martin; Zaslansky, Paul; Jud, Christoph; Liebi, Marianne; Guizar-Sicairos, Manuel; Pfeiffer, Franz

    2015-11-19

    When used in combination with raster scanning, small-angle X-ray scattering (SAXS) has proven to be a valuable imaging technique of the nanoscale, for example of bone, teeth and brain matter. Although two-dimensional projection imaging has been used to characterize various materials successfully, its three-dimensional extension, SAXS computed tomography, poses substantial challenges, which have yet to be overcome. Previous work using SAXS computed tomography was unable to preserve oriented SAXS signals during reconstruction. Here we present a solution to this problem and obtain a complete SAXS computed tomography, which preserves oriented scattering information. By introducing virtual tomography axes, we take advantage of the two-dimensional SAXS information recorded on an area detector and use it to reconstruct the full three-dimensional scattering distribution in reciprocal space for each voxel of the three-dimensional object in real space. The presented method could be of interest for a combined six-dimensional real and reciprocal space characterization of mesoscopic materials with hierarchically structured features with length scales ranging from a few nanometres to a few millimetres--for example, biomaterials such as bone or teeth, or functional materials such as fuel-cell or battery components.

  10. Measurement of carbon condensates using small-angle x-ray scattering during detonation of high explosives

    NASA Astrophysics Data System (ADS)

    Willey, T. M.; Bagge-Hansen, M.; Lauderbach, L.; Hodgin, R.; Hansen, D.; May, C.; van Buuren, T.; Dattelbaum, D. M.; Gustavsen, R. L.; Watkins, E. B.; Firestone, M. A.; Jensen, B. J.; Graber, T.; Bastea, S.; Fried, L.

    2017-01-01

    The lack of experimental validation for processes occurring at sub-micron length scales on time scales ranging from nanoseconds to microseconds hinders detonation model development. Particularly, quantification of late-time energy release requires measurement of carbon condensation kinetics behind detonation fronts. A new small-angle x-ray scattering (SAXS) endstation has been developed for use at The Dynamic Compression Sector to observe carbon condensation during detonation. The endstation and beamline demonstrate unprecedented fidelity; SAXS profiles can be acquired from single x-ray pulses, which in 24-bunch mode are about 80 ps in duration and arrive every 153.4 ns. This paper presents both the current temporal capabilities of this beamline, and the ability to distinguish different carbon condensate morphologies as they form behind detonation fronts. To demonstrate temporal capabilities, three shots acquired during detonation of hexanitrostilbene (HNS) are interleaved to show the evolution of the SAXS in about 50 ns steps. To show fidelity of the SAXS, the scattering from carbon condensates at several hundred nanoseconds varies with explosive: scattering from HNS is consistent with a complex morphology that we assert is associated with sp2 carbon., while Comp B scattering is consistent with soots containing three-dimensional diamond nanoparticles.

  11. Nonuniformity in natural rubber as revealed by small-angle neutron scattering, small-angle X-ray scattering, and atomic force microscopy.

    PubMed

    Karino, Takeshi; Ikeda, Yuko; Yasuda, Yoritaka; Kohjiya, Shinzo; Shibayama, Mitsuhiro

    2007-02-01

    The microscopic structures of natural rubber (NR) and deproteinized NR (DPNR) were investigated by means of small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), and atomic force microscopy (AFM). They were compared to those of isoprene rubber (IR), which is a synthetic analogue of NR in terms of chemical structure without any non-rubber components like proteins. Comparisons of the structure and mechanical properties of NR, DPNR, and IR lead to the following conclusions. (i) The well-known facts, for example, the outstanding green strength of NR and strain-induced crystallization, are due not much to the presence of proteins but to other components such as the presence of phospholipids and/or the higher stereoregularity of NR. It also became clear the naturally residing proteins accelerate the upturn of stress at low strain. The protein phases work as cross-linking sites and reinforcing fillers in the rubbery matrix. (ii) The microscopic structures of NR were successfully reproduced by SANS intensity functions consisting of squared-Lorentz and Lorentz functions, indicating the presence of inhomogeneities in bulk and thermal concentration fluctuations in swollen state, respectively. On the other hand, IR rubbers were homogeneous in bulk. (iii) The inhomogeneities in NR are assigned to protein aggregates of the order of 200 A or larger. Although these aggregates are larger in size as well as in volume fraction than those of cross-link inhomogeneities introduced by cross-linking, they are removed by deproteinization. (iv) Swelling of both NR and IR networks introduces gel-like concentration fluctuations whose mesh size is of the order of 20 A.

  12. Preparing Monodisperse Macromolecular Samples for Successful Biological Small-Angle X-ray and Neutron Scattering Experiments

    PubMed Central

    Jeffries, Cy M.; Graewert, Melissa A.; Blanchet, Clément E.; Langley, David B.; Whitten, Andrew E.; Svergun, Dmitri I

    2017-01-01

    Small-angle X-ray and neutron scattering (SAXS and SANS) are techniques used to extract structural parameters and determine the overall structures and shapes of biological macromolecules, complexes and assemblies in solution. The scattering intensities measured from a sample contain contributions from all atoms within the illuminated sample volume including the solvent and buffer components as well as the macromolecules of interest. In order to obtain structural information, it is essential to prepare an exactly matched solvent blank so that background scattering contributions can be accurately subtracted from the sample scattering to obtain the net scattering from the macromolecules in the sample. In addition, sample heterogeneity caused by contaminants, aggregates, mismatched solvents, radiation damage or other factors can severely influence and complicate data analysis so it is essential that the samples are pure and monodisperse for the duration of the experiment. This Protocol outlines the basic physics of SAXS and SANS and reveals how the underlying conceptual principles of the techniques ultimately ‘translate’ into practical laboratory guidance for the production of samples of sufficiently high quality for scattering experiments. The procedure describes how to prepare and characterize protein and nucleic acid samples for both SAXS and SANS using gel electrophoresis, size exclusion chromatography and light scattering. Also included are procedures specific to X-rays (in-line size exclusion chromatography SAXS) and neutrons, specifically preparing samples for contrast matching/variation experiments and deuterium labeling of proteins. PMID:27711050

  13. Measuring helium bubble diameter distributions in tungsten with grazing incidence small angle x-ray scattering (GISAXS)

    NASA Astrophysics Data System (ADS)

    Thompson, M.; Kluth, P.; Doerner, R. P.; Kirby, N.; Riley, D.; Corr, C. S.

    2016-02-01

    Grazing incidence small angle x-ray scattering was performed on tungsten samples exposed to helium plasma in the MAGPIE and Pisces-A linear plasma devices to measure the size distributions of resulting helium nano-bubbles. Nano-bubbles were fitted assuming spheroidal particles and an exponential diameter distribution. These particles had mean diameters between 0.36 and 0.62 nm. Pisces-A exposed samples showed more complex patterns, which may suggest the formation of faceted nano-bubbles or nano-scale surface structures.

  14. Irena : tool suite for modeling and analysis of small-angle scattering.

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

    Ilavsky, J.; Jemian, P.

    2009-04-01

    Irena, a tool suite for analysis of both X-ray and neutron small-angle scattering (SAS) data within the commercial Igor Pro application, brings together a comprehensive suite of tools useful for investigations in materials science, physics, chemistry, polymer science and other fields. In addition to Guinier and Porod fits, the suite combines a variety of advanced SAS data evaluation tools for the modeling of size distribution in the dilute limit using maximum entropy and other methods, dilute limit small-angle scattering from multiple non-interacting populations of scatterers, the pair-distance distribution function, a unified fit, the Debye-Bueche model, the reflectivity (X-ray and neutron)more » using Parratt's formalism, and small-angle diffraction. There are also a number of support tools, such as a data import/export tool supporting a broad sampling of common data formats, a data modification tool, a presentation-quality graphics tool optimized for small-angle scattering data, and a neutron and X-ray scattering contrast calculator. These tools are brought together into one suite with consistent interfaces and functionality. The suite allows robust automated note recording and saving of parameters during export.« less

  15. Alzheimer's disease imaging biomarkers using small-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Choi, Mina; Alam, Nadia; Dahal, Eshan; Ghammraoui, Bahaa; Badano, Aldo

    2016-03-01

    There is a need for novel imaging techniques for the earlier detection of Alzheimer's disease (AD). Two hallmarks of AD are amyloid beta (Aβ) plaques and tau tangles that are formed in the brain. Well-characterized x-ray cross sections of Aβ and tau proteins in a variety of structural states could potentially be used as AD biomarkers for small-angle x-ray scattering (SAXS) imaging without the need for injectable probes or contrast agents. First, however, the protein structures must be controlled and measured to determine accurate biomarkers for SAXS imaging. Here we report SAXS measurements of Aβ42 and tau352 in a 50% dimethyl sulfoxide (DMSO) solution in which these proteins are believed to remain monomeric because of the stabilizing interaction of DMSO solution. Our SAXS analysis showed the aggregation of both proteins. In particular, we found that the aggregation of Aβ42 slowly progresses with time in comparison to tau352 that aggregates at a faster rate and reaches a steady-state. Furthermore, the measured signals were compared to the theoretical SAXS profiles of Aβ42 monomer, Aβ42 fibril, and tau352 that were computed from their respective protein data bank structures. We have begun the work to systematically control the structural states of these proteins in vitro using various solvent conditions. Our future work is to utilize the distinct SAXS profiles of various structural states of Aβ and tau to build a library of signals of interest for SAXS imaging in brain tissue.

  16. Large-angle x-ray scatter in Talbot-Lau interferometry for breast imaging

    PubMed Central

    Vedantham, Srinivasan; Shi, Linxi; Karellas, Andrew

    2014-01-01

    Monte Carlo simulations were used to investigate large-angle x-ray scatter at design energy of 25 keV during small field of view (9.6 cm × 5 cm) differential phase contrast imaging of the breast using Talbot-Lau interferometry. Homogenous, adipose and fibroglandular breasts of uniform thickness ranging from 2 to 8 cm encompassing the field of view were modeled. Theoretically determined transmission efficiencies of the gratings were used to validate the Monte Carlo simulations, followed by simulations to determine the x-ray scatter reaching the detector. The recorded x-ray scatter was classified into x-ray photons that underwent at least one Compton interaction (incoherent scatter) and Rayleigh interaction alone (coherent scatter) for further analysis. Monte Carlo based estimates of transmission efficiencies showed good correspondence (r2 > 0.99) with theoretical estimates. Scatter-to-primary ratio increased with increasing breast thickness, ranging from 0.11 to 0.22 for 2 to 8 cm thick adipose breasts and from 0.12 to 0.28 for 2 to 8 cm thick fibroglandular breasts. The analyzer grating reduced incoherent scatter by ~18% for 2 cm thick adipose breast and by ~35% for 8 cm thick fibroglandular breast. Coherent scatter was the dominant contributor to the total scatter. Coherent-to-incoherent scatter ratio ranged from 2.2 to 3.1 for 2 to 8 cm thick adipose breasts and from 2.7 to 3.4 for 2 to 8 cm thick fibroglandular breasts. PMID:25295630

  17. X-ray scattering study

    NASA Technical Reports Server (NTRS)

    Wriston, R. S.; Froechtenigt, J. F.

    1972-01-01

    A soft X-ray glancing incidence telescope mirror and a group of twelve optical flat samples were used to study the scattering of X-rays. The mirror was made of Kanigen coated beryllium and the images produced were severely limited by scattering of X-rays. The best resolution attained was about fifteen arc seconds. The telescope efficiency was found to be 0.0006. The X-ray beam reflected from the twelve optical flat samples was analyzed by means of a long vacuum system of special design for these tests. The scattering then decreased with increasing angle of incidence until a critical angle was passed. At larger angles the scattering increased again. The samples all scattered more at 44 A than at 8 A. Metal samples were found to have about the same scattering at 44 A but greater scattering at 8 A than glass samples.

  18. X-ray diffraction gratings: Precise control of ultra-low blaze angle via anisotropic wet etching

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

    Voronov, Dmitriy L.; Naulleau, Patrick; Gullikson, Eric M.

    2016-07-25

    Diffraction gratings are used from micron to nanometer wavelengths as dispersing elements in optical instruments. At shorter wavelengths, crystals can be used as diffracting elements, but due to the 3D nature of the interaction with light are wavelength selective rather than wavelength dispersing. There is an urgent need to extend grating technology into the x-ray domain of wavelengths from 1 to 0.1 nm, but this requires the use of gratings that have a faceted surface in which the facet angles are very small, typically less than 1°. Small facet angles are also required in the extreme ultra-violet and soft x-ray energymore » ranges in free electron laser applications, in order to reduce power density below a critical damage threshold. In this work, we demonstrate a technique based on anisotropic etching of silicon designed to produce very small angle facets with a high degree of perfection.« less

  19. A Mo-anode-based in-house source for small-angle X-ray scattering measurements of biological macromolecules

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

    Bruetzel, Linda K.; Fischer, Stefan; Salditt, Annalena

    2016-02-15

    We demonstrate the use of a molybdenum-anode-based in-house small-angle X-ray scattering (SAXS) setup to study biological macromolecules in solution. Our system consists of a microfocus X-ray tube delivering a highly collimated flux of 2.5 × 10{sup 6} photons/s at a beam size of 1.2 × 1.2 mm{sup 2} at the collimation path exit and a maximum beam divergence of 0.16 mrad. The resulting observable scattering vectors q are in the range of 0.38 Å{sup −1} down to 0.009 Å{sup −1} in SAXS configuration and of 0.26 Å{sup −1} up to 5.7 Å{sup −1} in wide-angle X-ray scattering (WAXS) mode. Tomore » determine the capabilities of the instrument, we collected SAXS data on weakly scattering biological macromolecules including proteins and a nucleic acid sample with molecular weights varying from ∼12 to 69 kDa and concentrations of 1.5–24 mg/ml. The measured scattering data display a high signal-to-noise ratio up to q-values of ∼0.2 Å{sup −1} allowing for an accurate structural characterization of the samples. Moreover, the in-house source data are of sufficient quality to perform ab initio 3D structure reconstructions that are in excellent agreement with the available crystallographic structures. In addition, measurements for the detergent decyl-maltoside show that the setup can be used to determine the size, shape, and interactions (as characterized by the second virial coefficient) of detergent micelles. This demonstrates that the use of a Mo-anode based in-house source is sufficient to determine basic geometric parameters and 3D shapes of biomolecules and presents a viable alternative to valuable beam time at third generation synchrotron sources.« less

  20. In-situ small angle x-ray scattering investigation on nucleation and growth of silica colloids

    NASA Astrophysics Data System (ADS)

    Bahadur, J.; Tripathi, B. M.; Prakash, J.; Das, Avik; Sen, D.; Mazumder, S.

    2018-04-01

    The nucleation and growth of silica colloids has been studied using real time small-angle X-ray scattering measurements. The ammonium fluorosilicate was used as precursor and both weak (NH3) and strong base (NaOH) has been used as reducing agent for the precursor. It is observed that nucleation, growth and aggregation phenomenon occur simultaneously. The kinetics of the nucleation and growth of silica colloids depends on the strength of the reducing agent as well on its concentration. The kinetics is slow for NH3 but is very fast for higher concentration of NaOH.

  1. Joint small-angle X-ray and neutron scattering data analysis of asymmetric lipid vesicles

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

    Eicher, Barbara; Heberle, Frederick A.; Marquardt, Drew T.

    2017-02-28

    Low- and high-resolution models describing the internal transbilayer structure of asymmetric lipid vesicles have been developed. These models can be used for the joint analysis of small-angle neutron and X-ray scattering data. The models describe the underlying scattering length density/electron density profiles either in terms of slabs or through the so-called scattering density profile, previously applied to symmetric lipid vesicles. Both models yield structural details of asymmetric membranes, such as the individual area per lipid, and the hydrocarbon thickness of the inner and outer bilayer leaflets. The scattering density profile model, however, comes at a cost of increased computational effortmore » but results in greater structural resolution, showing a slightly lower packing of lipids in the outer bilayer leaflet of ~120 nm diameter palmitoyloleoyl phosphatidylcholine (POPC) vesicles, compared to the inner leaflet. Here, analysis of asymmetric dipalmitoyl phosphatidylcholine/POPC vesicles did not reveal evidence of transbilayer coupling between the inner and outer leaflets at 323 K, i.e.above the melting transition temperature of the two lipids.« less

  2. Use of dynamic light scattering and small-angle X-ray scattering to characterize new surfactants in solution conditions for membrane-protein crystallization

    PubMed Central

    Dahani, Mohamed; Barret, Laurie-Anne; Raynal, Simon; Jungas, Colette; Pernot, Pétra; Polidori, Ange; Bonneté, Françoise

    2015-01-01

    The structural and interactive properties of two novel hemifluorinated surfactants, F2H9-β-M and F4H5-β-M, the syntheses of which were based on the structure and hydrophobicity of the well known dodecyl-β-maltoside (DD-β-M), are described. The shape of their micellar assemblies was characterized by small-angle X-ray scattering and their intermicellar inter­actions in crystallizing conditions were measured by dynamic light scattering. Such information is essential for surfactant phase-diagram determination and membrane-protein crystallization. PMID:26144228

  3. Ultra-small-angle neutron scattering with azimuthal asymmetry

    DOE PAGES

    Gu, X.; Mildner, D. F. R.

    2016-05-16

    Small-angle neutron scattering (SANS) measurements from thin sections of rock samples such as shales demand as great a scattering vector range as possible because the pores cover a wide range of sizes. The limitation of the scattering vector range for pinhole SANS requires slit-smeared ultra-SANS (USANS) measurements that need to be converted to pinhole geometry. The desmearing algorithm is only successful for azimuthally symmetric data. Scattering from samples cut parallel to the plane of bedding is symmetric, exhibiting circular contours on a two-dimensional detector. Samples cut perpendicular to the bedding show elliptically dependent contours with the long axis corresponding tomore » the normal to the bedding plane. A method is given for converting such asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry SANS data. Furthermore, the aspect ratio from the SANS data is used to modify the slit-smeared USANS data to produce quasi-symmetric contours. Rotation of the sample about the incident beam may result in symmetric data but cannot extract the same information as obtained from pinhole geometry.« less

  4. Ultra-small-angle neutron scattering with azimuthal asymmetry

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

    Gu, X.; Mildner, D. F. R.

    Small-angle neutron scattering (SANS) measurements from thin sections of rock samples such as shales demand as great a scattering vector range as possible because the pores cover a wide range of sizes. The limitation of the scattering vector range for pinhole SANS requires slit-smeared ultra-SANS (USANS) measurements that need to be converted to pinhole geometry. The desmearing algorithm is only successful for azimuthally symmetric data. Scattering from samples cut parallel to the plane of bedding is symmetric, exhibiting circular contours on a two-dimensional detector. Samples cut perpendicular to the bedding show elliptically dependent contours with the long axis corresponding tomore » the normal to the bedding plane. A method is given for converting such asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry SANS data. Furthermore, the aspect ratio from the SANS data is used to modify the slit-smeared USANS data to produce quasi-symmetric contours. Rotation of the sample about the incident beam may result in symmetric data but cannot extract the same information as obtained from pinhole geometry.« less

  5. Synthesis and Small-Angle X-Ray Scattering Investigations of Ureido-Pyrimidone Hydrogen Bonding Star and Linear Poly(ethylene-co-propylene)s

    DTIC Science & Technology

    2006-02-01

    Synthesis and Small-Angle X-ray Scattering Investigations of Ureido- Pyrimidone Hydrogen Bonding Star and Linear Poly(ethylene-co-propylene)s...Scattering Investigations of Ureido- Pyrimidone Hydrogen Bonding Star and Linear Poly(ethylene-co-propylene)s Frederick L. Beyer Weapons and...control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS. 1. REPORT DATE (DD-MM-YYYY) February 2006 2 . REPORT TYPE Interim 3. DATES

  6. 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

  7. The measurement capabilities of cross-sectional profile of Nanoimprint template pattern using small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Yamanaka, Eiji; Taniguchi, Rikiya; Itoh, Masamitsu; Omote, Kazuhiko; Ito, Yoshiyasu; Ogata, Kiyoshi; Hayashi, Naoya

    2016-05-01

    Nanoimprint lithography (NIL) is one of the most potential candidates for the next generation lithography for semiconductor. It will achieve the lithography with high resolution and low cost. High resolution of NIL will be determined by a high definition template. Nanoimprint lithography will faithfully transfer the pattern of NIL template to the wafer. Cross-sectional profile of the template pattern will greatly affect the resist profile on the wafer. Therefore, the management of the cross-sectional profile is essential. Grazing incidence small angle x-ray scattering (GI-SAXS) technique has been proposed as one of the method for measuring cross-sectional profile of periodic nanostructure pattern. Incident x-rays are irradiated to the sample surface with very low glancing angle. It is close to the critical angle of the total reflection of the x-ray. The scattered x-rays from the surface structure are detected on a two-dimensional detector. The observed intensity is discrete in the horizontal (2θ) direction. It is due to the periodicity of the structure, and diffraction is observed only when the diffraction condition is satisfied. In the vertical (β) direction, the diffraction intensity pattern shows interference fringes reflected to height and shape of the structure. Features of the measurement using x-ray are that the optical constant for the materials are well known, and it is possible to calculate a specific diffraction intensity pattern based on a certain model of the cross-sectional profile. The surface structure is estimated by to collate the calculated diffraction intensity pattern that sequentially while changing the model parameters with the measured diffraction intensity pattern. Furthermore, GI-SAXS technique can be measured an object in a non-destructive. It suggests the potential to be an effective tool for product quality assurance. We have developed a cross-sectional profile measurement of quartz template pattern using GI-SAXS technique. In this

  8. Small angle x-ray scattering study on the conformation of polystyrene in toluene during adding anti-solvent CO2

    NASA Astrophysics Data System (ADS)

    Liu, Yi; Chen, Dong-Feng; Wang, Hong-Li; Chen, Na; Li, Dan; Han, Bu-Xing; Rong, Li-Xia; Zhao, Hui; Wang, Jun; Dong, Bao-Zhong

    2002-10-01

    The conformation of polystyrene in the anti-solvent process of supercritical fluids (compressed CO2 + polystyrene + toluene) has been studied by small angle x-ray scattering with synchrotron radiation as an x-ray source. Coil-to-globule transformation of the polystyrene chain was observed with the increase of the anti-solvent CO2 pressure; i.e. polystyrene coiled at a pressure lower than the cloud point pressure (Pc) and turned into a globule with a uniform density at pressures higher than Pc. Fractal behaviour was also found in the chain contraction and the mass fractal dimension increased with increasing CO2 pressure.

  9. Small-angle x-ray scattering measurement of a mist of ethanol nanodroplets: An approach to understanding ultrasonic separation of ethanol-water mixtures

    NASA Astrophysics Data System (ADS)

    Yano, Yohko F.; Matsuura, Kazuo; Fukazu, Tetsuo; Abe, Fusatsugu; Wakisaka, Akihiro; Kobara, Hitomi; Kaneko, Kazuyuki; Kumagai, Atsushi; Katsuya, Yoshio; Tanaka, Masahiko

    2007-07-01

    Small-angle x-ray scattering measurements using a brilliant x-ray source revealed nanometer sized liquid droplets in a mist formed by ultrasonic atomization. Ultrasonic atomization of ethanol-water mixtures produced a combination of water-rich droplets of micrometer order and ethanol-rich droplets as small as 1nm, which is 10-3 times smaller than the predicted size. These sizes were also obtained for mists generated from the pure liquids. These results will help to clarify the mechanism of "ultrasonic ethanol separation," which has the potential to become an alternative to distillation.

  10. Small-angle x-ray scattering study of polymer structure: Carbosilane dendrimers in hexane solution

    NASA Astrophysics Data System (ADS)

    Shtykova, E. V.; Feigin, L. A.; Volkov, V. V.; Malakhova, Yu. N.; Streltsov, D. R.; Buzin, A. I.; Chvalun, S. N.; Katarzhanova, E. Yu.; Ignatieva, G. M.; Muzafarov, A. M.

    2016-09-01

    The three-dimensional organization of monodisperse hyper-branched macromolecules of regular structure—carbosilane dendrimers of zero, third, and sixth generations—has been studied by small-angle X-ray scattering (SAXS) in solution. The use of modern methods of SAXS data interpretation, including ab initio modeling, has made it possible to determine the internal architecture of the dendrimers in dependence of the generation number and the number of cyclosiloxane end groups (forming the shell of dendritic macromolecules) and show dendrimers to be spherical. The structural results give grounds to consider carbosilane dendrimers promising objects for forming crystals with subsequent structural analysis and determining their structure with high resolution, as well as for designing new materials to be used in various dendrimer-based technological applications.

  11. A potential for overestimating the absolute magnitudes of second virial coefficients by small-angle X-ray scattering.

    PubMed

    Scott, David J; Patel, Trushar R; Winzor, Donald J

    2013-04-15

    Theoretical consideration is given to the effect of cosolutes (including buffer and electrolyte components) on the determination of second virial coefficients for proteins by small-angle X-ray scattering (SAXS)-a factor overlooked in current analyses in terms of expressions for a two-component system. A potential deficiency of existing practices is illustrated by reassessment of published results on the effect of polyethylene glycol concentration on the second virial coefficient for urate oxidase. This error reflects the substitution of I(0,c3,0), the scattering intensity in the limit of zero scattering angle and solute concentration, for I(0,0,0), the corresponding parameter in the limit of zero cosolute concentration (c3) as well. Published static light scattering results on the dependence of the apparent molecular weight of ovalbumin on buffer concentration are extrapolated to zero concentration to obtain the true value (M2) and thereby establish the feasibility of obtaining the analogous SAXS parameter, I(0,0,0), experimentally. Copyright © 2013 Elsevier Inc. All rights reserved.

  12. All-atom ensemble modeling to analyze small angle X-ray scattering of glycosylated proteins

    PubMed Central

    Guttman, Miklos; Weinkam, Patrick; Sali, Andrej; Lee, Kelly K.

    2013-01-01

    Summary The flexible and heterogeneous nature of carbohydrate chains often renders glycoproteins refractory to traditional structure determination methods. Small Angle X-ray scattering (SAXS) can be a useful tool for obtaining structural information of these systems. All-atom modeling of glycoproteins with flexible glycan chains was applied to interpret the solution SAXS data for a set of glycoproteins. For simpler systems (single glycan, with a well defined protein structure), all-atom modeling generates models in excellent agreement with the scattering pattern, and reveals the approximate spatial occupancy of the glycan chain in solution. For more complex systems (several glycan chains, or unknown protein substructure), the approach can still provide insightful models, though the orientations of glycans become poorly determined. Ab initio shape reconstructions appear to capture the global morphology of glycoproteins, but in most cases offer little information about glycan spatial occupancy. The all-atom modeling methodology is available as a webserver at http://modbase.compbio.ucsf.edu/allosmod-foxs. PMID:23473666

  13. Free jet micromixer to study fast chemical reactions by small angle X-ray scattering.

    PubMed

    Marmiroli, Benedetta; Grenci, Gianluca; Cacho-Nerin, Fernando; Sartori, Barbara; Ferrari, Enrico; Laggner, Peter; Businaro, Luca; Amenitsch, Heinz

    2009-07-21

    We present the design, fabrication process, and the first test results of a high aspect ratio micromixer combined with a free jet for under 100 micros time resolved studies of chemical reactions. The whole system has been optimized for synchrotron small angle X-ray scattering (SAXS) experiments. These studies are of particular interest to understand the early stages of chemical reactions, such as the kinetics of nanoparticle formation. The mixer is based on hydrodynamic focusing and works in the laminar regime. The use of a free jet overcomes the fouling of the channels and simultaneously circumvents background scattering from the walls. The geometrical parameters of the device have been optimized using finite element simulations, resulting in smallest features with radius <1 microm, and a channel depth of 60 microm, thus leading to an aspect ratio >60. To achieve the desired dimensions deep X-ray lithography (DXRL) has been employed. The device has been tested. First the focusing effect has been visualized using fluorescein. Then the evolution and stability of the jet, which exits the mixer nozzle at 13 m s(-1), have been characterized. Finally SAXS measurements have been conducted of the formation of calcium carbonate from calcium chloride and sodium carbonate. The fastest measurement is 75 micros after the beginning of the mixing of the reagents. The nanostructural evolution of chemical reactions is clearly discernible.

  14. Study of the gel films of Acetobacter Xylinum cellulose and its modified samples by {sup 1}H NMR cryoporometry and small-angle X-ray scattering

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

    Babushkina, T. A.; Klimova, T. P.; Shtykova, E. V.

    2010-03-15

    Gel films of Acetobacter Xylinum cellulose and its modified samples have been investigated by 1H nuclear magnetic resonance (NMR) cryoporometry and small-angle X-ray scattering. The joint use of these two methods made it possible to characterize the sizes of aqueous pores in gel films and estimate the sizes of structural inhomogeneities before and after the sorption of polyvinylpyrrolidone and Se{sub 0} nanoparticles (stabilized by polyvinylpyrrolidone) into the films. According to small-angle X-ray scattering data, the sizes of inhomogeneities in a gel film change only slightly upon the sorption of polyvinylpyrrolidone and nanoparticles. The impregnated material is sorbed into water-filled cavitiesmore » that are present in the gel film. {sup 1}H NMR cryoporometry allowed us to reveal the details of changes in the sizes of small aqueous pores during modifications.« less

  15. Element-selective investigation of domain structure in CoPd and FePd alloys using small-angle soft X-ray scattering

    NASA Astrophysics Data System (ADS)

    Weier, C.; Adam, R.; Frömter, R.; Bach, J.; Winkler, G.; Kobs, A.; Oepen, H. P.; Grychtol, P.; Kapteyn, H. C.; Murnane, M. M.; Schneider, C. M.

    2014-03-01

    Recent optical pump-probe experiments on magnetic multilayers and alloys identified perpendicular spin superdiffusion as one of possible mechanisms responsible for femtosecond magnetization dynamics. On the other hand, no strong evidence for the ultrafast lateral spin transport has been reported, so far. To address this question, we studied magnetic domain structure of CoPd and FePd thin films using small-angle scattering of soft X-rays. By tuning the synchrotron-generated X-rays to the absorption edges of Fe or Co we recorded Fourier images of the magnetic domain structure corresponding to a chosen element. Applying in - situ magnetic fields resulted in pronounced rearrangement of domain structure that was clearly observed in scattering images. Our analysis of both the stand-alone, as well as magnetically coupled CoPd/FePd layers provides insight into the formation of domains under small magnetic field perturbations and pave the way to better understanding of transient changes expected in magneto-dynamic measurements.

  16. 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

  17. Time-resolved Small Angle X-ray Scattering During the Formation of Detonation Nano-Carbon Condensates

    NASA Astrophysics Data System (ADS)

    Bagge-Hansen, Michael; Hammons, Josh; Nielsen, Mike; Lauderbach, Lisa; Hodgin, Ralph; Bastea, Sorin; van Buuren, Tony; Pagoria, Phil; May, Chadd; Jensen, Brian; Gustavsen, Rick; Watkins, Erik; Firestone, Millie; Dattelbaum, Dana; Fried, Larry; Cowan, Matt; Willey, Trevor

    2017-06-01

    Carbon nanomaterials are spontaneously generated under high pressure and temperature conditions present during the detonation of many high explosive (HE) materials. Thermochemical modeling suggests that the phase, size, and morphology of carbon condensates are strongly dependent on the type of HE used and associated evolution of temperature and pressure during the very early stages of detonation. Experimental validation of carbon condensation under these extreme conditions has been technically challenging. Here, we present synchrotron-based, time-resolved small-angle x-ray scattering (TR-SAXS) measurements collected during HE detonations, acquired from discrete sub-100 ps x-ray pulses, every 153.4 ns. We select from various HE materials and geometries to explore a range of achievable pressures and temperatures that span detonation conditions and, correspondingly, generate an array of nano-carbon products, including nano-diamonds and nano-onions. The TR-SAXS patterns evolve rapidly over the first few hundred nanoseconds. Comparing the results with modeling offers significant progress towards a general carbon equation of state. Prepared by LLNL under Contract DE-AC52-07NA27344.

  18. Antibodies under pressure: A Small-Angle X-ray Scattering study of Immunoglobulin G under high hydrostatic pressure.

    PubMed

    König, Nico; Paulus, Michael; Julius, Karin; Schulze, Julian; Voetz, Matthias; Tolan, Metin

    2017-12-01

    In the present work two subclasses of the human antibody Immunoglobulin G (IgG) have been investigated by Small-Angle X-ray Scattering under high hydrostatic pressures up to 5kbar. It is shown that IgG adopts a symmetric T-shape in solution which differs significantly from available crystal structures. Moreover, high-pressure experiments verify the high stability of the IgG molecule. It is not unfolded by hydrostatic pressures of up to 5kbar but a slight increase of the radius of gyration was observed at elevated pressures. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering

    PubMed Central

    Mitropoulos, Athanasios Ch.; Favvas, Evangelos P.; Stefanopoulos, Konstantinos L.; Vansant, Etienne F.

    2016-01-01

    Everett’s theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS) supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a) at a common point the system can reach in a finite (not an infinite) number of ways, b) a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c) the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM). Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed. PMID:27741263

  20. An Optimized Table-Top Small-Angle X-ray Scattering Set-up for the Nanoscale Structural Analysis of Soft Matter

    NASA Astrophysics Data System (ADS)

    Sibillano, T.; de Caro, L.; Altamura, D.; Siliqi, D.; Ramella, M.; Boccafoschi, F.; Ciasca, G.; Campi, G.; Tirinato, L.; di Fabrizio, E.; Giannini, C.

    2014-11-01

    The paper shows how a table top superbright microfocus laboratory X-ray source and an innovative restoring-data algorithm, used in combination, allow to analyze the super molecular structure of soft matter by means of Small Angle X-ray Scattering ex-situ experiments. The proposed theoretical approach is aimed to restore diffraction features from SAXS profiles collected from low scattering biomaterials or soft tissues, and therefore to deal with extremely noisy diffraction SAXS profiles/maps. As biological test cases we inspected: i) residues of exosomes' drops from healthy epithelial colon cell line and colorectal cancer cells; ii) collagen/human elastin artificial scaffolds developed for vascular tissue engineering applications; iii) apoferritin protein in solution. Our results show how this combination can provide morphological/structural nanoscale information to characterize new artificial biomaterials and/or to get insight into the transition between healthy and pathological tissues during the progression of a disease, or to morphologically characterize nanoscale proteins, based on SAXS data collected in a room-sized laboratory.

  1. Agglomeration dynamics of germanium islands on a silicon oxide substrate: A grazing incidence small-angle x-ray scattering study

    NASA Astrophysics Data System (ADS)

    Cheynis, F.; Leroy, F.; Passanante, T.; Müller, P.

    2013-04-01

    Grazing-incidence small-angle X-ray scattering (GISAXS) and grazing-incidence X-ray diffraction techniques are used to characterise the thermally induced solid-state dewetting of Ge(001) thin films leading to the formation of 3D Ge islands. A quantitative analysis based on the Kolmogorov-Johnson-Mehl-Avrami model is derived. The main physical parameters controlling the dewetting (activation energy and kinetic pre-factors) are determined. Assuming that the dewetting is driven by surface/interface minimisation and limited by surface diffusion, the Ge surface self-diffusion reads as Ds ,0c0 e-Ea/(kBT) ˜3×1018 e-2.6±0.3eV/(kBT) nm2/s. GISAXS technique enables to reconstruct the mean Ge-island shape, including facets.

  2. Study of particle evolution from Composition B-3 detonation by time-resolved small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Huber, R.; Podlesak, D.; Dattelbaum, D.; Firestone, M.; Gustavsen, R.; Jensen, B.; Ringstrand, B.; Watkins, E.; Bagge-Hansen, M.; Hodgin, R.; Lauderbach, L.; Willey, T.; van Buuren, T.; Graber, T.; Rigg, P.; Sinclair, N.; Seifert, S.

    2017-06-01

    High explosive (HE) detonations produce an assortment of gases (CO, CO2, N2) and solid carbon products (nanodiamond, graphite). The evolution of solid carbon particles, within the chemical reaction zone, help to propel the detonation wave forward. Due to the violent nature and short reaction times during HE detonations, experimental observation are limited. Through time-resolved small angle x-ray scattering (TRSAXS) we are able to observed nanocarbon formation on nanosecond time scales. This TRSAXS setup is the first of its kind in the United States at Argonne National Laboratory at the Advanced Photon Source in the Dynamic Compression Sector. From the empirical and analytical analysis of the x-ray scattering of an in-line detonation we are able to temporally follow morphology and size. Two detonation geometries were studied for the HE Comp B-3 (40% TNT/60% RDX), producing steady and overdriven conditions. Steady wave particle evolution plateaued by 2 microseconds, where overdriven condition particle size decreases at the collision of the two shock fronts then plateaus. Post detonation soot is also analyzed to confirm size and shape of nanocarbon formation from Comp B-3 detonations. LA-UR-17-21443.

  3. Structural evaluation of an amyloid fibril model using small-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Dahal, Eshan; Choi, Mina; Alam, Nadia; Bhirde, Ashwinkumar A.; Beaucage, Serge L.; Badano, Aldo

    2017-08-01

    Amyloid fibrils are highly structured protein aggregates associated with a wide range of diseases including Alzheimer’s and Parkinson’s. We report a structural investigation of an amyloid fibril model prepared from a commonly used plasma protein (bovine serum albumin (BSA)) using small-angle x-ray scattering (SAXS) technique. As a reference, the size estimates from SAXS are compared to dynamic light scattering (DLS) data and the presence of amyloid-like fibrils is confirmed using Congo red absorbance assay. Our SAXS results consistently show the structural transformation of BSA from spheroid to rod-like elongated structures during the fibril formation process. We observe the elongation of fibrils over two months with fibril length growing from 35.9  ±  3.0 nm to 51.5  ±  2.1 nm. Structurally metastable fibrils with distinct SAXS profiles have been identified. As proof of concept, we demonstrate the use of such distinct SAXS profiles to detect fibrils in the mixture solutions of two species by estimating their volume fractions. This easily detectable and well-characterized amyloid fibril model from BSA can be readily used as a control or standard reference to further investigate SAXS applications in the detection of structurally diverse amyloid fibrils associated with protein aggregation diseases.

  4. Absolute Intra-Molecular Distance Measurements with Ångström-Resolution using Anomalous Small-Angle X-ray Scattering

    DOE PAGES

    Zettl, Thomas; Mathew, Rebecca S.; Seifert, Sönke; ...

    2016-05-31

    Accurate determination of molecular distances is fundamental to understanding the structure, dynamics, and conformational ensembles of biological macromolecules. Here we present a method to determine the full,distance,distribution between small (~7 Å) gold labels attached to macromolecules with very high-precision(≤1 Å) and on an absolute distance scale. Our method uses anomalous small-angle X-ray scattering close to a gold absorption edge to separate the gold-gold interference pattern from other scattering contributions. Results for 10-30 bp DNA constructs achieve excellent signal-to-noise and are in good agreement with previous results obtained by single-energy,SAXS measurements without requiring the preparation and measurement of single labeled andmore » unlabeled samples. Finally, the use of small gold labels in combination with ASAXS read out provides an attractive approach to determining molecular distance distributions that will be applicable to a broad range of macromolecular systems.« less

  5. In situ grazing incidence small-angle X-ray scattering investigation of polystyrene nanoparticle spray deposition onto silicon.

    PubMed

    Herzog, Gerd; Benecke, Gunthard; Buffet, Adeline; Heidmann, Berit; Perlich, Jan; Risch, Johannes F H; Santoro, Gonzalo; Schwartzkopf, Matthias; Yu, Shun; Wurth, Wilfried; Roth, Stephan V

    2013-09-10

    We investigated the spray deposition and subsequent self-assembly during drying of a polystyrene nanoparticle dispersion with in situ grazing incidence small-angle X-ray scattering at high time resolution. During the fast deposition of the dispersion and the subsequent evaporation of the solvent, different transient stages of nanoparticle assembly can be identified. In the first stage, the solvent starts to evaporate without ordering of the nanoparticles. During the second stage, large-scale structures imposed by the breakup of the liquid film are observable. In this stage, the solvent evaporates further and nanoparticle ordering starts. In the late third drying stage, the nanoparticles self-assemble into the final layer structure.

  6. Healing X-ray scattering images

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

    Liu, Jiliang; Lhermitte, Julien; Tian, Ye

    X-ray scattering images contain numerous gaps and defects arising from detector limitations and experimental configuration. Here, we present a method to heal X-ray scattering images, filling gaps in the data and removing defects in a physically meaningful manner. Unlike generic inpainting methods, this method is closely tuned to the expected structure of reciprocal-space data. In particular, we exploit statistical tests and symmetry analysis to identify the structure of an image; we then copy, average and interpolate measured data into gaps in a way that respects the identified structure and symmetry. Importantly, the underlying analysis methods provide useful characterization of structuresmore » present in the image, including the identification of diffuseversussharp features, anisotropy and symmetry. The presented method leverages known characteristics of reciprocal space, enabling physically reasonable reconstruction even with large image gaps. The method will correspondingly fail for images that violate these underlying assumptions. The method assumes point symmetry and is thus applicable to small-angle X-ray scattering (SAXS) data, but only to a subset of wide-angle data. Our method succeeds in filling gaps and healing defects in experimental images, including extending data beyond the original detector borders.« less

  7. Healing X-ray scattering images

    DOE PAGES

    Liu, Jiliang; Lhermitte, Julien; Tian, Ye; ...

    2017-05-24

    X-ray scattering images contain numerous gaps and defects arising from detector limitations and experimental configuration. Here, we present a method to heal X-ray scattering images, filling gaps in the data and removing defects in a physically meaningful manner. Unlike generic inpainting methods, this method is closely tuned to the expected structure of reciprocal-space data. In particular, we exploit statistical tests and symmetry analysis to identify the structure of an image; we then copy, average and interpolate measured data into gaps in a way that respects the identified structure and symmetry. Importantly, the underlying analysis methods provide useful characterization of structuresmore » present in the image, including the identification of diffuseversussharp features, anisotropy and symmetry. The presented method leverages known characteristics of reciprocal space, enabling physically reasonable reconstruction even with large image gaps. The method will correspondingly fail for images that violate these underlying assumptions. The method assumes point symmetry and is thus applicable to small-angle X-ray scattering (SAXS) data, but only to a subset of wide-angle data. Our method succeeds in filling gaps and healing defects in experimental images, including extending data beyond the original detector borders.« less

  8. Operando Grazing Incidence Small-Angle X-ray Scattering/X-ray Diffraction of Model Ordered Mesoporous Lithium-Ion Battery Anodes.

    PubMed

    Bhaway, Sarang M; Qiang, Zhe; Xia, Yanfeng; Xia, Xuhui; Lee, Byeongdu; Yager, Kevin G; Zhang, Lihua; Kisslinger, Kim; Chen, Yu-Ming; Liu, Kewei; Zhu, Yu; Vogt, Bryan D

    2017-02-28

    Emergent lithium-ion (Li + ) batteries commonly rely on nanostructuring of the active electrode materials to decrease the Li + ion diffusion path length and to accommodate the strains associated with the insertion and de-insertion of Li + , but in many cases these nanostructures evolve during electrochemical charging-discharging. This change in the nanostructure can adversely impact performance, and challenges remain regarding how to control these changes from the perspective of morphological design. In order to address these questions, operando grazing-incidence small-angle X-ray scattering and X-ray diffraction (GISAXS/GIXD) were used to assess the structural evolution of a family of model ordered mesoporous NiCo 2 O 4 anode films during battery operation. The pore dimensions were systematically varied and appear to impact the stability of the ordered nanostructure during the cycling. For the anodes with small mesopores (≈9 nm), the ordered nanostructure collapses during the first two charge-discharge cycles, as determined from GISAXS. This collapse is accompanied by irreversible Li-ion insertion within the oxide framework, determined from GIXD and irreversible capacity loss. Conversely, anodes with larger ordered mesopores (17-28 nm) mostly maintained their nanostructure through the first two cycles with reversible Li-ion insertion. During the second cycle, there was a small additional deformation of the mesostructure. This preservation of the ordered structure lead to significant improvement in capacity retention during these first two cycles; however, a gradual loss in the ordered nanostructure from continuing deformation of the ordered structure during additional charge-discharge cycles leads to capacity decay in battery performance. These multiscale operando measurements provide insight into how changes at the atomic scale (lithium insertion and de-insertion) are translated to the nanostructure during battery operation. Moreover, small changes in the

  9. Characterisation of large scale structures in starch granules via small-angle neutron and X-ray scattering.

    PubMed

    Doutch, James; Gilbert, Elliot P

    2013-01-02

    Small angle scattering (SAS) techniques have a distinguished track record in illuminating the semi-crystalline lamellar structure of the starch granule. To date, there have been few attempts to use SAS techniques to characterise larger-scale structures reported from imaging techniques such as growth rings, blocklets or pores, nor how these structures would modulate the well-known scattering arising from the semi-crystalline lamellar structure. In this study, SAS data collected over an extended q range were gathered from dry and hydrated starch powders from varied botanical sources. The use of neutrons and X-rays, as well as comparing dry and hydrated granules, allowed different levels of contrast in scattering length density to be probed and therefore selected structural regions to be highlighted. The lowest q range, 0.002-0.04 Å(-1), was found to be dominated by scattering from the starch granules themselves, especially in the dry powders; however an inflection point from a low contrast structure was observed at 0.035 Å(-1). The associated scattering was interpreted within a unified scattering framework with the inflexion point correlating with a structure with radius of gyration ~90 Å - a size comparable to small blocklets or superhelices. In hydrated starches, it is observed that there is an inflection point between lamellar and q(-4) power-law scattering regions at approximately 0.004 Å(-1) which may correlate with growth rings and large blocklets. The implications of these findings on existing models of starch lamellar scattering are discussed. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

  10. Modeling the Hydration Layer around Proteins: Applications to Small- and Wide-Angle X-Ray Scattering

    PubMed Central

    Virtanen, Jouko Juhani; Makowski, Lee; Sosnick, Tobin R.; Freed, Karl F.

    2011-01-01

    Small-/wide-angle x-ray scattering (SWAXS) experiments can aid in determining the structures of proteins and protein complexes, but success requires accurate computational treatment of solvation. We compare two methods by which to calculate SWAXS patterns. The first approach uses all-atom explicit-solvent molecular dynamics (MD) simulations. The second, far less computationally expensive method involves prediction of the hydration density around a protein using our new HyPred solvation model, which is applied without the need for additional MD simulations. The SWAXS patterns obtained from the HyPred model compare well to both experimental data and the patterns predicted by the MD simulations. Both approaches exhibit advantages over existing methods for analyzing SWAXS data. The close correspondence between calculated and observed SWAXS patterns provides strong experimental support for the description of hydration implicit in the HyPred model. PMID:22004761

  11. Flow-through compression cell for small-angle and ultra-small-angle neutron scattering measurements

    NASA Astrophysics Data System (ADS)

    Hjelm, Rex P.; Taylor, Mark A.; Frash, Luke P.; Hawley, Marilyn E.; Ding, Mei; Xu, Hongwu; Barker, John; Olds, Daniel; Heath, Jason; Dewers, Thomas

    2018-05-01

    In situ measurements of geological materials under compression and with hydrostatic fluid pressure are important in understanding their behavior under field conditions, which in turn provides critical information for application-driven research. In particular, understanding the role of nano- to micro-scale porosity in the subsurface liquid and gas flow is critical for the high-fidelity characterization of the transport and more efficient extraction of the associated energy resources. In other applications, where parts are produced by the consolidation of powders by compression, the resulting porosity and crystallite orientation (texture) may affect its in-use characteristics. Small-angle neutron scattering (SANS) and ultra SANS are ideal probes for characterization of these porous structures over the nano to micro length scales. Here we show the design, realization, and performance of a novel neutron scattering sample environment, a specially designed compression cell, which provides compressive stress and hydrostatic pressures with effective stress up to 60 MPa, using the neutron beam to probe the effects of stress vectors parallel to the neutron beam. We demonstrate that the neutron optics is suitable for the experimental objectives and that the system is highly stable to the stress and pressure conditions of the measurements.

  12. Structural and mechanical properties of cardiolipin lipid bilayers determined using neutron spin echo, small angle neutron and X-ray scattering, and molecular dynamics simulations

    DOE PAGES

    Pan, Jianjun; Cheng, Xiaolin; Sharp, Melissa; ...

    2014-10-29

    We report that the detailed structural and mechanical properties of a tetraoleoyl cardiolipin (TOCL) bilayer were determined using neutron spin echo (NSE) spectroscopy, small angle neutron and X-ray scattering (SANS and SAXS, respectively), and molecular dynamics (MD) simulations. We used MD simulations to develop a scattering density profile (SDP) model, which was then utilized to jointly refine SANS and SAXS data. In addition to commonly reported lipid bilayer structural parameters, component distributions were obtained, including the volume probability, electron density and neutron scattering length density.

  13. Crystal Structures and Small-angle X-ray Scattering Analysis of UDP-galactopyranose Mutase from the Pathogenic Fungus Aspergillus fumigatus

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

    Dhatwalia, Richa; Singh, Harkewal; Oppenheimer, Michelle

    2015-10-15

    UDP-galactopyranose mutase (UGM) is a flavoenzyme that catalyzes the conversion of UDP-galactopyranose to UDP-galactofuranose, which is a central reaction in galactofuranose biosynthesis. Galactofuranose has never been found in humans but is an essential building block of the cell wall and extracellular matrix of many bacteria, fungi, and protozoa. The importance of UGM for the viability of many pathogens and its absence in humans make UGM a potential drug target. Here we report the first crystal structures and small-angle x-ray scattering data for UGM from the fungus Aspergillus fumigatus, the causative agent of aspergillosis. The structures reveal that Aspergillus UGM hasmore » several extra secondary and tertiary structural elements that are not found in bacterial UGMs yet are important for substrate recognition and oligomerization. Small-angle x-ray scattering data show that Aspergillus UGM forms a tetramer in solution, which is unprecedented for UGMs. The binding of UDP or the substrate induces profound conformational changes in the enzyme. Two loops on opposite sides of the active site move toward each other by over 10 {angstrom} to cover the substrate and create a closed active site. The degree of substrate-induced conformational change exceeds that of bacterial UGMs and is a direct consequence of the unique quaternary structure of Aspergillus UGM. Galactopyranose binds at the re face of the FAD isoalloxazine with the anomeric carbon atom poised for nucleophilic attack by the FAD N5 atom. The structural data provide new insight into substrate recognition and the catalytic mechanism and thus will aid inhibitor design.« less

  14. Time resolved small angle X-ray scattering experiments performed on detonating explosives at the advanced photon source: Calculation of the time and distance between the detonation front and the x-ray beam

    DOE PAGES

    Gustavsen, Richard L.; Dattelbaum, Dana Mcgraw; Watkins, Erik Benjamin; ...

    2017-03-10

    Time resolved Small Angle X-ray Scattering (SAXS) experiments on detonating explosives have been conducted at Argonne National Laboratory's Advanced Photon Source Dynamic Compression Sector. The purpose of the experiments is to measure the SAXS patterns at tens of ns to a few μs behind the detonation front. Corresponding positions behind the detonation front are of order 0.1–10 mm. From the scattering patterns, properties of the explosive products relative to the time behind the detonation front can be inferred. Lastly, this report describes how the time and distance from the x-ray probe location to the detonation front is calculated, as wellmore » as the uncertainties and sources of uncertainty associated with the calculated times and distances.« less

  15. Time resolved small angle X-ray scattering experiments performed on detonating explosives at the advanced photon source: Calculation of the time and distance between the detonation front and the x-ray beam

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

    Gustavsen, Richard L.; Dattelbaum, Dana Mcgraw; Watkins, Erik Benjamin

    Time resolved Small Angle X-ray Scattering (SAXS) experiments on detonating explosives have been conducted at Argonne National Laboratory's Advanced Photon Source Dynamic Compression Sector. The purpose of the experiments is to measure the SAXS patterns at tens of ns to a few μs behind the detonation front. Corresponding positions behind the detonation front are of order 0.1–10 mm. From the scattering patterns, properties of the explosive products relative to the time behind the detonation front can be inferred. Lastly, this report describes how the time and distance from the x-ray probe location to the detonation front is calculated, as wellmore » as the uncertainties and sources of uncertainty associated with the calculated times and distances.« less

  16. Characterization of Protein Flexibility Using Small-Angle X-Ray Scattering and Amplified Collective Motion Simulations

    PubMed Central

    Wen, Bin; Peng, Junhui; Zuo, Xiaobing; Gong, Qingguo; Zhang, Zhiyong

    2014-01-01

    Large-scale flexibility within a multidomain protein often plays an important role in its biological function. Despite its inherent low resolution, small-angle x-ray scattering (SAXS) is well suited to investigate protein flexibility and determine, with the help of computational modeling, what kinds of protein conformations would coexist in solution. In this article, we develop a tool that combines SAXS data with a previously developed sampling technique called amplified collective motions (ACM) to elucidate structures of highly dynamic multidomain proteins in solution. We demonstrate the use of this tool in two proteins, bacteriophage T4 lysozyme and tandem WW domains of the formin-binding protein 21. The ACM simulations can sample the conformational space of proteins much more extensively than standard molecular dynamics (MD) simulations. Therefore, conformations generated by ACM are significantly better at reproducing the SAXS data than are those from MD simulations. PMID:25140431

  17. Small Angle X-ray and Neutron Scattering: Powerful Tools for Studying the Structure of Drug-Loaded Liposomes

    PubMed Central

    Di Cola, Emanuela; Grillo, Isabelle; Ristori, Sandra

    2016-01-01

    Nanovectors, such as liposomes, micelles and lipid nanoparticles, are recognized as efficient platforms for delivering therapeutic agents, especially those with low solubility in water. Besides being safe and non-toxic, drug carriers with improved performance should meet the requirements of (i) appropriate size and shape and (ii) cargo upload/release with unmodified properties. Structural issues are of primary importance to control the mechanism of action of loaded vectors. Overall properties, such as mean diameter and surface charge, can be obtained using bench instruments (Dynamic Light Scattering and Zeta potential). However, techniques with higher space and time resolution are needed for in-depth structural characterization. Small-angle X-ray (SAXS) and neutron (SANS) scattering techniques provide information at the nanoscale and have therefore been largely used to investigate nanovectors loaded with drugs or other biologically relevant molecules. Here we revise recent applications of these complementary scattering techniques in the field of drug delivery in pharmaceutics and medicine with a focus to liposomal carriers. In particular, we highlight those aspects that can be more commonly accessed by the interested users. PMID:27043614

  18. In-situ small-angle x-ray scattering study of nanoparticles in the plasma plume induced by pulsed laser irradiation of metallic targets

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

    Lavisse, L.; Jouvard, J.-M.; Girault, M.

    2012-04-16

    Small angle x-ray scattering was used to probe in-situ the formation of nanoparticles in the plasma plume generated by pulsed laser irradiation of a titanium metal surface under atmospheric conditions. The size and morphology of the nanoparticles were characterized as function of laser irradiance. Two families of nanoparticles were identified with sizes on the order of 10 and 70 nm, respectively. These results were confirmed by ex-situ transmission electron microscopy experiments.

  19. Simbol-X Mirror Module Thermal Shields: II-Small Angle X-Ray Scattering Measurements

    NASA Astrophysics Data System (ADS)

    Barbera, M.; Ayers, T.; Collura, A.; Nasillo, G.; Pareschi, G.; Tagliaferri, G.

    2009-05-01

    The formation flight configuration of the Simbol-X mission implies that the X-ray mirror module will be open to Space on both ends. In order to reduce the power required to maintain the thermal stability and, therefore, the high angular resolution of the shell optics, a thin foil thermal shield will cover the mirror module. Different options are presently being studied for the foil material of these shields. We report results of an experimental investigation conducted to verify that the scattering of X-rays, by interaction with the thin foil material of the thermal shield, will not significantly affect the performances of the telescope.

  20. Dynamic Conformations of Nucleosome Arrays in Solution from Small-Angle X-ray Scattering

    NASA Astrophysics Data System (ADS)

    Howell, Steven C.

    Chromatin conformation and dynamics remains unsolved despite the critical role of the chromatin in fundamental genetic functions such as transcription, replication, and repair. At the molecular level, chromatin can be viewed as a linear array of nucleosomes, each consisting of 147 base pairs (bp) of double-stranded DNA (dsDNA) wrapped around a protein core and connected by 10 to 90 bp of linker dsDNA. Using small-angle X-ray scattering (SAXS), we investigated how the conformations of model nucleosome arrays in solution are modulated by ionic condition as well as the effect of linker histone proteins. To facilitate ensemble modeling of these SAXS measurements, we developed a simulation method that treats coarse-grained DNA as a Markov chain, then explores possible DNA conformations using Metropolis Monte Carlo (MC) sampling. This algorithm extends the functionality of SASSIE, a program used to model intrinsically disordered biological molecules, adding to the previous methods for simulating protein, carbohydrates, and single-stranded DNA. Our SAXS measurements of various nucleosome arrays together with the MC generated models provide valuable solution structure information identifying specific differences from the structure of crystallized arrays.

  1. Characterization of surface modified carbon fibers and their epoxy composites by small angle x-ray scattering

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

    Stoll, B.; Fellers, J.F.; Lin, J.S.

    1986-01-01

    This paper correlated the interlaminar shear strength of 7 different carbon fiber/epoxy composites with structural characteristics determined by Small Angle X-ray Scattering (SAXS) measurements. The carbon fibers were all of the same type but had different surface treatments. The SAXS patterns of the fibers and of the composites showed a highly nonlinear Guinier region which could not be approximated by traditional linear regression. A new approach to the Guinier approximation was developed to treat this nonlinear curve using a polynomial of second order. The radius of gyration (RG) of the fibers, as determined by this new method, correlated clearly withmore » both the extent of the surface treatment and the interlaminar shear strength of the composite. Also the difference in scattering between a dry fiber and a glycerine soaked fiber provides a way to characterize the changes obtained by surface treatments. These methods provide new ways to estimate the efficiency of a surface treatment and its effect on the interlaminar shear strength by analyzing the SAXS patterns of the fibers.« less

  2. Operando Grazing Incidence Small-Angle X-ray Scattering/X-ray Diffraction of Model Ordered Mesoporous Lithium-Ion Battery Anodes

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

    Bhaway, Sarang M.; Qiang, Zhe; Xia, Yanfeng

    Emergent lithium-ion (Li +) batteries commonly rely on nanostructuring of the active electrode materials to decrease the Li + ion diffusion path length and to accommodate the strains associated with the insertion and de-insertion of Li +, but in many cases these nanostructures evolve during electrochemical charging–discharging. This change in the nanostructure can adversely impact performance, and challenges remain regarding how to control these changes from the perspective of morphological design. In order to address these questions, operando grazing-incidence small-angle X-ray scattering and X-ray diffraction (GISAXS/GIXD) were used to assess the structural evolution of a family of model ordered mesoporousmore » NiCo 2O 4 anode films during battery operation. The pore dimensions were systematically varied and appear to impact the stability of the ordered nanostructure during the cycling. For the anodes with small mesopores (≈9 nm), the ordered nanostructure collapses during the first two charge–discharge cycles, as determined from GISAXS. This collapse is accompanied by irreversible Li-ion insertion within the oxide framework, determined from GIXD and irreversible capacity loss. Anodes with larger ordered mesopores (17–28 nm) mostly maintained their nanostructure through the first two cycles with reversible Li-ion insertion. During the second cycle, there was a small additional deformation of the mesostructure. Furthermore, this preservation of the ordered structure lead to significant improvement in capacity retention during these first two cycles; but, a gradual loss in the ordered nanostructure from continuing deformation of the ordered structure during additional charge–discharge cycles leads to capacity decay in battery performance. We translate these multiscale operando measurements provide insight into how changes at the atomic scale (lithium insertion and de-insertion) to the nanostructure during battery operation. Moreover, small changes in

  3. Operando Grazing Incidence Small-Angle X-ray Scattering/X-ray Diffraction of Model Ordered Mesoporous Lithium-Ion Battery Anodes

    DOE PAGES

    Bhaway, Sarang M.; Qiang, Zhe; Xia, Yanfeng; ...

    2017-02-07

    Emergent lithium-ion (Li +) batteries commonly rely on nanostructuring of the active electrode materials to decrease the Li + ion diffusion path length and to accommodate the strains associated with the insertion and de-insertion of Li +, but in many cases these nanostructures evolve during electrochemical charging–discharging. This change in the nanostructure can adversely impact performance, and challenges remain regarding how to control these changes from the perspective of morphological design. In order to address these questions, operando grazing-incidence small-angle X-ray scattering and X-ray diffraction (GISAXS/GIXD) were used to assess the structural evolution of a family of model ordered mesoporousmore » NiCo 2O 4 anode films during battery operation. The pore dimensions were systematically varied and appear to impact the stability of the ordered nanostructure during the cycling. For the anodes with small mesopores (≈9 nm), the ordered nanostructure collapses during the first two charge–discharge cycles, as determined from GISAXS. This collapse is accompanied by irreversible Li-ion insertion within the oxide framework, determined from GIXD and irreversible capacity loss. Anodes with larger ordered mesopores (17–28 nm) mostly maintained their nanostructure through the first two cycles with reversible Li-ion insertion. During the second cycle, there was a small additional deformation of the mesostructure. Furthermore, this preservation of the ordered structure lead to significant improvement in capacity retention during these first two cycles; but, a gradual loss in the ordered nanostructure from continuing deformation of the ordered structure during additional charge–discharge cycles leads to capacity decay in battery performance. We translate these multiscale operando measurements provide insight into how changes at the atomic scale (lithium insertion and de-insertion) to the nanostructure during battery operation. Moreover, small changes in

  4. Structural characterization of the phospholipid stabilizer layer at the solid-liquid interface of dispersed triglyceride nanocrystals with small-angle x-ray and neutron scattering

    NASA Astrophysics Data System (ADS)

    Schmiele, Martin; Schindler, Torben; Unruh, Tobias; Busch, Sebastian; Morhenn, Humphrey; Westermann, Martin; Steiniger, Frank; Radulescu, Aurel; Lindner, Peter; Schweins, Ralf; Boesecke, Peter

    2013-06-01

    Dispersions of crystalline nanoparticles with at least one sufficiently large unit cell dimension can give rise to Bragg reflections in the small-angle scattering range. If the nanocrystals possess only a small number of unit cells along these particular crystallographic directions, the corresponding Bragg reflections will be broadened. In a previous study of phospholipid stabilized dispersions of β-tripalmitin platelets [Unruh, J. Appl. Crystallogr.JACGAR0021-889810.1107/S0021889807044378 40, 1008 (2007)], the x-ray powder pattern simulation analysis (XPPSA) was developed. The XPPSA method facilitates the interpretation of the rather complicated small-angle x-ray scattering (SAXS) curves of such dispersions of nanocrystals. The XPPSA method yields the distribution function of the platelet thicknesses and facilitates a structural characterization of the phospholipid stabilizer layer at the solid-liquid interface between the nanocrystals and the dispersion medium from the shape of the broadened 001 Bragg reflection. In this contribution an improved and extended version of the XPPSA method is presented. The SAXS and small-angle neutron scattering patterns of dilute phospholipid stabilized tripalmitin dispersions can be reproduced on the basis of a consistent simulation model for the particles and their phospholipid stabilizer layer on an absolute scale. The results indicate a surprisingly flat arrangement of the phospholipid molecules in the stabilizer layer with a total thickness of only 12 Å. The stabilizer layer can be modeled by an inner shell for the fatty acid chains and an outer shell including the head groups and additional water. The experiments support a dense packing of the phospholipid molecules on the nanocrystal surfaces rather than isolated phospholipid domains.

  5. Micellar Surfactant Association in the Presence of a Glucoside-based Amphiphile Detected via High-Throughput Small Angle X-ray Scattering

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

    Stanic, Vesna; Broadbent, Charlotte; DiMasi, Elaine

    2016-11-14

    The interactions of mixtures of anionic and amphoteric surfactants with sugar amphiphiles were studied via high throughput small angle x-ray scattering (SAXS). The sugar amphiphile was composed of Caprate, Caprylate, and Oleate mixed ester of methyl glucoside, MeGCCO. Optimal surfactant interactions are sought which have desirable physical properties, which must be identified in a cost effective manner that can access the large phase space of possible molecular combinations. X-ray scattering patterns obtained via high throughput SAXS can probe a combinatorial sample space and reveal the incorporation of MeGCCO into the micelles and the molecular associations between surfactant molecules. Such datamore » make it possible to efficiently assess the effects of the new amphiphiles in the formulation. A specific finding of this study is that formulations containing comparatively monodisperse and homogeneous surfactant mixtures can be reliably tuned by addition of NaCl, which swells the surfactant micelles with a monotonic dependence on salt concentration. In contrast, the presence of multiple different surfactants destroys clear correlations with NaCl concentration, even in otherwise similar series of formulations.« less

  6. The small angle x-ray scattering of globular proteins in solution during heat denaturation

    NASA Astrophysics Data System (ADS)

    Banuelos, Jose; Urquidi, Jacob

    2008-10-01

    The ability of proteins to change their conformation in response to changes in their environment has consequences in biological processes like metabolism, chemical regulation in cells, and is believed to play a role in the onset of several neurodegenerative diseases. Factors such as a change in temperature, pressure, and the introduction of ions into the aqueous environment of a protein can give rise to the folding/unfolding of a protein. As a protein unfolds, the ratio of nonpolar to polar groups exposed to water changes, affecting a protein's thermodynamic properties. Using small angle x-ray scattering (SAXS), we are currently studying the intermediate protein conformations that arise during the folding/unfolding process as a function of temperature for five globular proteins. Trends in the observed intermediate structures of these globular proteins, along with correlations with data on protein thermodynamics may help elucidate shared characteristics between all proteins in the folding/unfolding process. Experimental design considerations will be discussed and preliminary results for some of these systems will be presented.

  7. The applications of small-angle X-ray scattering in studying nano-scaled polyoxometalate clusters in solutions

    NASA Astrophysics Data System (ADS)

    Li, Mu; Zhang, Mingxin; Wang, Weiyu; Cheng, Stephen Z. D.; Yin, Panchao

    2018-05-01

    Nano-scaled polyoxometalates (POMs) clusters with sizes ranging from 1 to 10 nm attract tremendous attention and have been extensively studied due to POMs' fascinating structural characteristics and prospects for wide-ranging applications. As a unique class of nanoparticles with well-defined structural topologies and monodispersed masses, the structures and properties of POMs in both bulk state and solutions have been explored with several well-developed protocols. Small-angle X-ray scattering (SAXS) technique, as a powerful tool for studying polymers and nanoparticles, has been recently extended to the investigating of solution behaviors of POMs. In this mini-review, the general principle and typical experimental procedures of SAXS are illustrated first. The applications of SAXS in characterizing POMs' morphology, counterion distribution around POMs, and short-range interactions among POMs in solutions are highlighted. [Figure not available: see fulltext.

  8. An analysis of FtsZ assembly using small angle X-ray scattering and electron microscopy.

    PubMed

    Kuchibhatla, Anuradha; Abdul Rasheed, A S; Narayanan, Janaky; Bellare, Jayesh; Panda, Dulal

    2009-04-09

    Small angle X-ray scattering (SAXS) was used for the first time to study the self-assembly of the bacterial cell division protein, FtsZ, with three different additives: calcium chloride, monosodium glutamate and DEAE-dextran hydrochloride in solution. The SAXS data were analyzed assuming a model form factor and also by a model-independent analysis using the pair distance distribution function. Transmission electron microscopy (TEM) was used for direct observation of the FtsZ filaments. By sectioning and negative staining with glow discharged grids, very high bundling as well as low bundling polymers were observed under different assembly conditions. FtsZ polymers formed different structures in the presence of different additives and these additives were found to increase the bundling of FtsZ protofilaments by different mechanisms. The combined use of SAXS and TEM provided us a significant insight of the assembly of FtsZ and microstructures of the assembled FtsZ polymers.

  9. Structure of Carbon Nanotube Porins in Lipid Bilayers: An in Situ Small-Angle X-ray Scattering (SAXS) Study [Atomic-level structure of carbon nanotube porins in lipid bilayers: an in-situ small-angle x-ray scattering (SAXS) study

    DOE PAGES

    Tran, Ich C.; Tunuguntla, Ramya H.; Kim, Kyunghoon; ...

    2016-06-20

    Carbon nanotube porins (CNTPs), small segments of carbon nanotubes capable of forming defined pores in lipid membranes, are important future components for bionanoelectronic devices as they could provide a robust analog of biological membrane channels. Furthermore, in order to control the incorporation of these CNT channels into lipid bilayers, it is important to understand the structure of the CNTPs before and after insertion into the lipid bilayer as well as the impact of such insertion on the bilayer structure. Here we employed a noninvasive in situ probe, small-angle X-ray scattering, to study the integration of CNT porins into dioleoylphosphatidylcholine bilayers.more » These results show that CNTPs in solution are stabilized by a monolayer of lipid molecules wrapped around their outer surface. We also demonstrate that insertion of CNTPs into the lipid bilayer results in decreased bilayer thickness with the magnitude of this effect increasing with the concentration of CNTPs.« less

  10. Biological Small Angle Scattering: Techniques, Strategies and Tips

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

    Chaudhuri, Barnali; Muñoz, Inés G.; Urban, Volker S.

    This book provides a clear, comprehensible and up-to-date description of how Small Angle Scattering (SAS) can help structural biology researchers. SAS is an efficient technique that offers structural information on how biological macromolecules behave in solution. SAS provides distinct and complementary data for integrative structural biology approaches in combination with other widely used probes, such as X-ray crystallography, Nuclear magnetic resonance, Mass spectrometry and Cryo-electron Microscopy. The development of brilliant synchrotron small-angle X-ray scattering (SAXS) beam lines has increased the number of researchers interested in solution scattering. SAS is especially useful for studying conformational changes in proteins, highly flexible proteins,more » and intrinsically disordered proteins. Small-angle neutron scattering (SANS) with neutron contrast variation is ideally suited for studying multi-component assemblies as well as membrane proteins that are stabilized in surfactant micelles or vesicles. SAS is also used for studying dynamic processes of protein fibrillation in amyloid diseases, and pharmaceutical drug delivery. The combination with size-exclusion chromatography further increases the range of SAS applications.The book is written by leading experts in solution SAS methodologies. The principles and theoretical background of various SAS techniques are included, along with practical aspects that range from sample preparation to data presentation for publication. Topics covered include techniques for improving data quality and analysis, as well as different scientific applications of SAS. With abundant illustrations and practical tips, we hope the clear explanations of the principles and the reviews on the latest progresses will serve as a guide through all aspects of biological solution SAS.The scope of this book is particularly relevant for structural biology researchers who are new to SAS. Advanced users of the technique will find it

  11. Small-scale screening method for low-viscosity antibody solutions using small-angle X-ray scattering.

    PubMed

    Fukuda, Masakazu; Watanabe, Atsushi; Hayasaka, Akira; Muraoka, Masaru; Hori, Yuji; Yamazaki, Tadao; Imaeda, Yoshimi; Koga, Akiko

    2017-03-01

    In this study, we investigated the concentration range in which self-association starts to form in humanized IgG monoclonal antibody (mAb) solutions. Furthermore, on the basis of the results, we developed a practical method of screening for low-viscosity antibody solutions by using small-angle X-ray scattering (SAXS) measurements utilizing small quantities of samples. With lower-viscosity mAb3, self-association was not detected in the range of 1-80mg/mL. With higher-viscosity mAb1, on the other hand, self-association was detected in the range of 10-20mg/mL and was clearly enhanced by a decrease in temperature. The viscosities of mAb solutions at 160, 180, and 200mg/mL at 25°C quantitatively correlated very well with the particle size parameters obtained by SAXS measurements of mAb solutions at 15mg/mL at 5°C. The quantity of mAb sample required for the SAXS measurements was only 0.15mg, which is about one-hundredth of that required for actual viscosity measurements at a high concentration, and such quantities could be available even at an early stage of development. In conclusion, the SAXS analysis method proposed in this study is a valuable tool for the development of concentrated mAb therapeutics with high manufacturability and high usability for subcutaneous injection. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Accounting for observed small angle X-ray scattering profile in the protein-protein docking server ClusPro.

    PubMed

    Xia, Bing; Mamonov, Artem; Leysen, Seppe; Allen, Karen N; Strelkov, Sergei V; Paschalidis, Ioannis Ch; Vajda, Sandor; Kozakov, Dima

    2015-07-30

    The protein-protein docking server ClusPro is used by thousands of laboratories, and models built by the server have been reported in over 300 publications. Although the structures generated by the docking include near-native ones for many proteins, selecting the best model is difficult due to the uncertainty in scoring. Small angle X-ray scattering (SAXS) is an experimental technique for obtaining low resolution structural information in solution. While not sufficient on its own to uniquely predict complex structures, accounting for SAXS data improves the ranking of models and facilitates the identification of the most accurate structure. Although SAXS profiles are currently available only for a small number of complexes, due to its simplicity the method is becoming increasingly popular. Since combining docking with SAXS experiments will provide a viable strategy for fairly high-throughput determination of protein complex structures, the option of using SAXS restraints is added to the ClusPro server. © 2015 Wiley Periodicals, Inc. © 2015 Wiley Periodicals, Inc.

  13. Size And Shape of Detergent Micelles Determined By Small-Angle X-Ray Scattering

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

    Lipfert, Jan; Columbus, Linda; Chu, Vincent B.

    2009-04-29

    We present a systematic analysis of the aggregation number and shape of micelles formed by nine detergents commonly used in the study of membrane proteins. Small-angle X-ray scattering measurements are reported for glucosides with 8 and 9 alkyl carbons (OG/NG), maltosides and phosphocholines with 10 and 12 alkyl carbons (DM/DDM and FC-10/FC-12), 1,2-dihexanoyl-sn-glycero-phosphocholine (DHPC), 1-palmitoyl-2-hydroxy-sn-glycero-3-[phospho-rac-(1-glycerol)] (LPPG), and 3-[(3-cholamidopropyl)dimethylammonio]-1-propane sulfonate (CHAPS). The SAXS intensities are well described by two-component ellipsoid models, with a dense outer shell corresponding to the detergent head groups and a less electron dense hydrophobic core. These models provide an intermediate resolution view of micelle size and shape.more » In addition, we show that Guinier analysis of the forward scattering intensity can be used to obtain an independent and model-free measurement of the micelle aggregation number and radius of gyration. This approach has the advantage of being easily generalizable to protein-detergent complexes, where simple geometric models are inapplicable. Furthermore, we have discovered that the position of the second maximum in the scattering intensity provides a direct measurement of the characteristic head group-head group spacing across the micelle core. Our results for the micellar aggregation numbers and dimensions agree favorably with literature values as far as they are available. We de novo determine the shape of FC-10, FC-12, DM, LPPG, and CHAPS micelles and the aggregation numbers of FC-10 and OG to be ca. 50 and 250, respectively. Combined, these data provide a comprehensive view of the determinants of micelle formation and serve as a starting point to correlate detergent properties with detergent-protein interactions.« less

  14. The atomic scale structure of CXV carbon: wide-angle x-ray scattering and modeling studies.

    PubMed

    Hawelek, L; Brodka, A; Dore, J C; Honkimaki, V; Burian, A

    2013-11-13

    The disordered structure of commercially available CXV activated carbon produced from finely powdered wood-based carbon has been studied using the wide-angle x-ray scattering technique, molecular dynamics and density functional theory simulations. The x-ray scattering data has been converted to the real space representation in the form of the pair correlation function via the Fourier transform. Geometry optimizations using classical molecular dynamics based on the reactive empirical bond order potential and density functional theory at the B3LYP/6-31g* level have been performed to generate nanoscale models of CXV carbon consistent with the experimental data. The final model of the structure comprises four chain-like and buckled graphitic layers containing a small percentage of four-fold coordinated atoms (sp(3) defects) in each layer. The presence of non-hexagonal rings in the atomic arrangement has been also considered.

  15. Edible oil structures at low and intermediate concentrations. II. Ultra-small angle X-ray scattering of in situ tristearin solids in triolein

    NASA Astrophysics Data System (ADS)

    Peyronel, Fernanda; Ilavsky, Jan; Mazzanti, Gianfranco; Marangoni, Alejandro G.; Pink, David A.

    2013-12-01

    Ultra-small angle X-ray scattering has been used for the first time to elucidate, in situ, the aggregation structure of a model edible oil system. The three-dimensional nano- to micro-structure of tristearin solid particles in triolein solvent was investigated using 5, 10, 15, and 20% solids. Three different sample preparation procedures were investigated: two slow cooling rates of 0.5°/min, case 1 (22 days of storage at room temperature) and case 2 (no storage), and one fast cooling of 30°/min, case 3 (no storage). The length scale investigated, by using the Bonse-Hart camera at beamline ID-15D at the Advanced Photon Source, Argonne National Laboratory, covered the range from 300 Å to 10 μm. The unified fit and the Guinier-Porod models in the Irena software were used to fit the data. The former was used to fit 3 structural levels. Level 1 structures showed that the primary scatterers were essentially 2-dimensional objects for the three cases. The scatterers possessed lateral dimensions between 1000 and 4300 Å. This is consistent with the sizes of crystalline nanoplatelets present which were observed using cryo-TEM. Level 2 structures were aggregates possessing radii of gyration, Rg2 between 1800 Å and 12000 Å and fractal dimensions of either D2=1 for case 3 or 1.8≤D2≤2.1 for case 1 and case 2. D2 = 1 is consistent with unaggregated 1-dimensional objects. 1.8 ≤ D2 ≤ 2.1 is consistent with these 1-dimensional objects (below) forming structures characteristic of diffusion or reaction limited cluster-cluster aggregation. Level 3 structures showed that the spatial distribution of the level 2 structures was uniform, on the average, for case 1, with fractal dimension D3≈3 while for case 2 and case 3 the fractal dimension was D3≈2.2, which suggested that the large-scale distribution had not come to equilibrium. The Guinier-Porod model showed that the structures giving rise to the aggregates with a fractal dimension given by D2 in the unified fit level 2

  16. Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source

    NASA Astrophysics Data System (ADS)

    Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

    2017-04-01

    As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

  17. Diffraction based method to reconstruct the spectrum of the Thomson scattering x-ray source.

    PubMed

    Chi, Zhijun; Yan, Lixin; Zhang, Zhen; Zhou, Zheng; Zheng, Lianmin; Wang, Dong; Tian, Qili; Wang, Wei; Nie, Zan; Zhang, Jie; Du, Yingchao; Hua, Jianfei; Shi, Jiaru; Pai, Chihao; Lu, Wei; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

    2017-04-01

    As Thomson scattering x-ray sources based on the collision of intense laser and relativistic electrons have drawn much attention in various scientific fields, there is an increasing demand for the effective methods to reconstruct the spectrum information of the ultra-short and high-intensity x-ray pulses. In this paper, a precise spectrum measurement method for the Thomson scattering x-ray sources was proposed with the diffraction of a Highly Oriented Pyrolytic Graphite (HOPG) crystal and was demonstrated at the Tsinghua Thomson scattering X-ray source. The x-ray pulse is diffracted by a 15 mm (L) ×15 mm (H)× 1 mm (D) HOPG crystal with 1° mosaic spread. By analyzing the diffraction pattern, both x-ray peak energies and energy spectral bandwidths at different polar angles can be reconstructed, which agree well with the theoretical value and simulation. The higher integral reflectivity of the HOPG crystal makes this method possible for single-shot measurement.

  18. Monitoring the recrystallisation of amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering.

    PubMed

    Palomäki, Emmi; Ahvenainen, Patrik; Ehlers, Henrik; Svedström, Kirsi; Huotari, Simo; Yliruusi, Jouko

    2016-07-11

    In this paper we present a fast model system for monitoring the recrystallization of quench-cooled amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering. The use of these two methods enables comparison between surface and bulk crystallization. Non-ordered mesoporous silica micro-particles were added to the system in order to alter the rate of crystallization of the amorphous xylitol. Raman measurements showed that adding silica to the system increased the rate of surface crystallization, while X-ray measurements showed that the rate of bulk crystallization decreased. Using this model system it is possible to measure fast changes, which occur in minutes or within a few hours. Raman-spectroscopy and wide-angle X-ray scattering were found to be complementary techniques when assessing surface and bulk crystallization of amorphous xylitol. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Time-Resolved Small-Angle X-ray Scattering Reveals Millisecond Transitions of a DNA Origami Switch.

    PubMed

    Bruetzel, Linda K; Walker, Philipp U; Gerling, Thomas; Dietz, Hendrik; Lipfert, Jan

    2018-04-11

    Self-assembled DNA structures enable creation of specific shapes at the nanometer-micrometer scale with molecular resolution. The construction of functional DNA assemblies will likely require dynamic structures that can undergo controllable conformational changes. DNA devices based on shape complementary stacking interactions have been demonstrated to undergo reversible conformational changes triggered by changes in ionic environment or temperature. An experimentally unexplored aspect is how quickly conformational transitions of large synthetic DNA origami structures can actually occur. Here, we use time-resolved small-angle X-ray scattering to monitor large-scale conformational transitions of a two-state DNA origami switch in free solution. We show that the DNA device switches from its open to its closed conformation upon addition of MgCl 2 in milliseconds, which is close to the theoretical diffusive speed limit. In contrast, measurements of the dimerization of DNA origami bricks reveal much slower and concentration-dependent assembly kinetics. DNA brick dimerization occurs on a time scale of minutes to hours suggesting that the kinetics depend on local concentration and molecular alignment.

  20. 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

  1. X-ray and Neutron Scattering Study of the Formation of Core–Shell-Type Polyoxometalates

    DOE PAGES

    Yin, Panchao; Wu, Bin; Mamontov, Eugene; ...

    2016-02-05

    A typical type of core-shell polyoxometalates can be obtained through the Keggin-type polyoxometalate-templated growth of a layer of spherical shell structure of {Mo 72Fe 30}. Small angle X-ray scattering is used to study the structural features and stability of the core-shell structures in aqueous solutions. Time-resolved small angle X-ray scattering is applied to monitor the synthetic reactions and a three-stage formation mechanism is proposed to describe the synthesis of the core-shell polyoxometalates based on the monitoring results. Quasi-elastic and inelastic neutron scattering are used to probe the dynamics of water molecules in the core-shell structures and two different types ofmore » water molecules, the confined and structured water, are observed. These water molecules play an important role in bridging core and shell structures and stabilizing the cluster structures. A typical type of core shell polyoxometalates can be obtained through the Keggin-type polyoxometalate-templated growth of a layer of spherical shell structure of {Mo 72Fe 30}. Small-angle X-ray scattering is used to study the structural features and stability of the core shell structures in aqueous solutions. Time-resolved small-angle X-ray scattering is applied to monitor the synthetic reactions, and a three-stage formation mechanism is proposed to describe the synthesis of the core shell polyoxometalates based on the monitoring results. New protocols have been developed by fitting the X-ray data with custom physical models, which provide more convincing, objective, and completed data interpretation. Quasi-elastic and inelastic neutron scattering are used to probe the dynamics of water molecules in the core shell structures, and two different types of water molecules, the confined and structured water, are observed. These water molecules play an important role in bridging core and shell structures and stabilizing the cluster structures.« less

  2. Superhydrophobic surfaces allow probing of exosome self organization using X-ray scattering

    NASA Astrophysics Data System (ADS)

    Accardo, Angelo; Tirinato, Luca; Altamura, Davide; Sibillano, Teresa; Giannini, Cinzia; Riekel, Christian; di Fabrizio, Enzo

    2013-02-01

    Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates.Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr34032e

  3. Low-angle X-ray scattering properties of irradiated spices

    NASA Astrophysics Data System (ADS)

    Almeida, A. P. G.; Braz, D.; Barroso, R. C.; Lopes, R. T.

    2007-09-01

    The scattering of X-rays at low angles (LAXS) is a technique dominated by the coherent scattering process. One characteristic observation of low-angle coherent scattering is the so-called molecular interference effect, being characterized by the presence of one or more peaks in the forward direction of scattering. In the present study, LAXS profiles from five different spices are carefully measured in order to establish characteristic scattering signatures. Samples of Ceylon cinnamon, cumin, nutmeg, paprika and black pepper were bought in local market in Rio de Janeiro, Brazil. The LAXS patterns were obtained using a Shimadzu DRX 6000 diffractometer in reflection geometry. Coherent scattering patterns are measured for the samples for θ=5-35°. The data were collected in 0.05° increments every 3 s. In order to evaluate the possible molecular structure changes caused to the irradiation procedure, the signatures obtained for control (non-irradiated) spices were compared with spice samples irradiated with different doses varying from 3 to 40 kGy. The LAXS patterns of all samples were obtained after 30, 60, 90, 120 days to evaluate the effect of storage period. Scattering profiles from spices irradiated with different irradiation doses were obtained and the results compared. For each spice, there is no considerable deviation in shape in function of the irradiation dose. It indicates that the molecular structure of each analyzed spices is preserved considering the dose range chosen. The results show that the molecular structure was found to be stable during storage at the ambient temperature for up to 4 months.

  4. Modular structure of the full-length DNA gyrase B subunit revealed by small-angle X-ray scattering.

    PubMed

    Costenaro, Lionel; Grossmann, J Günter; Ebel, Christine; Maxwell, Anthony

    2007-03-01

    DNA gyrase, the only topoisomerase able to introduce negative supercoils into DNA, is essential for bacterial transcription and replication; absent from humans, it is a successful target for antibacterials. From biophysical experiments in solution, we report a structural model at approximately 12-15 A resolution of the full-length B subunit (GyrB). Analytical ultracentrifugation shows that GyrB is mainly a nonglobular monomer. Ab initio modeling of small-angle X-ray scattering data for GyrB consistently yields a "tadpole"-like envelope. It allows us to propose an organization of GyrB into three domains-ATPase, Toprim, and Tail-based on their crystallographic and modeled structures. Our study reveals the modular organization of GyrB and points out its potential flexibility, needed during the gyrase catalytic cycle. It provides important insights into the supercoiling mechanism by gyrase and suggests new lines of research.

  5. Early nucleation events in the polymerization of actin, probed by time-resolved small-angle x-ray scattering

    PubMed Central

    Oda, Toshiro; Aihara, Tomoki; Wakabayashi, Katsuzo

    2016-01-01

    Nucleators generating new F-actin filaments play important roles in cell activities. Detailed information concerning the events involved in nucleation of actin alone in vitro is fundamental to understanding these processes, but such information has been hard to come by. We addressed the early process of salt-induced polymerization of actin using the time-resolved synchrotron small-angle X-ray scattering (SAXS). Actin molecules in low salt solution maintain a monomeric state by an electrostatic repulsive force between molecules. On mixing with salts, the repulsive force was rapidly screened, causing an immediate formation of many of non-polymerizable dimers. SAXS kinetic analysis revealed that tetramerization gives the highest energetic barrier to further polymerization, and the major nucleation is the formation of helical tetramers. Filaments start to grow rapidly with the formation of pentamers. These findings suggest an acceleration mechanism of actin assembly by a variety of nucleators in cells. PMID:27775032

  6. Anomalous small-angle scattering as a way to solve the Babinet principle problem

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

    Boiko, M. E., E-mail: m.e.boiko@mail.ioffe.ru; Sharkov, M. D.; Boiko, A. M.

    2013-12-15

    X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

  7. Anomalous small-angle scattering as a way to solve the Babinet principle problem

    NASA Astrophysics Data System (ADS)

    Boiko, M. E.; Sharkov, M. D.; Boiko, A. M.; Bobyl, A. V.

    2013-12-01

    X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

  8. Structural characterization of the human cerebral myelin sheath by small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    DeFelici, M.; Felici, R.; Ferrero, C.; Tartari, A.; Gambaccini, M.; Finet, S.

    2008-10-01

    Myelin is a multi-lamellar membrane surrounding neuronal axons and increasing their conduction velocity. When investigated by small-angle x-ray scattering (SAXS), the lamellar quasi-periodical arrangement of the myelin sheath gives rise to distinct peaks, which allow the determination of its molecular organization and the dimensions of its substructures. In this study we report on the myelin sheath structural determination carried out on a set of human brain tissue samples coming from surgical biopsies of two patients: a man around 60 and a woman nearly 90 years old. The samples were extracted either from white or grey cerebral matter and did not undergo any manipulation or chemical-physical treatment, which could possibly have altered their structure, except dipping them into a formalin solution for their conservation. Analysis of the scattered intensity from white matter of intact human cerebral tissue allowed the evaluation not only of the myelin sheath periodicity but also of its electronic charge density profile. In particular, the thicknesses of the cytoplasm and extracellular regions were established, as well as those of the hydrophilic polar heads and hydrophobic tails of the lipid bilayer. SAXS patterns were measured at several locations on each sample in order to establish the statistical variations of the structural parameters within a single sample and among different samples. This work demonstrates that a detailed structural analysis of the myelin sheath can also be carried out in randomly oriented samples of intact human white matter, which is of importance for studying the aetiology and evolution of the central nervous system pathologies inducing myelin degeneration.

  9. Purification, crystallization, small-angle X-ray scattering and preliminary X-ray diffraction analysis of the SH2 domain of the Csk-homologous kinase.

    PubMed

    Gunn, Natalie J; Gorman, Michael A; Dobson, Renwick C J; Parker, Michael W; Mulhern, Terrence D

    2011-03-01

    The C-terminal Src kinase (Csk) and Csk-homologous kinase (CHK) are endogenous inhibitors of the proto-oncogenic Src family of protein tyrosine kinases (SFKs). Phosphotyrosyl peptide binding to their Src-homology 2 (SH2) domains activates Csk and CHK, enhancing their ability to suppress SFK signalling; however, the detailed mechanistic basis of this activation event is unclear. The CHK SH2 was expressed in Escherichia coli and the purified protein was characterized as monomeric by synchrotron small-angle X-ray scattering in-line with size-exclusion chromatography. The CHK SH2 crystallized in 0.2 M sodium bromide, 0.1 M bis-Tris propane pH 6.5 and 20% polyethylene glycol 3350 and the best crystals diffracted to ∼1.6 Å resolution. The crystals belonged to space group P2, with unit-cell parameters a=25.8, b=34.6, c=63.2 Å, β=99.4°.

  10. High-throughput biological small-angle X-ray scattering with a robotically loaded capillary cell

    PubMed Central

    Nielsen, S. S.; Møller, M.; Gillilan, R. E.

    2012-01-01

    With the rise in popularity of biological small-angle X-ray scattering (BioSAXS) measurements, synchrotron beamlines are confronted with an ever-increasing number of samples from a wide range of solution conditions. To meet these demands, an increasing number of beamlines worldwide have begun to provide automated liquid-handling systems for sample loading. This article presents an automated sample-loading system for BioSAXS beamlines, which combines single-channel disposable-tip pipetting with a vacuum-enclosed temperature-controlled capillary flow cell. The design incorporates an easily changeable capillary to reduce the incidence of X-ray window fouling and cross contamination. Both the robot-control and the data-processing systems are written in Python. The data-processing code, RAW, has been enhanced with several new features to form a user-friendly BioSAXS pipeline for the robot. The flow cell also supports efficient manual loading and sample recovery. An effective rinse protocol for the sample cell is developed and tested. Fluid dynamics within the sample capillary reveals a vortex ring pattern of circulation that redistributes radiation-damaged material. Radiation damage is most severe in the boundary layer near the capillary surface. At typical flow speeds, capillaries below 2 mm in diameter are beginning to enter the Stokes (creeping flow) regime in which mixing due to oscillation is limited. Analysis within this regime shows that single-pass exposure and multiple-pass exposure of a sample plug are functionally the same with regard to exposed volume when plug motion reversal is slow. The robot was tested on three different beamlines at the Cornell High-Energy Synchrotron Source, with a variety of detectors and beam characteristics, and it has been used successfully in several published studies as well as in two introductory short courses on basic BioSAXS methods. PMID:22509071

  11. Intrinsic flexibility of West Nile virus protease in solution characterized using small-angle X-ray scattering.

    PubMed

    Garces, Andrea P; Watowich, Stanley J

    2013-10-01

    West Nile virus (WNV) is a mosquito-borne flavivirus with a rapidly expanding global distribution. Infection can cause severe neurological disease and fatality in humans. Efforts are ongoing to develop antiviral drugs that inhibit the WNV protease, a viral enzyme required for polyprotein processing. Unfortunately, little is known about the solution structure of recombinant WNV protease (NS2B-NS3pro) used for antiviral drug discovery and development, although X-ray crystal structures and nuclear magnetic resonance (NMR) studies have provided valuable insights into the interactions between NS2B-NS3pro and peptide-based inhibitors. We completed small-angle X-ray scattering and Fourier transform infrared spectroscopy experiments to determine the solution structure and dynamics of WNV NS2B-NS3pro in the absence of a bound substrate or inhibitor. Importantly, these solution studies suggested that all or most of the NS2B cofactor was highly flexible and formed an ensemble of structures, in contrast to the NS2B tertiary structures observed in crystallographic and NMR studies. The secondary structure of NS2B-NS3pro in solution had high β-content, similar to the secondary structure observed in crystallographic studies. This work provided evidence of the intrinsic flexibility and conformational heterogeneity of the NS2B chain of the WNV protease in the absence of substratelike ligands, which should be considered during antiviral drug discovery and development efforts.

  12. Measurement of carbon condensation using small-angle x-ray scattering during detonation of the high explosive hexanitrostilbene

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

    Bagge-Hansen, M.; Lauderbach, L. M.; Hodgin, R.

    2015-06-24

    The dynamics of carboncondensation in detonating high explosives remains controversial. Detonation model validation requires data for processes occurring at nanometer length scales on time scales ranging from nanoseconds to microseconds. A new detonation endstation has been commissioned to acquire and provide time-resolved small-angle x-ray scattering (SAXS) from detonating explosives. Hexanitrostilbene (HNS) was selected as the first to investigate due to its ease of initiation using exploding foils and flyers, vacuum compatibility, high thermal stability, and stoichiometric carbon abundance that produces high carbon condensate yields. The SAXS data during detonation, collected with 300 ns time resolution, provide unprecedented signal fidelity overmore » a broad q-range. This fidelity permits the first analysis of both the Guinier and Porod/power-law regions of the scattering profile during detonation, which contains information about the size and morphology of the resultant carbon condensate nanoparticles. To bolster confidence in these data, the scattering angle and intensity were additionally cross-referenced with a separate, highly calibrated SAXS beamline. The data show that HNS produces carbon particles with a radius of gyration of 2.7 nm in less than 400 ns after the detonation front has passed, and this size and morphology are constant over the next several microseconds. These data directly contradict previous pioneering work on RDX/TNT mixtures and TATB, where observations indicate significant particle growth (50% or more) continues over several microseconds. As a result, the power-law slope is about –3, which is consistent with a complex disordered, irregular, or folded sp 2 sub-arrangement within a relatively monodisperse structure possessing radius of gyration of 2.7 nm after the detonation of HNS.« less

  13. Stimulated Electronic X-Ray Raman Scattering

    NASA Astrophysics Data System (ADS)

    Weninger, Clemens; Purvis, Michael; Ryan, Duncan; London, Richard A.; Bozek, John D.; Bostedt, Christoph; Graf, Alexander; Brown, Gregory; Rocca, Jorge J.; Rohringer, Nina

    2013-12-01

    We demonstrate strong stimulated inelastic x-ray scattering by resonantly exciting a dense gas target of neon with femtosecond, high-intensity x-ray pulses from an x-ray free-electron laser (XFEL). A small number of lower energy XFEL seed photons drive an avalanche of stimulated resonant inelastic x-ray scattering processes that amplify the Raman scattering signal by several orders of magnitude until it reaches saturation. Despite the large overall spectral width, the internal spiky structure of the XFEL spectrum determines the energy resolution of the scattering process in a statistical sense. This is demonstrated by observing a stochastic line shift of the inelastically scattered x-ray radiation. In conjunction with statistical methods, XFELs can be used for stimulated resonant inelastic x-ray scattering, with spectral resolution smaller than the natural width of the core-excited, intermediate state.

  14. Small-Angle Neutron Scattering on Crosslink Distribution of Epoxy Networks.

    DTIC Science & Technology

    1985-10-01

    distinct second phase or heterogeneity has been detected. Small- angle X-ray scattering (SAXS), 1 nuclear magnetic resonance (NMR) ,2 electron ... paramagnetic resonance (EPR),3 and glass transition 4temperature (Tg) measurements reveal a second phase which is attri- . buted to a heterogeneous...FUNDING/SPONSORING lab. OFFICE SYMBOL 9. PROCUREMENT INSTRUMENT IDENTIFICATION NUMBER * ORGANIZATION I (If applticable)j F3361 5-84-C-5020 * Bc ADDRESS

  15. Experimental set-up for time resolved small angle X-ray scattering studies of nanoparticles formation using a free-jet micromixer

    NASA Astrophysics Data System (ADS)

    Marmiroli, Benedetta; Grenci, Gianluca; Cacho-Nerin, Fernando; Sartori, Barbara; Laggner, Peter; Businaro, Luca; Amenitsch, Heinz

    2010-02-01

    Recently, we have designed, fabricated and tested a free-jet micromixer for time resolved small angle X-ray scattering (SAXS) studies of nanoparticles formation in the <100 μs time range. The microjet has a diameter of 25 μm and a time of first accessible measurement of 75 μs has been obtained. This result can still be improved. In this communication, we present a method to estimate whether a given chemical or biological reaction can be investigated with the micromixer, and to optimize the beam size for the measurement at the chosen SAXS beamline. Moreover, we describe a system based on stereoscopic imaging which allows the alignment of the jet with the X-ray beam with a precision of 20 μm. The proposed experimental procedures have been successfully employed to observe the formation of calcium carbonate (CaCO 3) nanoparticles from the reaction of sodium carbonate (Na 2CO 3) and calcium chloride (CaCl 2). The induction time has been estimated in the order of 200 μs and the determined radius of the particles is about 14 nm.

  16. The use of small angle X-ray scattering (SAXS) for the characterisation of lustre surfaces in Renaissance majolica

    NASA Astrophysics Data System (ADS)

    Fermo, P.; Cariati, F.; Cipriani, C.; Canetti, M.; Padeletti, G.; Brunetti, B.; Sgamellotti, A.

    2002-01-01

    In this work some Renaissance lustre decorated ceramics have been examined. Our attention was directed to lustre which is a thin decorative metallic film applied on the surfaces of previously glazed ancient pottery. Some 16th century lustre ceramics shards from Deruta, Umbria (Italy) have been analysed by small angle X-ray scattering (SAXS) in order to characterise the dimension of the metal nanocrystals forming the thin lustre layer. This technique appeared to be a powerful tool to characterise lustre films nanostructure and may be successfully used for this purpose together with transmission electron microscopy (TEM). Furthermore, SAXS measurements are extremely suitable for the determination of polydispersity and average interparticle distance. The lustre surfaces have been also analysed by scanning electron microscopy plus X-ray energy dispersive spectrometry (SEM-EDX) in order to identify the metals present (silver, copper or both of them) and to establish copper/silver ratios. From the comparison between SAXS results and compositional data, it was possible to conclude that copper particles are smaller than the silver ones. We have evidenced how the microtexture as well as the chemical composition of the lustre layers are responsible for the gold or red colour typical of the lustre films.

  17. BioXTAS RAW: improvements to a free open-source program for small-angle X-ray scattering data reduction and analysis.

    PubMed

    Hopkins, Jesse Bennett; Gillilan, Richard E; Skou, Soren

    2017-10-01

    BioXTAS RAW is a graphical-user-interface-based free open-source Python program for reduction and analysis of small-angle X-ray solution scattering (SAXS) data. The software is designed for biological SAXS data and enables creation and plotting of one-dimensional scattering profiles from two-dimensional detector images, standard data operations such as averaging and subtraction and analysis of radius of gyration and molecular weight, and advanced analysis such as calculation of inverse Fourier transforms and envelopes. It also allows easy processing of inline size-exclusion chromatography coupled SAXS data and data deconvolution using the evolving factor analysis method. It provides an alternative to closed-source programs such as Primus and ScÅtter for primary data analysis. Because it can calibrate, mask and integrate images it also provides an alternative to synchrotron beamline pipelines that scientists can install on their own computers and use both at home and at the beamline.

  18. Selective molecular annealing: in situ small angle X-ray scattering study of microwave-assisted annealing of block copolymers.

    PubMed

    Toolan, Daniel T W; Adlington, Kevin; Isakova, Anna; Kalamiotis, Alexis; Mokarian-Tabari, Parvaneh; Dimitrakis, Georgios; Dodds, Christopher; Arnold, Thomas; Terrill, Nick J; Bras, Wim; Hermida Merino, Daniel; Topham, Paul D; Irvine, Derek J; Howse, Jonathan R

    2017-08-09

    Microwave annealing has emerged as an alternative to traditional thermal annealing approaches for optimising block copolymer self-assembly. A novel sample environment enabling small angle X-ray scattering to be performed in situ during microwave annealing is demonstrated, which has enabled, for the first time, the direct study of the effects of microwave annealing upon the self-assembly behavior of a model, commercial triblock copolymer system [polystyrene-block-poly(ethylene-co-butylene)-block-polystyrene]. Results show that the block copolymer is a poor microwave absorber, resulting in no change in the block copolymer morphology upon application of microwave energy. The block copolymer species may only indirectly interact with the microwave energy when a small molecule microwave-interactive species [diethylene glycol dibenzoate (DEGDB)] is incorporated directly into the polymer matrix. Then significant morphological development is observed at DEGDB loadings ≥6 wt%. Through spatial localisation of the microwave-interactive species, we demonstrate targeted annealing of specific regions of a multi-component system, opening routes for the development of "smart" manufacturing methodologies.

  19. X-ray scattering data and structural genomics

    NASA Astrophysics Data System (ADS)

    Doniach, Sebastian

    2003-03-01

    High throughput structural genomics has the ambitious goal of determining the structure of all, or a very large number of protein folds using the high-resolution techniques of protein crystallography and NMR. However, the program is facing significant bottlenecks in reaching this goal, which include problems of protein expression and crystallization. In this talk, some preliminary results on how the low-resolution technique of small-angle X-ray solution scattering (SAXS) can help ameliorate some of these bottlenecks will be presented. One of the most significant bottlenecks arises from the difficulty of crystallizing integral membrane proteins, where only a handful of structures are available compared to thousands of structures for soluble proteins. By 3-dimensional reconstruction from SAXS data, the size and shape of detergent-solubilized integral membrane proteins can be characterized. This information can then be used to classify membrane proteins which constitute some 25% of all genomes. SAXS may also be used to study the dependence of interparticle interference scattering on solvent conditions so that regions of the protein solution phase diagram which favor crystallization can be elucidated. As a further application, SAXS may be used to provide physical constraints on computational methods for protein structure prediction based on primary sequence information. This in turn can help in identifying structural homologs of a given protein, which can then give clues to its function. D. Walther, F. Cohen and S. Doniach. "Reconstruction of low resolution three-dimensional density maps from one-dimensional small angle x-ray scattering data for biomolecules." J. Appl. Cryst. 33(2):350-363 (2000). Protein structure prediction constrained by solution X-ray scattering data and structural homology identification Zheng WJ, Doniach S JOURNAL OF MOLECULAR BIOLOGY , v. 316(#1) pp. 173-187 FEB 8, 2002

  20. Structure of star-burst dendrimers: a comparison between small angle x-ray scattering and computer simulation results.

    PubMed

    Rathgeber, Silke; Pakula, Tadeusz; Urban, Volker

    2004-08-22

    We investigated the generation dependent shape and internal structure of star-burst dendrimers under good solvent conditions using small angle x-ray scattering and molecular modeling. Measurements have been performed on poly(amidoamine) dendrimers with generations ranging from g=0 up to g=8 at low concentrations in methanol. We described the static form factor P(q) by a model taking into account the compact, globular shape as well as the loose, polymeric character of dendrimers. Monomer distributions within dendrimers are of special interest for potential applications and have been characterized by the pair correlation function gamma(r), as well as by the monomer and end-group density profile, rho(r) and rho(e)(r), respectively. Monomer density profiles and gamma(r) can be derived from P(q) by modeling and via a model independent approach using the inverse Fourier transformation algorithm first introduced by Glatter. Experimental results are compared with computer simulations performed for single dendrimers of various generations using the cooperative motion algorithm. The simulation gives direct access to gamma(r) and rho(r), allows an independent determination of P(q), and yields in addition to the scattering experiment information about the distribution of the end groups. Excellent qualitative agreement between experiment and simulation has been found. (c) 2004 American Institute of Physics

  1. Position Accuracy of Gold Nanoparticles on DNA Origami Structures Studied with Small-Angle X-ray Scattering.

    PubMed

    Hartl, Caroline; Frank, Kilian; Amenitsch, Heinz; Fischer, Stefan; Liedl, Tim; Nickel, Bert

    2018-04-11

    DNA origami objects allow for accurate positioning of guest molecules in three dimensions. Validation and understanding of design strategies for particle attachment as well as analysis of specific particle arrangements are desirable. Small-angle X-ray scattering (SAXS) is suited to probe distances of nano-objects with subnanometer resolution at physiologically relevant conditions including pH and salt and at varying temperatures. Here, we show that the pair density distribution function (PDDF) obtained from an indirect Fourier transform of SAXS intensities in a model-free way allows to investigate prototypical DNA origami-mediated gold nanoparticle (AuNP) assemblies. We analyze the structure of three AuNP-dimers on a DNA origami block, an AuNP trimer constituted by those dimers, and a helical arrangement of nine AuNPs on a DNA origami cylinder. For the dimers, we compare the model-free PDDF and explicit modeling of the SAXS intensity data by superposition of scattering intensities of the scattering objects. The PDDF of the trimer is verified to be a superposition of its dimeric contributions, that is, here AuNP-DNA origami assemblies were used as test boards underlining the validity of the PDDF analysis beyond pairs of AuNPs. We obtain information about AuNP distances with an uncertainty margin of 1.2 nm. This readout accuracy in turn can be used for high precision placement of AuNP by careful design of the AuNP attachment sites on the DNA-structure and by fine-tuning of the connector types.

  2. Measurement of carbon condensates using small-angle x-ray scattering during detonation of the high explosive hexanitrostilbene

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

    Bagge-Hansen, M.; Lauderbach, L.; Hodgin, R.

    2015-06-28

    The dynamics of carbon condensation in detonating high explosives remains controversial. Detonation model validation requires data for processes occurring at nanometer length scales on time scales ranging from nanoseconds to microseconds. A new detonation endstation has been commissioned to acquire and provide time-resolved small-angle x-ray scattering (SAXS) from detonating explosives. Hexanitrostilbene (HNS) was selected as the first to investigate due to its ease of initiation using exploding foils and flyers, vacuum compatibility, high thermal stability, and stoichiometric carbon abundance that produces high carbon condensate yields. The SAXS data during detonation, collected with 300 ns time resolution, provide unprecedented signal fidelity overmore » a broad q-range. This fidelity permits the first analysis of both the Guinier and Porod/power-law regions of the scattering profile during detonation, which contains information about the size and morphology of the resultant carbon condensate nanoparticles. To bolster confidence in these data, the scattering angle and intensity were additionally cross-referenced with a separate, highly calibrated SAXS beamline. The data show that HNS produces carbon particles with a radius of gyration of 2.7 nm in less than 400 ns after the detonation front has passed, and this size and morphology are constant over the next several microseconds. These data directly contradict previous pioneering work on RDX/TNT mixtures and TATB, where observations indicate significant particle growth (50% or more) continues over several microseconds. The power-law slope is about −3, which is consistent with a complex disordered, irregular, or folded sp{sup 2} sub-arrangement within a relatively monodisperse structure possessing radius of gyration of 2.7 nm after the detonation of HNS.« less

  3. Measurement of carbon condensates using small-angle x-ray scattering during detonation of the high explosive hexanitrostilbene

    DOE PAGES

    Bagge-Hansen, M.; Lauderbach, L.; Hodgin, R.; ...

    2015-06-24

    In this study, the dynamics of carbon condensation in detonating high explosives remains controversial. Detonation model validation requires data for processes occurring at nanometer length scales on time scales ranging from nanoseconds to microseconds. A new detonation end station has been commissioned to acquire and provide time-resolved small-angle x-ray scattering (SAXS) from detonating explosives. Hexanitrostilbene (HNS) was selected as the first to investigate due to its ease of initiation using exploding foils and flyers, vacuum compatibility, high thermal stability, and stoichiometric carbon abundance that produces high carbon condensate yields. The SAXS data during detonation, collected with 300 ns time resolution,more » provide unprecedented signal fidelity over a broad q-range. This fidelity permits the first analysis of both the Guinier and Porod/power-law regions of the scattering profile during detonation, which contains information about the size and morphology of the resultant carbon condensate nanoparticles. To bolster confidence in these data, the scattering angle and intensity were additionally cross-referenced with a separate, highly calibrated SAXS beamline. The data show that HNS produces carbon particles with a radius of gyration of 2.7 nm in less than 400 ns after the detonation front has passed, and this size and morphology are constant over the next several microseconds. These data directly contradict previous pioneering work on RDX/TNT mixtures and TATB, where observations indicate significant particle growth (50% or more) continues over several microseconds. The power-law slope is about -3, which is consistent with a complex disordered, irregular, or folded sp 2 sub-arrangement within a relatively monodisperse structure possessing radius of gyration of 2.7 nm after the detonation of HNS.« less

  4. Quantitative determination of the lateral density and intermolecular correlation between proteins anchored on the membrane surfaces using grazing incidence small-angle X-ray scattering and grazing incidence X-ray fluorescence.

    PubMed

    Abuillan, Wasim; Vorobiev, Alexei; Hartel, Andreas; Jones, Nicola G; Engstler, Markus; Tanaka, Motomu

    2012-11-28

    As a physical model of the surface of cells coated with densely packed, non-crystalline proteins coupled to lipid anchors, we functionalized the surface of phospholipid membranes by coupling of neutravidin to biotinylated lipid anchors. After the characterization of fine structures perpendicular to the plane of membrane using specular X-ray reflectivity, the same membrane was characterized by grazing incidence small angle X-ray scattering (GISAXS). Within the framework of distorted wave Born approximation and two-dimensional Percus-Yevick function, we can analyze the form and structure factors of the non-crystalline, membrane-anchored proteins for the first time. As a new experimental technique to quantify the surface density of proteins on the membrane surface, we utilized grazing incidence X-ray fluorescence (GIXF). Here, the mean intermolecular distance between proteins from the sulfur peak intensities can be calculated by applying Abelé's matrix formalism. The characteristic correlation distance between non-crystalline neutravidin obtained by the GISAXS analysis agrees well with the intermolecular distance calculated by GIXF, suggesting a large potential of the combination of GISAXS and GIXF in probing the lateral density and correlation of non-crystalline proteins displayed on the membrane surface.

  5. An Assessment of Critical Dimension Small Angle X-ray Scattering Metrology for Advanced Semiconductor Manufacturing

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

    Settens, Charles M.

    2015-01-01

    Simultaneous migration of planar transistors to FinFET architectures, the introduction of a plurality of materials to ensure suitable electrical characteristics, and the establishment of reliable multiple patterning lithography schemes to pattern sub-10 nm feature sizes imposes formidable challenges to current in-line dimensional metrologies. Because the shape of a FinFET channel cross-section immediately influences the electrical characteristics, the evaluation of 3D device structures requires measurement of parameters beyond traditional critical dimension (CD), including their sidewall angles, top corner rounding and footing, roughness, recesses and undercuts at single nanometer dimensions; thus, metrologies require sub-nm and approaching atomic level measurement uncertainty. Synchrotron criticalmore » dimension small angle X-ray scattering (CD-SAXS) has unique capabilities to non-destructively monitor the cross-section shape of surface structures with single nanometer uncertainty and can perform overlay metrology to sub-nm uncertainty. In this dissertation, we perform a systematic experimental investigation using CD-SAXS metrology on a hierarchy of semiconductor 3D device architectures including, high-aspect-ratio contact holes, H2 annealed Si fins, and a series of grating type samples at multiple points along a FinFET fabrication process increasing in structural intricacy and ending with fully fabricated FinFET. Comparative studies between CD-SAXS metrology and other relevant semiconductor dimensional metrologies, particularly CDSEM, CD-AFM and TEM are used to determine physical limits of CD-SAXS approach for advanced semiconductor samples. CD-SAXS experimental tradeoffs, advice for model-dependent analysis and thoughts on the compatibility with a semiconductor manufacturing environment are discussed.« less

  6. Metastable ripple phase of fully hydrated dipalmitoylphosphatidylcholine as studied by small angle x-ray scattering

    PubMed Central

    Yao, Haruhiko; Matuoka, Sinzi; Tenchov, Boris; Hatta, Ichiro

    1991-01-01

    Fully hydrated dipalmitoylphosphatidylcholine (DPPC) undergoes liquid crystalline to metastable Pβ, phase transition in cooling. A small angle x-ray scattering study has been performed for obtaining further evidence about the structure of this phase. From a high-resolution observation of x-ray diffraction profiles, a distinct multipeak pattern has become obvious. Among them the (01) reflection in the secondary ripple structure is identified clearly. There are peaks assigned straightforwardly to (10) and (20) reflections in the primary ripple structure and peaks assigned to (10) and (20) reflections in the secondary ripple structure. Therefore the multipeak pattern is due to superposition of the reflections cause by the primary and secondary ripple structures. The lattice parameters are estimated as follows: for the primary ripple structure a = 7.09 nm, b = 13.64 nm, and γ = 95°, and for the secondary ripple structure a = 8.2 nm, b = 26.6 nm, and γ = 90°. The lattice parameters thus obtained for the secondary ripple structure are not conclusive, however. The hydrocarbon chains in the primary ripple structure have been reported as being tilted against the bilayer plane and, on the other hand, the hydrocarbon chains in the secondary ripple structure are likely to be perpendicular to the bilayer plane. This fact seems to be related to a sequential mechanism of phase transitions. On heating from the Lβ, phase where the hydrocarbon chains are tilted the primary ripple structure having tilted hydrocarbon chains takes place and on cooling from the Lα phase where the hydrocarbon chains are not tilted the secondary ripple structure with untilted chains tends to be stabilized. It appears that the truly metastable ripple phase is expressed by the second ripple structure although in the course of the actual cooling transition both the secondary and primary ripple structures form and coexist. PMID:19431787

  7. Small-angle X-ray scattering reveals the solution structure of the full-length DNA gyrase a subunit.

    PubMed

    Costenaro, Lionel; Grossmann, J Günter; Ebel, Christine; Maxwell, Anthony

    2005-02-01

    DNA gyrase is the topoisomerase uniquely able to actively introduce negative supercoils into DNA. Vital in all bacteria, but absent in humans, this enzyme is a successful target for antibacterial drugs. From biophysical experiments in solution, we report the low-resolution structure of the full-length A subunit (GyrA). Analytical ultracentrifugation shows that GyrA is dimeric, but nonglobular. Ab initio modeling from small-angle X-ray scattering allows us to retrieve the molecular envelope of GyrA and thereby the organization of its domains. The available crystallographic structure of the amino-terminal domain (GyrA59) forms a dimeric core, and two additional pear-shaped densities closely flank it in an unexpected position. Each accommodates very well a carboxyl-terminal domain (GyrA-CTD) built from a homologous crystallographic structure. The uniqueness of gyrase is due to the ability of the GyrA-CTDs to wrap DNA. Their position within the GyrA structure strongly suggests a large conformation change of the enzyme upon DNA binding.

  8. Determination by Small-angle X-ray Scattering of Pore Size Distribution in Nanoporous Track-etched Polycarbonate Membranes

    NASA Astrophysics Data System (ADS)

    Jonas, A. M.; Legras, R.; Ferain, E.

    1998-03-01

    Nanoporous track-etched membranes with narrow pore size distributions and average pore size diameters tunable from 100 to 1000 Åare produced by the chemical etching of latent tracks in polymer films after irradiation by a beam of accelerated heavy ions. Nanoporous membranes are used for highly demanding filtration purposes, or as templates to obtain metallic or polymeric nanowires (L. Piraux et al., Nucl. Instr. Meth. Phys. Res. 1997, B131, 357). Such applications call for developments in nanopore size characterization techniques. In this respect, we report on the characterization by small-angle X-ray scattering (SAXS) of nanopore size distribution (nPSD) in polycarbonate track-etched membranes. The obtention of nPSD requires inverting an ill-conditioned inhomogeneous equation. We present different numerical routes to overcome the amplification of experimental errors in the resulting solutions, including a regularization technique allowing to obtain the nPSD without a priori knowledge of its shape. The effect of deviations from cylindrical pore shape on the resulting distributions are analyzed. Finally, SAXS results are compared to results obtained by electron microscopy and conductometry.

  9. Structure of Immune Stimulating Complex Matrices and Immune Stimulating Complexes in Suspension Determined by Small-Angle X-Ray Scattering

    PubMed Central

    Pedersen, Jan Skov; Oliveira, Cristiano L.P.; Hübschmann, Henriette Baun; Arleth, Lise; Manniche, Søren; Kirkby, Nicolai; Nielsen, Hanne Mørck

    2012-01-01

    Immune stimulating complex (ISCOM) particles consisting of a mixture of Quil-A, cholesterol, and phospholipids were structurally characterized by small-angle x-ray scattering (SAXS). The ISCOM particles are perforated vesicles of very well-defined structures. We developed and implemented a novel (to our knowledge) modeling method based on Monte Carlo simulation integrations to describe the SAXS data. This approach is similar to the traditional modeling of SAXS data, in which a structure is assumed, the scattering intensity is calculated, and structural parameters are optimized by weighted least-squares methods when the model scattering intensity is fitted to the experimental data. SAXS data from plain ISCOM matrix particles in aqueous suspension, as well as those from complete ISCOMs (i.e., with an antigen (tetanus toxoid) incorporated) can be modeled as a polydisperse distribution of perforated bilayer vesicles with icosahedral, football, or tennis ball structures. The dominating structure is the tennis ball structure, with an outer diameter of 40 nm and with 20 holes 5–6 nm in diameter. The lipid bilayer membrane is 4.6 nm thick, with a low-electron-density, 2.0-nm-thick hydrocarbon core. Surprisingly, in the ISCOMs, the tetanus toxoid is located just below the membrane inside the particles. PMID:22677391

  10. Accurate optimization of amino acid form factors for computing small-angle X-ray scattering intensity of atomistic protein structures

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

    Tong, Dudu; Yang, Sichun; Lu, Lanyuan

    2016-06-20

    Structure modellingviasmall-angle X-ray scattering (SAXS) data generally requires intensive computations of scattering intensity from any given biomolecular structure, where the accurate evaluation of SAXS profiles using coarse-grained (CG) methods is vital to improve computational efficiency. To date, most CG SAXS computing methods have been based on a single-bead-per-residue approximation but have neglected structural correlations between amino acids. To improve the accuracy of scattering calculations, accurate CG form factors of amino acids are now derived using a rigorous optimization strategy, termed electron-density matching (EDM), to best fit electron-density distributions of protein structures. This EDM method is compared with and tested againstmore » other CG SAXS computing methods, and the resulting CG SAXS profiles from EDM agree better with all-atom theoretical SAXS data. By including the protein hydration shell represented by explicit CG water molecules and the correction of protein excluded volume, the developed CG form factors also reproduce the selected experimental SAXS profiles with very small deviations. Taken together, these EDM-derived CG form factors present an accurate and efficient computational approach for SAXS computing, especially when higher molecular details (represented by theqrange of the SAXS data) become necessary for effective structure modelling.« less

  11. A new small-angle X-ray scattering set-up on the crystallography beamline I711 at MAX-lab.

    PubMed

    Knaapila, M; Svensson, C; Barauskas, J; Zackrisson, M; Nielsen, S S; Toft, K N; Vestergaard, B; Arleth, L; Olsson, U; Pedersen, J S; Cerenius, Y

    2009-07-01

    A small-angle X-ray scattering (SAXS) set-up has recently been developed at beamline I711 at the MAX II storage ring in Lund (Sweden). An overview of the required modifications is presented here together with a number of application examples. The accessible q range in a SAXS experiment is 0.009-0.3 A(-1) for the standard set-up but depends on the sample-to-detector distance, detector offset, beamstop size and wavelength. The SAXS camera has been designed to have a low background and has three collinear slit sets for collimating the incident beam. The standard beam size is about 0.37 mm x 0.37 mm (full width at half-maximum) at the sample position, with a flux of 4 x 10(10) photons s(-1) and lambda = 1.1 A. The vacuum is of the order of 0.05 mbar in the unbroken beam path from the first slits until the exit window in front of the detector. A large sample chamber with a number of lead-throughs allows different sample environments to be mounted. This station is used for measurements on weakly scattering proteins in solutions and also for colloids, polymers and other nanoscale structures. A special application supported by the beamline is the effort to establish a micro-fluidic sample environment for structural analysis of samples that are only available in limited quantities. Overall, this work demonstrates how a cost-effective SAXS station can be constructed on a multipurpose beamline.

  12. The Small-Angle Neutron Scattering Data Analysis of the Phospholipid Transport Nanosystem Structure

    NASA Astrophysics Data System (ADS)

    Zemlyanaya, E. V.; Kiselev, M. A.; Zhabitskaya, E. I.; Aksenov, V. L.; Ipatova, O. M.; Ivankov, O. I.

    2018-05-01

    The small-angle neutron scattering technique (SANS) is employed for investigation of structure of the phospholipid transport nanosystem (PTNS) elaborated in the V.N.Orekhovich Institute of Biomedical Chemistry (Moscow, Russia). The SANS spectra have been measured at the YuMO small-angle spectrometer of IBR-2 reactor (Joint Institute of Nuclear Research, Dubna, Russia). Basic characteristics of polydispersed population of PTNS unilamellar vesicles (average radius of vesicles, polydispersity, thickness of membrane, etc.) have been determined in three cases of the PTNS concentrations in D2O: 5%, 10%, and 25%. Numerical analysis is based on the separated form factors method (SFF). The results are discussed in comparison with the results of analysis of the small-angle X-ray scattering spectra collected at the Kurchatov Synchrotron Radiation Source of the National Research Center “Kurchatov Institute” (Moscow, Russia).

  13. Nanometer-scale characterization of laser-driven compression, shocks, and phase transitions, by x-ray scattering using free electron lasers

    DOE PAGES

    Kluge, T.; Rödel, C.; Rödel, M.; ...

    2017-10-23

    In this paper, we study the feasibility of using small angle X-ray scattering (SAXS) as a new experimental diagnostic for intense laser-solid interactions. By using X-ray pulses from a hard X-ray free electron laser, we can simultaneously achieve nanometer and femtosecond resolution of laser-driven samples. This is an important new capability for the Helmholtz international beamline for extreme fields at the high energy density endstation currently built at the European X-ray free electron laser. We review the relevant SAXS theory and its application to transient processes in solid density plasmas and report on first experimental results that confirm the feasibilitymore » of the method. Finally, we present results of two test experiments where the first experiment employs ultra-short laser pulses for studying relativistic laser plasma interactions, and the second one focuses on shock compression studies with a nanosecond laser system.« less

  14. Nanometer-scale characterization of laser-driven compression, shocks, and phase transitions, by x-ray scattering using free electron lasers

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

    Kluge, T.; Rödel, C.; Rödel, M.

    In this paper, we study the feasibility of using small angle X-ray scattering (SAXS) as a new experimental diagnostic for intense laser-solid interactions. By using X-ray pulses from a hard X-ray free electron laser, we can simultaneously achieve nanometer and femtosecond resolution of laser-driven samples. This is an important new capability for the Helmholtz international beamline for extreme fields at the high energy density endstation currently built at the European X-ray free electron laser. We review the relevant SAXS theory and its application to transient processes in solid density plasmas and report on first experimental results that confirm the feasibilitymore » of the method. Finally, we present results of two test experiments where the first experiment employs ultra-short laser pulses for studying relativistic laser plasma interactions, and the second one focuses on shock compression studies with a nanosecond laser system.« less

  15. X-ray coherent scattering tomography of textured material (Conference Presentation)

    NASA Astrophysics Data System (ADS)

    Zhu, Zheyuan; Pang, Shuo

    2017-05-01

    Small-angle X-ray scattering (SAXS) measures the signature of angular-dependent coherently scattered X-rays, which contains richer information in material composition and structure compared to conventional absorption-based computed tomography. SAXS image reconstruction method of a 2 or 3 dimensional object based on computed tomography, termed as coherent scattering computed tomography (CSCT), enables the detection of spatially-resolved, material-specific isotropic scattering signature inside an extended object, and provides improved contrast for medical diagnosis, security screening, and material characterization applications. However, traditional CSCT methods assumes materials are fine powders or amorphous, and possess isotropic scattering profiles, which is not generally true for all materials. Anisotropic scatters cannot be captured using conventional CSCT method and result in reconstruction errors. To obtain correct information from the sample, we designed new imaging strategy which incorporates extra degree of detector motion into X-ray scattering tomography for the detection of anisotropic scattered photons from a series of two-dimensional intensity measurements. Using a table-top, narrow-band X-ray source and a panel detector, we demonstrate the anisotropic scattering profile captured from an extended object and the reconstruction of a three-dimensional object. For materials possessing a well-organized crystalline structure with certain symmetry, the scatter texture is more predictable. We will also discuss the compressive schemes and implementation of data acquisition to improve the collection efficiency and accelerate the imaging process.

  16. Abstract ID: 176 Geant4 implementation of inter-atomic interference effect in small-angle coherent X-ray scattering for materials of medical interest.

    PubMed

    Paternò, Gianfranco; Cardarelli, Paolo; Contillo, Adriano; Gambaccini, Mauro; Taibi, Angelo

    2018-01-01

    Advanced applications of digital mammography such as dual-energy and tomosynthesis require multiple exposures and thus deliver higher dose compared to standard mammograms. A straightforward manner to reduce patient dose without affecting image quality would be removal of the anti-scatter grid, provided that the involved reconstruction algorithms are able to take the scatter figure into account [1]. Monte Carlo simulations are very well suited for the calculation of X-ray scatter distribution and can be used to integrate such information within the reconstruction software. Geant4 is an open source C++ particle tracking code widely used in several physical fields, including medical physics [2,3]. However, the coherent scattering cross section used by the standard Geant4 code does not take into account the influence of molecular interference. According to the independent atomic scattering approximation (the so-called free-atom model), coherent radiation is indistinguishable from primary radiation because its angular distribution is peaked in the forward direction. Since interference effects occur between x-rays scattered by neighbouring atoms in matter, it was shown experimentally that the scatter distribution is affected by the molecular structure of the target, even in amorphous materials. The most important consequence is that the coherent scatter distribution is not peaked in the forward direction, and the position of the maximum is strongly material-dependent [4]. In this contribution, we present the implementation of a method to take into account inter-atomic interference in small-angle coherent scattering in Geant4, including a dedicated data set of suitable molecular form factor values for several materials of clinical interest. Furthermore, we present scatter images of simple geometric phantoms in which the Rayleigh contribution is rigorously evaluated. Copyright © 2017.

  17. Changes in small angle X-ray scattering parameters observed upon ligand binding to rabbit muscle pyruvate kinase are not correlated with allosteric transitions†

    PubMed Central

    Fenton, Aron W.; Williams, Rachel; Trewhella, Jill

    2010-01-01

    Protein fluorescence and small-angle X-ray scattering (SAXS) have been used to monitor effector affinity and conformational changes previously associated with allosteric regulation in rabbit muscle pyruvate kinase (M1-PYK). In the absence of substrate (phosphoenolpyruvate; PEP), SAXS-monitored conformational changes in M1-PYK elicited by the binding of phenylalanine (an allosteric inhibitor that reduces the affinity of M1-PYK for PEP) are similar to those observed upon binding of alanine or 2-aminobutyric acid. Under the current assay conditions, these small amino acids bind to the protein, but elicit a minimal change in the affinity of the protein for PEP. Therefore, if changes in scattering signatures represent cleft closure via domain rotation as previously interpreted, it can be concluded that these motions are not sufficient to elicit allosteric inhibition. Additionally, although PEP has similar affinities for the free enzyme and the M1-PYK/small-amino-acid complexes (i.e. the small amino acids have minimal allosteric effects), PEP binding elicits different changes in the SAXS signature of the free enzyme vs. the M1-PYK/small-amino-acid complexes. PMID:20712377

  18. A high pressure study of calmodulin-ligand interactions using small-angle X-ray and elastic incoherent neutron scattering.

    PubMed

    Cinar, Süleyman; Al-Ayoubi, Samy; Sternemann, Christian; Peters, Judith; Winter, Roland; Czeslik, Claus

    2018-01-31

    Calmodulin (CaM) is a Ca 2+ sensor and mediates Ca 2+ signaling through binding of numerous target ligands. The binding of ligands by Ca 2+ -saturated CaM (holo-CaM) is governed by attractive hydrophobic and electrostatic interactions that are weakened under high pressure in aqueous solutions. Moreover, the potential formation of void volumes upon ligand binding creates a further source of pressure sensitivity. Hence, high pressure is a suitable thermodynamic variable to probe protein-ligand interactions. In this study, we compare the binding of two different ligands to holo-CaM as a function of pressure by using X-ray and neutron scattering techniques. The two ligands are the farnesylated hypervariable region (HVR) of the K-Ras4B protein, which is a natural binding partner of holo-CaM, and the antagonist trifluoperazine (TFP), which is known to inhibit holo-CaM activity. From small-angle X-ray scattering experiments performed up to 3000 bar, we observe a pressure-induced partial unfolding of the free holo-CaM in the absence of ligands, where the two lobes of the dumbbell-shaped protein are slightly swelled. In contrast, upon binding TFP, holo-CaM forms a closed globular conformation, which is pressure stable at least up to 3000 bar. The HVR of K-Ras4B shows a different binding behavior, and the data suggest the dissociation of the holo-CaM/HVR complex under high pressure, probably due to a less dense protein contact of the HVR as compared to TFP. The elastic incoherent neutron scattering experiments corroborate these findings. Below 2000 bar, pressure induces enhanced atomic fluctuations in both holo-CaM/ligand complexes, but those of the holo-CaM/HVR complex seem to be larger. Thus, the inhibition of holo-CaM by TFP is supported by a low-volume ligand binding, albeit this is not associated with a rigidification of the complex structure on the sub-ns Å-scale.

  19. Small-angle solution scattering using the mixed-mode pixel array detector.

    PubMed

    Koerner, Lucas J; Gillilan, Richard E; Green, Katherine S; Wang, Suntao; Gruner, Sol M

    2011-03-01

    Solution small-angle X-ray scattering (SAXS) measurements were obtained using a 128 × 128 pixel X-ray mixed-mode pixel array detector (MMPAD) with an 860 µs readout time. The MMPAD offers advantages for SAXS experiments: a pixel full-well of >2 × 10(7) 10 keV X-rays, a maximum flux rate of 10(8) X-rays pixel(-1) s(-1), and a sub-pixel point-spread function. Data from the MMPAD were quantitatively compared with data from a charge-coupled device (CCD) fiber-optically coupled to a phosphor screen. MMPAD solution SAXS data from lysozyme solutions were of equal or better quality than data captured by the CCD. The read-noise (normalized by pixel area) of the MMPAD was less than that of the CCD by an average factor of 3.0. Short sample-to-detector distances were required owing to the small MMPAD area (19.2 mm × 19.2 mm), and were revealed to be advantageous with respect to detector read-noise. As predicted by the Shannon sampling theory and confirmed by the acquisition of lysozyme solution SAXS curves, the MMPAD at short distances is capable of sufficiently sampling a solution SAXS curve for protein shape analysis. The readout speed of the MMPAD was demonstrated by continuously monitoring lysozyme sample evolution as radiation damage accumulated. These experiments prove that a small suitably configured MMPAD is appropriate for time-resolved solution scattering measurements.

  20. Small-angle solution scattering using the mixed-mode pixel array detector

    PubMed Central

    Koerner, Lucas J.; Gillilan, Richard E.; Green, Katherine S.; Wang, Suntao; Gruner, Sol M.

    2011-01-01

    Solution small-angle X-ray scattering (SAXS) measurements were obtained using a 128 × 128 pixel X-ray mixed-mode pixel array detector (MMPAD) with an 860 µs readout time. The MMPAD offers advantages for SAXS experiments: a pixel full-well of >2 × 107 10 keV X-rays, a maximum flux rate of 108 X-rays pixel−1 s−1, and a sub-pixel point-spread function. Data from the MMPAD were quantitatively compared with data from a charge-coupled device (CCD) fiber-optically coupled to a phosphor screen. MMPAD solution SAXS data from lysozyme solutions were of equal or better quality than data captured by the CCD. The read-noise (normalized by pixel area) of the MMPAD was less than that of the CCD by an average factor of 3.0. Short sample-to-detector distances were required owing to the small MMPAD area (19.2 mm × 19.2 mm), and were revealed to be advantageous with respect to detector read-noise. As predicted by the Shannon sampling theory and confirmed by the acquisition of lysozyme solution SAXS curves, the MMPAD at short distances is capable of sufficiently sampling a solution SAXS curve for protein shape analysis. The readout speed of the MMPAD was demonstrated by continuously monitoring lysozyme sample evolution as radiation damage accumulated. These experiments prove that a small suitably configured MMPAD is appropriate for time-resolved solution scattering measurements. PMID:21335900

  1. Structural Significance of Lipid Diversity as Studied by Small Angle Neutron and X-ray Scattering

    DOE PAGES

    Kučerka, Norbert; Heberle, Frederick A.; Pan, Jianjun; ...

    2015-09-21

    In this paper, we review recent developments in the rapidly growing field of membrane biophysics, with a focus on the structural properties of single lipid bilayers determined by different scattering techniques, namely neutron and X-ray scattering. The need for accurate lipid structural properties is emphasized by the sometimes conflicting results found in the literature, even in the case of the most studied lipid bilayers. Increasingly, accurate and detailed structural models require more experimental data, such as those from contrast varied neutron scattering and X-ray scattering experiments that are jointly refined with molecular dynamics simulations. This experimental and computational approach producesmore » robust bilayer structural parameters that enable insights, for example, into the interplay between collective membrane properties and its components (e.g., hydrocarbon chain length and unsaturation, and lipid headgroup composition). Finally, from model studies such as these, one is better able to appreciate how a real biological membrane can be tuned by balancing the contributions from the lipid’s different moieties (e.g., acyl chains, headgroups, backbones, etc.).« less

  2. Geant4 simulations of soft proton scattering in X-ray optics. A tentative validation using laboratory measurements

    NASA Astrophysics Data System (ADS)

    Fioretti, Valentina; Mineo, Teresa; Bulgarelli, Andrea; Dondero, Paolo; Ivanchenko, Vladimir; Lei, Fan; Lotti, Simone; Macculi, Claudio; Mantero, Alfonso

    2017-12-01

    Low energy protons (< 300 keV) can enter the field of view of X-ray telescopes, scatter on their mirror surfaces at small incident angles, and deposit energy on the detector. This phenomenon can cause intense background flares at the focal plane decreasing the mission observing time (e.g. the XMM-Newton mission) or in the most extreme cases, damaging the X-ray detector. A correct modelization of the physics process responsible for the grazing angle scattering processes is mandatory to evaluate the impact of such events on the performance (e.g. observation time, sensitivity) of future X-ray telescopes as the ESA ATHENA mission. The Remizovich model describes particles reflected by solids at glancing angles in terms of the Boltzmann transport equation using the diffuse approximation and the model of continuous slowing down in energy. For the first time this solution, in the approximation of no energy losses, is implemented, verified, and qualitatively validated on top of the Geant4 release 10.2, with the possibility to add a constant energy loss to each interaction. This implementation is verified by comparing the simulated proton distribution to both the theoretical probability distribution and with independent ray-tracing simulations. Both the new scattering physics and the Coulomb scattering already built in the official Geant4 distribution are used to reproduce the latest experimental results on grazing angle proton scattering. At 250 keV multiple scattering delivers large proton angles and it is not consistent with the observation. Among the tested models, the single scattering seems to better reproduce the scattering efficiency at the three energies but energy loss obtained at small scattering angles is significantly lower than the experimental values. In general, the energy losses obtained in the experiment are higher than what obtained by the simulation. The experimental data are not completely representative of the soft proton scattering experienced by

  3. Transformation from Multilamellar to Unilamellar Vesicles by Addition of a Cationic Lipid to PEGylated Liposomes Explored with Synchrotron Small Angle X-ray Scattering

    NASA Astrophysics Data System (ADS)

    Sakuragi, Mina; Koiwai, Kazunori; Nakamura, Kouji; Masunaga, Hiroyasu; Ogawa, Hiroki; Sakurai, Kazuo

    2011-01-01

    PEGylated liposomes composed of a benzamidine derivative (TRX), hydrogenated soybean phosphatidylcholine (HSPC), and N-(monomethoxy-polyethyleneglycolcarbamyl) distearoyl phosphatidylethanolamine (PEG-PE) were examined in terms of how the addition of TRX affects their structures with small angle x-ray scattering (SAXS) as well as transmission electron microscopy (TEM). TEM images showed the presence of unilamella vesicles for both with and without TRX, though a small amount of multilamella vesicles were observed in absence of TRX. We analyzed SAXS profiles at contained TRX composition combined with contrast variation technique by adding PEG solution and unilamella vesicle model could be reproduced. Subsequently, we analyzed SAXS profiles at no TRX composition. The mixture model of unilamella and multilamella vesicle was reconstructed and we estimated about 10 % multilamella vesicles from a fitting parameter.

  4. 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

  5. Resolution of ab initio shapes determined from small-angle scattering.

    PubMed

    Tuukkanen, Anne T; Kleywegt, Gerard J; Svergun, Dmitri I

    2016-11-01

    Spatial resolution is an important characteristic of structural models, and the authors of structures determined by X-ray crystallography or electron cryo-microscopy always provide the resolution upon publication and deposition. Small-angle scattering of X-rays or neutrons (SAS) has recently become a mainstream structural method providing the overall three-dimensional structures of proteins, nucleic acids and complexes in solution. However, no quantitative resolution measure is available for SAS-derived models, which significantly hampers their validation and further use. Here, a method is derived for resolution assessment for ab initio shape reconstruction from scattering data. The inherent variability of the ab initio shapes is utilized and it is demonstrated how their average Fourier shell correlation function is related to the model resolution. The method is validated against simulated data for proteins with known high-resolution structures and its efficiency is demonstrated in applications to experimental data. It is proposed that henceforth the resolution be reported in publications and depositions of ab initio SAS models.

  6. Resolution of ab initio shapes determined from small-angle scattering

    PubMed Central

    Tuukkanen, Anne T.; Kleywegt, Gerard J.; Svergun, Dmitri I.

    2016-01-01

    Spatial resolution is an important characteristic of structural models, and the authors of structures determined by X-ray crystallography or electron cryo-microscopy always provide the resolution upon publication and deposition. Small-angle scattering of X-rays or neutrons (SAS) has recently become a mainstream structural method providing the overall three-dimensional structures of proteins, nucleic acids and complexes in solution. However, no quantitative resolution measure is available for SAS-derived models, which significantly hampers their validation and further use. Here, a method is derived for resolution assessment for ab initio shape reconstruction from scattering data. The inherent variability of the ab initio shapes is utilized and it is demonstrated how their average Fourier shell correlation function is related to the model resolution. The method is validated against simulated data for proteins with known high-resolution structures and its efficiency is demonstrated in applications to experimental data. It is proposed that henceforth the resolution be reported in publications and depositions of ab initio SAS models. PMID:27840683

  7. Dimensions and Global Twist of Single-Layer DNA Origami Measured by Small-Angle X-ray Scattering.

    PubMed

    Baker, Matthew A B; Tuckwell, Andrew J; Berengut, Jonathan F; Bath, Jonathan; Benn, Florence; Duff, Anthony P; Whitten, Andrew E; Dunn, Katherine E; Hynson, Robert M; Turberfield, Andrew J; Lee, Lawrence K

    2018-06-04

    The rational design of complementary DNA sequences can be used to create nanostructures that self-assemble with nanometer precision. DNA nanostructures have been imaged by atomic force microscopy and electron microscopy. Small-angle X-ray scattering (SAXS) provides complementary structural information on the ensemble-averaged state of DNA nanostructures in solution. Here we demonstrate that SAXS can distinguish between different single-layer DNA origami tiles that look identical when immobilized on a mica surface and imaged with atomic force microscopy. We use SAXS to quantify the magnitude of global twist of DNA origami tiles with different crossover periodicities: these measurements highlight the extreme structural sensitivity of single-layer origami to the location of strand crossovers. We also use SAXS to quantify the distance between pairs of gold nanoparticles tethered to specific locations on a DNA origami tile and use this method to measure the overall dimensions and geometry of the DNA nanostructure in solution. Finally, we use indirect Fourier methods, which have long been used for the interpretation of SAXS data from biomolecules, to measure the distance between DNA helix pairs in a DNA origami nanotube. Together, these results provide important methodological advances in the use of SAXS to analyze DNA nanostructures in solution and insights into the structures of single-layer DNA origami.

  8. Poisson's ratio of collagen fibrils measured by small angle X-ray scattering of strained bovine pericardium

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

    Wells, Hannah C.; Sizeland, Katie H.; Kayed, Hanan R.

    Type I collagen is the main structural component of skin, tendons, and skin products, such as leather. Understanding the mechanical performance of collagen fibrils is important for understanding the mechanical performance of the tissues that they make up, while the mechanical properties of bulk tissue are well characterized, less is known about the mechanical behavior of individual collagen fibrils. In this study, bovine pericardium is subjected to strain while small angle X-ray scattering (SAXS) patterns are recorded using synchrotron radiation. The change in d-spacing, which is a measure of fibril extension, and the change in fibril diameter are determined frommore » SAXS. The tissue is strained 0.25 (25%) with a corresponding strain in the collagen fibrils of 0.045 observed. The ratio of collagen fibril width contraction to length extension, or the Poisson's ratio, is 2.1 ± 0.7 for a tissue strain from 0 to 0.25. This Poisson's ratio indicates that the volume of individual collagen fibrils decreases with increasing strain, which is quite unlike most engineering materials. This high Poisson's ratio of individual fibrils may contribute to high Poisson's ratio observed for tissues, contributing to some of the remarkable properties of collagen-based materials.« less

  9. The Structure of Urease Activation Complexes Examined by Flexibility Analysis, Mutagenesis, and Small-Angle X-Ray Scattering

    PubMed Central

    Quiroz-Valenzuela, Soledad; Sukuru, Sai Chetan K.; Hausinger, Robert P.; Kuhn, Leslie A.; Heller, William T.

    2008-01-01

    Conformational changes of Klebsiella aerogenes urease apoprotein (UreABC)3 induced upon binding of the UreD and UreF accessory proteins were examined by a combination of flexibility analysis, mutagenesis, and small-angle x-ray scattering (SAXS). ProFlex analysis of urease provided evidence that the major domain of UreB can move in a hinge-like motion to account for prior chemical cross-linking results. Rigidification of the UreB hinge region, accomplished through a G11P mutation, reduced the extent of urease activation, in part by decreasing the nickel content of the mutant enzyme, and by sequestering a portion of the urease apoprotein in a novel activation complex that includes all of the accessory proteins. SAXS analyses of urease, (UreABC-UreD)3, and (UreABC-UreDF)3 confirm that UreD and UreF bind near UreB at the periphery of the (UreAC)3 structure. This study supports an activation model in which a domain-shifted UreB conformation in (UreABC-UreDF)3 allows CO2 and nickel ions to gain access to the nascent active site. PMID:18823937

  10. X-Ray Dust Scattering At Small Angles: The Complete Halo Around GX13+1

    NASA Technical Reports Server (NTRS)

    Smith, Randall K.

    2007-01-01

    The exquisite angular resolution available with Chandra should allow precision measurements of faint diffuse emission surrounding bright sources, such as the X-ray scattering halos created by interstellar dust. However, the ACIS CCDs suffer from pileup when observing bright sources, and this creates difficulties when trying to extract the scattered halo near the source. The initial study of the X-ray halo around GX13+1 using only the ACIS-I detector done by Smith, Edgar & Shafer (2002) suffered from a lack of sensitivity within 50" of the source, limiting what conclusions could be drawn. To address this problem, observations of GX13+1 were obtained with the Chandra HRC-I and simultaneously with the RXTE PCA. Combined with the existing ACIS-I data, this allowed measurements of the X-ray halo between 2-1000". After considering a range of dust models, each assumed to be smoothly distributed with or without a dense cloud along the line of sight, the results show that there is no evidence in this data for a dense cloud near the source, as suggested by Xiang et al. (2005). In addition, although no model leads to formally acceptable results, the Weingartner & Draine (2001) and all but one of the composite grain models from Zubko, Dwek & Arendt (2004) give particularly poor fits.

  11. Ultra-high-resolution inelastic X-ray scattering at high-repetition-rate self-seeded X-ray free-electron lasers

    PubMed Central

    Chubar, Oleg; Geloni, Gianluca; Kocharyan, Vitali; Madsen, Anders; Saldin, Evgeni; Serkez, Svitozar; Shvyd’ko, Yuri; Sutter, John

    2016-01-01

    Inelastic X-ray scattering (IXS) is an important tool for studies of equilibrium dynamics in condensed matter. A new spectrometer recently proposed for ultra-high-resolution IXS (UHRIX) has achieved 0.6 meV and 0.25 nm−1 spectral and momentum-transfer resolutions, respectively. However, further improvements down to 0.1 meV and 0.02 nm−1 are required to close the gap in energy–momentum space between high- and low-frequency probes. It is shown that this goal can be achieved by further optimizing the X-ray optics and by increasing the spectral flux of the incident X-ray pulses. UHRIX performs best at energies from 5 to 10 keV, where a combination of self-seeding and undulator tapering at the SASE-2 beamline of the European XFEL promises up to a 100-fold increase in average spectral flux compared with nominal SASE pulses at saturation, or three orders of magnitude more than what is possible with storage-ring-based radiation sources. Wave-optics calculations show that about 7 × 1012 photons s−1 in a 90 µeV bandwidth can be achieved on the sample. This will provide unique new possibilities for dynamics studies by IXS. PMID:26917127

  12. Ultra-high-resolution inelastic X-ray scattering at high-repetition-rate self-seeded X-ray free-electron lasers

    DOE PAGES

    Chubar, Oleg; Geloni, Gianluca; Kocharyan, Vitali; ...

    2016-03-01

    Inelastic X-ray scattering (IXS) is an important tool for studies of equilibrium dynamics in condensed matter. A new spectrometer recently proposed for ultra-high-resolution IXS (UHRIX) has achieved 0.6 meV and 0.25 nm ₋1spectral and momentum-transfer resolutions, respectively. However, further improvements down to 0.1 meV and 0.02 nm ₋1are required to close the gap in energy–momentum space between high- and low-frequency probes. It is shown that this goal can be achieved by further optimizing the X-ray optics and by increasing the spectral flux of the incident X-ray pulses. UHRIX performs best at energies from 5 to 10 keV, where a combinationmore » of self-seeding and undulator tapering at the SASE-2 beamline of the European XFEL promises up to a 100-fold increase in average spectral flux compared with nominal SASE pulses at saturation, or three orders of magnitude more than what is possible with storage-ring-based radiation sources. Wave-optics calculations show that about 7 × 10 12 photons s ₋1in a 90 µeV bandwidth can be achieved on the sample. Ultimately, this will provide unique new possibilities for dynamics studies by IXS.« less

  13. In situ ultra-small-angle X-ray scattering study under uniaxial stretching of colloidal crystals prepared by silica nanoparticles bearing hydrogen-bonding polymer grafts

    DOE PAGES

    Ishige, Ryohei; Williams, Gregory A.; Higaki, Yuji; ...

    2016-04-19

    A molded film of single-component polymer-grafted nanoparticles (SPNP), consisting of a spherical silica core and densely grafted polymer chains bearing hydrogen-bonding side groups capable of physical crosslinking, was investigated byin situultra-small-angle X-ray scattering (USAXS) measurement during a uniaxial stretching process. Static USAXS revealed that the molded SPNP formed a highly oriented twinned face-centered cubic (f.c.c.) lattice structure with the [11-1] plane aligned nearly parallel to the film surface in the initial state. Structural analysis ofin situUSAXS using a model of uniaxial deformation induced by rearrangement of the nanoparticles revealed that the f.c.c. lattice was distorted in the stretching direction inmore » proportion to the macroscopic strain until the strain reached 35%, and subsequently changed into other f.c.c. lattices with different orientations. The lattice distortion and structural transition behavior corresponded well to the elastic and plastic deformation regimes, respectively, observed in the stress–strain curve. The attractive interaction of the hydrogen bond is considered to form only at the top surface of the shell and then plays an effective role in cross-linking between nanoparticles. The rearrangement mechanism of the nanoparticles is well accounted for by a strong repulsive interaction between the densely grafted polymer shells of neighboring particles.« less

  14. Assessment study of ion-exchange chromatography combined with solution X-ray scattering measurement for protein characterization.

    PubMed

    Watanabe, Yasushi

    2018-03-02

    The performance of ion-exchange chromatography combined with small-angle X-ray scattering measurement was evaluated by characterization of the hen egg white lysozyme as a model protein. The X-ray transmittance was estimated using a micro-ionization chamber equipped with a sample cell holder for the real-time monitoring of the X-ray beam strength through the salt gradient elution. The radius of gyration of the eluted protein was estimated to be 1.50 ± 0.06 (n = 3) nm and 1.4 ± 0.1 nm as the value at the zero protein concentration. By using the X-ray transmittance values for the scattering intensity correction, the molecular weight of the eluted protein was estimated to be 15,200 ± 500 (n = 3) and 14,400 ± 200 as the value at the zero protein concentration. These values are close to those of the monomer of this protein. The ion-exchange chromatography combined with the small-angle X-ray scattering measurement system equipped with the X-ray transmittance monitor is a reliable method for protein characterization in solution. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. The morphology of blends of linear and branched polyethylenes by small-angle neutron and x-ray scattering

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

    Londono, J.D.; Wignall, G.D.; Lin, J.S.

    1995-12-31

    The solid-state morphology and liquid-state homogeneity of blends of high-density polyethylene (HDPE) and low-density polyethylene (LDPE) were investigated by small-angle neutron and x-ray scattering (SANS and SAXS). The solid state morphology was investigated as a function of composition and cooling rate from the melt. After slow cooling, the evidence indicated that the mixtures were either completely (HDPE-rich blends) or almost completely (LDPE-rich blends) phase separated into separate HDPE and LDPE lamellae over the whole compositional range. In contrast, for rapidly quenched blends the components are extensively co-crystallized for all concentrations, though the SANS data indicated that the branched component hadmore » a tendency to be preferentially located in the inter-lamellar regions. In the liquid state, the blends were homogeneous at all compositions, showing that the solid state morphology is not determined by the melt structure, but is a function of the crystallization kinetics. Further evidence for blend homogeneity in the liquid is presented. In particular the authors examine the hypothesis that a phase separated mixture might give a scattering pattern similar to a homogeneous blend if the domain sizes were larger than the maximum spatial resolution of the SANS experiment (D > 2{pi}/Q{sub min} {approximately} 2,000 {angstrom}). In this scenario, the differential scattering cross section d{Sigma}/d{Omega}(Q) {approximately} Q{sup {minus}2}, though phase separation decreases the cross section in this Q-range with respect to the homogeneous blend. For HDPE/LDPE blends in the melt, this decrease in intensity was not observed, thus ruling out the possibility of phase separation.« less

  16. Protein structural dynamics in solution unveiled via 100-ps time-resolved x-ray scattering.

    PubMed

    Cho, Hyun Sun; Dashdorj, Naranbaatar; Schotte, Friedrich; Graber, Timothy; Henning, Robert; Anfinrud, Philip

    2010-04-20

    We have developed a time-resolved x-ray scattering diffractometer capable of probing structural dynamics of proteins in solution with 100-ps time resolution. This diffractometer, developed on the ID14B BioCARS (Consortium for Advanced Radiation Sources) beamline at the Advanced Photon Source, records x-ray scattering snapshots over a broad range of q spanning 0.02-2.5 A(-1), thereby providing simultaneous coverage of the small-angle x-ray scattering (SAXS) and wide-angle x-ray scattering (WAXS) regions. To demonstrate its capabilities, we have tracked structural changes in myoglobin as it undergoes a photolysis-induced transition from its carbon monoxy form (MbCO) to its deoxy form (Mb). Though the differences between the MbCO and Mb crystal structures are small (rmsd < 0.2 A), time-resolved x-ray scattering differences recorded over 8 decades of time from 100 ps to 10 ms are rich in structure, illustrating the sensitivity of this technique. A strong, negative-going feature in the SAXS region appears promptly and corresponds to a sudden > 22 A(3) volume expansion of the protein. The ensuing conformational relaxation causes the protein to contract to a volume approximately 2 A(3) larger than MbCO within approximately 10 ns. On the timescale for CO escape from the primary docking site, another change in the SAXS/WAXS fingerprint appears, demonstrating sensitivity to the location of the dissociated CO. Global analysis of the SAXS/WAXS patterns recovered time-independent scattering fingerprints for four intermediate states of Mb. These SAXS/WAXS fingerprints provide stringent constraints for putative models of conformational states and structural transitions between them.

  17. 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

  18. Kinetics of copper growth on graphene revealed by time-resolved small-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Hodas, M.; Siffalovic, P.; Jergel, M.; Pelletta, M.; Halahovets, Y.; Vegso, K.; Kotlar, M.; Majkova, E.

    2017-01-01

    Metal growth on graphene has many applications. Transition metals are known to favor three-dimensional (3D) cluster growth on graphene. Copper is of particular interest for cost-effective surface-supported catalysis applications and as a contact material in electronics. This paper presents an in situ real-time study of Cu growth kinetics on graphene covering all stages preceding formation of a continuous film performed by laboratory-based grazing-incidence small-angle x-ray scattering (GISAXS) technique. In particular, nucleation and 3D cluster growth, coalescence, and percolation stages were identified. The cluster nucleation saturates after reaching a density of 1012c m-2 at ≈1 monolayer thickness. A Kratky plot and a paracrystal model with cumulative structural disorder were necessary to evaluate properly cluster growth and coalescence, respectively. The power law scaling constants 0.27 ±0.05 and 0.81 ±0.02 of the temporal evolution of Cu cluster size suggest the growth of isolated clusters and dynamic cluster coalescence keeping the cluster shape, respectively. Coalescence and percolation thresholds occur at Cu thicknesses of 2 ±0.4 and 8.8 ±0.7 nm , respectively. This paper demonstrates the potential of laboratory-based in situ GISAXS as a vital diagnostic tool for tailoring a large variety of Cu nanostructures on graphene based on an in situ Cu growth monitoring which is applicable in a broad range of deposition times.

  19. Effects of phosphonium-based ionic liquids on phospholipid membranes studied by small-angle X-ray scattering.

    PubMed

    Kontro, Inkeri; Svedström, Kirsi; Duša, Filip; Ahvenainen, Patrik; Ruokonen, Suvi-Katriina; Witos, Joanna; Wiedmer, Susanne K

    2016-12-01

    The effects of ionic liquids on model phospholipid membranes were studied by small-angle X-ray scattering, dynamic light scattering (DLS) and zeta potential measurements. Multilamellar 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine liposomes and large unilamellar vesicles composed of l-α-phosphatidylcholine (eggPC) and l-α-phosphatidylglycerol (eggPG) (80:20mol%) or eggPC, eggPG, and cholesterol (60:20:20mol%) were used as biomimicking membrane models. The effects of the phosphonium-based ionic liquids: tributylmethylphosphonium acetate, trioctylmethylphosphonium acetate, tributyl(tetradecyl)-phosphonium acetate, and tributyl(tetradecyl)-phosphonium chloride, were compared to those of 1-ethyl-3-methyl-imidazolium acetate. With multilamellar vesicles, the ionic liquids that did not disrupt liposomes decreased the lamellar spacing as a function of concentration. The magnitude of the effect depended on concentration for all studied ionic liquids. Using large unilamellar vesicles, first a slight decrease in the vesicle size, then aggregation of vesicles was observed by DLS for increasing ionic liquid concentrations. At concentrations just below those that caused aggregation of liposomes, large unilamellar vesicles were coated by ionic liquid cations, evidenced by a change in their zeta potential. The ability of phosphonium-based ionic liquids to affect liposomes is related to the length of the hydrocarbon chains in the cation. Generally, the ability of ionic liquids to disrupt liposomes goes hand in hand with inducing disorder in the phospholipid membrane. However, trioctylmethylphosphonium acetate selectively extracted and induced a well-ordered lamellar structure in phospholipids from disrupted cholesterol-containing large unilamellar vesicles. This kind of effect was not seen with any other combination of ionic liquids and liposomes. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  20. Geant4 simulations of a wide-angle x-ray focusing telescope

    NASA Astrophysics Data System (ADS)

    Zhao, Donghua; Zhang, Chen; Yuan, Weimin; Zhang, Shuangnan; Willingale, Richard; Ling, Zhixing

    2017-06-01

    The rapid development of X-ray astronomy has been made possible by widely deploying X-ray focusing telescopes on board many X-ray satellites. Geant4 is a very powerful toolkit for Monte Carlo simulations and has remarkable abilities to model complex geometrical configurations. However, the library of physical processes available in Geant4 lacks a description of the reflection of X-ray photons at a grazing incident angle which is the core physical process in the simulation of X-ray focusing telescopes. The scattering of low-energy charged particles from the mirror surfaces is another noteworthy process which is not yet incorporated into Geant4. Here we describe a Monte Carlo model of a simplified wide-angle X-ray focusing telescope adopting lobster-eye optics and a silicon detector using the Geant4 toolkit. With this model, we simulate the X-ray tracing, proton scattering and background detection. We find that: (1) the effective area obtained using Geant4 is in agreement with that obtained using Q software with an average difference of less than 3%; (2) X-rays are the dominant background source below 10 keV; (3) the sensitivity of the telescope is better by at least one order of magnitude than that of a coded mask telescope with the same physical dimensions; (4) the number of protons passing through the optics and reaching the detector by Firsov scattering is about 2.5 times that of multiple scattering for the lobster-eye telescope.

  1. Real-Time Grazing Incidence Small Angle X-Ray Scattering Studies of the Growth Kinetics of Sputter-Deposited Silicon Thin Films

    NASA Astrophysics Data System (ADS)

    Demasi, Alexander; Erdem, Gozde; Chinta, Priya; Headrick, Randall; Ludwig, Karl

    2012-02-01

    The fundamental kinetics of thin film growth remains an active area of investigation. In this study, silicon thin films were grown at room temperature on silicon substrates via both on-axis and off-axis plasma sputter deposition, while the evolution of surface morphology was measured in real time with in-situ grazing incidence small angle x-ray scattering (GISAXS) at the National Synchrotron Light Source. GISAXS is a surface-sensitive, non-destructive technique, and is therefore ideally suited to a study of this nature. In addition to investigating the effect of on-axis versus off-axis bombardment, the effect of sputter gas partial pressure was examined. Post-facto, ex-situ atomic force microscopy (AFM) was used to measure the final surface morphology of the films, which could subsequently be compared with the surface morphology determined by GISAXS. Comparisons are made between the observed surface evolution during growth and theoretical predictions. This work was supported by the Department of Energy, Office of Basic Energy Sciences.

  2. Studies of protein-protein and protein-water interactions by small angle x-ray scattering, terahertz spectroscopy, ASMOS, and computer simulation

    NASA Astrophysics Data System (ADS)

    Kim, Seung Joong

    The protein folding problem has been one of the most challenging subjects in biological physics due to its complexity. Energy landscape theory based on statistical mechanics provides a thermodynamic interpretation of the protein folding process. We have been working to answer fundamental questions about protein-protein and protein-water interactions, which are very important for describing the energy landscape surface of proteins correctly. At first, we present a new method for computing protein-protein interaction potentials of solvated proteins directly from SAXS data. An ensemble of proteins was modeled by Metropolis Monte Carlo and Molecular Dynamics simulations, and the global X-ray scattering of the whole model ensemble was computed at each snapshot of the simulation. The interaction potential model was optimized and iterated by a Levenberg-Marquardt algorithm. Secondly, we report that terahertz spectroscopy directly probes hydration dynamics around proteins and determines the size of the dynamical hydration shell. We also present the sequence and pH-dependence of the hydration shell and the effect of the hydrophobicity. On the other hand, kinetic terahertz absorption (KITA) spectroscopy is introduced to study the refolding kinetics of ubiquitin and its mutants. KITA results are compared to small angle X-ray scattering, tryptophan fluorescence, and circular dichroism results. We propose that KITA monitors the rearrangement of hydrogen bonding during secondary structure formation. Finally, we present development of the automated single molecule operating system (ASMOS) for a high throughput single molecule detector, which levitates a single protein molecule in a 10 microm diameter droplet by the laser guidance. I also have performed supporting calculations and simulations with my own program codes.

  3. Ab initio studies of ultrafast x-ray scattering of the photodissociation of iodine

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

    Debnarova, Andrea; Techert, Simone; Schmatz, Stefan

    2010-09-28

    We computationally examine various aspects of the reaction dynamics of the photodissociation and recombination of molecular iodine. We use our recently proposed formalism to calculate time-dependent x-ray scattering signal changes from first principles. Different aspects of the dynamics of this prototypical reaction are studied, such as coherent and noncoherent processes, features of structural relaxation that are periodic in time versus nonperiodic dissociative processes, as well as small electron density changes caused by electronic excitation, all with respect to x-ray scattering. We can demonstrate that wide-angle x-ray scattering offers a possibility to study the changes in electron densities in nonperiodic systems,more » which render it a suitable technique for the investigation of chemical reactions from a structural dynamics point of view.« less

  4. The Discovery of an Evolving Dust Scattered X-ray Halo Around GRB 031203

    NASA Technical Reports Server (NTRS)

    Vaughan, S.; Willingale, R.; OBrien, P. T.; Osborne, J. P.; Reeves, J. N.; Levan, A. J.; Watson, M. G.; Tedds, J. A.; Watson, D.; Santos-Lleo, M.

    2003-01-01

    We report the first detection of a time-dependent, dust-scattered X-ray halo around a gamma-ray burst. GRB3 031203 was observed by XMM-Newton starting six hours after the burst. The halo appeared as concentric ring-like structures centered on the GRB location. The radii of these structures increased with time as t(sup 1/2), consistent with small-angle X-ray scattering caused by a large column of dust along the line of sight to a cosmologically distant GRB. The rings are due to dust concentrated in two distinct slabs in the Galaxy located at distances of 880 and 1390 pc, consistent with known Galactic features. The halo brightness implies an initial soft X-ray pulse consistent with the observed GRB.

  5. A Hierarchical Algorithm for Fast Debye Summation with Applications to Small Angle Scattering

    PubMed Central

    Gumerov, Nail A.; Berlin, Konstantin; Fushman, David; Duraiswami, Ramani

    2012-01-01

    Debye summation, which involves the summation of sinc functions of distances between all pair of atoms in three dimensional space, arises in computations performed in crystallography, small/wide angle X-ray scattering (SAXS/WAXS) and small angle neutron scattering (SANS). Direct evaluation of Debye summation has quadratic complexity, which results in computational bottleneck when determining crystal properties, or running structure refinement protocols that involve SAXS or SANS, even for moderately sized molecules. We present a fast approximation algorithm that efficiently computes the summation to any prescribed accuracy ε in linear time. The algorithm is similar to the fast multipole method (FMM), and is based on a hierarchical spatial decomposition of the molecule coupled with local harmonic expansions and translation of these expansions. An even more efficient implementation is possible when the scattering profile is all that is required, as in small angle scattering reconstruction (SAS) of macromolecules. We examine the relationship of the proposed algorithm to existing approximate methods for profile computations, and show that these methods may result in inaccurate profile computations, unless an error bound derived in this paper is used. Our theoretical and computational results show orders of magnitude improvement in computation complexity over existing methods, while maintaining prescribed accuracy. PMID:22707386

  6. Dewetting of thin polymer films: an X-ray scattering study

    NASA Astrophysics Data System (ADS)

    Müller-Buschbaum, P.; Stamm, M.

    1998-06-01

    The surface morphology of different dewetting states of thin polymer films (polystyrene) on top of silicon substrates was investigated. With diffuse X-ray scattering in the region of total external reflection a high in-plane resolution was achieved. We observe a new nano-dewetting structure which coexists with the well known mesoscopic dewetting structures of holes, cellular pattern and drops. This nano-dewetting structure consists of small dimples with a diameter in the nanometer range. It results from the dewetting of a remaining ultra-thin polymer layer and can be explained with theoretical predictions of spinodal decomposition. The experimental results of the scattering study are confirmed with scanning-force microscopy measurements.

  7. Protein structural dynamics in solution unveiled via 100-ps time-resolved x-ray scattering

    PubMed Central

    Anfinrud, Philip

    2010-01-01

    We have developed a time-resolved x-ray scattering diffractometer capable of probing structural dynamics of proteins in solution with 100-ps time resolution. This diffractometer, developed on the ID14B BioCARS (Consortium for Advanced Radiation Sources) beamline at the Advanced Photon Source, records x-ray scattering snapshots over a broad range of q spanning 0.02–2.5 Å-1, thereby providing simultaneous coverage of the small-angle x-ray scattering (SAXS) and wide-angle x-ray scattering (WAXS) regions. To demonstrate its capabilities, we have tracked structural changes in myoglobin as it undergoes a photolysis-induced transition from its carbon monoxy form (MbCO) to its deoxy form (Mb). Though the differences between the MbCO and Mb crystal structures are small (rmsd < 0.2 Å), time-resolved x-ray scattering differences recorded over 8 decades of time from 100 ps to 10 ms are rich in structure, illustrating the sensitivity of this technique. A strong, negative-going feature in the SAXS region appears promptly and corresponds to a sudden > 22 Å3 volume expansion of the protein. The ensuing conformational relaxation causes the protein to contract to a volume ∼2 Å3 larger than MbCO within ∼10 ns. On the timescale for CO escape from the primary docking site, another change in the SAXS/WAXS fingerprint appears, demonstrating sensitivity to the location of the dissociated CO. Global analysis of the SAXS/WAXS patterns recovered time-independent scattering fingerprints for four intermediate states of Mb. These SAXS/WAXS fingerprints provide stringent constraints for putative models of conformational states and structural transitions between them. PMID:20406909

  8. The Structure of Urease Activiation Complexes Examined by Flexibility Analysis, Mutagenesis, and Small-angle X-ray Scattering Approaches

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

    Quiroz, Soledad; Sukuru, Sai Chetan K.; Hausinger, Robert P.

    2008-01-01

    Conformational changes of Klebsiella aerogenes urease apoprotein (UreABC){sub 3} induced upon binding of the UreD and UreF accessory proteins were examined by a combination of flexibility analysis, mutagenesis, and small-angle X-ray scattering (SAXS). ProFlex analysis of urease provided evidence that the major domain of UreB can move in a hinge-like motion to account for prior chemical cross-linking results. Rigidification of the UreB hinge region, accomplished through a G11P mutation, reduced the extent of urease activation, in part by decreasing the nickel content of the mutant enzyme, and by sequestering a portion of the urease apoprotein in a novel activation complexmore » that includes all of the accessory proteins. SAXS analyses of urease, (UreABC-UreD){sub 3}, and (UreABC-UreDF){sub 3} confirm that UreD and UreF bind near UreB at the periphery of the (UreAC){sub 3} structure. This study supports an activation model in which a domain-shifted UreB conformation in (UreABC-UreDF){sub 3} allows CO{sub 2} and nickel ions to gain access to the nascent active site.« less

  9. Small-angle X-ray scattering tensor tomography: model of the three-dimensional reciprocal-space map, reconstruction algorithm and angular sampling requirements.

    PubMed

    Liebi, Marianne; Georgiadis, Marios; Kohlbrecher, Joachim; Holler, Mirko; Raabe, Jörg; Usov, Ivan; Menzel, Andreas; Schneider, Philipp; Bunk, Oliver; Guizar-Sicairos, Manuel

    2018-01-01

    Small-angle X-ray scattering tensor tomography, which allows reconstruction of the local three-dimensional reciprocal-space map within a three-dimensional sample as introduced by Liebi et al. [Nature (2015), 527, 349-352], is described in more detail with regard to the mathematical framework and the optimization algorithm. For the case of trabecular bone samples from vertebrae it is shown that the model of the three-dimensional reciprocal-space map using spherical harmonics can adequately describe the measured data. The method enables the determination of nanostructure orientation and degree of orientation as demonstrated previously in a single momentum transfer q range. This article presents a reconstruction of the complete reciprocal-space map for the case of bone over extended ranges of q. In addition, it is shown that uniform angular sampling and advanced regularization strategies help to reduce the amount of data required.

  10. Pepsi-SAXS: an adaptive method for rapid and accurate computation of small-angle X-ray scattering profiles.

    PubMed

    Grudinin, Sergei; Garkavenko, Maria; Kazennov, Andrei

    2017-05-01

    A new method called Pepsi-SAXS is presented that calculates small-angle X-ray scattering profiles from atomistic models. The method is based on the multipole expansion scheme and is significantly faster compared with other tested methods. In particular, using the Nyquist-Shannon-Kotelnikov sampling theorem, the multipole expansion order is adapted to the size of the model and the resolution of the experimental data. It is argued that by using the adaptive expansion order, this method has the same quadratic dependence on the number of atoms in the model as the Debye-based approach, but with a much smaller prefactor in the computational complexity. The method has been systematically validated on a large set of over 50 models collected from the BioIsis and SASBDB databases. Using a laptop, it was demonstrated that Pepsi-SAXS is about seven, 29 and 36 times faster compared with CRYSOL, FoXS and the three-dimensional Zernike method in SAStbx, respectively, when tested on data from the BioIsis database, and is about five, 21 and 25 times faster compared with CRYSOL, FoXS and SAStbx, respectively, when tested on data from SASBDB. On average, Pepsi-SAXS demonstrates comparable accuracy in terms of χ 2 to CRYSOL and FoXS when tested on BioIsis and SASBDB profiles. Together with a small allowed variation of adjustable parameters, this demonstrates the effectiveness of the method. Pepsi-SAXS is available at http://team.inria.fr/nano-d/software/pepsi-saxs.

  11. X-ray scattering signatures of β-thalassemia

    NASA Astrophysics Data System (ADS)

    Desouky, Omar S.; Elshemey, Wael M.; Selim, Nabila S.

    2009-08-01

    X-ray scattering from lyophilized proteins or protein-rich samples is characterized by the presence of two characteristic broad peaks at scattering angles equivalent to momentum transfer values of 0.27 and 0.6 nm -1, respectively. These peaks arise from the interference of coherently scattered photons. Once the conformation of a protein is changed, these two peaks reflect such change with considerable sensitivity. The present work examines the possibility of characterizing the most common cause of hemolytic anaemia in Egypt and many Mediterranean countries; β-thalassemia, from its X-ray scattering profile. This disease emerges from a genetic defect causing reduced rate in the synthesis of one of the globin chains that make up hemoglobin. As a result, structurally abnormal hemoglobin molecules are formed. In order to detect such molecular disorder, hemoglobin samples of β-thalassemia patients are collected, lyophilized and measured using a conventional X-ray diffractometer. Results show significant differences in the X-ray scattering profiles of most of the diseased samples compared to control. The shape of the first scattering peak at 0.27 nm -1, in addition to the relative intensity of the first to the second scattering peaks, provides the most reliable signs of abnormality in diseased samples. The results are interpreted and confirmed with the aid of Fourier Transform Infrared (FTIR) spectroscopy of normal and thalassemia samples.

  12. Structure and dynamics of water in nonionic reverse micelles: a combined time-resolved infrared and small angle x-ray scattering study.

    PubMed

    van der Loop, Tibert H; Panman, Matthijs R; Lotze, Stephan; Zhang, Jing; Vad, Thomas; Bakker, Huib J; Sager, Wiebke F C; Woutersen, Sander

    2012-07-28

    We study the structure and reorientation dynamics of nanometer-sized water droplets inside nonionic reverse micelles (water/Igepal-CO-520/cyclohexane) with time-resolved mid-infrared pump-probe spectroscopy and small angle x-ray scattering. In the time-resolved experiments, we probe the vibrational and orientational dynamics of the O-D bonds of dilute HDO:H(2)O mixtures in Igepal reverse micelles as a function of temperature and micelle size. We find that even small micelles contain a large fraction of water that reorients at the same rate as water in the bulk, which indicates that the polyethylene oxide chains of the surfactant do not penetrate into the water volume. We also observe that the confinement affects the reorientation dynamics of only the first hydration layer. From the temperature dependent surface-water dynamics, we estimate an activation enthalpy for reorientation of 45 ± 9 kJ mol(-1) (11 ± 2 kcal mol(-1)), which is close to the activation energy of the reorientation of water molecules in ice.

  13. Characterization of the shape and line-edge roughness of polymer gratings with grazing incidence small-angle X-ray scattering and atomic force microscopy

    DOE PAGES

    Suh, Hyo Seon; Chen, Xuanxuan; Rincon-Delgadillo, Paulina A.; ...

    2016-04-22

    Grazing-incidence small-angle X-ray scattering (GISAXS) is increasingly used for the metrology of substrate-supported nanoscale features and nanostructured films. In the case of line gratings, where long objects are arranged with a nanoscale periodicity perpendicular to the beam, a series of characteristic spots of high-intensity (grating truncation rods, GTRs) are recorded on a two-dimensional detector. The intensity of the GTRs is modulated by the three-dimensional shape and arrangement of the lines. Previous studies aimed to extract an average cross-sectional profile of the gratings, attributing intensity loss at GTRs to sample imperfections. Such imperfections are just as important as the average shapemore » when employing soft polymer gratings which display significant line-edge roughness. Herein are reported a series of GISAXS measurements of polymer line gratings over a range of incident angles. Both an average shape and fluctuations contributing to the intensity in between the GTRs are extracted. Lastly, the results are critically compared with atomic force microscopy (AFM) measurements, and it is found that the two methods are in good agreement if appropriate corrections for scattering from the substrate (GISAXS) and contributions from the probe shape (AFM) are accounted for.« less

  14. Wide-angle X-ray scattering study of heat-treated PEEK and PEEK composite

    NASA Technical Reports Server (NTRS)

    Cebe, Peggy; Lowry, Lynn; Chung, Shirley Y.; Yavrouian, Andre; Gupta, Amitava

    1987-01-01

    Samples of poly(etheretherketone) (PEEK) neat resin and APC-2 carbon fiber composite were subjected to various heat treatments, and the effect of quenching and annealing treatments was studied by wide-angle X-ray scattering. It is found that high-temperature treatments may introduce disorder into neat resin and composite PEEK when followed by rapid cooling. The disorder is metastable and can revert to ordered state when the material is heated above its glass transition temperature and then cooled slowly. The disorder may result from residual thermal stresses.

  15. Mapping the structural order of laser-induced periodic surface structures in thin polymer films by microfocus beam grazing incidence small-angle X-ray scattering.

    PubMed

    Martín-Fabiani, Ignacio; Rebollar, Esther; García-Gutiérrez, Mari Cruz; Rueda, Daniel R; Castillejo, Marta; Ezquerra, Tiberio A

    2015-02-11

    In this work we present an accurate mapping of the structural order of laser-induced periodic surface structures (LIPSS) in spin-coated thin polymer films, via a microfocus beam grazing incidence small-angle X-ray scattering (μGISAXS) scan, GISAXS modeling, and atomic force microscopy imaging all along the scanned area. This combined study has allowed the evaluation of the effects on LIPSS formation due to nonhomogeneous spatial distribution of the laser pulse energy, mapping with micrometric resolution the evolution of the period and degree of structural order of LIPSS across the laser beam diameter in a direction perpendicular to the polarization vector. The experiments presented go one step further toward controlling nanostructure formation in LIPSS through a deep understanding of the parameters that influence this process.

  16. Assessment of surface roughness by use of soft x-ray scattering

    NASA Astrophysics Data System (ADS)

    Meng, Yan-li; Wang, Yong-gang; Chen, Shu-yan; Chen, Bo

    2009-08-01

    A soft x-ray reflectometer with laser produced plasma source has been designed, which can work from wavelength 8nm to 30 nm and has high performance. Using the soft x-ray reflectometer above, the scattering light distribution of silicon and zerodur mirrors which have super-smooth surfaces could be measured at different incidence angle and different wavelength. The measurement when the incidence angle is 2 degree and the wavelength is 11nm has been given in this paper. A surface scattering theory of soft x-ray grazing incidence optics based on linear system theory and an inverse scattering mathematical model is introduced. The vector scattering theory of soft x-ray scattering also is stated in detail. The scattering data are analyzed by both the methods above respectively to give information about the surface profiles. On the other hand, both the two samples are measured by WYKO surface profiler, and the surface roughness of the silicon and zerodur mirror is 1.3 nm and 1.5nm respectively. The calculated results are in quantitative agreement with those measured by WYKO surface profiler, which indicates that soft x-ray scattering is a very useful tool for the evaluation of highly polished surfaces. But there still some difference among the results of different theory and WYKO, and the possible reasons of such difference have been discussed in detail.

  17. Comprehension of direct extraction of hydrophilic antioxidants using vegetable oils by polar paradox theory and small angle X-ray scattering analysis.

    PubMed

    Li, Ying; Fabiano-Tixier, Anne Sylvie; Ruiz, Karine; Rossignol Castera, Anne; Bauduin, Pierre; Diat, Olivier; Chemat, Farid

    2015-04-15

    Since the polar paradox theory rationalised the fact that polar antioxidants are more effective in nonpolar media, extractions of phenolic compounds in vegetable oils were inspired and achieved in this study for obtaining oils enriched in phenolic compounds. Moreover, the influence of surfactants on the extractability of phenolic compounds was experimentally studied first, followed by the small angle X-ray scattering analysis for the oil structural observation before and after extraction so as to better understand the dissolving mechanism underpinning the extraction. The results showed a significant difference on the extraction yield of phenolic compounds among oils, which was mainly dependent on their composition instead of the unsaturation of fatty acids. Appropriate surfactant additions could significantly improve extraction yield for refined sunflower oils, which 1% w/w addition of glyceryl oleate was determined as the optimal. Besides, 5% w/w addition of lecithin performed the best in oil enrichments compared with mono- and di-glycerides. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Core–Shell Structure and Aggregation Number of Micelles Composed of Amphiphilic Block Copolymers and Amphiphilic Heterografted Polymer Brushes Determined by Small-Angle X-ray Scattering

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

    Szymusiak, Magdalena; Kalkowski, Joseph; Luo, Hanying

    2017-08-31

    A large group of functional nanomaterials employed in biomedical applications, including targeted drug delivery, relies on amphiphilic polymers to encapsulate therapeutic payloads via self-assembly processes. Knowledge of the micelle structures will provide critical insights into design of polymeric drug delivery systems. Core–shell micelles composed of linear diblock copolymers poly(ethylene glycol)-b-poly(caprolactone) (PEG-b-PCL), poly(ethylene oxide)-b-poly(lactic acid) (PEG-b-PLA), as well as a heterografted brush consisting of a poly(glycidyl methacrylate) backbone with PEG and PLA branches (PGMA-g-PEG/PLA) were characterized by dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS) measurements to gain structural information regarding the particle morphology, core–shell size, and aggregation number. Themore » structural information at this quasi-equilibrium state can also be used as a reference when studying the kinetics of polymer micellization.« less

  19. Core–Shell Structure and Aggregation Number of Micelles Composed of Amphiphilic Block Copolymers and Amphiphilic Heterografted Polymer Brushes Determined by Small-Angle X-ray Scattering

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

    Szymusiak, Magdalena; Kalkowski, Joseph; Luo, Hanying

    2017-08-16

    A large group of functional nanomaterials employed in biomedical applications, including targeted drug delivery, relies on amphiphilic polymers to encapsulate therapeutic payloads via self-assembly processes. Knowledge of the micelle structures will provide critical insights into design of polymeric drug delivery systems. Core–shell micelles composed of linear diblock copolymers poly(ethylene glycol)-b-poly(caprolactone) (PEG-b-PCL), poly(ethylene oxide)-b-poly(lactic acid) (PEG-b-PLA), as well as a heterografted brush consisting of a poly(glycidyl methacrylate) backbone with PEG and PLA branches (PGMA-g-PEG/PLA) were characterized by dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS) measurements to gain structural information regarding the particle morphology, core–shell size, and aggregation number. Themore » structural information at this quasi-equilibrium state can also be used as a reference when studying the kinetics of polymer micellization.« less

  20. Structure of Dimeric and Tetrameric Complexes of the BAR Domain Protein PICK1 Determined by Small-Angle X-Ray Scattering.

    PubMed

    Karlsen, Morten L; Thorsen, Thor S; Johner, Niklaus; Ammendrup-Johnsen, Ina; Erlendsson, Simon; Tian, Xinsheng; Simonsen, Jens B; Høiberg-Nielsen, Rasmus; Christensen, Nikolaj M; Khelashvili, George; Streicher, Werner; Teilum, Kaare; Vestergaard, Bente; Weinstein, Harel; Gether, Ulrik; Arleth, Lise; Madsen, Kenneth L

    2015-07-07

    PICK1 is a neuronal scaffolding protein containing a PDZ domain and an auto-inhibited BAR domain. BAR domains are membrane-sculpting protein modules generating membrane curvature and promoting membrane fission. Previous data suggest that BAR domains are organized in lattice-like arrangements when stabilizing membranes but little is known about structural organization of BAR domains in solution. Through a small-angle X-ray scattering (SAXS) analysis, we determine the structure of dimeric and tetrameric complexes of PICK1 in solution. SAXS and biochemical data reveal a strong propensity of PICK1 to form higher-order structures, and SAXS analysis suggests an offset, parallel mode of BAR-BAR oligomerization. Furthermore, unlike accessory domains in other BAR domain proteins, the positioning of the PDZ domains is flexible, enabling PICK1 to perform long-range, dynamic scaffolding of membrane-associated proteins. Together with functional data, these structural findings are compatible with a model in which oligomerization governs auto-inhibition of BAR domain function. Copyright © 2015 Elsevier Ltd. All rights reserved.

  1. Extracting magnetic cluster size and its distributions in advanced perpendicular recording media with shrinking grain size using small angle x-ray scattering

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

    Mehta, Virat; Ikeda, Yoshihiro; Takano, Ken

    2015-05-18

    We analyze the magnetic cluster size (MCS) and magnetic cluster size distribution (MCSD) in a variety of perpendicular magnetic recording (PMR) media designs using resonant small angle x-ray scattering at the Co L{sub 3} absorption edge. The different PMR media flavors considered here vary in grain size between 7.5 and 9.5 nm as well as in lateral inter-granular exchange strength, which is controlled via the segregant amount. While for high inter-granular exchange, the MCS increases rapidly for grain sizes below 8.5 nm, we show that for increased amount of segregant with less exchange the MCS remains relatively small, even for grain sizesmore » of 7.5 and 8 nm. However, the MCSD still increases sharply when shrinking grains from 8 to 7.5 nm. We show evidence that recording performance such as signal-to-noise-ratio on the spin stand correlates well with the product of magnetic cluster size and magnetic cluster size distribution.« less

  2. Measuring helium nano-bubble formation in tungsten with grazing-incidence small angle X-ray scattering

    NASA Astrophysics Data System (ADS)

    Thompson, Matt A. T.

    The behaviour of helium in tungsten is an important concern for the fusion materials community. Under helium plasma exposure, small nano-scale bubbles form beneath the material surface as helium precipitates from the tungsten matrix. Under certain conditions this can lead to the subsequent formation of a surface "nano-fuzz", though the mechanisms of this process are not presently understood. For sub-surface nano-bubble formation transmission electron microscopy (TEM) has been the most widely used technique. While certainly a powerful technique, TEM suffers from a number of significant drawbacks: sample preparation is difficult and destructive, and there are sampling limitations as nano-structures must be located and characterised individually. This makes quantitative characterisation of nano-scale modification in tungsten challenging, which in turn makes it difficult to perform systematic studies on the effects of factors such as temperature and plasma composition on nano-scale modification. Here, Grazing Incidence Small Angle X-ray Scattering (GISAXS) is presented as a powerful addition to the field of fusion materials. With GISAXS, one can measure the X-ray scattering from nano-scale features throughout a relatively large volume, allowing information about full nano-bubble size distributions to be obtained from a simple, non-destructive measurement. Where it typically takes days or weeks to prepare a sample and study it under TEM, GISAXS measurements can be performed in a matter of minutes, and the data analysis performed autonomously by a computer in hours. This thesis describes the work establishing GISAXS as a viable technique for fusion materials. A GISAXS pattern fitting model was first developed, and then validated via comparison between GISAXS and TEM measurements of helium induced nano-bubble formation in tungsten exposed to a helium discharge in the large helical device. Under these conditions, nano-bubbles were found to follow an approximately

  3. Review of the fundamental theories behind small angle X-ray scattering, molecular dynamics simulations, and relevant integrated application

    PubMed Central

    Boldon, Lauren; Laliberte, Fallon; Liu, Li

    2015-01-01

    In this paper, the fundamental concepts and equations necessary for performing small angle X-ray scattering (SAXS) experiments, molecular dynamics (MD) simulations, and MD-SAXS analyses were reviewed. Furthermore, several key biological and non-biological applications for SAXS, MD, and MD-SAXS are presented in this review; however, this article does not cover all possible applications. SAXS is an experimental technique used for the analysis of a wide variety of biological and non-biological structures. SAXS utilizes spherical averaging to produce one- or two-dimensional intensity profiles, from which structural data may be extracted. MD simulation is a computer simulation technique that is used to model complex biological and non-biological systems at the atomic level. MD simulations apply classical Newtonian mechanics’ equations of motion to perform force calculations and to predict the theoretical physical properties of the system. This review presents several applications that highlight the ability of both SAXS and MD to study protein folding and function in addition to non-biological applications, such as the study of mechanical, electrical, and structural properties of non-biological nanoparticles. Lastly, the potential benefits of combining SAXS and MD simulations for the study of both biological and non-biological systems are demonstrated through the presentation of several examples that combine the two techniques. PMID:25721341

  4. Review of the fundamental theories behind small angle X-ray scattering, molecular dynamics simulations, and relevant integrated application.

    PubMed

    Boldon, Lauren; Laliberte, Fallon; Liu, Li

    2015-01-01

    In this paper, the fundamental concepts and equations necessary for performing small angle X-ray scattering (SAXS) experiments, molecular dynamics (MD) simulations, and MD-SAXS analyses were reviewed. Furthermore, several key biological and non-biological applications for SAXS, MD, and MD-SAXS are presented in this review; however, this article does not cover all possible applications. SAXS is an experimental technique used for the analysis of a wide variety of biological and non-biological structures. SAXS utilizes spherical averaging to produce one- or two-dimensional intensity profiles, from which structural data may be extracted. MD simulation is a computer simulation technique that is used to model complex biological and non-biological systems at the atomic level. MD simulations apply classical Newtonian mechanics' equations of motion to perform force calculations and to predict the theoretical physical properties of the system. This review presents several applications that highlight the ability of both SAXS and MD to study protein folding and function in addition to non-biological applications, such as the study of mechanical, electrical, and structural properties of non-biological nanoparticles. Lastly, the potential benefits of combining SAXS and MD simulations for the study of both biological and non-biological systems are demonstrated through the presentation of several examples that combine the two techniques.

  5. β-connectin studies by small-angle x-ray scattering and single-molecule force spectroscopy by atomic force microscopy

    NASA Astrophysics Data System (ADS)

    Marchetti, S.; Sbrana, F.; Toscano, A.; Fratini, E.; Carlà, M.; Vassalli, M.; Tiribilli, B.; Pacini, A.; Gambi, C. M. C.

    2011-05-01

    The three-dimensional structure and the mechanical properties of a β-connectin fragment from human cardiac muscle, belonging to the I band, from I27 to I34, were investigated by small-angle x-ray scattering (SAXS) and single-molecule force spectroscopy (SMFS). This molecule presents an entropic elasticity behavior, associated to globular domain unfolding, that has been widely studied in the last 10 years. In addition, atomic force microscopy based SMFS experiments suggest that this molecule has an additional elastic regime, for low forces, probably associated to tertiary structure remodeling. From a structural point of view, this behavior is a mark of the fact that the eight domains in the I27-I34 fragment are not independent and they organize in solution, assuming a well-defined three-dimensional structure. This hypothesis has been confirmed by SAXS scattering, both on a diluted and a concentrated sample. Two different models were used to fit the SAXS curves: one assuming a globular shape and one corresponding to an elongated conformation, both coupled with a Coulomb repulsion potential to take into account the protein-protein interaction. Due to the predominance of the structure factor, the effective shape of the protein in solution could not be clearly disclosed. By performing SMFS by atomic force microscopy, mechanical unfolding properties were investigated. Typical sawtooth profiles were obtained and the rupture force of each unfolding domain was estimated. By fitting a wormlike chain model to each peak of the sawtooth profile, the entropic elasticity of octamer was described.

  6. The Importance of Protein-Protein Interactions on the pH-Induced Conformational Changes of Bovine Serum Albumin: A Small-Angle X-Ray Scattering Study

    PubMed Central

    Barbosa, Leandro R.S.; Ortore, Maria Grazia; Spinozzi, Francesco; Mariani, Paolo; Bernstorff, Sigrid; Itri, Rosangela

    2010-01-01

    Abstract The combined effects of concentration and pH on the conformational states of bovine serum albumin (BSA) are investigated by small-angle x-ray scattering. Serum albumins, at physiological conditions, are found at concentrations of ∼35–45 mg/mL (42 mg/mL in the case of humans). In this work, BSA at three different concentrations (10, 25, and 50 mg/mL) and pH values (2.0–9.0) have been studied. Data were analyzed by means of the Global Fitting procedure, with the protein form factor calculated from human serum albumin (HSA) crystallographic structure and the interference function described, considering repulsive and attractive interaction potentials within a random phase approximation. Small-angle x-ray scattering data show that BSA maintains its native state from pH 4.0 up to 9.0 at all investigated concentrations. A pH-dependence of the absolute net protein charge is shown and the charge number per BSA is quantified to 10(2), 8(1), 13(2), 20(2), and 26(2) for pH values 4.0, 5.4, 7.0, 8.0, and 9.0, respectively. The attractive potential diminishes as BSA concentration increases. The coexistence of monomers and dimers is observed at 50 mg/mL and pH 5.4, near the BSA isoelectric point. Samples at pH 2.0 show a different behavior, because BSA overall shape changes as a function of concentration. At 10 mg/mL, BSA is partially unfolded and a strong repulsive protein-protein interaction occurs due to the high amount of exposed charge. At 25 and 50 mg/mL, BSA undergoes some re-folding, which likely results in a molten-globule state. This work concludes by confirming that the protein concentration plays an important role on the pH-unfolded BSA state, due to a delicate compromise between interaction forces and crowding effects. PMID:20085727

  7. Conformational variability of the stationary phase survival protein E from Xylella fastidiosa revealed by X-ray crystallography, small-angle X-ray scattering studies, and normal mode analysis.

    PubMed

    Machado, Agnes Thiane Pereira; Fonseca, Emanuella Maria Barreto; Reis, Marcelo Augusto Dos; Saraiva, Antonio Marcos; Santos, Clelton Aparecido Dos; de Toledo, Marcelo Augusto Szymanski; Polikarpov, Igor; de Souza, Anete Pereira; Aparicio, Ricardo; Iulek, Jorge

    2017-10-01

    Xylella fastidiosa is a xylem-limited bacterium that infects a wide variety of plants. Stationary phase survival protein E is classified as a nucleotidase, which is expressed when bacterial cells are in the stationary growth phase and subjected to environmental stresses. Here, we report four refined X-ray structures of this protein from X. fastidiosa in four different crystal forms in the presence and/or absence of the substrate 3'-AMP. In all chains, the conserved loop verified in family members assumes a closed conformation in either condition. Therefore, the enzymatic mechanism for the target protein might be different of its homologs. Two crystal forms exhibit two monomers whereas the other two show four monomers in the asymmetric unit. While the biological unit has been characterized as a tetramer, differences of their sizes and symmetry are remarkable. Four conformers identified by Small-Angle X-ray Scattering (SAXS) in a ligand-free solution are related to the low frequency normal modes of the crystallographic structures associated with rigid body-like protomer arrangements responsible for the longitudinal and symmetric adjustments between tetramers. When the substrate is present in solution, only two conformers are selected. The most prominent conformer for each case is associated to a normal mode able to elongate the protein by moving apart two dimers. To our knowledge, this work was the first investigation based on the normal modes that analyzed the quaternary structure variability for an enzyme of the SurE family followed by crystallography and SAXS validation. The combined results raise new directions to study allosteric features of XfSurE protein. © 2017 Wiley Periodicals, Inc.

  8. Solution Structures of 2 : 1 And 1 : 1 DNA Polymerase - DNA Complexes Probed By Ultracentrifugation And Small-Angle X-Ray Scattering

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

    Tang, K.H.; /Ohio State U.; Niebuhr, M.

    2009-04-30

    We report small-angle X-ray scattering (SAXS) and sedimentation velocity (SV) studies on the enzyme-DNA complexes of rat DNA polymerase {beta} (Pol {beta}) and African swine fever virus DNA polymerase X (ASFV Pol X) with one-nucleotide gapped DNA. The results indicated formation of a 2 : 1 Pol {beta}-DNA complex, whereas only 1 : 1 Pol X-DNA complex was observed. Three-dimensional structural models for the 2 : 1 Pol {beta}-DNA and 1 : 1 Pol X-DNA complexes were generated from the SAXS experimental data to correlate with the functions of the DNA polymerases. The former indicates interactions of the 8 kDamore » 5{prime}-dRP lyase domain of the second Pol {beta} molecule with the active site of the 1 : 1 Pol {beta}-DNA complex, while the latter demonstrates how ASFV Pol X binds DNA in the absence of DNA-binding motif(s). As ASFV Pol X has no 5{prime}-dRP lyase domain, it is reasonable not to form a 2 : 1 complex. Based on the enhanced activities of the 2 : 1 complex and the observation that the 8 kDa domain is not in an optimal configuration for the 5{prime}-dRP lyase reaction in the crystal structures of the closed ternary enzyme-DNA-dNTP complexes, we propose that the asymmetric 2 : 1 Pol {beta}-DNA complex enhances the function of Pol {beta}.« less

  9. Advancing X-ray scattering metrology using inverse genetic algorithms.

    PubMed

    Hannon, Adam F; Sunday, Daniel F; Windover, Donald; Kline, R Joseph

    2016-01-01

    We compare the speed and effectiveness of two genetic optimization algorithms to the results of statistical sampling via a Markov chain Monte Carlo algorithm to find which is the most robust method for determining real space structure in periodic gratings measured using critical dimension small angle X-ray scattering. Both a covariance matrix adaptation evolutionary strategy and differential evolution algorithm are implemented and compared using various objective functions. The algorithms and objective functions are used to minimize differences between diffraction simulations and measured diffraction data. These simulations are parameterized with an electron density model known to roughly correspond to the real space structure of our nanogratings. The study shows that for X-ray scattering data, the covariance matrix adaptation coupled with a mean-absolute error log objective function is the most efficient combination of algorithm and goodness of fit criterion for finding structures with little foreknowledge about the underlying fine scale structure features of the nanograting.

  10. Small Angle X-Ray Scattering Study of Meso-Tetrakis (4-Sulfonatophenyl) Porphyrin in Aqueous Solution: A Self-Aggregation Model

    PubMed Central

    Gandini, S.C.M.; Gelamo, E.L.; Itri, R.; Tabak, M.

    2003-01-01

    The aggregate morphology of meso-tetrakis(4-sulfonatophenyl) porphyrin (TPPS4) in aqueous solution is investigated by using small angle x-ray scattering (SAXS) technique. Measurements were performed at pH 4.0 and 9.0 to monitor the pH influence on the structural parameters of the aggregates. Radii of gyration were obtained from distance distribution functions p(r) analysis. The experimental data of TPPS4 at pH 4.0 showed well-defined oscillations characteristic of large aggregates in contrast to the SAXS curve of 5 mM TPPS4 at pH 9.0, where both a significant decrease in the intensity and the disappearance of the oscillation peaks suggest the dissociation of the aggregate. A 340-Å long “hollow” cylinder with shell thickness of 20 Å, compatible to the porphyrin molecule dimension, represents well the scattering curve of the aggregates at pH 4.0. According to the fitting parameters, 26 porphyrin molecules self-associate into a ringlike configuration in the plane of the cylinder cross-section. The total number of porphyrin molecules in the whole aggregate was also estimated as ∼3000. The model compatible to SAXS data of a hollow cylinder with J-aggregation in the cross-section and H-aggregation (columnar stacking) between the cylinder layers is consistent with optical absorption spectroscopic data both in the literature and obtained in this work. PMID:12885669

  11. Structure factor of blends of solvent-free nanoparticle-organic hybrid materials: density-functional theory and small angle X-ray scattering.

    PubMed

    Yu, Hsiu-Yu; Srivastava, Samanvaya; Archer, Lynden A; Koch, Donald L

    2014-12-07

    We investigate the static structure factor S(q) of solvent-free nanoparticle-organic hybrid materials consisting of silica nanocores and space-filling polyethylene glycol coronas using a density-functional theory and small angle X-ray scattering measurements. The theory considers a bidisperse suspension of hard spheres with different radii and tethered bead-spring oligomers with different grafting densities to approximate the polydispersity effects in experiments. The experimental systems studied include pure samples with different silica core volume fractions and the associated mean corona grafting densities, and blends with different mixing ratios of the pure samples, in order to introduce varying polydispersity of corona grafting density. Our scattering experiments and theory show that, compared to the hard-sphere suspension with the same core volume fraction, S(q) for pure samples exhibit both substantially smaller values at small q and stronger particle correlations corresponding to a larger effective hard core at large q, indicating that the tethered incompressible oligomers enforce a more uniform particle distribution, and the densely grafted brush gives rise to an additional exclusionary effect between the nanoparticles. According to the theory, polydispersity in the oligomer grafting density controls the deviation of S(q) from the monodisperse system at smaller q, and the interplay of the enhanced effective core size and the entropic attraction among the particles is responsible for complex variations in the particle correlations at larger q. The successful comparison between the predictions and the measurements for the blends further suggests that S(q) can be used to assess the uniformity of grafting density in polymer-grafted nanoparticle materials.

  12. Small-Angle Scatter Measurement.

    NASA Astrophysics Data System (ADS)

    Wein, Steven Jay

    The design, analysis, and performance of a small -angle scatterometer are presented. The effects of the diffraction background, geometrical aberrations and system scatter at the small-angles are separated. Graphs are provided that quantify their contribution. The far-field irradiance distributions of weakly truncated and untruncated Gaussian beams are compared. The envelope of diffraction ringing is shown to decrease proportionately with the level of truncation in the pupil. Spherical aberration and defocus are shown to have little effect on the higher-order diffraction rings of Gaussian apertures and as such will have a negligible effect on most scatter measurements. A method is presented for determining the scattered irradiance level for a given BRDF in relation to the peak irradiance of the point spread function. A method of Gaussian apodization is presented and tested that allows the level of diffraction ringing to become a design parameter. Upon sufficient reduction of the diffraction background, the scattered light from the scatterometers' primary mirror is seen to be the limiting component of the small-angle instrument profile. The scatterometer described was able to make a meaningful measurement close enough to the specular direction at 0.6328mum in order to observe the characteristic height and width of the scatter function. This allowed the rms roughness and autocorrelation length of the surface to be determined from the scatter data at this wavelength. The inferred rms roughness agreed well with an independent optical profilometer measurement of the surface. The BRDF of the samples were also measured at 10.6mum. The rms roughness inferred from this scatter data did not agree with the other measurements. The BRDF did not scale in accordance with the scaler diffraction theory of microrough surfaces. The scattering in the visible was dominated by the effects of surface roughness whereas the scattering in the far-infrared was apparently dominated by the

  13. Multiple image x-radiography for functional lung imaging

    NASA Astrophysics Data System (ADS)

    Aulakh, G. K.; Mann, A.; Belev, G.; Wiebe, S.; Kuebler, W. M.; Singh, B.; Chapman, D.

    2018-01-01

    Detection and visualization of lung tissue structures is impaired by predominance of air. However, by using synchrotron x-rays, refraction of x-rays at the interface of tissue and air can be utilized to generate contrast which may in turn enable quantification of lung optical properties. We utilized multiple image radiography, a variant of diffraction enhanced imaging, at the Canadian light source to quantify changes in unique x-ray optical properties of lungs, namely attenuation, refraction and ultra small-angle scatter (USAXS or width) contrast ratios as a function of lung orientation in free-breathing or respiratory-gated mice before and after intra-nasal bacterial endotoxin (lipopolysaccharide) instillation. The lung ultra small-angle scatter and attenuation contrast ratios were significantly higher 9 h post lipopolysaccharide instillation compared to saline treatment whereas the refraction contrast decreased in magnitude. In ventilated mice, end-expiratory pressures result in an increase in ultra small-angle scatter contrast ratio when compared to end-inspiratory pressures. There were no detectable changes in lung attenuation or refraction contrast ratio with change in lung pressure alone. In effect, multiple image radiography can be applied towards following optical properties of lung air-tissue barrier over time during pathologies such as acute lung injury.

  14. X-ray Photoelectron Spectroscopy (XPS), Rutherford Back Scattering (RBS) studies

    NASA Technical Reports Server (NTRS)

    Neely, W. C.; Bozak, M. J.; Williams, J. R.

    1993-01-01

    X-ray photoelectron spectroscopy (XPS), Rutherford Back Scattering (RBS) studies of each of sample received were completed. Since low angle X-ray could not be performed because of instrumentation problems, Auger spectrometry was employed instead. The results of these measurements for each of the samples is discussed in turn.

  15. Scatter of X-rays on polished surfaces

    NASA Technical Reports Server (NTRS)

    Hasinger, G.

    1981-01-01

    In investigating the dispersion properties of telescope mirrors used in X-ray astronomy, the slight scattering characteristics of X-ray radiation by statistically rough surfaces were examined. The mathematics and geometry of scattering theory are described. The measurement test assembly is described and results of measurements on samples of plane mirrors are given. Measurement results are evaluated. The direct beam, the convolution of the direct beam and the scattering halo, curve fitting by the method of least squares, various autocorrelation functions, results of the fitting procedure for small scattering, and deviations in the kernel of the scattering distribution are presented. A procedure for quality testing of mirror systems through diagnosis of rough surfaces is described.

  16. Coherent amplification of X-ray scattering from meso-structures

    DOE PAGES

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

    2017-07-10

    Small-angle X-ray scattering (SAXS) often includes an unwanted background, which increases the required measurement time to resolve the sample structure. This is undesirable in all experiments, and may make measurement of dynamic or radiation-sensitive samples impossible. Here, we demonstrate a new technique, applicable when the scattering signal is background-dominated, which reduces the requisite exposure time. Our method consists of exploiting coherent interference between a sample with a designed strongly scattering `amplifier'. A modified angular correlation function is used to extract the symmetry of the interference term; that is, the scattering arising from the interference between the amplifier and the sample.more » This enables reconstruction of the sample's symmetry, despite the sample scattering itself being well below the intensity of background scattering. Thus, coherent amplification is used to generate a strong scattering term (well above background), from which sample scattering is inferred. We validate this method using lithographically defined test samples.« less

  17. Determination of line profiles on nano-structured surfaces using EUV and x-ray scattering

    NASA Astrophysics Data System (ADS)

    Soltwisch, Victor; Wernecke, Jan; Haase, Anton; Probst, Jürgen; Schoengen, Max; Krumrey, Michael; Scholze, Frank; Pomplun, Jan; Burger, Sven

    2014-09-01

    Non-imaging techniques like X-ray scattering are supposed to play an important role in the further development of CD metrology for the semiconductor industry. Grazing Incidence Small Angle X-ray Scattering (GISAXS) provides directly assessable information on structure roughness and long-range periodic perturbations. The disadvantage of the method is the large footprint of the X-ray beam on the sample due to the extremely shallow angle of incidence. This can be overcome by using wavelengths in the extreme ultraviolet (EUV) spectral range, EUV small angle scattering (EUVSAS), which allows for much steeper angles of incidence but preserves the range of momentum transfer that can be observed. Generally, the potentially higher momentum transfer at shorter wavelengths is counterbalanced by decreasing diffraction efficiency. This results in a practical limit of about 10 nm pitch for which it is possible to observe at least the +/- 1st diffraction orders with reasonable efficiency. At the Physikalisch-Technische Bundesanstalt (PTB), the available photon energy range extends from 50 eV up to 10 keV at two adjacent beamlines. PTB commissioned a new versatile Ellipso-Scatterometer which is capable of measuring 6" square substrates in a clean, hydrocarbon-free environment with full flexibility regarding the direction of the incident light polarization. The reconstruction of line profiles using a geometrical model with six free parameters, based on a finite element method (FEM) Maxwell solver and a particle swarm based least-squares optimization yielded consistent results for EUV-SAS and GISAXS. In this contribution we present scatterometry data for line gratings and consistent reconstruction results of the line geometry for EUV-SAS and GISAXS.

  18. Energy-angle correlation correction algorithm for monochromatic computed tomography based on Thomson scattering X-ray source

    NASA Astrophysics Data System (ADS)

    Chi, Zhijun; Du, Yingchao; Huang, Wenhui; Tang, Chuanxiang

    2017-12-01

    The necessity for compact and relatively low cost x-ray sources with monochromaticity, continuous tunability of x-ray energy, high spatial coherence, straightforward polarization control, and high brightness has led to the rapid development of Thomson scattering x-ray sources. To meet the requirement of in-situ monochromatic computed tomography (CT) for large-scale and/or high-attenuation materials based on this type of x-ray source, there is an increasing demand for effective algorithms to correct the energy-angle correlation. In this paper, we take advantage of the parametrization of the x-ray attenuation coefficient to resolve this problem. The linear attenuation coefficient of a material can be decomposed into a linear combination of the energy-dependent photoelectric and Compton cross-sections in the keV energy regime without K-edge discontinuities, and the line integrals of the decomposition coefficients of the above two parts can be determined by performing two spectrally different measurements. After that, the line integral of the linear attenuation coefficient of an imaging object at a certain interested energy can be derived through the above parametrization formula, and monochromatic CT can be reconstructed at this energy using traditional reconstruction methods, e.g., filtered back projection or algebraic reconstruction technique. Not only can monochromatic CT be realized, but also the distributions of the effective atomic number and electron density of the imaging object can be retrieved at the expense of dual-energy CT scan. Simulation results validate our proposal and will be shown in this paper. Our results will further expand the scope of application for Thomson scattering x-ray sources.

  19. Unraveling skyrmion spin texture using resonant soft x-ray scattering

    NASA Astrophysics Data System (ADS)

    Roy, Sujoy

    2015-03-01

    The recent discovery of skyrmions, that were originally predicted in context of high energy physics, in magnetic materials has sparked tremendous interest in the research community due to its rich physics and potential in spintronics applications. Skyrmions have an unusual spin texture that manifests as magnetic knot and can be easily moved around. Understanding the fundamental physics and mechanisms for controlling their dynamical properties presents important scientific challenges. So far experimental verifications of the skyrmions in magnetic systems have come from neutron scattering and Lorentz transmission electron microscopy (TEM) measurements. In this talk we report the first observation of the skyrmions using resonant soft x-ray scattering. We have used soft x-rays tuned to the Cu L3 edge to diffract off the skyrmion lattice in a multiferroic Cu2OSeO3 compound. We show that in Cu2OSeO3 there exist two skyrmion lattices arising due to the two inequivalent Cu-O sublattices that have two different magnetically active d-orbitals. The two skyrmion sublattices are mutually rotated with respect to each other. The angle of rotation could be changed by an external magnetic field, thereby indicating possible existence of a new phase. We have also studied skyrmion spin texture in an ultra-thin Fe/Gd multilayer that shows perpendicular anisotropy. The Fe/Gd sample exhibits a near perfect aligned stripe phase. Within a small range of temperature and magnetic field we observe a hexagonal scattering pattern due to skyrmion bubbles. Analysis of the scattering pattern suggests that the skyrmion lattice unit cell contains two skyrmions. The biskyrmion state is also revealed by Lorentz TEM images. The near room temperature discovery of skyrmion in a technology relevant material is a significant step towards using skyrmions in magnetic devices. Work at LBNL was supported by the Office of Basic Energy Sciences of the U.S. Department of Energy (Contract No. DE-AC02-05CH11231).

  20. Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

    PubMed Central

    Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole

    2016-01-01

    The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles. PMID:26917133

  1. Effects of macromolecular crowding on the structure of a protein complex: A small-angle scattering study of superoxide dismutase

    DOE PAGES

    Rajapaksha, Ajith; Stanley, Christopher B.; Todd, Brian A.

    2015-02-17

    Macromolecular crowding can alter the structure and function of biological macromolecules. We used small angle scattering (SAS) to measure the change in size of a protein complex, superoxide dismutase (SOD), induced by macromolecular crowding. Crowding was induced using 400 MW polyethylene glycol (PEG), triethylene glycol (TEG), methyl- -glucoside ( -MG) and trimethylamine N-oxide (TMAO). Parallel small angle neutron scattering (SANS) and small angle x-ray scattering (SAXS) allowed us to unambiguously attribute apparent changes in radius of gyration to changes in the structure of SOD. For a 40% PEG solution, we find that the volume of SOD was reduced by 9%.more » Considering the osmotic pressure due to PEG, this deformation corresponds to a highly compressible structure. SAXS done in the presence of TEG suggests that for further deformation beyond a 9% decrease in volume the resistance to deformation may increase dramatically.« less

  2. Using small angle x-ray scattering to measure the homogeneous nucleation rates of n-propanol, n-butanol, and n-pentanol in supersonic nozzle expansions

    NASA Astrophysics Data System (ADS)

    Ghosh, David; Manka, Alexandra; Strey, Reinhard; Seifert, Soenke; Winans, Randall E.; Wyslouzil, Barbara E.

    2008-09-01

    In our earlier publication [M. Gharibeh et al., J. Chem. Phys. 122, 094512 (2005)] we determined the temperatures and partial pressures corresponding to the maximum nucleation rate for a series n-alcohols (CiH2i+lOH; i =3-5) during condensation in a supersonic nozzle. Although we were able to determine the characteristic time ΔtJmax corresponding to the peak nucleation rate, we were unable to measure the number density of the aerosol and, thus, unable to directly quantify the nucleation rate J. In this paper we report the results of our pioneering small angle x-ray scattering (SAXS) experiments of n-alcohol droplets formed in a supersonic nozzle together with a new series of complementary pressure trace measurements. By combining the SAXS and pressure trace measurement data we determine the nucleation rates as a function of temperature and supersaturation.

  3. 2011 U.S. National School on Neutron and X-ray Scattering

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

    Lang, Jonathan; te Vethuis, Suzanne; Ekkebus, Allen E

    The 13th annual U.S. National School on Neutron and X-ray Scattering was held June 11 to 25, 2011, at both Oak Ridge and Argonne National Laboratories. This school brought together 65 early career graduate students from 56 different universities in the US and provided them with a broad introduction to the techniques available at the major large-scale neutron and synchrotron x-ray facilities. This school is focused primarily on techniques relevant to the physical sciences, but also touches on cross-disciplinary bio-related scattering measurements. During the school, students received lectures by over 30 researchers from academia, industry, and national laboratories and participatedmore » in a number of short demonstration experiments at Argonne's Advanced Photon Source (APS) and Oak Ridge's Spallation neutron Source (SNS) and High Flux Isotope Reactor (HFIR) facilities to get hands-on experience in using neutron and synchrotron sources. The first week of this year's school was held at Oak Ridge National Lab, where Lab director Thom Mason welcomed the students and provided a shitorical perspective of the neutron and x-ray facilities both at Oak Ridge and Argonne. The first few days of the school were dedicated to lectures laying out the basics of scattering theory and the differences and complementarity between the neutron and x-ray probes given by Sunil Sinha. Jack Carpenter provided an introduction into how neutrons are generated and detected. After this basic introduction, the students received lectures each morning on specific techniques and conducted demonstration experiments each afternoon on one of 15 different instruments at either the SNS or HFIR. Some of the topics covered during this week of the school included inelastic neutron scattering by Bruce Gaulin, x-ray and neutron reflectivity by Chuck Majkrazak, small-angle scattering by Volker Urban, powder diffraction by Ashfia Huq and diffuse scattering by Gene Ice.« less

  4. Quaternary arrangement of an active, native group II intron ribonucleoprotein complex revealed by small-angle X-ray scattering.

    PubMed

    Gupta, Kushol; Contreras, Lydia M; Smith, Dorie; Qu, Guosheng; Huang, Tao; Spruce, Lynn A; Seeholzer, Steven H; Belfort, Marlene; Van Duyne, Gregory D

    2014-04-01

    The stable ribonucleoprotein (RNP) complex formed between the Lactococcus lactis group II intron and its self-encoded LtrA protein is essential for the intron's genetic mobility. In this study, we report the biochemical, compositional, hydrodynamic and structural properties of active group II intron RNP particles (+A) isolated from its native host using a novel purification scheme. We employed small-angle X-ray scattering to determine the structural properties of these particles as they exist in solution. Using sucrose as a contrasting agent, we derived a two-phase quaternary model of the protein-RNA complex. This approach revealed that the spatial properties of the complex are largely defined by the RNA component, with the protein dimer located near the center of mass. A transfer RNA fusion engineered into domain II of the intron provided a distinct landmark consistent with this interpretation. Comparison of the derived +A RNP shape with that of the previously reported precursor intron (ΔA) particle extends previous findings that the loosely packed precursor RNP undergoes a dramatic conformational change as it compacts into its active form. Our results provide insights into the quaternary arrangement of these RNP complexes in solution, an important step to understanding the transition of the group II intron from the precursor to a species fully active for DNA invasion.

  5. Estimation of degree of polymerization of poly-acrylonitrile-grafted carbon nanotubes using Guinier plot of small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Cho, Hyunjung; Jin, Kyeong Sik; Lee, Jaegeun; Lee, Kun-Hong

    2018-07-01

    Small angle x-ray scattering (SAXS) was used to estimate the degree of polymerization of polymer-grafted carbon nanotubes (CNTs) synthesized using a ‘grafting from’ method. This analysis characterizes the grafted polymer chains without cleaving them from CNTs, and provides reliable data that can complement conventional methods such as thermogravimetric analysis or transmittance electron microscopy. Acrylonitrile was polymerized from the surface of the CNTs by using redox initiation to produce poly-acrylonitrile-grafted CNTs (PAN-CNTs). Polymerization time and the initiation rate were varied to control the degree of polymerization. Radius of gyration (R g ) of PAN-CNTs was determined using the Guinier plot obtained from SAXS solution analysis. The results showed consistent values according to the polymerization condition, up to a maximum R g = 125.70 Å whereas that of pristine CNTs was 99.23 Å. The dispersibility of PAN-CNTs in N,N-dimethylformamide was tested using ultraviolet–visible-near infrared spectroscopy and was confirmed to increase as the degree of polymerization increased. This analysis will be helpful to estimate the degree of polymerization of any polymer-grafted CNTs synthesized using the ‘grafting from’ method and to fabricate polymer/CNT composite materials.

  6. Estimation of degree of polymerization of poly-acrylonitrile-grafted carbon nanotubes using Guinier plot of small angle x-ray scattering.

    PubMed

    Cho, Hyunjung; Jin, Kyeong Sik; Lee, Jaegeun; Lee, Kun-Hong

    2018-07-06

    Small angle x-ray scattering (SAXS) was used to estimate the degree of polymerization of polymer-grafted carbon nanotubes (CNTs) synthesized using a 'grafting from' method. This analysis characterizes the grafted polymer chains without cleaving them from CNTs, and provides reliable data that can complement conventional methods such as thermogravimetric analysis or transmittance electron microscopy. Acrylonitrile was polymerized from the surface of the CNTs by using redox initiation to produce poly-acrylonitrile-grafted CNTs (PAN-CNTs). Polymerization time and the initiation rate were varied to control the degree of polymerization. Radius of gyration (R g ) of PAN-CNTs was determined using the Guinier plot obtained from SAXS solution analysis. The results showed consistent values according to the polymerization condition, up to a maximum R g  = 125.70 Å whereas that of pristine CNTs was 99.23 Å. The dispersibility of PAN-CNTs in N,N-dimethylformamide was tested using ultraviolet-visible-near infrared spectroscopy and was confirmed to increase as the degree of polymerization increased. This analysis will be helpful to estimate the degree of polymerization of any polymer-grafted CNTs synthesized using the 'grafting from' method and to fabricate polymer/CNT composite materials.

  7. Morphological transformations in the magnetite biomineralizing protein Mms6 in iron solutions: A small-angle x-ray scattering study

    DOE PAGES

    Zhang, Honghu; Liu, Xunpei; Feng, Shuren; ...

    2015-02-10

    In this study, magnetotactic bacteria that produce magnetic nanocrystals of uniform size and well-defined morphologies have inspired the use of biomineralization protein Mms6 to promote formation of uniform magnetic nanocrystals in vitro. Small angle X-ray scattering (SAXS) studies in physiological solutions reveal that Mms6 forms compact globular three-dimensional (3D) micelles (approximately 10 nm in diameter) that are, to a large extent, independent of concentration. In the presence of iron ions in the solutions, the general micellar morphology is preserved, however, with associations among micelles that are induced by iron ions. Compared with Mms6, the m2Mms6 mutant (with the sequence ofmore » hydroxyl/carboxyl containing residues in the C-terminal domain shuffled) exhibits subtle morphological changes in the presence of iron ions in solutions. The analysis of the SAXS data is consistent with a hierarchical core–corona micellar structure similar to that found in amphiphilic polymers. The addition of ferric and ferrous iron ions to the protein solution induces morphological changes in the micellar structure by transforming the 3D micelles into objects of reduced dimensionality of 2, with fractal-like characteristics (including Gaussian-chain-like) or, alternatively, platelet-like structures.« less

  8. Surface morphology of vacuum-evaporated pentacene film on Si substrate studied by in situ grazing-incidence small-angle X-ray scattering: I. The initial stage of formation of pentacene film

    NASA Astrophysics Data System (ADS)

    Hirosawa, Ichiro; Watanabe, Takeshi; Koganezawa, Tomoyuki; Kikuchi, Mamoru; Yoshimoto, Noriyuki

    2018-03-01

    The progress of the surface morphology of a growing sub-monolayered pentacene film on a Si substrate was studied by in situ grazing-incidence small angle X-ray scattering (GISAXS). The observed GISAXS profiles did not show sizes of pentacene islands but mainly protuberances on the boundaries around pentacene film. Scattering of X-ray by residual pits in the pentacene film was also detected in the GISAXS profiles of an almost fully covered film. The average radius of pentacene protuberances increased from 13 to 24 nm as the coverage increased to 0.83 monolayer, and the most frequent radius was almost constant at approximately 9 nm. This result suggests that the population of larger protuberances increase with increasing lengths of boundaries of the pentacene film. It can also be considered that the detected protuberances were crystallites of pentacene, since the average size of protuberances was nearly equal to crystallite sizes of pentacene films. The almost constant characteristic distance of 610 nm and amplitudes of pair correlation functions at low coverages suggest that the growth of pentacene films obeyed the diffusion-limited aggregation (DLA) model, as previously reported. It is also considered that the sites of islands show a triangular distribution for small variations of estimated correlation distances.

  9. Reflective small angle electron scattering to characterize nanostructures on opaque substrates

    NASA Astrophysics Data System (ADS)

    Friedman, Lawrence H.; Wu, Wen-Li; Fu, Wei-En; Chien, Yunsan

    2017-09-01

    Feature sizes in integrated circuits (ICs) are often at the scale of 10 nm and are ever shrinking. ICs appearing in today's computers and hand held devices are perhaps the most prominent examples. These smaller feature sizes demand equivalent advances in fast and accurate dimensional metrology for both development and manufacturing. Techniques in use and continuing to be developed include X-ray based techniques, optical scattering, and of course the electron and scanning probe microscopy techniques. Each of these techniques has their advantages and limitations. Here, the use of small angle electron beam scattering measurements in a reflection mode (RSAES) to characterize the dimensions and the shape of nanostructures on flat and opaque substrates is demonstrated using both experimental and theoretical evidence. In RSAES, focused electrons are scattered at angles smaller than 1 ° with the assistance of electron optics typically used in transmission electron microscopy. A proof-of-concept experiment is combined with rigorous electron reflection simulations to demonstrate the efficiency and accuracy of RSAES as a method of non-destructive measurement of shapes of features less than 10 nm in size on flat and opaque substrates.

  10. Reflective Small Angle Electron Scattering to Characterize Nanostructures on Opaque Substrates.

    PubMed

    Friedman, Lawrence H; Wu, Wen-Li; Fu, Wei-En; Chien, Yunsan

    2017-09-01

    Features sizes in integrated circuits (ICs) are often at the scale of 10 nm and are ever shrinking. ICs appearing in today's computers and hand held devices are perhaps the most prominent examples. These smaller feature sizes demand equivalent advances in fast and accurate dimensional metrology for both development and manufacturing. Techniques in use and continuing to be developed include X-ray based techniques, optical scattering and of course the electron and scanning probe microscopy techniques. Each of these techniques have their advantages and limitations. Here the use of small angle electron beam scattering measurements in a reflection mode (RSAES) to characterize the dimensions and the shape of nanostructures on flat and opaque substrates is demonstrated using both experimental and theoretical evidence. In RSAES, focused electrons are scattered at angles smaller than 1° with the assistance of electron optics typically used in transmission electron microscopy. A proof-of-concept experiment is combined with rigorous electron reflection simulations to demonstrate the efficiency and accuracy of RSAES as a method of non-destructive measurement of shapes of features less than 10 nm in size on flat and opaque substrates.

  11. Quantitative Correlation between Viscosity of Concentrated MAb Solutions and Particle Size Parameters Obtained from Small-Angle X-ray Scattering.

    PubMed

    Fukuda, Masakazu; Moriyama, Chifumi; Yamazaki, Tadao; Imaeda, Yoshimi; Koga, Akiko

    2015-12-01

    To investigate the relationship between viscosity of concentrated MAb solutions and particle size parameters obtained from small-angle X-ray scattering (SAXS). The viscosity of three MAb solutions (MAb1, MAb2, and MAb3; 40-200 mg/mL) was measured by electromagnetically spinning viscometer. The protein interactions of MAb solutions (at 60 mg/mL) was evaluated by SAXS. The phase behavior of 60 mg/mL MAb solutions in a low-salt buffer was observed after 1 week storage at 25°C. The MAb1 solutions exhibited the highest viscosity among the three MAbs in the buffer containing 50 mM NaCl. Viscosity of MAb1 solutions decreased with increasing temperature, increasing salt concentration, and addition of amino acids. Viscosity of MAb1 solutions was lowest in the buffer containing histidine, arginine, and aspartic acid. Particle size parameters obtained from SAXS measurements correlated very well with the viscosity of MAb solutions at 200 mg/mL. MAb1 exhibited liquid-liquid phase separation at a low salt concentration. Simultaneous addition of basic and acidic amino acids effectively suppressed intermolecular attractive interactions and decreased viscosity of MAb1 solutions. SAXS can be performed using a small volume of samples; therefore, the particle size parameters obtained from SAXS at intermediate protein concentration could be used to screen for low viscosity antibodies in the early development stage.

  12. Small-Angle X-ray Scattering and Single-Molecule FRET Spectroscopy Produce Highly Divergent Views of the Low-Denaturant Unfolded State

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

    Yoo, Tae Yeon; Meisburger, Steve P.; Hinshaw, James

    2012-10-10

    The results of more than a dozen single-molecule Foerster resonance energy transfer (smFRET) experiments suggest that chemically unfolded polypeptides invariably collapse from an expanded random coil to more compact dimensions as the denaturant concentration is reduced. In sharp contrast, small-angle X-ray scattering (SAXS) studies suggest that, at least for single-domain proteins at non-zero denaturant concentrations, such compaction may be rare. Here, we explore this discrepancy by studying protein L, a protein previously studied by SAXS (at 5 C), which suggested fixed unfolded-state dimensions from 1.4 to 5 M guanidine hydrochloride (GuHCl), and by smFRET (at 25 C), which suggested that,more » in contrast, the chain contracts by 15-30% over this same denaturant range. Repeating the earlier SAXS study under the same conditions employed in the smFRET studies, we observe little, if any, evidence that the unfolded state of protein L contracts as the concentration of GuHCl is reduced. For example, scattering profiles (and thus the shape and dimensions) collected within {approx} 4 ms after dilution to as low as 0.67 M GuHCl are effectively indistinguishable from those observed at equilibrium at higher denaturant. Our results thus argue that the disagreement between SAXS and smFRET is statistically significant and that the experimental evidence in favor of obligate polypeptide collapse at low denaturant cannot be considered conclusive yet.« less

  13. Microstructural characterization of dental zinc phosphate cements using combined small angle neutron scattering and microfocus X-ray computed tomography.

    PubMed

    Viani, Alberto; Sotiriadis, Konstantinos; Kumpová, Ivana; Mancini, Lucia; Appavou, Marie-Sousai

    2017-04-01

    To characterize the microstructure of two zinc phosphate cement formulations in order to investigate the role of liquid/solid ratio and composition of powder component, on the developed porosity and, consequently, on compressive strength. X-ray powder diffraction with the Rietveld method was used to study the phase composition of zinc oxide powder and cements. Powder component and cement microstructure were investigated with scanning electron microscopy. Small angle neutron scattering (SANS) and microfocus X-ray computed tomography (XmCT) were together employed to characterize porosity and microstructure of dental cements. Compressive strength tests were performed to evaluate their mechanical performance. The beneficial effects obtained by the addition of Al, Mg and B to modulate powder reactivity were mitigated by the crystallization of a Zn aluminate phase not involved in the cement setting reaction. Both cements showed spherical pores with a bimodal distribution at the micro/nano-scale. Pores, containing a low density gel-like phase, developed through segregation of liquid during setting. Increasing liquid/solid ratio from 0.378 to 0.571, increased both SANS and XmCT-derived specific surface area (by 56% and 22%, respectively), porosity (XmCT-derived porosity increased from 3.8% to 5.2%), the relative fraction of large pores ≥50μm, decreased compressive strength from 50±3MPa to 39±3MPa, and favored microstructural and compositional inhomogeneities. Explain aspects of powder design affecting the setting reaction and, in turn, cement performance, to help in optimizing cement formulation. The mechanism behind development of porosity and specific surface area explains mechanical performance, and processes such as erosion and fluoride release/uptake. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

  14. Nanometer-scale characterization of laser-driven plasmas, compression, shocks and phase transitions, by coherent small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Kluge, Thomas

    2015-11-01

    Combining ultra-intense short-pulse and high-energy long-pulse lasers, with brilliant coherent hard X-ray FELs, such as the Helmholtz International Beamline for Extreme Fields (HIBEF) under construction at the HED Instrument of European XFEL, or MEC at LCLS, holds the promise to revolutionize our understanding of many High Energy Density Physics phenomena. Examples include the relativistic electron generation, transport, and bulk plasma response, and ionization dynamics and heating in relativistic laser-matter interactions, or the dynamics of laser-driven shocks, quasi-isentropic compression, and the kinetics of phase transitions at high pressure. A particularly promising new technique is the use of coherent X-ray diffraction to characterize electron density correlations, and by resonant scattering to characterize the distribution of specific charge-state ions, either on the ultrafast time scale of the laser interaction, or associated with hydrodynamic motion. As well one can image slight density changes arising from phase transitions inside of shock-compressed high pressure matter. The feasibility of coherent diffraction techniques in laser-driven matter will be discussed. including recent results from demonstration experiments at MEC. Among other things, very sharp density changes from laser-driven compression are observed, having an effective step width of 10 nm or smaller. This compares to a resolution of several hundred nm achievedpreviously with phase contrast imaging. and on behalf of HIBEF User Consortium, for the Helmholtz International Beamline for Extreme Fields at the European XFEL.

  15. Talbot-Lau x-ray interferometry for high energy density plasma diagnostic.

    PubMed

    Stutman, D; Finkenthal, M

    2011-11-01

    High resolution density diagnostics are difficult in high energy density laboratory plasmas (HEDLP) experiments due to the scarcity of probes that can penetrate above solid density plasmas. Hard x-rays are one possible probe for such dense plasmas. We study the possibility of applying an x-ray method recently developed for medical imaging, differential phase-contrast with Talbot-Lau interferometers, for the diagnostic of electron density and small-scale hydrodynamic instabilities in HEDLP experiments. The Talbot method uses micro-periodic gratings to measure the refraction and ultra-small angle scatter of x-rays through an object and is attractive for HEDLP diagnostic due to its capability to work with incoherent and polychromatic x-ray sources such as the laser driven backlighters used for HEDLP radiography. Our paper studies the potential of the Talbot method for HEDLP diagnostic, its adaptation to the HEDLP environment, and its extension of high x-ray energy using micro-periodic mirrors. The analysis is illustrated with experimental results obtained using a laboratory Talbot interferometer. © 2011 American Institute of Physics

  16. Investigation of the Interaction between Nafion Ionomer and Surface Functionalized Carbon Black Using Both Ultrasmall Angle X-ray Scattering and Cryo-TEM

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

    Yang, Fan; Xin, Le; Uzunoglu, Aytekin

    In making a catalyst ink, the interaction between Nafion ionomer and catalyst support are the key factors that directly affect both ionic conductivity and electronic conductivity of the catalyst layer in a membrane electrode assembly (MEA). One of the major aims of this investigation is to understand the behavior of the catalyst support, Vulcan XC-72 (XC-72) aggregates, in the existence of the Nafion ionomer in a catalyst ink to fill the knowledge gap of the interaction of these components. The dispersion of catalyst ink not only depends on the solvent, but also depends on the interaction of Nafion and carbonmore » particles in the ink. The interaction of Nafion ionomer particles and XC-72 catalyst aggregates in liquid media was studied using ultra small angle x-ray scattering (USAXS) and cryogenic TEM techniques. Carbon black XC-72) and functionalized carbon black systems were introduced to study the interaction behaviors. A multiple curve fitting was used to extract the particle size and size distribution from scattering data. The results suggest that the particle size and size distribution of each system changed significantly in Nafion + XC-72 system, Nafion + NH2-XC72 system, and Nafion + SO3H-XC-72 system, which indicates that an interaction among these components (i.e. ionomer particles and XC-72 aggregates) exists. The cryogenic TEM, which allows for the observation the size of particles in a liquid, was used to validate the scattering results and shows excellent agreement.« less

  17. Note: Comparison of grazing incidence small angle x-ray scattering of a titania sponge structure at the beamlines BW4 (DORIS III) and P03 (PETRA III)

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

    Rawolle, M.; Koerstgens, V.; Ruderer, M. A.

    2012-10-15

    Grazing incidence small angle x-ray scattering (GISAXS) is a powerful technique for morphology investigation of nanostructured thin films. GISAXS measurements at the newly installed P03 beamline at the storage ring PETRA III in Hamburg, Germany, are compared to the GISAXS data from the beamline BW4 at the storage ring DORIS III, which had been used extensively for GISAXS investigations in the past. As an example, a titania thin film sponge structure is investigated. Compared to BW4, at beamline P03 the resolution of larger structures is slightly improved and a higher incident flux leads to a factor of 750 in scatteredmore » intensity. Therefore, the acquisition time in GISAXS geometry is reduced significantly at beamline P03.« less

  18. Location of cholesterol in liposomes by using small-angle X-ray scattering (SAXS) data and the generalized indirect Fourier transformation (GIFT) method.

    PubMed

    Aburai, Kenichi; Ogura, Taku; Hyodo, Ryo; Sakai, Hideki; Abe, Masahiko; Glatter, Otto

    2013-01-01

    We investigated the location of cholesterol (Chol) in liposomes and its interaction with phospholipids using small-angle x-ray scattering (SAXS) data and applying the generalized indirect Fourier transformation (GIFT) method. The GIFT method has been applied to lamellar liquid crystal systems and it gives quantitative data on bilayer thickness, electron density profile, and membrane flexibility (Caillé parameter). When the GIFT method is applied to the SAXS data of dipalmitoylphosphatidylcholine (DPPC) alone (Chol [-]) or a DPPC/Chol = 7/3 mixed system (Chol [+], molar ratio), change in the bilayer thickness was insignificant in both systems. However, the electron density for the Chol (+) system was higher than that for the Chol (-) system at the location of hydrophilic groups of phospholipids, and whereas Caillé parameter value increased with temperature for the Chol (-) system, no significant change with temperature was observed in the Caillé parameter for the Chol (+) system. These results indicated that Chol is located in the vicinity of the hydrophilic group of the phospholipids and constricts the packing of the acyl chain of phospholipids in the bilayer.

  19. SASfit: a tool for small-angle scattering data analysis using a library of analytical expressions.

    PubMed

    Breßler, Ingo; Kohlbrecher, Joachim; Thünemann, Andreas F

    2015-10-01

    SASfit is one of the mature programs for small-angle scattering data analysis and has been available for many years. This article describes the basic data processing and analysis workflow along with recent developments in the SASfit program package (version 0.94.6). They include (i) advanced algorithms for reduction of oversampled data sets, (ii) improved confidence assessment in the optimized model parameters and (iii) a flexible plug-in system for custom user-provided models. A scattering function of a mass fractal model of branched polymers in solution is provided as an example for implementing a plug-in. The new SASfit release is available for major platforms such as Windows, Linux and MacOS. To facilitate usage, it includes comprehensive indexed documentation as well as a web-based wiki for peer collaboration and online videos demonstrating basic usage. The use of SASfit is illustrated by interpretation of the small-angle X-ray scattering curves of monomodal gold nanoparticles (NIST reference material 8011) and bimodal silica nanoparticles (EU reference material ERM-FD-102).

  20. Versatile application of indirect Fourier transformation to structure factor analysis: from X-ray diffraction of molecular liquids to small angle scattering of protein solutions.

    PubMed

    Fukasawa, Toshiko; Sato, Takaaki

    2011-02-28

    We highlight versatile applicability of a structure-factor indirect Fourier transformation (IFT) technique, hereafter called SQ-IFT. The original IFT aims at the pair distance distribution function, p(r), of colloidal particles from small angle scattering of X-rays (SAXS) and neutrons (SANS), allowing the conversion of the experimental form factor, P(q), into a more intuitive real-space spatial autocorrelation function. Instead, SQ-IFT is an interaction potential model-free approach to the 'effective' or 'experimental' structure factor to yield the pair correlation functions (PCFs), g(r), of colloidal dispersions like globular protein solutions for small-angle scattering data as well as the radial distribution functions (RDFs) of molecular liquids in liquid diffraction (LD) experiments. We show that SQ-IFT yields accurate RDFs of liquid H(2)O and monohydric alcohol reflecting their local intermolecular structures, in which q-weighted structure function, qH(q), conventionally utilized in many LD studies out of necessity of performing direct Fourier transformation, is no longer required. We also show that SQ-IFT applied to theoretically calculated structure factors for uncharged and charged colloidal dispersions almost perfectly reproduces g(r) obtained as a solution of the Ornstein-Zernike (OZ) equation. We further demonstrate the relevance of SQ-IFT in its practical applications, using SANS effective structure factors of lysozyme solutions reported in recent literatures which revealed the equilibrium cluster formation due to coexisting long range electrostatic repulsion and short range attraction between the proteins. Finally, we present SAXS experiments on human serum albumin (HSA) at different ionic strength and protein concentration, in which we discuss the real space picture of spatial distributions of the proteins via the interaction potential model-free route.

  1. Characterization of oxidized tannins: comparison of depolymerization methods, asymmetric flow field-flow fractionation and small-angle X-ray scattering.

    PubMed

    Vernhet, Aude; Dubascoux, Stéphane; Cabane, Bernard; Fulcrand, Hélène; Dubreucq, Eric; Poncet-Legrand, Céline

    2011-09-01

    Condensed tannins are a major class of plant polyphenols. They play an important part in the colour and taste of foods and beverages. Due to their chemical reactivity, tannins are not stable once extracted from plants. A number of chemical reactions can take place, leading to structural changes of the native structures to give so-called derived tannins and pigments. This paper compares results obtained on native and oxidized tannins with different techniques: depolymerization followed by high-performance liquid chromatography analysis, small-angle X-ray scattering (SAXS) and asymmetric flow field-flow fractionation (AF4). Upon oxidation, new macromolecules were formed. Thioglycolysis experiments showed no evidence of molecular weight increase, but thioglycolysis yields drastically decreased. When oxidation was performed at high concentration (e.g., 10 g L(-1)), the weight average degree of polymerization determined from SAXS increased, whereas it remained stable when oxidation was done at low concentration (0.1 g L(-1)), indicating that the reaction was intramolecular, yet the conformations were different. Differences in terms of solubility were observed; ethanol being a better solvent than water. We also separated soluble and non-water-soluble species of a much oxidized fraction. Thioglycolysis showed no big differences between the two fractions, whereas SAXS and AF4 showed that insoluble macromolecules have a weight average molecular weight ten times higher than the soluble ones.

  2. Structural analysis of Fe–Mn–O nanoparticles in glass ceramics by small angle scattering

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

    Raghuwanshi, Vikram Singh, E-mail: vikram.raghuwanshi@helmholtz-berlin.de; Harizanova, Ruzha; Tatchev, Dragomir

    2015-02-15

    Magnetic nanocrystals containing Fe and Mn were obtained by annealing of silicate glasses with the composition 13.6Na{sub 2}O–62.9SiO{sub 2}–8.5MnO–15.0Fe{sub 2}O{sub 3−x} (mol%) at 580 °C for different periods of time. Here, we present Small Angle Neutron Scattering using Polarized neutrons (SANSPOL) and Anomalous Small Angle X-ray Scattering (ASAXS) investigation on these glass ceramic samples. Analysis of scattering data from both methods reveals the formation of spherical core–shell type of nanoparticles with mean sizes between 10 nm and 100 nm. ASAXS investigation shows the particles have higher concentration of iron atoms and the shell like region surrounding the particles is enrichedmore » in SiO{sub 2}. SANSPOL investigation shows the particles are found to be magnetic and are surrounded by a non-magnetic shell-like region. - Graphical abstract: Magnetic spherical core–shell nanoparticles in glass ceramics: SANSPOL and ASAXS investigations. - Highlights: • Formation and growth mechanisms of magnetic nanoparticles in silicate glass. • SANSPOL and ASAXS methods employed to evaluate quantitative information. • Analyses showed formation of nanoparticles with spherical core–shell structures. • Core of the particle is magnetic and surrounded by weak magnetic shell like region.« less

  3. First refraction contrast imaging via Laser-Compton Scattering X-ray at KEK

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

    Sakaue, Kazuyuki; Aoki, Tatsuro; Washio, Masakazu

    2012-07-31

    Laser-Compton Scattering (LCS) is one of the most feasible techniques for high quality, high brightness, and compact X-ray source. High energy electron beam produced by accelerators scatters off the laser photon at a small spot. As a laser target, we have been developing a pulsedlaser storage cavity for increasing an X-ray flux. The X-ray flux was still inadequate that was 2.1 Multiplication-Sign 10{sup 5}/sec, however, we performed first refraction contrast imaging in order to evaluate the quality of LCS X-ray. Edge enhanced contrast imaging was achieved by changing the distance from sample to detector. The edge enhancement indicates that themore » LCS X-ray has small source size, i.e. high brightness. We believe that the result has demonstrated good feasibility of linac-based high brightness X-ray sources via laser-electron Compton scatterings.« less

  4. Interior tomographic imaging for x-ray coherent scattering (Conference Presentation)

    NASA Astrophysics Data System (ADS)

    Pang, Sean; Zhu, Zheyuan

    2017-05-01

    Conventional computed tomography reconstructs the attenuation only high-dimensional images. Coherent scatter computed tomography, which reconstructs the angular dependent scattering profiles of 3D objects, can provide molecular signatures that improves the accuracy of material identification and classification. Coherent scatter tomography are traditionally acquired by setups similar to x-ray powder diffraction machine; a collimated source in combination with 2D or 1D detector collimation in order to localize the scattering point. In addition, the coherent scatter cross-section is often 3 orders of magnitude lower than that of the absorption cross-section for the same material. Coded aperture and structured illumination approaches has been shown to greatly improve the collection efficiency. In many applications, especially in security imaging and medical diagnosis, fast and accurate identification of the material composition of a small volume within the whole object would lead to an accelerated imaging procedure and reduced radiation dose. Here, we report an imaging method to reconstruct the material coherent scatter profile within a small volume. The reconstruction along one radial direction can reconstruct a scalar coherent scattering tomographic image. Our methods takes advantage of the finite support of the scattering profile in small angle regime. Our system uses a pencil beam setup without using any detector side collimation. Coherent scatter profile of a 10 mm scattering sample embedded in a 30 mm diameter phantom was reconstructed. The setup has small form factor and is suitable for various portable non-destructive detection applications.

  5. Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering

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

    Yuan, Xueming; Duan, Yonghao; He, Lilin

    A systematic study was done to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110 °C for 3 h at biomass loadings of 5, 10, 15, 20 and 25 wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ~25 to 625 Å, enabling assessment of contributions of pores with different sizes to increased porositymore » after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role.« less

  6. Characterization of white poplar and eucalyptus after ionic liquid pretreatment as a function of biomass loading using X-ray diffraction and small angle neutron scattering.

    PubMed

    Yuan, Xueming; Duan, Yonghao; He, Lilin; Singh, Seema; Simmons, Blake; Cheng, Gang

    2017-05-01

    A systematic study was performed to understand interactions among biomass loading during ionic liquid (IL) pretreatment, biomass type and biomass structures. White poplar and eucalyptus samples were pretreated using 1-ethyl-3-methylimidazolium acetate (EmimOAc) at 110°C for 3h at biomass loadings of 5, 10, 15, 20 and 25wt%. All of the samples were chemically characterized and tested for enzymatic hydrolysis. Physical structures including biomass crystallinity and porosity were measured by X-ray diffraction (XRD) and small angle neutron scattering (SANS), respectively. SANS detected pores of radii ranging from ∼25 to 625Å, enabling assessment of contributions of pores with different sizes to increased porosity after pretreatment. Contrasting dependences of sugar conversion on white poplar and eucalyptus as a function of biomass loading were observed and cellulose crystalline structure was found to play an important role. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Investigating Polymer–Metal Interfaces by Grazing Incidence Small-Angle X-Ray Scattering from Gradients to Real-Time Studies

    PubMed Central

    Schwartzkopf, Matthias; Roth, Stephan V.

    2016-01-01

    Tailoring the polymer–metal interface is crucial for advanced material design. Vacuum deposition methods for metal layer coating are widely used in industry and research. They allow for installing a variety of nanostructures, often making use of the selective interaction of the metal atoms with the underlying polymer thin film. The polymer thin film may eventually be nanostructured, too, in order to create a hierarchy in length scales. Grazing incidence X-ray scattering is an advanced method to characterize and investigate polymer–metal interfaces. Being non-destructive and yielding statistically relevant results, it allows for deducing the detailed polymer–metal interaction. We review the use of grazing incidence X-ray scattering to elucidate the polymer–metal interface, making use of the modern synchrotron radiation facilities, allowing for very local studies via in situ (so-called “stop-sputter”) experiments as well as studies observing the nanostructured metal nanoparticle layer growth in real time. PMID:28335367

  8. Polarized x-ray excitation for scatter reduction in x-ray fluorescence computed tomography.

    PubMed

    Vernekohl, Don; Tzoumas, Stratis; Zhao, Wei; Xing, Lei

    2018-05-25

    X-ray fluorescence computer tomography (XFCT) is a new molecular imaging modality which uses x-ray excitation to stimulate the emission of fluorescent photons in high atomic number contrast agents. Scatter contamination is one of the main challenges in XFCT imaging which limits the molecular sensitivity. When polarized x rays are used, it is possible to reduce the scatter contamination significantly by placing detectors perpendicular to the polarization direction. This study quantifies scatter contamination for polarized and unpolarized x-ray excitation and determines the advantages of scatter reduction. The amount of scatter in preclinical XFCT is quantified in Monte Carlo simulations. The fluorescent x rays are emitted isotropically, while scattered x rays propagate in polarization direction. The magnitude of scatter contamination is studied in XFCT simulations of a mouse phantom. In this study, the contrast agent gold is examined as an example, but a scatter reduction from polarized excitation is also expected for other elements. The scatter reduction capability is examined for different polarization intensities with a monoenergetic x-ray excitation energy of 82 keV. The study evaluates two different geometrical shapes of CZT detectors which are modeled with an energy resolution of 1 keV FWHM at an x-ray energy of 80 keV. Benefits of a detector placement perpendicular to the polarization direction are shown in iterative and analytic image reconstruction including scatter correction. The contrast to noise ratio (CNR) and the normalized mean square error (NMSE) are analyzed and compared for the reconstructed images. A substantial scatter reduction for common detector sizes was achieved for 100% and 80% linear polarization while lower polarization intensities provide a decreased scatter reduction. By placing the detector perpendicular to the polarization direction, a scatter reduction by factor up to 5.5 can be achieved for common detector sizes. The image

  9. SU-E-I-44: Some Preliminary Analysis of Angular Distribution of X-Ray Scattered On Soft Tissues

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

    Ganezer, K; Krmar, M; Cvejic, Z

    2015-06-15

    Purpose: The angular distribution of x-radiation scattered at small angles (up to 16 degrees) from several different animal soft tissue (skin, fat, muscle, retina, etc) were measured using standard equipment devoted to study of crystal structure which provides excellent geometry conditions of measurements. showed measurable differences for different tissues. In the simplest possible case when measured samples do not differ in structure (different concentration solutions) it can be seen that intensity of scattered radiation is decreasing function of the concentration and the peak of the maximum of scattering distribution depends on the concentration as well. Methods: An x-ray scattering profilemore » usually consists of sharp diffraction peak; however some properties of the spatial profiles of scattered radiation as intensity, the peak position, height, area, FWHM, the ratio of peak heights, etc. Results: The data contained measurable differences for different tissues. In the simplest possible case when measured samples do not differ in structure (different concentration solutions) it can be seen that intensity of scattered radiation is decreasing function of the concentration and the peak of the maximum of scattering distribution depends on the concentration as well. Measurements of different samples in the very preliminary phase showed that simple biological material used in study showed slightly different scattering pattern, especially at higher angles (around 10degrees). Intensity of radiation scattered from same tissue type is very dependent on water content and several more parameters. Conclusion: This preliminary study using animal soft tissues on the angular distributions of scattered x-rays suggests that angular distributions of X-rays scattered off of soft tissues might be useful in distinguishing healthy tissue from malignant soft tissue.« less

  10. Asymmetric masks for laboratory-based X-ray phase-contrast imaging with edge illumination.

    PubMed

    Endrizzi, Marco; Astolfo, Alberto; Vittoria, Fabio A; Millard, Thomas P; Olivo, Alessandro

    2016-05-05

    We report on an asymmetric mask concept that enables X-ray phase-contrast imaging without requiring any movement in the system during data acquisition. The method is compatible with laboratory equipment, namely a commercial detector and a rotating anode tube. The only motion required is that of the object under investigation which is scanned through the imaging system. Two proof-of-principle optical elements were designed, fabricated and experimentally tested. Quantitative measurements on samples of known shape and composition were compared to theory with good agreement. The method is capable of measuring the attenuation, refraction and (ultra-small-angle) X-ray scattering, does not have coherence requirements and naturally adapts to all those situations in which the X-ray image is obtained by scanning a sample through the imaging system.

  11. Protein crowding in solution, frozen and freeze-dried states: small-angle neutron and X-ray scattering study of lysozyme/sorbitol/water systems

    NASA Astrophysics Data System (ADS)

    Krueger, Susan; Khodadadi, Sheila; Clark, Nicholas; McAuley, Arnold; Cristiglio, Viviana; Theyencheri, Narayanan; Curtis, Joseph; Shalaev, Evgenyi

    2015-03-01

    For effective preservation, proteins are often stored as frozen solutions or in glassy states using a freeze-drying process. However, aggregation is often observed after freeze-thaw or reconstitution of freeze-dried powder and the stability of the protein is no longer assured. In this study, small-angle neutron and X-ray scattering (SANS and SAXS) have been used to investigate changes in protein-protein interaction distances of a model protein/cryoprotectant system of lysozyme/sorbitol/water, under representative pharmaceutical processing conditions. The results demonstrate the utility of SAXS and SANS methods to monitor protein crowding at different stages of freezing and drying. The SANS measurements of solution samples showed at least one protein interaction peak corresponding to an interaction distance of ~ 90 Å. In the frozen state, two protein interaction peaks were observed by SANS with corresponding interaction distances at 40 Å as well as 90 Å. On the other hand, both SAXS and SANS data for freeze-dried samples showed three peaks, suggesting interaction distances ranging from ~ 15 Å to 170 Å. Possible interpretations of these interaction peaks will be discussed, as well as the role of sorbitol as a cryoprotectant during the freezing and drying process.

  12. Determination of the size and phase composition of silver nanoparticles in a gel film of bacterial cellulose by small-angle X-ray scattering, electron diffraction, and electron microscopy

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

    Volkov, V. V.; Klechkovskaya, V. V., E-mail: klechvv@ns.crys.ras.ru; Shtykova, E. V.

    2009-03-15

    The nanoscale structural features in a composite (gel film of Acetobacter Xylinum cellulose with adsorbed silver nanoparticles, stabilized by N-polyvinylpyrrolidone) have been investigated by small-angle X-ray scattering. The size distributions of inhomogeneities in the porous structure of the cellulose matrix and the size distributions of silver nanoparticles in the composite have been determined. It is shown that the sizes of synthesized nanoparticles correlate with the sizes of inhomogeneities in the gel film. Particles of larger size (with radii up to 100 nm) have also been found. Electron microscopy of thin cross sections of a dried composite layer showed that largemore » particles are located on the cellulose layer surface. Electron diffraction revealed a crystal structure of silver nanoparticles in the composite.« less

  13. Synchrotron-based coherent scatter x-ray projection imaging using an array of monoenergetic pencil beams.

    PubMed

    Landheer, Karl; Johns, Paul C

    2012-09-01

    Traditional projection x-ray imaging utilizes only the information from the primary photons. Low-angle coherent scatter images can be acquired simultaneous to the primary images and provide additional information. In medical applications scatter imaging can improve x-ray contrast or reduce dose using information that is currently discarded in radiological images to augment the transmitted radiation information. Other applications include non-destructive testing and security. A system at the Canadian Light Source synchrotron was configured which utilizes multiple pencil beams (up to five) to create both primary and coherent scatter projection images, simultaneously. The sample was scanned through the beams using an automated step-and-shoot setup. Pixels were acquired in a hexagonal lattice to maximize packing efficiency. The typical pitch was between 1.0 and 1.6 mm. A Maximum Likelihood-Expectation Maximization-based iterative method was used to disentangle the overlapping information from the flat panel digital x-ray detector. The pixel value of the coherent scatter image was generated by integrating the radial profile (scatter intensity versus scattering angle) over an angular range. Different angular ranges maximize the contrast between different materials of interest. A five-beam primary and scatter image set (which had a pixel beam time of 990 ms and total scan time of 56 min) of a porcine phantom is included. For comparison a single-beam coherent scatter image of the same phantom is included. The muscle-fat contrast was 0.10 ± 0.01 and 1.16 ± 0.03 for the five-beam primary and scatter images, respectively. The air kerma was measured free in air using aluminum oxide optically stimulated luminescent dosimeters. The total area-averaged air kerma for the scan was measured to be 7.2 ± 0.4 cGy although due to difficulties in small-beam dosimetry this number could be inaccurate.

  14. Experiment and application of soft x-ray grazing incidence optical scattering phenomena

    NASA Astrophysics Data System (ADS)

    Chen, Shuyan; Li, Cheng; Zhang, Yang; Su, Liping; Geng, Tao; Li, Kun

    2017-08-01

    For short wavelength imaging systems,surface scattering effects is one of important factors degrading imaging performance. Study of non-intuitive surface scatter effects resulting from practical optical fabrication tolerances is a necessary work for optical performance evaluation of high resolution short wavelength imaging systems. In this paper, Soft X-ray optical scattering distribution is measured by a soft X-ray reflectometer installed by my lab, for different sample mirrors、wavelength and grazing angle. Then aim at space solar telescope, combining these scattered light distributions, and surface scattering numerical model of grazing incidence imaging system, PSF and encircled energy of optical system of space solar telescope are computed. We can conclude that surface scattering severely degrade imaging performance of grazing incidence systems through analysis and computation.

  15. In-Situ Anomalous Small-Angle X-ray Scattering Studies of Polymer Electrolyte Membrane Fuel Cell Catalyst Degradation

    NASA Astrophysics Data System (ADS)

    Gilbert, James Andrew

    Polymer electrolyte membrane fuel cells (PEMFCs) are a promising high efficiency energy conversion technology, but their cost effective implementation, especially for automotive power, has been hindered by degradation of the electrochemically-active surface area (ECA) of the Pt nanoparticle electrocatalysts. While numerous studies using ex-situ post-mortem techniques have provided insight into the effect of operating conditions on ECA loss, the governing mechanisms and underlying processes are not fully understood. Toward the goal of elucidating the electrocatalyst degradation mechanisms, we have followed particle size distribution (PSD) growth evolutions of Pt and Pt-alloy nanoparticle catalysts during potential cycling in an aqueous acidic environment (with and without flow of electrolyte) and in a fuel cell environment using in-situ anomalous small-angle X-ray scattering (ASAXS). The results of this thesis show a surface area loss mechanism of Pt nanoparticles supported on carbon to be predominantly controlled by Pt dissolution, the particle size dependence of Pt dissolution, the loss of dissolved Pt into the membrane and electrolyte, and, to a lesser extent, the re-deposition of dissolved Pt onto larger particles. The relative extent of these loss mechanisms are shown to be dependent on the environment, the temperature, and the potential cycling conditions. Correlation of ASAXS-determined particle growth with both calculated and voltammetrically-determined oxide coverages demonstrates that the oxide coverage is playing a key role in the dissolution process and in the corresponding growth of the mean Pt nanoparticle size and loss of ECA. This understanding potentially reduces the complex changes in PSDs and ECA resulting from various voltage profiles to the response to a single variable, oxide coverage. A better understanding of the degradation mechanisms of Pt and Pt-alloy nanoparticle distributions could lead to more stable electrocatalysts while

  16. 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

  17. Resonant Soft X-ray Scattering as a Powerful Probe of Buried Polymer Interfaces

    NASA Astrophysics Data System (ADS)

    Chen, Wei; Jiang, Zhang; Tirrell, Matthew

    Elucidation of polymer interfacial structures provides insights into interfacial molecular mechanisms for coating protection, adhesion, lubrication, friction, wettability, biocompatibility, and even charge transport properties. Resonant Soft X-ray Scattering (RSoXS) offers a unique element, site and valence specific probe to study spatial modulations of molecular orbital degrees of freedom on the nanoscopic length scale. This unique sensitivity is achieved by merging small angle x-ray scattering and x-ray absorption spectroscopy into a single experiment, where the scattering provides information about spatial modulations and the spectroscopy provides sensitivity to the molecular anisotropy. Here we applied RSoXS to polystyrene (PS) films at solid-solid interfaces and poly(2-methacryloyloxyethyl phosphorylcholine) (PMPC) brushes at solid-liquid interfaces. It is found that the interfacial width of PS thin film is about one order of magnitude large than those observed by traditional scattering techniques. In addition, although the ion-induced changes of PMPC thickness are not apparent in aqueous solutions, their chain conformations like polyzwitterion distribution and correlation varied, dependent on salt types, ionic strengths and ion valences. Consequently, it is evident that RSoXS is a powerful probe of buried polymer interlaces with both spatial and chemical sensitivities. This work was supported by the U.S. Department of Energy, Office of Science, Program in Basic Energy Sciences, Division of Materials Science and Engineering.

  18. Study of the grazing-incidence X-ray scattering of strongly disturbed fractal surfaces

    NASA Astrophysics Data System (ADS)

    Roshchin, B. S.; Chukhovsky, F. N.; Pavlyuk, M. D.; Opolchentsev, A. M.; Asadchikov, V. E.

    2017-03-01

    The applicability of different approaches to the description of hard X-ray scattering from rough surfaces is generally limited by a maximum surface roughness height of no more than 1 nm. Meanwhile, this value is several times larger for the surfaces of different materials subjected to treatment, especially in the initial treatment stages. To control the roughness parameters in all stages of surface treatment, a new approach has been developed, which is based on a series expansion of wavefield over the plane eigenstate-function waves describing the small-angle scattering of incident X-rays in terms of plane q-waves propagating through the interface between two media with a random function of relief heights. To determine the amplitudes of reflected and transmitted plane q-waves, a system of two linked integral equations was derived. The solutions to these equations correspond (in zero order) to the well-known Fresnel expressions for a smooth plane interface. Based on these solutions, a statistical fractal model of an isotropic rough interface is built in terms of root-mean-square roughness σ, two-point correlation length l, and fractal surface index h. The model is used to interpret X-ray scattering data for polished surfaces of single-crystal cadmium telluride samples.

  19. Study of the grazing-incidence X-ray scattering of strongly disturbed fractal surfaces

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

    Roshchin, B. S., E-mail: ross@crys.ras.ru; Chukhovsky, F. N.; Pavlyuk, M. D.

    2017-03-15

    The applicability of different approaches to the description of hard X-ray scattering from rough surfaces is generally limited by a maximum surface roughness height of no more than 1 nm. Meanwhile, this value is several times larger for the surfaces of different materials subjected to treatment, especially in the initial treatment stages. To control the roughness parameters in all stages of surface treatment, a new approach has been developed, which is based on a series expansion of wavefield over the plane eigenstate-function waves describing the small-angle scattering of incident X-rays in terms of plane q-waves propagating through the interface betweenmore » two media with a random function of relief heights. To determine the amplitudes of reflected and transmitted plane q-waves, a system of two linked integral equations was derived. The solutions to these equations correspond (in zero order) to the well-known Fresnel expressions for a smooth plane interface. Based on these solutions, a statistical fractal model of an isotropic rough interface is built in terms of root-mean-square roughness σ, two-point correlation length l, and fractal surface index h. The model is used to interpret X-ray scattering data for polished surfaces of single-crystal cadmium telluride samples.« less

  20. Anisotropic x-ray scattering and orientation fields in cardiac tissue cells

    NASA Astrophysics Data System (ADS)

    Bernhardt, M.; Nicolas, J.-D.; Eckermann, M.; Eltzner, B.; Rehfeldt, F.; Salditt, T.

    2017-01-01

    X-ray diffraction from biomolecular assemblies is a powerful technique which can provide structural information about complex architectures such as the locomotor systems underlying muscle contraction. However, in its conventional form, macromolecular diffraction averages over large ensembles. Progress in x-ray optics has now enabled to probe structures on sub-cellular scales, with the beam confined to a distinct organelle. Here, we use scanning small angle x-ray scattering (scanning SAXS) to probe the diffraction from cytoskeleton networks in cardiac tissue cells. In particular, we focus on actin-myosin composites, which we identify as the dominating contribution to the anisotropic diffraction patterns, by correlation with optical fluorescence microscopy. To this end, we use a principal component analysis approach to quantify direction, degree of orientation, nematic order, and the second moment of the scattering distribution in each scan point. We compare the fiber orientation from micrographs of fluorescently labeled actin fibers to the structure orientation of the x-ray dataset and thus correlate signals of two different measurements: the native electron density distribution of the local probing area versus specifically labeled constituents of the sample. Further, we develop a robust and automated fitting approach based on a power law expansion, in order to describe the local structure factor in each scan point over a broad range of the momentum transfer {q}{{r}}. Finally, we demonstrate how the methodology shown for freeze dried cells in the first part of the paper can be translated to alive cell recordings.

  1. Small-angle X-ray scattering and rheological characterization of alginate gels. 2. Time-resolved studies on ionotropic gels

    NASA Astrophysics Data System (ADS)

    Yuguchi, Y.; Urakawa, H.; Kajiwara, K.; Draget, K. I.; Stokke, B. T.

    2000-10-01

    Gelation was observed by time-resolved small-angle X-ray scattering and rheology on 10 mg/ml Ca-alginate gels prepared by in situ release of Ca 2+ from CaEGTA or CaCO 3 with total Ca 2+ concentration in the range 10-20 mM. This was carried out for alginates having a fraction of α- L-GulA (G) of FG=0.39 and 0.68, respectively, obtained by the selection of alginates isolated from two different brown algae, Ascophyllum nodosum and Laminaria hyperborea stipe. Correlation between the rheological data and SAXS data shows that a large fraction of the lateral association precedes the formation of a continuous network through the sample cell. Following the initial association of chain segments in junction zones, the analysis using two-component broken rod model indicates the formation of larger bundles, and that the relative weight of these bundles increases with increasing time. The molecular model for the bundles is proposed by associating 2-16 units (G-blocks) composed of 14 (1→4) linked residues of α- L-GulA in parallel according to the available crystallographic data. The storage modulus increases as the bundles composed of associated alginate chains grow during the gel formation. The gel elasticity is mainly sustained by single chains in the alginate sample with a low fraction of α- L-GulA. The alginates with a high fraction of α- L-GulA associate into thicker bundles which join to form a network. Here the gel elasticity seems to be due to the flexible joints between bundles, since the fraction of single chains is extremely low.

  2. Transmission X-ray scattering as a probe for complex liquid-surface structures

    DOE PAGES

    Fukuto, Masafumi; Yang, Lin; Nykypanchuk, Dmytro; ...

    2016-01-28

    The need for functional materials calls for increasing complexity in self-assembly systems. As a result, the ability to probe both local structure and heterogeneities, such as phase-coexistence and domain morphologies, has become increasingly important to controlling self-assembly processes, including those at liquid surfaces. The traditional X-ray scattering methods for liquid surfaces, such as specular reflectivity and grazing-incidence diffraction, are not well suited to spatially resolving lateral heterogeneities due to large illuminated footprint. A possible alternative approach is to use scanning transmission X-ray scattering to simultaneously probe local intermolecular structures and heterogeneous domain morphologies on liquid surfaces. To test the feasibilitymore » of this approach, transmission small- and wide-angle X-ray scattering (TSAXS/TWAXS) studies of Langmuir films formed on water meniscus against a vertically immersed hydrophilic Si substrate were recently carried out. First-order diffraction rings were observed in TSAXS patterns from a monolayer of hexagonally packed gold nanoparticles and in TWAXS patterns from a monolayer of fluorinated fatty acids, both as a Langmuir monolayer on water meniscus and as a Langmuir–Blodgett monolayer on the substrate. The patterns taken at multiple spots have been analyzed to extract the shape of the meniscus surface and the ordered-monolayer coverage as a function of spot position. These results, together with continual improvement in the brightness and spot size of X-ray beams available at synchrotron facilities, support the possibility of using scanning-probe TSAXS/TWAXS to characterize heterogeneous structures at liquid surfaces.« less

  3. Using X-ray Thomson Scattering to Characterize Highly Compressed, Near-Degenerate Plasmas at the NIF

    NASA Astrophysics Data System (ADS)

    Doeppner, Tilo; Kraus, D.; Neumayer, P.; Bachmann, B.; Divol, L.; Kritcher, A. L.; Landen, O. L.; Fletcher, L.; Glenzer, S. H.; Falcone, R. W.; MacDonald, M. J.; Saunders, A.; Witte, B.; Redmer, R.; Chapman, D.; Baggott, R.; Gericke, D. O.; Yi, S. A.

    2017-10-01

    We are developing x-ray Thomson scattering for implosion experiments at the National Ignition Facility to characterize plasma conditions in plastic and beryllium capsules near stagnation, reaching more than 20x compression and electron densities of 1025 cm-3, corresponding to a Fermi energy of 170 eV. Using a zinc He- α x-ray source at 9 keV, experiments at a large scattering angle of 120° measure non-collective scattering spectra with high sensitivity to K-shell ionization, and find higher charge states than predicted by widely used ionization models. Reducing the scattering angle to 30° probes the collective scattering regime with sensitivity to collisions and conductivity. We will discuss recent results and future plans. This work was performed under the auspices of the US Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

  4. Digenetic Changes in Macro- to Nano-Scale Porosity in the St. Peter Sandstone:L An (Ultra) Small Angle Neutron Scattering and Backscattered Electron Imagining Analysis

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

    Anovitz, Lawrence; Cole, David; Rother, Gernot

    2013-01-01

    Small- and Ultra-Small Angle Neutron Scattering (SANS and USANS) provide powerful tools for quantitative analysis of porous rocks, yielding bulk statistical information over a wide range of length scales. This study utilized (U)SANS to characterize shallowly buried quartz arenites from the St. Peter Sandstone. Backscattered electron imaging was also used to extend the data to larger scales. These samples contain significant volumes of large-scale porosity, modified by quartz overgrowths, and neutron scattering results show significant sub-micron porosity. While previous scattering data from sandstones suggest scattering is dominated by surface fractal behavior over many orders of magnitude, careful analysis of ourmore » data shows both fractal and pseudo-fractal behavior. The scattering curves are composed of subtle steps, modeled as polydispersed assemblages of pores with log-normal distributions. However, in some samples an additional surface-fractal overprint is present, while in others there is no such structure, and scattering can be explained by summation of non-fractal structures. Combined with our work on other rock-types, these data suggest that microporosity is more prevalent, and may play a much more important role than previously thought in fluid/rock interactions.« less

  5. Scatter fractions from linear accelerators with x-ray energies from 6 to 24 MV.

    PubMed

    Taylor, P L; Rodgers, J E; Shobe, J

    1999-08-01

    Computation of shielding requirements for a linear accelerator must take into account the amount of radiation scattered from the patient to areas outside the primary beam. Currently, the most frequently used data are from NCRP 49 that only includes data for x-ray energies up to 6 MV and angles from 30 degrees to 135 degrees. In this work we have determined by Monte Carlo simulation the scattered fractions of dose for a wide range of energies and angles of clinical significance including 6, 10, 18, and 24 MV and scattering angles from 10 degrees to 150 degrees. Calculations were made for a 400 cm2 circular field size impinging onto a spherical phantom. Scattered fractions of dose were determined at 1 m from the phantom. Angles from 10 degrees to 30 degrees are of concern for higher energies where the scatter is primarily in the forward direction. An error in scatter fraction may result in too little secondary shielding near the junction with the primary barrier. The Monte Carlo code ITS (Version 3.0) developed at Sandia National Laboratory and NIST was used to simulate scatter from the patient to the barrier. Of significance was the variation of calculated scattered dose with depth of measurement within the barrier indicating that accurate values may be difficult to obtain. Mean energies of scatter x-ray spectra are presented.

  6. Constrained Maximum Likelihood Estimation of Relative Abundances of Protein Conformation in a Heterogeneous Mixture from Small Angle X-Ray Scattering Intensity Measurements

    PubMed Central

    Onuk, A. Emre; Akcakaya, Murat; Bardhan, Jaydeep P.; Erdogmus, Deniz; Brooks, Dana H.; Makowski, Lee

    2015-01-01

    In this paper, we describe a model for maximum likelihood estimation (MLE) of the relative abundances of different conformations of a protein in a heterogeneous mixture from small angle X-ray scattering (SAXS) intensities. To consider cases where the solution includes intermediate or unknown conformations, we develop a subset selection method based on k-means clustering and the Cramér-Rao bound on the mixture coefficient estimation error to find a sparse basis set that represents the space spanned by the measured SAXS intensities of the known conformations of a protein. Then, using the selected basis set and the assumptions on the model for the intensity measurements, we show that the MLE model can be expressed as a constrained convex optimization problem. Employing the adenylate kinase (ADK) protein and its known conformations as an example, and using Monte Carlo simulations, we demonstrate the performance of the proposed estimation scheme. Here, although we use 45 crystallographically determined experimental structures and we could generate many more using, for instance, molecular dynamics calculations, the clustering technique indicates that the data cannot support the determination of relative abundances for more than 5 conformations. The estimation of this maximum number of conformations is intrinsic to the methodology we have used here. PMID:26924916

  7. Measuring the molecular dimensions of wine tannins: comparison of small-angle X-ray scattering, gel-permeation chromatography and mean degree of polymerization.

    PubMed

    McRae, Jacqui M; Kirby, Nigel; Mertens, Haydyn D T; Kassara, Stella; Smith, Paul A

    2014-07-23

    The molecular size of wine tannins can influence astringency, and yet it has been unclear as to whether the standard methods for determining average tannin molecular weight (MW), including gel-permeation chromatography (GPC) and depolymerization reactions, are actually related to the size of the tannin in wine-like conditions. Small-angle X-ray scattering (SAXS) was therefore used to determine the molecular sizes and corresponding MWs of wine tannin samples from 3 and 7 year old Cabernet Sauvignon wine in a variety of wine-like matrixes: 5-15% and 100% ethanol; 0-200 mM NaCl and pH 3.0-4.0, and compared to those measured using the standard methods. The SAXS results indicated that the tannin samples from the older wine were larger than those of the younger wine and that wine composition did not greatly impact on tannin molecular size. The average tannin MWs as determined by GPC correlated strongly with the SAXS results, suggesting that this method does give a good indication of tannin molecular size in wine-like conditions. The MW as determined from the depolymerization reactions did not correlate as strongly with the SAXS results. To our knowledge, SAXS measurements have not previously been attempted for wine tannins.

  8. Surface layer protein characterization by small angle x-ray scattering and a fractal mean force concept: from protein structure to nanodisk assemblies.

    PubMed

    Horejs, Christine; Pum, Dietmar; Sleytr, Uwe B; Peterlik, Herwig; Jungbauer, Alois; Tscheliessnig, Rupert

    2010-11-07

    Surface layers (S-layers) are the most commonly observed cell surface structure of prokaryotic organisms. They are made up of proteins that spontaneously self-assemble into functional crystalline lattices in solution, on various solid surfaces, and interfaces. While classical experimental techniques failed to recover a complete structural model of an unmodified S-layer protein, small angle x-ray scattering (SAXS) provides an opportunity to study the structure of S-layer monomers in solution and of self-assembled two-dimensional sheets. For the protein under investigation we recently suggested an atomistic structural model by the use of molecular dynamics simulations. This structural model is now refined on the basis of SAXS data together with a fractal assembly approach. Here we show that a nondiluted critical system of proteins, which crystallize into monomolecular structures, might be analyzed by SAXS if protein-protein interactions are taken into account by relating a fractal local density distribution to a fractal local mean potential, which has to fulfill the Poisson equation. The present work demonstrates an important step into the elucidation of the structure of S-layers and offers a tool to analyze the structure of self-assembling systems in solution by means of SAXS and computer simulations.

  9. Surface layer protein characterization by small angle x-ray scattering and a fractal mean force concept: From protein structure to nanodisk assemblies

    NASA Astrophysics Data System (ADS)

    Horejs, Christine; Pum, Dietmar; Sleytr, Uwe B.; Peterlik, Herwig; Jungbauer, Alois; Tscheliessnig, Rupert

    2010-11-01

    Surface layers (S-layers) are the most commonly observed cell surface structure of prokaryotic organisms. They are made up of proteins that spontaneously self-assemble into functional crystalline lattices in solution, on various solid surfaces, and interfaces. While classical experimental techniques failed to recover a complete structural model of an unmodified S-layer protein, small angle x-ray scattering (SAXS) provides an opportunity to study the structure of S-layer monomers in solution and of self-assembled two-dimensional sheets. For the protein under investigation we recently suggested an atomistic structural model by the use of molecular dynamics simulations. This structural model is now refined on the basis of SAXS data together with a fractal assembly approach. Here we show that a nondiluted critical system of proteins, which crystallize into monomolecular structures, might be analyzed by SAXS if protein-protein interactions are taken into account by relating a fractal local density distribution to a fractal local mean potential, which has to fulfill the Poisson equation. The present work demonstrates an important step into the elucidation of the structure of S-layers and offers a tool to analyze the structure of self-assembling systems in solution by means of SAXS and computer simulations.

  10. Surface layer protein characterization by small angle x-ray scattering and a fractal mean force concept: From protein structure to nanodisk assemblies

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

    Horejs, Christine; Pum, Dietmar; Sleytr, Uwe B.

    2010-11-07

    Surface layers (S-layers) are the most commonly observed cell surface structure of prokaryotic organisms. They are made up of proteins that spontaneously self-assemble into functional crystalline lattices in solution, on various solid surfaces, and interfaces. While classical experimental techniques failed to recover a complete structural model of an unmodified S-layer protein, small angle x-ray scattering (SAXS) provides an opportunity to study the structure of S-layer monomers in solution and of self-assembled two-dimensional sheets. For the protein under investigation we recently suggested an atomistic structural model by the use of molecular dynamics simulations. This structural model is now refined on themore » basis of SAXS data together with a fractal assembly approach. Here we show that a nondiluted critical system of proteins, which crystallize into monomolecular structures, might be analyzed by SAXS if protein-protein interactions are taken into account by relating a fractal local density distribution to a fractal local mean potential, which has to fulfill the Poisson equation. The present work demonstrates an important step into the elucidation of the structure of S-layers and offers a tool to analyze the structure of self-assembling systems in solution by means of SAXS and computer simulations.« less

  11. 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.

  12. In situ monitoring of laser-induced periodic surface structures formation on polymer films by grazing incidence small-angle X-ray scattering.

    PubMed

    Rebollar, Esther; Rueda, Daniel R; Martín-Fabiani, Ignacio; Rodríguez-Rodríguez, Álvaro; García-Gutiérrez, Mari-Cruz; Portale, Giuseppe; Castillejo, Marta; Ezquerra, Tiberio A

    2015-04-07

    The formation of laser-induced periodic surface structures (LIPSS) on model spin-coated polymer films has been followed in situ by grazing incidence small-angle X-ray scattering (GISAXS) using synchrotron radiation. The samples were irradiated at different repetition rates ranging from 1 up to 10 Hz by using the fourth harmonic of a Nd:YAG laser (266 nm) with pulses of 8 ns. Simultaneously, GISAXS patterns were acquired during laser irradiation. The variation of both the GISAXS signal with the number of pulses and the LIPSS period with laser irradiation time is revealing key kinetic aspects of the nanostructure formation process. By considering LIPSS as one-dimensional paracrystalline lattice and using a correlation found between the paracrystalline disorder parameter, g, and the number of reflections observed in the GISAXS patterns, the variation of the structural order of LIPSS can be assessed. The role of the laser repetition rate in the nanostructure formation has been clarified. For high pulse repetition rates (i.e., 10 Hz), LIPSS evolve in time to reach the expected period matching the wavelength of the irradiating laser. For lower pulse repetition rates LIPSS formation is less effective, and the period of the ripples never reaches the wavelength value. Results support and provide information on the existence of a feedback mechanism for LIPSS formation in polymer films.

  13. Small-angle X-Ray analysis of macromolecular structure: the structure of protein NS2 (NEP) in solution

    NASA Astrophysics Data System (ADS)

    Shtykova, E. V.; Bogacheva, E. N.; Dadinova, L. A.; Jeffries, C. M.; Fedorova, N. V.; Golovko, A. O.; Baratova, L. A.; Batishchev, O. V.

    2017-11-01

    A complex structural analysis of nuclear export protein NS2 (NEP) of influenza virus A has been performed using bioinformatics predictive methods and small-angle X-ray scattering data. The behavior of NEP molecules in a solution (their aggregation, oligomerization, and dissociation, depending on the buffer composition) has been investigated. It was shown that stable associates are formed even in a conventional aqueous salt solution at physiological pH value. For the first time we have managed to get NEP dimers in solution, to analyze their structure, and to compare the models obtained using the method of the molecular tectonics with the spatial protein structure predicted by us using the bioinformatics methods. The results of the study provide a new insight into the structural features of nuclear export protein NS2 (NEP) of the influenza virus A, which is very important for viral infection development.

  14. A liquid jet setup for x-ray scattering experiments on complex liquids at free-electron laser sources

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

    Steinke, I.; Lehmkühler, F., E-mail: felix.lehmkuehler@desy.de; Schroer, M. A.

    2016-06-15

    In this paper we describe a setup for x-ray scattering experiments on complex fluids using a liquid jet. The setup supports Small and Wide Angle X-ray Scattering (SAXS/WAXS) geometries. The jet is formed by a gas-dynamic virtual nozzle (GDVN) allowing for diameters ranging between 1 μm and 20 μm at a jet length of several hundred μm. To control jet properties such as jet length, diameter, or flow rate, the instrument is equipped with several diagnostic tools. Three microscopes are installed to quantify jet dimensions and stability in situ. The setup has been used at several beamlines performing both SAXSmore » and WAXS experiments. As a typical example we show an experiment on a colloidal dispersion in a liquid jet at the X-ray Correlation Spectroscopy instrument at the Linac Coherent Light Source free-electron laser.« less

  15. A liquid jet setup for x-ray scattering experiments on complex liquids at free-electron laser sources

    DOE PAGES

    Steinke, I.; Walther, M.; Lehmkühler, F.; ...

    2016-06-01

    In this study we describe a setup for x-ray scattering experiments on complex fluids using a liquid jet. The setup supports Small and Wide Angle X-ray Scattering (SAXS/WAXS) geometries. The jet is formed by a gas-dynamic virtual nozzle (GDVN) allowing for diameters ranging between 1 μm and 20 μm at a jet length of several hundred μm. To control jet properties such as jet length, diameter, or flow rate, the instrument is equipped with several diagnostic tools. Three microscopes are installed to quantify jet dimensions and stability in situ. The setup has been used at several beamlines performing both SAXSmore » and WAXS experiments. Finally, as a typical example we show an experiment on a colloidal dispersion in a liquid jet at the X-ray Correlation Spectroscopy instrument at the Linac Coherent Light Source free-electron laser.« less

  16. XUV and x-ray elastic scattering of attosecond electromagnetic pulses on atoms

    NASA Astrophysics Data System (ADS)

    Rosmej, F. B.; Astapenko, V. A.; Lisitsa, V. S.

    2017-12-01

    Elastic scattering of electromagnetic pulses on atoms in XUV and soft x-ray ranges is considered for ultra-short pulses. The inclusion of the retardation term, non-dipole interaction and an efficient scattering tensor approximation allowed studying the scattering probability in dependence of the pulse duration for different carrier frequencies. Numerical calculations carried out for Mg, Al and Fe atoms demonstrate that the scattering probability is a highly nonlinear function of the pulse duration and has extrema for pulse carrier frequencies in the vicinity of the resonance-like features of the polarization charge spectrum. Closed expressions for the non-dipole correction and the angular dependence of the scattered radiation are obtained.

  17. Spectral softening in the X-RAY afterglow of GRB 130925A as predicted by the dust scattering model

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

    Zhao, Yi-Nan; Shao, Lang, E-mail: lshao@hebtu.edu.cn

    2014-07-01

    Gamma-ray bursts (GRBs) usually occur in a dense star-forming region with a massive circumburst medium. The small-angle scattering of intense prompt X-ray emission off the surrounding dust grains will have observable consequences and sometimes can dominate the X-ray afterglow. In most of the previous studies, only the Rayleigh-Gans (RG) approximation is employed for describing the scattering process, which works accurately for the typical size of grains (with radius of a ≤ 0.1 μm) in the diffuse interstellar medium. When the size of the grains may significantly increase, as in a more dense region where GRBs would occur, the RG approximationmore » may not be valid enough for modeling detailed observational data. In order to study the temporal and spectral properties of the scattered X-ray emission more accurately with potentially larger dust grains, we provide a practical approach using the series expansions of anomalous diffraction (AD) approximation based on the complicated Mie theory. We apply our calculations to understand the puzzling X-ray afterglow of recently observed GRB 130925A that showed a significant spectral softening. We find that the X-ray scattering scenarios with either AD or RG approximation adopted could well reproduce both the temporal and spectral profile simultaneously. Given the plateau present in the early X-ray light curve, a typical distribution of smaller grains as in the interstellar medium would be suggested for GRB 130925A.« less

  18. Spectral Softening in the X-Ray Afterglow of GRB 130925A as Predicted by the Dust Scattering Model

    NASA Astrophysics Data System (ADS)

    Zhao, Yi-Nan; Shao, Lang

    2014-07-01

    Gamma-ray bursts (GRBs) usually occur in a dense star-forming region with a massive circumburst medium. The small-angle scattering of intense prompt X-ray emission off the surrounding dust grains will have observable consequences and sometimes can dominate the X-ray afterglow. In most of the previous studies, only the Rayleigh-Gans (RG) approximation is employed for describing the scattering process, which works accurately for the typical size of grains (with radius of a <= 0.1 μm) in the diffuse interstellar medium. When the size of the grains may significantly increase, as in a more dense region where GRBs would occur, the RG approximation may not be valid enough for modeling detailed observational data. In order to study the temporal and spectral properties of the scattered X-ray emission more accurately with potentially larger dust grains, we provide a practical approach using the series expansions of anomalous diffraction (AD) approximation based on the complicated Mie theory. We apply our calculations to understand the puzzling X-ray afterglow of recently observed GRB 130925A that showed a significant spectral softening. We find that the X-ray scattering scenarios with either AD or RG approximation adopted could well reproduce both the temporal and spectral profile simultaneously. Given the plateau present in the early X-ray light curve, a typical distribution of smaller grains as in the interstellar medium would be suggested for GRB 130925A.

  19. Heterodyne x-ray diffuse scattering from coherent phonons

    DOE PAGES

    Kozina, M.; Trigo, M.; Chollet, M.; ...

    2017-08-10

    Here in this paper, we report Fourier-transform inelastic x-ray scattering measurements of photoexcited GaAs with embedded ErAs nanoparticles. We observe temporal oscillations in the x-ray scattering intensity, which we attribute to inelastic scattering from coherent acoustic phonons. Unlike in thermal equilibrium, where inelastic x-ray scattering is proportional to the phonon occupation, we show that the scattering is proportional to the phonon amplitude for coherent states. The wavevectors of the observed phonons extend beyond the excitation wavevector. The nanoparticles break the discrete translational symmetry of the lattice, enabling the generation of large wavevector coherent phonons. Elastic scattering of x-ray photons frommore » the nanoparticles provides a reference for heterodyne mixing, yielding signals proportional to the phonon amplitude.« less

  20. Application of X-ray and neutron small angle scattering techniques to study the hierarchical structure of plant cell walls: a review.

    PubMed

    Martínez-Sanz, Marta; Gidley, Michael J; Gilbert, Elliot P

    2015-07-10

    Plant cell walls present an extremely complex structure of hierarchically assembled cellulose microfibrils embedded in a multi-component matrix. The biosynthesis process determines the mechanism of cellulose crystallisation and assembly, as well as the interaction of cellulose with other cell wall components. Thus, a knowledge of cellulose microfibril and bundle architecture, and the structural role of matrix components, is crucial for understanding cell wall functional and technological roles. Small angle scattering techniques, combined with complementary methods, provide an efficient approach to characterise plant cell walls, covering a broad and relevant size range while minimising experimental artefacts derived from sample treatment. Given the system complexity, approaches such as component extraction and the use of plant cell wall analogues are typically employed to enable the interpretation of experimental results. This review summarises the current research status on the characterisation of the hierarchical structure of plant cell walls using small angle scattering techniques. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

  1. Small-angle neutron scattering investigations of Co-doped iron oxide nanoparticles. Preliminary results

    NASA Astrophysics Data System (ADS)

    Creanga, Dorina; Balasoiu, Maria; Soloviov, Dmitro; Balasoiu-Gaina, Alexandra-Maria; Puscasu, Emil; Lupu, Nicoleta; Stan, Cristina

    2018-03-01

    Preliminary small-angle neutron scattering investigations on aqueous suspensions of several cobalt doped ferrites (CoxFe3-xO4, x=0; 0.5; 1) nanoparticles prepared by chemical co-precipitation method, are reported. The measurements were accomplished at the YuMO instrument in function at the IBR-2 reactor. Results of intermediary data treatment are presented and discussed.

  2. 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.

  3. Unravelling the shape and structural assembly of the photosynthetic GAPDH-CP12-PRK complex from Arabidopsis thaliana by small-angle X-ray scattering analysis.

    PubMed

    Del Giudice, Alessandra; Pavel, Nicolae Viorel; Galantini, Luciano; Falini, Giuseppe; Trost, Paolo; Fermani, Simona; Sparla, Francesca

    2015-12-01

    Oxygenic photosynthetic organisms produce sugars through the Calvin-Benson cycle, a metabolism that is tightly linked to the light reactions of photosynthesis and is regulated by different mechanisms, including the formation of protein complexes. Two enzymes of the cycle, glyceraldehyde-3-phosphate dehydrogenase (GAPDH) and phosphoribulokinase (PRK), form a supramolecular complex with the regulatory protein CP12 with the formula (GAPDH-CP122-PRK)2, in which both enzyme activities are transiently inhibited during the night. Small-angle X-ray scattering analysis performed on both the GAPDH-CP12-PRK complex and its components, GAPDH-CP12 and PRK, from Arabidopsis thaliana showed that (i) PRK has an elongated, bent and screwed shape, (ii) the oxidized N-terminal region of CP12 that is not embedded in the GAPDH-CP12 complex prefers a compact conformation and (iii) the interaction of PRK with the N-terminal region of CP12 favours the approach of two GAPDH tetramers. The interaction between the GAPDH tetramers may contribute to the overall stabilization of the GAPDH-CP12-PRK complex, the structure of which is presented here for the first time.

  4. Small-Angle X-Ray Scattering of the Cholesterol Incorporation into Human ApoA1-POPC Discoidal Particles

    PubMed Central

    Midtgaard, Søren Roi; Pedersen, Martin Cramer; Arleth, Lise

    2015-01-01

    Structural and functional aspects of high-density lipoproteins have been studied for over half a century. Due to the plasticity of this highly complex system, new aspects continue to be discovered. Here, we present a structural study of the human Apolipoprotein A1 (ApoA1) and investigate the role of its N-terminal domain, the so-called globular domain of ApoA1, in discoidal complexes with phospholipids and increasing amounts of cholesterol. Using a combination of solution-based small-angle x-ray scattering (SAXS) and molecular constrained data modeling, we show that the ApoA1-1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine (POPC)-based particles are disk shaped with an elliptical cross section and composed by a central lipid bilayer surrounded by two stabilizing ApoA1 proteins. This structure is very similar to the particles formed in the so-called nanodisc system, which is based on N-terminal truncated ApoA1 protein. Although it is commonly agreed that the nanodisc is plain disk shaped, several more advanced structures have been proposed for the full-length ApoA1 in combination with POPC and cholesterol. This prompted us to make a detailed comparative study of the ApoA1 and nanodisc systems upon cholesterol uptake. Based on the presented SAXS analysis it is found that the N-terminal domains of ApoA1-POPC-cholesterol particles are not globular but instead an integrated part of the protein belt stabilizing the particles. Upon incorporation of increasing amounts of cholesterol, the presence of the N-terminal domain allows the bilayer thickness to increase while maintaining an overall flat bilayer structure. This is contrasted by the energetically more strained and less favorable lens shape required to fit the SAXS data from the N-terminal truncated nanodisc system upon cholesterol incorporation. This suggests that the N-terminal domain of ApoA1 actively participates in the stabilization of the ApoA1-POPC-cholesterol discoidal particle and allows for a more optimal

  5. Focusing polycapillary to reduce parasitic scattering for inelastic x-ray measurements at high pressure

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

    Chow, P., E-mail: pchow@carnegiescience.edu; Xiao, Y. M.; Rod, E.

    2015-07-15

    The double-differential scattering cross-section for the inelastic scattering of x-ray photons from electrons is typically orders of magnitude smaller than that of elastic scattering. With samples 10-100 μm size in a diamond anvil cell at high pressure, the inelastic x-ray scattering signals from samples are obscured by scattering from the cell gasket and diamonds. One major experimental challenge is to measure a clean inelastic signal from the sample in a diamond anvil cell. Among the many strategies for doing this, we have used a focusing polycapillary as a post-sample optic, which allows essentially only scattered photons within its input fieldmore » of view to be refocused and transmitted to the backscattering energy analyzer of the spectrometer. We describe the modified inelastic x-ray spectrometer and its alignment. With a focused incident beam which matches the sample size and the field of view of polycapillary, at relatively large scattering angles, the polycapillary effectively reduces parasitic scattering from the diamond anvil cell gasket and diamonds. Raw data collected from the helium exciton measured by x-ray inelastic scattering at high pressure using the polycapillary method are compared with those using conventional post-sample slit collimation.« less

  6. Pt Catalyst Degradation in Aqueous and Fuel Cell Environments studied via In-Operando Anomalous Small-Angle X-ray Scattering

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

    Gilbert, James A.; Kariuki, Nancy N.; Wang, Xiaoping

    2015-08-01

    The evolution of Pt nanoparticle cathode electrocatalyst size distribution in a polymer electrolyte membrane fuel cell (PEMFC) was followed during accelerated stress tests using in-operando anomalous small-angle X-ray scattering (ASAXS). This evolution was compared to that observed in an aqueous electrolyte environment using stagnant electrolyte, flowing electrolyte, and flowing electrolyte at elevated temperature to reveal the different degradation trends in the PEMFC and aqueous environments and to determine the relevance of aqueous measurements to the stability of Pt nanoparticle catalyst in the fuel cell environment. The observed changes in the particle size distributions (PSDs) were analyzed to elucidate the extentmore » and mechanisms of particle growth and corresponding mass and active surface area losses in the different environments. These losses indicate a Pt nanoparticle surface area loss mechanism controlled by Pt dissolution, the particle size dependence of Pt dissolution, the loss of dissolved Pt into the membrane and electrolyte, and, to a lesser extent, the re-deposition of dissolved Pt onto larger particles. Based on the geometric surface area loss, mass loss, and mean particle size increase trends, the aqueous environment best reflecting the fuel cell environment was found to be one in which the electrolyte is flowing rather than stagnant. Pt nanoparticle surface area loss resulting from potential cycling can be inhibited by reducing the number of particles smaller than a critical particle diameter (CPD), which was found to be similar to 3.5 to similar to 4 nm, with the CPD dependent on both the cycling protocol (square wave vs triangle wave) and the catalyst environment (fuel cell, aqueous stagnant, aqueous flowing electrolyte, or elevated temperature flowing electrolyte)« less

  7. Structure and optical function of amorphous photonic nanostructures from avian feather barbs: a comparative small angle X-ray scattering (SAXS) analysis of 230 bird species

    PubMed Central

    Saranathan, Vinodkumar; Forster, Jason D.; Noh, Heeso; Liew, Seng-Fatt; Mochrie, Simon G. J.; Cao, Hui; Dufresne, Eric R.; Prum, Richard O.

    2012-01-01

    Non-iridescent structural colours of feathers are a diverse and an important part of the phenotype of many birds. These colours are generally produced by three-dimensional, amorphous (or quasi-ordered) spongy β-keratin and air nanostructures found in the medullary cells of feather barbs. Two main classes of three-dimensional barb nanostructures are known, characterized by a tortuous network of air channels or a close packing of spheroidal air cavities. Using synchrotron small angle X-ray scattering (SAXS) and optical spectrophotometry, we characterized the nanostructure and optical function of 297 distinctly coloured feathers from 230 species belonging to 163 genera in 51 avian families. The SAXS data provided quantitative diagnoses of the channel- and sphere-type nanostructures, and confirmed the presence of a predominant, isotropic length scale of variation in refractive index that produces strong reinforcement of a narrow band of scattered wavelengths. The SAXS structural data identified a new class of rudimentary or weakly nanostructured feathers responsible for slate-grey, and blue-grey structural colours. SAXS structural data provided good predictions of the single-scattering peak of the optical reflectance of the feathers. The SAXS structural measurements of channel- and sphere-type nanostructures are also similar to experimental scattering data from synthetic soft matter systems that self-assemble by phase separation. These results further support the hypothesis that colour-producing protein and air nanostructures in feather barbs are probably self-assembled by arrested phase separation of polymerizing β-keratin from the cytoplasm of medullary cells. Such avian amorphous photonic nanostructures with isotropic optical properties may provide biomimetic inspiration for photonic technology. PMID:22572026

  8. COSMIC-RAY PITCH-ANGLE SCATTERING IN IMBALANCED MHD TURBULENCE SIMULATIONS

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

    Weidl, Martin S.; Jenko, Frank; Teaca, Bogdan

    2015-09-20

    Pitch-angle scattering rates for cosmic-ray particles in MHD simulations with imbalanced turbulence are calculated for fully evolving electromagnetic turbulence. We compare with theoretical predictions derived from the quasilinear theory of cosmic-ray diffusion for an idealized slab spectrum and demonstrate how cross helicity affects the shape of the pitch-angle diffusion coefficient. Additional simulations in evolving magnetic fields or static field configurations provide evidence that the scattering anisotropy in imbalanced turbulence is not primarily due to coherence with propagating Alfvén waves, but an effect of the spatial structure of electric fields in cross-helical MHD turbulence.

  9. 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.

  10. The new NCPSS BL19U2 beamline at the SSRF for small-angle X-ray scattering from biological macromolecules in solution.

    PubMed

    Li, Na; Li, Xiuhong; Wang, Yuzhu; Liu, Guangfeng; Zhou, Ping; Wu, Hongjin; Hong, Chunxia; Bian, Fenggang; Zhang, Rongguang

    2016-10-01

    The beamline BL19U2 is located in the Shanghai Synchrotron Radiation Facility (SSRF) and is its first beamline dedicated to biological material small-angle X-ray scattering (BioSAXS). The electrons come from an undulator which can provide high brilliance for the BL19U2 end stations. A double flat silicon crystal (111) monochromator is used in BL19U2, with a tunable monochromatic photon energy ranging from 7 to 15 keV. To meet the rapidly growing demands of crystallographers, biochemists and structural biologists, the BioSAXS beamline allows manual and automatic sample loading/unloading. A Pilatus 1M detector (Dectris) is employed for data collection, characterized by a high dynamic range and a short readout time. The highly automated data processing pipeline SASFLOW was integrated into BL19U2, with help from the BioSAXS group of the European Molecular Biology Laboratory (EMBL, Hamburg), which provides a user-friendly interface for data processing. The BL19U2 beamline was officially opened to users in March 2015. To date, feedback from users has been positive and the number of experimental proposals at BL19U2 is increasing. A description of the new BioSAXS beamline and the setup characteristics is given, together with examples of data obtained.

  11. EUV-angle resolved scatter (EUV-ARS): a new tool for the characterization of nanometre structures

    NASA Astrophysics Data System (ADS)

    Fernández Herrero, Analía.; Mentzel, Heiko; Soltwisch, Victor; Jaroslawzew, Sina; Laubis, Christian; Scholze, Frank

    2018-03-01

    The advance of the semiconductor industry requires new metrology methods, which can deal with smaller and more complex nanostructures. Particularly for inline metrology a rapid, sensitive and non destructive method is needed. Small angle X-ray scattering under grazing incidence has already been investigated for this application and delivers significant statistical information which tracks the profile parameters as well as their variations, i.e. roughness. However, it suffers from the elongated footprint at the sample. The advantage of EUV radiation, with its longer wavelengths, is that larger incidence angles can be used, resulting in a significant reduction of the beam footprint. Targets with field sizes of 100 μm and smaller are accessible with our experimental set-up. We present a new experimental tool for the measurement of small structures based on the capabilities of soft X-ray and EUV scatterometry at the PTB soft X-ray beamline at the electron storage ring BESSY II. PTB's soft X-ray radiometry beamline uses a plane grating monochromator, which covers the spectral range from 0.7 nm to 25 nm and was especially designed to provide highly collimated radiation. An area detector covers the scattered radiation from a grazing exit angle up to an angle of 30° above the sample horizon and the fluorescence emission can be detected with an energy dispersive X-ray silicon drift detector. In addition, the sample can be rotated and linearly moved in vacuum. This new set-up will be used to explore the capabilities of EUV-scatterometry for the characterization of nanometre-sized structures.

  12. High resolution x-ray Thomson scattering measurements from cryogenic hydrogen jets using the linac coherent light source

    DOE PAGES

    Fletcher, L. B.; Zastrau, U.; Galtier, E.; ...

    2016-08-15

    Here, we present the first spectrally resolved measurements of x-rays scattered from cryogenic hydrogen jets in the single photon counting limit. The 120 Hz capabilities of the LCLS, together with a novel hydrogen jet design [J. B. Kim et al., Rev. Sci. Instrum. (these proceedings)], allow for the ability to record a near background free spectrum. Such high-dynamic-range x-ray scattering measurements enable a platform to study ultra-fast, laser-driven, heating dynamics of hydrogen plasmas. This measurement has been achieved using two highly annealed pyrolytic graphite crystal spectrometers to spectrally resolve 5.5 keV x-rays elastically and inelastically scattered from cryogenic hydrogen andmore » focused on Cornell-SLAC pixel array detectors [S. Herrmann et al., Nucl. Instrum. Methods Phys. Res., Sect. A 718, 550 (2013)].« less

  13. High resolution x-ray Thomson scattering measurements from cryogenic hydrogen jets using the linac coherent light source

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

    Fletcher, L. B., E-mail: lbfletch@slac.stanford.edu; Galtier, E.; Gamboa, E. J.

    2016-11-15

    We present the first spectrally resolved measurements of x-rays scattered from cryogenic hydrogen jets in the single photon counting limit. The 120 Hz capabilities of the LCLS, together with a novel hydrogen jet design [J. B. Kim et al., Rev. Sci. Instrum. (these proceedings)], allow for the ability to record a near background free spectrum. Such high-dynamic-range x-ray scattering measurements enable a platform to study ultra-fast, laser-driven, heating dynamics of hydrogen plasmas. This measurement has been achieved using two highly annealed pyrolytic graphite crystal spectrometers to spectrally resolve 5.5 keV x-rays elastically and inelastically scattered from cryogenic hydrogen and focusedmore » on Cornell-SLAC pixel array detectors [S. Herrmann et al., Nucl. Instrum. Methods Phys. Res., Sect. A 718, 550 (2013)].« less

  14. Synchrotron x-ray modification of nanoparticle superlattice formation

    NASA Astrophysics Data System (ADS)

    Lu, Chenguang; Akey, Austin J.; Herman, Irving P.

    2012-09-01

    The synchrotron x-ray radiation used to perform small angle x-ray scattering (SAXS) during the formation of three-dimensional nanoparticle superlattices by drop casting nanoparticle solutions affects the structure and the local crystalline order of the resulting films. The domain size decreases due to the real-time SAXS analysis during drying and more macroscopic changes are visible to the eye.

  15. X-ray Interferometry with Transmissive Beam Combiners for Ultra-High Angular Resolution Astronomy

    NASA Technical Reports Server (NTRS)

    Skinner, G. K.; Krismanic, John F.

    2009-01-01

    Abstract Interferometry provides one of the possible routes to ultra-high angular resolution for X-ray and gamma-ray astronomy. Sub-micro-arc-second angular resolution, necessary to achieve objectives such as imaging the regions around the event horizon of a super-massive black hole at the center of an active galaxy, can be achieved if beams from parts of the incoming wavefront separated by 100s of meters can be stably and accurately brought together at small angles. One way of achieving this is by using grazing incidence mirrors. We here investigate an alternative approach in which the beams are recombined by optical elements working in transmission. It is shown that the use of diffractive elements is a particularly attractive option. We report experimental results from a simple 2-beam interferometer using a low-cost commercially available profiled film as the diffractive elements. A rotationally symmetric filled (or mostly filled) aperture variant of such an interferometer, equivalent to an X-ray axicon, is shown to offer a much wider bandpass than either a Phase Fresnel Lens (PFL) or a PFL with a refractive lens in an achromatic pair. Simulations of an example system are presented.

  16. Development of an X-ray prism for a combined diffraction enhanced imaging and fluorescence imaging system

    NASA Astrophysics Data System (ADS)

    Bewer, Brian E.

    Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These X-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing a large change in intensity for a small angle change introduced by the X-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultra small angle X-ray scattering (USAXS) contrast thus improving visualization and extending the utility of X-ray imaging. To improve on the current DEI technique this body of work describes the design of an X-ray prism (XRP) included in the imaging system which allows the analyzer crystal to be aligned anywhere on the rocking curve without moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from muradians for direct mechanical movement of the analyzer crystal to milliradian control for movement the XRP angle. In addition to using an XRP for the traditional DEI acquisition method of two scans on opposite sides of the rocking curve preliminary tests will be presented showing the potential of using an XRP to scan quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single fast measurement thus removing the occurrence of motion artifacts for each point or line used during a scan. The XRP design is also intended to be compatible with combined imaging systems where more than one technique is used to investigate a sample. Candidates for complimentary techniques are investigated and measurements from a combined X-ray imaging system are presented.

  17. Recent applications of small-angle neutron scattering in strongly interacting soft condensed matter

    NASA Astrophysics Data System (ADS)

    Wignall, G. D.; Melnichenko, Y. B.

    2005-08-01

    Before the application of small-angle neutron scattering (SANS) to the study of polymer structure, chain conformation studies were limited to light and small-angle x-ray scattering techniques, usually conducted in dilute solution owing to the difficulties of separating the inter- and intrachain contributions to the structure. The unique role of neutron scattering in soft condensed matter arises from the difference in the coherent scattering length between deuterium (bD = 0.67 × 10-12 cm) and hydrogen (bH = -0.37 × 10-12 cm), which results in a marked difference in scattering power (contrast) between molecules synthesized from normal (hydrogeneous) and deuterated monomer units. Thus, deuterium labelling techniques may be used to 'stain' molecules and make them 'visible' in the condensed state and other crowded environments, such as concentrated solutions of overlapping chains. For over two decades, SANS has proved to be a powerful tool for studies of structure-property relationships in polymeric systems and has made it possible to extract unique information about their size, shape, conformational changes and molecular associations. These applications are now so numerous that an exhaustive review of the field is no longer practical, so the authors propose to focus on the use of SANS for studies of strongly interacting soft matter systems. This paper will therefore discuss basic theory and practical aspects of the technique and will attempt to explain the physics of scattering with the minimum of unnecessary detail and mathematical rigour. Examples will be given to demonstrate the power of SANS and to show how it has helped to unveil universal aspects of the behaviour of macromolecules in such apparently diverse systems as polymer solutions, blends, polyelectrolytes and supercritical mixtures. The aim of the authors is to aid potential users who have a general scientific background, but no specialist knowledge of scattering, to understand the potential of the

  18. Solution Structure of the 128 kDa Enzyme I Dimer from Escherichia coli and Its 146 kDa Complex with HPr Using Residual Dipolar Couplings and Small- and Wide-Angle X-ray Scattering

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

    Schwieters, Charles D.; Suh, Jeong-Yong; Grishaev, Alexander

    2010-09-17

    The solution structures of free Enzyme I (EI, {approx}128 kDa, 575 x 2 residues), the first enzyme in the bacterial phosphotransferase system, and its complex with HPr ({approx}146 kDa) have been solved using novel methodology that makes use of prior structural knowledge (namely, the structures of the dimeric EIC domain and the isolated EIN domain both free and complexed to HPr), combined with residual dipolar coupling (RDC), small- (SAXS) and wide- (WAXS) angle X-ray scattering and small-angle neutron scattering (SANS) data. The calculational strategy employs conjoined rigid body/torsion/Cartesian simulated annealing, and incorporates improvements in calculating and refining against SAXS/WAXS datamore » that take into account complex molecular shapes in the description of the solvent layer resulting in a better representation of the SAXS/WAXS data. The RDC data orient the symmetrically related EIN domains relative to the C{sub 2} symmetry axis of the EIC dimer, while translational, shape, and size information is provided by SAXS/WAXS. The resulting structures are independently validated by SANS. Comparison of the structures of the free EI and the EI-HPr complex with that of the crystal structure of a trapped phosphorylated EI intermediate reveals large ({approx}70-90{sup o}) hinge body rotations of the two subdomains comprising the EIN domain, as well as of the EIN domain relative to the dimeric EIC domain. These large-scale interdomain motions shed light on the structural transitions that accompany the catalytic cycle of EI.« less

  19. 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

  20. DNA conformations in mismatch repair probed in solution by X-ray scattering from gold nanocrystals

    PubMed Central

    Hura, Greg L.; Tsai, Chi-Lin; Claridge, Shelley A.; Mendillo, Marc L.; Smith, Jessica M.; Williams, Gareth J.; Mastroianni, Alexander J.; Alivisatos, A. Paul; Putnam, Christopher D.; Kolodner, Richard D.; Tainer, John A.

    2013-01-01

    DNA metabolism and processing frequently require transient or metastable DNA conformations that are biologically important but challenging to characterize. We use gold nanocrystal labels combined with small angle X-ray scattering to develop, test, and apply a method to follow DNA conformations acting in the Escherichia coli mismatch repair (MMR) system in solution. We developed a neutral PEG linker that allowed gold-labeled DNAs to be flash-cooled and stored without degradation in sample quality. The 1,000-fold increased gold nanocrystal scattering vs. DNA enabled investigations at much lower concentrations than otherwise possible to avoid concentration-dependent tetramerization of the MMR initiation enzyme MutS. We analyzed the correlation scattering functions for the nanocrystals to provide higher resolution interparticle distributions not convoluted by the intraparticle distribution. We determined that mispair-containing DNAs were bent more by MutS than complementary sequence DNA (csDNA), did not promote tetramer formation, and allowed MutS conversion to a sliding clamp conformation that eliminated the DNA bends. Addition of second protein responder MutL did not stabilize the MutS-bent forms of DNA. Thus, DNA distortion is only involved at the earliest mispair recognition steps of MMR: MutL does not trap bent DNA conformations, suggesting migrating MutL or MutS/MutL complexes as a conserved feature of MMR. The results promote a mechanism of mismatch DNA bending followed by straightening in initial MutS and MutL responses in MMR. We demonstrate that small angle X-ray scattering with gold labels is an enabling method to examine protein-induced DNA distortions key to the DNA repair, replication, transcription, and packaging. PMID:24101514

  1. An ultra-high vacuum chamber for scattering experiments featuring in-vacuum continuous in-plane variation of the angle between entrance and exit vacuum ports

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

    Englund, Carl-Johan; Agåker, Marcus, E-mail: marcus.agaker@physics.uu.se; Fredriksson, Pierre

    2015-09-15

    A concept that enables in-vacuum continuous variation of the angle between two ports in one plane has been developed and implemented. The vacuum chamber allows for measuring scattering cross sections as a function of scattering angle and is intended for resonant inelastic X-ray scattering experiments. The angle between the ports can be varied in the range of 30°-150°, while the pressure change is less than 2 × 10{sup −10} mbars.

  2. Monte Carlo calculation of large and small-angle electron scattering in air

    NASA Astrophysics Data System (ADS)

    Cohen, B. I.; Higginson, D. P.; Eng, C. D.; Farmer, W. A.; Friedman, A.; Grote, D. P.; Larson, D. J.

    2017-11-01

    A Monte Carlo method for angle scattering of electrons in air that accommodates the small-angle multiple scattering and larger-angle single scattering limits is introduced. The algorithm is designed for use in a particle-in-cell simulation of electron transport and electromagnetic wave effects in air. The method is illustrated in example calculations.

  3. Monte Carlo calculation of large and small-angle electron scattering in air

    DOE PAGES

    Cohen, B. I.; Higginson, D. P.; Eng, C. D.; ...

    2017-08-12

    A Monte Carlo method for angle scattering of electrons in air that accommodates the small-angle multiple scattering and larger-angle single scattering limits is introduced. In this work, the algorithm is designed for use in a particle-in-cell simulation of electron transport and electromagnetic wave effects in air. The method is illustrated in example calculations.

  4. Stimulated resonant x-ray Raman scattering with incoherent radiation

    NASA Astrophysics Data System (ADS)

    Weninger, Clemens; Rohringer, Nina

    2013-11-01

    We present a theoretical study on stimulated electronic Raman scattering in neon by resonant excitation with an x-ray free electron laser (XFEL). This study is in support of the recent experimental demonstration [C. Weninger , Phys. Rev. Lett. (to be published)] of stimulated x-ray Raman scattering. Focusing the broadband XFEL pulses into a cell of neon gas at atmospheric pressure a strong inelastic x-ray scattering signal in the forward direction was observed, as the x-ray energy was varied across the region of core-excited Rydberg states and the K edge. The broadband and intrinsically incoherent x-ray pulses from the XFEL lead to a rich, structured line shape of the scattered radiation. We present a generalized Maxwell-Liouville-von Neumann approach to self-consistently solve for the amplification of the scattered radiation along with the time evolution of the density matrix of the atomic and residual ionic system. An in-depth analysis of the evolution of the emission spectra as a function of the Raman gain is presented. Furthermore, we propose the use of statistical methods to obtain high-resolution scattering data beyond the lifetime broadening despite pumping with incoherent x-ray pulses.

  5. Theoretical modeling of multiprotein complexes by iSPOT: Integration of small-angle X-ray scattering, hydroxyl radical footprinting, and computational docking.

    PubMed

    Huang, Wei; Ravikumar, Krishnakumar M; Parisien, Marc; Yang, Sichun

    2016-12-01

    Structural determination of protein-protein complexes such as multidomain nuclear receptors has been challenging for high-resolution structural techniques. Here, we present a combined use of multiple biophysical methods, termed iSPOT, an integration of shape information from small-angle X-ray scattering (SAXS), protection factors probed by hydroxyl radical footprinting, and a large series of computationally docked conformations from rigid-body or molecular dynamics (MD) simulations. Specifically tested on two model systems, the power of iSPOT is demonstrated to accurately predict the structures of a large protein-protein complex (TGFβ-FKBP12) and a multidomain nuclear receptor homodimer (HNF-4α), based on the structures of individual components of the complexes. Although neither SAXS nor footprinting alone can yield an unambiguous picture for each complex, the combination of both, seamlessly integrated in iSPOT, narrows down the best-fit structures that are about 3.2Å and 4.2Å in RMSD from their corresponding crystal structures, respectively. Furthermore, this proof-of-principle study based on the data synthetically derived from available crystal structures shows that the iSPOT-using either rigid-body or MD-based flexible docking-is capable of overcoming the shortcomings of standalone computational methods, especially for HNF-4α. By taking advantage of the integration of SAXS-based shape information and footprinting-based protection/accessibility as well as computational docking, this iSPOT platform is set to be a powerful approach towards accurate integrated modeling of many challenging multiprotein complexes. Copyright © 2016 Elsevier Inc. All rights reserved.

  6. Small angle X-ray scattering as a high-throughput method to classify antimicrobial modes of action.

    PubMed

    von Gundlach, A R; Garamus, V M; Gorniak, T; Davies, H A; Reischl, M; Mikut, R; Hilpert, K; Rosenhahn, A

    2016-05-01

    Multi-drug resistant bacteria are currently undermining our health care system worldwide. While novel antimicrobial drugs, such as antimicrobial peptides, are urgently needed, identification of new modes of action is money and time consuming, and in addition current approaches are not available in a high throughput manner. Here we explore how small angle X-ray scattering (SAXS) as high throughput method can contribute to classify the mode of action for novel antimicrobials and therefore supports fast decision making in drug development. Using data bases for natural occurring antimicrobial peptides or predicting novel artificial peptides, many candidates can be discovered that will kill a selected target bacterium. However, in order to narrow down the selection it is important to know if these peptides follow all the same mode of action. In addition, the mode of action should be different from conventional antibiotics, in consequence peptide candidates can be developed further into drugs against multi-drug resistant bacteria. Here we used one short antimicrobial peptide with unknown mode of action and compared the ultrastructural changes of Escherichia coli cells after treatment with the peptide to cells treated with classic antibiotics. The key finding is that SAXS as a structure sensitive tool provides a rapid feedback on drug induced ultrastructural alterations in whole E. coli cells. We could demonstrate that ultrastructural changes depend on the used antibiotics and their specific mode of action. This is demonstrated using several well characterized antimicrobial compounds and the analysis of resulting SAXS curves by principal component analysis. To understand the result of the PCA analysis, the data is correlated with TEM images. In contrast to real space imaging techniques, SAXS allows to obtain nanoscale information averaged over approximately one million cells. The measurement takes only seconds, while conventional tests to identify a mode of action require

  7. Development study of the X-ray scattering properties of a group of optically polished flat samples

    NASA Technical Reports Server (NTRS)

    Froechtenigt, J. F.

    1973-01-01

    A group of twelve optically polished flat samples were used to study the scattering of X-rays. The X-ray beam reflected from the twelve optical flat samples was analyzed by means of a long vacuum system of special design for these tests. The scattering measurements were made at 8.34A and 0.92 deg angle of incidence. The results for ten of the samples are comparable, the two exceptions being the fire polished samples.

  8. Small-angle X-ray Solution Scattering Study of the Multi-aminoacyl-tRNA Synthetase Complex Reveals an Elongated and Multi-armed particle*

    PubMed Central

    Dias, José; Renault, Louis; Pérez, Javier; Mirande, Marc

    2013-01-01

    In animal cells, nine aminoacyl-tRNA synthetases are associated with the three auxiliary proteins p18, p38, and p43 to form a stable and conserved large multi-aminoacyl-tRNA synthetase complex (MARS), whose molecular mass has been proposed to be between 1.0 and 1.5 MDa. The complex acts as a molecular hub for coordinating protein synthesis and diverse regulatory signal pathways. Electron microscopy studies defined its low resolution molecular envelope as an overall rather compact, asymmetric triangular shape. Here, we have analyzed the composition and homogeneity of the native mammalian MARS isolated from rabbit liver and characterized its overall internal structure, size, and shape at low resolution by hydrodynamic methods and small-angle x-ray scattering in solution. Our data reveal that the MARS exhibits a much more elongated and multi-armed shape than expected from previous reports. The hydrodynamic and structural features of the MARS are large compared with other supramolecular assemblies involved in translation, including ribosome. The large dimensions and non-compact structural organization of MARS favor a large protein surface accessibility for all its components. This may be essential to allow structural rearrangements between the catalytic and cis-acting tRNA binding domains of the synthetases required for binding the bulky tRNA substrates. This non-compact architecture may also contribute to the spatiotemporal controlled release of some of its components, which participate in non-canonical functions after dissociation from the complex. PMID:23836901

  9. Small-angle X-ray solution scattering study of the multi-aminoacyl-tRNA synthetase complex reveals an elongated and multi-armed particle.

    PubMed

    Dias, José; Renault, Louis; Pérez, Javier; Mirande, Marc

    2013-08-16

    In animal cells, nine aminoacyl-tRNA synthetases are associated with the three auxiliary proteins p18, p38, and p43 to form a stable and conserved large multi-aminoacyl-tRNA synthetase complex (MARS), whose molecular mass has been proposed to be between 1.0 and 1.5 MDa. The complex acts as a molecular hub for coordinating protein synthesis and diverse regulatory signal pathways. Electron microscopy studies defined its low resolution molecular envelope as an overall rather compact, asymmetric triangular shape. Here, we have analyzed the composition and homogeneity of the native mammalian MARS isolated from rabbit liver and characterized its overall internal structure, size, and shape at low resolution by hydrodynamic methods and small-angle x-ray scattering in solution. Our data reveal that the MARS exhibits a much more elongated and multi-armed shape than expected from previous reports. The hydrodynamic and structural features of the MARS are large compared with other supramolecular assemblies involved in translation, including ribosome. The large dimensions and non-compact structural organization of MARS favor a large protein surface accessibility for all its components. This may be essential to allow structural rearrangements between the catalytic and cis-acting tRNA binding domains of the synthetases required for binding the bulky tRNA substrates. This non-compact architecture may also contribute to the spatiotemporal controlled release of some of its components, which participate in non-canonical functions after dissociation from the complex.

  10. Recent advances in the UltraScan SOlution MOdeller (US-SOMO) hydrodynamic and small-angle scattering data analysis and simulation suite.

    PubMed

    Brookes, Emre; Rocco, Mattia

    2018-03-28

    The UltraScan SOlution MOdeller (US-SOMO) is a comprehensive, public domain, open-source suite of computer programs centred on hydrodynamic modelling and small-angle scattering (SAS) data analysis and simulation. We describe here the advances that have been implemented since its last official release (#3087, 2017), which are available from release #3141 for Windows, Linux and Mac operating systems. A major effort has been the transition from the legacy Qt3 cross platform software development and user interface library to the modern Qt5 release. Apart from improved graphical support, this has allowed the direct implementation of the newest, almost two-orders of magnitude faster version of the ZENO hydrodynamic computation algorithm for all operating systems. Coupled with the SoMo-generated bead models with overlaps, ZENO provides the most accurate translational friction computations from atomic-level structures available (Rocco and Byron Eur Biophys J 44:417-431, 2015a), with computational times comparable with or faster than those of other methods. In addition, it has allowed us to introduce the direct representation of each atom in a structure as a (hydrated) bead, opening interesting new modelling possibilities. In the small-angle scattering (SAS) part of the suite, an indirect Fourier transform Bayesian algorithm has been implemented for the computation of the pairwise distance distribution function from SAS data. Finally, the SAS HPLC module, recently upgraded with improved baseline correction and Gaussian decomposition of not baseline-resolved peaks and with advanced statistical evaluation tools (Brookes et al. J Appl Cryst 49:1827-1841, 2016), now allows automatic top-peak frame selection and averaging.

  11. High-resolution soft X-ray beamline ADRESS at the Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies

    PubMed Central

    Strocov, V. N.; Schmitt, T.; Flechsig, U.; Schmidt, T.; Imhof, A.; Chen, Q.; Raabe, J.; Betemps, R.; Zimoch, D.; Krempasky, J.; Wang, X.; Grioni, M.; Piazzalunga, A.; Patthey, L.

    2010-01-01

    The concepts and technical realisation of the high-resolution soft X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for resonant inelastic X-ray scattering (RIXS) and angle-resolved photoelectron spectroscopy (ARPES) are described. The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0–180° rotatable linear polarizations) but also the energy without changing the gap. The beamline optics is based on the well established scheme of plane-grating monochromator operating in collimated light. The ultimate resolving power E/ΔE is above 33000 at 1 keV photon energy. The choice of blazed versus lamellar gratings and optimization of their profile parameters is described. Owing to glancing angles on the mirrors as well as optimized groove densities and profiles of the gratings, the beamline is capable of delivering high photon flux up to 1 × 1013 photons s−1 (0.01% BW)−1 at 1 keV. Ellipsoidal refocusing optics used for the RIXS endstation demagnifies the vertical spot size down to 4 µm, which allows slitless operation and thus maximal transmission of the high-resolution RIXS spectrometer delivering E/ΔE > 11000 at 1 keV photon energy. Apart from the beamline optics, an overview of the control system is given, the diagnostics and software tools are described, and strategies used for the optical alignment are discussed. An introduction to the concepts and instrumental realisation of the ARPES and RIXS endstations is given. PMID:20724785

  12. The Soft X-ray View of Ultra Fast Outflows

    NASA Astrophysics Data System (ADS)

    Reeves, J.; Braito, V.; Nardini, E.; Matzeu, G.; Lobban, A.; Costa, M.; Pounds, K.; Tombesi, F.; Behar, E.

    2017-10-01

    The recent large XMM-Newton programmes on the nearby quasars PDS 456 and PG 1211+143 have revealed prototype ultra fast outflows in the iron K band through highly blue shifted absorption lines. The wind velocities are in excess of 0.1c and are likely to make a significant contribution to the host galaxy feedback. Here we present evidence for the signature of the fast wind in the soft X-ray band from these luminous quasars, focusing on the spectroscopy with the RGS. In PDS 456, the RGS spectra reveal the presence of soft X-ray broad absorption line profiles, which suggests that PDS 456 is an X-ray equivalent to the BAL quasars, with outflow velocities reaching 0.2c. In PG 1211, the soft X-ray RGS spectra show a complex of several highly blue shifted absorption lines over a wide range of ionisation and reveal outflowing components with velocities between 0.06-0.17c. For both quasars, the soft X-ray absorption is highly variable, even on timescales of days and is most prominent when the quasar flux is low. Overall the results imply the presence of a soft X-ray component of the ultra fast outflows, which we attribute to a clumpy or inhomogeneous phase of the disk wind.

  13. T-REX: Thomson-Radiated Extreme X-rays Moving X-Ray Science into the ''Nuclear'' Applications Space with Thompson Scattered Photons

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

    Barty, C P; Hartemann, F V

    2004-09-21

    The scattering of laser photons from relativistic electrons (Thomson scattering) has been demonstrated to be a viable method for the production of ultrashort-duration pulses of tunable radiation in the 10-keV to 100-keV range. Photons in this range are capable of exciting or ionizing even the most tightly bound of atomic electrons. A wide variety of atomistic scale applications are possible. For example, Thomson x-ray sources have been constructed at LLNL (PLEIADES) and LBL as picosecond, stroboscopic probes of atomic-scale dynamics and at Vanderbilt University as element-specific tools for medical radiography and radiology. While these sources have demonstrated an attractive abilitymore » to simultaneously probe on an atomic spatial and temporal scale, they do not necessarily exploit the full potential of the Thomson scattering process to produce high-brightness, high-energy photons. In this white paper, we suggest that the peak brightness of Thomson sources can scale as fast as the 4th power of electron beam energy and that production via Thomson scattering of quasi-monochromatic, tunable radiation in the ''nuclear-range'' between 100-keV and several MeV is potentially a much more attractive application space for this process. Traditional sources in this regime are inherently ultra-broadband and decline rapidly in brightness as a function of photon energy. The output from dedicated, national-laboratory-scale, synchrotron facilities, e.g. APS, SPring8, ESRF etc., declines by more than 10 orders from 100 keV to 1 MeV. At 1 MeV, we conservatively estimate that Thomson-source, peak brightness can exceed that of APS (the best machine in the DOE complex) by more than 15 orders of magnitude. In much the same way that tunable lasers revolutionized atomic spectroscopy, this ''Peta-step'' advance in tunable, narrow-bandwidth, capability should enable entirely new fields of study and new, programmatically-interesting, applications such as: micrometer

  14. Coherent X-ray Scattering from Liquid-Air Interfaces

    NASA Astrophysics Data System (ADS)

    Shpyrko, Oleg

    Advances in synchrotron x-ray scattering techniques allow studies of structure and dynamics of liquid surfaces with unprecedented resolution. I will review x-ray scattering measurements of thermally excited capillary fluctuations in liquids, thin polymer liquid films and polymer surfaces in confined geometry. X-ray Diffuse scattering profile due to Debye-Waller like roughening of the surface allows to probe the distribution of capillary fluctuations over a wide range of length scales, while using X-ray Photon Correlation Spectroscopy (XPCS) one is able to directly couple to nanoscale dynamics of these surface fluctuations, over a wide range of temporal and spacial scales. I will also discuss recent XPCS measurements of lateral diffusion dynamics in Langmuir monolayers assembled at the liquid-air interface. This research was supported by NSF CAREER Grant 0956131.

  15. Operational properties of fluctuation X-ray scattering data

    DOE PAGES

    Malmerberg, Erik; Kerfeld, Cheryl A.; Zwart, Petrus H.

    2015-03-20

    X-ray scattering images collected on timescales shorter than rotation diffusion times using a (partially) coherent beam result in a significant increase in information content in the scattered data. These measurements, named fluctuation X-ray scattering (FXS), are typically performed on an X-ray free-electron laser (XFEL) and can provide fundamental insights into the structure of biological molecules, engineered nanoparticles or energy-related mesoscopic materials beyond what can be obtained with standard X-ray scattering techniques. In order to understand, use and validate experimental FXS data, the availability of basic data characteristics and operational properties is essential, but has been absent up to this point.more » In this communication, an intuitive view of the nature of FXS data and their properties is provided, the effect of FXS data on the derived structural models is highlighted, and generalizations of the Guinier and Porod laws that can ultimately be used to plan experiments and assess the quality of experimental data are presented.« less

  16. POLIX: A Thomson X-ray polarimeter for a small satellite mission

    NASA Astrophysics Data System (ADS)

    Paul, Biswajit; Gopala Krishna, M. R.; Puthiya Veetil, Rishin

    2016-07-01

    POLIX is a Thomson X-ray polarimeter for a small satellite mission of ISRO. The instrument consists of a collimator, a scatterer and a set proportional counters to detect the scattered X-rays. We will describe the design, specifications, sensitivity, and development status of this instrument and some of the important scientific goals. This instrument will provide unprecedented opportunity to measure X-ray polarisation in the medium energy range in a large number of sources of different classes with a minimum detectable linear polarisation degree of 2-3%. The prime objects for observation with this instrument are the X-ray bright accretion powered neutron stars, accreting black holes in different spectral states, rotation powered pulsars, magnetars, and active galactic nuclei. This instrument will be a bridge between the soft X-ray polarimeters and the Compton polarimeters.

  17. Structure of Poly(dialkylsiloxane) Melts:  Comparisons of Wide-Angle X-ray Scattering, Molecular Dynamics Simulations, and Integral Equation Theory

    DOE PAGES

    Habenschuss, Anton; Tsige, Mesfin; Curro, John G.; ...

    2007-08-21

    Here, wide-angle X-ray scattering, molecular dynamics (MD) simulations, and integral equation theory are used to study the structure of poly(diethylsiloxane) (PDES), poly(ethylmethylsiloxane) (PEMS), and poly(dimethylsiloxane) (PDMS) melts. The structure functions of PDES, PEMS, and PDMS are similar, but systematic trends in the intermolecular packing are observed. The local intramolecular structure is extracted from the experimental structure functions. The bond distances and bond angles obtained, including the large Si-O-Si angle, are in good agreement with the explicit atom (EA) and united atom (UA) potentials used in the simulations and theory and from other sources. Very good agreement is found between themore » MD simulations using the EA potentials and the experimental scattering results. Good agreement is also found between the polymer reference interaction site model (PRISM theory) and the UA MD simulations. The intermolecular structure is examined experimentally using an appropriately weighted radial distribution function and with theory and simulation using intermolecular site/site pair correlation functions. Finally, experiment, simulation, and theory show systematic increases in the chain/chain packing distances in the siloxanes as the number of sites in the pendant side chains is increased.« less

  18. High performance x-ray anti-scatter grid

    DOEpatents

    Logan, Clinton M.

    1995-01-01

    An x-ray anti-scatter grid for x-ray imaging, particularly for screening mammography, and method for fabricating same, x-rays incident along a direct path pass through a grid composed of a plurality of parallel or crossed openings, microchannels, grooves, or slots etched in a substrate, such as silicon, having the walls of the microchannels or slots coated with a high opacity material, such as gold, while x-rays incident at angels with respect to the slots of the grid, arising from scatter, are blocked. The thickness of the substrate is dependent on the specific application of the grid, whereby a substrate of the grid for mammography would be thinner than one for chest radiology. Instead of coating the walls of the slots, such could be filed with an appropriate liquid, such as mercury.

  19. Evolution of elastic x-ray scattering in laser-shocked warm dense lithium.

    PubMed

    Kugland, N L; Gregori, G; Bandyopadhyay, S; Brenner, C M; Brown, C R D; Constantin, C; Glenzer, S H; Khattak, F Y; Kritcher, A L; Niemann, C; Otten, A; Pasley, J; Pelka, A; Roth, M; Spindloe, C; Riley, D

    2009-12-01

    We have studied the dynamics of warm dense Li with near-elastic x-ray scattering. Li foils were heated and compressed using shock waves driven by 4-ns-long laser pulses. Separate 1-ns-long laser pulses were used to generate a bright source of 2.96 keV Cl Ly- alpha photons for x-ray scattering, and the spectrum of scattered photons was recorded at a scattering angle of 120 degrees using a highly oriented pyrolytic graphite crystal operated in the von Hamos geometry. A variable delay between the heater and backlighter laser beams measured the scattering time evolution. Comparison with radiation-hydrodynamics simulations shows that the plasma is highly coupled during the first several nanoseconds, then relaxes to a moderate coupling state at later times. Near-elastic scattering amplitudes have been successfully simulated using the screened one-component plasma model. Our main finding is that the near-elastic scattering amplitudes are quite sensitive to the mean ionization state Z[over ] and by extension to the choice of ionization model in the radiation-hydrodynamics simulations used to predict plasma properties within the shocked Li.

  20. Combined evaluation of grazing incidence X-ray fluorescence and X-ray reflectivity data for improved profiling of ultra-shallow depth distributions☆

    PubMed Central

    Ingerle, D.; Meirer, F.; Pepponi, G.; Demenev, E.; Giubertoni, D.; Wobrauschek, P.; Streli, C.

    2014-01-01

    The continuous downscaling of the process size for semiconductor devices pushes the junction depths and consequentially the implantation depths to the top few nanometers of the Si substrate. This motivates the need for sensitive methods capable of analyzing dopant distribution, total dose and possible impurities. X-ray techniques utilizing the external reflection of X-rays are very surface sensitive, hence providing a non-destructive tool for process analysis and control. X-ray reflectometry (XRR) is an established technique for the characterization of single- and multi-layered thin film structures with layer thicknesses in the nanometer range. XRR spectra are acquired by varying the incident angle in the grazing incidence regime while measuring the specular reflected X-ray beam. The shape of the resulting angle-dependent curve is correlated to changes of the electron density in the sample, but does not provide direct information on the presence or distribution of chemical elements in the sample. Grazing Incidence XRF (GIXRF) measures the X-ray fluorescence induced by an X-ray beam incident under grazing angles. The resulting angle dependent intensity curves are correlated to the depth distribution and mass density of the elements in the sample. GIXRF provides information on contaminations, total implanted dose and to some extent on the depth of the dopant distribution, but is ambiguous with regard to the exact distribution function. Both techniques use similar measurement procedures and data evaluation strategies, i.e. optimization of a sample model by fitting measured and calculated angle curves. Moreover, the applied sample models can be derived from the same physical properties, like atomic scattering/form factors and elemental concentrations; a simultaneous analysis is therefore a straightforward approach. This combined analysis in turn reduces the uncertainties of the individual techniques, allowing a determination of dose and depth profile of the implanted

  1. Small angle X-ray scattering and cross-linking for data assisted protein structure prediction in CASP 12 with prospects for improved accuracy.

    PubMed

    Ogorzalek, Tadeusz L; Hura, Greg L; Belsom, Adam; Burnett, Kathryn H; Kryshtafovych, Andriy; Tainer, John A; Rappsilber, Juri; Tsutakawa, Susan E; Fidelis, Krzysztof

    2018-03-01

    Experimental data offers empowering constraints for structure prediction. These constraints can be used to filter equivalently scored models or more powerfully within optimization functions toward prediction. In CASP12, Small Angle X-ray Scattering (SAXS) and Cross-Linking Mass Spectrometry (CLMS) data, measured on an exemplary set of novel fold targets, were provided to the CASP community of protein structure predictors. As solution-based techniques, SAXS and CLMS can efficiently measure states of the full-length sequence in its native solution conformation and assembly. However, this experimental data did not substantially improve prediction accuracy judged by fits to crystallographic models. One issue, beyond intrinsic limitations of the algorithms, was a disconnect between crystal structures and solution-based measurements. Our analyses show that many targets had substantial percentages of disordered regions (up to 40%) or were multimeric or both. Thus, solution measurements of flexibility and assembly support variations that may confound prediction algorithms trained on crystallographic data and expecting globular fully-folded monomeric proteins. Here, we consider the CLMS and SAXS data collected, the information in these solution measurements, and the challenges in incorporating them into computational prediction. As improvement opportunities were only partly realized in CASP12, we provide guidance on how data from the full-length biological unit and the solution state can better aid prediction of the folded monomer or subunit. We furthermore describe strategic integrations of solution measurements with computational prediction programs with the aim of substantially improving foundational knowledge and the accuracy of computational algorithms for biologically-relevant structure predictions for proteins in solution. © 2018 Wiley Periodicals, Inc.

  2. Scattering from fractals

    NASA Astrophysics Data System (ADS)

    Hurd, Alan J.

    The realization that structures in Nature often can be described by Mandelbrot's fractals has led to a revolution in many areas of physics. The interaction of waves with fractal systems has, understandably, become intensely studied since scattering is the method of choice to probe delicate fractal structures such as chainlike particle aggregates. Not all of these waves are electromagnetic. Neutron scattering, for example, is an important complementary tool to structural studies by X-ray and light scattering. Since the phenomenology of small-angle neutron scattering (SANS), as it is applied to fractal systems, is identical to that of small-angle X-ray scattering (SAXS), it falls within the scope of this paper.

  3. High performance x-ray anti-scatter grid

    DOEpatents

    Logan, C.M.

    1995-05-23

    Disclosed are an x-ray anti-scatter grid for x-ray imaging, particularly for screening mammography, and method for fabricating same, x-rays incident along a direct path pass through a grid composed of a plurality of parallel or crossed openings, microchannels, grooves, or slots etched in a substrate, such as silicon, having the walls of the microchannels or slots coated with a high opacity material, such as gold, while x-rays incident at angels with respect to the slots of the grid, arising from scatter, are blocked. The thickness of the substrate is dependent on the specific application of the grid, whereby a substrate of the grid for mammography would be thinner than one for chest radiology. Instead of coating the walls of the slots, such could be filed with an appropriate liquid, such as mercury. 4 Figs.

  4. Structure of the bifunctional aminoglycoside-resistance enzyme AAC(6')-Ie-APH(2'')-Ia revealed by crystallographic and small-angle X-ray scattering analysis.

    PubMed

    Smith, Clyde A; Toth, Marta; Weiss, Thomas M; Frase, Hilary; Vakulenko, Sergei B

    2014-10-01

    Broad-spectrum resistance to aminoglycoside antibiotics in clinically important Gram-positive staphylococcal and enterococcal pathogens is primarily conferred by the bifunctional enzyme AAC(6')-Ie-APH(2'')-Ia. This enzyme possesses an N-terminal coenzyme A-dependent acetyltransferase domain [AAC(6')-Ie] and a C-terminal GTP-dependent phosphotransferase domain [APH(2'')-Ia], and together they produce resistance to almost all known aminoglycosides in clinical use. Despite considerable effort over the last two or more decades, structural details of AAC(6')-Ie-APH(2'')-Ia have remained elusive. In a recent breakthrough, the structure of the isolated C-terminal APH(2'')-Ia enzyme was determined as the binary Mg2GDP complex. Here, the high-resolution structure of the N-terminal AAC(6')-Ie enzyme is reported as a ternary kanamycin/coenzyme A abortive complex. The structure of the full-length bifunctional enzyme has subsequently been elucidated based upon small-angle X-ray scattering data using the two crystallographic models. The AAC(6')-Ie enzyme is joined to APH(2'')-Ia by a short, predominantly rigid linker at the N-terminal end of a long α-helix. This α-helix is in turn intrinsically associated with the N-terminus of APH(2'')-Ia. This structural arrangement supports earlier observations that the presence of the intact α-helix is essential to the activity of both functionalities of the full-length AAC(6')-Ie-APH(2'')-Ia enzyme.

  5. Cryogenic x-ray diffraction microscopy utilizing high-pressure cryopreservation

    NASA Astrophysics Data System (ADS)

    Lima, Enju; Chushkin, Yuriy; van der Linden, Peter; Kim, Chae Un; Zontone, Federico; Carpentier, Philippe; Gruner, Sol M.; Pernot, Petra

    2014-10-01

    We present cryo x-ray diffraction microscopy of high-pressure-cryofixed bacteria and report high-convergence imaging with multiple image reconstructions. Hydrated D. radiodurans cells were cryofixed at 200 MPa pressure into ˜10-μm-thick water layers and their unstained, hydrated cellular environments were imaged by phasing diffraction patterns, reaching sub-30-nm resolutions with hard x-rays. Comparisons were made with conventional ambient-pressure-cryofixed samples, with respect to both coherent small-angle x-ray scattering and the image reconstruction. The results show a correlation between the level of background ice signal and phasing convergence, suggesting that phasing difficulties with frozen-hydrated specimens may be caused by high-background ice scattering.

  6. Generation of first hard X-ray pulse at Tsinghua Thomson Scattering X-ray Source.

    PubMed

    Du, Yingchao; Yan, Lixin; Hua, Jianfei; Du, Qiang; Zhang, Zhen; Li, Renkai; Qian, Houjun; Huang, Wenhui; Chen, Huaibi; Tang, Chuanxiang

    2013-05-01

    Tsinghua Thomson Scattering X-ray Source (TTX) is the first-of-its-kind dedicated hard X-ray source in China based on the Thomson scattering between a terawatt ultrashort laser and relativistic electron beams. In this paper, we report the experimental generation and characterization of the first hard X-ray pulses (51.7 keV) via head-on collision of an 800 nm laser and 46.7 MeV electron beams. The measured yield is 1.0 × 10(6) per pulse with an electron bunch charge of 200 pC and laser pulse energy of 300 mJ. The angular intensity distribution and energy spectra of the X-ray pulse are measured with an electron-multiplying charge-coupled device using a CsI scintillator and silicon attenuators. These measurements agree well with theoretical and simulation predictions. An imaging test using the X-ray pulse at the TTX is also presented.

  7. Studying Dust Scattering Halos with Galactic X-ray Binaries

    NASA Astrophysics Data System (ADS)

    Beeler, Doreen; Corrales, Lia; Heinz, Sebastian

    2018-01-01

    Dust is an important part of the interstellar medium (ISM) and contributes to the formation of stars and planets. Since the advent of modern X-ray telescopes, Galactic X-ray point sources have permitted a closer look at all phases of the ISM. Interstellar metals from oxygen to iron — in both gas and dust form — are responsible for absorption and scattering of X-ray light. Dust scatters the light in a forward direction and creates a diffuse halo image surrounding many bright Galactic X-ray binaries. We use all the bright X-ray point sources available in the Chandra HETG archive to study dust scattering halos from the local ISM. We have described a data analysis pipeline using a combination of the data reduction software CIAO and Python. We compare our results from Chandra HETG and ACIS-I observations of a well studied dust scattering halo around GX 13+1, in order to characterize any systematic errors associated with the HETG data set. We describe how our data products will be used to measure ISM scaling relations for X-ray extinction, dust abundance, and dust-to-metal ratios.

  8. Small-angle x-ray scattering from lipid bilayers is well described by modified Caillé theory but not by paracrystalline theory.

    PubMed Central

    Zhang, R; Tristram-Nagle, S; Sun, W; Headrick, R L; Irving, T C; Suter, R M; Nagle, J F

    1996-01-01

    X-ray scattering data at high instrumental resolution are reported for multilamellar vesicles of L alpha phase lipid bilayers of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine at 50 degrees C under varying osmotic pressure. The data are fitted to two theories that account for noncrystalline disorder, paracrystalline theory (PT) and modified Caillé theory (MCT). The MCT provides good fits to the data, much better than the PT fits. The particularly important characteristic of MCT is the long power law tails in the scattering. PT fits (as well as ordinary integration with no attempt to account for the noncrystalline disorder) increasingly underestimate this scattering intensity as the order h increases, thereby underestimating the form factors used to obtain electron density profiles. Images FIGURE 4 PMID:8770211

  9. Tuning Precursor Reactivity toward Nanometer-Size Control in Palladium Nanoparticles Studied by in Situ Small Angle X-ray Scattering

    DOE PAGES

    Wu, Liheng; Lian, Huada; Willis, Joshua J.; ...

    2018-01-03

    Synthesis of monodisperse nanoparticles (NPs) with precisely controlled size is critical for understanding their size-dependent properties. Although significant synthetic developments have been achieved, it is still challenging to synthesize well-defined NPs in a predictive way due to a lack of in-depth mechanistic understanding of reaction kinetics. Here we use synchrotron-based small-angle X-ray scattering (SAXS) to monitor in situ the formation of palladium (Pd) NPs through thermal decomposition of Pd–TOP (TOP: trioctylphosphine) complex via the “heat-up” method. We systematically study the effects of different ligands, including oleylamine, TOP, and oleic acid, on the formation kinetics of Pd NPs. Through quantitative analysismore » of the real-time SAXS data, we are able to obtain a detailed picture of the size, size distribution, and concentration of Pd NPs during the syntheses, and these results show that different ligands strongly affect the precursor reactivity. We find that oleylamine does not change the reactivity of the Pd–TOP complex but promote the formation of nuclei due to strong ligand–NP binding. On the other hand, TOP and oleic acid substantially change the precursor reactivity over more than an order of magnitude, which controls the nucleation kinetics and determines the final particle size. A theoretical model is used to demonstrate that the nucleation and growth kinetics are dependent on both precursor reactivity and ligand–NP binding affinity, thus providing a framework to explain the synthesis process and the effect of the reaction conditions. Quantitative understanding of the impacts of different ligands enables the successful synthesis of a series of monodisperse Pd NPs in the broad size range from 3 to 11 nm with nanometer-size control, which serve as a model system to study their size-dependent catalytic properties. Furthermore, the in situ SAXS probing can be readily extended to other functional NPs to greatly advance

  10. Tuning Precursor Reactivity toward Nanometer-Size Control in Palladium Nanoparticles Studied by in Situ Small Angle X-ray Scattering

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

    Wu, Liheng; Lian, Huada; Willis, Joshua J.

    Synthesis of monodisperse nanoparticles (NPs) with precisely controlled size is critical for understanding their size-dependent properties. Although significant synthetic developments have been achieved, it is still challenging to synthesize well-defined NPs in a predictive way due to a lack of in-depth mechanistic understanding of reaction kinetics. Here we use synchrotron-based small-angle X-ray scattering (SAXS) to monitor in situ the formation of palladium (Pd) NPs through thermal decomposition of Pd–TOP (TOP: trioctylphosphine) complex via the “heat-up” method. We systematically study the effects of different ligands, including oleylamine, TOP, and oleic acid, on the formation kinetics of Pd NPs. Through quantitative analysismore » of the real-time SAXS data, we are able to obtain a detailed picture of the size, size distribution, and concentration of Pd NPs during the syntheses, and these results show that different ligands strongly affect the precursor reactivity. We find that oleylamine does not change the reactivity of the Pd–TOP complex but promote the formation of nuclei due to strong ligand–NP binding. On the other hand, TOP and oleic acid substantially change the precursor reactivity over more than an order of magnitude, which controls the nucleation kinetics and determines the final particle size. A theoretical model is used to demonstrate that the nucleation and growth kinetics are dependent on both precursor reactivity and ligand–NP binding affinity, thus providing a framework to explain the synthesis process and the effect of the reaction conditions. Quantitative understanding of the impacts of different ligands enables the successful synthesis of a series of monodisperse Pd NPs in the broad size range from 3 to 11 nm with nanometer-size control, which serve as a model system to study their size-dependent catalytic properties. Furthermore, the in situ SAXS probing can be readily extended to other functional NPs to greatly advance

  11. Reconstruction of viruses from solution x-ray scattering data

    NASA Astrophysics Data System (ADS)

    Zheng, Yibin; Doerschuk, Peter C.; Johnson, John E.

    1995-08-01

    A model-based method for reconstructing the 3D structure of icosahedrally-symmetric viruses from solution x-ray scattering is presented. An example of the reconstruction, for data from cowpea mosaic virus, is described. The major opportunity provided by solution x-ray scattering is the ability to study the dynamics of virus particles in solution, information that is not accessible to crystal x-ray diffraction experiments.

  12. Tracking of Short Distance Transport Pathways in Biological Tissues by Ultra-Small Nanoparticles

    NASA Astrophysics Data System (ADS)

    Segmehl, Jana S.; Lauria, Alessandro; Keplinger, Tobias; Berg, John K.; Burgert, Ingo

    2018-03-01

    In this work, ultra-small europium-doped HfO2 nanoparticles were infiltrated into native wood and used as trackers for studying penetrability and diffusion pathways in the hierarchical wood structure. The high electron density, laser induced luminescence, and crystallinity of these particles allowed for a complementary detection of the particles in the cellular tissue. Confocal Raman microscopy and high-resolution synchrotron scanning wide-angle X-ray scattering (WAXS) measurements were used to detect the infiltrated particles in the native wood cell walls. This approach allows for simultaneously obtaining chemical information of the probed biological tissue and the spatial distribution of the integrated particles. The in-depth information about particle distribution in the complex wood structure can be used for revealing transport pathways in plant tissues, but also for gaining better understanding of modification treatments of plant scaffolds aiming at novel functionalized materials.

  13. NOTE: Characterization of cirrhosis and hepatocellular carcinoma using low-angle x-ray scattering signatures of serum

    NASA Astrophysics Data System (ADS)

    Elshemey, Wael M.; Desouky, Omar S.; Mohammed, Mohammed S.; Elsayed, Anwar A.; El-houseini, Motawa E.

    2003-09-01

    The diagnosis of hepatocellular carcinoma (HCC) usually occurs at late stages in the disease when there are few effective treatment options. The measurement of the concentration of tumour markers in the serum of patients is a complementary tool frequently used for the interpretation of diagnostic imaging results. It is also used as a prognostic tool for the detection of cancer. Unfortunately, the sensitivity of tumour markers is still low and many times it yields normal results for cirrhotic and HCC patients. In the current work, the detection possibility of the structural changes in serum proteins accompanying cirrhosis and HCC is investigated using a low-angle x-ray scattering (LAXS) technique. The results show that there are significant differences in the LAXS profiles of cirrhosis and HCC lyophilized serum samples compared to normal. The changes in shape, total counts and position of the first scattering peak at 4.8°, which was previously reported to be sensitive to the structural changes in protein, showed the most characteristic deviations from normal serum. The present results are promising and would offer a potentially helpful complementary tool for monitoring cirrhosis and HCC.

  14. Microstructure investigation on micropore formation in microporous silica materials prepared via a catalytic sol-gel process by small angle X-ray scattering.

    PubMed

    Shimizu, Wataru; Hokka, Junsuke; Sato, Takaaki; Usami, Hisanao; Murakami, Yasushi

    2011-08-04

    The so-called sol-gel technique has been shown to be a template-free, efficient way to create functional porous silica materials having uniform micropores. This appears to be closely linked with a postulation that the formation of weakly branched polymer-like aggregates in a precursor solution is a key to the uniform micropore generation. However, how such a polymer-like structure can precisely be controlled, and further, how the generated low-fractal dimension solution structure is imprinted on the solid silica materials still remain elusive. Here we present fabrication of microporous silica from tetramethyl orthosilicate (TMOS) using a recently developed catalytic sol-gel process based on a nonionic hydroxyacetone (HA) catalyst. Small angle X-ray scattering (SAXS), nitrogen adsorption porosimetry, and transmission electron microscope (TEM) allowed us to observe the whole structural evolution, ranging from polymer-like aggregates in the precursor solution to agglomeration with heat treatment and microporous morphology of silica powders after drying and hydrolysis. Using the HA catalyst with short chain monohydric alcohols (methanol or ethanol) in the precursor solution, polymer-like aggregates having microscopic correlation length (or mesh-size) < 2 nm and low fractal dimensions ∼2, which is identical to that of an ideal coil polymer, can selectively be synthesized, yielding the uniform micropores with diameters <2 nm in the solid materials. In contrast, the absence of HA or substitution of 1-propanol led to considerably different scattering behavior reflecting the particle-like aggregate formation in the precursor solution, which resulted in the formation of mesopores (diameter >2 nm) in the solid product due to apertures between the particle-like aggregates. The data demonstrate that the extremely fine porous silica architecture comes essentially from a gaussian polymer-like nature of the silica aggregates in the precursor having the microscopic mesh-size and

  15. Nanoporous active carbons at ambient conditions: a comparative study using X-ray scattering and diffraction, Raman spectroscopy and N2 adsorption

    NASA Astrophysics Data System (ADS)

    Shiryaev, A. A.; Voloshchuk, A. M.; Volkov, V. V.; Averin, A. A.; Artamonova, S. D.

    2017-05-01

    Furfural-derived sorbents and activated carbonaceous fibers were studied using Small- and Wide-angle X-ray scattering (SWAXS), X-ray diffraction and multiwavelength Raman spectroscopy after storage at ambient conditions. Correlations between structural features with degree of activation and with sorption parameters are observed for samples obtained from a common precursor and differing in duration of activation. However, the correlations are not necessarily applicable to the carbons obtained from different precursors. Using two independent approaches we show that treatment of SWAXS results should be performed with careful analysis of applicability of the Porod law to the sample under study. In general case of a pore with rough/corrugated surface deviations from the Porod law may became significant and reflect structure of the pore-carbon interface. Ignorance of these features may invalidate extraction of closed porosity values. In most cases the pore-matrix interface in the studied samples is not atomically sharp, but is characterized by 1D or 2D fluctuations of electronic density responsible for deviations from the Porod law. Intensity of the pores-related small-angle scattering correlates positively with SBET values obtained from N2 adsorption.

  16. Resonance energy shifts during nuclear Bragg diffraction of x rays

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

    Arthur, J.; Brown, G.S.; Brown, D.E.

    1989-10-09

    We have observed dramatic changes in the time distribution of synchrotron x rays resonantly scattered from {sup 57}Fe nuclei in a crystal of yttrium iron garnet, which depend on the deviation angle of the incident radiation from the Bragg angle. These changes are caused by small shifts in the effective energies of the hyperfine-split nuclear resonances, an effect of dynamical diffraction for the coherently excited nuclei in the crystal. The very high brightness of the synchro- tron x-ray source allows this effect to be observed in a 15-min measurement.

  17. X-ray characterization of solid small molecule organic materials

    DOEpatents

    Billinge, Simon; Shankland, Kenneth; Shankland, Norman; Florence, Alastair

    2014-06-10

    The present invention provides, inter alia, methods of characterizing a small molecule organic material, e.g., a drug or a drug product. This method includes subjecting the solid small molecule organic material to x-ray total scattering analysis at a short wavelength, collecting data generated thereby, and mathematically transforming the data to provide a refined set of data.

  18. Kinetics of Polymer-Fullerene Phase Separation during Solvent Annealing Studied by Table-Top X-ray Scattering.

    PubMed

    Vegso, Karol; Siffalovic, Peter; Jergel, Matej; Nadazdy, Peter; Nadazdy, Vojtech; Majkova, Eva

    2017-03-08

    Solvent annealing is an efficient way of phase separation in polymer-fullerene blends to optimize bulk heterojunction morphology of active layer in polymer solar cells. To track the process in real time across all relevant stages of solvent evaporation, laboratory-based in situ small- and wide-angle X-ray scattering measurements were applied simultaneously to a model P3HT:PCBM blend dissolved in dichlorobenzene. The PCBM molecule agglomeration starts at ∼7 wt % concentration of solid content of the blend in solvent. Although PCBM agglomeration is slowed-down at ∼10 wt % of solid content, the rate constant of phase separation is not changed, suggesting agglomeration and reordering of P3HT molecular chains. Having the longest duration, this stage most affects BHJ morphology. Phase separation is accelerated rapidly at concentration of ∼25 wt %, having the same rate constant as the growth of P3HT crystals. P3HT crystallization is driving force for phase separation at final stages before a complete solvent evaporation, having no visible temporal overlap with PCBM agglomeration. For the first time, such a study was done in laboratory demonstrating potential of the latest generation table-top high-brilliance X-ray source as a viable alternative before more sophisticated X-ray scattering experiments at synchrotron facilities are performed.

  19. Generation of High Brightness X-rays with the PLEIADES Thomson X-ray Source

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

    Brown, W J; Anderson, S G; Barty, C P J

    2003-05-28

    The use of short laser pulses to generate high peak intensity, ultra-short x-ray pulses enables exciting new experimental capabilities, such as femtosecond pump-probe experiments used to temporally resolve material structural dynamics on atomic time scales. PLEIADES (Picosecond Laser Electron InterAction for Dynamic Evaluation of Structures) is a next generation Thomson scattering x-ray source being developed at Lawrence Livermore National Laboratory (LLNL). Ultra-fast picosecond x-rays (10-200 keV) are generated by colliding an energetic electron beam (20-100 MeV) with a high intensity, sub-ps, 800 nm laser pulse. The peak brightness of the source is expected to exceed 10{sup 20} photons/s/0.1% bandwidth/mm2/mrad2. Simulationsmore » of the electron beam production, transport, and final focus are presented. Electron beam measurements, including emittance and final focus spot size are also presented and compared to simulation results. Measurements of x-ray production are also reported and compared to theoretical calculations.« less

  20. A compact permanent-magnet system for measuring magnetic circular dichroism in resonant inelastic soft X-ray scattering.

    PubMed

    Miyawaki, Jun; Suga, Shigemasa; Fujiwara, Hidenori; Niwa, Hideharu; Kiuchi, Hisao; Harada, Yoshihisa

    2017-03-01

    A compact and portable magnet system for measuring magnetic dichroism in resonant inelastic soft X-ray scattering (SX-RIXS) has been developed at the beamline BL07LSU in SPring-8. A magnetic circuit composed of Nd-Fe-B permanent magnets, which realised ∼0.25 T at the center of an 11 mm gap, was rotatable around the axis perpendicular to the X-ray scattering plane. Using the system, a SX-RIXS spectrum was obtained under the application of the magnetic field at an angle parallel, nearly 45° or perpendicular to the incident X-rays. A dedicated sample stage was also designed to be as compact as possible, making it possible to perform SX-RIXS measurements at arbitrary incident angles by rotating the sample stage in the gap between the magnetic poles. This system enables facile studies of magnetic dichroism in SX-RIXS for various experimental geometries of the sample and the magnetic field. A brief demonstration of the application is presented.

  1. Salts employed in hydrophobic interaction chromatography can change protein structure - insights from protein-ligand interaction thermodynamics, circular dichroism spectroscopy and small angle X-ray scattering.

    PubMed

    Komaromy, Andras Z; Kulsing, Chadin; Boysen, Reinhard I; Hearn, Milton T W

    2015-03-01

    Key requirements of protein purification by hydrophobic interaction chromatography (HIC) are preservation of the tertiary/quaternary structure, maintenance of biological function, and separation of the correctly folded protein from its unfolded forms or aggregates. This study examines the relationship between the HIC retention behavior of hen egg white lysozyme (HEWL) in high concentrations of several kosmotropic salts and its conformation, assessed by circular dichroism (CD) spectroscopy. Further, the physicochemical properties of HEWL in the presence of high concentrations of ammonium sulfate, sodium chloride and magnesium chloride were investigated by small angle X-ray scattering (SAXS) at different temperatures. Radii of gyration were extrapolated from Guinier approximations and the indirect transform program GNOM with protein-protein interaction and contrast variation taken into account. A bead model simulation provided information on protein structural changes using ab initio reconstruction with GASBOR. These results correlated to the secondary structure content obtained from CD spectroscopy of HEWL. These changes in SAXS and CD data were consistent with heat capacity ΔCp -values obtained from van't Hoff plot analyses of the retention data. Collectively, these insights enable informed decisions to be made on the choice of chromatographic conditions, leading to improved separation selectivity and opportunities for innovative column-assisted protein refolding methods. Copyright © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Solution x-ray scattering and structure formation in protein dynamics

    NASA Astrophysics Data System (ADS)

    Nasedkin, Alexandr; Davidsson, Jan; Niemi, Antti J.; Peng, Xubiao

    2017-12-01

    We propose a computationally effective approach that builds on Landau mean-field theory in combination with modern nonequilibrium statistical mechanics to model and interpret protein dynamics and structure formation in small- to wide-angle x-ray scattering (S/WAXS) experiments. We develop the methodology by analyzing experimental data in the case of Engrailed homeodomain protein as an example. We demonstrate how to interpret S/WAXS data qualitatively with a good precision and over an extended temperature range. We explain experimental observations in terms of protein phase structure, and we make predictions for future experiments and for how to analyze data at different ambient temperature values. We conclude that the approach we propose has the potential to become a highly accurate, computationally effective, and predictive tool for analyzing S/WAXS data. For this, we compare our results with those obtained previously in an all-atom molecular dynamics simulation.

  3. The roles of RIIbeta linker and N-terminal cyclic nucleotide-binding domain in determining the unique structures of Type IIbeta Protein Kinase A. A small angle X-ray and neutron scattering study

    DOE PAGES

    Blumenthal, Donald K.; Copps, Jeffrey; Smith-Nguyen, Eric V.; ...

    2014-08-11

    Protein kinase A (PKA) is ubiquitously expressed and is responsible for regulating many important cellular functions in response to changes in intracellular cAMP concentrations. Moreover, the PKA holoenzyme is a tetramer (R 2:C 2), with a regulatory subunit homodimer (R 2) that binds and inhibits two catalytic (C) subunits; binding of cAMP to the regulatory subunit homodimer causes activation of the catalytic subunits. Four different R subunit isoforms exist in mammalian cells, and these confer different structural features, subcellular localization, and biochemical properties upon the PKA holoenzymes they form. The holoenzyme containing RIIβ is structurally unique in that the typemore » IIβ holoenzyme is much more compact than the free RIIβ homodimer. We have used small angle x-ray scattering and small angle neutron scattering to study the solution structure and subunit organization of a holoenzyme containing an RIIβ C-terminal deletion mutant (RIIβ(1–280)), which is missing the C-terminal cAMP-binding domain to better understand the structural organization of the type IIβ holoenzyme and the RIIβ domains that contribute to stabilizing the holoenzyme conformation. These results demonstrate that compaction of the type IIβ holoenzyme does not require the C-terminal cAMP-binding domain but rather involves large structural rearrangements within the linker and N-terminal cyclic nucleotide-binding domain of the RIIβ homodimer. The structural rearrangements are significantly greater than seen previously with RIIα and are likely to be important in mediating short range and long range interdomain and intersubunit interactions that uniquely regulate the activity of the type IIβ isoform of PKA.« less

  4. How to improve x-ray scattering techniques to quantify bone mineral density using spectroscopy

    PubMed Central

    Krmar, M.; Ganezer, K.

    2012-01-01

    Purpose: The purpose of this study was to develop a new diagnostic technique for measuring bone mineral density (BMD) for the assessment of osteoporosis, which improves upon the coherent to Compton scattering ratio (CCSR) method, which was first developed in the 1980s. To help the authors achieve these goals, they have identified and studied two new indices for CCSR, the forward scattered to backward scattered (FS-BS) and the forward scattered to transmitted (FS-T) ratios. They believe that, at small angles, these two parameters can offer a practical in vivo determination of BMD that can be used to overcome the limitations of past CCSR systems, including high radiation dosages, costs, and examination durations. Methods: In previous CCSR studies, a high-activity radioactive source with a long half-live (usually 241Am) and an expensive and bulky cryogenic HPGe detector were applied to both in vivo and in vitro measurements. To make this technique more suitable for clinical applications, the possibility of using a standard diagnostic x-ray tube generating a continuous spectrum was investigated in this paper. Scattered radiation from trabecular bone-simulating phantoms containing various mineral densities that span the normal range of in vivo BMD was collected in this study using relatively inexpensive noncryogenic CdTe or NaI detectors. Results: The initial results demonstrate that a modified version of CCSR can be successfully applied to trabecular bone assessment using a diagnostic x-ray tube with a continuous spectrum in two variations, the FS-BS and the FS-T ratio. When FS-BS is measured, intensity spectra in the forward and backward directions must be collected while FS-T requires only the integral intensity of the scattered and transmitted (T) spectra in the energy region above 40 keV. For both of these methods, forward scattering angles less than or equal to 15° and backward scattering angles greater than or equal to (165°= 180° − 15°) are needed

  5. Photoluminescence studies on Cd(1-x)Zn(x)S:Mn2+ nanocrystals.

    PubMed

    Sethi, Ruchi; Kumar, Lokendra; Pandey, A C

    2009-09-01

    Highly monodispersed, undoped and doped with Mn2+, binary and ternary (CdS, ZnS, Cd(1-x)Zn(x)S) compound semiconductor nanocrystals have been synthesized by co-precipitation method using citric acid as a stabilizer. As prepared sample are characterized by X-ray diffraction, Small angle X-ray scattering, Transmission electron microscope, Optical absorption and Photoluminescence spectroscopy, for their optical and structural properties. X-ray diffraction, Small angle X-ray scattering and Transmission electron microscope results confirm the preparation of monodispersed nanocrystals. Photoluminescence studies show a significant blue shift in the wavelength with an increasing concentration of Zn in alloy nanocrystals.

  6. Azimuthal-angle dependence of L x-ray intensity following photoionization of Pb, Au, and W atoms by a linearly polarized photon

    NASA Astrophysics Data System (ADS)

    Namito, Y.; Ban, S.; Hirayama, H.

    2008-09-01

    We measured the L x-ray intensities of Pb, Au, and W for several different azimuthal angles and partially polarized photon beams by using high-purity low-energy Ge detectors. We utilized a monochromatized synchrotron beam as the source. It had an energy of 10.88 40keV , and its degree of linear polarization P ranged from 0.84 to 0.89. The scattering polar angle (θ) was 90°, and the azimuthal angle (ϕ1) was 0° or 90°, relative to the polarization direction. We obtained the x-ray intensity ratio R[=I(ϕ1=0°)/I(ϕ1=90°)] . We observed that the Ll intensities depended on the azimuthal scattering angle ϕ1 , i.e., R=0.92 0.94 , 0.91 0.94, and 0.90 0.93 for Pb, Au, and W, respectively. On the other hand, the dependence of Lα on the azimuthal scattering angle was not clear due to experimental uncertainty. The anisotropy of Lγ was not observed. These results agreed with the theoretical calculations based on Scofield’s theory.

  7. The approach to reflection x-ray microscopy below the critical angles

    NASA Astrophysics Data System (ADS)

    Artyukov, Igor A.; Busarov, Alexander; Popov, Nikolay L.; Vinogradov, Alexander V.

    2017-05-01

    There is a quest for new knowledge and methods to study various materials and processes on surfaces and interfaces at the nanoscale. It concerns ablation, phase transitions, physical and chemical transformations, dissolution, selforganization etc. Obviously, to achieve an appropriate resolution it is necessary to use a corresponding wavelength . Higher resolution can be obtained with shorter wavelengths. On the other hand, in surface modification, ablation, study of buried interfaces etc. the penetration length of radiation into the materials, which depends on the wavelength and angle of incidence, plays important role... Considering these factors the experimental studies in nano-physics and nanotechnology are usually carried out using X-ray radiation with a photon energy of 0.1-10 keV. As far as surfaces and films are investigated, it is reasonable to use an X-ray microscope operating in the reflection mode. However, in this spectral range a substantial portion of the radiation is reflected only at small grazing angles (e.g. <= 10°). Thus, the idea of grazing incidence reflection-mode X-ray microscope has been developed. In this paper, we consider one of possible schemes of such an X-ray microscope. Our analysis and simulation is based on the extension of the Fresnel propagation theory to tilted object problems.

  8. Instrumentation on Multi-Scaled Scattering of Bio-Macromolecular Solutions

    PubMed Central

    Chu, Benjamin; Fang, Dufei; Mao, Yimin

    2015-01-01

    The design, construction and initial tests on a combined laser light scattering and synchrotron X-ray scattering instrument can cover studies of length scales from atomic sizes in Angstroms to microns and dynamics from microseconds to seconds are presented. In addition to static light scattering (SLS), dynamic light scattering (DLS), small angle X-ray scattering (SAXS) and wide angle X-ray diffraction (WAXD), the light scattering instrument is being developed to carry out studies in mildly turbid solutions, in the presence of multiple scattering. Three-dimensional photon cross correlation function (3D-PCCF) measurements have been introduced to couple with synchrotron X-ray scattering to study the structure, size and dynamics of macromolecules in solution. PMID:25946340

  9. SoftWAXS: a computational tool for modeling wide-angle X-ray solution scattering from biomolecules.

    PubMed

    Bardhan, Jaydeep; Park, Sanghyun; Makowski, Lee

    2009-10-01

    This paper describes a computational approach to estimating wide-angle X-ray solution scattering (WAXS) from proteins, which has been implemented in a computer program called SoftWAXS. The accuracy and efficiency of SoftWAXS are analyzed for analytically solvable model problems as well as for proteins. Key features of the approach include a numerical procedure for performing the required spherical averaging and explicit representation of the solute-solvent boundary and the surface of the hydration layer. These features allow the Fourier transform of the excluded volume and hydration layer to be computed directly and with high accuracy. This approach will allow future investigation of different treatments of the electron density in the hydration shell. Numerical results illustrate the differences between this approach to modeling the excluded volume and a widely used model that treats the excluded-volume function as a sum of Gaussians representing the individual atomic excluded volumes. Comparison of the results obtained here with those from explicit-solvent molecular dynamics clarifies shortcomings inherent to the representation of solvent as a time-averaged electron-density profile. In addition, an assessment is made of how the calculated scattering patterns depend on input parameters such as the solute-atom radii, the width of the hydration shell and the hydration-layer contrast. These results suggest that obtaining predictive calculations of high-resolution WAXS patterns may require sophisticated treatments of solvent.

  10. X-ray induced dimerization of cinnamic acid: Time-resolved inelastic X-ray scattering study

    NASA Astrophysics Data System (ADS)

    Inkinen, Juho; Niskanen, Johannes; Talka, Tuomas; Sahle, Christoph J.; Müller, Harald; Khriachtchev, Leonid; Hashemi, Javad; Akbari, Ali; Hakala, Mikko; Huotari, Simo

    2015-11-01

    A classic example of solid-state topochemical reactions is the ultraviolet-light induced photodimerization of α-trans-cinnamic acid (CA). Here, we report the first observation of an X-ray-induced dimerization of CA and monitor it in situ using nonresonant inelastic X-ray scattering spectroscopy (NRIXS). The time-evolution of the carbon core-electron excitation spectra shows the effects of two X-ray induced reactions: dimerization on a short time-scale and disintegration on a long time-scale. We used spectrum simulations of CA and its dimerization product, α-truxillic acid (TA), to gain insight into the dimerization effects. From the time-resolved spectra, we extracted component spectra and time-dependent weights corresponding to CA and TA. The results suggest that the X-ray induced dimerization proceeds homogeneously in contrast to the dimerization induced by ultraviolet light. We also utilized the ability of NRIXS for direct tomography with chemical-bond contrast to image the spatial progress of the reactions in the sample crystal. Our work paves the way for other time-resolved studies on chemical reactions using inelastic X-ray scattering.

  11. Small angle light scattering characterization of single micrometric particles in microfluidic flows

    NASA Astrophysics Data System (ADS)

    Dannhauser, David; Romeo, Giovanni; Causa, Filippo; Netti, Paolo A.

    2013-04-01

    A CCD-camera based small angle light scattering (SALS) apparatus has been used to characterize single micrometric particles flowing in a micro-channel. The measured scattering vector spans the range 2x10-2 - 6:8x101μm-1. The incident laser light is collimated to a spot of about 50 μm in diameter at the sample position with a divergence lower than 0.045 rad. Such small collimated laser beam opens the possibility to perform on-line SALS of micron-sized particles flowing in micro-channels. By properly designing the micro-channel and using a viscoelastic liquid as suspending medium we are able to realize a precise 3D focusing of the target particles. The forward scattering emitted from the particle is collected by a lens with high numerical aperture. At the focal point of that lens a homemade beam stop is blocking the incident light. Finally, a second lens maps the scattered light on the CCD sensor, allowing to obtain far field images on short distances. Measurements with mono-disperse polystyrene particles, both in quiescent and in-flow conditions have been realized. Experiments in-flow allow to measure the single particle scattering. Results are validated by comparison with calculations based on the Lorenz-Mie theory. The quality of the measured intensity profiles confirms the possibility to use our apparatus in real multiplex applications, with particles down to 1 μm in radius.

  12. Experimental characterization of an ultra-fast Thomson scattering x-ray source with three-dimensional time and frequency-domain analysis

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

    Kuba, J; Slaughter, D R; Fittinghoff, D N

    We present a detailed comparison of the measured characteristics of Thomson backscattered x-rays produced at the PLEIADES (Picosecond Laser-Electron Interaction for the Dynamic Evaluation of Structures) facility at Lawrence Livermore National Laboratory to predicted results from a newly developed, fully three-dimensional time and frequency-domain code. Based on the relativistic differential cross section, this code has the capability to calculate time and space dependent spectra of the x-ray photons produced from linear Thomson scattering for both bandwidth-limited and chirped incident laser pulses. Spectral broadening of the scattered x-ray pulse resulting from the incident laser bandwidth, perpendicular wave vector components in themore » laser focus, and the transverse and longitudinal phase space of the electron beam are included. Electron beam energy, energy spread, and transverse phase space measurements of the electron beam at the interaction point are presented, and the corresponding predicted x-ray characteristics are determined. In addition, time-integrated measurements of the x-rays produced from the interaction are presented, and shown to agree well with the simulations.« less

  13. X-ray studies of dynamic aging in an aluminum alloy subjected to severe plastic deformation

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

    Sitdikov, V.D., E-mail: svil@mail.rb.ru; Laboratory for Mechanics of Bulk Nanomaterials, Saint Petersburg State University, 28 Universitetsky pr., Saint Petersburg 198504; Chizhov, P.S.

    In this work, X-ray scattering methods were applied for a quantitative characterization of the microstructure of an aluminum alloy of the Al–Mg–Si system during dynamic aging realized through the high pressure torsion technique. A qualitative and quantitative phase analysis of the alloy was performed, together with Al alloy lattice parameter determination. From the reflections broadening the effective size of the coherent scattering domains and the lattice microstrain were determined in the framework of the Halder–Wagner approach. Using the method of small-angle X-ray scattering, the quantitative characteristics of the size, shape and spatial distribution of the secondary phase particles formed inmore » the Al alloy during dynamic aging were established. In order to validate the obtained results, the method of small-angle X-ray scattering was preliminarily tested on similar samples after artificial aging and compared with the results from small-angle neutron diffraction widely known in literature. - Highlights: • Spherical fcc β-Mg2Si precipitates formed in Al 6201 alloy during dynamic aging in the course of severe plastic deformation. • The size, shape and distribution of the precipitates due to artificial and dynamic aging were revealed by SAXS method. • Monoclinic needle-like β' precipitates and Al5FeSi intermetallic phase were detected in 6201 alloy after T6 treatment.« less

  14. 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.

  15. Effect of annealing conditions on the microstructure and magnetic properties of sintered Nd-Fe-B magnets as seen by magnetic small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Périgo, Élio A.; Titov, Ivan; Weber, Raoul; Mettus, Denis; Peral, Inma; Vallcorba, Oriol; Honecker, Dirk; Feoktystov, Artem; Michels, Andreas

    2018-03-01

    We have investigated the effect of the annealing conditions (heating rate and temperature) on the magnetic microstructure of sintered Nd-Fe-B magnets by means of magnetometry, scanning electron microscopy, high-energy synchrotron x-ray diffraction, and small-angle neutron scattering (SANS). While the temperature treatment has a strong effect on the coercivity (reduction by about 50% on annealing), the associated changes in the microstructure do surprisingly not show up (or at best only very weakly) in the neutron-scattering signal, which probes a mesoscopic real-space length scale ranging between about 1–300 nm. On the other hand, the x-ray data reveal microstructural changes in the Nd-rich phases, presumably due to modifications in grain-boundary regions. Moreover, we observe an unusual diamond-shaped angular anisotropy in the SANS cross section, which strongly points towards the existence of texture in the nuclear microstructure.

  16. 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.

  17. Dynamical scattering in coherent hard x-ray nanobeam Bragg diffraction

    NASA Astrophysics Data System (ADS)

    Pateras, A.; Park, J.; Ahn, Y.; Tilka, J. A.; Holt, M. V.; Kim, H.; Mawst, L. J.; Evans, P. G.

    2018-06-01

    Unique intensity features arising from dynamical diffraction arise in coherent x-ray nanobeam diffraction patterns of crystals having thicknesses larger than the x-ray extinction depth or exhibiting combinations of nanoscale and mesoscale features. We demonstrate that dynamical scattering effects can be accurately predicted using an optical model combined with the Darwin theory of dynamical x-ray diffraction. The model includes the highly divergent coherent x-ray nanobeams produced by Fresnel zone plate focusing optics and accounts for primary extinction, multiple scattering, and absorption. The simulation accurately reproduces the dynamical scattering features of experimental diffraction patterns acquired from a GaAs/AlGaAs epitaxial heterostructure on a GaAs (001) substrate.

  18. Accelerated x-ray scatter projection imaging using multiple continuously moving pencil beams

    NASA Astrophysics Data System (ADS)

    Dydula, Christopher; Belev, George; Johns, Paul C.

    2017-03-01

    Coherent x-ray scatter varies with angle and photon energy in a manner dependent on the chemical composition of the scattering material, even for amorphous materials. Therefore, images generated from scattered photons can have much higher contrast than conventional projection radiographs. We are developing a scatter projection imaging prototype at the BioMedical Imaging and Therapy (BMIT) facility of the Canadian Light Source (CLS) synchrotron in Saskatoon, Canada. The best images are obtained using step-and-shoot scanning with a single pencil beam and area detector to capture sequentially the scatter pattern for each primary beam location on the sample. Primary x-ray transmission is recorded simultaneously using photodiodes. The technological challenge is to acquire the scatter data in a reasonable time. Using multiple pencil beams producing partially-overlapping scatter patterns reduces acquisition time but increases complexity due to the need for a disentangling algorithm to extract the data. Continuous sample motion, rather than step-and-shoot, also reduces acquisition time at the expense of introducing motion blur. With a five-beam (33.2 keV, 3.5 mm2 beam area) continuous sample motion configuration, a rectangular array of 12 x 100 pixels with 1 mm sampling width has been acquired in 0.4 minutes (3000 pixels per minute). The acquisition speed is 38 times the speed for single beam step-and-shoot. A system model has been developed to calculate detected scatter patterns given the material composition of the object to be imaged. Our prototype development, image acquisition of a plastic phantom and modelling are described.

  19. PREFACE Proceedings of the XIV International Conference on Small-Angle Scattering, SAS-2009

    NASA Astrophysics Data System (ADS)

    King, Stephen; Terrill, Nicholas

    2010-10-01

    The XIV International Conference on Small-Angle Scattering, SAS-2009, was held in Oxford UK, 13-18 September 2009, and was jointly organised under the auspices of the International Union of Crystallography Commission on SAS by a team from the Diamond Light Source and the ISIS Pulsed Neutron Source - their first such joint venture - with help from the UK Science and Technology Facilities Council. It was the first time that this long running and successful series of conferences on the application, science and technology of small-angle scattering techniques had been staged in the UK. The UK has a proud heritage in small-angle scattering: as home to one of the world's first SANS instruments (at AERE Harwell), as the site of the world's first 2nd generation X-ray Synchrotron (the SRS at Daresbury with its suite of SAXS beamlines), and latterly as the location of the world's most successful pulsed source SANS instrument. Indeed, 2009 also marked the 25th Anniversary of neutron operations at ISIS and the opening of a Second Target Station. Whilst the SRS ceased operations in 2008, its mantle has been inherited by the Diamond synchrotron. Many delegates took the opportunity to visit both Diamond and ISIS during a conference excursion. Despite the prevailing global economic downturn, we were delighted that 434 delegates from 32 different countries were able to attend SAS-2009; two-thirds were drawn from the UK, Germany, Japan, the USA and France, but there were also sizeable contingents from Australia, Korea, Taiwan and South America. In many ways this geographical spread reflects the present and emerging distribution, respectively, of 3rd generation X-ray synchrotrons and high-flux neutron sources, although the scope of the conference was not solely limited to these probes. Financial support from the IUCr enabled us to grant bursaries to attend SAS-2009 to 12 delegates from emerging countries (Algeria, Argentina, Brazil, India, Nepal, Romania, Russia and the Ukraine). The

  20. Real-time, ray casting-based scatter dose estimation for c-arm x-ray system.

    PubMed

    Alnewaini, Zaid; Langer, Eric; Schaber, Philipp; David, Matthias; Kretz, Dominik; Steil, Volker; Hesser, Jürgen

    2017-03-01

    Dosimetric control of staff exposure during interventional procedures under fluoroscopy is of high relevance. In this paper, a novel ray casting approximation of radiation transport is presented and the potential and limitation vs. a full Monte Carlo transport and dose measurements are discussed. The x-ray source of a Siemens Axiom Artix C-arm is modeled by a virtual source model using single Gaussian-shaped source. A Geant4-based Monte Carlo simulation determines the radiation transport from the source to compute scatter from the patient, the table, the ceiling and the floor. A phase space around these scatterers stores all photon information. Only those photons are traced that hit a surface of phantom that represents medical staff in the treatment room, no indirect scattering is considered; and a complete dose deposition on the surface is calculated. To evaluate the accuracy of the approximation, both experimental measurements using Thermoluminescent dosimeters (TLDs) and a Geant4-based Monte Carlo simulation of dose depositing for different tube angulations of the C-arm from cranial-caudal angle 0° and from LAO (Left Anterior Oblique) 0°-90° are realized. Since the measurements were performed on both sides of the table, using the symmetry of the setup, RAO (Right Anterior Oblique) measurements were not necessary. The Geant4-Monte Carlo simulation agreed within 3% with the measured data, which is within the accuracy of measurement and simulation. The ray casting approximation has been compared to TLD measurements and the achieved percentage difference was -7% for data from tube angulations 45°-90° and -29% from tube angulations 0°-45° on the side of the x-ray source, whereas on the opposite side of the x-ray source, the difference was -83.8% and -75%, respectively. Ray casting approximation for only LAO 90° was compared to a Monte Carlo simulation, where the percentage differences were between 0.5-3% on the side of the x-ray source where the highest dose

  1. X-band RF gun and linac for medical Compton scattering X-ray source

    NASA Astrophysics Data System (ADS)

    Dobashi, Katsuhito; Uesaka, Mitsuru; Fukasawa, Atsushi; Sakamoto, Fumito; Ebina, Futaro; Ogino, Haruyuki; Urakawa, Junji; Higo, Toshiyasu; Akemoto, Mitsuo; Hayano, Hitoshi; Nakagawa, Keiichi

    2004-12-01

    Compton scattering hard X-ray source for 10-80 keV are under construction using the X-band (11.424 GHz) electron linear accelerator and YAG laser at Nuclear Engineering Research laboratory, University of Tokyo. This work is a part of the national project on the development of advanced compact medical accelerators in Japan. National Institute for Radiological Science is the host institute and U.Tokyo and KEK are working for the X-ray source. Main advantage is to produce tunable monochromatic hard (10-80 keV) X-rays with the intensities of 108-1010 photons/s (at several stages) and the table-top size. Second important aspect is to reduce noise radiation at a beam dump by adopting the deceleration of electrons after the Compton scattering. This realizes one beamline of a 3rd generation SR source at small facilities without heavy shielding. The final goal is that the linac and laser are installed on the moving gantry. We have designed the X-band (11.424 GHz) traveling-wave-type linac for the purpose. Numerical consideration by CAIN code and luminosity calculation are performed to estimate the X-ray yield. X-band thermionic-cathode RF-gun and RDS(Round Detuned Structure)-type X-band accelerating structure are applied to generate 50 MeV electron beam with 20 pC microbunches (104) for 1 microsecond RF macro-pulse. The X-ray yield by the electron beam and Q-switch Nd:YAG laser of 2 J/10 ns is 107 photons/RF-pulse (108 photons/sec at 10 pps). We design to adopt a technique of laser circulation to increase the X-ray yield up to 109 photons/pulse (1010 photons/s). 50 MW X-band klystron and compact modulator have been constructed and now under tuning. The construction of the whole system has started. X-ray generation and medical application will be performed in the early next year.

  2. Determination of the topological shape of integral membrane protein light-harvesting complex LH2 from photosynthetic bacteria in the detergent solution by small-angle X-ray scattering.

    PubMed

    Hong, Xinguo; Weng, Yu-Xiang; Li, Ming

    2004-02-01

    The topological shape of the integral membrane protein light-harvesting complex LH2 from photosynthetic bacteria Rhodobacter spheroides 2.4.1 in detergent solution has been determined from synchrotron small-angle X-ray scattering data using direct curve-fitting by the ellipsoid, ab initio shape determination methods of simulated annealing algorithm and multipole expansion, respectively. The results indicate that the LH2 protein in aqueous solution is encapsulated by a monolayered detergent shell. The detergent-stabilized structure has the shape of an oblate plate, with a thickness of 40 A, a long axis of 110 A, and a short axis of 85 A. After correction for the detergent shell, the shape of the LH2 core is also an oblate plate with a height of 40 A, a long axis of 80 A, and a short axis of 55 A. In contrast to the cylindrical crystal structure with a height of 40 A and a diameter of 68 A, the molecular shape of the LH2 complex in detergent solution clearly deviates from the ringlike crystal structure, with an eccentricity found to be 0.59-consistent with the result of single molecular spectroscopy study of the isolated single LH2 molecules.

  3. Determination of the Topological Shape of Integral Membrane Protein Light-Harvesting Complex LH2 from Photosynthetic Bacteria in the Detergent Solution by Small-Angle X-Ray Scattering

    PubMed Central

    Hong, Xinguo; Weng, Yu-Xiang; Li, Ming

    2004-01-01

    The topological shape of the integral membrane protein light-harvesting complex LH2 from photosynthetic bacteria Rhodobacter spheroides 2.4.1 in detergent solution has been determined from synchrotron small-angle X-ray scattering data using direct curve-fitting by the ellipsoid, ab initio shape determination methods of simulated annealing algorithm and multipole expansion, respectively. The results indicate that the LH2 protein in aqueous solution is encapsulated by a monolayered detergent shell. The detergent-stabilized structure has the shape of an oblate plate, with a thickness of 40 Å, a long axis of 110 Å, and a short axis of 85 Å . After correction for the detergent shell, the shape of the LH2 core is also an oblate plate with a height of 40 Å, a long axis of 80 Å, and a short axis of 55 Å. In contrast to the cylindrical crystal structure with a height of 40 Å and a diameter of 68 Å, the molecular shape of the LH2 complex in detergent solution clearly deviates from the ringlike crystal structure, with an eccentricity found to be 0.59—consistent with the result of single molecular spectroscopy study of the isolated single LH2 molecules. PMID:14747343

  4. Correlative Light and Scanning X-Ray Scattering Microscopy of Healthy and Pathologic Human Bone Sections

    PubMed Central

    Giannini, C.; Siliqi, D.; Bunk, O.; Beraudi, A.; Ladisa, M.; Altamura, D.; Stea, S.; Baruffaldi, F.

    2012-01-01

    Scanning small and wide angle X-ray scattering (scanning SWAXS) experiments were performed on healthy and pathologic human bone sections. Via crystallographic tools the data were transformed into quantitative images and as such compared with circularly polarized light (CPL) microscopy images. SWAXS and CPL images allowed extracting information of the mineral nanocrystalline phase embedded, with and without preferred orientation, in the collagen fibrils, mapping local changes at sub-osteon resolution. This favorable combination has been applied for the first time to biopsies of dwarfism syndrome and Paget's disease to shed light onto the cortical structure of natural bone in healthy and pathologic sections. PMID:22666538

  5. Densitometry and temperature measurement of combustion gas by X-ray Compton scattering

    PubMed Central

    Sakurai, Hiroshi; Kawahara, Nobuyuki; Itou, Masayoshi; Tomita, Eiji; Suzuki, Kosuke; Sakurai, Yoshiharu

    2016-01-01

    Measurement of combustion gas by high-energy X-ray Compton scattering is reported. The intensity of Compton-scattered X-rays has shown a position dependence across the flame of the combustion gas, allowing us to estimate the temperature distribution of the combustion flame. The energy spectra of Compton-scattered X-rays have revealed a significant difference across the combustion reaction zone, which enables us to detect the combustion reaction. These results demonstrate that high-energy X-ray Compton scattering can be employed as an in situ technique to probe inside a combustion reaction. PMID:26917151

  6. Densitometry and temperature measurement of combustion gas by X-ray Compton scattering.

    PubMed

    Sakurai, Hiroshi; Kawahara, Nobuyuki; Itou, Masayoshi; Tomita, Eiji; Suzuki, Kosuke; Sakurai, Yoshiharu

    2016-03-01

    Measurement of combustion gas by high-energy X-ray Compton scattering is reported. The intensity of Compton-scattered X-rays has shown a position dependence across the flame of the combustion gas, allowing us to estimate the temperature distribution of the combustion flame. The energy spectra of Compton-scattered X-rays have revealed a significant difference across the combustion reaction zone, which enables us to detect the combustion reaction. These results demonstrate that high-energy X-ray Compton scattering can be employed as an in situ technique to probe inside a combustion reaction.

  7. X-ray induced dimerization of cinnamic acid: Time-resolved inelastic X-ray scattering study

    PubMed Central

    Inkinen, Juho; Niskanen, Johannes; Talka, Tuomas; Sahle, Christoph J.; Müller, Harald; Khriachtchev, Leonid; Hashemi, Javad; Akbari, Ali; Hakala, Mikko; Huotari, Simo

    2015-01-01

    A classic example of solid-state topochemical reactions is the ultraviolet-light induced photodimerization of α-trans-cinnamic acid (CA). Here, we report the first observation of an X-ray-induced dimerization of CA and monitor it in situ using nonresonant inelastic X-ray scattering spectroscopy (NRIXS). The time-evolution of the carbon core-electron excitation spectra shows the effects of two X-ray induced reactions: dimerization on a short time-scale and disintegration on a long time-scale. We used spectrum simulations of CA and its dimerization product, α-truxillic acid (TA), to gain insight into the dimerization effects. From the time-resolved spectra, we extracted component spectra and time-dependent weights corresponding to CA and TA. The results suggest that the X-ray induced dimerization proceeds homogeneously in contrast to the dimerization induced by ultraviolet light. We also utilized the ability of NRIXS for direct tomography with chemical-bond contrast to image the spatial progress of the reactions in the sample crystal. Our work paves the way for other time-resolved studies on chemical reactions using inelastic X-ray scattering. PMID:26568420

  8. Development of fast parallel multi-technique scanning X-ray imaging at Synchrotron Soleil

    NASA Astrophysics Data System (ADS)

    Medjoubi, K.; Leclercq, N.; Langlois, F.; Buteau, A.; Lé, S.; Poirier, S.; Mercère, P.; Kewish, C. M.; Somogyi, A.

    2013-10-01

    A fast multimodal scanning X-ray imaging scheme is prototyped at Soleil Synchrotron. It permits the simultaneous acquisition of complementary information on the sample structure, composition and chemistry by measuring transmission, differential phase contrast, small-angle scattering, and X-ray fluorescence by dedicated detectors with ms dwell time per pixel. The results of the proof of principle experiments are presented in this paper.

  9. Multiple magnetic scattering in small-angle neutron scattering of Nd-Fe-B nanocrystalline magnet.

    PubMed

    Ueno, Tetsuro; Saito, Kotaro; Yano, Masao; Ito, Masaaki; Shoji, Tetsuya; Sakuma, Noritsugu; Kato, Akira; Manabe, Akira; Hashimoto, Ai; Gilbert, Elliot P; Keiderling, Uwe; Ono, Kanta

    2016-06-20

    We have investigated the influence of multiple scattering on the magnetic small-angle neutron scattering (SANS) from a Nd-Fe-B nanocrystalline magnet. We performed sample-thickness- and neutron-wavelength-dependent SANS measurements, and observed the scattering vector dependence of the multiple magnetic scattering. It is revealed that significant multiple scattering exists in the magnetic scattering rather than the nuclear scattering of Nd-Fe-B nanocrystalline magnet. It is considered that the mean free path of the neutrons for magnetic scattering is rather short in Nd-Fe-B magnets. We analysed the SANS data by the phenomenological magnetic correlation model considering the magnetic microstructures and obtained the microstructural parameters.

  10. Multiple magnetic scattering in small-angle neutron scattering of Nd–Fe–B nanocrystalline magnet

    PubMed Central

    Ueno, Tetsuro; Saito, Kotaro; Yano, Masao; Ito, Masaaki; Shoji, Tetsuya; Sakuma, Noritsugu; Kato, Akira; Manabe, Akira; Hashimoto, Ai; Gilbert, Elliot P.; Keiderling, Uwe; Ono, Kanta

    2016-01-01

    We have investigated the influence of multiple scattering on the magnetic small-angle neutron scattering (SANS) from a Nd–Fe–B nanocrystalline magnet. We performed sample-thickness- and neutron-wavelength-dependent SANS measurements, and observed the scattering vector dependence of the multiple magnetic scattering. It is revealed that significant multiple scattering exists in the magnetic scattering rather than the nuclear scattering of Nd–Fe–B nanocrystalline magnet. It is considered that the mean free path of the neutrons for magnetic scattering is rather short in Nd–Fe–B magnets. We analysed the SANS data by the phenomenological magnetic correlation model considering the magnetic microstructures and obtained the microstructural parameters. PMID:27321149

  11. Hard-X-ray dark-field imaging using a grating interferometer.

    PubMed

    Pfeiffer, F; Bech, M; Bunk, O; Kraft, P; Eikenberry, E F; Brönnimann, Ch; Grünzweig, C; David, C

    2008-02-01

    Imaging with visible light today uses numerous contrast mechanisms, including bright- and dark-field contrast, phase-contrast schemes and confocal and fluorescence-based methods. X-ray imaging, on the other hand, has only recently seen the development of an analogous variety of contrast modalities. Although X-ray phase-contrast imaging could successfully be implemented at a relatively early stage with several techniques, dark-field imaging, or more generally scattering-based imaging, with hard X-rays and good signal-to-noise ratio, in practice still remains a challenging task even at highly brilliant synchrotron sources. In this letter, we report a new approach on the basis of a grating interferometer that can efficiently yield dark-field scatter images of high quality, even with conventional X-ray tube sources. Because the image contrast is formed through the mechanism of small-angle scattering, it provides complementary and otherwise inaccessible structural information about the specimen at the micrometre and submicrometre length scale. Our approach is fully compatible with conventional transmission radiography and a recently developed hard-X-ray phase-contrast imaging scheme. Applications to X-ray medical imaging, industrial non-destructive testing and security screening are discussed.

  12. Anisotropy enhanced X-ray scattering from solvated transition metal complexes

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

    Biasin, Elisa; van Driel, Tim B.; Levi, Gianluca

    Time-resolved X-ray scattering patterns from photoexcited molecules in solution are in many cases anisotropic at the ultrafast time scales accessible at X-ray free-electron lasers (XFELs). This anisotropy arises from the interaction of a linearly polarized UV–Vis pump laser pulse with the sample, which induces anisotropic structural changes that can be captured by femtosecond X-ray pulses. In this work, a method for quantitative analysis of the anisotropic scattering signal arising from an ensemble of molecules is described, and it is demonstrated how its use can enhance the structural sensitivity of the time-resolved X-ray scattering experiment. This method is applied on time-resolvedmore » X-ray scattering patterns measured upon photoexcitation of a solvated di-platinum complex at an XFEL, and the key parameters involved are explored. Here it is shown that a combined analysis of the anisotropic and isotropic difference scattering signals in this experiment allows a more precise determination of the main photoinduced structural change in the solute,i.e.the change in Pt—Pt bond length, and yields more information on the excitation channels than the analysis of the isotropic scattering only. Finally, it is discussed how the anisotropic transient response of the solvent can enable the determination of key experimental parameters such as the instrument response function.« less

  13. Anisotropy enhanced X-ray scattering from solvated transition metal complexes

    DOE PAGES

    Biasin, Elisa; van Driel, Tim B.; Levi, Gianluca; ...

    2018-02-13

    Time-resolved X-ray scattering patterns from photoexcited molecules in solution are in many cases anisotropic at the ultrafast time scales accessible at X-ray free-electron lasers (XFELs). This anisotropy arises from the interaction of a linearly polarized UV–Vis pump laser pulse with the sample, which induces anisotropic structural changes that can be captured by femtosecond X-ray pulses. In this work, a method for quantitative analysis of the anisotropic scattering signal arising from an ensemble of molecules is described, and it is demonstrated how its use can enhance the structural sensitivity of the time-resolved X-ray scattering experiment. This method is applied on time-resolvedmore » X-ray scattering patterns measured upon photoexcitation of a solvated di-platinum complex at an XFEL, and the key parameters involved are explored. Here it is shown that a combined analysis of the anisotropic and isotropic difference scattering signals in this experiment allows a more precise determination of the main photoinduced structural change in the solute,i.e.the change in Pt—Pt bond length, and yields more information on the excitation channels than the analysis of the isotropic scattering only. Finally, it is discussed how the anisotropic transient response of the solvent can enable the determination of key experimental parameters such as the instrument response function.« less

  14. Microstructural Parameters in 8 MeV Electron-Irradiated BOMBYX MORI Silk Fibers by Wide-ANGLE X-Ray Scattering Studies (waxs)

    NASA Astrophysics Data System (ADS)

    Sangappa, Asha, S.; Sanjeev, Ganesh; Subramanya, G.; Parameswara, P.; Somashekar, R.

    2010-01-01

    The present work looks into the microstructural modification in electron irradiated Bombyx mori P31 silk fibers. The irradiation process was performed in air at room temperature using 8 MeV electron accelerator at different doses: 0, 25, 50 and 100 kGy. Irradiation of polymer is used to cross-link or degrade the desired component or to fix the polymer morphology. The changes in microstructural parameters in these natural polymer fibers have been computed using wide angle X-ray scattering (WAXS) data and employing line profile analysis (LPA) using Fourier transform technique of Warren. Exponential, Lognormal and Reinhold functions for the column length distributions have been used for the determination of crystal size, lattice strain and enthalpy parameters.

  15. WE-EF-207-06: Dedicated Cone-Beam Breast CT with Laterally-Shifted Detector: Monte Carlo Evaluation of X-Ray Scatter Distribution and Scatter-To-Primary Ratio

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

    Shi, L; Vedantham, S; Karellas, A

    2015-06-15

    Purpose: To determine the spatial distribution of x-ray scatter and scatter-to-primary ratio (SPR) in projections during cone-beam breast CT (CBBCT) with laterally-shifted detector that results in coronal (fan-angle) truncation. Methods: We hypothesized that CBBCT with coronal truncation would lower SPR due to reduction in irradiated breast volume, and that the location of maximum x-ray scatter fluence (scatter-peak) in the detector plane can be determined from the ratio of irradiated-to-total breast volume, breast dimensions and system geometry. Monte Carlo simulations (GEANT4) reflecting a prototype CBBCT system were used to record the position-dependent primary and scatter x-ray photon fluence incident on themore » detector without coronal truncation (full fan-angle, 2f=24-degrees) and with coronal truncation (fan-angle, f+ f=12+2.7-degrees). Semi-ellipsoidal breasts (10/14/18-cm diameter, chest-wall to nipple length: 0.75xdiameter, 2%/14%/100% fibroglandular content) aligned with the axis-of-rotation (AOR) were modeled. Mono-energy photons were simulated and weighted for 2 spectra (49kVp, 1.4-mm Al HVL; 60kVp, 3.76-mm Al HVL). In addition to SPR, the scatter maps were analyzed to identify the location of the scatter-peak. Results: For CBBCT without fan-angle truncation, the scatter-peaks were aligned with the projection of the AOR onto the detector for all breasts. With truncated fan-beam, the scatter-peaks were laterally-shifted from the projection of the AOR along the fan-angle direction by 14/38/70-pixels for 10/14/18-cm diameter breasts. The corresponding theoretical shifts were 14.8/39.7/68-pixels (p=0.47, 2-tailed paired-ratio t-test). Along the cone-angle, the shift in scatter-peaks between truncated and full-fan angle CBBCT were 2/2/4 -pixels for 10/14/18-cm diameter breasts. CBBCT with fan-angle truncation reduced SPR by 14/22/28% for 10/14/18-cm diameter breasts. 60kVp reduced SPR by 21–25% compared to 49kVp. Peak SPR for CBBCT with fan-angle

  16. Resonant magnetic scattering of polarized soft x rays

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

    Sacchi, M.; Hague, C.F.; Gullikson, E.M.

    1997-04-01

    Magnetic effects on X-ray scattering (Bragg diffraction, specular reflectivity or diffuse scattering) are a well known phenomenon, and they also represent a powerful tool for investigating magnetic materials since it was shown that they are strongly enhanced when the photon energy is tuned across an absorption edge (resonant process). The resonant enhancement of the magnetic scattering has mainly been investigated at high photon energies, in order to match the Bragg law for the typical lattice spacings of crystals. In the soft X-ray range, even larger effects are expected, working for instance at the 2p edges of transition metals of themore » first row or at the 3d edges of rare earths (300-1500 eV), but the corresponding long wavelengths prevent the use of single crystals. Two approaches have been recently adopted in this energy range: (i) the study of the Bragg diffraction from artificial structures of appropriate 2d spacing; (ii) the analysis of the specular reflectivity, which contains analogous information but has no constraints related to the lattice spacing. Both approaches have their own specific advantages: for instance, working under Bragg conditions provides information about the (magnetic) periodicity in ordered structures, while resonant reflectivity can easily be related to electronic properties and absorption spectra. An important aspect common to all the resonant X-ray scattering techniques is the element selectivity inherent to the fact of working at a specific absorption edge: under these conditions, X-ray scattering becomes in fact a spectroscopy. Results are presented for films of iron and cobalt.« less

  17. Small angle scattering from protein/sugar conjugates

    NASA Astrophysics Data System (ADS)

    Jackson, Andrew; White, John

    2006-11-01

    The Maillard reaction between free amine groups on proteins and sugars is well known. We have examined the effect of the reaction of the casein group of milk proteins with sugars on their nanoscale structure and aggregation. The small angle neutron scattering from beta casein and sodium caseinate and their sugar conjugates have been studied as a function of solution concentration. At high conjugate concentration (greater than ca. 5 mg/ml) the addition of sugar reduces supra-micellar aggregation of the protein whilst at lower concentration, where the protein is expected to be deaggregated already, little effect is seen. Guinier analysis of the scattering data show a radius of gyration of around 75 A˚ for beta casein in solution and around 80 A˚ for the sucrose conjugate.

  18. Demonstration of imaging X-ray Thomson scattering on OMEGA EP.

    PubMed

    Belancourt, Patrick X; Theobald, Wolfgang; Keiter, Paul A; Collins, Tim J B; Bonino, Mark J; Kozlowski, Pawel M; Regan, Sean P; Drake, R Paul

    2016-11-01

    Foams are a common material for high-energy-density physics experiments because of low, tunable densities, and being machinable. Simulating these experiments can be difficult because the equation of state is largely unknown for shocked foams. The focus of this experiment was to develop an x-ray scattering platform for measuring the equation of state of shocked foams on OMEGA EP. The foam used in this experiment is resorcinol formaldehyde with an initial density of 0.34 g/cm 3 . One long-pulse (10 ns) beam drives a shock into the foam, while the remaining three UV beams with a 2 ns square pulse irradiate a nickel foil to create the x-ray backlighter. The primary diagnostic for this platform, the imaging x-ray Thomson spectrometer, spectrally resolves the scattered x-ray beam while imaging in one spatial dimension. Ray tracing analysis of the density profile gives a compression of 3 ± 1 with a shock speed of 39 ± 6 km/s. Analysis of the scattered x-ray spectra gives an upper bound temperature of 20 eV.

  19. The roles of the RIIβ linker and N-terminal cyclic nucleotide-binding domain in determining the unique structures of the type IIβ protein kinase A: a small angle x-ray and neutron scattering study.

    PubMed

    Blumenthal, Donald K; Copps, Jeffrey; Smith-Nguyen, Eric V; Zhang, Ping; Heller, William T; Taylor, Susan S

    2014-10-10

    Protein kinase A (PKA) is ubiquitously expressed and is responsible for regulating many important cellular functions in response to changes in intracellular cAMP concentrations. The PKA holoenzyme is a tetramer (R2:C2), with a regulatory subunit homodimer (R2) that binds and inhibits two catalytic (C) subunits; binding of cAMP to the regulatory subunit homodimer causes activation of the catalytic subunits. Four different R subunit isoforms exist in mammalian cells, and these confer different structural features, subcellular localization, and biochemical properties upon the PKA holoenzymes they form. The holoenzyme containing RIIβ is structurally unique in that the type IIβ holoenzyme is much more compact than the free RIIβ homodimer. We have used small angle x-ray scattering and small angle neutron scattering to study the solution structure and subunit organization of a holoenzyme containing an RIIβ C-terminal deletion mutant (RIIβ(1-280)), which is missing the C-terminal cAMP-binding domain to better understand the structural organization of the type IIβ holoenzyme and the RIIβ domains that contribute to stabilizing the holoenzyme conformation. Our results demonstrate that compaction of the type IIβ holoenzyme does not require the C-terminal cAMP-binding domain but rather involves large structural rearrangements within the linker and N-terminal cyclic nucleotide-binding domain of the RIIβ homodimer. The structural rearrangements are significantly greater than seen previously with RIIα and are likely to be important in mediating short range and long range interdomain and intersubunit interactions that uniquely regulate the activity of the type IIβ isoform of PKA. © 2014 by The American Society for Biochemistry and Molecular Biology, Inc.

  20. Structure of a Unimolecular Dendritic Reverse Micelle in Dense CO2 Via Small Angle Scattering

    NASA Astrophysics Data System (ADS)

    Lin, J. S.

    1997-03-01

    Dilute solutions in dense CO2 (5Kpsi and 25 degC) of a unimolecular reverse micelle were studied via small angle x ray scattering (SAXS). The unimolecular micelle was based on a fourth generation poly(propylene imine) dendrimer, functionalized with perfluoropolyether acid fluoride chains. A value of 26 added chains per dendrimer was obtained from other characterization techniques, and this number of chains was fixed in the fitting of the SAXS data to an f-arm star model. The molecular weight ( 33.5K g mol-1) agreed well with estimates from other techniques. The observed negative second virial coefficient, A2 = -1.2 x 10-4 cm^3 g-2 mol, correlates with prior observations, as does the observed radius of gyration, Rg = 32ÅSponsors: Div. of Mat. Sci., Basic Energy Sc., USDOE, contract DE-AC05-96OR22464, Oak Ridge Nat. Lab., managed by Lockheed Martin Energy Research Corp.; The Royal Commission for the Exhibition of 1851; National Science Foundation; Consortium for the Sythesis and Processing of Polymeric Materials in Carbon Dioxide.

  1. Crystal defect studies using x-ray diffuse scattering

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

    Larson, B.C.

    1980-01-01

    Microscopic lattice defects such as point (single atom) defects, dislocation loops, and solute precipitates are characterized by local electronic density changes at the defect sites and by distortions of the lattice structure surrounding the defects. The effect of these interruptions of the crystal lattice on the scattering of x-rays is considered in this paper, and examples are presented of the use of the diffuse scattering to study the defects. X-ray studies of self-interstitials in electron irradiated aluminum and copper are discussed in terms of the identification of the interstitial configuration. Methods for detecting the onset of point defect aggregation intomore » dislocation loops are considered and new techniques for the determination of separate size distributions for vacancy loops and interstitial loops are presented. Direct comparisons of dislocation loop measurements by x-rays with existing electron microscopy studies of dislocation loops indicate agreement for larger size loops, but x-ray measurements report higher concentrations in the smaller loop range. Methods for distinguishing between loops and three-dimensional precipitates are discussed and possibilities for detailed studies considered. A comparison of dislocation loop size distributions obtained from integral diffuse scattering measurements with those from TEM show a discrepancy in the smaller sizes similar to that described above.« less

  2. Observations of Ultra-Luminous X-ray Sources, and Implications

    NASA Astrophysics Data System (ADS)

    Colbert, E. J. M.

    2004-05-01

    I will review observations of Ultra-Luminous X-ray Sources (ULXs; Lx > 1E39 erg/s), in particular those observations that have helped reveal the nature of these curious objects. Some recent observations suggest that ULXs are a heterogenous class. Although ULX phenomenology is not fully understood, I will present some examples from the (possibly overlapping) sub-classes. Since ULXs are the most luminous objects in starburst galaxies, they, and ``normal'' luminous black-hole high-mass X-ray binaries are intimately tied to the global galaxian X-ray-star-formation connection. Further work is needed to understand how ULXs form, and how they are associated with the putative population of intermediate-mass black holes.

  3. Industry-relevant magnetron sputtering and cathodic arc ultra-high vacuum deposition system for in situ x-ray diffraction studies of thin film growth using high energy synchrotron radiation.

    PubMed

    Schroeder, J L; Thomson, W; Howard, B; Schell, N; Näslund, L-Å; Rogström, L; Johansson-Jõesaar, M P; Ghafoor, N; Odén, M; Nothnagel, E; Shepard, A; Greer, J; Birch, J

    2015-09-01

    We present an industry-relevant, large-scale, ultra-high vacuum (UHV) magnetron sputtering and cathodic arc deposition system purposefully designed for time-resolved in situ thin film deposition/annealing studies using high-energy (>50 keV), high photon flux (>10(12) ph/s) synchrotron radiation. The high photon flux, combined with a fast-acquisition-time (<1 s) two-dimensional (2D) detector, permits time-resolved in situ structural analysis of thin film formation processes. The high-energy synchrotron-radiation based x-rays result in small scattering angles (<11°), allowing large areas of reciprocal space to be imaged with a 2D detector. The system has been designed for use on the 1-tonne, ultra-high load, high-resolution hexapod at the P07 High Energy Materials Science beamline at PETRA III at the Deutsches Elektronen-Synchrotron in Hamburg, Germany. The deposition system includes standard features of a typical UHV deposition system plus a range of special features suited for synchrotron radiation studies and industry-relevant processes. We openly encourage the materials research community to contact us for collaborative opportunities using this unique and versatile scientific instrument.

  4. X-ray Thomson scattering measurements from hohlraum-driven spheres on the OMEGA laser [X-ray Thomson scattering measurements from hohlraum targets on the OMEGA laser

    DOE PAGES

    Saunders, A. M.; Jenei, A.; Doppner, T.; ...

    2016-08-30

    X-ray Thomson scattering (XRTS) is a powerful diagnostic for probing warm and hot dense matter. We present the design and results of the first XRTS experiments with hohlraum-driven CH 2 targets on the OMEGA laser. X-rays seen directly from the XRTS x-ray source overshadow the elastic scattering signal from the target capsule, but can be controlled in future experiments. From the inelastic scattering signal, an average plasma temperature is inferred that is in reasonable agreement with the temperatures predicted by simulations. Here, knowledge gained in this experiment show a promising future for further XRTS measurements on indirectly driven OMEGA targets.

  5. X-ray Thomson scattering measurements from hohlraum-driven spheres on the OMEGA laser [X-ray Thomson scattering measurements from hohlraum targets on the OMEGA laser

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

    Saunders, A. M.; Jenei, A.; Doppner, T.

    X-ray Thomson scattering (XRTS) is a powerful diagnostic for probing warm and hot dense matter. We present the design and results of the first XRTS experiments with hohlraum-driven CH 2 targets on the OMEGA laser. X-rays seen directly from the XRTS x-ray source overshadow the elastic scattering signal from the target capsule, but can be controlled in future experiments. From the inelastic scattering signal, an average plasma temperature is inferred that is in reasonable agreement with the temperatures predicted by simulations. Here, knowledge gained in this experiment show a promising future for further XRTS measurements on indirectly driven OMEGA targets.

  6. Ultra-wideband, Wide Angle and Polarization-insensitive Specular Reflection Reduction by Metasurface based on Parameter-adjustable Meta-Atoms.

    PubMed

    Su, Jianxun; Lu, Yao; Zhang, Hui; Li, Zengrui; Lamar Yang, Yaoqing; Che, Yongxing; Qi, Kainan

    2017-02-09

    In this paper, an ultra-wideband, wide angle and polarization-insensitive metasurface is designed, fabricated, and characterized for suppressing the specular electromagnetic wave reflection or backward radar cross section (RCS). Square ring structure is chosen as the basic meta-atoms. A new physical mechanism based on size adjustment of the basic meta-atoms is proposed for ultra-wideband manipulation of electromagnetic (EM) waves. Based on hybrid array pattern synthesis (APS) and particle swarm optimization (PSO) algorithm, the selection and distribution of the basic meta-atoms are optimized simultaneously to obtain the ultra-wideband diffusion scattering patterns. The metasurface can achieve an excellent RCS reduction in an ultra-wide frequency range under x- and y-polarized normal incidences. The new proposed mechanism greatly extends the bandwidth of RCS reduction. The simulation and experiment results show the metasurface can achieve ultra-wideband and polarization-insensitive specular reflection reduction for both normal and wide-angle incidences. The proposed methodology opens up a new route for realizing ultra-wideband diffusion scattering of EM wave, which is important for stealth and other microwave applications in the future.

  7. Pulsed Laser Ablation-Induced Green Synthesis of TiO2 Nanoparticles and Application of Novel Small Angle X-Ray Scattering Technique for Nanoparticle Size and Size Distribution Analysis.

    PubMed

    Singh, Amandeep; Vihinen, Jorma; Frankberg, Erkka; Hyvärinen, Leo; Honkanen, Mari; Levänen, Erkki

    2016-12-01

    This paper aims to introduce small angle X-ray scattering (SAXS) as a promising technique for measuring size and size distribution of TiO 2 nanoparticles. In this manuscript, pulsed laser ablation in liquids (PLAL) has been demonstrated as a quick and simple technique for synthesizing TiO 2 nanoparticles directly into deionized water as a suspension from titanium targets. Spherical TiO 2 nanoparticles with diameters in the range 4-35 nm were observed with transmission electron microscopy (TEM). X-ray diffraction (XRD) showed highly crystalline nanoparticles that comprised of two main photoactive phases of TiO 2 : anatase and rutile. However, presence of minor amounts of brookite was also reported. The traditional methods for nanoparticle size and size distribution analysis such as electron microscopy-based methods are time-consuming. In this study, we have proposed and validated SAXS as a promising method for characterization of laser-ablated TiO 2 nanoparticles for their size and size distribution by comparing SAXS- and TEM-measured nanoparticle size and size distribution. SAXS- and TEM-measured size distributions closely followed each other for each sample, and size distributions in both showed maxima at the same nanoparticle size. The SAXS-measured nanoparticle diameters were slightly larger than the respective diameters measured by TEM. This was because SAXS measures an agglomerate consisting of several particles as one big particle which slightly increased the mean diameter. TEM- and SAXS-measured mean diameters when plotted together showed similar trend in the variation in the size as the laser power was changed which along with extremely similar size distributions for TEM and SAXS validated the application of SAXS for size distribution measurement of the synthesized TiO 2 nanoparticles.

  8. PREFACE: Structure and dynamics determined by neutron and x-ray scattering Structure and dynamics determined by neutron and x-ray scattering

    NASA Astrophysics Data System (ADS)

    Müller-Buschbaum, Peter

    2011-06-01

    Neutron and x-ray scattering have emerged as powerful methods for the determination of structure and dynamics. Driven by emerging new, powerful neutron and synchrotron radiation sources, the continuous development of new instrumentation and novel scattering techniques gives rise to exciting possibilities. For example, in situ observations become possible via a high neutron or x-ray flux at the sample and, as a consequence, morphological transitions with small time constants can be detected. This special issue covers a broad range of different materials from soft to hard condensed matter. Hence, different material classes such as colloids, polymers, alloys, oxides and metals are addressed. The issue is dedicated to the 60th birthday of Professor Winfried Petry, scientific director of the Research Neutron Source Heinz Maier-Leibnitz (FRM-II), Germany, advisor at the physics department for the Bayerische Elite-Akademie, chair person of the Arbeitsgemeinschaft Metall- und Materialphysik of the German Physical Society (DPG) and a member of the professional council of the German Science Foundation (Deutsche Forschungsgemeinschaft, DFG). We would like to acknowledge and thank all contributors for their submissions, which made this special issue possible in the first place. Moreover, we would like to thank the staff at IOP Publishing for helping us with the administrative aspects and for coordinating the refereeing process, and Valeria Lauter for the beautiful cover artwork. Finally, to the readers, we hope that you find this special issue a valuable resource that provides insights into the present possibilities of neutron and x-ray scattering as powerful tools for the investigation of structure and dynamics. Structure and dynamics determined by neutron and x-ray scattering contents In situ studies of mass transport in liquid alloys by means of neutron radiography F Kargl, M Engelhardt, F Yang, H Weis, P Schmakat, B Schillinger, A Griesche and A Meyer Magnetic spin

  9. Three-dimensional reciprocal space x-ray coherent scattering tomography of two-dimensional object.

    PubMed

    Zhu, Zheyuan; Pang, Shuo

    2018-04-01

    X-ray coherent scattering tomography is a powerful tool in discriminating biological tissues and bio-compatible materials. Conventional x-ray scattering tomography framework can only resolve isotropic scattering profile under the assumption that the material is amorphous or in powder form, which is not true especially for biological samples with orientation-dependent structure. Previous tomography schemes based on x-ray coherent scattering failed to preserve the scattering pattern from samples with preferred orientations, or required elaborated data acquisition scheme, which could limit its application in practical settings. Here, we demonstrate a simple imaging modality to preserve the anisotropic scattering signal in three-dimensional reciprocal (momentum transfer) space of a two-dimensional sample layer. By incorporating detector movement along the direction of x-ray beam, combined with a tomographic data acquisition scheme, we match the five dimensions of the measurements with the five dimensions (three in momentum transfer domain, and two in spatial domain) of the object. We employed a collimated pencil beam of a table-top copper-anode x-ray tube, along with a panel detector to investigate the feasibility of our method. We have demonstrated x-ray coherent scattering tomographic imaging at a spatial resolution ~2 mm and momentum transfer resolution 0.01 Å -1 for the rotation-invariant scattering direction. For any arbitrary, non-rotation-invariant direction, the same spatial and momentum transfer resolution can be achieved based on the spatial information from the rotation-invariant direction. The reconstructed scattering profile of each pixel from the experiment is consistent with the x-ray diffraction profile of each material. The three-dimensional scattering pattern recovered from the measurement reveals the partially ordered molecular structure of Teflon wrap in our sample. We extend the applicability of conventional x-ray coherent scattering tomography to

  10. Combination of acoustic levitation with small angle scattering techniques and synchrotron radiation circular dichroism. Application to the study of protein solutions.

    PubMed

    Cristiglio, Viviana; Grillo, Isabelle; Fomina, Margarita; Wien, Frank; Shalaev, Evgenyi; Novikov, Alexey; Brassamin, Séverine; Réfrégiers, Matthieu; Pérez, Javier; Hennet, Louis

    2017-01-01

    The acoustic levitation technique is a useful sample handling method for small solid and liquids samples, suspended in air by means of an ultrasonic field. This method was previously used at synchrotron sources for studying pharmaceutical liquids and protein solutions using x-ray diffraction and small angle x-ray scattering (SAXS). In this work we combined for the first time this containerless method with small angle neutron scattering (SANS) and synchrotron radiation circular dichroism (SRCD) to study the structural behavior of proteins in solutions during the water evaporation. SANS results are also compared with SAXS experiments. The aggregation behavior of 45μl droplets of lysozyme protein diluted in water was followed during the continuous increase of the sample concentration by evaporating the solvent. The evaporation kinetics was followed at different drying stage by SANS and SAXS with a good data quality. In a prospective work using SRCD, we also studied the evolution of the secondary structure of the myoglobin protein in water solution in the same evaporation conditions. Acoustic levitation was applied for the first time with SANS and the high performances of the used neutron instruments made it possible to monitor fast container-less reactions in situ. A preliminary work using SRCD shows the potentiality of its combination with acoustic levitation for studying the evolution of the protein structure with time. This multi-techniques approach could give novel insights into crystallization and self-assembly phenomena of biological compound with promising potential applications in pharmaceutical, food and cosmetics industry. This article is part of a Special Issue entitled "Science for Life" Guest Editor: Dr. Austen Angell, Dr. Salvatore Magazù and Dr. Federica Migliardo. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Air-core grid for scattered x-ray rejection

    DOEpatents

    Logan, C.M.; Lane, S.M.

    1995-10-03

    The invention is directed to a grid used in x-ray imaging applications to block scattered radiation while allowing the desired imaging radiation to pass through, and to process for making the grid. The grid is composed of glass containing lead oxide, and eliminates the spacer material used in prior known grids, and is therefore, an air-core grid. The glass is arranged in a pattern so that a large fraction of the area is open allowing the imaging radiation to pass through. A small pore size is used and the grid has a thickness chosen to provide high scatter rejection. For example, the grid may be produced with a 200 {micro}m pore size, 80% open area, and 4 mm thickness. 2 figs.

  12. Air-core grid for scattered x-ray rejection

    DOEpatents

    Logan, Clinton M.; Lane, Stephen M.

    1995-01-01

    The invention is directed to a grid used in x-ray imaging applications to block scattered radiation while allowing the desired imaging radiation to pass through, and to process for making the grid. The grid is composed of glass containing lead oxide, and eliminates the spacer material used in prior known grids, and is therefore, an air-core grid. The glass is arranged in a pattern so that a large fraction of the area is open allowing the imaging radiation to pass through. A small pore size is used and the grid has a thickness chosen to provide high scatter rejection. For example, the grid may be produced with a 200 .mu.m pore size, 80% open area, and 4 mm thickness.

  13. Diffuse x-ray scattering and transmission electron microscopy study of defects in antimony-implanted silicon

    NASA Astrophysics Data System (ADS)

    Takamura, Y.; Marshall, A. F.; Mehta, A.; Arthur, J.; Griffin, P. B.; Plummer, J. D.; Patel, J. R.

    2004-04-01

    Ion implantation followed by laser annealing has been used to create supersaturated and electrically active concentrations of antimony in silicon. Upon subsequent thermal annealing, however, these metastable dopants deactivate towards the equilibrium solubility limit. In this work, the formation of inactive antimony structures has been studied with grazing incidence diffuse x-ray scattering, and transmission electron microscopy, and the results are correlated to previous high-resolution x-ray diffraction data. We find that at a concentration of 6.0×1020 cm-3, small, incoherent clusters of radius 3-4 Å form during annealing at 900 °C. At a higher concentration of 2.2×1021 cm-3, deactivation at 600 °C occurs through the formation of small, antimony aggregates and antimony precipitates. The size of these precipitates from diffuse x-ray scattering is roughly 15 Å in radius for anneal times from 15 to 180 seconds. This value is consistent with the features observed in high-resolution and mass contrast transmission electron microscopy images. The coherent nature of the aggregates and precipitates causes the expansion of the surrounding silicon matrix as the deactivation progresses. In addition, the sensitivity of the diffuse x-ray scattering technique has allowed us to detect the presence of small clusters of radius ˜2 Å in unprocessed Czochralski silicon wafers. These defects are not observed in floating zone silicon wafers, and are tentatively attributed to thermal donors.

  14. Evaluation of solution stability for two-component polydisperse systems by small-angle scattering

    NASA Astrophysics Data System (ADS)

    Kryukova, A. E.; Konarev, P. V.; Volkov, V. V.

    2017-12-01

    The article is devoted to the modelling of small-angle scattering data using the program MIXTURE designed for the study of polydisperse multicomponent mixtures. In this work we present the results of solution stability studies for theoretical small-angle scattering data sets from two-component models. It was demonstrated that the addition of the noise to the data influences the stability range of the restored structural parameters. The recommendations for the optimal minimization schemes that permit to restore the volume size distributions for polydisperse systems are suggested.

  15. Survey of background scattering from materials found in small-angle neutron scattering.

    PubMed

    Barker, J G; Mildner, D F R

    2015-08-01

    Measurements and calculations of beam attenuation and background scattering for common materials placed in a neutron beam are presented over the temperature range of 300-700 K. Time-of-flight (TOF) measurements have also been made, to determine the fraction of the background that is either inelastic or quasi-elastic scattering as measured with a 3 He detector. Other background sources considered include double Bragg diffraction from windows or samples, scattering from gases, and phonon scattering from solids. Background from the residual air in detector vacuum vessels and scattering from the 3 He detector dome are presented. The thickness dependence of the multiple scattering correction for forward scattering from water is calculated. Inelastic phonon background scattering at small angles for crystalline solids is both modeled and compared with measurements. Methods of maximizing the signal-to-noise ratio by material selection, choice of sample thickness and wavelength, removal of inelastic background by TOF or Be filters, and removal of spin-flip scattering with polarized beam analysis are discussed.

  16. Survey of background scattering from materials found in small-angle neutron scattering

    PubMed Central

    Barker, J. G.; Mildner, D. F. R.

    2015-01-01

    Measurements and calculations of beam attenuation and background scattering for common materials placed in a neutron beam are presented over the temperature range of 300–700 K. Time-of-flight (TOF) measurements have also been made, to determine the fraction of the background that is either inelastic or quasi-elastic scattering as measured with a 3He detector. Other background sources considered include double Bragg diffraction from windows or samples, scattering from gases, and phonon scattering from solids. Background from the residual air in detector vacuum vessels and scattering from the 3He detector dome are presented. The thickness dependence of the multiple scattering correction for forward scattering from water is calculated. Inelastic phonon background scattering at small angles for crystalline solids is both modeled and compared with measurements. Methods of maximizing the signal-to-noise ratio by material selection, choice of sample thickness and wavelength, removal of inelastic background by TOF or Be filters, and removal of spin-flip scattering with polarized beam analysis are discussed. PMID:26306088

  17. Soft X-ray radiation damage in EM-CCDs used for Resonant Inelastic X-ray Scattering

    NASA Astrophysics Data System (ADS)

    Gopinath, D.; Soman, M.; Holland, A.; Keelan, J.; Hall, D.; Holland, K.; Colebrook, D.

    2018-02-01

    Advancement in synchrotron and free electron laser facilities means that X-ray beams with higher intensity than ever before are being created. The high brilliance of the X-ray beam, as well as the ability to use a range of X-ray energies, means that they can be used in a wide range of applications. One such application is Resonant Inelastic X-ray Scattering (RIXS). RIXS uses the intense and tuneable X-ray beams in order to investigate the electronic structure of materials. The photons are focused onto a sample material and the scattered X-ray beam is diffracted off a high resolution grating to disperse the X-ray energies onto a position sensitive detector. Whilst several factors affect the total system energy resolution, the performance of RIXS experiments can be limited by the spatial resolution of the detector used. Electron-Multiplying CCDs (EM-CCDs) at high gain in combination with centroiding of the photon charge cloud across several detector pixels can lead to sub-pixel spatial resolution of 2-3 μm. X-ray radiation can cause damage to CCDs through ionisation damage resulting in increases in dark current and/or a shift in flat band voltage. Understanding the effect of radiation damage on EM-CCDs is important in order to predict lifetime as well as the change in performance over time. Two CCD-97s were taken to PTB at BESSY II and irradiated with large doses of soft X-rays in order to probe the front and back surfaces of the device. The dark current was shown to decay over time with two different exponential components to it. This paper will discuss the use of EM-CCDs for readout of RIXS spectrometers, and limitations on spatial resolution, together with any limitations on instrument use which may arise from X-ray-induced radiation damage.

  18. Short-focus and ultra-wide-angle lens design in wavefront coding

    NASA Astrophysics Data System (ADS)

    Zhang, Jiyan; Huang, Yuanqing; Xiong, Feibing

    2016-10-01

    Wavefront coding (WFC) is a hybrid technology designed to increase depth of field of conventional optics. The goal of our research is to apply this technology to the short-focus and ultra-wide-angle lens which suffers from the aberration related with large field of view (FOV) such as coma and astigmatism. WFC can also be used to compensate for other aberration which is sensitive to the FOV. Ultra-wide-angle lens has a little depth of focus because it has small F number and short-focus. We design a hybrid lens combing WFC with the ultra-wide-angle lens. The full FOV and relative aperture of the final design are up to170° and 1/1.8 respectively. The focal length is 2 mm. We adopt the cubic phase mask (CPM) in the design. The conventional design will have a wide variation of the point spread function (PSF) across the FOV and it is very sensitive with the variation of the FOV. The new design we obtain the PSF is nearly invariant over the whole FOV. But the result of the design also shows the little difference between the horizontal and vertical length of the PSF. We analyze that the CPM is non-symmetric phase mask and the FOV is so large, which will generate variation in the final image quality. For that reason, we apply a new method to avoid that happened. We try to make the rays incident on the CPM with small angle and decrease the deformation of the PSF. The experimental result shows the new method to optimize the CPM is fit for the ultra-wide-angle lens. The research above will be a helpful instruction to design the ultra-wide-angle lens with WFC.

  19. Small-Angle X-Ray Scattering Analysis of the Bifunctional Antibiotic Resistance Enzyme Aminoglycoside (6′) Acetyltransferase-Ie/Aminoglycoside (2″) Phosphotransferase-Ia Reveals a Rigid Solution Structure

    PubMed Central

    Caldwell, Shane J.

    2012-01-01

    Aminoglycoside (6′) acetyltransferase-Ie/aminoglycoside (2″) phosphotransferase-Ia [AAC(6′)-Ie/APH(2″)-Ia] is one of the most problematic aminoglycoside resistance factors in clinical pathogens, conferring resistance to almost every aminoglycoside antibiotic available to modern medicine. Despite 3 decades of research, our understanding of the structure of this bifunctional enzyme remains limited. We used small-angle X-ray scattering (SAXS) to model the structure of this bifunctional enzyme in solution and to study the impact of substrate binding on the enzyme. It was observed that the enzyme adopts a rigid conformation in solution, where the N-terminal AAC domain is fixed to the C-terminal APH domain and not loosely tethered. The addition of acetyl-coenzyme A, coenzyme A, GDP, guanosine 5′-[β,γ-imido]triphosphate (GMPPNP), and combinations thereof to the protein resulted in only modest changes to the radius of gyration (RG) of the enzyme, which were not consistent with any large changes in enzyme structure upon binding. These results imply some selective advantage to the bifunctional enzyme beyond coexpression as a single polypeptide, likely linked to an improvement in enzymatic properties. We propose that the rigid structure contributes to improved electrostatic steering of aminoglycoside substrates toward the two active sites, which may provide such an advantage. PMID:22290965

  20. X-ray echo spectroscopy (Conference Presentation)

    NASA Astrophysics Data System (ADS)

    Shvyd'ko, Yuri V.

    2016-09-01

    X-ray echo spectroscopy, a counterpart of neutron spin-echo, was recently introduced [1] to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a point-like x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x-rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-meV and 0.02-meV ultra-high-resolution IXS applications (resolving power > 10^8) with broadband 5-13 meV dispersing systems will be presented featuring more than 1000-fold signal enhancement. The technique is general, applicable in different photon frequency domains. [1.] Yu. Shvyd'ko, Phys. Rev. Lett. 116, accepted (2016), arXiv:1511.01526.

  1. Direct measurement of the propagation velocity of defects using coherent X-rays

    DOE PAGES

    Ulbrandt, Jeffrey G.; Rainville, Meliha G.; Wagenbach, Christa; ...

    2016-03-28

    The properties of artificially grown thin films are often strongly affected by the dynamic relationships between surface growth processes and subsurface structure. Coherent mixing of X-ray signals promises to provide an approach to better understand such processes. Here, we demonstrate the continuously variable mixing of surface and bulk scattering signals during realtime studies of sputter deposition of a-Si and a-WSi2 films by controlling the X-ray penetration and escape depths in coherent grazing-incidence small-angle X-ray scattering. Under conditions where the X-ray signal comes from both the growth surface and the thin film bulk, oscillations in temporal correlations arise from coherent interferencemore » between scattering from stationary bulk features and from the advancing surface. We also observe evidence that elongated bulk features propagate upwards at the same velocity as the surface. Moreover, a highly surface-sensitive mode is demonstrated that can access the surface dynamics independently of the subsurface structure.« less

  2. Nonlinear X-Ray and Auger Spectroscopy at X-Ray Free-Electron Laser Sources

    NASA Astrophysics Data System (ADS)

    Rohringer, Nina

    2015-05-01

    X-ray free-electron lasers (XFELs) open the pathway to transfer non-linear spectroscopic techniques to the x-ray domain. A promising all x-ray pump probe technique is based on coherent stimulated electronic x-ray Raman scattering, which was recently demonstrated in atomic neon. By tuning the XFEL pulse to core-excited resonances, a few seed photons in the spectral tail of the XFEL pulse drive an avalanche of resonant inelastic x-ray scattering events, resulting in exponential amplification of the scattering signal by of 6-7 orders of magnitude. Analysis of the line profile of the emitted radiation permits to demonstrate the cross over from amplified spontaneous emission to coherent stimulated resonance scattering. In combination with statistical covariance mapping, a high-resolution spectrum of the resonant inelastic scattering process can be obtained, opening the path to coherent stimulated x-ray Raman spectroscopy. An extension of these ideas to molecules and a realistic feasibility study of stimulated electronic x-ray Raman scattering in CO will be presented. Challenges to realizing stimulated electronic x-ray Raman scattering at present-day XFEL sources will be discussed, corroborated by results of a recent experiment at the LCLS XFEL. Due to the small gain cross section in molecular targets, other nonlinear spectroscopic techniques such as nonlinear Auger spectroscopy could become a powerful alternative. Theory predictions of a novel pump probe technique based on resonant nonlinear Auger spectroscopic will be discussed and the method will be compared to stimulated x-ray Raman spectroscopy.

  3. Reaction of bone nanostructure to a biodegrading Magnesium WZ21 implant - A scanning small-angle X-ray scattering time study.

    PubMed

    Grünewald, T A; Ogier, A; Akbarzadeh, J; Meischel, M; Peterlik, H; Stanzl-Tschegg, S; Löffler, J F; Weinberg, A M; Lichtenegger, H C

    2016-02-01

    Understanding the implant-bone interaction is of prime interest for the development of novel biodegrading implants. Magnesium is a very promising material in the class of biodegrading metallic implants, owing to its mechanical properties and excellent immunologic response during healing. However, the influence of degrading Mg implants on the bone nanostructure is still an open question of crucial importance for the design of novel Mg implant alloys. This study investigates the changes in the nanostructure of bone following the application of a degrading WZ21 Mg implant (2wt% Y, 1wt% Zn, 0.25wt% Ca and 0.15wt% Mn) in a murine model system over the course of 15months by small angle X-ray scattering. Our investigations showed a direct response of the bone nanostructure after as little as 1month with a realignment of nano-sized bone mineral platelets along the bone-implant interface. The growth of new bone tissue after implant resorption is characterized by zones of lower mineral platelet thickness and slightly decreased order in the stacking of the platelets. The preferential orientation of the mineral platelets strongly deviates from the normal orientation along the shaft and still roughly follows the implant direction after 15months. We explain our findings by considering geometrical, mechanical and chemical factors during the process of implant resorption. The advancement of surgical techniques and the increased life expectancy have caused a growing demand for improved bone implants. Ideally, they should be bio-resorbable, support bone as long as necessary and then be replaced by healthy bone tissue. Magnesium is a promising candidate for this purpose. Various studies have demonstrated its excellent mechanical performance, degradation behaviour and immunologic properties. The structural response of bone, however, is not well known. On the nanometer scale, the arrangement of collagen fibers and calcium mineral platelets is an important indicator of structural

  4. X-Ray Absorption Measured in the Resonant Auger Scattering Mode

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

    Hikosaka, Y.; Shigemasa, E.; Kaneyasu, T.

    2008-08-15

    We report both experimental and theoretical studies on x-ray absorption measured in the resonant Auger scattering mode of gas phase carbon monoxide near the O1s{yields}2{pi} region. Both experiment and theory display a crucial difference between the x-ray absorption profiles obtained in the conventional and resonant scattering modes. Lifetime vibrational interference is the main source of the difference. It is demonstrated that such interference, which arises from a coherent excitation to overlapping intermediate levels, ruins the idea for obtaining x-ray absorption spectra in a lifetime broadening free regime.

  5. Bringing diffuse X-ray scattering into focus

    DOE PAGES

    Wall, Michael E.; Wolff, Alexander M.; Fraser, James S.

    2018-02-16

    X-ray crystallography is experiencing a renaissance as a method for probing the protein conformational ensemble. The inherent limitations of Bragg analysis, however, which only reveals the mean structure, have given way to a surge in interest in diffuse scattering, which is caused by structure variations. Diffuse scattering is present in all macromolecular crystallography experiments. Recent studies are shedding light on the origins of diffuse scattering in protein crystallography, and provide clues for leveraging diffuse scattering to model protein motions with atomic detail.

  6. Bringing diffuse X-ray scattering into focus

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

    Wall, Michael E.; Wolff, Alexander M.; Fraser, James S.

    X-ray crystallography is experiencing a renaissance as a method for probing the protein conformational ensemble. The inherent limitations of Bragg analysis, however, which only reveals the mean structure, have given way to a surge in interest in diffuse scattering, which is caused by structure variations. Diffuse scattering is present in all macromolecular crystallography experiments. Recent studies are shedding light on the origins of diffuse scattering in protein crystallography, and provide clues for leveraging diffuse scattering to model protein motions with atomic detail.

  7. Novel ultra-lightweight and high-resolution MEMS x-ray optics

    NASA Astrophysics Data System (ADS)

    Mitsuishi, Ikuyuki; Ezoe, Yuichiro; Takagi, Utako; Mita, Makoto; Riveros, Raul; Yamaguchi, Hitomi; Kato, Fumiki; Sugiyama, Susumu; Fujiwara, Kouzou; Morishita, Kohei; Nakajima, Kazuo; Fujihira, Shinya; Kanamori, Yoshiaki; Yamasaki, Noriko Y.; Mitsuda, Kazuhisa; Maeda, Ryutaro

    2009-05-01

    We have been developing ultra light-weight X-ray optics using MEMS (Micro Electro Mechanical Systems) technologies.We utilized crystal planes after anisotropic wet etching of silicon (110) wafers as X-ray mirrors and succeeded in X-ray reflection and imaging. Since we can etch tiny pores in thin wafers, this type of optics can be the lightest X-ray telescope. However, because the crystal planes are alinged in certain directions, we must approximate ideal optical surfaces with flat planes, which limits angular resolution of the optics on the order of arcmin. In order to overcome this issue, we propose novel X-ray optics based on a combination of five recently developed MEMS technologies, namely silicon dry etching, X-ray LIGA, silicon hydrogen anneal, magnetic fluid assisted polishing and hot plastic deformation of silicon. In this paper, we describe this new method and report on our development of X-ray mirrors fabricated by these technologies and X-ray reflection experiments of two types of MEMS X-ray mirrors made of silicon and nickel. For the first time, X-ray reflections on these mirrors were detected in the angular response measurements. Compared to model calculations, surface roughness of the silicon and nickel mirrors were estimated to be 5 nm and 3 nm, respectively.

  8. Spectrally resolving and scattering-compensated x-ray luminescence/fluorescence computed tomography

    PubMed Central

    Cong, Wenxiang; Shen, Haiou; Wang, Ge

    2011-01-01

    The nanophosphors, or other similar materials, emit near-infrared (NIR) light upon x-ray excitation. They were designed as optical probes for in vivo visualization and analysis of molecular and cellular targets, pathways, and responses. Based on the previous work on x-ray fluorescence computed tomography (XFCT) and x-ray luminescence computed tomography (XLCT), here we propose a spectrally-resolving and scattering-compensated x-ray luminescence/fluorescence computed tomography (SXLCT or SXFCT) approach to quantify a spatial distribution of nanophosphors (other similar materials or chemical elements) within a biological object. In this paper, the x-ray scattering is taken into account in the reconstruction algorithm. The NIR scattering is described in the diffusion approximation model. Then, x-ray excitations are applied with different spectra, and NIR signals are measured in a spectrally resolving fashion. Finally, a linear relationship is established between the nanophosphor distribution and measured NIR data using the finite element method and inverted using the compressive sensing technique. The numerical simulation results demonstrate the feasibility and merits of the proposed approach. PMID:21721815

  9. Effective phase function of light scattered at small angles by polydisperse particulate media

    NASA Astrophysics Data System (ADS)

    Turcu, I.

    2008-06-01

    Particles with typical dimensions higher than the light wavelength and relative refraction indexes close to one, scatter light mainly in the forward direction where the scattered light intensity has a narrow peak. For particulate media accomplishing these requirements the light scattered at small angles in a far-field detecting set-up can be described analytically by an effective phase function (EPF) even in the multiple scattering regime. The EPF model which was built for monodispersed systems has been extended to polydispersed media. The main ingredients consist in the replacement of the single particle phase function and of the optical thickness with their corresponding averaged values. Using a Gamma particle size distribution (PSD) as a testing model, the effect of polydispersity was systematically investigated. The increase of the average radius or/and of the PSD standard deviation leads to the decrease of the angular spreading of the small angle scattered light.

  10. A new ultrasonic transducer sample cell for in situ small-angle scattering experiments

    NASA Astrophysics Data System (ADS)

    Gupta, Sudipta; Bleuel, Markus; Schneider, Gerald J.

    2018-01-01

    Ultrasound irradiation is a commonly used technique for nondestructive diagnostics or targeted destruction. We report on a new versatile sonication device that fits in a variety of standard sample environments for neutron and X-ray scattering instruments. A piezoelectric transducer permits measuring of the time-dependent response of the sample in situ during or after sonication. We use small-angle neutron scattering (SANS) to demonstrate the effect of a time-dependent perturbation on the structure factor of micelles formed from sodium dodecyl sulfate surfactant molecules. We observe a substantial change in the micellar structure during and after exposure to ultrasonic irradiation. We also observe a time-dependent relaxation to the equilibrium values of the unperturbed system. The strength of the perturbation of the structure factor depends systematically on the duration of sonication. The relaxation behavior can be well reproduced after multiple times of sonication. Accumulation of the recorded intensities of the different sonication cycles improves the signal-to-noise ratio and permits reaching very short relaxation times. In addition, we present SANS data for the micellar form factor on alkyl-poly (ethylene oxide) surfactant molecules irradiated by ultrasound. Due to the flexibility of our new in situ sonication device, different experiments can be performed, e.g., to explore molecular potentials in more detail by introducing a systematic time-dependent perturbation.

  11. Small angle neutron scattering study of nano sized microstructure in Fe-Cr ODS steels for gen IV in-core applications.

    PubMed

    Han, Young-Soo; Mao, Xiadong; Jang, Jinsung

    2013-11-01

    The nano-sized microstructures in Fe-Cr oxide dispersion strengthened steel for Gen IV in-core applications were studied using small angle neutron scattering. The oxide dispersion strengthened steel was manufactured through hot isostatic pressing with various chemical compositions and fabrication conditions. Small angle neutron scattering experiments were performed using a 40 m small angle neutron scattering instrument at HANARO. Nano sized microstructures, namely, yttrium oxides and Cr-oxides were quantitatively analyzed by small angle neutron scattering. The yttrium oxides and Cr-oxides were also observed by transmission electron microscopy. The microstructural analysis results from small angle neutron scattering were compared with those obtained by transmission electron microscopy. The effects of the chemical compositions and fabrication conditions on the microstructure were investigated in relation to the quantitative microstructural analysis results obtained by small angle neutron scattering. The volume fraction of Y-oxide increases after fabrication, and this result is considered to be due to the formation of non-stochiometric Y-Ti-oxides.

  12. Upgrade of MacCHESS facility for X-ray scattering of biological macromolecules in solution

    PubMed Central

    Acerbo, Alvin Samuel; Cook, Michael J.; Gillilan, Richard Edward

    2015-01-01

    X-ray scattering of biological macromolecules in solution is an increasingly popular tool for structural biology and benefits greatly from modern high-brightness synchrotron sources. The upgraded MacCHESS BioSAXS station is now located at the 49-pole wiggler beamline G1. The 20-fold improved flux over the previous beamline F2 provides higher sample throughput and autonomous X-ray scattering data collection using a unique SAXS/WAXS dual detectors configuration. This setup achieves a combined q-range from 0.007 to 0.7 Å−1, enabling better characterization of smaller molecules, while opening opportunities for emerging wide-angle scattering methods. In addition, a facility upgrade of the positron storage ring to continuous top-up mode has improved beam stability and eliminated beam drift over the course of typical BioSAXS experiments. Single exposure times have been reduced to 2 s for 3.560 mg ml−1 lysozyme with an average quality factor I/σ of 20 in the Guinier region. A novel disposable plastic sample cell design that incorporates lower background X-ray window material provides users with a more pristine sample environment than previously available. Systematic comparisons of common X-ray window materials bonded to the cell have also been extended to the wide-angle regime, offering new insight into best choices for various q-space ranges. In addition, a quantitative assessment of signal-to-noise levels has been performed on the station to allow users to estimate necessary exposure times for obtaining usable signals in the Guinier regime. Users also have access to a new BioSAXS sample preparation laboratory which houses essential wet-chemistry equipment and biophysical instrumentation. User experiments at the upgraded BioSAXS station have been on-going since commissioning of the beamline in Summer 2013. A planned upgrade of the G1 insertion device to an undulator for the Winter 2014 cycle is expected to further improve flux by an order of magnitude. PMID

  13. Improved In vivo Assessment of Pulmonary Fibrosis in Mice using X-Ray Dark-Field Radiography

    NASA Astrophysics Data System (ADS)

    Yaroshenko, Andre; Hellbach, Katharina; Yildirim, Ali Önder; Conlon, Thomas M.; Fernandez, Isis Enlil; Bech, Martin; Velroyen, Astrid; Meinel, Felix G.; Auweter, Sigrid; Reiser, Maximilian; Eickelberg, Oliver; Pfeiffer, Franz

    2015-12-01

    Idiopathic pulmonary fibrosis (IPF) is a chronic and progressive lung disease with a median life expectancy of 4-5 years after initial diagnosis. Early diagnosis and accurate monitoring of IPF are limited by a lack of sensitive imaging techniques that are able to visualize early fibrotic changes at the epithelial-mesenchymal interface. Here, we report a new x-ray imaging approach that directly visualizes the air-tissue interfaces in mice in vivo. This imaging method is based on the detection of small-angle x-ray scattering that occurs at the air-tissue interfaces in the lung. Small-angle scattering is detected with a Talbot-Lau interferometer, which provides the so-called x-ray dark-field signal. Using this imaging modality, we demonstrate-for the first time-the quantification of early pathogenic changes and their correlation with histological changes, as assessed by stereological morphometry. The presented radiography method is significantly more sensitive in detecting morphological changes compared with conventional x-ray imaging, and exhibits a significantly lower radiation dose than conventional x-ray CT. As a result of the improved imaging sensitivity, this new imaging modality could be used in future to reduce the number of animals required for pulmonary research studies.

  14. The INTEGRAL long monitoring of persistent ultra compact X-ray bursters

    NASA Astrophysics Data System (ADS)

    Fiocchi, M.; Bazzano, A.; Ubertini, P.; Bird, A. J.; Natalucci, L.; Sguera, V.

    2008-12-01

    Context: The combination of compact objects, short period variability and peculiar chemical composition of the ultra compact X-ray binaries make up a very interesting laboratory to study accretion processes and thermonuclear burning on the neutron star surface. Improved large optical telescopes and more sensitive X-ray satellites have increased the number of known ultra compact X-ray binaries allowing their study with unprecedented detail. Aims: We analyze the average properties common to all ultra compact bursters observed by INTEGRAL from 0.2 keV to 150 keV. Methods: We have performed a systematic analysis of the INTEGRAL public data and Key-Program proprietary observations of a sample of the ultra compact X-ray binaries. In order to study their average properties in a very broad energy band, we combined INTEGRAL with BeppoSAX and SWIFT data whenever possible. For sources not showing any significant flux variations along the INTEGRAL monitoring, we build the average spectrum by combining all available data; in the case of variable fluxes, we use simultaneous INTEGRAL and SWIFT observations when available. Otherwise we compared IBIS and PDS data to check the variability and combine BeppoSAX with INTEGRAL /IBIS data. Results: All spectra are well represented by a two component model consisting of a disk-blackbody and Comptonised emission. The majority of these compact sources spend most of the time in a canonical low/hard state, with a dominating Comptonised component and accretion rate dot {M} lower than 10-9 {M⊙}/yr, not depending on the model used to fit the data. INTEGRAL is an ESA project with instruments and Science Data Center funded by ESA member states (especially the PI countries: Denmark, France, Germany, Italy, Switzerland, Spain), Czech Republic and Poland, and with the participation of Russia and the USA.

  15. Femtosecond response of polyatomic molecules to ultra-intense hard X-rays.

    PubMed

    Rudenko, A; Inhester, L; Hanasaki, K; Li, X; Robatjazi, S J; Erk, B; Boll, R; Toyota, K; Hao, Y; Vendrell, O; Bomme, C; Savelyev, E; Rudek, B; Foucar, L; Southworth, S H; Lehmann, C S; Kraessig, B; Marchenko, T; Simon, M; Ueda, K; Ferguson, K R; Bucher, M; Gorkhover, T; Carron, S; Alonso-Mori, R; Koglin, J E; Correa, J; Williams, G J; Boutet, S; Young, L; Bostedt, C; Son, S-K; Santra, R; Rolles, D

    2017-06-01

    X-ray free-electron lasers enable the investigation of the structure and dynamics of diverse systems, including atoms, molecules, nanocrystals and single bioparticles, under extreme conditions. Many imaging applications that target biological systems and complex materials use hard X-ray pulses with extremely high peak intensities (exceeding 10 20 watts per square centimetre). However, fundamental investigations have focused mainly on the individual response of atoms and small molecules using soft X-rays with much lower intensities. Studies with intense X-ray pulses have shown that irradiated atoms reach a very high degree of ionization, owing to multiphoton absorption, which in a heteronuclear molecular system occurs predominantly locally on a heavy atom (provided that the absorption cross-section of the heavy atom is considerably larger than those of its neighbours) and is followed by efficient redistribution of the induced charge. In serial femtosecond crystallography of biological objects-an application of X-ray free-electron lasers that greatly enhances our ability to determine protein structure-the ionization of heavy atoms increases the local radiation damage that is seen in the diffraction patterns of these objects and has been suggested as a way of phasing the diffraction data. On the basis of experiments using either soft or less-intense hard X-rays, it is thought that the induced charge and associated radiation damage of atoms in polyatomic molecules can be inferred from the charge that is induced in an isolated atom under otherwise comparable irradiation conditions. Here we show that the femtosecond response of small polyatomic molecules that contain one heavy atom to ultra-intense (with intensities approaching 10 20 watts per square centimetre), hard (with photon energies of 8.3 kiloelectronvolts) X-ray pulses is qualitatively different: our experimental and modelling results establish that, under these conditions, the ionization of a molecule is

  16. Femtosecond response of polyatomic molecules to ultra-intense hard X-rays

    DOE PAGES

    Rudenko, A.; Inhester, L.; Hanasaki, K.; ...

    2017-05-31

    We report x-ray free-electron lasers enable the investigation of the structure and dynamics of diverse systems, including atoms, molecules, nanocrystals and single bioparticles, under extreme conditions. Many imaging applications that target biological systems and complex materials use hard X-ray pulses with extremely high peak intensities (exceeding 10 20 watts per square centimetre). However, fundamental investigations have focused mainly on the individual response of atoms and small molecules using soft X-rays with much lower intensities. Studies with intense X-ray pulses have shown that irradiated atoms reach a very high degree of ionization, owing to multiphoton absorption, which in a heteronuclear molecularmore » system occurs predominantly locally on a heavy atom (provided that the absorption cross-section of the heavy atom is considerably larger than those of its neighbours) and is followed by efficient redistribution of the induced charge. In serial femtosecond crystallography of biological objects—an application of X-ray free-electron lasers that greatly enhances our ability to determine protein structure—the ionization of heavy atoms increases the local radiation damage that is seen in the diffraction patterns of these objects and has been suggested as a way of phasing the diffraction data. On the basis of experiments using either soft or less-intense hard X-rays, it is thought that the induced charge and associated radiation damage of atoms in polyatomic molecules can be inferred from the charge that is induced in an isolated atom under otherwise comparable irradiation conditions. Here we show that the femtosecond response of small polyatomic molecules that contain one heavy atom to ultra-intense (with intensities approaching 10 20 watts per square centimetre), hard (with photon energies of 8.3 kiloelectronvolts) X-ray pulses is qualitatively different: our experimental and modelling results establish that, under these conditions, the ionization

  17. Femtosecond response of polyatomic molecules to ultra-intense hard X-rays

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

    Rudenko, A.; Inhester, L.; Hanasaki, K.

    We report x-ray free-electron lasers enable the investigation of the structure and dynamics of diverse systems, including atoms, molecules, nanocrystals and single bioparticles, under extreme conditions. Many imaging applications that target biological systems and complex materials use hard X-ray pulses with extremely high peak intensities (exceeding 10 20 watts per square centimetre). However, fundamental investigations have focused mainly on the individual response of atoms and small molecules using soft X-rays with much lower intensities. Studies with intense X-ray pulses have shown that irradiated atoms reach a very high degree of ionization, owing to multiphoton absorption, which in a heteronuclear molecularmore » system occurs predominantly locally on a heavy atom (provided that the absorption cross-section of the heavy atom is considerably larger than those of its neighbours) and is followed by efficient redistribution of the induced charge. In serial femtosecond crystallography of biological objects—an application of X-ray free-electron lasers that greatly enhances our ability to determine protein structure—the ionization of heavy atoms increases the local radiation damage that is seen in the diffraction patterns of these objects and has been suggested as a way of phasing the diffraction data. On the basis of experiments using either soft or less-intense hard X-rays, it is thought that the induced charge and associated radiation damage of atoms in polyatomic molecules can be inferred from the charge that is induced in an isolated atom under otherwise comparable irradiation conditions. Here we show that the femtosecond response of small polyatomic molecules that contain one heavy atom to ultra-intense (with intensities approaching 10 20 watts per square centimetre), hard (with photon energies of 8.3 kiloelectronvolts) X-ray pulses is qualitatively different: our experimental and modelling results establish that, under these conditions, the ionization

  18. Using acoustic levitation in synchrotron based laser pump hard x-ray probe experiments

    NASA Astrophysics Data System (ADS)

    Hu, Bin; Lerch, Jason; Suthar, Kamlesh; Dichiara, Anthony

    Acoustic levitation provides a platform to trap and hold a small amount of material by using standing pressure waves without a container. The technique has a potential to be used for laser pump x-ray probe experiments; x-ray scattering and laser distortion from the container can be avoided, sample consumption can be minimized, and unwanted chemistry that may occur at the container interface can be avoided. The method has been used at synchrotron sources for studying protein and pharmaceutical solutions using x-ray diffraction (XRD) and small angle x-ray scattering (SAXS). However, pump-probe experiments require homogeneously excited samples, smaller than the absorption depth of the material that must be held stably at the intersection of both the laser and x-ray beams. We discuss 1) the role of oscillations in acoustic levitation and the optimal acoustic trapping conditions for x-ray/laser experiments, 2) opportunities to automate acoustic levitation for fast sample loading and manipulation, and 3) our experimental results using SAXS to monitor laser induced thermal expansion in gold nanoparticles solution. We also performed Finite Element Analysis to optimize the trapping performance and stability of droplets ranging from 0.4 mm to 2 mm. Our early x-ray/laser demonstrated the potential of the technique for time-resolved X-ray science.

  19. Surface layering and melting in an ionic liquid studied by resonant soft X-ray reflectivity

    PubMed Central

    Mezger, Markus; Ocko, Benjamin M.; Reichert, Harald; Deutsch, Moshe

    2013-01-01

    The molecular-scale structure of the ionic liquid [C18mim]+[FAP]− near its free surface was studied by complementary methods. X-ray absorption spectroscopy and resonant soft X-ray reflectivity revealed a depth-decaying near-surface layering. Element-specific interfacial profiles were extracted with submolecular resolution from energy-dependent soft X-ray reflectivity data. Temperature-dependent hard X-ray reflectivity, small- and wide-angle X-ray scattering, and infrared spectroscopy uncovered an intriguing melting mechanism for the layered region, where alkyl chain melting drove a negative thermal expansion of the surface layer spacing. PMID:23431181

  20. Determination of coal ash content by the combined x-ray fluorescence and scattering spectrum

    NASA Astrophysics Data System (ADS)

    Mikhailov, I. F.; Baturin, A. A.; Mikhailov, A. I.; Borisova, S. S.; Fomina, L. P.

    2018-02-01

    An alternative method is proposed for the determination of the inorganic constituent mass fraction (ash) in solid fuel by the ratio of Compton and Rayleigh X-ray scattering peaks IC/IR subject to the iron fluorescence intensity. An original X-ray optical scheme with a Ti/Mo (or Sc/Cu) double-layer secondary radiator allows registration of the combined fluorescence-and-scattering spectrum at the specified scattering angle. An algorithm for linear calibration of the Compton-to-Rayleigh IC/IR ratio is proposed which uses standard samples with two certified characteristics: mass fractions of ash (Ad) and iron oxide (WFe2O3). Ash mass fractions have been determined for coals of different deposits in the wide range of Ad from 9.4% to 52.7% mass and WFe2O3 from 0.3% to 4.95% mass. Due to the high penetrability of the probing radiation with energy E > 17 keV, the sample preparation procedure is rather simplified in comparison with the traditional method of Ad determination by the sum of fluorescence intensities of all constituent elements.

  1. Toroidal silicon polarization analyzer for resonant inelastic x-ray scattering

    DOE PAGES

    Gao, Xuan; Casa, Diego; Kim, Jungho; ...

    2016-08-15

    Resonant Inelastic X-ray Scattering (RIXS) is a powerful probe for studying electronic excitations in materials. Standard high energy RIXS measurements do not measure the polarization of the scattered x-rays, which is unfortunate since it carries information about the nature and symmetry of the excitations involved in the scattering process. Moreover we report the fabrication of thin Si-based polarization analyzers with a double-concave toroidal surface, useful for L-edge RIXS studies in heavier atoms such as the 5-d transition metals.

  2. The life science X-ray scattering beamline at NSLS-II

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

    DiFabio, Jonathan; Yang, Lin; Chodankar, Shirish

    We report the current development status of the High Brightness X-ray Scattering for Life Sciences (or Life Science X-ray Scattering, LiX) beamline at the NSLS-II facility of Brookhaven National Laboratory. This instrument will operate in the x-ray energy range of 2.1-18 keV, provide variable beam sizes from 1 micron to ~0.5 mm, and support user experiments in three scientific areas: (1) high-throughput solution scattering, in-line size exclusion chromatography and flow mixers-based time-resolved solution scattering of biological macro-molecules, (2) diffraction from single- and multi-layered lipid membranes, and (3) scattering-based scanning probe imaging of biological tissues. In order to satisfy the beammore » stability required for these experiments and to switch rapidly between different types of experiments, we have adopted a secondary source with refractive lenses for secondary focusing, a detector system consisting of three Pilatus detectors, and specialized experimental modules that can be quickly exchanged and each dedicated to a defined set of experiments. The construction of this beamline is on schedule for completion in September 2015. User experiments are expected to start in Spring 2016.« less

  3. The life science X-ray scattering beamline at NSLS-II

    DOE PAGES

    DiFabio, Jonathan; Yang, Lin; Chodankar, Shirish; ...

    2015-09-30

    We report the current development status of the High Brightness X-ray Scattering for Life Sciences (or Life Science X-ray Scattering, LiX) beamline at the NSLS-II facility of Brookhaven National Laboratory. This instrument will operate in the x-ray energy range of 2.1-18 keV, provide variable beam sizes from 1 micron to ~0.5 mm, and support user experiments in three scientific areas: (1) high-throughput solution scattering, in-line size exclusion chromatography and flow mixers-based time-resolved solution scattering of biological macro-molecules, (2) diffraction from single- and multi-layered lipid membranes, and (3) scattering-based scanning probe imaging of biological tissues. In order to satisfy the beammore » stability required for these experiments and to switch rapidly between different types of experiments, we have adopted a secondary source with refractive lenses for secondary focusing, a detector system consisting of three Pilatus detectors, and specialized experimental modules that can be quickly exchanged and each dedicated to a defined set of experiments. The construction of this beamline is on schedule for completion in September 2015. User experiments are expected to start in Spring 2016.« less

  4. The life science x-ray scattering beamline at NSLS-II

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

    DiFabio, Jonathan; Chodankar, Shirish; Pjerov, Sal

    We report the current development status of the High Brightness X-ray Scattering for Life Sciences (or Life Science X-ray Scattering, LiX) beamline at the NSLS-II facility of Brookhaven National Laboratory. This instrument will operate in the x-ray energy range of 2.1-18 keV, provide variable beam sizes from 1 micron to ∼0.5 mm, and support user experiments in three scientific areas: (1) high-throughput solution scattering, in-line size exclusion chromatography and flow mixers-based time-resolved solution scattering of biological macro-molecules, (2) diffraction from single- and multi-layered lipid membranes, and (3) scattering-based scanning probe imaging of biological tissues. In order to satisfy the beammore » stability required for these experiments and to switch rapidly between different types of experiments, we have adopted a secondary source with refractive lenses for secondary focusing, a detector system consisting of three Pilatus detectors, and specialized experimental modules that can be quickly exchanged and each dedicated to a defined set of experiments. The construction of this beamline is on schedule for completion in September 2015. User experiments are expected to start in Spring 2016.« less

  5. Calculation of x-ray scattering patterns from nanocrystals at high x-ray intensity

    PubMed Central

    Abdullah, Malik Muhammad; Jurek, Zoltan; Son, Sang-Kil; Santra, Robin

    2016-01-01

    We present a generalized method to describe the x-ray scattering intensity of the Bragg spots in a diffraction pattern from nanocrystals exposed to intense x-ray pulses. Our method involves the subdivision of a crystal into smaller units. In order to calculate the dynamics within every unit, we employ a Monte-Carlo-molecular dynamics-ab-initio hybrid framework using real space periodic boundary conditions. By combining all the units, we simulate the diffraction pattern of a crystal larger than the transverse x-ray beam profile, a situation commonly encountered in femtosecond nanocrystallography experiments with focused x-ray free-electron laser radiation. Radiation damage is not spatially uniform and depends on the fluence associated with each specific region inside the crystal. To investigate the effects of uniform and non-uniform fluence distribution, we have used two different spatial beam profiles, Gaussian and flattop. PMID:27478859

  6. Multiplexed high resolution soft x-ray RIXS

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

    Chuang, Y.-D.; Voronov, D.; Warwick, T.

    2016-07-27

    High-resolution Resonance Inelastic X-ray Scattering (RIXS) is a technique that allows us to probe the electronic excitations of complex materials with unprecedented precision. However, the RIXS process has a low cross section, compounded by the fact that the optical spectrometers used to analyze the scattered photons can only collect a small solid angle and overall have a small efficiency. Here we present a method to significantly increase the throughput of RIXS systems, by energy multiplexing, so that a complete RIXS map of scattered intensity versus photon energy in and photon energy out can be recorded simultaneously{sup 1}. This parallel acquisitionmore » scheme should provide a gain in throughput of over 100.. A system based on this principle, QERLIN, is under construction at the Advanced Light Source (ALS).« less

  7. Observations of Intermediate-mass Black Holes and Ultra-Luminous X-ray sources

    NASA Astrophysics Data System (ADS)

    Colbert, E. J. M.

    2003-12-01

    I will review various observations that suggest that intermediate-mass black holes (IMBHs) with masses ˜102-104 M⊙ exist in our Universe. I will also discuss some of the limitations of these observations. HST Observations of excess dark mass in globular cluster cores suggest IMBHs may be responsible, and some mass estimates from lensing experiments are nearly in the IMBH range. The intriguing Ultra-Luminous X-ray sources (ULXs, or IXOs) are off-nuclear X-ray point sources with X-ray luminosities LX ≳ 1039 erg s-1. ULXs are typically rare (1 in every 5 galaxies), and the nature of their ultra-luminous emission is currently debated. I will discuss the evidence for IMBHs in some ULXs, and briefly outline some phenomenology. Finally, I will discuss future observations that can be made to search for IMBHs.

  8. Compton scattering artifacts in electron excited X-ray spectra measured with a silicon drift detector.

    PubMed

    Ritchie, Nicholas W M; Newbury, Dale E; Lindstrom, Abigail P

    2011-12-01

    Artifacts are the nemesis of trace element analysis in electron-excited energy dispersive X-ray spectrometry. Peaks that result from nonideal behavior in the detector or sample can fool even an experienced microanalyst into believing that they have trace amounts of an element that is not present. Many artifacts, such as the Si escape peak, absorption edges, and coincidence peaks, can be traced to the detector. Others, such as secondary fluorescence peaks and scatter peaks, can be traced to the sample. We have identified a new sample-dependent artifact that we attribute to Compton scattering of energetic X-rays generated in a small feature and subsequently scattered from a low atomic number matrix. It seems likely that this artifact has not previously been reported because it only occurs under specific conditions and represents a relatively small signal. However, with the advent of silicon drift detectors and their utility for trace element analysis, we anticipate that more people will observe it and possibly misidentify it. Though small, the artifact is not inconsequential. Under some conditions, it is possible to mistakenly identify the Compton scatter artifact as approximately 1% of an element that is not present.

  9. Ultra-wideband, Wide Angle and Polarization-insensitive Specular Reflection Reduction by Metasurface based on Parameter-adjustable Meta-Atoms

    PubMed Central

    Su, Jianxun; Lu, Yao; Zhang, Hui; Li, Zengrui; (Lamar) Yang, Yaoqing; Che, Yongxing; Qi, Kainan

    2017-01-01

    In this paper, an ultra-wideband, wide angle and polarization-insensitive metasurface is designed, fabricated, and characterized for suppressing the specular electromagnetic wave reflection or backward radar cross section (RCS). Square ring structure is chosen as the basic meta-atoms. A new physical mechanism based on size adjustment of the basic meta-atoms is proposed for ultra-wideband manipulation of electromagnetic (EM) waves. Based on hybrid array pattern synthesis (APS) and particle swarm optimization (PSO) algorithm, the selection and distribution of the basic meta-atoms are optimized simultaneously to obtain the ultra-wideband diffusion scattering patterns. The metasurface can achieve an excellent RCS reduction in an ultra-wide frequency range under x- and y-polarized normal incidences. The new proposed mechanism greatly extends the bandwidth of RCS reduction. The simulation and experiment results show the metasurface can achieve ultra-wideband and polarization-insensitive specular reflection reduction for both normal and wide-angle incidences. The proposed methodology opens up a new route for realizing ultra-wideband diffusion scattering of EM wave, which is important for stealth and other microwave applications in the future. PMID:28181593

  10. Surface Pb nanoparticle aggregation, coalescence and differential capacitance in a deep eutectic solvent using a simultaneous sample-rotated small angle x-ray scattering and electrochemical methods approach [Surface Pb nanoparticle aggregation, coalescence and differential capacitance in a deep eutectic solvent using a simultaneous grazing transmission small angle x-ray scattering and electrochemical methods approach

    DOE PAGES

    Hammons, Joshua A.; Ilavsky, Jan

    2017-01-18

    Nanoparticle electrodeposition is a simple and scalable approach to synthesizing supported nanoparticles. Used with a deep eutectic solvent (DES), surface nanoparticles can be assembled and exhibit unique surface charge separation when the DES is adsorbed on the nanoparticle surface. Key to understanding and controlling the assembly and the capacitance is a thorough understanding of surface particle mobility and charge screening, which requires an in-situ approach. In this study, Pb particle formation, size, shape and capacitance are resolved in a 1:2 choline Cl –: urea deep eutectic solvent whilst sweeping the cell potential in the range: 0.2 V to –1.2 Vmore » (vs. Ag/AgCl). These system parameters were resolved using a complementary suite of sample-rotated small angle X-ray scattering (SR-SAXS) and electrochemical impedance spectroscopy (EIS), which are presented and discussed in detail. This approach is able to show that both particle and ion transport are impeded in the DES, as aggregation occurs over the course of 6 minutes, and dissolved Pb ions accumulate and remain near the surface after a nucleation pulse is applied. The DES-Pb interactions strongly depend on the cell potential as evidenced by the specific differential capacitance of the Pb deposit, which has a maximum value of 2.5 +/– 0.5 F g –1 at –1.0 V vs. Ag/AgCl. Together, the SR-SAXS-EIS approach is able to characterize the unique nanoparticle capacitance, mobility and ion mobility in a DES and can be used to study a wide range of nanoparticle deposition systems in-situ.« less

  11. Surface Pb nanoparticle aggregation, coalescence and differential capacitance in a deep eutectic solvent using a simultaneous sample-rotated small angle x-ray scattering and electrochemical methods approach [Surface Pb nanoparticle aggregation, coalescence and differential capacitance in a deep eutectic solvent using a simultaneous grazing transmission small angle x-ray scattering and electrochemical methods approach

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

    Hammons, Joshua A.; Ilavsky, Jan

    Nanoparticle electrodeposition is a simple and scalable approach to synthesizing supported nanoparticles. Used with a deep eutectic solvent (DES), surface nanoparticles can be assembled and exhibit unique surface charge separation when the DES is adsorbed on the nanoparticle surface. Key to understanding and controlling the assembly and the capacitance is a thorough understanding of surface particle mobility and charge screening, which requires an in-situ approach. In this study, Pb particle formation, size, shape and capacitance are resolved in a 1:2 choline Cl –: urea deep eutectic solvent whilst sweeping the cell potential in the range: 0.2 V to –1.2 Vmore » (vs. Ag/AgCl). These system parameters were resolved using a complementary suite of sample-rotated small angle X-ray scattering (SR-SAXS) and electrochemical impedance spectroscopy (EIS), which are presented and discussed in detail. This approach is able to show that both particle and ion transport are impeded in the DES, as aggregation occurs over the course of 6 minutes, and dissolved Pb ions accumulate and remain near the surface after a nucleation pulse is applied. The DES-Pb interactions strongly depend on the cell potential as evidenced by the specific differential capacitance of the Pb deposit, which has a maximum value of 2.5 +/– 0.5 F g –1 at –1.0 V vs. Ag/AgCl. Together, the SR-SAXS-EIS approach is able to characterize the unique nanoparticle capacitance, mobility and ion mobility in a DES and can be used to study a wide range of nanoparticle deposition systems in-situ.« less

  12. New contrasts for x-ray imaging and synergy with optical imaging

    NASA Astrophysics Data System (ADS)

    Wang, Ge

    2017-02-01

    Due to its penetrating power, fine resolution, unique contrast, high-speed, and cost-effectiveness, x-ray imaging is one of the earliest and most popular imaging modalities in biomedical applications. Current x-ray radiographs and CT images are mostly on gray-scale, since they reflect overall energy attenuation. Recent advances in x-ray detection, contrast agent, and image reconstruction technologies have changed our perception and expectation of x-ray imaging capabilities, and generated an increasing interest in imaging biological soft tissues in terms of energy-sensitive material decomposition, phase-contrast, small angle scattering (also referred to as dark-field), x-ray fluorescence and luminescence properties. These are especially relevant to preclinical and mesoscopic studies, and potentially mendable for hybridization with optical molecular tomography. In this article, we review new x-ray imaging techniques as related to optical imaging, suggest some combined x-ray and optical imaging schemes, and discuss our ideas on micro-modulated x-ray luminescence tomography (MXLT) and x-ray modulated opto-genetics (X-Optogenetics).

  13. Structural analysis of polymer thin films using GISAXS in the tender X-ray region: Concept and design of GISAXS experiments using the tender X-ray energy at BL-15A2 at the Photon Factory

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

    Takagi, H., E-mail: takagih@post.kek.jp; Igarashi, N.; Mori, T.

    If small angle X-ray scattering (SAXS) utilizing the soft X-ray region is available, advanced and unique experiments, which differ from traditional SAXS methods, can be realized. For example, grazing-incidence small angle X-ray scattering (GISAXS) using hard X-ray is a powerful tool for understanding the nanostructure in both vertical and lateral directions of thin films, while GISAXS utilizing the tender X-ray region (SX-GISAXS) enables depth-resolved analysis as well as a standard GISAXS analysis in thin films. Thus, at BL-15A2 at the Photon Factory, a dedicated diffractometer for SX-GISAXS (above 2.1 keV) was constructed. This diffractometer is composed of four vacuum chambers andmore » can be converted into the vacuum state from the sample chamber in front of the detector surface. Diffractions are clearly observed until 12th peak when measuring collagen by SAXS with an X-ray energy of 2.40 keV and a camera length of 825 mm. Additionally, we conducted the model experiment using SX-GISAXS with an X-ray energy of 2.40 keV to confirm that a poly(methyl methacrylate)-poly(n-butyl acrylate) block copolymer thin film has a microphase-separated structure in the thin film, which is composed of lamellae aligned both parallel and perpendicular to the substrate surface. Similarly, in a polystyrene-poly(methyl methacrylate) block copolymer thin film, SX-GISAXS with 3.60 keV and 5.73 keV revealed that hexagonally packed cylinders are aligned parallel to the substrate surface. The incident angle dependence of the first order peak position of the q{sub z} direction obtained from experiments at various incident X-ray energies agrees very well with the theoretical one calculated from the distorted wave Born approximation.« less

  14. Clusters in intense x-ray pulses

    NASA Astrophysics Data System (ADS)

    Bostedt, Christoph

    2012-06-01

    Free-electron lasers can deliver extremely intense, coherent x-ray flashes with femtosecond pulse length, opening the door for imaging single nanoscale objects in a single shot. All matter irradiated by these intense x-ray pulses, however, will be transformed into a highly-excited non-equilibrium plasma within femtoseconds. During the x-ray pulse complex electron dynamics and the onset of atomic disorder will be induced, leading to a time-varying sample. We have performed first experiments about x-ray laser pulse -- cluster interaction with a combined spectroscopy and imaging approach at both, the FLASH free electron laser in Hamburg (Germany) and the LCLS x-ray free-electron laser in Stanford (California). Atomic clusters are ideal for investigating the light - matter interaction because their size can be tuned from the molecular to the bulk regime, thus allowing to distinguish between intra and inter atomic processes. Imaging experiments with xenon clusters show power-density dependent changes in the scattering patterns. Modeling the scattering data indicates that the optical constants of the clusters change during the femtosecond pulse due to the transient creation of high charge states. The results show that ultra fast scattering is a promising approach to study transient states of matter on a femtosecond time scale. Coincident recording of time-of-flight spectra and scattering patterns allows the deconvolution of focal volume and particle size distribution effects. Single-shot single-particle experiments with keV x-rays reveal that for the highest power densities an highly excited and hot cluster plasma is formed for which recombination is suppressed. Time resolved infrared pump -- x-ray probe experiments have started. Here, the clusters are pumped into a nanoplasma state and their time evolution is probed with femtosecond x-ray scattering. The data show strong variations in the scattering patterns stemming from electronic reconfigurations in the cluster

  15. Development of an x-ray prism for analyzer based imaging systems

    NASA Astrophysics Data System (ADS)

    Bewer, Brian; Chapman, Dean

    2010-08-01

    Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP) was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.

  16. Development of an x-ray prism for analyzer based imaging systems.

    PubMed

    Bewer, Brian; Chapman, Dean

    2010-08-01

    Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP) was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.

  17. Wide-angle x-ray scattering and solid-state nuclear magnetic resonance data combined to test models for cellulose microfibrils in mung bean cell walls.

    PubMed

    Newman, Roger H; Hill, Stefan J; Harris, Philip J

    2013-12-01

    A synchrotron wide-angle x-ray scattering study of mung bean (Vigna radiata) primary cell walls was combined with published solid-state nuclear magnetic resonance data to test models for packing of (1→4)-β-glucan chains in cellulose microfibrils. Computer-simulated peak shapes, calculated for 36-chain microfibrils with perfect order or uncorrelated disorder, were sharper than those in the experimental diffractogram. Introducing correlated disorder into the models broaden the simulated peaks but only when the disorder was increased to unrealistic magnitudes. Computer-simulated diffractograms, calculated for 24- and 18-chain models, showed good fits to experimental data. Particularly good fits to both x-ray and nuclear magnetic resonance data were obtained for collections of 18-chain models with mixed cross-sectional shapes and occasional twinning. Synthesis of 18-chain microfibrils is consistent with a model for cellulose-synthesizing complexes in which three cellulose synthase polypeptides form a particle and six particles form a rosette.

  18. Structure of the bifunctional aminoglycoside-resistance enzyme AAC(6′)-Ie-APH(2′′)-Ia revealed by crystallographic and small-angle X-ray scattering analysis

    PubMed Central

    Smith, Clyde A.; Toth, Marta; Weiss, Thomas M.; Frase, Hilary; Vakulenko, Sergei B.

    2014-01-01

    Broad-spectrum resistance to aminoglycoside antibiotics in clinically important Gram-positive staphylococcal and entero­coccal pathogens is primarily conferred by the bifunctional enzyme AAC(6′)-Ie-APH(2′′)-Ia. This enzyme possesses an N-terminal coenzyme A-dependent acetyltransferase domain [AAC(6′)-Ie] and a C-terminal GTP-dependent phosphotransferase domain [APH(2′′)-Ia], and together they produce resistance to almost all known aminoglycosides in clinical use. Despite considerable effort over the last two or more decades, structural details of AAC(6′)-Ie-APH(2′′)-Ia have remained elusive. In a recent breakthrough, the structure of the isolated C-terminal APH(2′′)-Ia enzyme was determined as the binary Mg2GDP complex. Here, the high-resolution structure of the N-terminal AAC(6′)-Ie enzyme is reported as a ternary kanamycin/coenzyme A abortive complex. The structure of the full-length bifunctional enzyme has subsequently been elucidated based upon small-angle X-ray scattering data using the two crystallographic models. The AAC(6′)-Ie enzyme is joined to APH(2′′)-Ia by a short, predominantly rigid linker at the N-terminal end of a long α-helix. This α-helix is in turn intrinsically associated with the N-terminus of APH(2′′)-Ia. This structural arrangement supports earlier observations that the presence of the intact α-helix is essential to the activity of both functionalities of the full-length AAC(6′)-Ie-APH(2′′)-Ia enzyme. PMID:25286858

  19. X-ray resonant magnetic scattering ellipsometer

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

    Xu, Z.; Randall, K.J.; Gluskin, E.

    1996-09-01

    It is very difficult to characterize the polarization of a synchrotron radiation source in the soft and/or intermediate x-ray energy region particularly from 1 to 2 keV. Conventional multilayer mirror or single-crystal polarimeters do not work over this energy region because their throughput (the reflectivities combined with the phase shift) becomes insignificant. In this paper, we present a new ellipsometer scheme that is able to fully characterize the polarization of synchrotron radiation sources in this energy region. It is based on the dichroic x-ray resonant ferromagnetic scattering that yields information on both the polarization of the x-ray and the materialmore » (element specific) dielectric-constant tensor [C.-C. Kao {ital et} {ital al}., Phys. Rev. B {bold 50}, 9599 (1994)] due to the interband ferromagnetic Kerr effect [B.R. Cooper, Phys. Rev. A {bold 139}, 1504 (1965)]. {copyright} {ital 1996 American Institute of Physics.}« less

  20. Small-angle neutron scattering study of a monoclonal antibody using free-energy constraints.

    PubMed

    Clark, Nicholas J; Zhang, Hailiang; Krueger, Susan; Lee, Hyo Jin; Ketchem, Randal R; Kerwin, Bruce; Kanapuram, Sekhar R; Treuheit, Michael J; McAuley, Arnold; Curtis, Joseph E

    2013-11-14

    Monoclonal antibodies (mAbs) contain hinge-like regions that enable structural flexibility of globular domains that have a direct effect on biological function. A subclass of mAbs, IgG2, have several interchain disulfide bonds in the hinge region that could potentially limit structural flexibility of the globular domains and affect the overall configuration space available to the mAb. We have characterized human IgG2 mAb in solution via small-angle neutron scattering (SANS) and interpreted the scattering data using atomistic models. Molecular Monte Carlo combined with molecular dynamics simulations of a model mAb indicate that a wide range of structural configurations are plausible, spanning radius of gyration values from ∼39 to ∼55 Å. Structural ensembles and representative single structure solutions were derived by comparison of theoretical SANS profiles of mAb models to experimental SANS data. Additionally, molecular mechanical and solvation free-energy calculations were carried out on the ensemble of best-fitting mAb structures. The results of this study indicate that low-resolution techniques like small-angle scattering combined with atomistic molecular simulations with free-energy analysis may be helpful to determine the types of intramolecular interactions that influence function and could lead to deleterious changes to mAb structure. This methodology will be useful to analyze small-angle scattering data of many macromolecular systems.

  1. High-energy synchrotron x-ray techniques for studying irradiated materials

    DOE PAGES

    Park, Jun-Sang; Zhang, Xuan; Sharma, Hemant; ...

    2015-03-20

    High performance materials that can withstand radiation, heat, multiaxial stresses, and corrosive environment are necessary for the deployment of advanced nuclear energy systems. Nondestructive in situ experimental techniques utilizing high energy x-rays from synchrotron sources can be an attractive set of tools for engineers and scientists to investigate the structure–processing–property relationship systematically at smaller length scales and help build better material models. In this paper, two unique and interconnected experimental techniques, namely, simultaneous small-angle/wide-angle x-ray scattering (SAXS/WAXS) and far-field high-energy diffraction microscopy (FF-HEDM) are presented. Finally, the changes in material state as Fe-based alloys are heated to high temperatures ormore » subject to irradiation are examined using these techniques.« less

  2. X-ray Diffuse Scattering from Ultrafast Laser Excited Solids

    NASA Astrophysics Data System (ADS)

    Trigo, Mariano; Sheu, Yu-Miin; Chen, Jian; Reis, David; Fahy, Stephen; Murray, Eamonn; Graber, Timothy; Henning, Robert

    2009-03-01

    Intense, ultrashort laser pulses can be used to excite and detect coherent phonons in solids. However, optical experiments can only probe a reduced fraction of the Brillouin zone and hence most of the decay channels of such coherent phonons become invisible. In contrast, time-resolved x-ray diffuse scattering (TRXDS) has the potential to be the ultimate tool to study these phonon decay processes throughout the Brillouin-zone of the crystal. In our work, performed at the BioCARS beamline at the Advanced Photon Source, we use synchrotron time-resolved diffuse x-ray scattering to study Si and Bi under intense laser excitation with 100 ps resolution. We show that reasonable signal levels can be achieved with incident flux of 10^12 photons comparable to the flux that will be available at future 4th generation sources such as the LCLS in a single pulse. These sources will also provide three orders of magnitude shorter pulses; thus, this experiment serves as a test of the feasibility of time-resolved X-ray diffuse scattering as a tool for studying nonequilibrium phonon dynamics in solids.

  3. The dust scattering halo of Cygnus X-3

    NASA Astrophysics Data System (ADS)

    Corrales, L. R.; Paerels, F.

    2015-10-01

    Dust grains scatter X-ray light through small angles, producing a diffuse halo image around bright X-ray point sources situated behind a large amount of interstellar material. We present analytic solutions to the integral for the dust scattering intensity, which allow for a Bayesian analysis of the scattering halo around Cygnus X-3. Fitting the optically thin 4-6 keV halo surface brightness profile yields the dust grain size and spatial distribution. We assume a power-law distribution of grain sizes (n ∝ a-p) and fit for p, the grain radius cut-off amax, and dust mass column. We find that a p ≈ 3.5 dust grain size distribution with amax ≈ 0.2 μm fits the halo profile relatively well, whether the dust is distributed uniformly along the line of sight or in clumps. We find that a model consisting of two dust screens, representative of foreground spiral arms, requires the foreground Perseus arm to contain 80 per cent of the total dust mass. The remaining 20 per cent of the dust, which may be associated with the outer spiral arm of the Milky Way, is located within 1 kpc of Cyg X-3. Regardless of which model was used, we found τ_sca ˜ 2 E_keV^{-2}. We examine the energy resolved haloes of Cyg X-3 from 1 to 6 keV and find that there is a sharp drop in scattering halo intensity when E < 2-3 keV, which cannot be explained with multiple scattering effects. We hypothesize that this may be caused by large dust grains or material with unique dielectric properties, causing the scattering cross-section to depart from the Rayleigh-Gans approximation that is used most often in X-ray scattering studies. The foreground Cyg OB2 association, which contains several evolved stars with large extinction values, is a likely culprit for grains of unique size or composition.

  4. Standoff detection of hidden objects using backscattered ultra-intense laser-produced x-rays

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

    Kuwabara, H.; Mori, Y.; Kitagawa, Y.

    2013-08-28

    Ultra-intense laser-produced sub-ps X-ray pulses can detect backscattered signals from objects hidden in aluminium containers. Coincident measurements using primary X-rays enable differentiation among acrylic, copper, and lead blocks inside the container. Backscattering reveals the shapes of the objects, while their material composition can be identified from the modification methods of the energy spectra of backscattered X-ray beams. This achievement is an important step toward more effective homeland security.

  5. Reflection thermal diffuse x-ray scattering for quantitative determination of phonon dispersion relations

    DOE PAGES

    Mei, A. B.; Hellman, O.; Schlepuetz, C. M.; ...

    2015-11-03

    Synchrotron reflection x-ray thermal diffuse scattering (TDS) measurements, rather than previously reported transmission TDS, are carried out at room temperature and analyzed using a formalism based upon second-order interatomic force constants and long-range Coulomb interactions to obtain quantitative determinations of MgO phonon dispersion relations (h) over bar omega(j) (q), phonon densities of states g((h) over bar omega), and isochoric temperature-dependent vibrational heat capacities c v (T). We use MgO as a model system for investigating reflection TDS due to its harmonic behavior as well as its mechanical and dynamic stability. Resulting phonon dispersion relations and densities of states are foundmore » to be in good agreement with independent reports from inelastic neutron and x-ray scattering experiments. Temperature-dependent isochoric heat capacities c v (T), computed within the harmonic approximation from (h) over bar omega(j) (q) values, increase with temperature from 0.4 x 10 -4 eV/atom K at 100 K to 1.4 x 10 -4 eV/atom K at 200 K and 1.9 x 10 -4 eV/atom K at 300 K, in excellent agreement with isobaric heat capacity values c p (T) between 4 and 300 K. We anticipate that the experimental approach developed here will be valuable for determining vibrational properties of heteroepitaxial thin films since the use of grazing-incidence (θ ≲ θ c where θ c is the density-dependent critical angle) allows selective tuning of x-ray penetration depths to ≲ 10 nm.« less

  6. 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.

  7. Inverse Compton scattering X-ray source yield optimization with a laser path folding system inserted in a pre-existent RF linac

    NASA Astrophysics Data System (ADS)

    Chaleil, A.; Le Flanchec, V.; Binet, A.; Nègre, J. P.; Devaux, J. F.; Jacob, V.; Millerioux, M.; Bayle, A.; Balleyguier, P.; Prazeres, R.

    2016-12-01

    An inverse Compton scattering source is under development at the ELSA linac of CEA, Bruyères-le-Châtel. Ultra-short X-ray pulses are produced by inverse Compton scattering of 30 ps-laser pulses by relativistic electron bunches. The source will be able to operate in single shot mode as well as in recurrent mode with 72.2 MHz pulse trains. Within this framework, an optical multipass system that multiplies the number of emitted X-ray photons in both regimes has been designed in 2014, then implemented and tested on ELSA facility in the course of 2015. The device is described from both geometrical and timing viewpoints. It is based on the idea of folding the laser optical path to pile-up laser pulses at the interaction point, thus increasing the interaction probability. The X-ray output gain measurements obtained using this system are presented and compared with calculated expectations.

  8. Disordered porous solids : from chord distributions to small angle scattering

    NASA Astrophysics Data System (ADS)

    Levitz, P.; Tchoubar, D.

    1992-06-01

    Disordered biphasic porous solids are examples of complex interfacial media. Small angle scattering strongly depends on the geometrical properties of the internal surface partitioning a porous system. Properties of the second derivative of the bulk autocorrelation function quantitatively defines the level of connection between the small angle scattering and the statistical properties of this interface. A tractable expression of this second derivative, involving the pore and the mass chord distribution functions, was proposed by Mering and Tchoubar (MT). Based on the present possibility to make a quantitative connection between imaging techniques and the small angle scattering, this paper tries to complete and to extend the MT approach. We first discuss how chord distribution functions can be used as fingerprints of the structural disorder. An explicit relation between the small angle scattering and these chord distributions is then proposed. In a third part, the application to different types of disorder is critically discussed and predictions are compared to available experimental data. Using image processing, we will consider three types of disorder : the long-range Debye randomness, the “ correlated " disorder with a special emphasis on the structure of a porous glass (the vycor), and, finally, complex structures where length scale invariance properties can be observed. Les solides poreux biphasiques sont des exemples de milieux interfaciaux complexes. La diffusion aux petits angles (SAS) dépend fortement des propriétés géométriques de l'interface partitionant le milieu poreux. Les propriétés de la dérivée seconde de la fonction d'autocorrélation de densité définit quantitativement le niveau de connection entre la diffusion aux petits angles et les caractéristiques statistiques de cette interface. Une expression utilisable de cette seconde dérivée, impliquant les distributions de cordes associées à la phase massique et au réseau de pores, fut

  9. Inelastic X-ray Scattering from Shocked Liquid Deuterium

    DOE PAGES

    Regan, S. P.; Falk, K.; Gregori, G.; ...

    2012-12-28

    The Fermi-degenerate plasma conditions created in liquid deuterium by a laser-ablation—driven shock wave were probed with noncollective, spectrally resolved, inelastic x-ray Thomson scattering employing Cl Ly α line emission at 2.96 keV. Thus, these first x-ray Thomson scattering measurements of the microscopic properties of shocked deuterium show an inferred spatially averaged electron temperature of 8±5 eV, an electron density of 2.2(±0.5)×10 23 cm -3, and an ionization of 0.8 (-0.25, +0.15). Our two-dimensional hydrodynamic simulations using equation-of-state models suited for the extreme parameters occurring in inertial confinement fusion research and planetary interiors are consistent with the experimental results.

  10. SMART-X: Square Meter, Arcsecond Resolution Telescope for X-rays

    NASA Astrophysics Data System (ADS)

    Vikhlinin, Alexey; SMART-X Collaboration

    2013-04-01

    SMART-X is a concept for a next-generation X-ray observatory with large-area, 0.5" angular resolution grazing incidence adjustable X-ray mirrors, high-throughput critical angle transmission gratings, and X-ray microcalorimeter and CMOS-based imager in the focal plane. High angular resolution is enabled by new technology based on controlling the shape of mirror segments using thin film piezo actuators deposited on the back surface. Science applications include observations of growth of supermassive black holes since redshifts of ~10, ultra-deep surveys over 10's of square degrees, galaxy assembly at z=2-3, as well as new opportunities in the high-resolution X-ray spectroscopy and time domains. We also review the progress in technology development, tests, and mission design over the past year.

  11. Innovative diffraction gratings for high-resolution resonant inelastic soft x-ray scattering spectroscopy

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

    Voronov, D.L.; Warwick, T.; Gullikson, E. M.

    2016-07-27

    High-resolution Resonant Inelastic X-ray Scattering (RIXS) requires diffraction gratings with very exacting characteristics. The gratings should provide both very high dispersion and high efficiency which are conflicting requirements and extremely challenging to satisfy in the soft x-ray region for a traditional grazing incidence geometry. To achieve high dispersion one should increase the groove density of a grating; this however results in a diffraction angle beyond the critical angle range and results in drastic efficiency loss. The problem can be solved by use of multilayer coated blazed gratings (MBG). In this work we have investigated the diffraction characteristics of MBGs viamore » numerical simulations and have developed a procedure for optimization of grating design for a multiplexed high resolution imaging spectrometer for RIXS spectroscopy to be built in sector 6 at the Advanced Light Source (ALS). We found that highest diffraction efficiency can be achieved for gratings optimized for 4{sup th} or 5{sup th} order operation. Fabrication of such gratings is an extremely challenging technological problem. We present a first experimental prototype of these gratings and report its performance. High order and high line density gratings have the potential to be a revolutionary new optical element that should have great impact in the area of soft x-ray RIXS.« less

  12. Ab initio calculation of the ion feature in x-ray Thomson scattering.

    PubMed

    Plagemann, Kai-Uwe; Rüter, Hannes R; Bornath, Thomas; Shihab, Mohammed; Desjarlais, Michael P; Fortmann, Carsten; Glenzer, Siegfried H; Redmer, Ronald

    2015-07-01

    The spectrum of x-ray Thomson scattering is proportional to the dynamic structure factor. An important contribution is the ion feature which describes elastic scattering of x rays off electrons. We apply an ab initio method for the calculation of the form factor of bound electrons, the slope of the screening cloud of free electrons, and the ion-ion structure factor in warm dense beryllium. With the presented method we can calculate the ion feature from first principles. These results will facilitate a better understanding of x-ray scattering in warm dense matter and an accurate measurement of ion temperatures which would allow determining nonequilibrium conditions, e.g., along shock propagation.

  13. Materials identification using a small-scale pixellated x-ray diffraction system

    NASA Astrophysics Data System (ADS)

    O'Flynn, D.; Crews, C.; Drakos, I.; Christodoulou, C.; Wilson, M. D.; Veale, M. C.; Seller, P.; Speller, R. D.

    2016-05-01

    A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved.

  14. High duty cycle inverse Compton scattering X-ray source

    DOE PAGES

    Ovodenko, A.; Agustsson, R.; Babzien, M.; ...

    2016-12-22

    Inverse Compton Scattering (ICS) is an emerging compact X-ray source technology, where the small source size and high spectral brightness are of interest for multitude of applications. However, to satisfy the practical flux requirements, a high-repetition-rate ICS system needs to be developed. To this end, this article reports the experimental demonstration of a high peak brightness ICS source operating in a burst mode at 40 MHz. A pulse train interaction has been achieved by recirculating a picosecond CO 2 laser pulse inside an active optical cavity synchronized to the electron beam. The pulse train ICS performance has been characterized atmore » 5- and 15- pulses per train and compared to a single pulse operation under the same operating conditions. Lastly, with the observed near-linear X-ray photon yield gain due to recirculation, as well as noticeably higher operational reliability, the burst-mode ICS offers a great potential for practical scalability towards high duty cycles.« less

  15. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    DOE PAGES

    Lawrence, Robert M.; Conrad, Chelsie E.; Zatsepin, Nadia A.; ...

    2015-08-20

    Serial femtosecond crystallography (SFX) using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ~700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ~40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is a pertinent step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  16. Demonstration of x-ray Thomson scattering using picosecond K-α x-ray sources in the characterization of dense heated matter

    DOE PAGES

    Kritcher, A. L.; Neumayer, P.; Lee, H. J.; ...

    2008-10-31

    Here, we present K-α x-ray Thomson scattering from shock compressed matter for use as a diagnostic in determining the temperature, density, and ionization state with picosecond resolution. The development of this source as a diagnostic as well as stringent requirements for successful K-α x-ray Thomson scattering are addressed. Here, the first elastic and inelastic scattering measurements on a medium size laser facility have been observed. We present scattering data from solid density carbon plasmas with >1X 10 5 photons in the elastic peak that validate the capability of single shot characterization of warm dense matter and the ability to usemore » this scattering source at future free electron lasers and for fusion experiments at the National Ignition Facility (NIF), LLNL.« less

  17. Polarization-dependent force driving the Eg mode in bismuth under optical excitation: comparison of first-principles theory with ultra-fast x-ray experiments

    NASA Astrophysics Data System (ADS)

    Fahy, Stephen; Murray, Eamonn

    2015-03-01

    Using first principles electronic structure methods, we calculate the induced force on the Eg (zone centre transverse optical) phonon mode in bismuth immediately after absorption of a ultrafast pulse of polarized light. To compare the results with recent ultra-fast, time-resolved x-ray diffraction experiments, we include the decay of the force due to carrier scattering, as measured in optical Raman scattering experiments, and simulate the optical absorption process, depth-dependent atomic driving forces, and x-ray diffraction in the experimental geometry. We find excellent agreement between the theoretical predictions and the observed oscillations of the x-ray diffraction signal, indicating that first-principles theory of optical absorption is well suited to the calculation of initial atomic driving forces in photo-excited materials following ultrafast excitation. This work is supported by Science Foundation Ireland (Grant No. 12/IA/1601) and EU Commission under the Marie Curie Incoming International Fellowships (Grant No. PIIF-GA-2012-329695).

  18. Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

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

    Van Benschoten, Andrew H.; Afonine, Pavel V.; Terwilliger, Thomas C.

    2015-07-28

    A method of simulating X-ray diffuse scattering from multi-model PDB files is presented. Despite similar agreement with Bragg data, different translation–libration–screw refinement strategies produce unique diffuse intensity patterns. Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling andmore » validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier’s equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls-as-xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophosphodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. These methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis.« less

  19. Wide-Angle X-Ray Scattering and Solid-State Nuclear Magnetic Resonance Data Combined to Test Models for Cellulose Microfibrils in Mung Bean Cell Walls1

    PubMed Central

    Newman, Roger H.; Hill, Stefan J.; Harris, Philip J.

    2013-01-01

    A synchrotron wide-angle x-ray scattering study of mung bean (Vigna radiata) primary cell walls was combined with published solid-state nuclear magnetic resonance data to test models for packing of (1→4)-β-glucan chains in cellulose microfibrils. Computer-simulated peak shapes, calculated for 36-chain microfibrils with perfect order or uncorrelated disorder, were sharper than those in the experimental diffractogram. Introducing correlated disorder into the models broaden the simulated peaks but only when the disorder was increased to unrealistic magnitudes. Computer-simulated diffractograms, calculated for 24- and 18-chain models, showed good fits to experimental data. Particularly good fits to both x-ray and nuclear magnetic resonance data were obtained for collections of 18-chain models with mixed cross-sectional shapes and occasional twinning. Synthesis of 18-chain microfibrils is consistent with a model for cellulose-synthesizing complexes in which three cellulose synthase polypeptides form a particle and six particles form a rosette. PMID:24154621

  20. Development of an x-ray prism for analyzer based imaging systems

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

    Bewer, Brian; Chapman, Dean

    Analyzer crystal based imaging techniques such as diffraction enhanced imaging (DEI) and multiple imaging radiography (MIR) utilize the Bragg peak of perfect crystal diffraction to convert angular changes into intensity changes. These x-ray techniques extend the capability of conventional radiography, which derives image contrast from absorption, by providing large intensity changes for small angle changes introduced from the x-ray beam traversing the sample. Objects that have very little absorption contrast may have considerable refraction and ultrasmall angle x-ray scattering contrast improving visualization and extending the utility of x-ray imaging. To improve on the current DEI technique an x-ray prism (XRP)more » was designed and included in the imaging system. The XRP allows the analyzer crystal to be aligned anywhere on the rocking curve without physically moving the analyzer from the Bragg angle. By using the XRP to set the rocking curve alignment rather than moving the analyzer crystal physically the needed angle sensitivity is changed from submicroradians for direct mechanical movement of the analyzer crystal to tens of milliradians for movement of the XRP angle. However, this improvement in angle positioning comes at the cost of absorption loss in the XRP and depends on the x-ray energy. In addition to using an XRP for crystal alignment it has the potential for scanning quickly through the entire rocking curve. This has the benefit of collecting all the required data for image reconstruction in a single measurement thereby removing some problems with motion artifacts which remain a concern in current DEI/MIR systems especially for living animals.« less

  1. A small-angle neutron scattering study of the kinetics of phase separation in a supersaturated Ni-12.5 at. pct Si alloy

    NASA Astrophysics Data System (ADS)

    Polat, S.; Chen, Haydn; Epperson, J. E.

    1989-04-01

    The kinetic behavior of precipitation in a supersaturated Ni-12.5 at. pct Si alloy single crystal has been studied by the small-angle neutron scattering (SANS) technique to supplement earlier transmission electron microscopy (TEM) and wide-angle X-ray diffraction (XRD) work. The SANS measurements performed at room temperature on quenched specimens subjected to isothermal anneals at 400, 450, 505, and 550 °C for various amounts of time have revealed the presence of an interference peak in the scattering function. The particle size, determined according to the Guinier approximation, is found to grow in accordance with the diffusion controlled model put forth by Lifshitz and Slyozov, and independently by Wagner. The activation energy for solute diffusion is determined using the rate constants governing the growth of particle size and the variation of the mean interparticle distance. Results are in agreement with the values given in the literature. Transition from an earlier growth stage has been observed, and enhanced diffusion is noted at temperatures below 505 °C; both observations are consistent with the previous X-ray results. The dynamical scaling law appears to be followed by the data obtained in the coarsening stage. A disruption of scaling occurs at the point when the particle growth changes from a parabolic rate behavior to a cubic coarsening rate. Dynamical scaling offers the potential for projecting the service lifetimes for components from experimental measurements carried out over a much shorter time interval. Discrepancies in the size parameters determined by different techniques are discussed.

  2. 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.

  3. The study of X-ray scattering to determine surface topography of smooth surfaces. [X-ray telescope mirrors

    NASA Technical Reports Server (NTRS)

    Williams, A. C.

    1982-01-01

    The scattering of X-rays from state-of-the-art polished mirrors is discussed with reference to the requirements of the Advanced X-ray Astrophysics Facility telescope. An experimental set-up is described which allows information to be obtained with subarcsecond resolution. A sample of the data obtained is presented along with a possible theoretical model for its interpretation.

  4. Design and performance of BOREAS, the beamline for resonant X-ray absorption and scattering experiments at the ALBA synchrotron light source

    DOE PAGES

    Barla, Alessandro; Nicolas, Josep; Cocco, Daniele; ...

    2016-10-07

    The optical design of the BOREAS beamline operating at the ALBA synchrotron radiation facility is described. BOREAS is dedicated to resonant X-ray absorption and scattering experiments using soft X-rays, in an unusually extended photon energy range from 80 to above 4000 eV, and with full polarization control. Its optical scheme includes a fixed-included-angle, variable-line-spacing grating monochromator and a pair of refocusing mirrors, equipped with benders, in a Kirkpatrick–Baez arrangement. It is equipped with two end-stations, one for X-ray magnetic circular dichroism and the other for resonant magnetic scattering. In conclusion, the commissioning results show that the expected beamline performance ismore » achieved both in terms of energy resolution and of photon flux at the sample position.« less

  5. X-ray diffraction-based electronic structure calculations and experimental x-ray analysis for medical and materials applications

    NASA Astrophysics Data System (ADS)

    Mahato, Dip Narayan

    This thesis includes x-ray experiments for medical and materials applications and the use of x-ray diffraction data in a first-principles study of electronic structures and hyperfine properties of chemical and biological systems. Polycapillary focusing lenses were used to collect divergent x rays emitted from conventional x-ray tubes and redirect them to form an intense focused beam. These lenses are routinely used in microbeam x-ray fluorescence analysis. In this thesis, their potential application to powder diffraction and focused beam orthovoltage cancer therapy has been investigated. In conventional x-ray therapy, very high energy (˜ MeV) beams are used, partly to reduce the skin dose. For any divergent beam, the dose is necessarily highest at the entry point, and decays exponentially into the tissue. To reduce the skin dose, high energy beams, which have long absorption lengths, are employed, and rotated about the patient to enter from different angles. This necessitates large expensive specialized equipment. A focused beam could concentrate the dose within the patient. Since this is inherently skin dose sparing, lower energy photons could be employed. A primary concern in applying focused beams to therapy is whether the focus would be maintained despite Compton scattering within the tissue. To investigate this, transmission and focal spot sizes as a function of photon energy of two polycapillary focusing lenses were measured. The effects of tissue-equivalent phantoms of different thicknesses on the focal spot size were studied. Scatter fraction and depth dose were calculated. For powder diffraction, the polycapillary optics provide clean Gaussian peaks, which result in angular resolution that is much smaller than the peak width due to the beam convergence. Powder diffraction (also called coherent scatter) without optics can also be used to distinguish between tissue types that, because they have different nanoscale structures, scatter at different angles

  6. A new high quality X-ray source for Cultural Heritage

    NASA Astrophysics Data System (ADS)

    Walter, Philippe; Variola, Alessandro; Zomer, Fabian; Jaquet, Marie; Loulergue, Alexandre

    2009-09-01

    Compton based photon sources have generated much interest since the rapid advance in laser and accelerator technologies has allowed envisaging their utilisation for ultra-compact radiation sources. These should provide X-ray short pulses with a relatively high average flux. Moreover, the univocal dependence between the scattered photon energy and its angle gives the possibility of obtaining a quasi-monochromatic beam with a simple diaphragm system. For the most ambitious projects the expected performance takes into account a rate of 10-10 photons/s, with an angular divergence of few mrad, an X-ray energy cut-off of few tens of keV and a bandwidth ΔE/E˜1-10%. Even if the integrated rate cannot compete with synchrotron radiation sources, the cost and the compactness of these Compton based machines make them attractive for a wide spectrum of applications. We explore here the interest of these systems for Cultural Heritage preservation. To cite this article: P. Walter et al., C. R. Physique 10 (2009).

  7. X-ray solution scattering combined with computation characterizing protein folds and multiple conformational states : computation and application.

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

    Yang, S.; Park, S.; Makowski, L.

    Small angle X-ray scattering (SAXS) is an increasingly powerful technique to characterize the structure of biomolecules in solution. We present a computational method for accurately and efficiently computing the solution scattering curve from a protein with dynamical fluctuations. The method is built upon a coarse-grained (CG) representation of the protein. This CG approach takes advantage of the low-resolution character of solution scattering. It allows rapid determination of the scattering pattern from conformations extracted from CG simulations to obtain scattering characterization of the protein conformational landscapes. Important elements incorporated in the method include an effective residue-based structure factor for each aminomore » acid, an explicit treatment of the hydration layer at the surface of the protein, and an ensemble average of scattering from all accessible conformations to account for macromolecular flexibility. The CG model is calibrated and illustrated to accurately reproduce the experimental scattering curve of Hen egg white lysozyme. We then illustrate the computational method by calculating the solution scattering pattern of several representative protein folds and multiple conformational states. The results suggest that solution scattering data, when combined with a reliable computational method, have great potential for a better structural description of multi-domain complexes in different functional states, and for recognizing structural folds when sequence similarity to a protein of known structure is low. Possible applications of the method are discussed.« less

  8. Distinguishability of N Composition Profiles In SiON Films On Si By Angle-Resolved X-ray Photoelectron Spectroscopy

    NASA Astrophysics Data System (ADS)

    Powell, C. J.; Werner, W. S. M.; Smekal, W.

    2007-09-01

    We report on the use of the NIST Database for the Simulation of Electron Spectra for Surface Analysis (SESSA) to determine N 1s, O 1s, and Si 2p3/2 photoelectron intensities for a 25 Å SiON film on a Si substrate with different distributions of N in the film. These simulations were made to assess the distinguishability of angle-resolved x-ray photoelectron spectroscopy (ARXPS) signals for each N distribution. Our approach differs from conventional simulations of ARXPS data in that we do not neglect elastic scattering of the photoelectrons and the finite solid angle of the analyzer. Appreciable dispersion of the photoelectron intensities was found only for the N 1s intensities at an emission angle of 75° (with respect to the surface normal). Conventional analyses of ARXPS data that include such large emission angles are unlikely to be valid due to angle-dependent changes of the attenuation length. We demonstrate the magnitude of elastic-scattering and analyzer solid-angle effects on the calculated angular distributions.

  9. Incoherent-scatter computed tomography with monochromatic synchrotron x ray: feasibility of multi-CT imaging system for simultaneous measurement-of fluorescent and incoherent scatter x rays

    NASA Astrophysics Data System (ADS)

    Yuasa, T.; Akiba, M.; Takeda, T.; Kazama, M.; Hoshino, A.; Watanabe, Y.; Hyodo, K.; Dilmanian, F. A.; Akatsuka, T.; Itai, Y.

    1997-10-01

    We describe a new system of incoherent scatter computed tomography (ISCT) using monochromatic synchrotron X rays, and we discuss its potential to be used in in vivo imaging for medical use. The system operates on the basis of computed tomography (CT) of the first generation. The reconstruction method for ISCT uses the least squares method with singular value decomposition. The research was carried out at the BLNE-5A bending magnet beam line of the Tristan Accumulation Ring in KEK, Japan. An acrylic cylindrical phantom of 20-mm diameter containing a cross-shaped channel was imaged. The channel was filled with a diluted iodine solution with a concentration of 200 /spl mu/gI/ml. Spectra obtained with the system's high purity germanium (HPGe) detector separated the incoherent X-ray line from the other notable peaks, i.e., the iK/sub /spl alpha// and K/sub /spl beta/1/ X-ray fluorescent lines and the coherent scattering peak. CT images were reconstructed from projections generated by integrating the counts In the energy window centering around the incoherent scattering peak and whose width was approximately 2 keV. The reconstruction routine employed an X-ray attenuation correction algorithm. The resulting image showed more homogeneity than one without the attenuation correction.

  10. Improving a high-efficiency, gated spectrometer for x-ray Thomson scattering experiments at the National Ignition Facility.

    PubMed

    Döppner, T; Kraus, D; Neumayer, P; Bachmann, B; Emig, J; Falcone, R W; Fletcher, L B; Hardy, M; Kalantar, D H; Kritcher, A L; Landen, O L; Ma, T; Saunders, A M; Wood, R D

    2016-11-01

    We are developing x-ray Thomson scattering for applications in implosion experiments at the National Ignition Facility. In particular we have designed and fielded MACS, a high-efficiency, gated x-ray spectrometer at 7.5-10 keV [T. Döppner et al., Rev. Sci. Instrum. 85, 11D617 (2014)]. Here we report on two new Bragg crystals based on Highly Oriented Pyrolytic Graphite (HOPG), a flat crystal and a dual-section cylindrically curved crystal. We have performed in situ calibration measurements using a brass foil target, and we used the flat HOPG crystal to measure Mo K-shell emission at 18 keV in 2nd order diffraction. Such high photon energy line emission will be required to penetrate and probe ultra-high-density plasmas or plasmas of mid-Z elements.

  11. Probing multi-scale mechanical damage in connective tissues using X-ray diffraction.

    PubMed

    Bianchi, Fabio; Hofmann, Felix; Smith, Andrew J; Thompson, Mark S

    2016-11-01

    The accumulation of microstructural collagen damage following repetitive loading is linked to painful and debilitating tendon injuries. As a hierarchical, semi-crystalline material, collagen mechanics can be studied using X-ray diffraction. The aim of the study was to describe multi-structural changes in tendon collagen following controlled plastic damage (5% permanent strain). We used small angle X-ray scattering (SAXS) to interrogate the spacing of collagen molecules within a fibril, and wide angle X-ray scattering (WAXS) to measure molecular strains under macroscopic loading. Simultaneous recordings of SAXS and WAXS patterns, together with whole-tissue strain in physiologically hydrated rat-tail tendons were made during increments of in situ tensile loading. Results showed that while tissue level modulus was unchanged, fibril modulus decreased significantly, and molecular modulus significantly increased. Further, analysis of higher order SAXS peaks suggested structural changes in the gap and overlap regions, possibly localising the damage to molecular cross-links. Our results provide new insight into the fundamental damage processes at work in collagenous tissues and point to new directions for their mitigation and repair. This article reports the first in situ loading synchrotron studies on mechanical damage in collagenous tissues. We provide new insight into the nano- and micro-structural mechanisms of damage processes. Pre-damaged tendons showed differential alteration of moduli at macro, micro and nano-scales as measured using X-ray scattering techniques. Detailed analysis of higher order diffraction peaks suggested damage is localised to molecular cross-links. The results are consistent with previous X-ray scattering studies of tendons and also with recent thermal stability studies on damaged material. Detailed understanding of damage mechanisms is essential in the development of new therapies promoting tissue repair. Copyright © 2016 Acta Materialia Inc

  12. Wavelength-independent constant period spin-echo modulated small angle neutron scattering

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

    Sales, Morten, E-mail: lsp260@alumni.ku.dk; Plomp, Jeroen; Bouwman, Wim

    2016-06-15

    Spin-Echo Modulated Small Angle Neutron Scattering (SEMSANS) in Time-of-Flight (ToF) mode has been shown to be a promising technique for measuring (very) small angle neutron scattering (SANS) signals and performing quantitative Dark-Field Imaging (DFI), i.e., SANS with 2D spatial resolution. However, the wavelength dependence of the modulation period in the ToF spin-echo mode has so far limited the useful modulation periods to those resolvable with the limited spatial resolution of the detectors available. Here we present our results of an approach to keep the period of the induced modulation constant for the wavelengths utilised in ToF. This is achieved bymore » ramping the magnetic fields in the coils responsible for creating the spatially modulated beam in synchronisation with the neutron pulse, thus keeping the modulation period constant for all wavelengths. Such a setup enables the decoupling of the spatial detector resolution from the resolution of the modulation period by the use of slits or gratings in analogy to the approach in grating-based neutron DFI.« less

  13. 16th National School on Neutron and X-ray Scattering

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

    Chakoumakos, Bryan; Achilles, Cherie; Cybulskis, Viktor

    Students talk about their experience at the 16th National School on Neutron and X-ray Scattering, or NXS 2014. Jointly conducted by Oak Ridge and Argonne national laboratories, NXS immerses graduate students in national user facilities to learn in a hands-on environment how to use neutrons and X-rays in their research.

  14. 16th National School on Neutron and X-ray Scattering

    ScienceCinema

    Chakoumakos, Bryan; Achilles, Cherie; Cybulskis, Viktor; Gilbert, Ian

    2018-02-14

    Students talk about their experience at the 16th National School on Neutron and X-ray Scattering, or NXS 2014. Jointly conducted by Oak Ridge and Argonne national laboratories, NXS immerses graduate students in national user facilities to learn in a hands-on environment how to use neutrons and X-rays in their research.

  15. Proton energy and scattering angle radiographs to improve proton treatment planning: a Monte Carlo study

    NASA Astrophysics Data System (ADS)

    Biegun, A. K.; Takatsu, J.; Nakaji, T.; van Goethem, M. J.; van der Graaf, E. R.; Koffeman, E. N.; Visser, J.; Brandenburg, S.

    2016-12-01

    The novel proton radiography imaging technique has a large potential to be used in direct measurement of the proton energy loss (proton stopping power, PSP) in various tissues in the patient. The uncertainty of PSPs, currently obtained from translation of X-ray Computed Tomography (xCT) images, should be minimized from 3-5% or higher to less than 1%, to make the treatment plan with proton beams more accurate, and thereby better treatment for the patient. With Geant4 we simulated a proton radiography detection system with two position-sensitive and residual energy detectors. A complex phantom filled with various materials (including tissue surrogates), was placed between the position sensitive detectors. The phantom was irradiated with 150 MeV protons and the energy loss radiograph and scattering angles were studied. Protons passing through different materials in the phantom lose energy, which was used to create a radiography image of the phantom. The multiple Coulomb scattering of a proton traversing different materials causes blurring of the image. To improve image quality and material identification in the phantom, we selected protons with small scattering angles. A good quality proton radiography image, in which various materials can be recognized accurately, and in combination with xCT can lead to more accurate relative stopping powers predictions.

  16. Environmental chamber for in situ dynamic control of temperature and relative humidity during x-ray scattering

    NASA Astrophysics Data System (ADS)

    Salas-de la Cruz, David; Denis, Jeffrey G.; Griffith, Matthew D.; King, Daniel R.; Heiney, Paul A.; Winey, Karen I.

    2012-02-01

    We have designed, constructed, and evaluated an environmental chamber that has in situ dynamic control of temperature (25 to 90 °C) and relative humidity (0% to 95%). The compact specimen chamber is designed for x-ray scattering in transmission with an escape angle of 2θ = ±30°. The specimen chamber is compatible with a completely evacuated system such as the Rigaku PSAXS system, in which the specimen chamber is placed inside a larger evacuated chamber (flight path). It is also compatible with x-ray systems consisting of evacuated flight tubes separated by small air gaps for sample placement. When attached to a linear motor (vertical displacement), the environmental chamber can access multiple sample positions. The temperature and relative humidity inside the specimen chamber are controlled by passing a mixture of dry and saturated gas through the chamber and by heating the chamber walls. Alternatively, the chamber can be used to control the gaseous environment without humidity. To illustrate the value of this apparatus, we have probed morphology transformations in Nafion® membranes and a polymerized ionic liquid as a function of relative humidity in nitrogen.

  17. Hierarchical Pore Morphology of Cretaceous Shale: A Small-Angle Neutron Scattering and Ultrasmall-Angle Neutron Scattering Study

    DOE PAGES

    Bahadur, J.; Melnichenko, Y. B.; Mastalerz, Maria; ...

    2014-09-25

    Shale reservoirs are becoming an increasingly important source of oil and natural gas supply and a potential candidate for CO 2 sequestration. Understanding the pore morphology in shale may provide clues to making gas extraction more efficient and cost-effective. The porosity of Cretaceous shale samples from Alberta, Canada, collected from different depths with varying mineralogical compositions, has been investigated by small- and ultrasmall-angle neutron scattering. Moreover these samples come from the Second White Specks and Belle Fourche formations, and their organic matter content ranges between 2 and 3%. The scattering length density of the shale specimens has been estimated usingmore » the chemical composition of the different mineral components. Scattering experiments reveal the presence of fractal and non-fractal pores. It has been shown that the porosity and specific surface area are dominated by the contribution from meso- and micropores. The fraction of closed porosity has been calculated by comparing the porosities estimated by He pycnometry and scattering techniques. There is no correlation between total porosity and mineral components, a strong correlation has been observed between closed porosity and major mineral components in the studied specimens.« less

  18. X-Ray Form Factor, Attenuation and Scattering Tables

    National Institute of Standards and Technology Data Gateway

    SRD 66 X-Ray Form Factor, Attenuation and Scattering Tables (Web, free access)   This database collects tables and graphs of the form factors, the photoabsorption cross section, and the total attenuation coefficient for any element (Z <= 92).

  19. Ion charge state distribution effects on elastic X-ray Thomson scattering

    NASA Astrophysics Data System (ADS)

    Iglesias, Carlos A.

    2018-03-01

    Analytic models commonly applied in elastic X-ray Thomson scattering cross-section calculations are used to generate results from a discrete ion charge distribution and an average charge description. Comparisons show that interchanging the order of the averaging procedure can appreciably alter the cross-section, especially for plasmas with partially filled K-shell bound electrons. In addition, two common approximations to describe the free electron density around an ion are shown to yield significantly different elastic X-ray Thomson scattering cross-sections.

  20. Synchrotron x-ray thermal diffuse scattering probes for phonons in Si/SiGe/Si trilayer nanomembranes

    DOE PAGES

    McElhinny, Kyle M.; Gopalakrishnan, Gokul; Savage, Donald E.; ...

    2016-05-17

    Nanostructures offer the opportunity to control the vibrational properties of via the scattering of phonons due to boundaries and mass disorder as well as through changes in the phonon dispersion due to spatial confinement. Advances in understanding these effects have the potential to lead to thermoelectrics with an improved figure of merit by lowering the thermal conductivity and to provide insight into electron-phonon scattering rates in nanoelectronics. However, characterizing the phonon population in nanomaterials has been challenging because of their small volume and because optical techniques probe only a small fraction of reciprocal space. Recent developments in x-ray scattering nowmore » allow the phonon population to be evaluated across all of reciprocal space in samples with volumes as small as several cubic micrometers. We apply this approach, synchrotron x-ray thermal diffuse scattering (TDS), to probe the population of phonons within a Si/SiGe/Si trilayer nanomembrane. The distributions of scattered intensity from Si/SiGe/Si trilayer nanomembranes and Si nanomembranes with uniform composition are qualitatively similar, with features arising from the elastic anisotropy of the diamond structure. The TDS signal for the Si/SiGe/Si nanomembrane, however, has higher intensity than the Si membrane of the same total thickness by approximately 3.75%. Possible origins of the enhancement in scattering from SiGe in comparison with Si include the larger atomic scattering factor of Ge atoms within the SiGe layer or reduced phonon frequencies due to alloying.« less