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Sample records for two-dimensional small-angle x-ray

  1. Processing two-dimensional X-ray diffraction and small-angle scattering data in DAWN 2.

    Science.gov (United States)

    Filik, J; Ashton, A W; Chang, P C Y; Chater, P A; Day, S J; Drakopoulos, M; Gerring, M W; Hart, M L; Magdysyuk, O V; Michalik, S; Smith, A; Tang, C C; Terrill, N J; Wharmby, M T; Wilhelm, H

    2017-06-01

    A software package for the calibration and processing of powder X-ray diffraction and small-angle X-ray scattering data is presented. It provides a multitude of data processing and visualization tools as well as a command-line scripting interface for on-the-fly processing and the incorporation of complex data treatment tasks. Customizable processing chains permit the execution of many data processing steps to convert a single image or a batch of raw two-dimensional data into meaningful data and one-dimensional diffractograms. The processed data files contain the full data provenance of each process applied to the data. The calibration routines can run automatically even for high energies and also for large detector tilt angles. Some of the functionalities are highlighted by specific use cases.

  2. Small angle X-ray scattering experiments with three-dimensional imaging gas detectors

    International Nuclear Information System (INIS)

    La Monaca, A.; Iannuzzi, M.; Messi, R.

    1985-01-01

    Measurements of small angle X-ray scattering of lupolen - R, dry collagen and dry cornea are presented. The experiments have been performed with synchrotron radiation and a new three-dimensional imaging drif-chamber gas detector

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

    Science.gov (United States)

    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.

  4. Small Angle X-Ray Scattering Detector

    Energy Technology Data Exchange (ETDEWEB)

    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., qmax/qmin approx=lO0.

  5. Small angle neutron scattering and small angle X-ray scattering ...

    Indian Academy of Sciences (India)

    Abstract. The morphology of carbon nanofoam samples comprising platinum nanopar- ticles dispersed in the matrix was characterized by small angle neutron scattering (SANS) and small angle X-ray scattering (SAXS) techniques. Results show that the structure of pores of carbon matrix exhibits a mass (pore) fractal nature ...

  6. ORNL 10-m small-angle X-ray scattering camera

    International Nuclear Information System (INIS)

    Hendricks, R.W.

    1979-12-01

    A new small-angle x-ray scattering camera utilizing a rotating anode x-ray source, crystal monochromatization of the incident beam, pinhole collimation, and a two-dimensional position-sensitive proportional counter was developed. The sample, and the resolution element of the detector are each approximately 1 x 1 mm 2 , the camera was designed so that the focal spot-to-sample and sample-to-detector distances may each be varied in 0.5-m increments up to 5 m to provide a system resolution in the range 0.5 to 4.0 mrad. A large, general-purpose specimen chamber has been provided into which a wide variety of special-purpose specimen holders can be mounted. The detector has an active area of 200 x 200 mm and has up to 200 x 200 resolution elements. The data are recorded in the memory of a minicomputer by a high-speed interface which uses a microprocessor to map the position of an incident photon into an absolute minicomputer memory address. The data recorded in the computer memory can be processed on-line by a variety of programs designed to enhance the user's interaction with the experiment. At the highest angular resolution (0.4 mrad), the flux incident on the specimen is 1.0 x 10 6 photons/s with the x-ray source operating at 45 kV and 100 mA. SAX and its associated programs OVF and MOT are high-priority, pre-queued, nonresident foreground tasks which run under the ModComp II MAX III operating system to provide complete user control of the ORNL 10-m small-angle x-ray scattering camera

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

    Energy Technology Data Exchange (ETDEWEB)

    Yagi, N; Ohta, N; Matsuo, T [Japan Synchrotron Radiation Research Institute, 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Tanaka, T; Terada, Y; Kamasaka, H; Kometani, T, E-mail: yagi@spring8.or.j [Ezaki Glico Co. Ltd., 4-6-5 Utajima, Nishiyodogawa-ku, Osaka 555-8502 (Japan)

    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 6{mu}m at BL40XU and 50{mu}m 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.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

    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.

  9. Investigations of time resolved x-ray wide-angle scattering and x-ray small-angle scattering at DESY

    International Nuclear Information System (INIS)

    Zachmann, H.G.; Gehrke, R.; Prieske, W.; Riekel, C.

    1985-01-01

    Instrumentation is described for the simultaneous wide-angle and small-angle x-ray scattering. The method was applied to the study of the isothermal crystallization of polyethylene terephthalates. In agreement with the classical theories of crystallization, the data showed that the density difference between the crystals and the non-crystalline regions does not change with time. The mechanisms of melting, recrystallization, and crystal thickening were investigated by small-angle x-ray scattering with stepwise changes and continuous changes of temperature using polyethylene terephthalate

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

    Energy Technology Data Exchange (ETDEWEB)

    Van Vaerenbergh, Pierre; Léonardon, Joachim; Sztucki, Michael; Boesecke, Peter; Gorini, Jacques; Claustre, Laurent; Sever, Franc; Morse, John; Narayanan, Theyencheri [ESRF - The European Synchrotron, F-38043 Grenoble (France)

    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 desired 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.

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

    Science.gov (United States)

    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.

  12. A high resolution position sensitive X-ray MWPC for small angle X-ray diffraction

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Stephenson, R.; Tappern, G.J.

    1981-02-01

    A small sealed-off delay line readout MWPC X-ray detector has been designed and built for small angle X-ray diffraction applications. Featuring a sensitive area of 100 mm x 25 mm it yields a spatial resolution of 0.13 mm (standard deviation) with a high rate capability and good quantum efficiency for copper K radiation. (author)

  13. Two-dimensional x-ray diffraction

    CERN Document Server

    He, Bob B

    2009-01-01

    Written by one of the pioneers of 2D X-Ray Diffraction, this useful guide covers the fundamentals, experimental methods and applications of two-dimensional x-ray diffraction, including geometry convention, x-ray source and optics, two-dimensional detectors, diffraction data interpretation, and configurations for various applications, such as phase identification, texture, stress, microstructure analysis, crystallinity, thin film analysis and combinatorial screening. Experimental examples in materials research, pharmaceuticals, and forensics are also given. This presents a key resource to resea

  14. Small angle x-ray scattering from proteins in solution

    International Nuclear Information System (INIS)

    de Souza, C.F.; Torriani, I.L.; Bonafe, C.F.S.; Merrelles, N.C.; Vachette, P.

    1989-01-01

    In this work the authors report experiments performed with giant respiratory proteins from annelids (erythrocruorins), known to have a molecular weight in the order of four million Daltons. Preliminary x-ray scattering data was obtained using a conventional rotating anode source. High resolution small angle scattering curves were obtained with synchrotron radiation from the DCI storage ring at LURE. Data from solutions with several protein concentrations were analyzed in order to determine low resolution dimensional parameters, using Guinier plots from the smeared scattering curves and the inverse transformation method

  15. In situ microfluidic dialysis for biological small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Skou, Magda; Skou, Soren; Jensen, Thomas Glasdam

    2014-01-01

    Owing to the demand for low sample consumption and automated sample changing capabilities at synchrotron small-angle X-ray (solution) scattering (SAXS) beamlines, X-ray microfluidics is receiving continuously increasing attention. Here, a remote-controlled microfluidic device is presented for sim...... in incidental sample purification. Hence, this versatile microfluidic device enables investigation of experimentally induced structural changes under dynamically controllable sample conditions. (C) 2014 International Union of Crystallography......Owing to the demand for low sample consumption and automated sample changing capabilities at synchrotron small-angle X-ray (solution) scattering (SAXS) beamlines, X-ray microfluidics is receiving continuously increasing attention. Here, a remote-controlled microfluidic device is presented...

  16. Small-angle X-ray scattering studies of thermally-induced globular protein gels

    International Nuclear Information System (INIS)

    Clark, A.H.; Tuffnell, C.D.

    1980-01-01

    Small-angle X-ray scattering has been applied to gels formed by heating globular proteins, in aqueous solution, above their unfolding temperatures. A number of BSA gels, previously characterised by electron microscopy, have been studied, and by setting up theoretical models for the scattering process, the X-ray data have been shown to be consistent with the microscope conclusions regarding network structure. It is concluded that the networks form by a linearly-directed aggregation of unfolded, disc-like, protein molecules, three-dimensional geometry being achieved by occasional branching, and/or cross-linking. Long-range inhomogeneities in network structure, easily observed by electron microscopy, and correlated with variations in pH or ionic strength, have an effect on X-ray scattering, and hence the X-ray method is sensitive not only to different network strand thicknesses, but to different degrees of uniformity as well. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Liu Yifei; Manjubala, Inderchand; Fratzl, Peter [Department of Biomaterials, Max Planck Institute of Colloids and Interfaces, 14424 Potsdam (Germany); Roschger, Paul [4th Medical Department, Ludwig Boltzmann Institute of Osteology at Hanusch Hospital of WGKK and AUVA Trauma Centre Meidling, 1140 Vienna (Austria); Schell, Hanna; Duda, Georg N, E-mail: fratzl@mpikg.mpg.d [Julius Wolff Institut and Center for Musculoskeletal Surgery, Charite- University Medicine Berlin, Augustenburger Platz 1, 13353 Berlin (Germany)

    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.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

    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.

  19. Application of a one-dimensional position-sensitive detector to a Kratky small-angle x-ray camera

    International Nuclear Information System (INIS)

    Russell, T.P.; Stein, R.S.; Kopp, M.K.; Zedler, R.E.; Hendricks, R.W.; Lin, J.S.

    1979-01-01

    A conventional Kratky small-angle collimation system has been modified to allow the use of a one-dimensional position-sensitive x-ray detector. The detector was designed specifically for use with a long-slit camera and has uniform sensitivity over the entire beam in the slit-length direction. Procedures for alignment of the collimation system are given, and a variety of tests of the performance of the system are presented. Among the latter are measurements of electronic noise and parasitic scattering as well as comparisons against samples which were also measured on other cameras. The good agreement of these comparisons demonstrates the success of the use of a position-sensitive detector with the Kratky collimation system

  20. Application of a one-dimensional position-sensitive detector to a Kratky small-angle x-ray camera

    Energy Technology Data Exchange (ETDEWEB)

    Russell, T.P.; Stein, R.S.; Kopp, M.K.; Zedler, R.E.; Hendricks, R.W.; Lin, J.S.

    1979-01-01

    A conventional Kratky small-angle collimation system has been modified to allow the use of a one-dimensional position-sensitive x-ray detector. The detector was designed specifically for use with a long-slit camera and has uniform sensitivity over the entire beam in the slit-length direction. Procedures for alignment of the collimation system are given, and a variety of tests of the performance of the system are presented. Among the latter are measurements of electronic noise and parasitic scattering as well as comparisons against samples which were also measured on other cameras. The good agreement of these comparisons demonstrates the success of the use of a position-sensitive detector with the Kratky collimation system.

  1. X-ray imaging device for one-dimensional and two-dimensional radioscopy

    International Nuclear Information System (INIS)

    1978-01-01

    The X-ray imaging device for the selectable one-dimensional or two-dimensional pictures of objects illuminated by X-rays, comprising an X-ray source, an X-ray screen, and an opto-electrical picture development device placed behind the screen, is characterized by an anamorphotic optical system, which is positioned with a one-dimensional illumination between the X-ray screen and the opto-electrical device and that a two-dimensional illumination will be developed, and that in view of the lens system which forms part of the opto-electrical device, there is placed an X-ray screen in a specified beam direction so that a magnified image may be formed by equalisation of the distance between the X-ray screen and the lens system. (G.C.)

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

    Energy Technology Data Exchange (ETDEWEB)

    Yennawar, Hemant [Pennsylvania State University, 8 Althouse Laboratory, University Park, PA 16802 (United States); Møller, Magda [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); University of Copenhagen, DK-2100 Copenhagen (Denmark); Gillilan, Richard [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); Yennawar, Neela, E-mail: nhy1@psu.edu [Pennsylvania State University, 8 Althouse Laboratory, University Park, PA 16802 (United States)

    2011-05-01

    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 crystal 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.

  3. Recent developments in X-ray and neutron small-angle scattering instrumentation and data analysis

    International Nuclear Information System (INIS)

    Schelten, J.

    1978-01-01

    The developments in instrumentation and data analysis that have occurred in the field of small-angle X-ray and neutron scattering since 1973 are reviewed. For X-rays, the cone camera collimation was invented, synchrotrons and storage rings were demonstrated to be intense sources of X-radiation, and one- and two-dimensional position-sensitive detectors were interfaced to cameras with both point and line collimation. For neutrons, the collimators and detectors on the Juelich and Grenoble machines were improved, new D11-type instruments were built or are under construction at several sites, double-crystal instruments were set up, and various new machines have been proposed. Significant progress in data analysis and evaluation has been made through application of mathematical techniques such as the use of spline functions, error minimization with constraints, and linear programming. Several special experiments, unusual in respect to the anisotropy of the scattering pattern, gravitational effects, moving scatterers, and dynamic fast time slicing, are discussed. (Auth.)

  4. Small-angle X-ray scattering of solutions

    International Nuclear Information System (INIS)

    Koch, M.H.J.; Stuhrmann, H.B.; Vachette, P.; Tardieu, A.

    1982-01-01

    The use of synchrotron radiation in small-angle X-ray scattering (SAXS) techniques in biological structural studies is described. The main features of the monochromatic radiation systems and the white radiation systems are considered. The detectors, data acquisition and experimental procedures are briefly described. Experimental results are presented for 1) measurements on dilute solutions and weak scatterers, 2) measurement of conformational transitions, 3) contrast variation experiments, 4) time-resolved measurements and 5) complex contrast variation. (U.K.)

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

    Science.gov (United States)

    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.

  6. Progresses in the measurement and evaluation of small-angle x-ray scattering data

    International Nuclear Information System (INIS)

    Bergmann, A.

    2000-08-01

    Scattering methods are a widely used technique for determining size and shape of particles in the mesoscopic size range. This work deals on the one hand with the development of instruments in the field of Small Angle x-ray Scattering (SAXS) and on the other hand with methodical contributions concerning the interpretation of small angle scattering data. After a short introduction about Small Angle Scattering (SAS) and its application in chapter one, follows in chapter two a derivation of the theory of Small Angle x-ray scattering. Thereafter indirect transformations (Generalized Indirect Fourier Transformation [GIFT], Indirect Fourier Transformation [IFT]) are discussed and in this connection the optimization of multidimensional hyper surfaces is described. There are different possibilities for optimizing such multidimensional surfaces. The pros and contras of the different optimization methods with respect to the evaluation of small angle scattering data from interacting systems are discussed in detail. Global optimization methods are mainly used, if the hypersurface, which has to be optimized, shows many local minima. The goal of the optimization is it to find the global minimum. It is essential, that the parameters of the hyper surface are independent of each other, as it is the case in the GIFT. If someone deals with problems in only few dimensions or with many boundary conditions, mostly local optimization routines are sufficient. Therefore a number of starting parameters for the optimization is chosen, which can be obtained systematically or randomly. The best solution obtained represents the result of the optimization procedure. Chapter 3 deals with the description of instruments used in the field of Small Angle x-ray Scattering. After a description of the components (x-ray sources, monochromators, detectors) of these instruments, the different beam geometries are discussed. In chapter 4 improvements of SAXS measurements on Kratky slit systems by Goebel

  7. Small angles X-ray diffraction and Mössbauer characterization of ...

    Indian Academy of Sciences (India)

    The effect of thermal annealing on the structure and magnetic properties of crystalline Tb/Fe multilayers has been studied using conversion electron Mössbauer spectrometry and small-angle X-ray diffraction. The growth of Tb–Fe amorphous alloy from the interface is observed with increasing annealing temperature.

  8. A preliminary study of breast cancer diagnosis using laboratory based small angle x-ray scattering

    Science.gov (United States)

    Round, A. R.; Wilkinson, S. J.; Hall, C. J.; Rogers, K. D.; Glatter, O.; Wess, T.; Ellis, I. O.

    2005-09-01

    Breast tissue collected from tumour samples and normal tissue from bi-lateral mastectomy procedures were examined using small angle x-ray scattering. Previous work has indicated that breast tissue disease diagnosis could be performed using small angle x-ray scattering (SAXS) from a synchrotron radiation source. The technique would be more useful to health services if it could be made to work using a conventional x-ray source. Consistent and reliable differences in x-ray scatter distributions were observed between samples from normal and tumour tissue samples using the laboratory based 'SAXSess' system. Albeit from a small number of samples, a sensitivity of 100% was obtained. This result encourages us to pursue the implementation of SAXS as a laboratory based diagnosis technique.

  9. A preliminary study of breast cancer diagnosis using laboratory based small angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Round, A R [Daresbury Laboratories, Warrington, WA4 4AD (United Kingdom); Wilkinson, S J [Daresbury Laboratories, Warrington, WA4 4AD (United Kingdom); Hall, C J [Daresbury Laboratories, Warrington, WA4 4AD (United Kingdom); Rogers, K D [Department of Materials and Medical Sciences, Cranfield University, Swindon, SN6 8LA (United Kingdom); Glatter, O [Department of Chemistry, University of Graz (Austria); Wess, T [School of Optometry and Vision Sciences, Cardiff University, Cardiff CF10 3NB, Wales (United Kingdom); Ellis, I O [Nottingham City Hospital, Nottingham (United Kingdom)

    2005-09-07

    Breast tissue collected from tumour samples and normal tissue from bi-lateral mastectomy procedures were examined using small angle x-ray scattering. Previous work has indicated that breast tissue disease diagnosis could be performed using small angle x-ray scattering (SAXS) from a synchrotron radiation source. The technique would be more useful to health services if it could be made to work using a conventional x-ray source. Consistent and reliable differences in x-ray scatter distributions were observed between samples from normal and tumour tissue samples using the laboratory based 'SAXSess' system. Albeit from a small number of samples, a sensitivity of 100% was obtained. This result encourages us to pursue the implementation of SAXS as a laboratory based diagnosis technique.

  10. A preliminary study of breast cancer diagnosis using laboratory based small angle x-ray scattering

    International Nuclear Information System (INIS)

    Round, A R; Wilkinson, S J; Hall, C J; Rogers, K D; Glatter, O; Wess, T; Ellis, I O

    2005-01-01

    Breast tissue collected from tumour samples and normal tissue from bi-lateral mastectomy procedures were examined using small angle x-ray scattering. Previous work has indicated that breast tissue disease diagnosis could be performed using small angle x-ray scattering (SAXS) from a synchrotron radiation source. The technique would be more useful to health services if it could be made to work using a conventional x-ray source. Consistent and reliable differences in x-ray scatter distributions were observed between samples from normal and tumour tissue samples using the laboratory based 'SAXSess' system. Albeit from a small number of samples, a sensitivity of 100% was obtained. This result encourages us to pursue the implementation of SAXS as a laboratory based diagnosis technique

  11. Ordered array of ω particles in β-Ti matrix studied by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Šmilauerová, J.; Harcuba, P.; Stráský, J.; Stráská, J.; Janeček, M.; Pospíšil, J.; Kužel, R.; Brunátová, T.; Holý, V.; Ilavský, J.

    2014-01-01

    Nanosized particles of ω phase in a β-Ti alloy were investigated by small-angle X-ray scattering using synchrotron radiation. We demonstrated that the particles are spontaneously weakly ordered in a three-dimensional cubic array along the 〈100〉-directions in the β-Ti matrix. The small-angle scattering data fit well to a three-dimensional short-range-order model; from the fit we determined the evolution of the mean particle size and mean distance between particles during ageing. The self-ordering of the particles is explained by elastic interaction between the particles, since the relative positions of the particles coincide with local minima of the interaction energy. We performed numerical Monte Carlo simulation of the particle ordering and we obtained a good agreement with the experimental data

  12. Small angle X-ray scattering from hydrating tricalcium silicate

    International Nuclear Information System (INIS)

    Vollet, D.

    1983-01-01

    The small-angle X-ray scattering technique was used to study the structural evolution of hydrated tricalcium silicate at room temperature. The changes in specific area of the associated porosity and the evolution of density fluctuations in the solid hydrated phase were deduced from the scattering data. A correlation of these variations with the hydration mechanism is tried. (Author) [pt

  13. Small angles X-ray diffraction and Mössbauer characterization of ...

    Indian Academy of Sciences (India)

    Abstract. The effect of thermal annealing on the structure and magnetic properties of crystalline Tb/Fe multilayers has been studied using conversion electron Mössbauer spectrometry and small-angle X-ray diffraction. The growth of Tb–Fe amorphous alloy from the interface is observed with increasing annealing ...

  14. A customizable software for fast reduction and analysis of large X-ray scattering data sets: applications of the new DPDAK package to small-angle X-ray scattering and grazing-incidence small-angle X-ray scattering.

    Science.gov (United States)

    Benecke, Gunthard; Wagermaier, Wolfgang; Li, Chenghao; Schwartzkopf, Matthias; Flucke, Gero; Hoerth, Rebecca; Zizak, Ivo; Burghammer, Manfred; Metwalli, Ezzeldin; Müller-Buschbaum, Peter; Trebbin, Martin; Förster, Stephan; Paris, Oskar; Roth, Stephan V; Fratzl, Peter

    2014-10-01

    X-ray scattering experiments at synchrotron sources are characterized by large and constantly increasing amounts of data. The great number of files generated during a synchrotron experiment is often a limiting factor in the analysis of the data, since appropriate software is rarely available to perform fast and tailored data processing. Furthermore, it is often necessary to perform online data reduction and analysis during the experiment in order to interactively optimize experimental design. This article presents an open-source software package developed to process large amounts of data from synchrotron scattering experiments. These data reduction processes involve calibration and correction of raw data, one- or two-dimensional integration, as well as fitting and further analysis of the data, including the extraction of certain parameters. The software, DPDAK (directly programmable data analysis kit), is based on a plug-in structure and allows individual extension in accordance with the requirements of the user. The article demonstrates the use of DPDAK for on- and offline analysis of scanning small-angle X-ray scattering (SAXS) data on biological samples and microfluidic systems, as well as for a comprehensive analysis of grazing-incidence SAXS data. In addition to a comparison with existing software packages, the structure of DPDAK and the possibilities and limitations are discussed.

  15. X-ray and neutron small-angle scattering studies of human serum lipoproteins

    International Nuclear Information System (INIS)

    Luzzati, V.; Tardieu, A.; Mateu, L.; Sardet, C.; Stuhrmann, H.B.; Aggerbeck, L.; Scanu, A.M.

    1976-01-01

    The paper describes an extended x-ray study of two types of human serum lipoproteins and a neutron study of one of them. The results are similar and to some extent complementary. Serum lipoproteins provide an excellent illustration of the wealth of information that can be obtained by a small-angle scattering approach to the structure of particles with non-uniform density distribution, by using solvents of variable density

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

    Science.gov (United States)

    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.

  17. Small angle X ray diffraction investigation of twinned opal_like structures

    NARCIS (Netherlands)

    Samusev, A.K.; Sinev, I.S.; Samusev, K.B.; Rybin, M.V.; Mistonov, A.A.; Grigoryeva, N.A.; Grigoriev, S.V.; Petukhov, A.V.; Byelov, D.; Trofimova, E.Y.; Kurdyukov, D.A.; Golubev, V.G.; Limonov, M.F.

    2012-01-01

    Small angle X ray diffraction from synthetic opal films has been investigated as a function of the orientation of the sample. All the observed (hkl) diffraction reflections have been interpreted. The reconstruct tion of the reciprocal lattice of the studied opal films has been carried out. The

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

    Science.gov (United States)

    Grant, Thomas D; Luft, Joseph R; Carter, Lester G; Matsui, Tsutomu; Weiss, Thomas M; Martel, Anne; Snell, Edward H

    2015-01-01

    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 targets for which high-resolution structures have been determined via X-ray crystallography or nuclear magnetic resonance (NMR) spectroscopy. The 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.

  19. Degradation of periodic multilayers as seen by small-angle x-ray scattering and x-ray diffraction

    CERN Document Server

    Rafaja, D; Simek, D; Zdeborova, L; Valvoda, V

    2002-01-01

    The capabilities of small-angle x-ray scattering (SAXS) and wide-angle x-ray diffraction (XRD) to recognize structural changes in periodic multilayers were compared on Fe/Au multilayers with different degrees of structural degradation. Experimental results have shown that both methods are equally sensitive to the multilayer degradation, i.e., to the occurrence of non-continuous interfaces, to short-circuits in the multilayer structure and to the multilayer precipitation. XRD yielded additional information on the multilayer crystallinity, whilst SAXS could better recognize fragments of a long-range periodicity (remnants of the original multilayer structure). Changes in the multilayer structure were initiated by successive annealing at 200 and 300 deg. C. Experimental data were complemented by numerical simulations performed using a combination of optical theory and the distorted wave Born approximation for SAXS or the kinematical Born approximation for XRD.

  20. Comparison of X-ray and neutron small-angle scattering from an Al-Zn alloy

    International Nuclear Information System (INIS)

    Gerold, V.; Epperson, J.E.; Gerstenberg, K.W.

    1978-01-01

    The normalized integrated small-angle scattered intensity for Al-Zn alloys should be independent of whether the measurements are made with X-rays or neutrons. In order to check this, and thus the correction and standardization processes, the small-angle scattering from an Al-5.05 at.% Zn alloy containing GP zones was measured with these two types of radiation. The data were corrected and converted to absolute units with reference to the commonly accepted secondary standards: vanadium for the neutron data and polyethylene (Lupolen) for the X-ray data. The results are shown to differ by, at best, 6% if reasonable values for the change in atomic volume with alloy composition are taken into account. These findings are compared with those available from the literature, and the consistency is found to be somewhat lacking. Additional careful work is clearly needed to determine if the difficulty is traceable to the data correction or to the conversion to absolute units. (Auth.)

  1. Data Analysis Of Small Angle X-Ray Solution Scattering And Its ...

    African Journals Online (AJOL)

    Small Angle X-ray Scattering analysis was used for the study of the protein, Human Tumour Necrosis Factor (TNF) homogeneously dispersed in solution. The experiment consisted in sending a well collimated beam of synchrotron radiation of wavelength, λ through the sample and measuring the variation of the intensity as a ...

  2. Small-angle and wide-angle X-ray scattering study on the bilayer structure of synthetic and bovine heart cardiolipins

    International Nuclear Information System (INIS)

    Takahashi, Hiroshi; Hayakawa, Tomohiro; Ito, Kazuki; Takata, Masaki; Kobayashi, Toshihide

    2010-01-01

    Cardiolipin (CL) is a membrane phospholipid containing four fatty acid chains. CL plays an important role in energy transformation in mitochondria. The disorder of CL biosynthesis is involved in a genetic disease, Barth syndrome. Alteration of fatty acid composition of CLs has been found in Barth syndrome patients, i.e., the decrease of unsaturated fatty acid chains. In this study, we investigated how the degree of saturation alters the structure of CL bilayers by using X-ray scattering. Bovine heart CL and two synthetic CLs were compared. Fatty acid compositions of these three CLs have different saturation. Small-angle X-ray scattering data showed that the decrease of the number of double bonds in the unsaturated fatty acid chains causes to thicken the CL bilayers. In addition, wide-angle X-ray scattering data suggested that the decrease reduces the degree of disorder of the hydrophobic region in a liquid crystalline phase. These results may be related to the dysfunction of mitochondria in Barth syndrome.

  3. Small-angle and wide-angle X-ray scattering study on the bilayer structure of synthetic and bovine heart cardiolipins

    Energy Technology Data Exchange (ETDEWEB)

    Takahashi, Hiroshi [Biophysics Laboratory, Department of Chemistry and Chemical Biology, Gunma University, Maebashi, Gunma, 371-8510 (Japan); Hayakawa, Tomohiro [Life Science Laboratory, Advanced Materials Laboratories, Sony Corporation, Yushima, Bunkyo-ku, Tokyo, 113-8510 (Japan); Ito, Kazuki; Takata, Masaki [Structural Materials Science Laboratory, RIKEN SPring-8 Center, Sayo, Hyogo 679-5148 (Japan); Kobayashi, Toshihide, E-mail: htakahas@chem-bio.gunma-u.ac.j [Lipid Biology Laboratory, RIKEN, Wako, Saitama 351-0198 (Japan)

    2010-10-01

    Cardiolipin (CL) is a membrane phospholipid containing four fatty acid chains. CL plays an important role in energy transformation in mitochondria. The disorder of CL biosynthesis is involved in a genetic disease, Barth syndrome. Alteration of fatty acid composition of CLs has been found in Barth syndrome patients, i.e., the decrease of unsaturated fatty acid chains. In this study, we investigated how the degree of saturation alters the structure of CL bilayers by using X-ray scattering. Bovine heart CL and two synthetic CLs were compared. Fatty acid compositions of these three CLs have different saturation. Small-angle X-ray scattering data showed that the decrease of the number of double bonds in the unsaturated fatty acid chains causes to thicken the CL bilayers. In addition, wide-angle X-ray scattering data suggested that the decrease reduces the degree of disorder of the hydrophobic region in a liquid crystalline phase. These results may be related to the dysfunction of mitochondria in Barth syndrome.

  4. Application of small-angle X-ray scattering for differentiation among breast tumors

    International Nuclear Information System (INIS)

    Changizi, V.; Kheradmand, A. Arab; Oghabian, M.A.

    2008-01-01

    Small-angle X-ray scattering (SAXS) is an X-ray diffraction-based technique where a narrow collimated beam of X-rays is focused onto a sample and the scattered X-rays recorded by a detector. The pattern of the scattered X-rays carries information on the molecular structure of the material. As breast cancer is the most widespread cancer in women and differentiation among its tumors is important, this project compared the results of coherent X-ray scattering measurements obtained from benign and malignant breast tissues. The energy-dispersive method with a setup including X-ray tube, primary collimator, sample holder, secondary collimator and high-purity germanium (HpGe) detector was used. One hundred thirty-one breast-tissue samples, including normal, fibrocystic changes and carcinoma, were studied at the 6 deg scattering angle. Diffraction profiles (corrected scattered intensity versus momentum transfer) of normal, fibrocystic changes and carcinoma were obtained. These profiles showed a few peak positions for adipose (1.15 ± 0.06 nm -1 ), mixed normal (1.15 ± 0.06 nm -1 and 1.4 ± 0.04 nm -1 ), fibrocystic changes (1.46 ± 0.05 nm -1 and 1.74 ± 0.04 nm -1 ) and carcinoma (1.55 ± 0.04 nm -1 , 1.73 ± 0.06 nm -1 , 1.85 ± 0.05 nm -1 ). We were able to differentiate between normal, fibrocystic changes (benign) and carcinoma (malignant) breast tissues by SAXS. However, we were unable to differentiate between different types of carcinoma. (author)

  5. Application of small-angle X-ray scattering for differentiation among breast tumors

    Directory of Open Access Journals (Sweden)

    Changizi V

    2008-01-01

    Full Text Available Small-angle X-ray scattering (SAXS is an X-ray diffraction-based technique where a narrow collimated beam of X-rays is focused onto a sample and the scattered X-rays recorded by a detector. The pattern of the scattered X-rays carries information on the molecular structure of the material. As breast cancer is the most widespread cancer in women and differentiation among its tumors is important, this project compared the results of coherent X-ray scattering measurements obtained from benign and malignant breast tissues. The energy-dispersive method with a setup including X-ray tube, primary collimator, sample holder, secondary collimator and high-purity germanium (HpGe detector was used. One hundred thirty-one breast-tissue samples, including normal, fibrocystic changes and carcinoma, were studied at the 6° scattering angle. Diffraction profiles (corrected scattered intensity versus momentum transfer of normal, fibrocystic changes and carcinoma were obtained. These profiles showed a few peak positions for adipose (1.15 ± 0.06 nm -1 , mixed normal (1.15 ± 0.06 nm -1 and 1.4 ± 0.04 nm -1 , fibrocystic changes (1.46 ± 0.05 nm -1 and 1.74 ± 0.04 nm -1 and carcinoma (1.55 ± 0.04 nm -1 , 1.73 ± 0.06 nm -1 , 1.85 ± 0.05 nm -1 . We were able to differentiate between normal, fibrocystic changes (benign and carcinoma (malignant breast tissues by SAXS. However, we were unable to differentiate between different types of carcinoma.

  6. Structural features of various kinds of carbon fibers as determined by small-angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Li, Denghua; Du, Sujun [Shanxi Transportation Research Institute, National and Local Joint Engineering Laboratory of Advanced Road Materials, Taiyuan (China); Lu, Chunxiang; Wu, Gangping; Yang, Yu; Wang, Lina [Chinese Academy of Sciences, National Engineering Laboratory for Carbon Fiber Technology, Institute of Coal Chemistry, Taiyuan (China)

    2016-11-15

    The structural features of polyacrylonitrile and pitch-based carbon fibers were analyzed from a comprehensive point of view by X-ray measurements and related techniques. The results indicated that the undulating graphite ribbon with embedded microvoid was the main structural unit for graphitic fibers. The void's parameters for these fibers could be obtained directly by small-angle X-ray scattering following the classic method deduced based on the typical two-phase system (i.e., Porod's law, Guinier's law and Debye's law). The non-graphitic fibers, however, were composed of two-dimensional turbostratic crystallites in the aggregation of microfibril and thus had a quasi two-phase structure (microfibril, interfibrillar amorphous structure and microvoid embedded within the microfibril). The extended Debye or Beaucage model in this case should be applied in order to obtain the structural parameters. It also revealed that the quasi two-phase system would complete its transformation to two-phase system during high-temperature graphitization. Therefore, the degree of graphitization was speculated to be the essential indicator distinguishing graphitic fibers from non-graphitic ones and would be helpful in understanding the transformation of structural features during the graphitization of carbon fibers. (orig.)

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

    Science.gov (United States)

    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.

  8. Fractal morphology in lignite coal: a small angle x-ray scattering investigation

    International Nuclear Information System (INIS)

    Chitra, R.; Sen, D.; Mazumder, S.; Chandrasekaran, K.S.

    1999-01-01

    Small angle x-ray scattering technique has been used to study the pore morphology in lignite coal from Neyveli lignite mine (Tamilnadu, India). The sample were collected from three different locations of the same mine. SAXS profiles from all the three samples show almost identical functionality, irrespective of the locations from where the samples were collected. SAXS experiment using two different wavelengths also exhibit same functionality indicating the absence of multiple scattering. The analysis indicates the surface fractal nature of the pore morphology. The surface fractal dimension is calculated to be 2.58. (author)

  9. Femtosecond X-ray diffraction from two-dimensional protein crystals

    Directory of Open Access Journals (Sweden)

    Matthias Frank

    2014-03-01

    Full Text Available X-ray diffraction patterns from two-dimensional (2-D protein crystals obtained using femtosecond X-ray pulses from an X-ray free-electron laser (XFEL are presented. To date, it has not been possible to acquire transmission X-ray diffraction patterns from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permit a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy approach at the Linac Coherent Light Source, Bragg diffraction was acquired to better than 8.5 Å resolution for two different 2-D protein crystal samples each less than 10 nm thick and maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.

  10. Study of change in dispersion and orientation of clay platelets in a polymer nanocomposite during tensile test by variostage small-angle X-ray scattering

    CSIR Research Space (South Africa)

    Bandyopadhyay, J

    2012-04-01

    Full Text Available To understand the change in dispersion and orientation of clay platelets in three-dimensional space during tensile test, neat polymer and its nanocomposite samples were studied by small- and wide-angle X-ray scattering (SWAXS). The samples after...

  11. BioXTAS RAW, a software program for high-throughput automated small-angle X-ray scattering data reduction and preliminary analysis

    DEFF Research Database (Denmark)

    Nielsen, S.S.; Toft, K.N.; Snakenborg, Detlef

    2009-01-01

    A fully open source software program for automated two-dimensional and one-dimensional data reduction and preliminary analysis of isotropic small-angle X-ray scattering (SAXS) data is presented. The program is freely distributed, following the open-source philosophy, and does not rely on any...... commercial software packages. BioXTAS RAW is a fully automated program that, via an online feature, reads raw two-dimensional SAXS detector output files and processes and plots data as the data files are created during measurement sessions. The software handles all steps in the data reduction. This includes...... mask creation, radial averaging, error bar calculation, artifact removal, normalization and q calibration. Further data reduction such as background subtraction and absolute intensity scaling is fast and easy via the graphical user interface. BioXTAS RAW also provides preliminary analysis of one...

  12. Small angle neutron and x-ray scattering studies of self-assembled nano structured materials

    International Nuclear Information System (INIS)

    Choi, Sung Min

    2009-01-01

    Full text: Small angle neutron and x-ray scattering are very powerful techniques to investigate nano structured materials. In this presentation, examples of nano structured materials investigated by neutron and x-ray scattering will be presented. Part I: The unique anisotropic physical properties of columnar discotic liquid crystals (DLCs) have attracted considerable interest for their potential applications as electronic devices. For many practical applications, however, it is crucial to obtain uniaxially oriented and highly ordered columnar superstructures of DLC molecules covering macroscopic area. Here, we present a simple and straight-forward approach to fabricate uniaxially oriented and highly ordered columnar superstructures of cobalt octa(n-decylthio) porphyrazine (CoS 1 0), a discotic supra-molecule, in bulk and on substrates [1] over a macroscopic length scale, utilizing an applied magnetic field and the interaction of CoS 1 0 with an OTS-functionalized substrate. The details of the oriented and ordered columnar nano-structures are investigated by SANS and GISAXS. Part II: Self-assembly of one-dimensional (1D) nanoparticles with metallic or semiconducting properties into highly ordered superstructures using various interactions has been of great interest as a route towards materials with new functionalities. Here, we report a new phase diagram of negatively charged 1D nanoparticle (cROD) and cationic liposome (CL) complexes in water which exhibit three different highly ordered phases [2]. Small angle neutron and x-ray scattering measurements show that the cROD-CL complexes exhibit three different highly ordered phases, intercalated lamellar, doubly intercalated lamellar and centered rectangular phases, depending on particle curvature and electrostatic interactions. The new phase diagram can be used to understand and design new highly ordered self-assemblies of 1D nanoparticles in soft matter which provide new functionalities. (author)

  13. Three-dimensional reciprocal space x-ray coherent scattering tomography of two-dimensional object.

    Science.gov (United States)

    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

  14. Small-angle X-ray scattering studies of metastable intermediates of beta-lactoglobulin isolated after heat-induced aggregation

    DEFF Research Database (Denmark)

    Carrotta, R.; Arleth, L.; Pedersen, J.S.

    2003-01-01

    Small-angle x-ray scattering was used for studying intermediate species, isolated after heat-induced aggregation of the A variant of bovine P-lactoglobulin. The intermediates were separated in two fractions, the heated metastable dimer and heated metastable oligomers larger than the dimer. The pa...

  15. Investigation of polydisperse, disordered, and fractal systems by small-angle x-ray and neutron scattering

    International Nuclear Information System (INIS)

    Schmidt, P.W.; Tang, Y.; Roell, A.; Steiner, M.; Hoehr, A.; Neumann, H.B.

    1990-01-01

    Small-angle x-ray and neutron scattering are useful methods for investigating the structure of materials on a scale from about 10 to 2000 A. Some experimental procedures and methods of data analysis for small-angle scattering are outlined, and the use of small-angle scattering for studies of polydisperse systems (i.e., systems of particles of different size) of independently scattering particles is reviewed. Some general properties of the small-angle scattering from mass and surface fractals are discussed, and some applications of these concepts in recent experimental studies are presented. Results obtained in calculations of the small-angle scattering from a model of a surface are summarized. (author) 3 figs., 18 refs

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

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Sen; Luo, Sheng-Nian

    2018-02-16

    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, fundamental harmonic bandwidth and high harmonics. The effects of bandwidth, spectral shape and high harmonics on particle size determination are evaluated quantitatively.

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

    Science.gov (United States)

    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.

  18. Quantitative anomalous small-angle X-ray scattering - The determination of chemical concentrations in nano-scale phases

    International Nuclear Information System (INIS)

    Goerigk, G.; Huber, K.; Mattern, N.; Williamson, D.L.

    2012-01-01

    In the last years Anomalous Small-Angle X-ray Scattering became a precise quantitative method resolving scattering contributions two or three orders of magnitude smaller compared to the overall small-angle scattering, which are related to the so-called pure-resonant scattering contribution. Additionally to the structural information precise quantitative information about the different constituents of multi-component systems like the fraction of a chemical component implemented into the materials nano-structures are obtained from these scattering contributions. The application of the Gauss elimination algorithm to the vector equation established by ASAXS measurements at three X-ray energies is demonstrated for three examples from chemistry and solid state physics. All examples deal with the quantitative analysis of the Resonant Invariant (RI-analysis). From the integrals of the pure-resonant scattering contribution the chemical concentrations in nano-scaled phases are determined. In one example the correlated analysis of the Resonant Invariant and the Non-resonant Invariant (NI-analysis) is employed. (authors)

  19. Small-angle x-ray scattering from the early growth stages of zeolite A

    International Nuclear Information System (INIS)

    Singh, P.; White, J.

    1999-01-01

    Full text: The work presented here with the use of SAXS (Small-Angle X-ray Scattering) is in attempt to identify a different paradigm to the organic template induced crystallization of zeolites, in particular zeolite 'A'. The reactions have been followed by small angle X-ray scattering from the time of first mixing of the constituents until the final separation of zeolite A crystals. The processes happening during the growth are expected to follow successive transformation of intermediate metastable phases until the formation of thermodynamically most stable phase and scattering signatures from these developments may be useful for extracting interesting information about the processes in situ. The scattering functions from a synthesis system of zeolite 'A' at the initial and final stage of reaction are presented.The different growth processes of zeolite 'A' from different silicate and aluminium sources are found. The differences are attributed to different rate limiting steps in the syntheses

  20. Three-dimensional x-ray diffraction detection and visualization

    International Nuclear Information System (INIS)

    Allahkarami, Masoud; Hanan, Jay C

    2014-01-01

    A new method of sensing and analyzing three-dimensional (3D) x-ray diffraction (XRD) cones was introduced. Using a two-dimensional area detector, a sequence of frames was collected while moving the detector away from the sample with small equally spaced steps and keeping all other parameters constant. A 3D dataset was created from the subsequent frames. The 3D x-ray diffraction (XRD 3 ) pattern contains far more information than a one-dimensional profile collected with the conventional diffractometer and 2D x-ray diffraction (XRD 2 ). The present work discusses some fundamentals about XRD 3 , such as the data collection method, 3D visualization, diffraction data interpretation and potential applications of XRD 3 . (paper)

  1. Study of humic acids by small-angle X-ray and neutron scattering

    International Nuclear Information System (INIS)

    Timchenko, A.; Trubetskaya, O.; Kihara, H.

    1999-01-01

    Humic acids are an important component of natural ecological system and represent a polydisperse complex of natural biopolymers with molecular masses from several to hundreds kilodaltons. They are both a source of organic compounds and a protector against anthropogenic pollutions of biosphere. The aim of the report is to underline some possibilities of small-angle X-ray and neutron scattering to study HA and their fractions. (author)

  2. Investigation of nanoscale structures by small-angle X-ray scattering in a radiochromic dosimeter

    DEFF Research Database (Denmark)

    Skyt, Peter Sandegaard; Jensen, Grethe Vestergaard; Wahlstedt, Isak Hannes

    2014-01-01

    This study examines the nanoscale structures in a radiochromic dosimeter that was based on leuco-malachite-green dye and the surfactant sodium dodecyl sulfate (SDS) suspended in a gelatin matrix. Small-angle X-ray scattering was used to investigate the structures of a range of compositions...

  3. Three-dimensional x-ray stereometry from paired coplanar images: a progress report.

    Science.gov (United States)

    Baumrind, S; Moffitt, F H; Curry, S

    1983-10-01

    More than fifty years ago, Broadbent reported the development of a three-dimensional cephalometric method which complexed information from pairs of x-ray images oriented in two planes at right angles to each other. Empirical problems have prevented the routine clinical use of this "biplanar" method, notwithstanding its obvious conceptual brilliance. The present article reports on recent work toward the development of an alternative method of three-dimensional cephalometry in which the two images of each x-ray pair are positioned in the same plane rather than being at right angles to each other. It is believed that this "coplanar" method avoids many of the technical problems that have limited the use of the Broadbent method.

  4. Integrative structural modeling with small angle X-ray scattering profiles

    Directory of Open Access Journals (Sweden)

    Schneidman-Duhovny Dina

    2012-07-01

    Full Text Available Abstract Recent technological advances enabled high-throughput collection of Small Angle X-ray Scattering (SAXS profiles of biological macromolecules. Thus, computational methods for integrating SAXS profiles into structural modeling are needed more than ever. Here, we review specifically the use of SAXS profiles for the structural modeling of proteins, nucleic acids, and their complexes. First, the approaches for computing theoretical SAXS profiles from structures are presented. Second, computational methods for predicting protein structures, dynamics of proteins in solution, and assembly structures are covered. Third, we discuss the use of SAXS profiles in integrative structure modeling approaches that depend simultaneously on several data types.

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

    Science.gov (United States)

    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.

  6. Anomalous small-angle x-ray scattering of a femtosecond irradiated germano silicate fibre preform.

    Energy Technology Data Exchange (ETDEWEB)

    Hindle, F.; Fertein, E.; Seifert, S.; Przygodski, C.S.; Bocquet, R.; Douay, M.; Bychkov, E.; Experimental Facilities Division (APS); LPCA, CNRS; PhLAM; Univ. des Sciences et Tech. de Lille

    2005-01-01

    RADIATION is shown to induce significant mesoscopic structure. The scattering intensity for irradiated glasses is close to two orders of magnitude greater than that of unexposed material. Anomalous small-angle X-ray scattering (ASAXS) around the germanium K-edge for the silica and germanium doped silica regions of a fiber preform is used to demonstrate that identical structures are induced in both glass materials, with germanium displaying a capacity to isomorphically replace silicon in the case of the germanium doped silica. Analysis of measured scattering indicates that photo-inscribed features are produced at two distinct scales with typical radii of R {approx} 20 Angstroms and R{sub min} {approx} 200 Angstroms.

  7. Small angle X-ray scattering on concentrated hemoglobin solutions

    International Nuclear Information System (INIS)

    Zinke, M.; Damaschun, G.; Mueller, J.J.; Ruckpaul, K.

    1978-01-01

    The small-angle X-ray scattering technique was used to determine the intermolecular structure and interaction potentials in oxi-and deoxi-hemoglobin solutions. The pair correlation function obtained by the ZERNICKE-PRINS equation characterizes the intermolecular structure of the hemoglobin molecules. The intermolecular structure is concentration dependent. The hemoglobin molecules have a 'short range order structure' with a range of about 4 molecule diameters at 324 g/l. The potential functions of the hemoglobin-hemoglobin interaction have been determined on the basis of fluid theories. Except for the deoxi-hemoglobin solution having the concentration 370 g/l, the pair interaction consists in a short repulsion and a weak short-range attraction against kT. The potential minimum is between 1.2 - 1.5 nm above the greatest hemoglobin diameter. (author)

  8. A high resolution, high counting rate bidimensional, MWPC imaging detector for small angle X-ray diffraction studies

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Sawyer, E.C.; Stephenson, R.

    1981-07-01

    The performance is reported of a 200 mm x 200 mm X-ray imaging MWPC aimed at applications in small angle X-ray diffraction and scattering. With quantum energies of approximately 8 keV high spatial resolution (+- 0.5 mm x +- 0.14 mm) with a capability for data taking at >approximately 350 kHz is reported. The detection efficiency is approximately 75% and the detector operates as a sealed unit with a long lifetime. (author)

  9. Small-angle x-ray scattering investigation of the solution structure of troponin C

    International Nuclear Information System (INIS)

    Hubbard, S.R.; Hodgson, K.O.; Doniach, S.

    1988-01-01

    X-ray crystallographic studies of troponin C have revealed a novel protein structure consisting of two globular domains, each containing two Ca 2+ -binding sites, connected via a nine-turn alpha-helix, three turns of which are fully exposed to solvent. Since the crystals were grown at pH approximately 5, it is of interest to determine whether this structure is applicable to the protein in solution under physiological conditions. We have used small-angle x-ray scattering to examine the solution structure of troponin C at pH 6.8 and the effect of Ca 2+ on the structure. The scattering data are consistent with an elongated structure in solution with a radius of gyration of approximately 23.0 A, which is quite comparable to that computed for the crystal structure. The experimental scattering profile and the scattering profile computed from the crystal structure coordinates do, however, exhibit differences at the 40-A level. A weak Ca 2+ -facilitated dimerization of troponin C was observed. The data rule out large Ca 2+ -induced structural changes, indicating rather that the molecule with Ca 2+ bound is only slightly more compact than the Ca 2+ -free molecule

  10. Interpretation and Utility of the Moments of Small-Angle X-Ray Scattering Distributions.

    Science.gov (United States)

    Modregger, Peter; Kagias, Matias; Irvine, Sarah C; Brönnimann, Rolf; Jefimovs, Konstantins; Endrizzi, Marco; Olivo, Alessandro

    2017-06-30

    Small angle x-ray scattering has been proven to be a valuable method for accessing structural information below the spatial resolution limit implied by direct imaging. Here, we theoretically derive the relation that links the subpixel differential phase signal provided by the sample to the moments of scattering distributions accessible by refraction sensitive x-ray imaging techniques. As an important special case we explain the scatter or dark-field contrast in terms of the sample's phase signal. Further, we establish that, for binary phase objects, the nth moment scales with the difference of the refractive index decrement to the power of n. Finally, we experimentally demonstrate the utility of the moments by quantitatively determining the particle sizes of a range of powders with a laboratory-based setup.

  11. Traceable size determination of PMMA nanoparticles based on Small Angle X-ray Scattering (SAXS)

    Energy Technology Data Exchange (ETDEWEB)

    Gleber, G; Cibik, L; Mueller, P; Krumrey, M [Physikalisch-Technische Bundesanstalt (PTB), Abbestrasse 2-12, 10587 Berlin (Germany); Haas, S; Hoell, A, E-mail: gudrun.gleber@ptb.d [Helmholtz-Zentrum-Berlin fuer Materialien und Energie (HZB), Albert-Einstein-Strasse 15, 12489 Berlin (Germany)

    2010-10-01

    The size and size distribution of PMMA nanoparticles has been investigated with SAXS (small angle X-ray scattering) using monochromatized synchrotron radiation. The uncertainty has contributions from the wavelength or photon energy of the radiation, the scattering angle and the fit procedure for the obtained scattering curves. The wavelength can be traced back to the lattice constant of silicon, and the scattering angle is traceable via geometric measurements of the detector pixel size and the distance between the sample and the detector. SAXS measurements and data evaluations have been performed at different distances and photon energies for two PMMA nanoparticle suspensions with low polydispersity and nominal diameters of 108 nm and 192 nm, respectively, as well as for a mixture of both. The relative variation of the diameters obtained for different experimental conditions was below {+-} 0.3 %. The determined number-weighted mean diameters of (109.0 {+-} 0.7) nm and (188.0 {+-} 1.3) nm, respectively, are close to the nominal values.

  12. Traceable size determination of PMMA nanoparticles based on Small Angle X-ray Scattering (SAXS)

    Science.gov (United States)

    Gleber, G.; Cibik, L.; Haas, S.; Hoell, A.; Müller, P.; Krumrey, M.

    2010-10-01

    The size and size distribution of PMMA nanoparticles has been investigated with SAXS (small angle X-ray scattering) using monochromatized synchrotron radiation. The uncertainty has contributions from the wavelength or photon energy of the radiation, the scattering angle and the fit procedure for the obtained scattering curves. The wavelength can be traced back to the lattice constant of silicon, and the scattering angle is traceable via geometric measurements of the detector pixel size and the distance between the sample and the detector. SAXS measurements and data evaluations have been performed at different distances and photon energies for two PMMA nanoparticle suspensions with low polydispersity and nominal diameters of 108 nm and 192 nm, respectively, as well as for a mixture of both. The relative variation of the diameters obtained for different experimental conditions was below ± 0.3 %. The determined number-weighted mean diameters of (109.0 ± 0.7) nm and (188.0 ± 1.3) nm, respectively, are close to the nominal values.

  13. Traceable size determination of PMMA nanoparticles based on Small Angle X-ray Scattering (SAXS)

    International Nuclear Information System (INIS)

    Gleber, G; Cibik, L; Mueller, P; Krumrey, M; Haas, S; Hoell, A

    2010-01-01

    The size and size distribution of PMMA nanoparticles has been investigated with SAXS (small angle X-ray scattering) using monochromatized synchrotron radiation. The uncertainty has contributions from the wavelength or photon energy of the radiation, the scattering angle and the fit procedure for the obtained scattering curves. The wavelength can be traced back to the lattice constant of silicon, and the scattering angle is traceable via geometric measurements of the detector pixel size and the distance between the sample and the detector. SAXS measurements and data evaluations have been performed at different distances and photon energies for two PMMA nanoparticle suspensions with low polydispersity and nominal diameters of 108 nm and 192 nm, respectively, as well as for a mixture of both. The relative variation of the diameters obtained for different experimental conditions was below ± 0.3 %. The determined number-weighted mean diameters of (109.0 ± 0.7) nm and (188.0 ± 1.3) nm, respectively, are close to the nominal values.

  14. Quantitative analysis of inclusions in low carbon free cutting steel using small-angle X-ray and neutron scattering

    International Nuclear Information System (INIS)

    Oba, Yojiro; Koppoju, Suresh; Ohnuma, Masato; Kinjo, Yuki; Tomota, Yo; Morooka, Satoshi; Suzuki, Jun-ichi; Yamaguchi, Daisuke; Koizumi, Satoshi; Sato, Masugu; Shiraga, Tetsuo

    2012-01-01

    The microstructure of inclusions in low carbon free cutting steel without lead addition was investigated using small-angle X-ray scattering (SAXS) coupled with small-angle neutron scattering (SANS). The two-dimensional (2D) SAXS pattern shows clear scattering due to inclusions composed of large elongated particles aligned along the rolling direction, and small isotropic particles. From a comparison of the simulated and experimental 2D SAXS patterns, the shapes of the inclusions are regarded as ellipsoid for the larger inclusions and spherical for the smaller inclusions. The length of the minor axis in the large inclusion is 6.9 μm, while the diameter of the small inclusion is 0.50 μm. The aspect ratio of the large inclusion is estimated to be 3.8 in the lower q region, and is reduced slightly to 3.5 in the higher q region from the azimuthal plots. The results of an alloy contrast variation (ACV) analysis using both the SAXS and SANS data indicate that the chemical composition of the inclusions is almost NaCl-type manganese sulfide, and that the amount of iron sulfide is low. The volume fractions are 1.4% for the large inclusions and 0.2% for the small inclusions. This is consistent with the area fraction estimated using an optical microscope, and indicates that nearly all of the sulfur in the steel sample forms the manganese sulfide inclusions. (author)

  15. Small-angle X-ray scattering (SAXS) for metrological size determination of nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Gleber, Gudrun; Krumrey, Michael; Cibik, Levent; Marggraf, Stefanie; Mueller, Peter [Physikalisch-Technische Bundesanstalt, Abbestr. 2-12, 10587 Berlin (Germany); Hoell, Armin [Helmholtz-Zentrum Berlin, Albert-Einstein-Str. 15, 12489 Berlin (Germany)

    2011-07-01

    To measure the size of nanoparticles, different measurement methods are available but their results are often not compatible. In the framework of an European metrology project we use Small-Angle X-ray Scattering (SAXS) to determine the size and size distribution of nanoparticles in aqueous solution, where the special challange is the traceability of the results. The experiments were performed at the Four-Crystal Monochromator (FCM) beamline in the laboratory of Physikalisch-Technische Bundesanstalt (PTB) at BESSY II using the SAXS setup of the Helmholtz-Zentrum Berlin (HZB). We measured different particles made of PMMA and gold in a diameter range of 200 nm down to about 10 nm. The aspects of traceability can be classified in two parts: the first is the experimental part with the uncertainties of distances, angles, and wavelength, the second is the part of analysis, with the uncertainty of the choice of the model used for fitting the data. In this talk we want to show the degree of uncertainty, which we reached in this work yet.

  16. The modular small-angle X-ray scattering data correction sequence.

    Science.gov (United States)

    Pauw, B R; Smith, A J; Snow, T; Terrill, N J; Thünemann, A F

    2017-12-01

    Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering: if it is not done sufficiently well, this may become evident only during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction, both in the laboratory and at the synchrotron. When applied in the proposed order to the raw signals, the resulting absolute scattering cross section will provide a high degree of accuracy for a very wide range of samples, with its values accompanied by uncertainty estimates. The method can be applied without modification to any pinhole-collimated instruments with photon-counting direct-detection area detectors.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  2. Studying nanostructure gradients in injection-molded polypropylene/montmorillonite composites by microbeam small-angle x-ray scattering

    DEFF Research Database (Denmark)

    Stribeck, Norbert; Schneider, Konrad; Zeinolebadi, Ahmad

    2014-01-01

    The core–shell structure in oriented cylindrical rods of polypropylene (PP) and nanoclay composites (NCs) from PP and montmorillonite (MMT) is studied by microbeam small-angle x-ray scattering (SAXS). The structure of neat PP is almost homogeneous across the rod showing regular semicrystalline......-shaped phyllosilicate filler particles....

  3. Automated microfluidic sample-preparation platform for high-throughput structural investigation of proteins by small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Nielsen, Søren Skou

    2011-01-01

    A new microfluidic sample-preparation system is presented for the structural investigation of proteins using small-angle X-ray scattering (SAXS) at synchrotrons. The system includes hardware and software features for precise fluidic control, sample mixing by diffusion, automated X-ray exposure...... control, UV absorbance measurements and automated data analysis. As little as 15 l of sample is required to perform a complete analysis cycle, including sample mixing, SAXS measurement, continuous UV absorbance measurements, and cleaning of the channels and X-ray cell with buffer. The complete analysis...

  4. Neutron and synchrotorn x-ray small angle scattering instruments for applications in biology at the Brookhaven National Laboratory

    International Nuclear Information System (INIS)

    Schoenborn, B.P.; Wise, D.S.; Schneider, D.K.

    1983-01-01

    Facilities for small angle x-ray and neutron scattering are described, with emphasis on the characterization of the primary beam of the neutron instrument and the spectrometer control logic of the synchrotron instrument

  5. Small-angle X-ray-scattering investigation and structural-model study of the fatty-acid synthetase from pig liver

    International Nuclear Information System (INIS)

    Folkhard, W.; Felser, B.; Pilz, I.; Kratky, O.; Dutler, H.; Vogel, H.

    1977-01-01

    The structure of the fatty acid synthetase from pig liver was studied on models based upon structural and functional properties selected from pertinent results available from numerous investigations carried out with fatty acid synthetase from this and other sources. When comparing small-angle X-ray-scattering curves calculated with these models and curves obtained from small-angle X-ray-scattering experiments carried out with the pig-liver enzyme, we tried to select a model which would lead to an acceptable correlation between the calculated and the experimental curves and at the same time fulfil the known structural and the functional requirements. The comparison of the curves was started with a model of low complexity. The observed discrepancy, together with arguments from the structural and the functional properties, helped decide which is the next most reasonable model to be considered. This procedure was repeated for five models of increasing complexity. In the model which led to the best fit the multienzyme complex is composed of two halves in an asymmetric conformation including hollow spaces. This highly anisotropic model would imply that the two halves change their conformation each time a synthetic cycle is completed and that the growing fatty acid is handed over from one half to the other. (orig.) [de

  6. Two-dimensional time-resolved X-ray diffraction study of liquid/solid fraction and solid particle size in Fe-C binary system with an electrostatic levitator furnace

    International Nuclear Information System (INIS)

    Yonemura, M; Okada, J; Ishikawa, T; Nanao, S; Watanabe, Y; Shobu, T; Toyokawa, H

    2013-01-01

    Liquid state provides functions such as matter transport or a reaction field and plays an important role in manufacturing processes such as refining, forging or welding. However, experimental procedures are significantly difficult for an observation of solidification process of iron and iron-based alloys in order to identify rapid transformations subjected to fast temperature evolution. Therefore, in order to study the solidification in iron and iron-based alloys, we considered a combination of high energy X-ray diffraction measurements and an electrostatic levitation method (ESL). In order to analyze the liquid/solid fraction, the solidification of melted spherical specimens was measured at a time resolution of 0.1 seconds during rapid cooling using the two-dimensional time-resolved X-ray diffraction. Furthermore, the observation of particle sizes and phase identification was performed on a trial basis using X-ray small angle scattering with X-ray diffraction.

  7. Assembly of positioner of automated two-dimensional scan coupled to X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Silva, Leonardo Santiago Melgaço

    2011-01-01

    This work describes the design and assembling of a prototype automated positioner two-dimensional scanning coupled to X-ray fluorescence spectrometry. The work aims to achieve a portable and easy to use, device of broad utility in the analysis of samples by X-ray fluorescence area of expertise and research. The two-dimensional scanning of the positioner is by means of two stepper motors controlled by a microcontroller PIC 16F877A, encoder and optical sensors. The user interacts with the XY table through an interface program for the Windows operating system, which communicates with the microcontroller through the serial port. The system of Fluorescence Spectroscopy incorporated into the positioner consists of a system commercially available system from the company AMPTEK, where the primary source of excitation of the sample was a source of 241 Am of 59.5 KeV emissions. Resolution and accuracy of tests were performed in the XY scanning process and reproducibility of the same kit with the fluorescence spectrometry X-ray. Qualitative tests by X-ray fluorescence spectrometry in samples were performed to demonstrate the applicability and versatility of the project. It follows that the prototype illustrates a possible adequately to portable device for X-ray spectrometry of two-dimensional. (author)

  8. Ion track annealing in quartz investigated by small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Schauries, D.; Afra, B.; Rodriguez, M.D. [Department of Electronic Materials Engineering, Research School of Physics and Engineering, The Australian National University, Canberra, ACT 2601 (Australia); Trautmann, C. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Technische Universität Darmstadt, 64287 Darmstadt (Germany); Hawley, A. [Australian Synchrotron, 800 Blackburn Road, Clayton, VIC 3168 (Australia); Kluth, P. [Department of Electronic Materials Engineering, Research School of Physics and Engineering, The Australian National University, Canberra, ACT 2601 (Australia)

    2015-12-15

    We report on the reduction of cross-section and length of amorphous ion tracks embedded within crystalline quartz during thermal annealing. The ion tracks were created via Au ion irradiation with an energy of 2.2 GeV. The use of synchrotron-based small angle X-ray scattering (SAXS) allowed characterization of the latent tracks, without the need for chemical etching. Temperatures between 900 and 1000 °C were required to see a notable change in track size. The shrinkage in cross-section and length was found to be comparable for tracks aligned perpendicular and parallel to the c-axis.

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

    Directory of Open Access Journals (Sweden)

    Wim Bras

    2014-11-01

    Full Text Available 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.

  10. Structure factor of dimyristoylphosphatidylcholine unilamellar vesicles: small-angle x-ray scattering study

    International Nuclear Information System (INIS)

    Kiselev, M.A.; Aksenov, V.L.; Lombardo, D.; Kisselev, A.M.; Lesieur, P.

    2003-01-01

    Small-angle X-ray scattering (SAXS) experiments have been performed on dimyristoylphosphatidylcholine (DMPC) unilamellar vesicles in 40% aqueous sucrose solution. Model of separated form factors was applied for the evaluation of SAXS curves from large unilamellar vesicles. For the first time vesicle structure factor, polydispersity, average radius and membrane thickness were calculated simultaneously from the SAXS curves at T=30 deg C for DMPC concentrations in the range from 15 to 75 mM (1-5% w/w). Structure factor correction to the scattering curve was shown to be negligibly small for the lipid concentration of 15 mM (1% w/w). It was proved to be necessary to introduce structure factor correction to the scattering curves for lipid concentrations ≥ 30 mM (2% w/w)

  11. Structure Factor of Dimyristoylphosphatidylcholine Unilamellar Vesicles Small-Angle X-Ray Scattering Study

    CERN Document Server

    Kiselev, M A; Kisselev, A M; Lesieur, P; Aksenov, V L

    2003-01-01

    Small-angle X-ray scattering (SAXS) experiments have been performed on dimyristoylphosphatidylcholine (DMPC) unilamellar vesicles in 40 % aqueous sucrose solution. Model of separated form factors was applied for the evaluation of SAXS curves from large unilamellar vesicles. For the first time vesicle structure factor, polydispersity, average radius and membrane thickness were calculated simultaneously from the SAXS curves at T=306{\\circ}C for DMPC concentrations in the range from 15 to 75 mM (1-5 % w/w). Structure factor correction to the scattering curve was shown to be negligibly small for the lipid concentration of 15 mM (1 % w/w). It was proved to be necessary to introduce structure factor correction to the scattering curves for lipid concentrations {\\ge}30 mM (2 % w/w).

  12. Structural evolution of regenerated silk fibroin under shear: Combined wide- and small-angle x-ray scattering experiments using synchrotron radiation

    International Nuclear Information System (INIS)

    Rossle, Manfred; Panine, Pierre; Urban, Volker S.; Riekel, Christine

    2004-01-01

    The structural evolution of regenerated Bombyx mori silk fibroin during shearing with a Couette cell has been studied in situ by synchrotron radiation small- and wide-angle x-ray scattering techniques. An elongation of fibroin molecules was observed with increasing shear rate, followed by an aggregation phase. The aggregates were found to be amorphous with β-conformation according to infrared spectroscopy. Scanning x-ray microdiffraction with a 5 (micro)m beam on aggregated material, which had solidified in air, showed silk II reflections and a material with equatorial reflections close to the silk I structure reflections, but with strong differences in reflection intensities. This silk I type material shows up to two low-angle peaks suggesting the presence of water molecules that might be intercalated between hydrogen-bonded sheets.

  13. Structural evolution of regenerated silk fibroin under shear: Combined wide- and small-angle x-ray scattering experiments using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Rossle, Manfred [European Molecular Biology Laboratory (EMBL), France; Panine, Pierre [European Synchrotron Radiation Facility (ESRF); Urban, Volker S [ORNL; Riekel, Christine [European Synchrotron Radiation Facility (ESRF)

    2004-04-01

    The structural evolution of regenerated Bombyx mori silk fibroin during shearing with a Couette cell has been studied in situ by synchrotron radiation small- and wide-angle x-ray scattering techniques. An elongation of fibroin molecules was observed with increasing shear rate, followed by an aggregation phase. The aggregates were found to be amorphous with {beta}-conformation according to infrared spectroscopy. Scanning x-ray microdiffraction with a 5 {micro}m beam on aggregated material, which had solidified in air, showed silk II reflections and a material with equatorial reflections close to the silk I structure reflections, but with strong differences in reflection intensities. This silk I type material shows up to two low-angle peaks suggesting the presence of water molecules that might be intercalated between hydrogen-bonded sheets.

  14. Development of soft x-ray time-resolved photoemission spectroscopy system with a two-dimensional angle-resolved time-of-flight analyzer at SPring-8 BL07LSU

    Energy Technology Data Exchange (ETDEWEB)

    Ogawa, Manami; Yamamoto, Susumu; Nakamura, Fumitaka; Yukawa, Ryu; Fukushima, Akiko; Harasawa, Ayumi; Kakizaki, Akito; Matsuda, Iwao [Institute for Solid State Physics, University of Tokyo, 5-1-5 Kashiwanoha, Chiba 277-8581 (Japan); Kousa, Yuka; Kondoh, Hiroshi [Department of Chemistry, Keio University, Yokohama 223-8522 (Japan); Tanaka, Yoshihito [RIKEN/SPring-8 Center, 1-1-1, Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan)

    2012-02-15

    We have developed a soft x-ray time-resolved photoemission spectroscopy system using synchrotron radiation (SR) at SPring-8 BL07LSU and an ultrashort pulse laser system. Two-dimensional angle-resolved measurements were performed with a time-of-flight-type analyzer. The photoemission spectroscopy system is synchronized to light pulses of SR and laser using a time control unit. The performance of the instrument is demonstrated by mapping the band structure of a Si(111) crystal over the surface Brillouin zones and observing relaxation of the surface photo-voltage effect using the pump (laser) and probe (SR) method.

  15. Small-angle X-ray scattering at high brilliance european synchrotrons for biotechnology and nano-technology

    International Nuclear Information System (INIS)

    Svergun, D.; Malfois, M.; Svergun, D.; Douka, M.; Riekel, Ch.; Perez, J.; Roessle, M.; Amenitsch, H.; Gunter Grossman, J.; Vestergaard, B.; Receveur-Brechot, V.; Roth, St.V.; Ferrari, E.

    2007-01-01

    Different issues such as micro-fluidic devices for SAXS (small-angle X-ray diffraction), the use of electro-spray and ion trapping for SAXS in the gas phase, the study of flexible and disordered proteins through SAXS, the time-resolved SAXS studies in solution, or the study of nano-structured soft materials, were addressed in this workshop. This document gathers the transparencies of the presentations

  16. Small-angle X-ray scattering at high brilliance european synchrotrons for biotechnology and nano-technology

    Energy Technology Data Exchange (ETDEWEB)

    Svergun, D.; Malfois, M. [EMBL c/o DESY, Hamburg (Germany); Svergun, D. [Institute of Crystallography, Russian Academy of Sciences, Moscow (Russian Federation); Douka, M. [Commission Europeenne, DG III, Bruxelles (Belgium); Riekel, Ch. [European Synchrotron Radiation Facility (ESRF), 38 - Grenoble (France); Perez, J. [Soleil, 91 - Saclay (France); Roessle, M. [European Molecular Biology Laboratory (EMBL), 38 - Grenoble (France); Amenitsch, H. [IBN/Elettra (Germany); Gunter Grossman, J. [Daresbury Synchrotron Radiation Source (SRS) (United Kingdom); Vestergaard, B. [University of Pharmaceutical Sciences, Copenhagen (Denmark); Receveur-Brechot, V. [Centre National de la Recherche Scientifique (CNRS/AFMB), 13 - Marseille (France); Roth, St.V. [Deutsches Elektronen Synchrotron (HASYLAB), Hamburg (Germany); Ferrari, E. [National Institute for the Physics of Matter (CNR-INFM), Trieste (Italy)

    2007-07-01

    Different issues such as micro-fluidic devices for SAXS (small-angle X-ray diffraction), the use of electro-spray and ion trapping for SAXS in the gas phase, the study of flexible and disordered proteins through SAXS, the time-resolved SAXS studies in solution, or the study of nano-structured soft materials, were addressed in this workshop. This document gathers the transparencies of the presentations.

  17. Dimensional nanometrology with grazing incidence small angle X-ray scattering (GISAXS)

    Energy Technology Data Exchange (ETDEWEB)

    Wernecke, Jan; Krumrey, Michael; Cibik, Levent; Marggraf, Stefanie; Mueller, Peter [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany)

    2011-07-01

    Reliable methods for dimensional characterisation of structures in the nanometer range are now a necessity in many fields of industry and science, e.g. for next-generation EUV lithography, new photovoltaic devices or magnetic nanoparticles. The method we have chosen for measurements of statistically averaged structural properties of nanostructured surfaces is GISAXS. This is a versatile technique to probe statistic properties such as mean particle size, spacial distribution and roughness of nanostructured surfaces and nanoparticle assemblies on top of or buried in bulk material. The GISAXS experiments were performed at the Four-Crystal Monochromator (FCM) beamline in the laboratory of PTB at BESSY II using the SAXS setup of the Helmholtz-Zentrum Berlin (HZB). This presentation will give a short overview of the instrumentation and the capabilities of the laboratory to perform dimensional nanometrology with GISAXS and will show first experimental results. Gratings for EUV lithography have been investigated in terms of coating layer thickness, roughness, grating period and blaze angle. Furthermore, dimensional properties of Au nanoparticles on silicon substrate were determined. The obtained particle sizes were in good agreement with SAXS measurements of these particles in liquid suspension.

  18. Study of pore growth in glassy carbon using small angle x-ray scattering

    International Nuclear Information System (INIS)

    Hoyt, J.

    1982-07-01

    Small-angle x-ray scattering was used to study the average pore size in glass-like carbon as a function of both heat-treatment time and heat-treatment temperature. A pore-growth model based on graphitization processes is presented. The simple mechanism shows that the change in the average radius of gyration with time is related to the total number of pores as a function of time, which in turn depends on the irreversible thermal-expansion phenomenon. The results of this study are inconsistent with a vacancy-migration pore-growth mechanism proposed earlier

  19. GALAXI: Gallium anode low-angle x-ray instrument

    Directory of Open Access Journals (Sweden)

    Emmanuel Kentzinger

    2016-03-01

    Full Text Available The high brilliance laboratory small angle X-ray scattering instrument GALAXI, which is operated by JCNS, Forschungszentrum Jülich, permits the investigation of chemical correlations in bulk materials or of structures deposited on a surface at nanometre and mesoscopic length scales. The instrument is capable to perform GISAXS experiments in reflection at grazing incidence as well as SAXS experiments in transmission geometry. The X-ray flux on sample is comparable or higher than the one obtained at a comparable beamline at a second generation synchrotron radiation source.

  20. An apparatus for high speed measurements of small-angle x-ray scattering profiles with a linear position sensitive detector

    International Nuclear Information System (INIS)

    Hashimoto, Takeji; Suehiro, Shoji; Shibayama, Mitsuhiro; Saijo, Kenji; Kawai, Hiromichi

    1981-01-01

    An apparatus for high speed measurements of small-angle X-ray scattering (SAXS) is described. This apparatus utilizes a 12 kW rotating anode X-ray generator, a linear position sensitive proportional counter (multicathode delay line PSPC), and a two-parameter multichannel pulse height analyzer (MCA) with 12 kwords (16 bits/word) memory area available for SAXA intensity data as a function of position (scattering angles) and time slice. The two-parameter MCA is constructed within a microcomputer system, by utilizing its R/W memory for data storage, and the memory incrementing and real-time CRT display is implemented by using two direct memory access (DMA) controllers. The cycle time of the access is about 10 μs. The measuring time for SAXS profiles with this apparatus can be shortened approximately by three orders of magnitude in comparison with the measuring time with SAXS apparatuses utilizing a conventional step-scanning goniometer and a conventional X-ray tube, thus permitting time-resolved analyses of SAXS profiles. Some applications of the apparatus to dynamic SAXS measurements are presented for polymeric systems, the preliminary results of which seem to indicate the possibility of obtaining a new class of data on dynamics in structural transformation, deformation, formation and annihilation in the scale of a few tens to several hundred Angstroms. (author)

  1. Kinoform optics applied to X-ray photon correlation spectroscopy.

    Science.gov (United States)

    Sandy, A R; Narayanan, S; Sprung, M; Su, J-D; Evans-Lutterodt, K; Isakovic, A F; Stein, A

    2010-05-01

    Moderate-demagnification higher-order silicon kinoform focusing lenses have been fabricated to facilitate small-angle X-ray photon correlation spectroscopy (XPCS) experiments. The geometric properties of such lenses, their focusing performance and their applicability for XPCS measurements are described. It is concluded that one-dimensional vertical X-ray focusing via silicon kinoform lenses significantly increases the usable coherent flux from third-generation storage-ring light sources for small-angle XPCS experiments.

  2. Morphological and structural characterization of PHBV/organoclay nanocomposites by small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Carli, Larissa N., E-mail: lncarli@ucs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, Porto Alegre, 91501-970, RS (Brazil); Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Bianchi, Otavio, E-mail: obianchi@ucs.br [Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Machado, Giovanna, E-mail: giovannamachado@uol.com.br [Centro de Tecnologias Estrategicas do Nordeste, Av. Prof. Luiz Freire, 01, Cidade Universitaria, Recife, 50740-540, PE (Brazil); Programa de Pos-Graduacao de Materiais, Universidade Federal de Pernambuco, Av. Prof. Moraes Rego, 1235, Recife, 50670-901, PE (Brazil); Crespo, Janaina S., E-mail: jscrespo@ucs.br [Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Mauler, Raquel S., E-mail: raquel.mauler@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, Porto Alegre, 91501-970, RS (Brazil)

    2013-03-01

    In this work, the morphological and structural behaviors of poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) nanocomposites were investigated using small angle X-ray scattering (SAXS), wide angle X-ray diffraction (WAXD) and transmission electron microscopy (TEM). The nanocomposites with 1, 3 and 5 wt.% of organically modified montmorillonite Cloisite Registered-Sign 30B (OMMT) were prepared by melt processing in a twin screw extruder using two different processing conditions (low and high shear intensity). The lamellar long period of the polymer was lower for the nanocomposites, with high polydispersity values. However, the crystalline thickness increased with the clay content and was independent of the processing conditions. This behavior resulted in a high linear crystallinity of the nanocomposites with 3 and 5 wt.% OMMT. The disruption factor ({beta}) was in agreement with the WAXD and TEM findings, indicating a good dispersion of the nanoparticles in the PHBV matrix with 3 wt.% of OMMT during the high shear intensity of melt processing. Highlights: Black-Right-Pointing-Pointer SAXS was used for morphological and crystalline studies of PHBV/OMMT nanocomposites. Black-Right-Pointing-Pointer The crystalline structure was influenced by the presence of clay. Black-Right-Pointing-Pointer The degree of clay dispersion in a polymer matrix was quantified. Black-Right-Pointing-Pointer The morphology comprised exfoliated particles, nanoscale and microscale clusters. Black-Right-Pointing-Pointer The results obtained by SAXS agreed well with TEM and WAXD results.

  3. Insights into the interactions among Surfactin, betaines, and PAM: surface tension, small-angle neutron scattering, and small-angle X-ray scattering study.

    Science.gov (United States)

    Xiao, Jingwen; Liu, Fang; Garamus, Vasil M; Almásy, László; Handge, Ulrich A; Willumeit, Regine; Mu, Bozhong; Zou, Aihua

    2014-04-01

    The interactions among neutral polymer polyacrylamide (PAM) and the biosurfactant Surfactin and four betaines, N-dodecyl-N,N-dimethyl-3-ammonio-1-propanesulfonate (SDDAB), N-tetradecyl-N,N-dimethyl-3-ammonio-1-propanesulfonate (STDAB), N-hexadecyl-N,N-dimethyl-3-ammonio-1-propanesulfonate (SHDAB), and N-dodecyl-N,N-dimethyl-2-ammonio-acetate (C12BE), in phosphate buffer solution (PBS) have been studied by surface tension measurements, small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), and rheological experiments. It has been confirmed that the length of alkyl chain is a key parameter of interaction between betaines and PAM. Differences in scattering contrast between X-ray and neutrons for surfactants and PAM molecules provide the opportunity to separately follow the changes of structure of PAM and surfactant aggregates. At concentrations of betaines higher than CMC (critical micelle concentration) and C2 (CMC of surfactant with the presence of polymer), spherical micelles are formed in betaines and betaines/PAM solutions. Transition from spherical to rod-like aggregates (micelles) has been observed in solutions of Surfactin and Surfactin/SDDAB (αSurfactin = 0.67 (molar fraction)) with addition of 0.8 wt % of PAM. The conformation change of PAM molecules only can be observed for Surfactin/SDDAB/PAM system. Viscosity values follow the structural changes suggested from scattering measurements i.e., gradually increases for mixtures PAM → Surfactin/PAM → Surfactin/SDDAB/PAM in PBS.

  4. Rapid small-angle X-ray diffraction of a tonically contracting molluscan smooth muscle recorded with imaging plates

    International Nuclear Information System (INIS)

    Tajima, Y.; Okada, K.; Yoshida, O.; Seto, T.; Amemiya, Y.

    1989-01-01

    Small-angle X-ray diffraction patterns from the anterior byssus retractor muscles of Mytilus edulis contracting tonically in response to stimulation with acetylcholine were recorded in a 30 s exposure with synchrotron radiation and a high-sensitivity X-ray area detector called an imaging plate. The 190 A layer line from the thin filaments increased in intensity with increase in tonic tension up to 6x10 4 kg m -2 . Above this value, the layer-line intensity remained almost constant and comparable to that for a contracting skeletal muscle, indicating that the same structural changes of the thin filaments occur in both muscles. (orig.)

  5. Studies of protein structure in solution and protein folding using synchrotron small-angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Lingling [Stanford Univ., CA (United States)

    1996-04-01

    Synchrotron small angle x-ray scattering (SAXS) has been applied to the structural study of several biological systems, including the nitrogenase complex, the heat shock cognate protein (hsc70), and lysozyme folding. The structural information revealed from the SAXS experiments is complementary to information obtained by other physical and biochemical methods, and adds to our knowledge and understanding of these systems.

  6. Compact structure of ribosomal protein S4 in solution as revealed by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Serdyuk, I.N.; Sarkisyan, M.A.; Gogia, Z.V.

    1981-01-01

    The authors report the results of a small-angle X-ray scattering study of ribosomal protein preparations obtained by neutron scattering method. The theoretical resolution of the diffractometer (Kratky camera, the entrance slit 80 μm, the receiving slit 190 μm, the sample-detector distance 20.4 cm) was the same as the resolution of X-ray diffractometers, on which high rsub(g) values for ribosomal proteins were obtained. They used protein S4 adjusted to 20 mg/ml without any essential loss of solubility. The scattering indicatrix obtained in a wide range of angles has demonstrated that the X-ray rsub(g) obtained here coincides with the earlier obtained neutron rsub(g) and the outer part of the scattering curve is similar to that of slightly elongated compact bodies. They conclude that all discrepancies between their data on the study of ribosomal protein structure in solution and other data are not connected with the characteristics of the instruments used but only with the quality of the protein preparations. (Auth.)

  7. Panoramic Dental X-Ray

    Science.gov (United States)

    ... Physician Resources Professions Site Index A-Z Panoramic Dental X-ray Panoramic dental x-ray uses a very small dose of ... x-ray , is a two-dimensional (2-D) dental x-ray examination that captures the entire mouth ...

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

    Science.gov (United States)

    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.

  9. Grazing incidence small angle X-ray scattering study of silver nanoparticles in ion-exchanged glasses

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Weidong, E-mail: 57399942@qq.com [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); Wu, Zhaojun [Department of Practice Teaching and Equipment Management, Qiqihar University, Qiqihar 161006 (China); Gu, Xiaohua [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); Xing, Xueqing; Mo, Guang [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Wu, Zhonghua, E-mail: wuzh@ihep.ac.cn [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)

    2015-05-15

    The size and distribution of silver nanoparticles in ion-exchanged silicate glass induced by thermal treatments in air at different temperatures were investigated by means of grazing incidence small angle X-ray scattering technique, X-ray diffraction and optical absorption spectra. Silver–sodium ion exchange of soda-lime silicate glasses was done at 350 °C for 240 min, then the samples were treated by thermal annealing in air at different temperatures 400, 500 and 550 °C, respectively, for 1 h. After the annealing treatment above 400 °C for 1 h, smaller Ag nanoparticles occurred, together with bigger ones. Both dissolution of smaller Ag nanoparticles and diffusion of larger ones are discussed in these stages of annealing in this contribution.

  10. Low-angle polarized neutron and X-ray scattering from magnetic nanolayers and nanostructures

    CERN Document Server

    Paul, Amitesh

    2017-01-01

    This research monograph presents the latest results related to the characterization of low dimensional systems. Low-angle polarized neutron scattering and X-ray scattering at grazing incidence are used as the two main techniques to explore various physical phenomena of these systems. Special focus is put on systems like thin film transition metal and rare-earth layers, oxide heterostructures, hybrid systems, self-assembled nanostructures and self-diffusion.  Readers will gain in-depth knowledge about the usage of specular scattering and off-specular scattering techniques. Investigation of in-plane and out-of-plane structures and magnetism with vector magnetometric information is illustrated comprehensively. The book caters to a wide audience working in the field of nano-dimensional magnetic systems and the neutron and X-ray reflectometry community in particular.

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

    Energy Technology Data Exchange (ETDEWEB)

    Settens, Charles M. [State Univ. of New York (SUNY), Albany, NY (United States)

    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 critical 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.

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

    International Nuclear Information System (INIS)

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

    2011-01-01

    The Src-homology 2 (SH2) domain of Csk-family protein tyrosine kinases acts as a conformational switch to regulate their catalytic activity, which in turn promotes the inhibition of their proto-oncogenic targets, the Src-family kinases. Here, the expression, purification, small-angle X-ray scattering and preliminary diffraction analysis of the SH2 domain of the Csk-homologous kinase is reported. 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°

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

    Czech Academy of Sciences Publication Activity Database

    Viani, Alberto; Sotiriadis, Konstantinos; Kumpová, Ivana; Mancini, L.; Appavou, M.-S.

    2017-01-01

    Roč. 33, č. 4 (2017), s. 402-417 ISSN 0109-5641 R&D Projects: GA MŠk(CZ) LO1219 Keywords : zinc phosphate cements * small angle neutron scattering * X-ray micro-computed tomography * X-ray powder diffraction * zinc oxide * acid-base cements Subject RIV: JJ - Other Materials OBOR OECD: Composites (including laminates, reinforced plastics, cermets, combined natural and synthetic fibre fabrics Impact factor: 4.070, year: 2016 https://www.sciencedirect.com/science/article/pii/S0109564116305127

  14. The current status of small-angle x-ray scattering beamline at Diamond Light Source

    International Nuclear Information System (INIS)

    Inoue, Katsuaki; Doutch, James; Terrill, Nick

    2013-01-01

    The small-angle X-ray scattering (SAXS) covers the major disciplines of biology, chemistry and physics delivering structural and dynamic information in nanoscience, mesoscopic architectures, supramolecular structures, and nucleation/growth of crystals. SAXS is also proving to be important in archaeological, environmental, and conservation sciences, and has further indicated its ability to span wide-ranging scientific disciplines. Thus, strong needs for SAXS studies are increasing significantly in a broad range of scientific fields year by year. Based on such a background, the demand for high throughput SAXS experiments is increasing. At the synchrotron facility, Diamond Light Source, one SAXS beamline, Non-crystalline diffraction I22 is now operational and highly automated throughput small-angle X-ray scattering (HATSAXS) beamline B21 is now under construction. I22 is the Undulator beamline and wide varieties of experiments, including time-resolved experiments are attempted. Based on the concept of HATSAXS, the key feature of B21 will focuses on the automation of end-station equipment. A automated sample changer has been purchased for solution SAXS measurements on biomolecules. A robotic-arm-type automated sample changer that is capable of handling several kinds of samples in material science is also being constructed. B21 is expected to successfully provide all users highly automated throughput measurements with the highest possible reliability and accuracy. Construction of this beamline will end in the second half of 2012, and will be open for users in the early summer of 2013 after commissioning. (author)

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

    Science.gov (United States)

    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.

  16. Automated acquisition and analysis of small angle X-ray scattering data

    International Nuclear Information System (INIS)

    Franke, Daniel; Kikhney, Alexey G.; Svergun, Dmitri I.

    2012-01-01

    Small Angle X-ray Scattering (SAXS) is a powerful tool in the study of biological macromolecules providing information about the shape, conformation, assembly and folding states in solution. Recent advances in robotic fluid handling make it possible to perform automated high throughput experiments including fast screening of solution conditions, measurement of structural responses to ligand binding, changes in temperature or chemical modifications. Here, an approach to full automation of SAXS data acquisition and data analysis is presented, which advances automated experiments to the level of a routine tool suitable for large scale structural studies. The approach links automated sample loading, primary data reduction and further processing, facilitating queuing of multiple samples for subsequent measurement and analysis and providing means of remote experiment control. The system was implemented and comprehensively tested in user operation at the BioSAXS beamlines X33 and P12 of EMBL at the DORIS and PETRA storage rings of DESY, Hamburg, respectively, but is also easily applicable to other SAXS stations due to its modular design.

  17. Laser ablation and injection moulding as techniques for producing micro channels compatible with Small Angle X-Ray Scattering

    DEFF Research Database (Denmark)

    Haider, R.; Marmiroli, B.; Gavalas, I.

    2018-01-01

    Microfluidic mixing is an important means for in-situ sample preparation and handling while Small Angle X-Ray Scattering (SAXS) is a proven tool for characterising (macro-)molecular structures. In combination those two techniques enable investigations of fast reactions with high time resolution......, the requirement for low scattering especially limits the techniques suitable for producing the mixer, as the fabrication process can induce molecular orientations and stresses that can adversely influence the scattering signal. Not only is it important to find a production method that results in a device with low...

  18. Development of confocal micro X-ray fluorescence instrument using two X-ray beams

    International Nuclear Information System (INIS)

    Tsuji, Kouichi; Nakano, Kazuhiko; Ding Xunliang

    2007-01-01

    A new confocal micro X-ray fluorescence instrument was developed. This instrument has two independent micro X-ray tubes with Mo targets. A full polycapillary X-ray lens was attached to each X-ray tube. Another half polycapillary lens was attached to a silicon drift X-ray detector (SDD). The focal spots of the three lenses were adjusted to a common position. The effects of the excitation of two X-ray beams were investigated. The instrument enabled highly sensitive three-dimensional X-ray fluorescence analysis. We confirmed that the X-ray fluorescence intensity from the sample increased by applying the two independent X-ray tubes in confocal configuration. Elemental depth profiling of black wheat was demonstrated with the result that each element in the surface coat of a wheat grain showed unique distribution

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

    DEFF Research Database (Denmark)

    Knaapila, M.; Svensson, C.; Barauskas, J.

    2009-01-01

    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...

  20. Time-slicing subsystem of the biology small-angle x-ray scattering station at the National Synchrotron Light Source

    International Nuclear Information System (INIS)

    Stubblefield, F.W.

    1985-11-01

    The time-slicing subsystem of the Biology Small-Angle X-ray Scattering divides the time period during which the data for small-angle x-ray diffraction patterns from biological samples is collected into time slices (or frames). The subsystem, being part of a multiprocessor experiment control and data acquisition system, has its own dedicated processor; it also has special-purpose front-end electronics sufficient to generate the gating and other control signals required to produce a sequence of as many as 256 time slices, measured with a basic time unit of 1 μsec. The electronics also synchronizes with execution of the time slice sequence the application of stimuli to the biological sample, the measurement of voltages generated by the sample, and the application of auxiliary device trigger pulses and routes detector data and auxiliary scaler data into appropriate time-slice-indexed buffers in a large external data memory array. The structure of the entire experiment control and data acquisition system is briefly reviewed. Details of the structure and operation of the time slice subsystem are presented. 7 refs., 5 figs

  1. Identifying low and high density amorphous phases during zeolite amorphisation using small and wide angle X-ray scattering

    International Nuclear Information System (INIS)

    Meneau, F.; Greaves, G.N.

    2005-01-01

    In situ experiments following the thermal amorphisation of zeolites reveal massive increases in small angle X-ray scattering (SAXS), persisting well beyond the stage where wide angle X-ray scattering (WAXS) can detect that any crystalline phase is present. This heterogeneity in the amorphised phase is attributed to the transition from a low density amorphous phase (LDA) to a high density amorphous phase (HDA) at the glass transition. The fractions of zeolite, LDA and HDA phases obtained from SAXS analysis are discussed in the context of non-linear changes detected in 29 Si solid state NMR during zeolite amorphisation. Whilst the HDA phase is chemically disordered, the LDA phase exhibits much of the Al-Si ordering present in the starting zeolite. These findings are considered in the context of perfect glasses predicted to occur when super strong liquids are supercooled

  2. Direct monitoring of calcium-triggered phase transitions in cubosomes using small-angle X-ray scattering combined with microfluidics

    DEFF Research Database (Denmark)

    Ghazal, Aghiad; Gontsarik, Mark; Kutter, Jörg P.

    2016-01-01

    This article introduces a simple microfluidic device that can be combined with synchrotron small-angle X-ray scattering (SAXS) for monitoring dynamic structural transitions. The microfluidic device is a thiol-ene-based system equipped with 125 µm-thick polystyrene windows, which are suitable for ....... The combination of microfluidics with X-ray techniques can be used for investigating protein unfolding, for monitoring the formation of nanoparticles in real time, and for other biomedical and pharmaceutical investigations.......-ray experiments. The device was prepared by soft lithography using elastomeric molds followed by a simple UV-initiated curing step to polymerize the chip material and simultaneously seal the device with the polystyrene windows. The microfluidic device was successfully used to explore the dynamics...

  3. Small angle X-ray scattering and transmission electron microscopy study of the Lactobacillus brevis S-layer protein

    Energy Technology Data Exchange (ETDEWEB)

    Jaeaeskelaeinen, Pentti [Department of Biomedical Engineering and Computational Science, PO Box 2200, FI-02015 Aalto University School of Science and Technology (Finland); Engelhardt, Peter [Haartman Institute, Department of Pathology, PO Box 21, FIN-00014 University of Helsinki (Finland); Hynoenen, Ulla; Palva, Airi [Department of Basic Veterinary Sciences, Division of Microbiology, FIN-00014 University of Helsinki (Finland); Torkkeli, Mika; Serimaa, Ritva, E-mail: ritva.serimaa@helsinki.f [Department of Physics, POB 64, 00014 University of Helsinki (Finland)

    2010-10-01

    The structure of self-assembly domain containing recombinant truncation mutants of Lactobacillus brevis surface layer protein SlpA in aqueous solution was studied using small-angle X-ray scattering and transmission electron microscopy. The proteins were found out to interact with each other forming stable globular oligomers of about 10 monomers. The maximum diameter of the oligomers varied between 75 A and 435 A.

  4. Modeling the structure of RNA molecules with small-angle X-ray scattering data.

    Directory of Open Access Journals (Sweden)

    Michal Jan Gajda

    Full Text Available We propose a novel fragment assembly method for low-resolution modeling of RNA and show how it may be used along with small-angle X-ray solution scattering (SAXS data to model low-resolution structures of particles having as many as 12 independent secondary structure elements. We assessed this model-building procedure by using both artificial data on a previously proposed benchmark and publicly available data. With the artificial data, SAXS-guided models show better similarity to native structures than ROSETTA decoys. The publicly available data showed that SAXS-guided models can be used to reinterpret RNA structures previously deposited in the Protein Data Bank. Our approach allows for fast and efficient building of de novo models of RNA using approximate secondary structures that can be readily obtained from existing bioinformatic approaches. We also offer a rigorous assessment of the resolving power of SAXS in the case of small RNA structures, along with a small multimetric benchmark of the proposed method.

  5. 3-d chemical imaging using angle-scan nanotomography in a soft X-ray scanning transmission X-ray microscope

    Energy Technology Data Exchange (ETDEWEB)

    Hitchcock, A.P.; Johansson, G.A. [McMaster, BIMR, Hamilton (Canada); Mitchell, G.E. [Dow Chemical, Analytical Science, Midland, MI (United States); Keefe, M.H. [Dow Chemical, Dow Latex, Midland, MI (United States); Tyliszcak, T. [LBNL, Advanced Light Source, Berkeley, CA (United States)

    2008-08-15

    Three-dimensional chemical mapping using angle scan nanotomography in a soft X-ray scanning transmission X-ray microscope (STXM) has been used to investigate the spatial distributions of a low density polyacrylate polyelectrolyte ionomer inside submicron sized polystyrene microspheres. Acquisition of tomograms at multiple photon energies provides true, quantifiable 3-d chemical sensitivity. Both pre-O 1s and C 1s results are shown. The study reveals aspects of the 3-d distribution of the polyelectrolyte that were inferred indirectly or had not been known prior to this study. The potential and challenges for extension of the technique to studies of other polymeric and to biological systems is discussed. (orig.)

  6. X-ray small angle scattering of polymer solutions

    International Nuclear Information System (INIS)

    Koyama, Ryuzo

    1975-01-01

    In recent papers, the calculated results were reported on the angular dependence of the intensity of scattered light or X-ray by chain polymers, on the basis of a stiff chain model. As the results, the curves of S 2 P (theta) corresponding to Kratky plot, for different molecular expansion, showed a plateau, and the height of the plateau was proportional to the inverse of molecular expansion coefficient α 2 . But as seen later, there is some possibility that the assumption made in the calculation overestimated the expansion of small segments which theoretically determines scattering curves at large scattering angles, such as the plateau. Accordingly, modified calculation was carried out by adopting the stiff chain polymer model as the previous case. When the contour length of a chain segment is very long, it can be treated approximately as a Gaussian coil, thus the equation for a chain segment expansion coefficient α (t) was obtained. Then the mean square distance of chain segments of polymer molecules was able to be determined, and the equation for a particle scattering factor P(theta) was obtained. The numerical calculation of P(theta) showed that this modified assumption considerably decreased the effect of molecular expansion on P(theta), and the curves of S 2 P(theta) increased monotonously without showing the plateau. The result of this calculation was compared with the experimental curves of polystyrene-toluene solution, and the agreement better than before was obtained. (Kako, I.)

  7. Optimization of the x-ray monitoring angle for creating a correlation model between internal and external respiratory signals

    Energy Technology Data Exchange (ETDEWEB)

    Akimoto, Mami; Nakamura, Mitsuhiro; Mukumoto, Nobutaka; Yamada, Masahiro; Ueki, Nami; Matsuo, Yukinori; Sawada, Akira; Mizowaki, Takashi; Kokubo, Masaki; Hiraoka, Masahiro [Department of Radiation Oncology and Image-applied Therapy, Graduate School of Medicine, Kyoto University, Kyoto 606-8507 (Japan); Department of Radiation Oncology and Image-applied Therapy, Graduate School of Medicine, Kyoto University, Kyoto 606-8507, Japan and Department of Radiological Technology, Faculty of Medical Science, Kyoto College of Medical Science, Nantan, Kyoto 622-0041 (Japan); Department of Radiation Oncology and Image-applied Therapy, Graduate School of Medicine, Kyoto University, Kyoto 606-8507 (Japan); Department of Radiation Oncology, Kobe City Medical Center General Hospital, Kobe, Hyogo 650-0047, Japan and Division of Radiation Oncology, Institute of Biomedical Research and Innovation, Kobe, Hyogo 650-0047 (Japan); Department of Radiation Oncology and Image-applied Therapy, Graduate School of Medicine, Kyoto University, Kyoto 606-8507 (Japan)

    2012-10-15

    Purpose: To perform dynamic tumor tracking irradiation with the Vero4DRT (MHI-TM2000), a correlation model [four dimensional (4D) model] between the displacement of infrared markers on the abdominal wall and the three-dimensional position of a tumor indicated by a minimum of three implanted gold markers is required. However, the gold markers cannot be detected successfully on fluoroscopic images under the following situations: (1) overlapping of the gold markers; and (2) a low intensity ratio of the gold marker to its surroundings. In the present study, the authors proposed a method to readily determine the optimal x-ray monitoring angle for creating a 4D model utilizing computed tomography (CT) images. Methods: The Vero4DRT mounting two orthogonal kV x-ray imaging subsystems can separately rotate the gantry along an O-shaped guide-lane and the O-ring along its vertical axis. The optimal x-ray monitoring angle was determined on CT images by minimizing the root-sum-square of water equivalent path lengths (WEPLs) on the orthogonal lines passing all of the gold markers while rotating the O-ring and the gantry. The x-ray monitoring angles at which the distances between the gold markers were within 5 mm at the isocenter level were excluded to prevent false detection of the gold markers in consideration of respiratory motions. First, the relationship between the WEPLs (unit: mm) and the intensity ratios of the gold markers was examined to assess the validity of our proposed method. Second, our proposed method was applied to the 4D-CT images at the end-expiration phase for 11 lung cancer patients who had four to five gold markers. To prove the necessity of the x-ray monitoring angle optimization, the intensity ratios of the least visible markers (minimum intensity ratios) that were estimated from the WEPLs were compared under the following conditions: the optimal x-ray monitoring angle and the angles used for setup verification. Additionally, the intra- and

  8. Two-dimensional in situ metrology of X-ray mirrors using the speckle scanning technique

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal [Diamond Light Source Ltd, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom)

    2015-06-06

    The two-dimensional slope error of an X-ray mirror has been retrieved by employing the speckle scanning technique, which will be valuable at synchrotron radiation facilities and in astronomical telescopes. In situ metrology overcomes many of the limitations of existing metrology techniques and is capable of exceeding the performance of present-day optics. A novel technique for precisely characterizing an X-ray bimorph mirror and deducing its two-dimensional (2D) slope error map is presented. This technique has also been used to perform fast optimization of a bimorph mirror using the derived 2D piezo response functions. The measured focused beam size was significantly reduced after the optimization, and the slope error map was then verified by using geometrical optics to simulate the focused beam profile. This proposed technique is expected to be valuable for in situ metrology of X-ray mirrors at synchrotron radiation facilities and in astronomical telescopes.

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

    Directory of Open Access Journals (Sweden)

    Lauren Boldon

    2015-02-01

    Full Text Available 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.

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

    Science.gov (United States)

    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.

  11. Measurements of accurate x-ray scattering data of protein solutions using small stationary sample cells

    Science.gov (United States)

    Hong, Xinguo; Hao, Quan

    2009-01-01

    In this paper, we report a method of precise in situ x-ray scattering measurements on protein solutions using small stationary sample cells. Although reduction in the radiation damage induced by intense synchrotron radiation sources is indispensable for the correct interpretation of scattering data, there is still a lack of effective methods to overcome radiation-induced aggregation and extract scattering profiles free from chemical or structural damage. It is found that radiation-induced aggregation mainly begins on the surface of the sample cell and grows along the beam path; the diameter of the damaged region is comparable to the x-ray beam size. Radiation-induced aggregation can be effectively avoided by using a two-dimensional scan (2D mode), with an interval as small as 1.5 times the beam size, at low temperature (e.g., 4 °C). A radiation sensitive protein, bovine hemoglobin, was used to test the method. A standard deviation of less than 5% in the small angle region was observed from a series of nine spectra recorded in 2D mode, in contrast to the intensity variation seen using the conventional stationary technique, which can exceed 100%. Wide-angle x-ray scattering data were collected at a standard macromolecular diffraction station using the same data collection protocol and showed a good signal/noise ratio (better than the reported data on the same protein using a flow cell). The results indicate that this method is an effective approach for obtaining precise measurements of protein solution scattering.

  12. Measurements of accurate x-ray scattering data of protein solutions using small stationary sample cells

    International Nuclear Information System (INIS)

    Hong Xinguo; Hao Quan

    2009-01-01

    In this paper, we report a method of precise in situ x-ray scattering measurements on protein solutions using small stationary sample cells. Although reduction in the radiation damage induced by intense synchrotron radiation sources is indispensable for the correct interpretation of scattering data, there is still a lack of effective methods to overcome radiation-induced aggregation and extract scattering profiles free from chemical or structural damage. It is found that radiation-induced aggregation mainly begins on the surface of the sample cell and grows along the beam path; the diameter of the damaged region is comparable to the x-ray beam size. Radiation-induced aggregation can be effectively avoided by using a two-dimensional scan (2D mode), with an interval as small as 1.5 times the beam size, at low temperature (e.g., 4 deg. C). A radiation sensitive protein, bovine hemoglobin, was used to test the method. A standard deviation of less than 5% in the small angle region was observed from a series of nine spectra recorded in 2D mode, in contrast to the intensity variation seen using the conventional stationary technique, which can exceed 100%. Wide-angle x-ray scattering data were collected at a standard macromolecular diffraction station using the same data collection protocol and showed a good signal/noise ratio (better than the reported data on the same protein using a flow cell). The results indicate that this method is an effective approach for obtaining precise measurements of protein solution scattering.

  13. Analysis of the aggregation structure from amphiphilic block copolymers in solutions by small-angle x-ray scattering

    CERN Document Server

    Rong Li Xia; Wang Jun; Wei Liu He; Li Fu Mian; Li Zi Chen

    2002-01-01

    The aggregation structure of polystyrene-p vinyl benzoic amphiphilic block copolymers which were prepared in different conditions was investigated by synchrotron radiation small-angle x-ray scattering (SAXS). The micelle was self-assembled in selective solvents of the block copolymers. Authors' results demonstrate that the structure of the micelle depends on the factors, such as the composition of the copolymers, the nature of the solvent and the concentration of the solution

  14. Tertiary and quaternary structural differences between two genetic variants of bovine casein by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Pessen, H.; Kumosinski, T.F.; Farrell, H.M. Jr.; Brumberger, H.

    1991-01-01

    The casein complexes of bovine milk consist of four major protein fractions, alpha s1, alpha s2, beta, and kappa. Colloidal particles of casein (termed micelles) contain inorganic calcium and phosphate; they are very roughly spherical with an average radius of 650 A. Removal of Ca2+ leads to the formation of smaller protein aggregates with an average radius of 94 A. Two genetic variants, A and B, of the predominant fraction, alpha s1-casein, result in milks with markedly different physical properties, such as solubility and heat stability. To investigate the molecular basis for these differences, small-angle X-ray scattering was performed on the respective colloidal micelles and submicelles. Scattering curves for submicelles of both variants showed multiple Gaussian character; data for the B variant were previously interpreted in terms of two concentric regions of different electron density, i.e., a compact core and a relatively loose shell. For the submicelle of A, there was a third Gaussian, reflecting a negative contribution due to interparticle interference. Molecular parameters for submicelles of both A and B are in agreement with hydrodynamic data in the literature. Data for the micelles, for which scattering yields cross-sectional information, were fitted by a sum of three Gaussians for both variants; for these, the corresponding two lower radii of gyration represent the two concentric regions of the submicelles, while the third reflects the average packing of submicelles within the micellar cross section. Most of the molecular parameters obtained showed small but consistent differences between A and B, but for submicelles within the micelle several differences were particularly notable: A has a greater molecular weight for the compact region of the constituent submicelle (82,000 vs 60,000) and a much greater submicellar packing number

  15. Scanning small angle X-ray scattering investigations of bone

    International Nuclear Information System (INIS)

    Rinnerthaler, S.

    1998-06-01

    An important characteristic of bone is its strength, which is determined by bone mass, architecture and material quality. From a physical point of view bone is a composite material consisting of an organic matrix (collagen) and of inlets of mineral crystals (hydroxyapatite). These components build up a hierarchical, heterogeneous structure. The size of the mineral crystals lies in the nano-meter range and can be investigated by positionsensitive Small-Angle X-ray Scattering (Scanning-SAXS) in a non-destructive way. The average thickness, the degree and direction of the predominant orientation, as well as some information about shape and arrangement of the mineral crystals were determined in bones of humans, mice, and baboons by Scanning-SAXS with respect to age, bone diseases (osteogenesis imperfecta, pycnodysostosis) or medical treatments (fluoride or alendronate) of osteoporosis. The crystal thickness and the degree of orientation is much smaller in young individuals than in adults and the predominant orientation of the mineral crystals is different in a mixture of bone and mineralized cartilage compared to bone. Further, because position-resolved measurements are now possible, results from Scanning-SAXS measurements could be compared with the results of other position resolved methods. Due to this new feature it was possible, for the first time, to correlate directly 'mottled' bone visible in back-scattered electron imaging with small η-parameters evaluated from SAXS-patterns and the course of the collagen fibers with the predominant orientation of the mineral crystals. Scanning-SAXS proved to be a powerful tool to characterize bone nano-structure. (author)

  16. X-ray small-angle scattering of polytetrahydrofuran solution, 3

    International Nuclear Information System (INIS)

    Izumi, Yoshinobu; Fuji, Masayuki; Shinbo, Kazuyuki; Miyake, Yasuhiro

    1975-01-01

    In a previous report, the conformation of polytetrahydrofuran (PTHF) in isopropyl alcohol as a theta solvent and in n-butyl alcohol as an intermediate solvent was examined by the small angle scattering of X-ray. As the result, the experimental scattering curve at theta temperature was explained well with the calculated curve obtained by superposing, while it was impossible to apply the similar method to the analysis of the scattering curve in the intermediate solvent. Recently, as the results of the calculation by Koyama on the angular distribution of light intensity scattered by stiff chain polymers and of the studies by Edwards and de Gennes on the asymptotic behavior of scattering curves in good solvents, the direct comparison of experimental and calculated scattering curves became possible. In this report, the comparison of the scattering curves of PTHF-alcohol systems is described. The systems employed were PTHF-n-propyl alcohol, PTHF-isobutyl alcohol, PTHF-sec-butyl alcohol, and PTHF-tert-butyl alcohol in addition to the previous two systems. The Guinier plots of the cross section factors of the PTHF-alcohol systems showed that the Guinier approximation on cross sections was not satisfied in cases of PTHF-isobutyl alcohol and PTHF-sec-butyl alcohol. The light scattering data at 44.6 0 C, the theta temperature of PTHF-isopropyl alcohol, are given. From the figures comparing experimental and calculated scattering curves, it was shown that there was appreciable solvent effect on the scattering curves of PTHF-alcohol systems. The relation predicted by Edwards and de Gennes was satisfied well in case of the systems in good solvents. (Kako, I.)

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Hura, Greg L.; Menon, Angeli L.; Hammel, Michal; Rambo, Robert P.; Poole II, Farris L.; Tsutakawa, Susan E.; Jenney Jr, Francis E.; Classen, Scott; Frankel, Kenneth A.; Hopkins, Robert C.; Yang, Sungjae; Scott, Joseph W.; Dillard, Bret D.; Adams, Michael W. W.; Tainer, John A.

    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 for 41 proteins. We believe that high-throughput SAXS is an enabling technology that may change the way that structural genomics research is done.

  19. Small angle x-ray studies reveal that Aspergillus niger glucoamylase has a defined extended conformation and can form dimers in solution

    DEFF Research Database (Denmark)

    Jørgensen, Anders Dysted; Nøhr, Jane; Kastrup, Jette Sandholm

    2008-01-01

    is poorly understood and structurally undescribed, and data regarding domain organization and intramolecular functional cooperativity are conflicting or non-comprehensive. Here, we report a combined small angle x-ray scattering and calorimetry study of Aspergillus niger glucoamylase 1, glucoamylase 2, which...

  20. Topological investigation of electronic silicon nanoparticulate aggregates using ultra-small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Jonah, E. O.; Britton, D. T.; Beaucage, P.; Rai, D. K.; Beaucage, G.; Magunje, B.; Ilavsky, J.; Scriba, M. R.; Härting, M.

    2012-01-01

    The network topology of two types of silicon nanoparticles, produced by high energy milling and pyrolysis of silane, in layers deposited from inks on permeable and impermeable substrates has been quantitatively characterized using ultra-small-angle X-ray scattering, supported by scanning electron microscopy observations. The milled particles with a highly polydisperse size distribution form agglomerates, which in turn cluster to form larger aggregates with a very high degree of aggregation. Smaller nanoparticles with less polydisperse size distribution synthesized by thermal catalytic pyrolysis of silane form small open clusters. The Sauter mean diameters of the primary particles of the two types of nanoparticles were obtained from USAXS particle volume to surface ratio, with values of ∼41 and ∼21 nm obtained for the high energy milled and pyrolysis samples, respectively. Assuming a log-normal distribution of the particles, the geometric standard deviation of the particles was calculated to be ∼1.48 for all the samples, using parameters derived from the unified fit to the USAXS data. The flow properties of the inks and substrate combination lead to quantitative changes in the mean particle separation, with slowly curing systems with good capillary flow resulting in denser networks with smaller aggregates and better contact between particles.

  1. Determination of the thermodynamic state of concentrated hemoglobin solutions by means of small angle X-ray scattering

    International Nuclear Information System (INIS)

    Zinke, M.

    1979-01-01

    Exemplified by hemoglobin, the thermodynamic equilibrium properties of the dissolved macromolecular system could be determined solely from the small angle X-ray scattering of concentrated macromolecular solutions via the intermolecular structure of the dissolved macromolecules and their intermolecular potentials. From the scattering experiment on concentrated Hb solutions the concentration dependence of the following properties of the dissolved Hb system were determined: fluctuation, isothermic compressibility, internal energy, surface tension, and osmotic pressure. (author)

  2. Crystallization behavior of polyethylene on silicon wafers in solution casting processes traced by time-resolved measurements of synchrotron grazing-incidence small-angle and wide-angle X-ray scattering

    International Nuclear Information System (INIS)

    Sasaki, S; Masunaga, H; Takata, M; Itou, K; Tashiro, K; Okuda, H; Takahara, A

    2009-01-01

    Crystallization behavior of polyethylene (PE) on silicon wafers in solution casting processes has been successfully traced by time-resolved grazing-incidence small-angle and wide-angle X-ray scattering (GISWAXS) measurements utilizing synchrotron radiation. A p-xylene solution of PE kept at ca. 343 K was dropped on a silicon wafer at ca. 298 K. While the p-xylene evaporated naturally from the dropped solution sample, PE chains crystallized to be a thin film. Raman spectral measurements were performed simultaneously with the GISWAXS measurements to evaluate quantitatively the p-xylene the dropped solution contained. Grazing-incidence wide-angle X-ray scattering (GIWAXS) patterns indicated nucleation and crystal growth in the dropped solution and the following as-cast film. GIWAXS and Raman spectral data revealed that crystallization of PE was enhanced after complete evaporation of the p-xylene from the dropped solution. The [110] and [200] directions of the orthorhombic PE crystal became relatively parallel to the wafer surface with time, which implied that the flat-on lamellae with respect to the wafer surface were mainly formed in the as-cast film. On the other hand, grazing-incidence small-angle X-ray scattering (GISAXS) patterns implied formation of isolated lamellae in the dropped solution. The lamellae and amorphous might alternatively be stacked in the preferred direction perpendicular to the wafer surface. The synchrotron GISWAXS experimental method could be applied for kinetic study on hierarchical structure of polymer thin films.

  3. Watching Nanoparticles Form: An In Situ (Small-/Wide-Angle X-ray Scattering/Total Scattering) Study of the Growth of Yttria-Stabilised Zirconia in Supercritical Fluids

    DEFF Research Database (Denmark)

    Tyrsted, Christoffer; Pauw, Brian; Jensen, Kirsten Marie Ørnsbjerg

    2012-01-01

    Understanding nanoparticle formation reactions requires multitechnique in situ characterisation, since no single characterisation technique provides adequate information. Here, the first combined small-angle X-ray scattering (SAXS)/wide-angle X-ray scattering (WAXS)/total-scattering study of nano...... of nanoparticle formation is presented. We report on the formation and growth of yttria-stabilised zirconia (YSZ) under the extreme conditions of supercritical methanol for particles with Y2O3 equivalent molar fractions of 0, 4, 8, 12 and 25%....

  4. X-ray studies on a two-dimensional diffusion limited system for cell growth

    International Nuclear Information System (INIS)

    Hlatky, L.R.; Alpen, E.L.

    1985-01-01

    X-ray studies were performed on cells grown in a new type of in vitro multicellular system, the ''sandwich'' system. This system is a two-dimensional array of cells, sandwiched between transparent slides which are impermeable to oxygen. The cell system is subject to self-created diffusion gradients of nutrients, metabolic products and, most importantly, oxygen. Sandwiches are analogous to living cross sections of multicellular spheroids or of poorly vascularized tumors. They contain a necrotic center, which the authors show to be due to diffusion limitations, an intermediate region which has a large fraction of quiescent cells and a cycling outer rim. One advantage sandwiches have over three-dimensional tumor models (sheproids) is that can control the amount of cell to cell contact and thereby separate effects due to oxygen or other gradients from effects due to contact. The authors present x-ray survival curves for sandwiches of various cell densities and compare them to x-ray survival curves done for spheroids and monolayers of the same cell line

  5. Small angle x-ray scattering as a potential tool for cancer diagnosis

    International Nuclear Information System (INIS)

    Kitchen, M.; Siu, K.K.W.; Lewis, R.A.

    2003-01-01

    Full text: The diagnostic potential of Small Angle X-ray Scattering (SAXS) patterns has recently been investigated for malignant breast tissues. The demonstrated systematic differences in the scattering signatures of malignant, benign and normal breast tissue specimens are believed to arise from the changes in the fibrous proteins making up the extracellular matrix (ECM) with the disease progression. The technique may also have the potential to aid in the diagnosis of gliomas, a highly aggressive type of brain tumour. Although complex and difficult to interpret, SAXS data from malignant tissues may prove to be a more effective classification tool than conventional histology techniques. Here we present the methodology of the technique, as applied to breast cancer and brain tumour specimens to date, and some directions for future investigations. We also present a novel analysis method, which employs wavelet decomposition and a naive Bayesian classifier, as a potential semi-automated classification tool

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

    OpenAIRE

    Grudinin , Sergei; Garkavenko , Maria; Kazennov , Andrei

    2017-01-01

    International audience; 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 ord...

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

    Science.gov (United States)

    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.

  8. Penetration route of functional molecules in stratum corneum studied by time-resolved small- and wide-angle x-ray diffraction

    International Nuclear Information System (INIS)

    Hatta, Ichiro; Ohta, Noboru; Yagi, Naoto; Nakazawa, Hiromitsu; Obata, Yasuko; Inoue, Katsuaki

    2011-01-01

    We studied effects of functional molecules on corneocytes in stratum corneum using time-resolved small- and wide-angle x-ray diffraction after applying a functional molecule. From these results it was revealed that in the stratum corneum a typical hydrophilic molecule, ethanol, penetrates via the transcellular route and on the other hand a typical hydrophobic molecule, d-limonene, penetrates via the intercellular route.

  9. A new method for information retrieval in two-dimensional grating-based X-ray phase contrast imaging

    International Nuclear Information System (INIS)

    Wang Zhi-Li; Gao Kun; Chen Jian; Ge Xin; Tian Yang-Chao; Wu Zi-Yu; Zhu Pei-Ping

    2012-01-01

    Grating-based X-ray phase contrast imaging has been demonstrated to be an extremely powerful phase-sensitive imaging technique. By using two-dimensional (2D) gratings, the observable contrast is extended to two refraction directions. Recently, we have developed a novel reverse-projection (RP) method, which is capable of retrieving the object information efficiently with one-dimensional (1D) grating-based phase contrast imaging. In this contribution, we present its extension to the 2D grating-based X-ray phase contrast imaging, named the two-dimensional reverse-projection (2D-RP) method, for information retrieval. The method takes into account the nonlinear contributions of two refraction directions and allows the retrieval of the absorption, the horizontal and the vertical refraction images. The obtained information can be used for the reconstruction of the three-dimensional phase gradient field, and for an improved phase map retrieval and reconstruction. Numerical experiments are carried out, and the results confirm the validity of the 2D-RP method

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

    Science.gov (United States)

    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.

  11. Combined in situ small and wide angle X-ray scattering studies of TiO2 nano-particle annealing to 1023 K

    DEFF Research Database (Denmark)

    Kehres, Jan; Andreasen, Jens Wenzel; Krebs, Frederik C

    2010-01-01

    Combined in situ small- and wide-angle X-ray scattering (SAXS/WAXS) studies were performed in a recently developed laboratory setup to investigate the dynamical properties of dry oleic acid-capped titanium dioxide nanorods during annealing in an inert gas stream in a temperature interval of 298-1...

  12. Synchrotron small-angle x-ray scattering investigation on integral membrane protein light-harvesting complex LH2 from photosynthetic bacterium rhodopseudomonas acidophila

    International Nuclear Information System (INIS)

    Du Luchao; Weng Yuxiang; Hong Xinguo; Xian Dingchang; Kobayashi Katsumi

    2006-01-01

    Structures of membrane protein in solution are different from that in crystal phase. We present the primary results of small angle x-ray scattering (SAXS) resolved topological structures of a light harvesting antenna membrane protein complex LH2 from photosynthetic bacteria Rhodopseudomonas acidophila in detergent solution for the first time. Our results show that the elliptical shape of the LH2 complex in solution clearly deviates from its circular structure in crystal phase determined by x-ray diffraction. This result provides an insight into the structure and function interplay in LH2. (authors)

  13. Angle dependent focal spot size of a conical X-ray target

    International Nuclear Information System (INIS)

    Saeed Raza, Hamid; Jin Kim, Hyun; Nam Kim, Hyun; Oh Cho, Sung

    2015-01-01

    Misaligned phantoms may severely affect the focal spot calculations. A method is proposed to determine the geometry of the X-ray target and the position of the image radiograph around the X-ray target to get a relatively smaller focal spot size. Results reveal that the focal spot size is not always isotropic around the target but it decreases as the point of observation shifts radially away from the center line of the conical X-ray target. This research will help in producing high quality X-ray images in multi-directions by properly aligning the phantoms and the radiograph tallies. - Highlights: • Misaligned phantoms may severely affect the focal spot calculations. • The aim of this research is to analyze systematically the angle dependent behavior of the focal spot size around a conical shaped X-ray target. • A general purpose Monte Carlo (MCNP5) computer code is used to achieve a relatively small focal spot size. • Angular distribution of the X-ray focal spot size mainly depends on the angular orientation of the phantom and its aligned FIR tally. • This research will help in producing high quality X-ray images in multi-directions

  14. Proteins on surfaces investigated by microbeam grazing incidence small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Gebhardt, Ronald; Riekel, Christian; Burghammer, Manfred [European Synchrotron Radiation Facility, B.P. 220, F-38043 Grenoble Cedex (France); Vendrely, Charlotte [Universite de Cergy-Pontoise, ERRMECE, F-95000, Cergy-Pontoise (France); Mueller-Buschbaum, Peter [TU Muenchen, Physik Department E13, Muenchen (Germany)

    2009-07-01

    Grazing incidence small angle scattering with a 1 micron x-ray beam ({mu}GISAXS) is applied to study structural ordering of casein micelles and fibroin in solution cast films. {mu}GISAXS scans provide the possibility to locate highly ordered areas and to investigate variation in the molecular packing. In the case of the casein micelles, ordered film structures have been generated by decreasing their natural size dispersion. While dynamic light scattering was used to characterize the different size fractions in solution, {mu}GISAXS and roughness are measured on the resulting casein films. GISAXS-Patterns are analyzed by simulations providing the dimension and nearest neighbor distances of casein micelles. In the case of fibroin, ordering of nano-fibers formed during the drying process is investigated. The experimental data are analyzed by simulations and compared to SEM, AFM and Raman scattering experiments.

  15. A new package: MySAS for small angle scattering data analysis

    International Nuclear Information System (INIS)

    Huang Chaoqiang; Xia Qingzhong; Yan Guanyun; Sun Guang'ai; Chen Bo

    2010-01-01

    In this paper, A MySAS package, which is verified on Windows XP, can easily convert two-dimensional data in small angle neutron and X-ray scattering analysis, operate individually and execute one particular operation as numerical data reduction or analysis, and graphical visualization. This MySAS package can implement the input and output routines via scanning certain properties, thus recalling completely sets of repetition input and selecting the input files. On starting from the two-dimensional files, the MySAS package can correct the anisotropic or isotropic data for physical interpretation and select the relevant pixels. Over 50 model functions are fitted by the POWELL code using χ 2 as the figure of merit function. (authors)

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

    International Nuclear Information System (INIS)

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

    2017-01-01

    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 effort 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.

  17. Quantification of RNA in bacteriophage MS2-like viruses in solution by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Kuzmanovic, Deborah A.; Elashvili, Ilya; Wick, Charles; O'Connell, Catherine; Krueger, Susan

    2006-01-01

    Recombinant forms of bacteriophage MS2 virus particles, wild-type MS2 and MS2 capsids have been examined in solution using small-angle X-ray scattering (SAXS). SAXS was used to determine the overall size of the virus particles and to quantify the amount of encapsulated viral RNA. These studies show that analysis of natural and recombinant forms of MS2 virus by SAXS can be used as both a quantitative measure of nucleic acid content in situ and diagnostic indicator of sample integrity

  18. Particle-scale structure in frozen colloidal suspensions from small-angle x-ray scattering

    KAUST Repository

    Spannuth, Melissa

    2011-02-01

    During directional solidification of the solvent in a colloidal suspension, the colloidal particles segregate from the growing solid, forming high-particle-density regions with structure on a hierarchy of length scales ranging from that of the particle-scale packing to the large-scale spacing between these regions. Previous work has concentrated mostly on the medium- to large-length scale structure, as it is the most accessible and thought to be more technologically relevant. However, the packing of the colloids at the particle scale is an important component not only in theoretical descriptions of the segregation process, but also to the utility of freeze-cast materials for new applications. Here we present the results of experiments in which we investigated this structure across a wide range of length scales using a combination of small-angle x-ray scattering and direct optical imaging. As expected, during freezing the particles were concentrated into regions between ice dendrites forming a microscopic pattern of high- and low-particle-density regions. X-ray scattering indicates that the particles in the high-density regions were so closely packed as to be touching. However, the arrangement of the particles does not conform to that predicted by standard interparticle pair potentials, suggesting that the particle packing induced by freezing differs from that formed during equilibrium densification processes. © 2011 American Physical Society.

  19. Particle-scale structure in frozen colloidal suspensions from small-angle x-ray scattering

    KAUST Repository

    Spannuth, Melissa; Mochrie, S. G. J.; Peppin, S. S. L.; Wettlaufer, J. S.

    2011-01-01

    During directional solidification of the solvent in a colloidal suspension, the colloidal particles segregate from the growing solid, forming high-particle-density regions with structure on a hierarchy of length scales ranging from that of the particle-scale packing to the large-scale spacing between these regions. Previous work has concentrated mostly on the medium- to large-length scale structure, as it is the most accessible and thought to be more technologically relevant. However, the packing of the colloids at the particle scale is an important component not only in theoretical descriptions of the segregation process, but also to the utility of freeze-cast materials for new applications. Here we present the results of experiments in which we investigated this structure across a wide range of length scales using a combination of small-angle x-ray scattering and direct optical imaging. As expected, during freezing the particles were concentrated into regions between ice dendrites forming a microscopic pattern of high- and low-particle-density regions. X-ray scattering indicates that the particles in the high-density regions were so closely packed as to be touching. However, the arrangement of the particles does not conform to that predicted by standard interparticle pair potentials, suggesting that the particle packing induced by freezing differs from that formed during equilibrium densification processes. © 2011 American Physical Society.

  20. Characterization of Nanocellulose Using Small-Angle Neutron, X-ray, and Dynamic Light Scattering Techniques.

    Science.gov (United States)

    Mao, Yimin; Liu, Kai; Zhan, Chengbo; Geng, Lihong; Chu, Benjamin; Hsiao, Benjamin S

    2017-02-16

    Nanocellulose extracted from wood pulps using TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl radical)-mediated oxidation and sulfuric acid hydrolysis methods was characterized by small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), and dynamic light scattering (DLS) techniques. The dimensions of this nanocellulose (TEMPO-oxidized cellulose nanofiber (TOCN) and sulfuric acid hydrolyzed cellulose nanocrystal (SACN)) revealed by the different scattering methods were compared with those characterized by transmission electron microscopy (TEM). The SANS and SAXS data were analyzed using a parallelepiped-based form factor. The width and thickness of the nanocellulose cross section were ∼8 and ∼2 nm for TOCN and ∼20 and ∼3 nm for SACN, respectively, where the fitting results from SANS and SAXS profiles were consistent with each other. DLS was carried out under both the V V mode with the polarizer and analyzer parallel to each other and the H V mode having them perpendicular to each other. Using rotational and translational diffusion coefficients obtained under the H V mode yielded a nanocellulose length qualitatively consistent with that observed by TEM, whereas the length derived by the translational diffusion coefficient under the V V mode appeared to be overestimated.

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

    Energy Technology Data Exchange (ETDEWEB)

    Dhatwalia, Richa; Singh, Harkewal; Oppenheimer, Michelle; Karr, Dale B.; Nix, Jay C.; Sobrado, Pablo; Tanner, John J. (LBNL); (Missouri); (VPI)

    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 has 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.

  2. Probabilistic Evaluation of Three-Dimensional Reconstructions from X-Ray Images Spanning a Limited Angle

    Directory of Open Access Journals (Sweden)

    Jörn Ostermann

    2012-12-01

    Full Text Available An important part of computed tomography is the calculation of a three-dimensional reconstruction of an object from series of X-ray images. Unfortunately, some applications do not provide sufficient X-ray images. Then, the reconstructed objects no longer truly represent the original. Inside of the volumes, the accuracy seems to vary unpredictably. In this paper, we introduce a novel method to evaluate any reconstruction, voxel by voxel. The evaluation is based on a sophisticated probabilistic handling of the measured X-rays, as well as the inclusion of a priori knowledge about the materials that the object receiving the X-ray examination consists of. For each voxel, the proposed method outputs a numerical value that represents the probability of existence of a predefined material at the position of the voxel while doing X-ray. Such a probabilistic quality measure was lacking so far. In our experiment, false reconstructed areas get detected by their low probability. In exact reconstructed areas, a high probability predominates. Receiver Operating Characteristics not only confirm the reliability of our quality measure but also demonstrate that existing methods are less suitable for evaluating a reconstruction.

  3. Study on the structure of Fe sub 2 O sub 3 xerogels by small angle X-ray scattering

    CERN Document Server

    Liu Yi; Zhao Xin; Yang Tong Hua; Zhao Hui; Rong Li Xia; Zhang Jing; Wang Jun; Dong Bao Zhong

    2002-01-01

    Small angle X-ray scattering (SAXS) with synchrotron radiation as X-ray source is used to study the pore structure of Fe sub 2 O sub 3 xerogels prepared by sol-gel procedure and then heat-treated at different temperatures. By analysing the distribution of diameters of the pores, specific surfaces and fractal behaviors in samples, the characters and mechanisms of pores growing are discussed. The results show that the pores in Fe sub 2 O sub 3 xerogels are polydisperse and the structure of the pores is mass fractal. With increase in heat-treatment temperature, the average size of diameters of the pores and the dimension of fractal of Fe sub 2 O sub 3 xerogels are increased, whereas the scale range possessing fractal behavior become narrow

  4. Formation process of hierarchical structures in crystalline polymers as analyzed by simultaneous measurements of small-angle X-ray scattering and other techniques

    International Nuclear Information System (INIS)

    Yamamoto, Katsuhiro; Sakurai, Shinichi

    2006-01-01

    Crystalline polymers spontaneously form hierarchical structures, which provide us a potential use as a specialty material. Recently, not only a crystalline homopolymer but also semi-crystalline block copolymers and crystalline polymer blends have been attracting interests for the study of a hierarchical structure. In order to analyze such hierarchical structures in a variety of length scales, a simultaneous measurement of small-(SAXS) and wide-angle (WAXS) X-ray scattering with differential scanning calorimetry (DSC), or with small-angle light scattering (Hv-SALS) are most suitable. In this review, we show some examples of the simultaneous measurements. With DSC, exothermic heat flow can be simultaneously measured with X-ray scattering. On the other hand, with Hv-SALS it is possible to analyze evolution of a spherulitic structure, which is the structure at the highest rank in the hierarchy. For both cases, one can realize that it is impossible to obtain good statistics for SAXS and WAXS measurements without synchrotron radiations. (author)

  5. Corrections of residual fluorescence distortions for a glancing-emergence-angle x-ray-absorption technique

    International Nuclear Information System (INIS)

    Brewe, D.L.; Pease, D.M.; Budnick, J.I.

    1994-01-01

    Distortions appear in x-ray-absorption spectra obtained by monitoring the fluorescence from thick samples with concentrated absorbing species. The glancing-emergence-angle technique for obtaining spectra from this type of sample eliminates distortions from the measured spectra by monitoring the fluorescence leaving the sample at a small angle relative to the sample surface. This technique is limited by the small signal available from the inherently limited detector solid angle. In addition, no precise estimate of the required restriction on maximum emergent angle θ max has been available. We have calculated residual extended x-ray-absorption fine structure distortions as a function of θ max , and performed experimental tests of the calculations. These calculations provide a means to estimate the required detector geometry for negligible distortions, or alternatively, allow the use of a larger θ max , increasing the available signal, with the remaining residual distortions removed by application of the calculations. The calculations are also applicable to other detector geometries, and account for detectors subtending a large solid angle by an integration over the subtended angle. This represents an improvement over previous calculations. The application to more general detector configurations is also discussed

  6. A survey on coordinate metrology using dimensional X-ray CT

    International Nuclear Information System (INIS)

    Matsuzaki, Kazuya

    2016-01-01

    X-ray computed tomography (X-ray CT) has been occupying indispensable position in geometrical and dimensional measurements in industry, which is capable of measuring both external and internal dimensions of industrial products. Since dimensional X-ray CT has problems about ensuring traceability and estimating uncertainty, requirement of developing measurement standard for dimensional X-ray CT is increasing. Some of national metrology institutes (NMIs) including NMIJ have been working on developing measurement standard. In this report, the background of coordinate metrology using dimensional X-ray CT is reviewed. Then, measurement error sources are discussed. Finally, the plan to develop high accuracy dimensional X-ray CT is presented. (author)

  7. Conformational Flexibility of Proteins Involved in Ribosome Biogenesis: Investigations via Small Angle X-ray Scattering (SAXS

    Directory of Open Access Journals (Sweden)

    Dritan Siliqi

    2018-02-01

    Full Text Available The dynamism of proteins is central to their function, and several proteins have been described as flexible, as consisting of multiple domains joined by flexible linkers, and even as intrinsically disordered. Several techniques exist to study protein structures, but small angle X-ray scattering (SAXS has proven to be particularly powerful for the quantitative analysis of such flexible systems. In the present report, we have used SAXS in combination with X-ray crystallography to highlight their usefulness at characterizing flexible proteins, using as examples two proteins involved in different steps of ribosome biogenesis. The yeast BRCA2 and CDKN1A-interactig protein, Bcp1, is a chaperone for Rpl23 of unknown structure. We showed that it consists of a rigid, slightly elongated protein, with a secondary structure comprising a mixture of alpha helices and beta sheets. As an example of a flexible molecule, we studied the SBDS (Shwachman-Bodian-Diamond Syndrome protein that is involved in the cytoplasmic maturation of the 60S subunit and constitutes the mutated target in the Shwachman-Diamond Syndrome. In solution, this protein coexists in an ensemble of three main conformations, with the N- and C-terminal ends adopting different orientations with respect to the central domain. The structure observed in the protein crystal corresponds to an average of those predicted by the SAXS flexibility analysis.

  8. Small angle X-ray scattering study on the conformation of polystyrene in the anti-solvent process of supercritical fluids

    International Nuclear Information System (INIS)

    Liu Yi; Wang Hongli; Zhao Xin; Chen Na; Li Dan; Liu Zhimin; Han Buxing; Rong Lixia; Zhao Hui; Wang Jun; Dong Baozhong

    2003-01-01

    The conformation of polystyrene in the anti-solvent process of supercritical fluids (compressed CO 2 + polystyrene + tetrahydrofuran) is studied by synchrotron radiation X-ray small angle scattering (SAXS). Coil-to-globule transform of polystyrene chain is observed with increasing the concentration of CO 2 . It is found that polystyrene coils at the pressure lower than cloud point pressure (p c ) and changes into globule with uniform density at the pressure higher than p c

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

    Science.gov (United States)

    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

  10. Small-angle scattering in materials science

    International Nuclear Information System (INIS)

    Paris, O.; Fratzl, P.

    1999-01-01

    Small-angle scattering (SAS) of X-rays (SAXS) or neutrons (SANS) are a powerful tools to investigate inhomogeneities in the size range from ∼ 1 nm to ∼ 100 nm. Typical examples in materials science are pores, precipitates in metal alloys or nano-particles in composites. Frequently, these inhomogeneities are not spherical and their alignment is not random, quite in contrast to many other applications of SAS. This requires the use of pinhole geometry and area detectors for the experimental set-up. The present paper focuses on evaluation techniques of two-dimensional (2D) SAS-patterns from some materials investigated by the authors, i.e. metal alloys, carbon composites, wood and bone. Although the examples shown are derived exclusively from SAXS measurements, most of them could stem from SANS measurements as well. (author)

  11. Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source

    Energy Technology Data Exchange (ETDEWEB)

    Ohsuka, Shinji, E-mail: ohsuka@crl.hpk.co.jp [Hamamatsu Photonics K.K., 5000 Hirakuchi, Hamakita-ku, Hamamatsu-City, 434-8601 (Japan); The Graduate School for the Creation of New Photonics Industries, 1955-1 Kurematsu-cho, Nishi-ku, Hamamatsu-City, 431-1202 (Japan); Ohba, Akira; Onoda, Shinobu; Nakamoto, Katsuhiro [Hamamatsu Photonics K.K., 5000 Hirakuchi, Hamakita-ku, Hamamatsu-City, 434-8601 (Japan); Nakano, Tomoyasu [Hamamatsu Photonics K.K., 5000 Hirakuchi, Hamakita-ku, Hamamatsu-City, 434-8601 (Japan); Ray-Focus Co. Ltd., 6009 Shinpara, Hamakita-ku, Hamamatsu-City, 434-0003 (Japan); Miyoshi, Motosuke; Soda, Keita; Hamakubo, Takao [Research Center for Advanced Science and Technology, The University of Tokyo, 4-6-1 Komaba, Meguro-ku, Tokyo 153-8904 (Japan)

    2014-09-15

    We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

  12. Laboratory-size three-dimensional x-ray microscope with Wolter type I mirror optics and an electron-impact water window x-ray source.

    Science.gov (United States)

    Ohsuka, Shinji; Ohba, Akira; Onoda, Shinobu; Nakamoto, Katsuhiro; Nakano, Tomoyasu; Miyoshi, Motosuke; Soda, Keita; Hamakubo, Takao

    2014-09-01

    We constructed a laboratory-size three-dimensional water window x-ray microscope that combines wide-field transmission x-ray microscopy with tomographic reconstruction techniques, and observed bio-medical samples to evaluate its applicability to life science research fields. It consists of a condenser and an objective grazing incidence Wolter type I mirror, an electron-impact type oxygen Kα x-ray source, and a back-illuminated CCD for x-ray imaging. A spatial resolution limit of around 1.0 line pairs per micrometer was obtained for two-dimensional transmission images, and 1-μm scale three-dimensional fine structures were resolved.

  13. Note: An X-ray powder diffractometer with a wide scattering-angle range of 72° using asymmetrically positioned one-dimensional detectors

    Energy Technology Data Exchange (ETDEWEB)

    Katsuya, Yoshio; Tanaka, Masahiko [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Song, Chulho [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Ito, Kimihiko; Kubo, Yoshimi [Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Synchrotron X-ray Group, Quantum Beam Unit, NIMS, 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan)

    2016-01-15

    An X-ray powder diffractometer has been developed for a time-resolved measurement without the requirement of a scattering angle (2θ) scan. Six one-dimensional detector modules are asymmetrically arranged in a vertical line at a designed distance of 286.5 mm. A detector module actually covers a diffraction angle of about 12° with an angular resolution of 0.01°. A diffracted intensity pattern is simultaneously recorded in a 2θ angular range from 1.63° to 74.37° in a “one shot” measurement. We tested the performance of the diffractometer with reference CeO{sub 2} powders and demonstrated diffraction measurements from an operating lithium-air battery.

  14. Three-dimensional reconstruction of neutron, gamma-ray, and x-ray sources using spherical harmonic decomposition

    Science.gov (United States)

    Volegov, P. L.; Danly, C. R.; Fittinghoff, D.; Geppert-Kleinrath, V.; Grim, G.; Merrill, F. E.; Wilde, C. H.

    2017-11-01

    Neutron, gamma-ray, and x-ray imaging are important diagnostic tools at the National Ignition Facility (NIF) for measuring the two-dimensional (2D) size and shape of the neutron producing region, for probing the remaining ablator and measuring the extent of the DT plasmas during the stagnation phase of Inertial Confinement Fusion implosions. Due to the difficulty and expense of building these imagers, at most only a few two-dimensional projections images will be available to reconstruct the three-dimensional (3D) sources. In this paper, we present a technique that has been developed for the 3D reconstruction of neutron, gamma-ray, and x-ray sources from a minimal number of 2D projections using spherical harmonics decomposition. We present the detailed algorithms used for this characterization and the results of reconstructed sources from experimental neutron and x-ray data collected at OMEGA and NIF.

  15. Three-dimensional phase-contrast X-ray microtomography with scanning–imaging X-ray microscope optics

    International Nuclear Information System (INIS)

    Takeuchi, Akihisa; Uesugi, Kentaro; Suzuki, Yoshio

    2013-01-01

    A novel three-dimensional X-ray microtomographic micro-imaging system which enables simultaneous measurement of differential phase contrast and absorption contrast has been developed. The optical system consists of a scanning microscope with one-dimensional focusing device and an imaging microscope with one-dimensional objective. A three-dimensional (3D) X-ray tomographic micro-imaging system has been developed. The optical system is based on a scanning–imaging X-ray microscope (SIXM) optics, which is a hybrid system consisting of a scanning microscope optics with a one-dimensional (1D) focusing (line-focusing) device and an imaging microscope optics with a 1D objective. In the SIXM system, each 1D dataset of a two-dimensional (2D) image is recorded independently. An object is illuminated with a line-focused beam. Positional information of the region illuminated by the line-focused beam is recorded with the 1D imaging microscope optics as line-profile data. By scanning the object with the line focus, 2D image data are obtained. In the same manner as for a scanning microscope optics with a multi-pixel detector, imaging modes such as phase contrast and absorption contrast can be arbitrarily configured after the image data acquisition. By combining a tomographic scan method and the SIXM system, quantitative 3D imaging is performed. Results of a feasibility study of the SIXM for 3D imaging are shown

  16. Study on two-dimensional distribution of X-ray image based on improved Elman algorithm

    International Nuclear Information System (INIS)

    Wang, Fang; Wang, Ming-Yuan; Tian, Feng-Shuo; Liu, Yu-Fang; Li, Lei; Zhao, Jing

    2015-01-01

    The principle of the X-ray detector which can simultaneously perform the measurement of the exposure rate and 2D (two-dimensional) distribution is described. A commercially available CMOS image sensor has been adopted as the key part to receive X-ray without any scintillators. The correlation between the pixel value (PV) and the absorbed exposure rate of X-ray is studied using the improved Elman neural network. Comparing the optimal adjustment process of the BP (Back Propagation) neural network and the improved Elman neural network, the neural network parameters are selected based on the fitting curve and the error curve. The experiments using the practical production data show that the proposed method achieves high accurate predictions to 10 −15 , which is consistent with the anticipated value. It is proven that it is possible to detect the exposure rate using the X-ray detector with the improved Elman algorithm for its advantages of fast converges and smooth error curve. - Highlights: • A method to measure the X-ray radiation with low cost and miniaturization. • A general CMOS image sensor is used to detect X-ray. • The system can measure exposure rate and 2D distribution simultaneously. • The Elman algorithm is adopted to improve the precision of the radiation detector

  17. Glancing angle x-ray studies of oxide films

    International Nuclear Information System (INIS)

    Davenport, A.J.; Isaacs, H.S.

    1989-01-01

    High brightness synchrotron radiation incident at glancing angles has been used to study inhibiting species present in low concentrations in oxide films on aluminum. Glancing incident angle fluorescence measurements give surface-sensitive information on the valence state of elements from the shape of the x-ray absorption edge. Angle-resolved measurements show the depth distribution of the species present. 15 refs., 4 figs

  18. Classifying and assembling two-dimensional X-ray laser diffraction patterns of a single particle to reconstruct the three-dimensional diffraction intensity function: resolution limit due to the quantum noise

    International Nuclear Information System (INIS)

    Tokuhisa, Atsushi; Taka, Junichiro; Kono, Hidetoshi; Go, Nobuhiro

    2012-01-01

    A new algorithm is developed for reconstructing the high-resolution three-dimensional diffraction intensity function of a globular biological macromolecule from many quantum-noise-limited two-dimensional X-ray laser diffraction patterns, each for an unknown orientation. The structural resolution is expressed as a function of the incident X-ray intensity and quantities characterizing the target molecule. A new two-step algorithm is developed for reconstructing the three-dimensional diffraction intensity of a globular biological macromolecule from many experimentally measured quantum-noise-limited two-dimensional X-ray laser diffraction patterns, each for an unknown orientation. The first step is classification of the two-dimensional patterns into groups according to the similarity of direction of the incident X-rays with respect to the molecule and an averaging within each group to reduce the noise. The second step is detection of common intersecting circles between the signal-enhanced two-dimensional patterns to identify their mutual location in the three-dimensional wavenumber space. The newly developed algorithm enables one to detect a signal for classification in noisy experimental photon-count data with as low as ∼0.1 photons per effective pixel. The wavenumber of such a limiting pixel determines the attainable structural resolution. From this fact, the resolution limit due to the quantum noise attainable by this new method of analysis as well as two important experimental parameters, the number of two-dimensional patterns to be measured (the load for the detector) and the number of pairs of two-dimensional patterns to be analysed (the load for the computer), are derived as a function of the incident X-ray intensity and quantities characterizing the target molecule

  19. Three-dimensional visualization of material flow during friction stir welding by two pairs of X-ray transmission systems

    International Nuclear Information System (INIS)

    Morisada, Y.; Fujii, H.; Kawahito, Y.; Nakata, K.; Tanaka, M.

    2011-01-01

    Material flow during friction stir welding is crucial to obtaining sound joints. However, this phenomenon is still not fully understood despite many investigations and numerous models. In this study, the material flow is three-dimensionally visualized by X-ray radiography using a tiny spherical tungsten tracer. The movement of the tracer during the friction stir welding is observed by two pairs of X-ray transmission real-time imaging systems. The three-dimensional material flow is obtained by following the locus of the tracer.

  20. Anomalous and resonance small-angle scattering

    International Nuclear Information System (INIS)

    Epperson, J.E.; Thiyagarajan, P.

    1988-01-01

    Significant changes in the small-angle scattered intensity can be induced by making measurements with radiation close to an absorption edge of an appropriate atomic species contained in the sample. These changes can be related quantitatively to the real and imaginary anomalous-dispersion terms for the scattering factor (X-rays) or scattering length (neutrons). The physics inherent in these anomalous-dispersion terms is first discussed before consideration of how they enter the relevant scattering theory. Two major areas of anomalous-scattering research have emerged; macromolecules in solution and unmixing of metallic alloys. Research in each area is reviewed, illustrating both the feasibility and potential of these techniques. All the experimental results reported to date have been obtained with X-rays. However, it is pointed out that the formalism is the same for the analog experiment with neutrons, and a number of suitable isotopes exist which exhibit resonance in an accessible range of energy. Potential applications of resonance small-angle neutron scattering are discussed. (orig.)

  1. 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.

    Science.gov (United States)

    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.

  2. Small-angle X-ray scattering on growth of AgCl crystallites in photochromic glasses

    International Nuclear Information System (INIS)

    Takatohi, U.E.; Bittencourt, D.R.S.; Watanabe, S.

    1997-01-01

    Reversible changes in the optical properties of photochromic glasses are observed owing to the presence of small silver halide crystals inside the glassy matrix. These crystals grow during the glass heat-treatment processing. Samples with molar composition of 40SiO 2 .10Al 2 O 3 .16.1K 2 O.33.9B 2 O 3 , doped with AgCl and CuO, were produced and submitted to different heat treatments: (i) for 0.5 h at temperatures from 753 to 893 K and (ii) at 873 K for periods of time from 0.25 to 1.25 h. Small-angle X-ray scattering (SAXS) was used to characterize the samples. The samples heat treated between 843 and 893 K presented an increasing growth rate of the Guinier radius (R g ). Samples heat treated at a fixed temperature of 873 K and different time t showed a law R g 3 = kt + c. Variations in the optical absorbance at 280 nm and the additional absorbance spectra of samples exposed to light showed correlation with the SAXS results. (orig.)

  3. Refraction angle and edge visibility in X-ray diffraction enhanced imaging

    International Nuclear Information System (INIS)

    Chen Yu; Jia Quanjie; Li Gang; Wang Yuzhu; Xue Xianying; Jiang Xiaoming

    2007-01-01

    Diffraction-enhanced X-ray imaging could extract accurately the refraction angles of the sample, which is very important to increase the image contrast of low Z samples. In this paper, the DEI experiments with X-rays of different energies were performed both on wedge-shaped and rounded model samples. Refraction angles of the two samples were all obtained accurately, and the results agreed well with the calculations. Quantitative analyses based on Edge Visibility were performed for the wedge-shaped model sample. The results revealed that the calculated positions for the Best Edge Visibility of the slope with fixed refraction angle were calculable in good agreement with the experimental results. A quantitative research on the Edge Visibility of real tissues sample was carried out and the optimal condition for best contrast of DEI images were discussed. (authors)

  4. Comparing natural and artificial carious lesions in human crowns by means of conventional hard x-ray micro-tomography and two-dimensional x-ray scattering with synchrotron radiation

    Science.gov (United States)

    Botta, Lea Maria; White, Shane N.; Deyhle, Hans; Dziadowiec, Iwona; Schulz, Georg; Thalmann, Peter; Müller, Bert

    2016-10-01

    Dental caries, one of the most prevalent infectious bacterial diseases in the world, is caused by specific types of acid-producing bacteria. Caries is a disease continuum resulting from the earliest loss of ions from apatite crystals through gross cavitation. Enamel dissolution starts when the pH-value drops below 5.5. Neutralizing the pH-value in the oral cavity opposes the process of demineralization, and so caries lesions occur in a dynamic cyclic de-mineralizing/remineralizing environment. Unfortunately, biomimetic regeneration of cavitated enamel is not yet possible, although remineralization of small carious lesions occurs under optimal conditions. Therefore, the development of methods that can regenerate carious lesions, and subsequently recover and retain teeth, is highly desirable. For the present proceedings we analyzed one naturally occurring sub-surface and one artificially produced lesion. For the characterization of artificial and natural lesions micro computed tomography is the method of choice when looking to determine three-dimensional mineral distribution and to quantify the degree of mineralization. In this pilot study we elucidate that the de-mineralized enamel in natural and artificially induced lesions shows comparable X-ray attenuation behavior, thereby implying that the study protocol employed herein seems to be appropriate. Once we know that the lesions are comparable, a series of well-reproducible in vitro experiments on enamel regeneration could be performed. In order to quantify further lesion morphology, the anisotropy of the enamel's nanostructure can be characterized by using spatially resolved, small-angle X-ray scattering. We wanted to demonstrate that the artificially induced defect fittingly resembles the natural carious lesion.

  5. Effect of Cobalt Fillers on Polyurethane Segmentations Investigated by Synchrotron Small Angle X-Ray Scattering

    Directory of Open Access Journals (Sweden)

    Krit Koyvanich

    2013-01-01

    Full Text Available The segmentation between rigid and rubbery chains in polyurethanes (PUs influences polymeric properties and implementations. Several models have successfully been proposed to visualize the configuration between the hard segment (HS and soft segment (SS. For particulate PU composites, the arrangement of HS and SS is more complicated because the fillers tend to disrupt the chain formation and segmentation. In this work, the effect of ferromagnetic cobalt (Co powders (average diameter 2 μm on PU synthesized from a reaction between polyether polyol (soft segment and diphenylmethane-4,4′-diisocyanate (hard segment was studied with varying loadings (0, 20, 40, and 60 wt.%. The 300 μm thick PU/Co samples were tape-casted and then received heat treatment at 80°C for 180 min. From synchrotron small angle X-ray scattering (SAXS, the plot of the X-ray scattering intensity (I against the scattering vector (q exhibited a typical single peak of PU whose intensity was reduced by the increase in the Co loading. Characteristic SAXS peaks in the case of 0-20 wt.% Co agreed well with the scattering by globular hard segment domains according to Zernike-Prins and Percus-Yevick models. The higher Co loadings led to larger deviations from all theoretical models.

  6. X-ray imaging with toroidal mirror

    International Nuclear Information System (INIS)

    Aoki, Sadao; Sakayanagi, Yoshimi

    1978-01-01

    X-ray imaging is made with a single toroidal mirror or two successive toroidal mirrors. Geometrical images at the Gaussian image plane are described by the ray trace. Application of a single toroidal mirror to small-angle scattering is presented. (author)

  7. Automation and remote access of EMBL small angle X-ray scattering beamline X33 dedicated to biological macromolecules

    International Nuclear Information System (INIS)

    Weifeng Shang; Roessle, M.; Blanchet, C.; Zozulya, A.; Franke, D.; Petoukhov, M.; Kikhney, A.; Svergun, D.

    2009-01-01

    Full text: The small-angle X-ray scattering beamline X33 of the European Molecular Biology Laboratory (EMBL) at the DORIS III storage ring (HASYLAB/DESY) has been dedicated to structural studies of non-crystalline biological systems for more than two decades. In the last several years, the introduction of new optical systems (monochromator, mirror, slits etc) and detector systems (large area image plate Mar345 and PILATUS 1M) leads to an improvement of photon flux by a factor of 3 and a reduction of the exposure time by a factor of 7. Moreover, an automated sample changer has been constructed and in operation since August 2007. The data analysis pipeline consisting of the program suite yields the radius of gyration and forward scattering intensity using Guinier analysis (AutoRg), pair distance distribution function p(r) using indirect Fourier transform method (AutoGNOM), and bead models using ab initio shape determination (DAMMIN and DAMMIF). The results of these analysis which are immediately available after each measurement provides an invaluable tool for data quality control during the data collection. Furthermore, works on remote control of the integrated data collection and analysis software is ongoing and expected to be operated in late 2009 where users can send their samples and control the measurements at home institutes. (author)

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Bruetzel, Linda K.; Fischer, Stefan; Salditt, Annalena; Sedlak, Steffen M.; Nickel, Bert; Lipfert, Jan, E-mail: Jan.Lipfert@lmu.de [Department of Physics, Nanosystems Initiative Munich, and Center for Nanoscience, Ludwig-Maximilians-University Munich, Amalienstr. 54, 80799 Munich, Germany and Geschwister-Scholl Platz 1, 80539 Munich (Germany)

    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. To 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.

  10. Metal ion controlled self-assembly of a chemically reengineered protein drug studied by small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Jesper, Nygaard; Munch, Henrik K.; Thulstrup, Peter W.

    2012-01-01

    . A small-angle X-ray scattering analysis of the bipyridine-modified insulin system confirmed an organization into a novel well-ordered structure based on insulin trimers, as induced by the addition of Fe(II). In contrast, unmodified monomeric insulin formed larger and more randomly structured assemblies......Precise control of the oligomeric state of proteins is of central importance for biological function and for the properties of biopharmaceutical drugs. Here, the self-assembly of 2,2′-bipyridine conjugated monomeric insulin analogues, induced through coordination to divalent metal ions, was studied....... This protein drug system was designed to form non-native homo-oligomers through selective coordination of two divalent metal ions, Fe(II) and Zn(II), respectively. The insulin type chosen for this study is a variant designed for a reduced tendency toward native dimer formation at physiological concentrations...

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

    Science.gov (United States)

    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.

  12. New developments in the simultaneous measurement system of wide-angle and small-angle x-ray scatterings and vibrational spectra for the static and dynamic analyses of the hierarchical structures of polymer solids

    International Nuclear Information System (INIS)

    Tashiro, Kohji; Yamamoto, Hiroko; Yoshioka, Taiyo; Ninh, Tran Hai; Shimada, Shigeru; Nakatani, Takeshi; Iwamoto, Hiroyuki; Ohta, Noboru; Masunaga, Hiroyasu

    2012-01-01

    A simultaneous measurement system of wide-angle X-ray diffraction (WAXD), small-angle X-ray scattering (SAXS) and Raman or transmission-type infrared spectroscopy was developed by us. Its purposes is to clarify the static and dynamic structural changes of polymer materials subjected to the various external condition changes. Some examples described here include the study of the stretch-induced reorientation phenomenon of a-axially-oriented polyethylene, the study of structural change in photo-induced solid-state polymerization reaction of muconic acid ester monomer crystal, the study of the two-stage high-temperature phase transitions of aliphatic nylons, the study of stress-induced crystalline phase transition of an oriented poly(tetramethylene terephthalate) sample and its relation to the higher-order structural change, and the study of structural regularization process of poly(L-lactic acid) in the isothermal crystallization of the meso phase. These case studies in the clarification of hierarchical structural changes of polymer materials have proven that the simultaneous measurement systems can be useful to examine the structural changes in polymer systems. (author)

  13. Low-angle X-ray scattering from spices

    International Nuclear Information System (INIS)

    Desouky, O.S.; Ashour, Ahmed H.; Abdullah, Mohamed I.; Elshemey, Wael M.

    2002-01-01

    Low-angle scattering of X-rays is characterized by the presence of one or more peaks in the forward direction of scattering. These peaks are due to the interference of photons coherently scattered from the molecules of the medium. Thus these patterns are closely linked to the molecular structure of the investigated medium. In this work, low-angle X-ray scattering (LAXS) profiles of five spices; pimpinella anisum (anise), coriandrum sativum (coriander), cuminum cyminum (cumin), foenculum vulgare (fennel) and nigella sativa (nigella or black cumin) are presented after extensive measurements. It is found that all spices exhibit one characteristic peak at a scattering angle around 10 deg. This is equivalent to a value x=0.0565 A -1 , where x=sin(θ/2)/λ. The full width at half maximum (FWHM) of this peak is found to be characteristic for each type of the investigated spices. The possibility to detect the irradiation of these spices from their LAXS profiles is also examined after 10, 20, 30 and 40 kGy doses of gamma radiation. Except for anise, coriander and cumin at 40 kGy, there are no detectable deviations from the control samples in the scattering profiles of irradiated samples. These results comply with the recommendations of the FDA (US Food and Drug Administration) which defines 30 kGy as the maximum dose for irradiation of spices. The present technique could be used to detect over-irradiation, which causes damage to the molecular structure of some spices

  14. Systematic Errors in Dimensional X-ray Computed Tomography

    DEFF Research Database (Denmark)

    that it is possible to compensate them. In dimensional X-ray computed tomography (CT), many physical quantities influence the final result. However, it is important to know which factors in CT measurements potentially lead to systematic errors. In this talk, typical error sources in dimensional X-ray CT are discussed...

  15. Combining Single-Molecule Optical Trapping and Small-Angle X-Ray Scattering Measurements to Compute the Persistence Length of a Protein ER/K alpha-Helix

    DEFF Research Database (Denmark)

    Sivaramakrishnan, S.; Sung, J.; Ali, M.

    2009-01-01

    as a force transducer, rigid spacer, or flexible linker in proteins. In this study, we quantity this flexibility in terms of persistence length, namely the length scale over which it is rigid. We use single-molecule optical trapping and small-angle x-ray scattering, combined with Monte Carlo simulations...

  16. X-ray diffraction at Bragg angles around π/2

    International Nuclear Information System (INIS)

    Mayolo, C.M.G. de.

    1991-01-01

    X-ray diffraction at Bragg angles around π/2 is studied from the theoretical and experimental points of view. The proposed corrections to the dynamical theory in the θ β ≅ π/2 cases, has been reviewed showing the equivalence between two formalisms leading to a corrected expression for the dependence of the angular parameter y with the angle of incidence. An expression for y valid in the conventional and θ β ≅ π/2 cases has been obtained. A general expression for Bragg law and for energy resolution after a Bragg diffraction was also deduced. (author)

  17. Small-angle X-ray scattering on growth of AgCl crystallites in photochromic glasses

    Energy Technology Data Exchange (ETDEWEB)

    Takatohi, U.E. [Inst. Adventista de Ensino, Sao Paulo (Brazil); Bittencourt, D.R.S.; Watanabe, S.

    1997-10-01

    Reversible changes in the optical properties of photochromic glasses are observed owing to the presence of small silver halide crystals inside the glassy matrix. These crystals grow during the glass heat-treatment processing. Samples with molar composition of 40SiO{sub 2}.10Al{sub 2}O{sub 3}.16.1K{sub 2}O.33.9B{sub 2}O{sub 3}, doped with AgCl and CuO, were produced and submitted to different heat treatments: (i) for 0.5 h at temperatures from 753 to 893 K and (ii) at 873 K for periods of time from 0.25 to 1.25 h. Small-angle X-ray scattering (SAXS) was used to characterize the samples. The samples heat treated between 843 and 893 K presented an increasing growth rate of the Guinier radius (R{sub g}). Samples heat treated at a fixed temperature of 873 K and different time t showed a law R{sub g}{sup 3} = kt + c. Variations in the optical absorbance at 280 nm and the additional absorbance spectra of samples exposed to light showed correlation with the SAXS results. (orig.). 16 refs.

  18. Very large-scale structures in sintered silica aerogels as evidenced by atomic force microscopy and ultra-small angle X-ray scattering experiments

    CERN Document Server

    Marliere, C; Etienne, P; Woignier, T; Dieudonné, P; Phalippou, J

    2001-01-01

    During the last few years the bulk structure of silica aerogels has been extensively studied mainly by scattering techniques (neutrons, X-rays, light). It has been shown that small silica particles aggregate to constitute a fractal network. Its spatial extension and fractal dimension are strongly dependent on the synthesis conditions (e.g., pH of gelifying solutions). These typical lengths range from 1 to 10 nm. Ultra-small angle X-ray scattering (USAXS) and atomic force microscopy (AFM) experiments have been carried out on aerogels at different steps of densification. The results presented in this paper reveal the existence of a spatial arrangement of the solid part at a very large length scale. The evolution of this very large-scale structure during the densification process has been studied and reveals a contraction of this macro-structure made of aggregates of clusters. (16 refs).

  19. Development of a two-dimensional ASIC for hard X-ray spectroscopy and imaging with a CdTe pixel detector

    International Nuclear Information System (INIS)

    Hiruta, Tatsuro; Tamura, K.; Ikeda, H.; Nakazawa, K.; Takasima, T.; Takahashi, T.

    2006-01-01

    We are developing a two-dimensional analog ASIC for the readout of pixel sensors based on silicon (Si) or cadmium telluride (CdTe) for spectroscopic imaging observations in the X-ray and gamma-ray regions. The aim for the ASIC is to obtain a low-noise performance better than 100 electrons (rms) with self-triggering capabilities. As the first step of prototyping, we have fabricated several ASICs. We obtained an energy resolution of 5.4 keV (FWHM) for 81 keV gamma-rays from 133 Ba with a one-dimensional ASIC connected to a CdTe diode and also verified a readout architecture via a two-dimensional ASIC with 144 pixel channels. Based on the results obtained and experience gained through prototype ASICs, we are developing a 4096-channel two-dimensional analog ASIC

  20. Three-dimensional measurements of the lower extremity in children and adolescents using a low-dose biplanar X-ray device

    International Nuclear Information System (INIS)

    Gheno, Ramon; Nectoux, Eric; Herbaux, Bernard; Baldisserotto, Matteo; Glock, Luiz; Cotten, Anne; Boutry, Nathalie

    2012-01-01

    To evaluate three-dimensional (3D) measurements of the lower extremity using a biplanar low-dose X-ray device in children and adolescents. Firstly, 3D measurements of eight dried bones were analysed by a biplanar low-dose X-ray device (LDX) using stereoscopic software and compared with 3D computed tomography (CT). Secondly, 47 lower limbs of children and adolescents were studied using LDX two-dimensional (2D) and 3D measurements. Both parts were evaluated for femoral and tibial lengths and mechanical angles, frontal and lateral knee angulations, and the femoral neck-shaft angle. The 3D specimen comparison between LDX and CT measurements showed no significant differences: femoral length (P = 0.069), tibial length (P = 0.059), femoral mechanical angle (P = 0.475), tibial mechanical angle (P = 0.067), frontal knee angulation (P = 0.198), lateral knee angulation (P = 0.646) and femoral neck-shaft angle (P = 0.068). The comparison between LDX 2D and 3D measurements showed significant differences in tibial length (P = 0.003), femoral mechanical angle (P < 0.001) and femoral neck-shaft angle (P = 0.001); other parameters were unremarkable. The 3D LDX system presented reliable measurements compared with 3D CT. Differences between LDX 2D and 3D measurements were noted in the femoral mechanical angle, femoral neck-shaft angle and tibial length. Moderate to good interobserver agreement for the 3D LDX measurements were found. (orig.)

  1. Protein folding and protein metallocluster studies using synchrotron small angler X-ray scattering

    International Nuclear Information System (INIS)

    Eliezer, D.

    1994-06-01

    Proteins, biological macromolecules composed of amino-acid building blocks, possess unique three dimensional shapes or conformations which are intimately related to their biological function. All of the information necessary to determine this conformation is stored in a protein's amino acid sequence. The problem of understanding the process by which nature maps protein amino-acid sequences to three-dimensional conformations is known as the protein folding problem, and is one of the central unsolved problems in biophysics today. The possible applications of a solution are broad, ranging from the elucidation of thousands of protein structures to the rational modification and design of protein-based drugs. The scattering of X-rays by matter has long been useful as a tool for the characterization of physical properties of materials, including biological samples. The high photon flux available at synchrotron X-ray sources allows for the measurement of scattering cross-sections of dilute and/or disordered samples. Such measurements do not yield the detailed geometrical information available from crystalline samples, but do allow for lower resolution studies of dynamical processes not observable in the crystalline state. The main focus of the work described here has been the study of the protein folding process using time-resolved small-angle x-ray scattering measurements. The original intention was to observe the decrease in overall size which must accompany the folding of a protein from an extended conformation to its compact native state. Although this process proved too fast for the current time-resolution of the technique, upper bounds were set on the probable compaction times of several small proteins. In addition, an interesting and unexpected process was detected, in which the folding protein passes through an intermediate state which shows a tendency to associate. This state is proposed to be a kinetic molten globule folding intermediate

  2. X-ray magnetic circular dichroism and small angle neutron scattering studies of thiol capped gold nanoparticles

    International Nuclear Information System (INIS)

    de la Venta, J.; Bouzas, V.; Pucci, A.; Laguna-Marco, M.A.; Haskel, D.; te Velthuis, S.G.E; Hoffmann, A.; Lal, J.; Bleuel, M.; Ruggeri, G.; de Julian Fernandez, C.; Garcia, M.A.

    2009-01-01

    X-ray magnetic circular dichroism (XMCD) and Small Angle Neutron Scattering (SANS) measurements were performed on thiol capped Au nanoparticles (NPs) embedded into polyethylene. An XMCD signal of 0.8 · 10 -4 was found at the Au L 3 edge of thiol capped Au NPs embedded in a polyethylene matrix for which Superconducting Quantum Interference Device (SQUID) magnetometry yielded a saturation magnetization, M s , of 0.06 emu/g Au . SANS measurements showed that the 3.2 nm average-diameter nanoparticles are 28% polydispersed, but no detectable SANS magnetic signal was found with the resolution and sensitivity accessible with the neutron experiment. A comparison with previous experiments carried out on Au NPs and multilayers, yield to different values between XMCD signals and magnetization measured by SQUID magnetometer. We discuss the origin of those differences

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

    KAUST Repository

    Sibillano, T.

    2014-11-10

    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.

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

    KAUST Repository

    Sibillano, T.; De Caro, L.; Altamura, D.; Siliqi, D.; Ramella, M.; Boccafoschi, F.; Ciasca, G.; Campi, G.; Tirinato, Luca; Di Fabrizio, Enzo M.; Giannini, C.

    2014-01-01

    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.

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

    Science.gov (United States)

    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.

  6. Development and applications of grazing exit micro X-ray fluorescence instrument using a polycapillary X-ray lens

    International Nuclear Information System (INIS)

    Emoto, T.; Sato, Y.; Konishi, Y.; Ding, X.; Tsuji, K.

    2004-01-01

    A polycapillary X-ray lens is an effective optics to obtain a μm-size X-ray beam for micro-X-ray fluorescence spectrometry (μ-XRF). We developed a μ-XRF instrument using a polycapillary X-ray lens, which also enabled us to perform Grazing Exit μ-XRF (GE-μ-XRF). The evaluated diameter of the primary X-ray beam was 48 μm at the focal distance of the X-ray lens. Use of this instrument enabled two-dimensional mapping of the elemental distributions during growth of the plant 'Quinoa'. The results of the mapping revealed elemental transition during growth. In addition, a small region of thin film was analyzed by GE-μ-XRF. We expect that GE-μ-XRF will become an effective method of estimating the film thickness of a small region

  7. Small scale soft x-ray lasers

    International Nuclear Information System (INIS)

    Skinner, C.H.; DiCicco, D.S.; Kim, D.; Voorhees, D.; Suckewer, S.

    1990-01-01

    The widespread application of soft x-ray laser technology is contingent on the development of small scale soft x-ray lasers that do not require large laser facilities. Progress in the development of soft x-ray lasers pumped by a Nd laser of energy 6-12J is reported below. Application of an existing soft x-ray laser to x-ray microscopy has begun. A soft x-ray laser of output energy 1-3 mJ at 18,2 nm has been used to record high resolution images of biological specimens. The contact images were recorded on photoresist which was later viewed in a scanning electron microscope. The authors present a composite optical x-ray laser microscope design

  8. Fluid adsorption in ordered mesoporous solids determined by in situ small-angle X-ray scattering.

    Science.gov (United States)

    Findenegg, Gerhard H; Jähnert, Susanne; Müter, Dirk; Prass, Johannes; Paris, Oskar

    2010-07-14

    The adsorption of two organic fluids (n-pentane and perfluoropentane) in a periodic mesoporous silica material (SBA-15) is investigated by in situ small-angle X-ray scattering (SAXS) using synchrotron radiation. Structural changes are monitored as the ordered and disordered pores in the silica matrix are gradually filled with the fluids. The experiments yield integrated peak intensities from up to ten Bragg reflections from the 2D hexagonal pore lattice, and additionally diffuse scattering contributions arising from disordered (mostly intrawall) porosity. The analysis of the scattering data is based on a separation of these two contributions. Bragg scattering is described by adopting a form factor model for ordered pores of cylindrical symmetry which accounts for the filling of the microporous corona, the formation of a fluid film at the pore walls, and condensation of the fluid in the core. The filling fraction of the disordered intrawall pores is extracted from the diffuse scattering intensity and its dependence on the fluid pressure is analyzed on the basis of a three-phase model. The data analysis introduced here provides an important generalisation of a formalism presented recently (J. Phys. Chem. C, 2009, 13, 15201), which was applicable to contrast-matching fluids only. In this way, the adsorption behaviour of fluids into ordered and disordered pores in periodic mesoporous materials can be analyzed quantitatively irrespective of the fluid density.

  9. Small-angle x-ray scattering study on conformation of amorphous polymer chain in the bulk

    International Nuclear Information System (INIS)

    Hayashi, Hisao; Hamada, Fumiyuki; Nakajima, Akio

    1975-01-01

    In a previous paper, the new method for the determination of the conformation of polymer chains in concentrated solution and in bulk by small angle X-ray scattering was reported. The purpose of this paper is to estimate the dimension and conformation of polystyrene chains in bulk by this method. The tagged polymer used was the copolymer of styrene and p-iodostyrene. Excess scattering was obtained by subtracting the intensity of polystyrene matrix from that of a mixture containing polystyrene and a small fraction of the tagged polystyrene. Since the excess scattering originates from the group of iodine atoms in the tagged polystyrene, the radius of gyration of the tagged polystyrene is estimated by Guinier plot. Measurement was made with a Kratky camera, and in order to obtain high scattering intensity, the primary beam with line-shaped cross section was used. The intercepts of two limiting curves in the plotted radius of gyration diagram showed good agreement, and the measured molecular dimension agreed with the unperturbed dimension of this polymer. It was concluded that the molecular chains in bulk are mutually penetrable, and the centers of gravity of the molecules distribute almost randomly. It was suggested from the plot of the excess scattering intensity that the conformation of the tagged molecules is a random coil. The present results did not support the ordered structure revealed by bundle model and meander model. (Kako, I.)

  10. X-ray optics and X-ray microscopes: new challenges

    International Nuclear Information System (INIS)

    Susini, J.

    2004-01-01

    Soon after the discovery of X-rays in 1895 by W. Roentgen, it became rapidly clear that the methods traditionally used in the visible light regime, namely refraction, diffraction and reflection were difficult to apply for X-ray optics. The physical origins of these difficulties are closely linked to the very nature of interaction of X-rays with matter. The small deviation δ of the refractive index of condensed matter from unity makes it difficult to extend refraction-based optics from the optical spectral region to the X-ray region because the refraction angle is proportional to δ. Similarly it is very challenging to extend diffraction-based focusing techniques to X-rays because the diffraction angle scales inversely with wavelength. Finally, the use of reflection-based optics is also limited by the very small critical angle for total reflection. All those fundamental limitations prevented for almost one century, the development of X-ray microscopy whereas electron microscopy became a standard tool. In the past twenty years, interests for X-ray microscopy revived, mainly because of several major advances in X-ray sources and X-ray optics. X-ray microscopy techniques are now emerging as powerful and complementary tools for submicron investigations. Soft X-ray microscopes offer traditionally the possibility to form direct images of thick hydrated biological material in near-native environment, at a spatial resolution well beyond that achievable with visible light microscopy. Natural contrast is available in the soft X-ray region, in the so-called ''water-window'', due to the presence of absorption edges of the major constituents (C,N,O). Recent advances in manufacturing techniques have enlarged the accessible energy range of micro-focussing optics and offer new applications in a broad range of disciplines. X-ray microscopy in the 1 - 30 keV energy range is better suited for fluorescence to map trace elements, tomography for 3D imaging and micro-diffraction. The

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

    Science.gov (United States)

    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.

  12. X-ray and visible light transmission as two-dimensional, full-field moisture-sensing techniques: A preliminary comparison

    International Nuclear Information System (INIS)

    Tidwell, V.C.; Glass, R.J.

    1992-01-01

    Two independent high-resolution moisture-sensing techniques, x-ray absorption and light transmission, have been developed for use in two-dimensional, thin-slab experimental systems. The techniques yield full-field measurement capabilities with exceptional resolution of moisture content in time and space. These techniques represent powerful tools for the experimentalist to investigate processes governing unsaturated flow and transport through fractured and nonfractured porous media. Evaluation of these techniques has been accomplished by direct comparison of data obtained by means of the x-ray and light techniques as well as comparison with data collected by gravimetric and gamma-ray densitometry techniques. Results show excellent agreement between data collected by the four moisture-content measurement techniques. This program was established to support the Yucca Mountain Site Characterization Project

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

    Science.gov (United States)

    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

  14. Classifying and assembling two-dimensional X-ray laser diffraction patterns of a single particle to reconstruct the three-dimensional diffraction intensity function: resolution limit due to the quantum noise.

    Science.gov (United States)

    Tokuhisa, Atsushi; Taka, Junichiro; Kono, Hidetoshi; Go, Nobuhiro

    2012-05-01

    A new two-step algorithm is developed for reconstructing the three-dimensional diffraction intensity of a globular biological macromolecule from many experimentally measured quantum-noise-limited two-dimensional X-ray laser diffraction patterns, each for an unknown orientation. The first step is classification of the two-dimensional patterns into groups according to the similarity of direction of the incident X-rays with respect to the molecule and an averaging within each group to reduce the noise. The second step is detection of common intersecting circles between the signal-enhanced two-dimensional patterns to identify their mutual location in the three-dimensional wavenumber space. The newly developed algorithm enables one to detect a signal for classification in noisy experimental photon-count data with as low as ~0.1 photons per effective pixel. The wavenumber of such a limiting pixel determines the attainable structural resolution. From this fact, the resolution limit due to the quantum noise attainable by this new method of analysis as well as two important experimental parameters, the number of two-dimensional patterns to be measured (the load for the detector) and the number of pairs of two-dimensional patterns to be analysed (the load for the computer), are derived as a function of the incident X-ray intensity and quantities characterizing the target molecule. © 2012 International Union of Crystallography

  15. DMSO-induced dehydration of DPPC membranes studied by x-ray diffraction, small angle neutron scattering and calorimetry

    International Nuclear Information System (INIS)

    Kiselev, M.A.; Kiselev, A.M.; Lesieur, P.; Grabielle-Madelmond, C.; Ollivon, M.

    1998-01-01

    The properties of dimethyl sulfoxide (DMSO), a cryoprotector well known for its biological and therapeutic applications, were investigated on lipid membranes by x-ray diffraction, differential scanning calorimetry (DSC) and small angle neutron scattering (SANS). The DSC study of water freezing and melting of ice was performed in the ternary system which consists of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC)/DMSO/water system. The influence of DMSO on the DPPC membrane structure was established in the excess of solvent in the region of DMSO mole fraction from 0.0 to 1.0. The methods applied demonstrated the differences in the membrane structure in three sub-regions of DMSO mole fraction (X DMSO ) from 0.0 to 0.3 for the first, from 0.3 to 0.9 for the second, and from 0.9 to 1.0 for the third sub-region. The results for 0.0 ≤ X DMSO ≤ 0.3 can be explained in the framework of DMSO-induced dehydration of intermembrane space

  16. X-ray fluorescence analysis of thin films at glancing-incident and -takeoff angles

    International Nuclear Information System (INIS)

    Tsuji, K.; Sato, S.; Hirokawa, K.

    1995-01-01

    We have developed a new analytical method, Glancing-Incidence and -Takeoff X-Ray Fluorescence (GIT-XRF) method for the first time. Here, we present an idea for a thin-film analysis and a surface analysis by the GIT-XRF method. In this method, the dependence of the fluorescent x-ray intensity on takeoff angle is measured at various incident angles of the primary x-ray. Compared with a total reflection x-ray fluorescence method, the GIT-XRF method allows a detailed thin-film analysis, because the thin film is cross-checked by many experimental curves. Moreover, a surface-sensitive analysis is also possible by the GIT-XRF method. (author)

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

    Science.gov (United States)

    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.

  18. Development and applications of grazing exit micro X-ray fluorescence instrument using a polycapillary X-ray lens

    Energy Technology Data Exchange (ETDEWEB)

    Emoto, T.; Sato, Y.; Konishi, Y.; Ding, X.; Tsuji, K. E-mail: tsuji@a-chem.eng.osaka-cu.ac.jp

    2004-08-31

    A polycapillary X-ray lens is an effective optics to obtain a {mu}m-size X-ray beam for micro-X-ray fluorescence spectrometry ({mu}-XRF). We developed a {mu}-XRF instrument using a polycapillary X-ray lens, which also enabled us to perform Grazing Exit {mu}-XRF (GE-{mu}-XRF). The evaluated diameter of the primary X-ray beam was 48 {mu}m at the focal distance of the X-ray lens. Use of this instrument enabled two-dimensional mapping of the elemental distributions during growth of the plant 'Quinoa'. The results of the mapping revealed elemental transition during growth. In addition, a small region of thin film was analyzed by GE-{mu}-XRF. We expect that GE-{mu}-XRF will become an effective method of estimating the film thickness of a small region.

  19. X-ray magnetic circular dichroism and small angle neutron scattering studies of thiol capped gold nanoparticles.

    Energy Technology Data Exchange (ETDEWEB)

    de la Venta, J.; Bouzas, V.; Pucci, A.; Laguna-Marco, M. A.; Haskel, D.; te Velthuis, S. G. E; Hoffmann, A.; Lal, J.; Bleuel, M.; Ruggeri, G.; de Julian Fernandez, C.; Garcia, M. A.; Univ.Complutense de Madrid; Inst. de Magnetismo Aplicado; Univ. of Pisa; Lab. di Magnetismo Molecolare

    2009-01-01

    X-ray magnetic circular dichroism (XMCD) and Small Angle Neutron Scattering (SANS) measurements were performed on thiol capped Au nanoparticles (NPs) embedded into polyethylene. An XMCD signal of 0.8 {center_dot} 10{sup -4} was found at the Au L{sub 3} edge of thiol capped Au NPs embedded in a polyethylene matrix for which Superconducting Quantum Interference Device (SQUID) magnetometry yielded a saturation magnetization, M{sub s}, of 0.06 emu/g{sub Au}. SANS measurements showed that the 3.2 nm average-diameter nanoparticles are 28% polydispersed, but no detectable SANS magnetic signal was found with the resolution and sensitivity accessible with the neutron experiment. A comparison with previous experiments carried out on Au NPs and multilayers, yield to different values between XMCD signals and magnetization measured by SQUID magnetometer. We discuss the origin of those differences.

  20. X-ray magnetic circular dichroism and small angle neutron scattering study of thiol capped gold nanoparticles.

    Energy Technology Data Exchange (ETDEWEB)

    de la Venta, J.; Bouzas, V.; Pucci, A.; Laguna-Marco, M. A.; Haskel, D.; Pinel, E. F.; te Velthuis, S. G. E.; Hoffmann, A.; Lal, J.; Bleuel, M.; Ruggeri, G.; de Julian, C.; Garcia, M. A.; Univ. Complutense de Madrid; Inst. de Magnetismo Aplicado UCM; Univ. Pisa; Univ. di Padova

    2009-11-01

    X-ray magnetic circular dichroism (XMCD) and Small Angle Neutron Scattering (SANS) measurements were performed on thiol capped Au nanoparticles (NPs) embedded into polyethylene. An XMCD signal of 0.8 {center_dot} 10{sup -4} was found at the Au L{sub 3} edge of thiol capped Au NPs embedded in a polyethylene matrix for which Superconducting Quantum Interference Device (SQUID) magnetometry yielded a saturation magnetization, M{sub s}, of 0.06 emu/g{sub Au}. SANS measurements showed that the 3.2 nm average-diameter nanoparticles are 28% polydispersed, but no detectable SANS magnetic signal was found with the resolution and sensitivity accessible with the neutron experiment. A comparison with previous experiments carried out on Au NPs and multilayers, yield to different values between XMCD signals and magnetization measured by SQUID magnetometer. We discuss the origin of those differences.

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

    Science.gov (United States)

    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.

  2. Recent developments and ASAXS measurements at the ultra small angle X-ray scattering instrument of HASYLAB

    CERN Document Server

    Krosigk, G V; Gehrke, R; Kranold, R

    2001-01-01

    The wiggler beamline BW4 at the synchrotron radiation facility HASYLAB (DESY) is mainly designed for Ultra Small Angle X-ray Scattering (USAXS) and usually operated with detector-sample distances up to 13 m and at photon energies between 4 and 16 keV. With a new optical design the largest observable correlation distances have now been increased up to 9x10 sup 3 A. A grazing incidence set-up [P. Mueller-Buschbaum et al., Europhys. Lett. 42 (5) (1998) 517], vapor chamber, furnace, tensile testing machine and other instruments make the USAXS beamline attractive for a variety of scattering experiments [A. Endres et al., Rev. Sci. Instrum. 11 (1997) 68; A. Karl et al., J. Macromolecular Sci.-Phys. B 38 (5 and 6) (1999) 901; S. Minko et al., J. Macromolecular Sci., Phys. B 38 (5 and 6) (1999) 913]. A fully evacuated beampath allows high quality measurements with very low background signal. A photodiode mounted in the primary beam stop registers the primary beam flux simultaneously to the data acquisition and thus p...

  3. Limited-angle x-ray luminescence tomography: methodology and feasibility study

    International Nuclear Information System (INIS)

    Carpenter, C M; Pratx, G; Sun, C; Xing, L

    2011-01-01

    X-ray luminescence tomography (XLT) has recently been proposed as a new imaging modality for biological imaging applications. This modality utilizes phosphor nanoparticles which luminesce near-infrared light when excited by x-ray photons. The advantages of this modality are that it uniquely combines the high sensitivity of radioluminescent nanoparticles and the high spatial localization of collimated x-ray beams. Currently, XLT has been demonstrated using x-ray spatial encoding to resolve the imaging volume. However, there are applications where the x-ray excitation may be limited by geometry, where increased temporal resolution is desired, or where a lower dose is mandatory. This paper extends the utility of XLT to meet these requirements by incorporating a photon propagation model into the reconstruction algorithm in an x-ray limited-angle (LA) geometry. This enables such applications as image-guided surgery, where the ability to resolve lesions at depths of several centimeters can be the key to successful resection. The hybrid x-ray/diffuse optical model is first formulated and then demonstrated in a breast-sized phantom, simulating a breast lumpectomy geometry. Both numerical and experimental phantoms are tested, with lesion-simulating objects of various sizes and depths. Results show localization accuracy with median error of 2.2 mm, or 4% of object depth, for small 2-14 mm diameter lesions positioned from 1 to 4.5 cm in depth. This compares favorably with fluorescence optical imaging, which is not able to resolve such small objects at this depth. The recovered lesion size has lower size bias in the x-ray excitation direction than the optical direction, which is expected due to the increased optical scatter. However, the technique is shown to be quite invariant in recovered size with respect to depth, as the standard deviation is less than 2.5 mm. Sensitivity is a function of dose; radiological doses are found to provide sufficient recovery for μg ml -1

  4. Modern X-ray difraction. X-ray diffractometry for material scientists, physicists, and chemicists

    International Nuclear Information System (INIS)

    Spiess, L.; Schwarzer, R.; Behnken, H.; Teichert, G.

    2005-01-01

    The book yields a comprehensive survey over the applications of X-ray diffraction in fields like material techniques, metallurgy, electrotechniques, machine engineering, as well as micro- and nanotechniques. The necessary fundamental knowledge on X-ray diffraction are mediated foundedly and illustratively. Thereby new techniques and evaluation procedures are presented as well as well known methods. The content: Production and properties of X radiation, diffraction of X radiation, hardware for X-ray diffraction, methods of X-ray diffraction, lattice-constant determination, phase analysis, X-ray profile analysis, crystal structure analysis, X-ray radiographic stress analysis, X-ray radiographic texture analysis, crystal orientation determination, pecularities at thin films, small angle scattering

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

    Directory of Open Access Journals (Sweden)

    Athanasios Ch Mitropoulos

    Full Text Available 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.

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

    Science.gov (United States)

    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

  7. An introduction to three-dimensional X-ray diffraction microscopy

    DEFF Research Database (Denmark)

    Poulsen, Henning Friis

    2012-01-01

    Three-dimensional X-ray diffraction microscopy is a fast and nondestructive structural characterization technique aimed at studies of the individual crystalline elements (grains or subgrains) within millimetre-sized polycrystalline specimens. It is based on two principles: the use of highly...... penetrating hard X-rays from a synchrotron source and the application of tomographic reconstruction algorithms for the analysis of the diffraction data. In favourable cases, the position, morphology, phase and crystallographic orientation can be derived for up to 1000 elements simultaneously. For each grain...

  8. Ultrasmall-angle X-ray scattering analysis of photonic crystal structure

    International Nuclear Information System (INIS)

    Abramova, V. V.; Sinitskii, A. S.; Grigor'eva, N. A.; Grigor'ev, S. V.; Belov, D. V.; Petukhov, A. V.; Mistonov, A. A.; Vasil'eva, A. V.; Tret'yakov, Yu. D.

    2009-01-01

    The results of an ultrasmall-angle X-ray scattering study of iron(III) oxide inverse opal thin films are presented. The photonic crystals examined are shown to have fcc structure with amount of stacking faults varying among the samples. The method used in this study makes it possible to easily distinguish between samples with predominantly twinned fcc structure and nearly perfect fcc stacking. The difference observed between samples fabricated under identical conditions is attributed to random layer stacking in the self-assembled colloidal crystals used as templates for fabricating the inverse opals. The present method provides a versatile tool for analyzing photonic crystal structure in studies of inverse opals made of various materials, colloidal crystals, and three-dimensional photonic crystals of other types.

  9. Assessment of firing conditions in old fired-clay bricks. The contribution of X-ray powder diffraction with the Rietveld method and small angle neutron scattering

    Czech Academy of Sciences Publication Activity Database

    Viani, Alberto; Sotiriadis, Konstantinos; Len, A.; Šašek, Petr; Ševčík, Radek

    2016-01-01

    Roč. 116, June (2016), s. 33-43 ISSN 1044-5803 R&D Projects: GA MŠk(CZ) LO1219 Keywords : fired- clay brick * Rietveld method * small angle neutron scattering * X-ray diffraction * firing temperature Subject RIV: AL - Art, Architecture, Cultural Heritage Impact factor: 2.714, year: 2016 http://www.sciencedirect.com/science/article/pii/S1044580316300870

  10. Small-angle X-ray scattering documents the growth of metal-organic frameworks

    NARCIS (Netherlands)

    Goesten, M.G.; Stavitski, I.; Juan-Alcañiz, J.; Martinez-Joaristi, A.; Petukhov, A.V.; Kapteijn, F.; Gascon, J.

    2013-01-01

    We present a combined in situ small- and wide-angle scattering (SAXS/WAXS) study on the crystallization of two topical metal-organic frameworks synthesized from similar metal and organic precursors: NH2-MIL-53(Al) and NH2-MIL-101(Al). A thorough analysis of SAXS data reveals the most important

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

    Science.gov (United States)

    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°.

  12. Studies in small angle scattering techniques

    International Nuclear Information System (INIS)

    Moellenbach, K.

    1980-03-01

    Small angle scattering of neutrons, X-rays and γ-rays are found among the spectroscopic methods developed in the recent years. Although these techniques differ from each other in many respects, e.g. radiation sources and technical equipment needed, their power to resolve physical phenomena and areas of application can be discussed in a general scheme. Selected examples are given illustrating the use of specific technical methods. Jahn-Teller driven structural phase transitions in Rare Earth zircons were studied with neutron scattering as well as small angle γ-ray diffraction. The study of neutron scattering from formations of magnetic domains in the Ising ferromagnet LiTbF 4 is a second example. Both these examples represent more than experimental test cases since the theoretical interpretations of the data obtained are discussed as well. As a last example the use of small angle scattering methods for the study of molecular biological samples is discussed. In particular the experimental procedures used in connection with scattering from aqueous solutions of proteins and protein complexes are given. (Auth.)

  13. Assembly of positioner of automated two-dimensional scan coupled to X-ray fluorescence spectrometry; Montagem de posicionador de varredura bidimensional automatizada acoplado a espectrometria de fluorescência de raios-X

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Leonardo Santiago Melgaço

    2011-07-01

    This work describes the design and assembling of a prototype automated positioner two-dimensional scanning coupled to X-ray fluorescence spectrometry. The work aims to achieve a portable and easy to use, device of broad utility in the analysis of samples by X-ray fluorescence area of expertise and research. The two-dimensional scanning of the positioner is by means of two stepper motors controlled by a microcontroller PIC 16F877A, encoder and optical sensors. The user interacts with the XY table through an interface program for the Windows operating system, which communicates with the microcontroller through the serial port. The system of Fluorescence Spectroscopy incorporated into the positioner consists of a system commercially available system from the company AMPTEK, where the primary source of excitation of the sample was a source of {sup 241}Am of 59.5 KeV emissions. Resolution and accuracy of tests were performed in the XY scanning process and reproducibility of the same kit with the fluorescence spectrometry X-ray. Qualitative tests by X-ray fluorescence spectrometry in samples were performed to demonstrate the applicability and versatility of the project. It follows that the prototype illustrates a possible adequately to portable device for X-ray spectrometry of two-dimensional. (author)

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

    Science.gov (United States)

    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.

  15. Detection of small conformational changes of proteins by small-angle scattering

    International Nuclear Information System (INIS)

    Durchschlag, H.; Purr, G.; Zipper, P.; Wilfing, R.

    1991-01-01

    In the past the technique of small-angle scattering has been a powerful tool for studying conformational changes of protein which occur, for example, upon binding with ligands. Results obtained by different authors from X-ray and neutron experiments on a variety of proteins and under various conditions have been compiled. This offers the possibility of comparing the extent of changes in the molecular parameters investigated (e.g. change of the radius of gyration). Problems encountered with the detection of small changes are discussed. As an example, conformational changes of the enzyme citrate synthase upon substrate binding (oxaloacetate) are presented. X-ray crystallography had already found distinct changes between open and closed forms of the enzyme. Small-angle X-ray scattering studies registered slight changes of some parameters in solution. These changes could be paralleled with the results of other solution techniques (UV absorption, fluorescence and circular dichroism spectroscopy, analytical ultracentrifugation). The results found for citrate synthase are also compared with previous findings for malate synthase, an enzyme of similar enzymatic function. Above all, this study shows that care has to be taken when studying small conformational changes. It is absolutely necessary to use different methods and conditions and to study the problem from different points of view to avoid pitfalls. (orig.)

  16. DMSO-induced dehydration of DPPC membranes studied by x-ray diffraction, small angle neutron scattering and calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Kiselev, M A; Kiselev, A M [Frank Laboratory of Neutron Physics, Joint Institute for Nuclear Research, Dubna (Russian Federation); Lesieur, P [LURE, Universite Paris-Sud, Bat. 209-D, F91405 Orsay cedex, (France); Grabielle-Madelmond, C; Ollivon, M [Physico-Chimie des systemes polyphases, URA 1218 du CNRS, Faculte de Pharmacie, tour B, F-92296, Chatenay Malabry (France)

    1998-12-01

    The properties of dimethyl sulfoxide (DMSO), a cryoprotector well known for its biological and therapeutic applications, were investigated on lipid membranes by x-ray diffraction, differential scanning calorimetry (DSC) and small angle neutron scattering (SANS). The DSC study of water freezing and melting of ice was performed in the ternary system which consists of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC)/DMSO/water system. The influence of DMSO on the DPPC membrane structure was established in the excess of solvent in the region of DMSO mole fraction from 0.0 to 1.0. The methods applied demonstrated the differences in the membrane structure in three sub-regions of DMSO mole fraction (X{sub DMSO}) from 0.0 to 0.3 for the first, from 0.3 to 0.9 for the second, and from 0.9 to 1.0 for the third sub-region. The results for 0.0 {<=} X{sub DMSO} {<=} 0.3 can be explained in the framework of DMSO-induced dehydration of intermembrane space 11 refs., 7 figs. Submitted to the Conference `ISSRNS`98`, 15-20 Jun 1998, Ustron-Jaszowiec, Poland

  17. Repeated sorption of water in SBA-15 investigated by means of in situ small-angle x-ray scattering

    International Nuclear Information System (INIS)

    Erko, M; Paris, O; Wallacher, D; Findenegg, G H

    2012-01-01

    The effect of repeated cycles of water adsorption/desorption on the structural stability of ordered mesoporous silica SBA-15 is studied by small-angle x-ray scattering (SAXS). In situ sorption measurements are conducted using a custom-built sorption apparatus in connection with a laboratory SAXS setup. Two striking irreversible changes are observed in the sorption isotherms as derived from the integrated SAXS intensity. First, the capillary condensation pressure shifts progressively to lower relative pressure values with increasing number of sorption cycles. This effect is attributed to chemisorption of water at the silica walls, resulting in a change of the fluid-wall interaction. Second, the sorption cycles do not close completely at vanishing vapour pressure, suggesting that progressively more water remains trapped within the porous material after each cycle. This effect is interpreted to be the result of an irreversible collapse of parts of mesopores, originating from pore wall deformation due to the large Laplace pressure of water acting on the pore walls at capillary condensation and capillary evaporation. (paper)

  18. The development for small scale soft X-ray spectrometer

    International Nuclear Information System (INIS)

    Sun Kexu; Jiang Shaoen; Yi Rongqing; Cui Yanli

    2004-12-01

    For the development of small-scale soft X-ray spectrometer, first, some small-scale soft X-ray detection elements are developed, it is included GaAs irradiated with neutron, GaAs irradiated with proton, multi-layer mirror, plane mirror and small scale X-ray diode et al. Soft X-ray spectrometers built of multi-layer mirror-GaAs (with neutron irradiation), and plane mirror-small-scale XRD, and plane mirror-GaAs (with proton irradiation) are prepared. These spectrometers are examined in Shen Guang-II laser facility, and some external estimation are given. (authors)

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

    Science.gov (United States)

    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.

  20. X-ray fluorescence imaging with polycapillary X-ray optics

    International Nuclear Information System (INIS)

    Yonehara, Tasuku; Yamaguchi, Makoto; Tsuji, Kouichi

    2010-01-01

    X-ray fluorescence spectrometry imaging is a powerful tool to provide information about the chemical composition and elemental distribution of a specimen. X-ray fluorescence spectrometry images were conventionally obtained by using a μ-X-ray fluorescence spectrometry spectrometer, which requires scanning a sample. Faster X-ray fluorescence spectrometry imaging would be achieved by eliminating the process of sample scanning. Thus, we developed an X-ray fluorescence spectrometry imaging instrument without sample scanning by using polycapillary X-ray optics, which had energy filter characteristics caused by the energy dependence of the total reflection phenomenon. In the present paper, we show that two independent straight polycapillary X-ray optics could be used as an energy filter of X-rays for X-ray fluorescence. Only low energy X-rays were detected when the angle between the two optical axes was increased slightly. Energy-selective X-ray fluorescence spectrometry images with projection mode were taken by using an X-ray CCD camera equipped with two polycapillary optics. It was shown that Fe Kα (6.40 keV) and Cu Kα (8.04 keV) could be discriminated for Fe and Cu foils.

  1. Phase and Texture of Solution-Processed Copper Phthalocyanine Thin Films Investigated by Two-Dimensional Grazing Incidence X-Ray Diffraction

    Directory of Open Access Journals (Sweden)

    Lulu Deng

    2011-07-01

    Full Text Available The phase and texture of a newly developed solution-processed copper phthalocyanine (CuPc thin film have been investigated by two-dimensional grazing incidence X-ray diffraction. The results show that it has β phase crystalline structure, with crystallinity greater than 80%. The average size of the crystallites is found to be about 24 nm. There are two different arrangements of crystallites, with one dominating the diffraction pattern. Both of them have preferred orientation along the thin film normal. Based on the similarities to the vacuum deposited CuPc thin films, the new solution processing method is verified to offer a good alternative to vacuum process, for the fabrication of low cost small molecule based organic photovoltaics.

  2. Reliability of tunnel angle in ACL reconstruction: two-dimensional versus three-dimensional guide technique.

    Science.gov (United States)

    Leiter, Jeff R S; de Korompay, Nevin; Macdonald, Lindsey; McRae, Sheila; Froese, Warren; Macdonald, Peter B

    2011-08-01

    To compare the reliability of tibial tunnel position and angle produced with a standard ACL guide (two-dimensional guide) or Howell 65° Guide (three-dimensional guide) in the coronal and sagittal planes. In the sagittal plane, the dependent variables were the angle of the tibial tunnel relative to the tibial plateau and the position of the tibial tunnel with respect to the most posterior aspect of the tibia. In the coronal plane, the dependent variables were the angle of the tunnel with respect to the medial joint line of the tibia and the medial and lateral placement of the tibial tunnel relative to the most medial aspect of the tibia. The position and angle of the tibial tunnel in the coronal and sagittal planes were determined from anteroposterior and lateral radiographs, respectively, taken 2-6 months postoperatively. The two-dimensional and three-dimensional guide groups included 28 and 24 sets of radiographs, respectively. Tibial tunnel position was identified, and tunnel angle measurements were completed. Multiple investigators measured the position and angle of the tunnel 3 times, at least 7 days apart. The angle of the tibial tunnel in the coronal plane using a two-dimensional guide (61.3 ± 4.8°) was more horizontal (P guide (64.7 ± 6.2°). The position of the tibial tunnel in the sagittal plane was more anterior (P guide group compared to the three-dimensional guide group (43.3 ± 2.9%). The Howell Tibial Guide allows for reliable placement of the tibial tunnel in the coronal plane at an angle of 65°. Tibial tunnels were within the anatomical footprint of the ACL with either technique. Future studies should investigate the effects of tibial tunnel angle on knee function and patient quality of life. Case-control retrospective comparative study, Level III.

  3. Implementation of double-C-arm synchronous real-time X-ray positioning system computer aided for aspiration biopsy of small lung lesion

    International Nuclear Information System (INIS)

    Zhu Hong; Wang Dong; Ye Yukun; Zhou Yuan; Lu Jianfeng; Yang Jingyu; Wang Lining

    2007-01-01

    Objective: To evaluate the feasibility of a new type of real-time three-dimensional X-ray positioning system for aspiration biopsy of small lung lesions. Methods: Using X-ray imaging technology and X-ray collimator technology and combining with double-C-arm X-ray machine, two different synchronous real-time images were obtained from the vertical to the horizontal plane. Then, with the computer image processing and computer vision processing technologies, dynamic tracking for 3D information of a pulmonary lesion and the needle in aspiration, and the relative position of the two, were established. Results: There was no interference while the two imaging perpendicularly X-ray beam met, two synchronous real-time image acquisition and tracking of a lung lesion and a needle could be completed in free respiration. The average positioning system error was about 0.5 mm, the largest positioning error was about 1.0 mm, real-time display rate was 5 screen/sec. Conclusions: the establishment of a new type of double-C-arm synchronous real-time X-ray positioning system is feasible. It is available for the fast and accurate aspiration biopsy of small lung lesions. (authors)

  4. Collagen Orientation and Crystallite Size in Human Dentin: A Small Angle X-ray Scattering Study

    Energy Technology Data Exchange (ETDEWEB)

    Pople, John A

    2001-03-29

    The mechanical properties of dentin are largely determined by the intertubular dentin matrix, which is a complex composite of type I collagen fibers and a carbonate-rich apatite mineral phase. The authors perform a small angle x-ray scattering (SAXS) study on fully mineralized human dentin to quantify this fiber/mineral composite architecture from the nanoscopic through continuum length scales. The SAXS results were consistent with nucleation and growth of the apatite phase within periodic gaps in the collagen fibers. These mineralized fibers were perpendicular to the dentinal tubules and parallel with the mineralization growth front. Within the plane of the mineralization front, the mineralized collagen fibers were isotropic near the pulp, but became mildly anisotropic in the mid-dentin. Analysis of the data also indicated that near the pulp the mineral crystallites were approximately needle-like, and progressed to a more plate-like shape near the dentino-enamel junction. The thickness of these crystallites, {approx} 5 nm, did not vary significantly with position in the tooth. These results were considered within the context of dentinogenesis and maturation.

  5. A Grazing-Incidence Small-Angle X-Ray Scattering View of Vertically Aligned ZnO Nano wires

    International Nuclear Information System (INIS)

    Lavcevic, M.L.; Silovic, L.; Dubcek, P.; Pavlovic, M.; Bernstorff, S.

    2013-01-01

    We report a grazing-incidence small-angle X-ray scattering study of ZnO films with vertically aligned and randomly distributed nano wires, grown through a hydrothermal growth process on nano structured ZnO seeding coatings and deposited by electron beam evaporation on silicon and glass, respectively. The comparison of the scattering patterns of seeding coatings and nano wires showed that the scattering of vertically aligned nano wires exhibited a specific feature: the dominant characteristic of their scattering patterns is the appearance of fine structure effects around the specular peak. These effects were clarified by the combined reflection and scattering phenomena, suggested for the aligned nano wires-substrate system. Furthermore, they enabled the calculation of the average gyration radius of nano wires in horizontal direction. The calculated value was in good agreement with the radii of nano wires estimated by surface electron microscopy. Therefore, the observed feature in the scattering pattern can serve as evidence of the aligned growth of nano wires.

  6. Three-dimensional structure determination protocol for noncrystalline biomolecules using x-ray free-electron laser diffraction imaging.

    Science.gov (United States)

    Oroguchi, Tomotaka; Nakasako, Masayoshi

    2013-02-01

    Coherent and intense x-ray pulses generated by x-ray free-electron laser (XFEL) sources are paving the way for structural determination of noncrystalline biomolecules. However, due to the small scattering cross section of electrons for x rays, the available incident x-ray intensity of XFEL sources, which is currently in the range of 10(12)-10(13) photons/μm(2)/pulse, is lower than that necessary to perform single-molecule diffraction experiments for noncrystalline biomolecules even with the molecular masses of megadalton and submicrometer dimensions. Here, we propose an experimental protocol and analysis method for visualizing the structure of those biomolecules by the combined application of coherent x-ray diffraction imaging and three-dimensional reconstruction methods. To compensate the small scattering cross section of biomolecules, in our protocol, a thin vitreous ice plate containing several hundred biomolecules/μm(2) is used as sample, a setup similar to that utilized by single-molecule cryoelectron microscopy. The scattering cross section of such an ice plate is far larger than that of a single particle. The images of biomolecules contained within irradiated areas are then retrieved from each diffraction pattern, and finally provide the three-dimensional electron density model. A realistic atomic simulation using large-scale computations proposed that the three-dimensional structure determination of the 50S ribosomal subunit embedded in a vitreous ice plate is possible at a resolution of 0.8 nm when an x-ray beam of 10(16) photons/500×500 nm(2)/pulse is available.

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

    Energy Technology Data Exchange (ETDEWEB)

    Stanic, Vesna [Brazilian Synchrotron Light Source, Campinas (Brazil); Broadbent, Charlotte [Columbia Univ., New York, NY (United States). Engineering Dept.; DiMasi, Elaine [Brookhaven National Lab. (BNL), Upton, NY (United States). Photon Sciences Division; Galleguillos, Ramiro [Lubrizol Advanced Materials, Cleveland, OH (United States); Woodward, Valerie [Lubrizol Advanced Materials, Cleveland, OH (United States)

    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 data 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Marmiroli, Benedetta [Institute for Biophysics and Nanosystem Research, Austrian Academy of Science, Schmiedlstrasse 6, Graz (Austria); Grenci, Gianluca [TASC INFM/CNR, SS 14 km 163.5, Basovizza, TS (Italy); Cacho-Nerin, Fernando; Sartori, Barbara; Laggner, Peter [Institute for Biophysics and Nanosystem Research, Austrian Academy of Science, Schmiedlstrasse 6, Graz (Austria); Businaro, Luca [TASC INFM/CNR, SS 14 km 163.5, Basovizza, TS (Italy); Amenitsch, Heinz, E-mail: heinz.amenitsch@elettra.trieste.i [Institute for Biophysics and Nanosystem Research, Austrian Academy of Science, Schmiedlstrasse 6, Graz (Austria)

    2010-02-15

    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 mus time range. The microjet has a diameter of 25 mum and a time of first accessible measurement of 75 mus 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 mum. The proposed experimental procedures have been successfully employed to observe the formation of calcium carbonate (CaCO{sub 3}) nanoparticles from the reaction of sodium carbonate (Na{sub 2}CO{sub 3}) and calcium chloride (CaCl{sub 2}). The induction time has been estimated in the order of 200 mus and the determined radius of the particles is about 14 nm.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

    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.

  10. Small-angle x-ray scattering and density measurements of liquid Se50-Te50 mixture at high temperatures and high pressures using synchrotron radiation

    International Nuclear Information System (INIS)

    Kajihara, Y; Inui, M; Matsuda, K; Tomioka, Y

    2010-01-01

    We have carried out small-angle x-ray scattering and x-ray transmission measurements of liquid Se 50 -Te 50 mixture at SPring-8 in Japan and obtained the structure factor S(Q) at small-Q region (0.6 -1 ) and the density at high temperatures and high pressures up to 1000 0 C and 180 MPa. We report preliminary results in this paper. With increasing temperature, the density shows a minimum at around 500 0 C and a maximum at around 700 0 C. On the other hand, S(0) becomes maximum and S(Q) strongly depends on Q at around 600 0 C, which is about the middle temperature where the density shows the minimum and maximum. The temperatures shift to lower side when the pressure increases. These results prove that, with increasing temperature, the sample exhibits gradual transition from low-density structure to high-density structure, which causes mesoscopic density fluctuations in the intermediate temperature region.

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

    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.

  13. Small angle X-ray scattering from protein in solution

    International Nuclear Information System (INIS)

    Souza, C.F. de; Torriani, I.L.

    1988-01-01

    In this work we report experiments performed with giant respiratory proteins from annelids. X-ray scattering data were obtained both by the use of conventional rotating anod source and synchotron radiation. Data from solutions with several protein concentrations were analyzed. (A.C.A.S.) [pt

  14. Small-angle neutron scattering in materials science

    International Nuclear Information System (INIS)

    Fratzl, P.

    1999-01-01

    Small-angle scattering (SAS) in an ideal tool for studying the structure of materials in the mesoscopic size range between 1 and about 100 nanometers. The basic principles of the method are reviewed, with particular emphasis on data evaluation and interpretation for isotropic as well as oriented or single-crystalline materials. Examples include metal alloys, composites and porous materials. The last section gives a comparison between the use of neutrons and (synchrotron) x-rays for small-angle scattering in materials physics. (author)

  15. X-ray irradiation induced reduction and nanoclustering of lead in borosilicate glass

    NARCIS (Netherlands)

    Stanley, H.B.; Banerjee, D.; Breemen, van L.C.A.; Ciston, J.; Liebscher, C.H.; Martis, V.; Merino, D.H.; Longo, A.; Pattison, P.; Peters, G.W.M.; Portale, G.; Sen, Sabyasachi; Bras, W.

    2014-01-01

    We have studied the formation of nanoparticles in lead sulfide (PbS)-doped borosilicate glass subjected to a two-step nucleation and growth heat treatment using in situ small-angle X-ray scattering (SAXS). The microstructure produced was subsequently characterized using X-ray powder diffraction

  16. Small-angle X-Ray analysis of macromolecular structure: the structure of protein NS2 (NEP) in solution

    Science.gov (United States)

    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.

  17. Development of Scanning-Imaging X-Ray Microscope for Quantitative Three-Dimensional Phase Contrast Microimaging

    International Nuclear Information System (INIS)

    Takeuchi, Akihisa; Suzuki, Yoshio; Uesugi, Kentaro

    2013-01-01

    A novel x-ray microscope system has been developed for the purpose of quantitative and sensitive three-dimensional (3D) phase-contrast x-ray microimaging. The optical system is a hybrid that consists of a scanning microscope optics with a one-dimensional (1D) focusing (line-focusing) device and an imaging microscope optics with a 1D objective. These two optics are orthogonally arranged regarding their common optical axis. Each is used for forming each dimension of two-dimensional (2D) image. The same data acquisition process as that of the scanning microscope system enables quantitative and sensitive x-ray imaging such as phase contrast and absorption contrast. Because a 2D image is measured with only 1D translation scan, much shorter measurement time than that of conventional scanning optics has been realized. By combining a computed tomography (CT) technique, some 3D CT application examples are demonstrated

  18. Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector.

    Science.gov (United States)

    Abboud, A; Kirchlechner, C; Keckes, J; Conka Nurdan, T; Send, S; Micha, J S; Ulrich, O; Hartmann, R; Strüder, L; Pietsch, U

    2017-06-01

    The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

  19. Dynamic angle selection in X-ray computed tomography

    Energy Technology Data Exchange (ETDEWEB)

    Dabravolski, Andrei, E-mail: andrei.dabravolski@uantwerpen.be [iMinds-Vision Lab, University of Antwerp, Universiteitsplein 1, 2610 Wilrijk (Belgium); Batenburg, Kees Joost, E-mail: joost.batenburg@uantwerpen.be [iMinds-Vision Lab, University of Antwerp, Universiteitsplein 1, 2610 Wilrijk (Belgium); Centrum Wiskunde and Informatica (CWI), Science Park 123, 1098 XG Amsterdam (Netherlands); Sijbers, Jan, E-mail: jan.sijbers@uantwerpen.be [iMinds-Vision Lab, University of Antwerp, Universiteitsplein 1, 2610 Wilrijk (Belgium)

    2014-04-01

    Highlights: • We propose the dynamic angle selection algorithm for CT scanning. • The approach is based on the concept of information gain over a set of solutions. • Projection angles are selected based on the already available projection data. • The approach can lead to more accurate results from fewer projections. - Abstract: In X-ray tomography, a number of radiographs (projections) are recorded from which a tomogram is then reconstructed. Conventionally, these projections are acquired equiangularly, resulting in an unbiased sampling of the Radon space. However, especially in case when only a limited number of projections can be acquired, the selection of the angles has a large impact on the quality of the reconstructed image. In this paper, a dynamic algorithm is proposed, in which new projection angles are selected by maximizing the information gain about the object, given the set of possible new angles. Experiments show that this approach can select projection angles for which the accuracy of the reconstructed image is significantly higher compared to the standard angle selections schemes.

  20. Dynamic angle selection in X-ray computed tomography

    International Nuclear Information System (INIS)

    Dabravolski, Andrei; Batenburg, Kees Joost; Sijbers, Jan

    2014-01-01

    Highlights: • We propose the dynamic angle selection algorithm for CT scanning. • The approach is based on the concept of information gain over a set of solutions. • Projection angles are selected based on the already available projection data. • The approach can lead to more accurate results from fewer projections. - Abstract: In X-ray tomography, a number of radiographs (projections) are recorded from which a tomogram is then reconstructed. Conventionally, these projections are acquired equiangularly, resulting in an unbiased sampling of the Radon space. However, especially in case when only a limited number of projections can be acquired, the selection of the angles has a large impact on the quality of the reconstructed image. In this paper, a dynamic algorithm is proposed, in which new projection angles are selected by maximizing the information gain about the object, given the set of possible new angles. Experiments show that this approach can select projection angles for which the accuracy of the reconstructed image is significantly higher compared to the standard angle selections schemes

  1. Small-angle X-ray scattering studies on the X-ray induced aggregation of ribonnuclease, lactate dehydrogenase, glyceraldehyde-3-phosphate dehydrogenase and serum albumin. A comparison with malate synthase

    International Nuclear Information System (INIS)

    Zipper, P.; Gatterer, H.G.; Schutz, J.; Durchschlag, H.

    1980-01-01

    The X-ray induced aggregation of ribonuclease, lactate dehydrogenase (LDH), glyceraldehyde-3-phosphate dehydrogenase (GAPDH) and serum albumin in aqueous solution was monitored in situ by means of small-angle X-ray scattering. Measurements carried out with ribonuclease, LDH and serum albumin in the absence of dithiothreitol (DTT) and with GAPDH in the presence of 0.2mM DTT established the following series for the rates of aggregation of the proteins under these conditions: ribonuclease >LDH> >GAPDH> serum albumin. Within six hours from the beginning of irradiation (i.e. about the time required for the exposure of one complete scattering curve under the conditions of our experiments) the following increases of R tilde resulted: ribonuclease 9%, LDH 7%, GAPDH 4%, serum albumin <1%. Changes of R tilde exceeding 1% are, of course, too high to be tolerated in conventional scattering experiments. Measurements carried out with LDH and GAPDH in the presence of 2mM DTT established a strong protective effect of DTT against the X-ray induced aggregation of these enzymes. The initial increase of R tilde upon irradiation of LDH and GAPDH in the presence of 2mM DTT was found to be even lower than the increase of R tilde observed when serum albumin was irradiated in the absence of DTT. However, the observed decrease of anti x of LDH and GAPDH at the early stages of irradiation suggested the occurrence of fragmentation of the enzymes as another consequence of radiation damage. This finding is discussed in context with the results from previous scattering experiments and electrophoretic studies on malate synthase. (author)

  2. Wide field X-ray telescopes: Detecting X-ray transients/afterglows related to gamma ray bursts

    International Nuclear Information System (INIS)

    Hudec, Rene; Pina, Ladislav; Inneman, Adolf; Gorenstein, Paul; Rezek, Tomas

    1999-01-01

    The recent discovery of X-ray afterglows of GRBs opens the possibility of analyses of GRBs by their X-ray detections. However, imaging X-ray telescopes in current use mostly have limited field of view. Alternative X-ray optics geometries achieving very large fields of view have been theoretically suggested in the 70ies but not constructed and used so far. We review the geometries and basic properties of the wide-field X-ray optical systems based on one- and two-dimensional lobster-eye geometry and suggest technologies for their development and construction. First results of the development of double replicated X-ray reflecting flats for use in one-dimensional X-ray optics of lobster eye type are presented and discussed. Optimum strategy for locating GRBs upon their X-ray counterparts is also presented and discussed

  3. Small angle X-ray scattering by TiO2/ZrO2 mixed oxide particles and a Synroc precursor

    International Nuclear Information System (INIS)

    Gazeau, D.; Zemb, T.; Amal, R.; Bartlett, J.

    1992-09-01

    This high resolution small angle X-ray scattering study of a concentrated oxide sol, precursor of the SYNROC matrix for the storage of the high level radioactive waste, evidences a locally cylindrical microstructure. Locally, nanometric cylinders show disordered axis with some concentration dependent connections. This microstructure explains the paradoxal stability of this oxide dispersions upon the addition of concentrated acidic solutions. This stability has a steric origin and electrostatic repulsions are not needed. The addition of aluminium to the initial titanium-zirconium mixture enhances branching on the locally cylindrical microstructure. Finally, we show that the solid powder obtained after calcination (drying) of the sol has the same specific area (∼ 1000 m 2 /g) than the sol. (Author). 23 refs., 7 figs., 1 tab

  4. Azimuthal and polar angle dependence of L X-ray differential cross-sections of Yb at 59.54 keV photon energy

    Energy Technology Data Exchange (ETDEWEB)

    Akkuş, T.; Şahin, Y.; Yılmaz, D., E-mail: ddemir@atauni.edu.tr

    2016-01-01

    Highlights: • The azimuthal and polar angle dependence of L X-ray for Yb is investigated. • The azimuthal angle dependence of Ll and Lα X-rays are observed. • The azimuthal anisotropy of Lβ and Lγ X-rays are not observed. • The polar anisotropy of Ll and Lα X-rays are observed. • The polar anisotropy of Lβ and Lγ X-rays are not observed. - Abstract: The azimuthal and polar angle dependence of L X-ray was investigated in the same experimental setup to remove the existing ambiguity about alignments measurements. We measured Ll, Lα, Lβ and Lγ X-ray differential cross sections of Yb for several different azimuthal angles (30°, 20°, 10°, 0°, −10° and −20°) and polar angles (90°, 100°, 110°, 120°, 130° and 140°) at 59.54 keV photon energy by using a Si(Li) detector. The azimuthal angle dependence of Ll and Lα X-rays were observed. The azimuthal anisotropy of Lβ and Lγ X-rays were not observed. On the other hand, differential cross-sections for Lβ and Lγ X-rays were found independent on the polar angle within experimental error, those for Ll and Lα X-rays depended on the polar angles. Azimuthal and polar angles dependence of L X-ray differential cross-sections contrast with the other experimental and theoretical results, which report evidence of the isotropic emission of Ll and Lα X-rays following photoionization.

  5. Evaluation of stress gradient by x-ray stress measurement based on change in angle phi

    International Nuclear Information System (INIS)

    Sasaki, Toshihiko; Kuramoto, Makoto; Yoshioka, Yasuo.

    1985-01-01

    A new principle of X-ray stress evaluation for a sample with steep stress gradient has been prosed. The feature of this method is that the stress is determined by using so-called phi-method based on the change of phi-angle and thus has no effect on the penetration depth of X-rays. The procedure is as follows; firstly, an average stress within the penetration depth of X-rays is determined by changing only phi-angle under a fixed psi-angle, and then a distribution of the average stress vs. the penetration depth of X-rays is detected by repeating the similar procedure at different psi-angles. The following conclusions were found out as the result of residual stress measurements on a carbon steel of type S 55 C polished by emery paper. This method is practical enough to use for a plane stress problem. And the assumption of a linear stress gradient adopted in the authors' previous investigations is valid. In case of a triaxial stress analysis, this method is effective for the solution of three shearing stresses. However, three normal stresses can not be solved perfectly except particular psi-angles. (author)

  6. Two-axis Neutron and X-ray Reflectivity

    DEFF Research Database (Denmark)

    Bouwman, W.G.; Vigild, M.E.; Findeisen, E.

    1997-01-01

    Sample alignment for neutron (and in some cases x-ray) reflectometry can be complicated due to a coupling between angle and position which occurs when slits are used to define the path of the beam. Misalignments in sample position or sample rotation angle give rise to systematic errors in the exp...

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

    Science.gov (United States)

    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.

  8. Small Pixel Hybrid CMOS X-ray Detectors

    Science.gov (United States)

    Hull, Samuel; Bray, Evan; Burrows, David N.; Chattopadhyay, Tanmoy; Falcone, Abraham; Kern, Matthew; McQuaide, Maria; Wages, Mitchell

    2018-01-01

    Concepts for future space-based X-ray observatories call for a large effective area and high angular resolution instrument to enable precision X-ray astronomy at high redshift and low luminosity. Hybrid CMOS detectors are well suited for such high throughput instruments, and the Penn State X-ray detector lab, in collaboration with Teledyne Imaging Sensors, has recently developed new small pixel hybrid CMOS X-ray detectors. These prototype 128x128 pixel devices have 12.5 micron pixel pitch, 200 micron fully depleted depth, and include crosstalk eliminating CTIA amplifiers and in-pixel correlated double sampling (CDS) capability. We report on characteristics of these new detectors, including the best read noise ever measured for an X-ray hybrid CMOS detector, 5.67 e- (RMS).

  9. Topological investigation of electronic silicon nanoparticulate aggregates using ultra-small-angle X-ray scattering

    CSIR Research Space (South Africa)

    Jonah, EO

    2012-10-01

    Full Text Available The network topology of two types of silicon nanoparticles, produced by high energy milling and pyrolysis of silane, in layers deposited from inks on permeable and impermeable substrates has been quantitatively characterized using ultra-small-angle...

  10. Nano-Structural Investigation on Cellulose Highly Dissolved in Ionic Liquid: A Small Angle X-ray Scattering Study

    Directory of Open Access Journals (Sweden)

    Takatsugu Endo

    2017-01-01

    Full Text Available We investigated nano-structural changes of cellulose dissolved in 1-ethyl-3-methylimidazolium acetate—an ionic liquid (IL—using a small angle X-ray scattering (SAXS technique over the entire concentration range (0–100 mol %. Fibril structures of cellulose disappeared at 40 mol % of cellulose, which is a significantly higher concentration than the maximum concentration of dissolution (24–28 mol % previously determined in this IL. This behavior is explained by the presence of the anion bridging, whereby an anion prefers to interact with multiple OH groups of different cellulose molecules at high concentrations, discovered in our recent work. Furthermore, we observed the emergence of two aggregated nano-structures in the concentration range of 30–80 mol %. The diameter of one structure was 12–20 nm, dependent on concentration, which is ascribed to cellulose chain entanglement. In contrast, the other with 4.1 nm diameter exhibited concentration independence and is reminiscent of a cellulose microfibril, reflecting the occurrence of nanofibrillation. These results contribute to an understanding of the dissolution mechanism of cellulose in ILs. Finally, we unexpectedly proposed a novel cellulose/IL composite: the cellulose/IL mixtures of 30–50 mol % that possess liquid crystallinity are sufficiently hard to be moldable.

  11. Ultra-small-angle X-ray scattering characterization of diesel/gasoline soot: sizes and particle-packing conditions

    Science.gov (United States)

    Kameya, Yuki; Lee, Kyeong O.

    2013-10-01

    Regulations on particulate emissions from internal combustion engines tend to become more stringent, accordingly the importance of particulate filters in the after-treatment system has been increasing. In this work, the applicability of ultra-small-angle X-ray scattering (USAXS) to diesel soot cake and gasoline soot was investigated. Gasoline-direct-injection engine soot was collected at different fuel injection timings. The unified fits method was applied to analyze the resultant scattering curves. The validity of analysis was supported by comparing with carbon black and taking the sample images using a transmission electron microscope, which revealed that the primary particle size ranged from 20 to 55 nm. In addition, the effects of particle-packing conditions on the USAXS measurement were demonstrated by using samples suspended in acetone. Then, the investigation was extended to characterization of diesel soot cake deposited on a diesel particulate filter (DPF). Diesel soot was trapped on a small piece of DPF at different deposition conditions which were specified using the Peclet number. The dependence of scattering curve on soot-deposition conditions was demonstrated. To support the interpretation of the USAXS results, soot cake samples were observed using a scanning electron microscope and the influence of particle-packing conditions on scattering curve was discussed.

  12. Ultra-small-angle X-ray scattering characterization of diesel/gasoline soot: sizes and particle-packing conditions

    International Nuclear Information System (INIS)

    Kameya, Yuki; Lee, Kyeong O.

    2013-01-01

    Regulations on particulate emissions from internal combustion engines tend to become more stringent, accordingly the importance of particulate filters in the after-treatment system has been increasing. In this work, the applicability of ultra-small-angle X-ray scattering (USAXS) to diesel soot cake and gasoline soot was investigated. Gasoline-direct-injection engine soot was collected at different fuel injection timings. The unified fits method was applied to analyze the resultant scattering curves. The validity of analysis was supported by comparing with carbon black and taking the sample images using a transmission electron microscope, which revealed that the primary particle size ranged from 20 to 55 nm. In addition, the effects of particle-packing conditions on the USAXS measurement were demonstrated by using samples suspended in acetone. Then, the investigation was extended to characterization of diesel soot cake deposited on a diesel particulate filter (DPF). Diesel soot was trapped on a small piece of DPF at different deposition conditions which were specified using the Peclet number. The dependence of scattering curve on soot-deposition conditions was demonstrated. To support the interpretation of the USAXS results, soot cake samples were observed using a scanning electron microscope and the influence of particle-packing conditions on scattering curve was discussed

  13. Ultra-small-angle X-ray scattering characterization of diesel/gasoline soot: sizes and particle-packing conditions

    Energy Technology Data Exchange (ETDEWEB)

    Kameya, Yuki, E-mail: ykameya@anl.gov; Lee, Kyeong O. [Argonne National Laboratory, Center for Transportation Research (United States)

    2013-10-15

    Regulations on particulate emissions from internal combustion engines tend to become more stringent, accordingly the importance of particulate filters in the after-treatment system has been increasing. In this work, the applicability of ultra-small-angle X-ray scattering (USAXS) to diesel soot cake and gasoline soot was investigated. Gasoline-direct-injection engine soot was collected at different fuel injection timings. The unified fits method was applied to analyze the resultant scattering curves. The validity of analysis was supported by comparing with carbon black and taking the sample images using a transmission electron microscope, which revealed that the primary particle size ranged from 20 to 55 nm. In addition, the effects of particle-packing conditions on the USAXS measurement were demonstrated by using samples suspended in acetone. Then, the investigation was extended to characterization of diesel soot cake deposited on a diesel particulate filter (DPF). Diesel soot was trapped on a small piece of DPF at different deposition conditions which were specified using the Peclet number. The dependence of scattering curve on soot-deposition conditions was demonstrated. To support the interpretation of the USAXS results, soot cake samples were observed using a scanning electron microscope and the influence of particle-packing conditions on scattering curve was discussed.

  14. Introducing a standard method for experimental determination of the solvent response in laser pump, x-ray probe time-resolved wide-angle x-ray scattering experiments on systems in solution

    DEFF Research Database (Denmark)

    Kjær, Kasper Skov; Brandt van Driel, Tim; Kehres, Jan

    2013-01-01

    In time-resolved laser pump, X-ray probe wide-angle X-ray scattering experiments on systems in solution the structural response of the system is accompanied by a solvent response. The solvent response is caused by reorganization of the bulk solvent following the laser pump event, and in order...... response-the solvent term-experimentally when applying laser pump, X-ray probe time-resolved wide-angle X-ray scattering. The solvent term describes difference scattering arising from the structural response of the solvent to changes in the hydrodynamic parameters: pressure, temperature and density. We...... is demonstrated to exhibit first order behaviour with respect to the amount of energy deposited in the solution. We introduce a standardized method for recording solvent responses in laser pump, X-ray probe time-resolved X-ray wide-angle scattering experiments by using dye mediated solvent heating. Furthermore...

  15. Characterization of a confocal three-dimensional micro X-ray fluorescence facility based on polycapillary X-ray optics and Kirkpatrick-Baez mirrors

    International Nuclear Information System (INIS)

    Sun Tianxi; Ding Xunliang; Liu Zhiguo; Zhu Guanghua; Li Yude; Wei Xiangjun; Chen Dongliang; Xu Qing; Liu Quanru; Huang Yuying; Lin Xiaoyan; Sun Hongbo

    2008-01-01

    A new confocal three-dimensional micro X-ray fluorescence (3D micro-XRF) facility based on polycapillary X-ray optics in the detection channel and Kirkpatrick-Baez (KB) mirrors in the excitation channel is designed. The lateral resolution (l x , l y ) of this confocal three-dimensional micro-X-ray fluorescence facility is 76.3(l x ) and 53.4(l y ) μm respectively, and its depth resolution d z is 77.1 μm at θ = 90 o . A plant sample (twig of B. microphylla) and airborne particles are analyzed

  16. Structure of Nanoporous Biocarbon for Hydrogen Storage as Determined by Small Angle X-Ray Scattering

    Science.gov (United States)

    Wood, Mikael; Burress, J.; Pobst, J.; Carter, S.; Pfeifer, P.; Wexler, C.; Shah, P.; Suppes, G.

    2008-03-01

    As a member of the Alliance for Collaborative Research in Alternative Fuel Technology (ALL-CRAFT) our research group studies the properties of nanoporous biocarbon, produced from waste corn cob, with the goal of achieving the Department of Energy's gravimetric and volumetric standards for both hydrogen and methane gas storage. Small Angle X-Ray Scattering (SAXS) is a valuable tool in our investigation of the geometry of the pore space in our carbon samples. In this talk, we will compare the experimental SAXS data with theoretical results for various pore geometries to determine which pore models are consistent with experiment. Using data from nitrogen adsorption isotherms, along with SAXS, yields significant structural information about the pore space. This analysis should allow us to fully optimize our production process and to achieve the DOE's target storage capacities. This work supported by: 1. National Science Foundation (PFI-0438469) 2. U.S. Department of Education (P200A040038) 3. U.S. Department of Energy (DE-AC02-06CH11357) 4. University of Missouri (RB-06-040) 5. U.S. Department of Defense (N00164-07-P-1306) 6. U.S. Department of Energy (DE-FG02-07ER46411)

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

    Science.gov (United States)

    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.

  18. Lobster eye X-ray optics: Data processing from two 1D modules

    Science.gov (United States)

    Nentvich, O.; Urban, M.; Stehlikova, V.; Sieger, L.; Hudec, R.

    2017-07-01

    The X-ray imaging is usually done by Wolter I telescopes. They are suitable for imaging of a small part of the sky, not for all-sky monitoring. This monitoring could be done by a Lobster eye optics which can theoretically have a field of view up to 360 deg. All sky monitoring system enables a quick identification of source and its direction. This paper describes the possibility of using two independent one-dimensional Lobster Eye modules for this purpose instead of Wolter I and their post-processing into an 2D image. This arrangement allows scanning with less energy loss compared to Wolter I or two-dimensional Lobster Eye optics. It is most suitable especially for very weak sources.

  19. Characterization of structure and coagulation behaviour of refractory organic substances (ROS) using small-angle neutron scattering (SANS), small-angle x-ray scattering (SAXS) and x-ray microscopy; Charakterisierung von Struktur und Koagulationsverhalten von Refraktaeren Organischen Saeuren (ROS) mit Hilfe von Neutronenkleinwinkelstreuung (SANS), Roentgenkleinwinkelstreuung (SAXS) und Roentgenmikroskopie

    Energy Technology Data Exchange (ETDEWEB)

    Pranzas, P.K. [GKSS-Forschungszentrum Geesthacht GmbH (Germany). Inst. fuer Werkstofforschung

    1999-07-01

    In this work structure, coagulation and complexation behaviour of aquatic refractory organic substances (ROS) (humic and fulvic acids) were characterized. For this purpose a structural analytical system with the methods small-angle neutron scattering (SANS), small-angle x-ray scattering (SAXS) and X-ray microscopy with synchrotron radiation was developed and established. Size distributions of ROS of different origin were calculated from the scattering curves. Spherical ROS units were obtained, which coagulated by forming chainlike structures or disordered ROS agglomerates at higher concentrations. Additionally the average molecular weights of several ROS were calculated. Studies of the coagulation behaviour of ROS towards copper ions resulted in larger ROS-agglomerates besides the spherical ROS units. A linear relation between the addition of Cu{sup 2+} and the formation of the ROS-Cu{sup 2+}-agglomerates was found. With X-ray microscopy an extensive ROS-Cu{sup 2}-network structure could be registrated. For mercury and cadmium ions such coagulation interactions were not found. Investigations with X-ray microscopy of the coagulation behaviour of ROS towards the cationic surfactant DTB resulted in micel-like structures of equal size, which were spread throughout the solution. With increasing concentrations of DTB larger agglomerates up to network structures were obtained. (orig.) [German] In dieser Arbeit wurden Struktur, Koagulations- und Komplexierungsverhalten von aquatischen refraktaeren organischen Saeuren (ROS) (Humin- und Fulvinsaeuren) charakterisiert. Zu diesem Zweck wurde ein strukturanalytisches Gesamtsystem mit den Methoden Neutronenkleinwinkelstreuung (SANS), Roentgenkleinwinkelstreuung (SAXS) und Roentgenmikroskopie mit Synchrotronstrahlung entwickelt und etabliert. Fuer ROS unterschiedlicher Herkunft in Loesung wurden Groessenverteilungen aus den Streukurven berechnet. Es wurden kugelfoermige ROS-Einheiten gefunden, die bei hoeheren ROS

  20. Computer simulation for the effect of target angle in diagnostic x-ray tube output and half-value layer

    International Nuclear Information System (INIS)

    Hayami, Akimune; Fuchihata, Hajime; Yamazaki, Takeshi; Mori, Yoshinobu; Ozeki, Syuji.

    1980-01-01

    The change of target angle of X-ray tube plays an important role in changing both the output and the quality of X-rays. A computer simulation was made to estimate the effect of target angle on the output and the quality (half-value layer: HVL) in the central ray using Storm's semiempirical formula. The data here presented are the values of output and HVL for the target angles of 10, 15, 20 and 30 degrees and for the total filtrations of 1, 2, 3 and 4 mm Al eq., at an increment of 10 kV steps of applied voltage between 50 and 150 kV. The output values and HVL's as a function of target angle, applied voltage and total filtration are shown for a full-wave rectified diagnostic X-ray generator. As a result, changes ranging from 17 to 76% in the output and 5 to 66% in the HVL were noted by varying the target angle from 10 to 30 degrees. Therefore, the target angle of X-ray tube should be clearly stated whenever the output and the quality (HVL) of X-ray generator are discussed. (author)

  1. Characterization of X-ray Lobster Optics with a Hybrid CMOS sensor

    Science.gov (United States)

    Chattopadhyay, Tanmoy; Falcone, Abraham; Burrows, David N.; Bray, Evan; McQuaide, Maria; Kern, Matthew; Wages, Mitchell; Hull, Samuel; Inneman, Adolf; Hudec, Rene; Stehlikova, Veronika

    2018-01-01

    X-ray lobster optics provide a unique way to focus X-rays onto a small focal plane imager with wide field of view imaging. Such an instrument with angular resolution of a few arcminutes can be used to study GRB afterglows, as well as the variability and spectroscopic characteristics for various astrophysical objects. At Penn State University, we have characterized a lobster optic with an H1RG X-Ray hybrid CMOS detector (100 μm thick Silicon with 18 μm pixel size). The light-weight compact lobster optic with a 25 cm focal length provides two dimensional imaging with ~25 cm2 effective area at 2 keV. We utilize a 47 meter long X-ray beam line at Penn state University to do our experiments where we characterize the overall effective area of the instrument at 1.5 - 8 keV for both on-axis and off-axis angles. In this presentation, we will describe the characterization test stand and methods, as well as the detailed results. While this is simply a proof-of-concept experiment, such an instrument with significant collecting area can be explored for future rocket or CubeSat experiments.

  2. Modeling small angle scattering data using FISH

    International Nuclear Information System (INIS)

    Elliott, T.; Buckely, C.E.

    2002-01-01

    Full text: Small angle neutron scattering (SANS) and small angle x-ray scattering (SAXS) are important techniques for the characterisation of samples on the nanometer scale. From the scattered intensity pattern information about the sample such as particle size distribution, concentration and particle interaction can be determined. Since the experimental data is in reciprocal space and information is needed about real space, modeling of the scattering data to obtain parameters is extremely important and several paradigms are available. The use of computer programs to analyze the data is imperative for a robust description of the sample to be obtained. This presentation gives an overview of the SAS process and describes the data-modeling program FISH, written by R. Heenan 1983-2000. The results of using FISH to obtain the particle size distribution of bubbles in the aluminum hydrogen system and other systems of interest are described. Copyright (2002) Australian X-ray Analytical Association Inc

  3. The three dimensional X-ray diffraction technique

    DEFF Research Database (Denmark)

    Juul Jensen, Dorte; Poulsen, Henning Friis

    2012-01-01

    This introductory tutorial describes the so called 3 dimensional X-ray diffraction (3DXRD) technique, which allows bulk non-destructive structural characterizations of crystalline materials. The motivations and history behind the development of this technique are described and its potentials...

  4. 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.

    Science.gov (United States)

    Saranathan, Vinodkumar; Forster, Jason D; Noh, Heeso; Liew, Seng-Fatt; Mochrie, Simon G J; Cao, Hui; Dufresne, Eric R; Prum, Richard O

    2012-10-07

    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.

  5. Understanding nucleic acid structural changes by comparing wide-angle x-ray scattering (WAXS) experiments to molecular dynamics simulations

    Energy Technology Data Exchange (ETDEWEB)

    Pabit, Suzette A.; Katz, Andrea M.; Pollack, Lois [School of Applied and Engineering Physics, Cornell University, Ithaca, New York 14853 (United States); Tolokh, Igor S. [Department of Computer Science, Virginia Tech, Blacksburg, Virginia 24061 (United States); Drozdetski, Aleksander [Department of Physics, Virginia Tech, Blacksburg, Virginia 24061 (United States); Baker, Nathan [Pacific Northwest National Laboratory, Richland, Washington 99352 (United States); Onufriev, Alexey V. [Department of Computer Science, Virginia Tech, Blacksburg, Virginia 24061 (United States); Department of Physics, Virginia Tech, Blacksburg, Virginia 24061 (United States)

    2016-05-28

    Wide-angle x-ray scattering (WAXS) is emerging as a powerful tool for increasing the resolution of solution structure measurements of biomolecules. Compared to its better known complement, small angle x-ray scattering (SAXS), WAXS targets higher scattering angles and can enhance structural studies of molecules by accessing finer details of solution structures. Although the extension from SAXS to WAXS is easy to implement experimentally, the computational tools required to fully harness the power of WAXS are still under development. Currently, WAXS is employed to study structural changes and ligand binding in proteins; however, the methods are not as fully developed for nucleic acids. Here, we show how WAXS can qualitatively characterize nucleic acid structures as well as the small but significant structural changes driven by the addition of multivalent ions. We show the potential of WAXS to test all-atom molecular dynamics (MD) simulations and to provide insight into understanding how the trivalent ion cobalt(III) hexammine (CoHex) affects the structure of RNA and DNA helices. We find that MD simulations capture the RNA structural change that occurs due to addition of CoHex.

  6. Evidence of relationships between texture and structure in smectite systems by small angle synchrotron X ray scattering

    International Nuclear Information System (INIS)

    Pons, Charles-Henri

    1980-01-01

    Phyllosilicates are major constituents of soils, and their partially swelled or dispersed states play an important role in sedimentary geology, in soil science, in biochemistry, and also in various technological applications (drilling sludge, oil synthesis catalysts). Properties of these systems are also in direct relationship with problems such as fixation of pollutants by soil (pesticides, heavy metals, radioactive materials, so on). After having recalled works performed during the past forty years on water-smectite dispersions to define prevailing factors of processes of formation of colloidal states, the author presents the different phyllosilicates which have been studied, and recalls the determining factors of inflation and dispersion mechanisms. Then, he recalls methods of interpretation of X diffraction diagrams and of small angle scattering. He reports the detailed study of the inflation mechanism in the case of montmorillonite- Na, and discusses results obtained with other phyllosilicates or with other cations than sodium. In appendix, the author reports the study of bi-ionic (Na-Ca) montmorillonite suspensions prepared by two different methods. He also discusses the method of interpretation of neutron small angle scattering which had been used on similar systems, and shows why this method leads to questionable conclusions

  7. PILATUS: a two-dimensional X-ray detector for macromolecular crystallography

    CERN Document Server

    Eikenberry, E F; Huelsen, G; Toyokawa, H; Horisberger, R P; Schmitt, B; Schulze-Briese, C; Tomizaki, T

    2003-01-01

    A large quantum-limited area X-ray detector for protein crystallography is under development at the Swiss Light Source. The final detector will be 2kx2k pixels covering 40x40 cm sup 2. A three-module prototype with 1120x157 pixels covering an active area of 24.3x3.4 cm sup 2 has been tested. X-rays above 6 keV with peak count rates exceeding 5x10 sup 5 X-ray/pixel/s could be detected in single photon counting mode. Statistics of module production and results of threshold trimming are presented. To demonstrate the potential of this new detector, protein crystal data were collected at beamline 6S of the SLS.

  8. Wide field x-ray telescopes: Detecting x-ray transients/afterglows related to GRBs

    International Nuclear Information System (INIS)

    Hudec, Rene; Pina, Ladislav; Inneman, Adolf; Gorenstein, Paul

    1998-01-01

    The recent discovery of X-ray afterglows of GRBs opens the possibility of analyses of GRBs by their X-ray detections. However, imaging X-ray telescopes in current use mostly have limited fields of view. Alternative X-ray optics geometries achieving very large fields of view have been theoretically suggested in the 70's but not constructed and used so far. We review the geometries and basic properties of the wide-field X-ray optical systems based on one- and two-dimensional lobster-eye geometry and suggest technologies for their development and construction. First results of the development of double replicated X-ray reflecting flats for use in one-dimensional X-ray optics of lobster-eye type are presented and discussed. The optimum strategy for locating GRBs upon their X-ray counterparts is also presented and discussed

  9. Studies on micro-domain structure in segmented polyether polyurethane-ureas by positron annihilation lifetime and small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Yin Chuanyuan; Gu Qingchao

    1997-01-01

    The micro-domain structure of segmented polyether polyurethane-ureas is investigated by means of positron annihilation lifetime spectroscopy, small-angle X-ray scattering and differential scanning calorimetry. The experimental results show that the decrease in the domain volume and free volume results from the increase in the hard segment (polyurethane-urea segment) contents as the number-average molecular weight M n -bar of the soft segments (polyethylene glycol segments) is the same, and that the increase in domain volume and free volume result from the increase in the M n -bar of the soft segments when the hard segment content is the same or nearly the same. These results demonstrate that positron annihilation lifetime spectroscopy is a sensitive technique to probe the micro-domain structure in polymers

  10. Three-dimensional reconstruction of the giant mimivirus particle with an x-ray free-electron laser.

    Science.gov (United States)

    Ekeberg, Tomas; Svenda, Martin; Abergel, Chantal; Maia, Filipe R N C; Seltzer, Virginie; Claverie, Jean-Michel; Hantke, Max; Jönsson, Olof; Nettelblad, Carl; van der Schot, Gijs; Liang, Mengning; DePonte, Daniel P; Barty, Anton; Seibert, M Marvin; Iwan, Bianca; Andersson, Inger; Loh, N Duane; Martin, Andrew V; Chapman, Henry; Bostedt, Christoph; Bozek, John D; Ferguson, Ken R; Krzywinski, Jacek; Epp, Sascha W; Rolles, Daniel; Rudenko, Artem; Hartmann, Robert; Kimmel, Nils; Hajdu, Janos

    2015-03-06

    We present a proof-of-concept three-dimensional reconstruction of the giant mimivirus particle from experimentally measured diffraction patterns from an x-ray free-electron laser. Three-dimensional imaging requires the assembly of many two-dimensional patterns into an internally consistent Fourier volume. Since each particle is randomly oriented when exposed to the x-ray pulse, relative orientations have to be retrieved from the diffraction data alone. We achieve this with a modified version of the expand, maximize and compress algorithm and validate our result using new methods.

  11. Magnetic nanoparticles studied by small angle X-ray scattering

    International Nuclear Information System (INIS)

    Oliveira, Cristiano Luis Pinto; Antonel, Soledad; Negri, Martin

    2011-01-01

    because they exhibit magnetic (ferromagnetic) and electrical properties in the same material. Then, the nickel nanoparticles could be used for the development of electroelastic materials. In this case, the electrical conductivity of the material can be strongly dependent on the applied magnetic field, for example the case of nickel metal nanoparticles dispersed in a polymer, resulting in an anisotropic material with combined piezomagnetic and piezoelectric properties. In order to investigate the structural characteristics of cobalt-iron oxides and nickel nanoparticles, powder samples of those magnetic materials were studied by Small-Angle X-Ray Scattering. As will be shown, from the analysis and modeling of the scattering data, structural information could be obtained, enabling a detailed description of the structural properties of the studied samples which could be directly correlated to the magnetic properties. (author)

  12. Magnetic nanoparticles studied by small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Cristiano Luis Pinto [Universidade de Sao Paulo (IF/USP), SP (Brazil). Inst. de Fisica. Grupo de Fluidos Complexos; Antonel, Soledad; Negri, Martin [Universidad de Buenos Aires (UBA) (Argentina). Facultad de Ciencias Exactas y Naturales. Dept. de Quimica Inorganica, Analitica y Quimica Fisica

    2011-07-01

    nanoparticles are very interesting because they exhibit magnetic (ferromagnetic) and electrical properties in the same material. Then, the nickel nanoparticles could be used for the development of electroelastic materials. In this case, the electrical conductivity of the material can be strongly dependent on the applied magnetic field, for example the case of nickel metal nanoparticles dispersed in a polymer, resulting in an anisotropic material with combined piezomagnetic and piezoelectric properties. In order to investigate the structural characteristics of cobalt-iron oxides and nickel nanoparticles, powder samples of those magnetic materials were studied by Small-Angle X-Ray Scattering. As will be shown, from the analysis and modeling of the scattering data, structural information could be obtained, enabling a detailed description of the structural properties of the studied samples which could be directly correlated to the magnetic properties. (author)

  13. Determination of structural changes of dispersed clay platelets in a polymer blend during solid-state rheological property measurement by small-angle X-ray scattering

    CSIR Research Space (South Africa)

    Bandyopadhyay, J

    2011-05-01

    Full Text Available -angle X-ray scattering studies showed that the degree of anisotropy and mean orientation angles of clay platelets in blend matrix were altered significantly after frequency and temperature sweep tests....

  14. Fusion of three-dimensional X-ray angiography and three-dimensional echocardiography

    Energy Technology Data Exchange (ETDEWEB)

    Rasche, Volker [University of Ulm, Department of Internal Medicine II, Ulm (Germany); Philips Medical Systems, Bothell, WA (United States); Mansour, Moussa; Reddy, Vivek; Singh, Jagmeet P.; Ruskin, Jeremy [Massachusetts General Hospital, Harvard Medical School, Cardiac Arrhythmia Service, Boston, MA (United States); Qureshi, Answer [Massachusetts General Hospital, Harvard Medical School, Echocardiography, Boston, MA (United States); Manzke, Robert; Sokka, Sham [Philips Research North America, Clinical Sites Research, Briacliff Manor, NY (United States)

    2008-03-15

    Cardiovascular intervention guidance requires knowledge of heart function relative to its blood supply or venous drainage. Functional and vascular anatomic data are usually generated on different imaging systems, so fusion of the data is necessary to simultaneously visualize the results for intervention planning and guidance. The objective of this work is to establish the feasibility of fusing volumetric ultrasound (U/S) data with three-dimensional (3D) X-ray imaging data for visualization of cardiac morphology, function and coronary venous drainage. Temporally resolved U/S volume data was registered with the 3D reconstruction of vascular structures derived from X-ray modeling and reconstruction. U/S image registration was obtained by optical tracking fiducial markers with simultaneous X-ray imaging. The proposed technique was applied to phantom data for accuracy assessment of the registration process and to biventricular pacemaker implantation as clinical example. Fusion of U/S data with 3D X-ray reconstruction data produced an RMS registration error below 2 mm. Preliminary clinical feasibility of U/S-derived data synchronously with X-ray derived 3D coronary venography was established. This technique can be applied for fusion of functional U/S data with 3D anatomic X-ray data of the coronary veins during a biventricular pacemaker implantation procedures. (orig.)

  15. Fusion of three-dimensional X-ray angiography and three-dimensional echocardiography

    International Nuclear Information System (INIS)

    Rasche, Volker; Mansour, Moussa; Reddy, Vivek; Singh, Jagmeet P.; Ruskin, Jeremy; Qureshi, Answer; Manzke, Robert; Sokka, Sham

    2008-01-01

    Cardiovascular intervention guidance requires knowledge of heart function relative to its blood supply or venous drainage. Functional and vascular anatomic data are usually generated on different imaging systems, so fusion of the data is necessary to simultaneously visualize the results for intervention planning and guidance. The objective of this work is to establish the feasibility of fusing volumetric ultrasound (U/S) data with three-dimensional (3D) X-ray imaging data for visualization of cardiac morphology, function and coronary venous drainage. Temporally resolved U/S volume data was registered with the 3D reconstruction of vascular structures derived from X-ray modeling and reconstruction. U/S image registration was obtained by optical tracking fiducial markers with simultaneous X-ray imaging. The proposed technique was applied to phantom data for accuracy assessment of the registration process and to biventricular pacemaker implantation as clinical example. Fusion of U/S data with 3D X-ray reconstruction data produced an RMS registration error below 2 mm. Preliminary clinical feasibility of U/S-derived data synchronously with X-ray derived 3D coronary venography was established. This technique can be applied for fusion of functional U/S data with 3D anatomic X-ray data of the coronary veins during a biventricular pacemaker implantation procedures. (orig.)

  16. Enhancement of measurement accuracy of X-ray PIV in comparison with the micro-PIV technique.

    Science.gov (United States)

    Park, Hanwook; Jung, Sung Yong; Park, Jun Hong; Kim, Jun Ho; Lee, Sang Joon

    2018-03-01

    The X-ray PIV (particle image velocimetry) technique has been used as a non-invasive measurement modality to investigate the haemodynamic features of blood flow. However, the extraction of two-dimensional velocity field data from the three-dimensional volumetric information contained in X-ray images is technically unclear. In this study, a new two-dimensional velocity field extraction technique is proposed to overcome technological limitations. To resolve the problem of finding a correction coefficient, the velocity field information obtained by X-ray PIV and micro-PIV techniques for disturbed flow in a concentric stenosis with 50% severity was quantitatively compared. Micro-PIV experiments were conducted for single-plane and summation images, which provide similar positional information of particles as X-ray images. The correction coefficient was obtained by establishing the relationship between velocity data obtained from summation images (V S ) and centre-plane images (V C ). The velocity differences between V S and V C along the vertical and horizontal directions were quantitatively analysed as a function of the geometric angle of the test model for applying the present two-dimensional velocity field extraction technique to a conduit of arbitrary geometry. Finally, the two-dimensional velocity field information at arbitrary positions could be successfully extracted from X-ray images by using the correction coefficient and several velocity parameters derived from V S .

  17. Estimation of bearing contact angle in-situ by X-ray kinematography

    Science.gov (United States)

    Fowler, P. H.; Manders, F.

    1982-01-01

    The mounted, preloaded contact angle of the structural bearings in the assembled design mechanical assembly was measured. A modification of the Turns method is presented, based upon the clarity and definition of moving parts achieved with X-ray technique and cinematic display. Contact angle is estimated by counting the number of bearings passing a given point as a function of number of turns of the shaft. Ball and pitch diameter variations are discussed. Ball train and shaft angle uncertainties are also discussed.

  18. Note: Application of a pixel-array area detector to simultaneous single crystal x-ray diffraction and x-ray absorption spectroscopy measurements

    International Nuclear Information System (INIS)

    Sun, Cheng-Jun; Brewe, Dale L.; Heald, Steve M.; Zhang, Bangmin; Chen, Jing-Sheng; Chow, G. M.; Venkatesan, T.

    2014-01-01

    X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr 0.67 Sr 0.33 MnO 3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam

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

    DEFF Research Database (Denmark)

    Yennawar, Hemant; Møller, Magda; Gillilan, Richard

    2011-01-01

    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...

  20. Small-angle scattering studies of the fully hydrated phospholipid DPPC

    Energy Technology Data Exchange (ETDEWEB)

    Mason, P.C.; Gaulin, B.D. [Department of Physics and Astronomy, McMaster University, Hamilton, Ontario, L8S 4M1 (CANADA); Epand, R.M. [Department of Biochemistry, McMaster University, Hamilton, Ontario, L8N 3Z5 (CANADA); Wignall, G.D.; Lin, J.S. [Center for Small-Angle Scattering Research, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States)

    1999-01-01

    Small-angle neutron and x-ray scattering studies have been carried out on fully hydrated dipalmitoylphosphatidylcholine (DPPC) multilamellar vesicles. This system is known to exhibit two distinct ripple (P{sub {beta}{sup {prime}}}) phases, which depend on sample history, at temperatures intermediate to its high-temperature liquid crystalline (L{sub {alpha}}), phase, and its low-temperature gel (L{sub {beta}{sup {prime}}}), phase. On cooling from the L{sub {alpha}} phase, the P{sub {beta}{sup {prime}}} phase displays a complex multipeak diffraction pattern that differs significantly from the diffraction pattern seen in the P{sub {beta}{sup {prime}}} phase obtained on warming from the L{sub {beta}{sup {prime}}} phase. Examining the P{sub {beta}{sup {prime}}} phase on cooling using small-angle neutron scattering and x-ray diffraction techniques leads to the conclusion that this phase is characterized by a long wavelength ripple ({lambda}{sub r}{approximately}330thinsp{Angstrom}) and a highly monoclinic unit cell ({gamma}{approximately}125{degree}). As the P{sub {beta}{sup {prime}}} phase is traversed in temperature, the ripple wavelength changes significantly while the monoclinicity remains unchanged. Ripples from the P{sub {beta}{sup {prime}}} phase are seen to persist into the L{sub {beta}{sup {prime}}} phase on cooling, leading to increased small-angle scattering characteristic of a disordered stacking of the lamellae. {copyright} {ital 1999} {ital The American Physical Society}

  1. Neutron and X-ray diffraction from modulated structures

    International Nuclear Information System (INIS)

    Harris, P.

    1994-07-01

    This thesis describes X-ray and neutron scattering experiments performed on two examples of modulated structures. After an introduction to the subject of modulated structures, the thesis is divided in three parts. A single crystal elastic neutron scattering experiment between 4.2 and 115 Κ has been performed and four-circle X-ray data have been collected at 8 Κ for the monoclinic low-temperature phase of the layered perovskite PAMC. The results from the neutron scattering experiment indicate that magnetoelastic effects influence the ordering of the crystal. The X-ray experiments have made it possible to determine the crystal structure in the low-temperature phase. The superspace group is P2 1 /b(β-30)Os, with β = 1/3. A small-angle neutron scattering experiment has been performed on the magnetic structure of manganese silicide. When a magnetic field is applied, the modulation vectors turn towards the field direction, showing domain growth and diverging peak widths as they approach the field direction. Phase 'A' is established to have the modulation vectors directed perpendicular to the field direction. Cooling in zero field shows increasing peak widths at low temperatures, indicating a lock-in transition below the lowest reached temperature. To be able to analyse the data of the magnetic order in MnSi, and analytical calculation of the three dimensional resolution function for a small-angle neutron scattering spectrometer has been performed. The calculation is done by application of a combination of phase space analysis and Gaussian approximations for the neutron distribution as well as for the transmission functions of the different apertures. A finite mosaic spread of the crystal and finite correlation widths of the Bragg reflections have been included in the cross section. (au) (3 tabs., 48 ills., 100 refs.)

  2. Two Dimensional X-Ray Diffraction (2D-XRD) studies on Olivine of U.S.A

    International Nuclear Information System (INIS)

    Jabeen, S.; Raza, S.M.; Ahmed, M.A.; Zai, M.Y.; Elacher, K.

    2011-01-01

    The Olivine (Mg, Fe) 2SiO/sub 4/ of USA has been studied with two dimensional X-ray diffractometer (D8 discover with GADDS). The two distinct phases of orthorhombic structure, one with Mg/sub 8/[Fe/sub 2/SiO/sub 4/] and the other with Mg/sub 2/SiO/sub 4/ is observed. We also observed phase transitions due to presence of iron and Silicon preferably the structural change of Mg/sub 8/[Fe/sub 2/SiO/sub 4/] from orthorhombic to spinel like (spinel chord) structure. Magnesium ions in Mg/sub 8/[Fe/sub 2/SiO/sub 4/] shuffle, arrange at the five vertices of a pentagon and the remaining three at the central but with displaced position from the plane of the pentagon, Thus resulting into a three dimensional spinel chord like structure. We evidenced the same from diverse orientations of phase peaks and indeed from Kossel lines. (author)

  3. Calculation of accurate small angle X-ray scattering curves from coarse-grained protein models

    Directory of Open Access Journals (Sweden)

    Stovgaard Kasper

    2010-08-01

    Full Text Available Abstract Background Genome sequencing projects have expanded the gap between the amount of known protein sequences and structures. The limitations of current high resolution structure determination methods make it unlikely that this gap will disappear in the near future. Small angle X-ray scattering (SAXS is an established low resolution method for routinely determining the structure of proteins in solution. The purpose of this study is to develop a method for the efficient calculation of accurate SAXS curves from coarse-grained protein models. Such a method can for example be used to construct a likelihood function, which is paramount for structure determination based on statistical inference. Results We present a method for the efficient calculation of accurate SAXS curves based on the Debye formula and a set of scattering form factors for dummy atom representations of amino acids. Such a method avoids the computationally costly iteration over all atoms. We estimated the form factors using generated data from a set of high quality protein structures. No ad hoc scaling or correction factors are applied in the calculation of the curves. Two coarse-grained representations of protein structure were investigated; two scattering bodies per amino acid led to significantly better results than a single scattering body. Conclusion We show that the obtained point estimates allow the calculation of accurate SAXS curves from coarse-grained protein models. The resulting curves are on par with the current state-of-the-art program CRYSOL, which requires full atomic detail. Our method was also comparable to CRYSOL in recognizing native structures among native-like decoys. As a proof-of-concept, we combined the coarse-grained Debye calculation with a previously described probabilistic model of protein structure, TorusDBN. This resulted in a significant improvement in the decoy recognition performance. In conclusion, the presented method shows great promise for

  4. X-ray spectral determination by detection of radiation scattered at different angles

    International Nuclear Information System (INIS)

    Barrea, Raul; Mainardi, R.T.

    1987-01-01

    A precise knowledge of the spectral content of an X-ray beam is of fundamental importance in areas such as X-ray fluorescence analysis by absolute methods, radiodiagnosis, radiotherapy, computed tomography, etc. A simple practical method was developed to determine X-ray spectra emitted by X-ray tubes. It is based on the scattering of the beam on a solid target and detection of this radiation at different angles. This methodology can easily be adapted to the successive attenuation of the beam procedure. Numerical parameter values of a proposed analytical function for the energy spectrum are found measuring the radiation intensity with a suitable detector (ionization chamber or plastic scintillation detector) and equating it with the convolution integral of the proposed spectrum with the incoherent scattering function. This procedure of spectra determination is enclosed in the same group of those generically referred as successive modifications of the irradiation set up used in absolute methods of X-ray fluorescence analysis. (Author) [es

  5. Development and Characterization of Two-Dimensional Gratings for Single-Shot X-ray Phase-Contrast Imaging

    Directory of Open Access Journals (Sweden)

    Margarita Zakharova

    2018-03-01

    Full Text Available Single-shot grating-based phase-contrast imaging techniques offer additional contrast modalities based on the refraction and scattering of X-rays in a robust and versatile configuration. The utilization of a single optical element is possible in such methods, allowing the shortening of the acquisition time and increasing flux efficiency. One of the ways to upgrade single-shot imaging techniques is to utilize customized optical components, such as two-dimensional (2D X-ray gratings. In this contribution, we present the achievements in the development of 2D gratings with UV lithography and gold electroplating. Absorption gratings represented by periodic free-standing gold pillars with lateral structure sizes from 5 µm to 25 µm and heights from 5 µm to 28 µm have shown a high degree of periodicity and defect-free patterns. Grating performance was tested in a radiographic setup using a self-developed quality assessment algorithm based on the intensity distribution histograms. The algorithm allows the final user to estimate the suitability of a specific grating to be used in a particular setup.

  6. Two-dimensional position-sensitive detectors for small-angle neutron scattering

    International Nuclear Information System (INIS)

    McElhaney, S.A.; Vandermolen, R.I.

    1990-05-01

    In this paper, various detectors available for small angle neutron scattering (SANS) are discussed, along with some current developments being actively pursued. A section has been included to outline the various methodologies of position encoding/decoding with discussions on trends and limitations. Computer software/hardware vary greatly from institute and experiment and only a general discussion is given to this area. 85 refs., 33 figs

  7. Plasma-assisted atomic layer epitaxial growth of aluminum nitride studied with real time grazing angle small angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, Virginia R.; Nepal, Neeraj; Johnson, Scooter D.; Robinson, Zachary R.; Nath, Anindya; Kozen, Alexander C.; Qadri, Syed B.; DeMasi, Alexander; Hite, Jennifer K.; Ludwig, Karl F.; Eddy, Charles R.

    2017-05-01

    Wide bandgap semiconducting nitrides have found wide-spread application as light emitting and laser diodes and are under investigation for further application in optoelectronics, photovoltaics, and efficient power switching technologies. Alloys of the binary semiconductors allow adjustments of the band gap, an important semiconductor material characteristic, which is 6.2 eV for aluminum nitride (AlN), 3.4 eV for gallium nitride, and 0.7 eV for (InN). Currently, the highest quality III-nitride films are deposited by metalorganic chemical vapor deposition and molecular beam epitaxy. Temperatures of 900 °C and higher are required to deposit high quality AlN. Research into depositing III-nitrides with atomic layer epitaxy (ALEp) is ongoing because it is a fabrication friendly technique allowing lower growth temperatures. Because it is a relatively new technique, there is insufficient understanding of the ALEp growth mechanism which will be essential to development of the process. Here, grazing incidence small angle x-ray scattering is employed to observe the evolving behavior of the surface morphology during growth of AlN by ALEp at temperatures from 360 to 480 °C. Increased temperatures of AlN resulted in lower impurities and relatively fewer features with short range correlations.

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

    Science.gov (United States)

    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. Small-angle x-ray scattering study of kinetics of spinodal decomposition in N-isopropylacrylamide gels

    International Nuclear Information System (INIS)

    Liao, G.; Xie, Y.; Ludwig, K.F. Jr.; Bansil, R.; Gallagher, P.; Xie, Y.; Gallagher, P.

    1999-01-01

    We present synchrotron-based time-resolved small-angle x-ray scattering (SAXS) measurements of spinodal decomposition in a covalently cross-linked N-isopropylacrylamide gel. The range of wave numbers examined is well beyond the position of the maximum in the structure factor S(q,t). The equilibrium structure factor is described by the sum of a Lorentzian and a Gaussian. Following a temperature jump into the two phase region, the scattered intensity increases with time and eventually saturates. For early times the linear Cahn-Hilliard-Cook (CHC) theory can be used to describe the time evolution of the scattered intensity. From this analysis we found that the growth rate R(q) is linearly dependent on q 2 , in agreement with mean-field theoretical predictions. However the Onsager transport coefficient Λ(q)∼q -4 , which is stronger than the q dependence predicted by the mean-field theory. We found that the growth rate R(q)>0, even though the wave numbers q probed by SAXS are greater than √ (2) q m where q m is the position of the peak of S(q,t), also in agreement with the mean-field predictions for a deep quench. We have also examined the range of validity of the linear CHC theory, and found that its breakdown occurs earlier at higher wave numbers. At later times, a pinning of the structure was observed. The relaxation to a final, microphase-separated morphology is faster and occurs earlier at the highest wave numbers, which probe length scales comparable to the average distance between crosslinks. copyright 1999 The American Physical Society

  10. X-ray diffraction study of the structure of detonation nanodiamonds

    International Nuclear Information System (INIS)

    Ozerin, A. N.; Kurkin, T. S.; Ozerina, L. A.; Dolmatov, V. Yu.

    2008-01-01

    The spatial structure of aggregates formed by detonation nanodiamonds is investigated using the wide-angle and small-angle X-ray scattering techniques. The effective sizes of crystallites and the crystallite size distribution function are determined. The shape of scattering aggregates is restored from the small-angle X-ray scattering data. An analysis of the results obtained allowed the conclusion that the nanodiamond aggregates have an extended spatial structure composed of nine to ten clusters, each involving four to five crystallites with a crystal lattice of the diamond type

  11. Proceedings of the International school and symposium on small angle scattering

    International Nuclear Information System (INIS)

    Borbely, S.; Rosta, L.

    1999-04-01

    The meeting was devoted to small angle neutron and X-ray scattering with regard to the wide interest for this method in various fields of basic and applied research. Scientists from European laboratories gave introductory talks to various subject fields related to small angle scattering (SAS) techniques or data analysis methods as well as topical research area e.g. soft condensed matter, biology or materials science. An important number of contributed talks were presented on neutron or X-ray scattering and even on combining both of them, demonstrating the very useful complementarity of these methods. Some other papers give nice examples of SAS experiments completed by results of other techniques such as NMRE of light scattering. The variety of presented contributions is a nice demonstration for the interdisciplinary use of small angle scattering from physics through biology, chemistry, materials science to engineering. 18 items are indexed separately for the INIS database. (K.A.)

  12. A high-resolution multiwire area detector for X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Faruqi, A R; Andrews, H [Medical Research Council, Cambridge (UK). Lab. of Molecular Biology

    1989-11-10

    A high-resolution multiwire area detector has been developed for recording X-ray scattering from biological specimens. The detector is 100x100 mm{sup 2} and, under the present operating conditions, has a spatial resolution of about 250 {mu}m in both directions. The detector is set up on a double-mirror focusing camera on a rotating anode X-ray generator and has been used in a number of small-angle experiments, two of which are described in this paper. (orig.).

  13. Assessment of Escherichia coli selenophosphate synthetase oligomeric states by analytical ultracentrifugation and small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Silva, I.R.; Faim, F.M.; Oliveira Neto, M.; Thiemann, O.H. [Universidade de Sao Paulo (USP-SC), Sao Carlos, SP (Brazil); Borges, J.C. [Universidade de Sao Paulo (IQSC/USP), Sao Carlos, SP (Brazil). Inst. de Quimica

    2012-07-01

    Full text: Selenium is an essential micronutrient for many organisms and is present in selenium-containing proteins as selenocysteine (Sec) and RNAs as selenouridine. Specific selenium incorporation into selenoproteins and RNAs requires the generation of a biologically active selenium donor compound, selenophosphate, which is produced from the activation of selenide with adenosine 5-triphosphate (ATP) in a reaction catalyzed by Selenophosphate Synthetase (SELD). Therefore, SELD is a key enzyme of the selenium pathway in the cell. The Escherichia coli SELD open reading frame was cloned into pET28a (Novagen) expression vector and the recombinant protein was over expressed in Escherichia coli BL21(DE3) strain. In order to purify the protein, we used metal-chelate affinity chromatography followed by a gel filtration step. Analytical Ultracentrifugation (AUC) and Small Angle X-ray Scattering (SAXS) were employed to study the oligomeric states of the soluble protein. The results of AUC revealed dimer-tetramer and tetramer-octamer equilibrium at low concentrations of protein, with dissociation constants of 70 2 and 560 40 M, respectively. Moreover, the SAXS results pointed the oligomeric state of the protein at higher concentrations as predominantly dimeric and the p(r) and the SAXS envelope revealed the SELD as elongated. We also performed initial crystallization trials with protein samples at 7 mg/ml in 96-well sitting-drop crystallization plates at room temperature using a crystallization robot. Needle crystals appeared after some days. X-ray diffraction for these crystals were tested in the MX2 beamline at the Brazilian Synchrotron Laboratory (LNLS Campinas). We are now working to improve these crystals in order to obtain suitable crystals for structure determination. (author)

  14. Angle-resolved environmental X-ray photoelectron spectroscopy: A new laboratory setup for photoemission studies at pressures up to 0.4 Torr

    International Nuclear Information System (INIS)

    Mangolini, F.; Wabiszewski, G. E.; Egberts, P.; Åhlund, J.; Backlund, K.; Karlsson, P. G.; Adiga, V. P.; Streller, F.; Wannberg, B.; Carpick, R. W.

    2012-01-01

    The paper presents the development and demonstrates the capabilities of a new laboratory-based environmental X-ray photoelectron spectroscopy system incorporating an electrostatic lens and able to acquire spectra up to 0.4 Torr. The incorporation of a two-dimensional detector provides imaging capabilities and allows the acquisition of angle-resolved data in parallel mode over an angular range of 14° without tilting the sample. The sensitivity and energy resolution of the spectrometer have been investigated by analyzing a standard Ag foil both under high vacuum (10 −8 Torr) conditions and at elevated pressures of N 2 (0.4 Torr). The possibility of acquiring angle-resolved data at different pressures has been demonstrated by analyzing a silicon/silicon dioxide (Si/SiO 2 ) sample. The collected angle-resolved spectra could be effectively used for the determination of the thickness of the native silicon oxide layer.

  15. Small-Size High-Current Generators for X-Ray Backlighting

    Science.gov (United States)

    Chaikovsky, S. A.; Artyomov, A. P.; Zharova, N. V.; Zhigalin, A. S.; Lavrinovich, I. V.; Oreshkin, V. I.; Ratakhin, N. A.; Rousskikh, A. G.; Fedunin, A. V.; Fedushchak, V. F.; Erfort, A. A.

    2017-12-01

    The paper deals with the soft X-ray backlighting based on the X-pinch as a powerful tool for physical studies of fast processes. Proposed are the unique small-size pulsed power generators operating as a low-inductance capacitor bank. These pulse generators provide the X-pinch-based soft X-ray source (hν = 1-10 keV) of micron size at 2-3 ns pulse duration. The small size and weight of pulse generators allow them to be transported to any laboratory for conducting X-ray backlighting of test objects with micron space resolution and nanosecond exposure time. These generators also allow creating synchronized multi-frame radiographic complexes with frame delay variation in a broad range.

  16. X-ray optics for scanning fluorescence microscopy and other applications

    International Nuclear Information System (INIS)

    Ryon, R.W.; Warburton, W.K.

    1992-05-01

    Scanning x-ray fluorescence microscopy is analogous to scanning electron microscopy. Maps of chemical element distribution are produced by scanning with a very small x-ray beam. Goal is to perform such scanning microscopy with resolution in the range of <1 to 10 μm, using standard laboratory x-ray tubes. We are investigating mirror optics in the Kirkpatrick-Baez (K-B) configuration. K-B optics uses two curved mirrors mounted orthogonally along the optical axis. The first mirror provides vertical focus, the second mirror provides horizontal focus. We have used two types of mirrors: synthetic multilayers and crystals. Multilayer mirrors are used with lower energy radiation such as Cu Kα. At higher energies such as Ag Kα, silicon wafers are used in order to increase the incidence angles and thereby the photon collection efficiency. In order to increase the surface area of multilayers which reflects x-rays at the Bragg angle, we have designed mirrors with the spacing between layers graded along the optic axis in order to compensate for the changing angle of incidence. Likewise, to achieve a large reflecting surface with silicon, the wafers are placed on a specially designed lever arm which is bent into a log spiral by applying force at one end. In this way, the same diffracting angle is maintained over the entire surface of the wafer, providing a large solid angle for photon collection

  17. Small angle scattering methods to study porous materials under high uniaxial strain

    Energy Technology Data Exchange (ETDEWEB)

    Le Floch, Sylvie, E-mail: sylvie.le-floch@univ-lyon1.fr; Balima, Félix; Pischedda, Vittoria; Legrand, Franck; San-Miguel, Alfonso [Institut Lumière Matière, UMR5306 Université Lyon 1-CNRS, Université de Lyon, 69622 Villeurbanne Cedex (France)

    2015-02-15

    We developed a high pressure cell for the in situ study of the porosity of solids under high uniaxial strain using neutron small angle scattering. The cell comprises a hydraulically actioned piston and a main body equipped with two single-crystal sapphire windows allowing for the neutron scattering of the sample. The sample cavity is designed to allow for a large volume variation as expected when compressing highly porous materials. We also implemented a loading protocol to adapt an existing diamond anvil cell for the study of porous materials by X-ray small angle scattering under high pressure. The two techniques are complementary as the radiation beam and the applied pressure are in one case perpendicular to each other (neutron cell) and in the other case parallel (X-ray cell). We will illustrate the use of these two techniques in the study of lamellar porous systems up to a maximum pressure of 0.1 GPa and 0.3 GPa for the neutron and X-ray cells, respectively. These devices allow obtaining information on the evolution of porosity with pressure in the pore dimension subdomain defined by the wave-numbers explored in the scattering process. The evolution with the applied load of such parameters as the fractal dimension of the pore-matrix interface or the apparent specific surface in expanded graphite and in expanded vermiculite is used to illustrate the use of the high pressure cells.

  18. Three-Dimensional X-Ray Diffraction Technique for Metals Science

    DEFF Research Database (Denmark)

    Zhang, Yubin; Fan, Guohua

    2017-01-01

    The three-dimensional X-ray diffraction (3DXRD) is a new, advanced technique for materials characterization. This technique utilizes high-energy synchrotron X-rays to characterize the 3D crystallographic structure and strain/stress state of bulk materials. As the measurement is non......-destructive, the microstructural evolution as a function of time can be followed, i.e. it allows 4D (x, y, z characterizations, t). The high brilliance of synchrotron X-rays ensures that diffraction signals from volumes of micrometer scale can be quickly detected and distinguished from the background noise, i.e. its spatial...... implemented in several large synchrotron facilities, e.g. the Advanced Photon Source (APS) in USA and the Spring-8 in Japan. Another family of 3DXRD technique that utilizes white beam synchrotron X-rays has also been developed in parallel in cooperation between Oak Ridge National Laboratory and APS...

  19. Observations on the Performance of X-Ray Computed Tomography for Dimensional Metrology

    Science.gov (United States)

    Corcoran, H. C.; Brown, S. B.; Robson, S.; Speller, R. D.; McCarthy, M. B.

    2016-06-01

    X-ray computed tomography (XCT) is a rising technology within many industries and sectors with a demand for dimensional metrology, defect, void analysis and reverse engineering. There are many variables that can affect the dimensional metrology of objects imaged using XCT, this paper focusses on the effects of beam hardening due to the orientation of the workpiece, in this case a holeplate, and the volume of material the X-rays travel through. Measurements discussed include unidirectional and bidirectional dimensions, radii of cylinders, fit point deviations of the fitted shapes and cylindricity. Results indicate that accuracy and precision of these dimensional measurements are affected in varying amounts, both by the amount of material the X-rays have travelled through and the orientation of the object.

  20. OBSERVATIONS ON THE PERFORMANCE OF X-RAY COMPUTED TOMOGRAPHY FOR DIMENSIONAL METROLOGY

    Directory of Open Access Journals (Sweden)

    H. C. Corcoran

    2016-06-01

    Full Text Available X-ray computed tomography (XCT is a rising technology within many industries and sectors with a demand for dimensional metrology, defect, void analysis and reverse engineering. There are many variables that can affect the dimensional metrology of objects imaged using XCT, this paper focusses on the effects of beam hardening due to the orientation of the workpiece, in this case a holeplate, and the volume of material the X-rays travel through. Measurements discussed include unidirectional and bidirectional dimensions, radii of cylinders, fit point deviations of the fitted shapes and cylindricity. Results indicate that accuracy and precision of these dimensional measurements are affected in varying amounts, both by the amount of material the X-rays have travelled through and the orientation of the object.

  1. Development of quantitative x-ray microtomography

    International Nuclear Information System (INIS)

    Deckman, H.W.; Dunsmuir, J.A.; D'Amico, K.L.; Ferguson, S.R.; Flannery, B.P.

    1990-01-01

    The authors have developed several x-ray microtomography systems which function as quantitative three dimensional x-ray microscopes. In this paper the authors describe the evolutionary path followed from making the first high resolution experimental microscopes to later generations which can be routinely used for investigating materials. Developing the instrumentation for reliable quantitative x-ray microscopy using synchrotron and laboratory based x-ray sources has led to other imaging modalities for obtaining temporal and spatial two dimensional information

  2. Structure of a mouse immunoglobulin G that lacks the entire CH1 domain: Protein sequencing and small-angle X-ray scattering studies

    International Nuclear Information System (INIS)

    Igarashi, Takako; Tanaka, Toshiyuki; Nakanishi, Mamoru; Arata, Yoji; Sato, Mamoru; Katsube, Yukiteru; Takio, Koji

    1990-01-01

    The structure of a short-chain IgG2a antibody, which is a member of the family of mouse anti-dansyl switch variant antibodies with identical variable regions but different heavy-chain constant regions, is reported. Amino acid sequencing analyses have demonstrated that in the short-chain IgG2a antibody the entire C H 1 domain is deleted whereas the hinge region remains intact. Small-angle X-ray scattering data were collected for the short-chain IgG2a antibody and compared with those for the switch variant IgG1, IgG2a, and IgG2b antibodies with the normal heavy chain. It has been concluded that deletion of the C H 1 domain results in a large structural change and the short-chain IgG2a antibody possesses an elongated molecular shape with a much smaller hinge angle as compared with the normal IgG2a antibody that is a Y-shaped molecule

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

    International Nuclear Information System (INIS)

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

    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. Analysis of thin films prepared by vacuum-evaporation and dropping solution by Takeoff Angle-Dependent X-Ray Fluorescence spectroscopy at glancing incidence

    International Nuclear Information System (INIS)

    Tsuji, Kouichi; Hirokawa, Kichinosuke; Mitose, Kengo.

    1995-01-01

    We have introduced Takeoff Angle-Dependent X-Ray Fluorescence (TAD-XRF) method for thin film and surface analysis. In this method, the sample on the optically flat substrate is irradiated with the glancing incidence of the primary X-ray, and the fluorescent X-rays emitted from the sample are detected at the glancing takeoff angle. We had previously calculated the relationship between the fluorescent X-ray intensity and the takeoff angle at the glancing incidence. The characterization of the thin film is achieved by investigating the dependence of the fluorescent X-ray intensity on the takeoff angle with the calculated curve. Using this analytical method, we have reported the results of the TAD-XRF measured for the evaporated thin films and the dried films from dropping solution in this paper. The effect of the thickness of the thin film, the density of the substrate and the incident angle on the TAD-XRF curve has been reported. In the case of the dried film from the dropping solution, a broad peak was observed at the takeoff angle which was close to the critical angle for the total reflection of the fluorescent X-ray in the TAD-XRF curve. This broad peak was explained by the double-excitation of the incident beam and the refracted beam of the fluorescent X-ray with the assumption that the X-ray which has a same wavelength to the observed fluorescent X-ray impinges upon the sample surface, because the reciprocity theorem is expected in the X-ray region. (author)

  5. X-ray scattering studies of non-equilibrium ordering processes

    International Nuclear Information System (INIS)

    Nagler, S.E.

    1991-01-01

    We report on the progress of the project entitled ''X-ray Scattering Studies of Non-Equilibrium Ordering Processes.'' The past year has seen continued progress in the study of kinetic effects in metallic binary alloys and polymers. In addition, work has begun on a low dimensional CDW system: blue bronze. A sample chamber has been constructed to perform small angle neutron scattering measurements on a model quantum system with phase separation: solid He3/He4. Work is continuing on magnetic systems. Planned future experiments include an investigation of crystallization in Rubidium

  6. Theoretical concepts of X-ray nanoscale analysis theory and applications

    CERN Document Server

    Benediktovitch, Andrei; Ulyanenkov, Alexander

    2013-01-01

    This book provides a concise survey of modern theoretical concepts of X-ray materials analysis. The principle features of the book are: basics of X-ray scattering, interaction between X-rays and matter and new theoretical concepts of X-ray scattering. The various X-ray techniques are considered in detail: high-resolution X-ray diffraction, X-ray reflectivity, grazing-incidence small-angle X-ray scattering and X-ray residual stress analysis. All the theoretical methods presented use the unified physical approach. This makes the book especially useful for readers learning and performing data ana

  7. Two electron response to an intense x-ray free electron laser pulse

    International Nuclear Information System (INIS)

    Moore, L R; Parker, J S; Meharg, K J; Armstrong, G S J; Taylor, K T

    2009-01-01

    New x-ray free electron lasers (FELs) promise an ultra-fast ultra-intense regime in which new physical phenomena, such as double core hole formation in at atom, should become directly observable. Ahead of x-ray FEL experiments, an initial key task is to theoretically explore such fundamental laser-atom interactions and processes. To study the response of a two-electron positive ion to an intense x-ray FEL pulse, our theoretical approach is a direct numerical integration, incorporating non-dipole Hamiltonian terms, of the full six-dimensional time-dependent Schroedinger equation. We present probabilities of double K-shell ionization in the two-electron positive ions Ne 8+ and Ar 16+ exposed to x-ray FEL pulses with frequencies in the range 50 au to 300 au and intensities in the range 10 17 to 10 22 W/cm 2 .

  8. The influence of the oblique incident X-ray that affected the image quality of the X-ray CCD sensor

    International Nuclear Information System (INIS)

    Suzuki, Yosuke; Matsumoto, Nobue; Morita, Hiroshi; Ohkawa, Hiromitsu

    1998-01-01

    The influence of the oblique incident X-ray that affected the image quality of the X-ray CCD sensor was examined and its correction was investigated. CDR was adopted in this study and evaluated image quality, by measuring MTF. The oblique projection was clinically permissible to about an oblique incident angle of 40 degrees although it exerts an influence on the magnifying power and density. The estimation of the oblique entrance direction and oblique incident angle was possible, by developing an oblique incident correction marker. When an oblique incident angle of θ degrees was measured, a correction is possible, by compressing the image cos (θ) times perpendicular to the rotational axis of CCD sensor. There was small decline of MTF, in the image where a correction for the influence of oblique incidence was made. By observation of the digital subtracted picture of the image after correction of oblique projection and that of normal, the resemblance in the two images indicated that this correction method was reasonable. (author)

  9. Discovery of two eclipsing X-ray binaries in M 51

    Science.gov (United States)

    Wang, Song; Soria, Roberto; Urquhart, Ryan; Liu, Jifeng

    2018-04-01

    We discovered eclipses and dips in two luminous (and highly variable) X-ray sources in M 51. One (CXOM51 J132943.3+471135) is an ultraluminous supersoft source, with a thermal spectrum at a temperature of about 0.1 keV and characteristic blackbody radius of about 104 km. The other (CXOM51 J132946.1+471042) has a two-component spectrum with additional thermal-plasma emission; it approached an X-ray luminosity of 1039erg s-1 during outbursts in 2005 and 2012. From the timing of three eclipses in a series of Chandra observations, we determine the binary period (52.75 ± 0.63 hr) and eclipse fraction (22% ± 0.1%) of CXOM51 J132946.1+471042. We also identify a blue optical counterpart in archival Hubble Space Telescope images, consistent with a massive donor star (mass of ˜20-35M⊙). By combining the X-ray lightcurve parameters with the optical constraints on the donor star, we show that the mass ratio in the system must be M_2/M_1 ≳ 18, and therefore the compact object is most likely a neutron star (exceeding its Eddington limit in outburst). The general significance of our result is that we illustrate one method (applicable to high-inclination sources) of identifying luminous neutron star X-ray binaries, in the absence of X-ray pulsations or phase-resolved optical spectroscopy. Finally, we discuss the different X-ray spectral appearance expected from super-Eddington neutron stars and black holes at high viewing angles.

  10. Three-dimensional propagation in near-field tomographic X-ray phase retrieval

    International Nuclear Information System (INIS)

    Ruhlandt, Aike; Salditt, Tim

    2016-01-01

    An extension of phase retrieval algorithms for near-field X-ray (propagation) imaging to three dimensions is presented, enhancing the quality of the reconstruction by exploiting previously unused three-dimensional consistency constraints. This paper presents an extension of phase retrieval algorithms for near-field X-ray (propagation) imaging to three dimensions, enhancing the quality of the reconstruction by exploiting previously unused three-dimensional consistency constraints. The approach is based on a novel three-dimensional propagator and is derived for the case of optically weak objects. It can be easily implemented in current phase retrieval architectures, is computationally efficient and reduces the need for restrictive prior assumptions, resulting in superior reconstruction quality

  11. Ultrafast coherent diffractive imaging of nanoparticles using X-ray free-electron laser radiation

    International Nuclear Information System (INIS)

    Kassemeyer, Stephan

    2014-01-01

    Coherent diffractive imaging with X-ray free-electron lasers (X-FEL) promises high-resolution structure determination of single microscopic particles without the need for crystallization. The diffraction signal of small samples can be very weak, a difficulty that can not be countered by merely increasing the number of photons because the sample would be damaged by a high absorbed radiation dose. Traditional X-ray crystallography avoids this problem by bringing many sample particles into a periodic arrangement, which amplifies the individual signals while distributing the absorbed dose. Depending on the sample, however, crystallization can be very difficult or even impossible. This thesis presents algorithms for a new imaging approach using X-FEL radiation that works with single, non-crystalline sample particles. X-FELs can deliver X-rays with a peak brilliance many orders of magnitude higher than conventional X-ray sources, compensating for their weak interaction cross sections. At the same time, FELs can produce ultra-short pulses down to a few femtoseconds. In this way it is possible to perform ultra-fast imaging, essentially ''freezing'' the atomic positions in time and terminating the imaging process before the sample is destroyed by the absorbed radiation. This thesis primarily focuses on the three-dimensional reconstruction of single (and not necessarily crystalline) particles using coherent diffractive imaging at X-FELs: in order to extract three-dimensional information from scattering data, two-dimensional diffraction patterns from many different viewing angles must be combined. Therefore, the diffraction signal of many identical sample copies in random orientations is measured. The main result of this work is a globally optimal algorithm that can recover the sample orientations solely based on the diffraction signal, enabling three-dimensional imaging for arbitrary samples. The problem of finding three-dimensional orientations is

  12. Three-dimensional imagery by encoding sources of X rays

    International Nuclear Information System (INIS)

    Magnin, Isabelle

    1987-01-01

    This research thesis addresses the theoretical and practical study of X ray coded sources, and thus notably aims at exploring whether it would be possible to transform a standard digital radiography apparatus (as those operated in radiology hospital departments) into a low cost three-dimensional imagery system. The author first recalls the principle of conventional tomography and improvement attempts, and describes imagery techniques based on the use of encoding openings and source encoding. She reports the modelling of an imagery system based on encoded sources of X ray, and addresses the original notion of three-dimensional response for such a system. The author then addresses the reconstruction method by considering the reconstruction of a plane object, of a multi-plane object, and of real three-dimensional object. The frequency properties and the tomographic capacities of various types of source codes are analysed. She describes a prototype tomography apparatus, and presents and discusses three-dimensional actual phantom reconstructions. She finally introduces a new principle of dynamic three-dimensional radiography which implements an acquisition technique by 'gating code'. The acquisition principle should allow the reconstruction of volumes animated by periodic deformations, such as the heart for example [fr

  13. A novel application of small-angle scattering techniques: Quality assurance testing of virus quantification technology

    International Nuclear Information System (INIS)

    Kuzmanovic, Deborah A.; Elashvili, Ilya; O'Connell, Catherine; Krueger, Susan

    2008-01-01

    Small-angle scattering (SAS) techniques, like small-angle X-ray scattering (SAXS) and small-angle neutron scattering (SANS), were used to measure and thus to validate the accuracy of a novel technology for virus sizing and concentration determination. These studies demonstrate the utility of SAS techniques for use in quality assurance measurements and as novel technology for the physical characterization of viruses

  14. Automated three-dimensional X-ray analysis using a dual-beam FIB

    International Nuclear Information System (INIS)

    Schaffer, Miroslava; Wagner, Julian; Schaffer, Bernhard; Schmied, Mario; Mulders, Hans

    2007-01-01

    We present a fully automated method for three-dimensional (3D) elemental analysis demonstrated using a ceramic sample of chemistry (Ca)MgTiO x . The specimen is serially sectioned by a focused ion beam (FIB) microscope, and energy-dispersive X-ray spectrometry (EDXS) is used for elemental analysis of each cross-section created. A 3D elemental model is reconstructed from the stack of two-dimensional (2D) data. This work concentrates on issues arising from process automation, the large sample volume of approximately 17x17x10 μm 3 , and the insulating nature of the specimen. A new routine for post-acquisition data correction of different drift effects is demonstrated. Furthermore, it is shown that EDXS data may be erroneous for specimens containing voids, and that back-scattered electron images have to be used to correct for these errors

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

    Science.gov (United States)

    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.

  16. Experimental demonstration of high resolution three-dimensional x-ray holography

    International Nuclear Information System (INIS)

    McNulty, I.; Trebes, J.E.; Brase, J.M.; Yorkey, T.J.; Levesque, R.; Szoke, H.; Anderson, E.H.; Jacobsen, C.

    1992-01-01

    Tomographic x-ray holography may make possible the imaging of biological objects at high resolution in three dimensions. We performed a demonstration experiment with soft x-rays to explore the feasibility of this technique. Coherent 3.2-nm undulator radiation was used to record Fourier transform holograms of a microfabricated test object from various illumination angles. The holograms were numerically reconstructed according to the principles of diffraction tomography, yielding images of the object that are well resolved in three dimensions

  17. A modulated differential scanning calorimetry and small-angle x-ray scattering study of the interfacial region in structured latices

    Directory of Open Access Journals (Sweden)

    Hourston Douglas J.

    2001-01-01

    Full Text Available The interfacial structure of poly(styrene (PS-poly(methyl acrylate (PMA structured latices has been investigated by means of modulated-temperature differential scanning calorimetry (M-TDSC and small-angle x-ray scattering (SAXS. The differential of heat capacity, dCp/dT, signal from M-TDSC was used to quantify the weight fraction of interface in these latices. For PS-PMA (50:50 by weight structured latices in which the PS component had different crosslink densities (0, 1, 3, 5 and 10 mol% of crosslinking agent, the weight fraction of interface was about 13%. With increasing crosslink density, the fraction of interface increased only slightly. A core-shell model has been used to analyse SAXS data for these PS-PMA latices. M-TDSC can only provide information about the weight fraction of interface, but the combination of M-TDSC and SAXS can provide much more information on the morphology of such structured latices.

  18. Study on the conformal variations of bovine and human serum albumin in solution using small angle X-ray scattering

    International Nuclear Information System (INIS)

    Olivieri, Johnny Rizzieri.

    1992-01-01

    It is reported a Small Angle X-Ray Scattering (SAXS) study of BSA (Bovine Serum Albumin) and HSA (Human Serum Albumin) on pH between 2.5 and 7.0. The measured scattering intensities, normalized in relation to incident beam, exposition time and scattering due to solvent and capillary, and corrected due to concentration and beam shape effects, have shown a strong dependence of the protein shape with pH for both albumins. It was found that the radius of gyration varies between 26.7 and 35 A, and the analyses of the distance distribution function. P(r), indicated that these proteins undergoes conformational changes with pH. Different theoretical shapes have been proposed and analysed comparing the computed P(r) function generated from the models with the experimental P(r). A large variety of shapes were found in both proteins, indicating that BSA and HSA are very flexibility macromolecules. (author). 60 refs., 49 figs., 7 tabs

  19. Reconstruction of the two-dimensional gravitational potential of galaxy clusters from X-ray and Sunyaev-Zel'dovich measurements

    Science.gov (United States)

    Tchernin, C.; Bartelmann, M.; Huber, K.; Dekel, A.; Hurier, G.; Majer, C. L.; Meyer, S.; Zinger, E.; Eckert, D.; Meneghetti, M.; Merten, J.

    2018-06-01

    Context. The mass of galaxy clusters is not a direct observable, nonetheless it is commonly used to probe cosmological models. Based on the combination of all main cluster observables, that is, the X-ray emission, the thermal Sunyaev-Zel'dovich (SZ) signal, the velocity dispersion of the cluster galaxies, and gravitational lensing, the gravitational potential of galaxy clusters can be jointly reconstructed. Aims: We derive the two main ingredients required for this joint reconstruction: the potentials individually reconstructed from the observables and their covariance matrices, which act as a weight in the joint reconstruction. We show here the method to derive these quantities. The result of the joint reconstruction applied to a real cluster will be discussed in a forthcoming paper. Methods: We apply the Richardson-Lucy deprojection algorithm to data on a two-dimensional (2D) grid. We first test the 2D deprojection algorithm on a β-profile. Assuming hydrostatic equilibrium, we further reconstruct the gravitational potential of a simulated galaxy cluster based on synthetic SZ and X-ray data. We then reconstruct the projected gravitational potential of the massive and dynamically active cluster Abell 2142, based on the X-ray observations collected with XMM-Newton and the SZ observations from the Planck satellite. Finally, we compute the covariance matrix of the projected reconstructed potential of the cluster Abell 2142 based on the X-ray measurements collected with XMM-Newton. Results: The gravitational potentials of the simulated cluster recovered from synthetic X-ray and SZ data are consistent, even though the potential reconstructed from X-rays shows larger deviations from the true potential. Regarding Abell 2142, the projected gravitational cluster potentials recovered from SZ and X-ray data reproduce well the projected potential inferred from gravitational-lensing observations. We also observe that the covariance matrix of the potential for Abell 2142

  20. Structure of human low-density lipoprotein subfractions, determined by X-ray small-angle scattering.

    Science.gov (United States)

    Baumstark, M W; Kreutz, W; Berg, A; Frey, I; Keul, J

    1990-01-19

    The structure of low-density lipoprotein (LDL) particles from three different density ranges (LDL-1: d = 1.006-1.031 g/ml; LDL-3: d = 1.034-1.037 g/ml; LDL-6: d = 1.044-1.063 g/ml) was determined by X-ray small-angle scattering. By using a theoretical particle model, which accounted for the polydispersity of the samples, we were able to obtain fits of the scattering intensity that were inside the noise interval of the measured intensity. The assumption of deviations from radial symmetry is not supported by our data. This implies a spread-out conformation of the apolipoprotein B (apoB) molecule, which appears to be localized in the outer surface shell. A globular structure is not consistent with our data. Furthermore, different models exist concerning the structure of the cholesterol ester core below the phase transition temperature. The electron density data suggest an arrangement in which the steroid moieties are localized at average radii of 3.2 and 6.4 nm. Model calculations show that packing problems can only be avoided if approximately half of the acyl chains of each shell are pointing towards the center of the particle, the other half towards the surface. This arrangement of the acyl chains has never been proposed before. The LDL particles of different density classes differ mainly with respect to the size of the core but also with respect to the width of the surface shells. Model calculations show that the size of different LDL particles can be accurately predicted from the compositional data.

  1. Two electron response to an intense x-ray free electron laser pulse

    Energy Technology Data Exchange (ETDEWEB)

    Moore, L R; Parker, J S; Meharg, K J; Armstrong, G S J; Taylor, K T, E-mail: l.moore@qub.ac.u [DAMTP, David Bates Building, Queen' s University Belfast, Belfast, BT7 1NN (United Kingdom)

    2009-11-01

    New x-ray free electron lasers (FELs) promise an ultra-fast ultra-intense regime in which new physical phenomena, such as double core hole formation in at atom, should become directly observable. Ahead of x-ray FEL experiments, an initial key task is to theoretically explore such fundamental laser-atom interactions and processes. To study the response of a two-electron positive ion to an intense x-ray FEL pulse, our theoretical approach is a direct numerical integration, incorporating non-dipole Hamiltonian terms, of the full six-dimensional time-dependent Schroedinger equation. We present probabilities of double K-shell ionization in the two-electron positive ions Ne{sup 8+} and Ar{sup 16+} exposed to x-ray FEL pulses with frequencies in the range 50 au to 300 au and intensities in the range 10{sup 17} to 10{sup 22} W/cm{sup 2}.

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

    Science.gov (United States)

    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.

  3. Analyzing three-dimensional position of region of interest using an image of contrast media using unilateral X-ray exposure

    International Nuclear Information System (INIS)

    Harauchi, Hajime; Gotou, Hiroshi; Tanooka, Masao

    1994-01-01

    Analyzing three-dimensional internal structure of object in an X-ray study is usually performed by using two or more of the incidents of an X-ray direction. In this report, we analyzed the three-dimensional position of tubes with a phantom by using both contrast media and imaging of one direction in the X-ray study. The concentration of the iodine in contrast media can be known by using the log-subtraction image of only the one-directional incident X-ray. Also the diameter of tube filled with contrast media is calculated by the concentration of iodine. So we can show the three-dimensional position of tubes geometrically, by the diameter of tube and the measured value of the film. We verified this method by an experiment according to the theory. (author)

  4. The over-the-limb hard X-ray events

    Science.gov (United States)

    Hudson, H. S.

    Over-the-limb hard X-ray events offer a uniquely direct view of the hard X-ray emission from the solar corona during a major flare. Limb occultation at angles greater than about 10 deg (an arbitrary definition of this class of events) excludes any confusion with brighter chromospheric sources. Published observations of seven over-the-limb events, beginning with the prototype flare of March 30, 1969, are reviewed. The hard X-ray spectra appear to fall into two classes: hard events, with power-law index of about 2.0; and soft events, with power-law index about 5.4. This tendency towards bimodality is only significant at the 90-percent confidence level due to the smallness of the number of events observed to date. If borne out by future data, the bimodality would suggest the existence of two different acceleration mechanisms.

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

    International Nuclear Information System (INIS)

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

    2013-01-01

    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

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

    Energy Technology Data Exchange (ETDEWEB)

    Boiko, M. E., E-mail: m.e.boiko@mail.ioffe.ru; Sharkov, M. D.; Boiko, A. M.; Bobyl, A. V. [Russian Academy of Sciences, Ioffe Physicotechnical Institute (Russian Federation)

    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

    Science.gov (United States)

    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. Solution small-angle x-ray scattering as a screening and predictive tool in the fabrication of asymmetric block copolymer membranes

    KAUST Repository

    Dorin, Rachel Mika; Marques, Debora S.; Sai, Hiroaki; Vainio, Ulla; Phillip, William A.; Peinemann, Klaus; Nunes, Suzana Pereira; Wiesner, Ulrich B.

    2012-01-01

    Small-angle X-ray scattering (SAXS) analysis of the diblock copolymer poly(styrene-b-(4-vinyl)pyridine) in a ternary solvent system of 1,4-dioxane, tetrahydrofuran, and N,N-dimethylformamide, and the triblock terpolymer poly(isoprene-b-styrene-b-(4-vinyl)-pyridine) in a binary solvent system of 1,4-dioxane and tetrahydrofuran, reveals a concentration-dependent onset of ordered structure formation. Asymmetric membranes fabricated from casting solutions with polymer concentrations at or slightly below this ordering concentration possess selective layers with the desired nanostructure. In addition to rapidly screening possible polymer solution concentrations, solution SAXS analysis also predicts hexagonal and square pore lattices of the final membrane surface structure. These results suggest solution SAXS as a powerful tool for screening casting solution concentrations and predicting surface structure in the fabrication of asymmetric ultrafiltration membranes from self-assembled block copolymers. (Figure presented) © 2012 American Chemical Society.

  9. Solution small-angle x-ray scattering as a screening and predictive tool in the fabrication of asymmetric block copolymer membranes

    KAUST Repository

    Dorin, Rachel Mika

    2012-05-15

    Small-angle X-ray scattering (SAXS) analysis of the diblock copolymer poly(styrene-b-(4-vinyl)pyridine) in a ternary solvent system of 1,4-dioxane, tetrahydrofuran, and N,N-dimethylformamide, and the triblock terpolymer poly(isoprene-b-styrene-b-(4-vinyl)-pyridine) in a binary solvent system of 1,4-dioxane and tetrahydrofuran, reveals a concentration-dependent onset of ordered structure formation. Asymmetric membranes fabricated from casting solutions with polymer concentrations at or slightly below this ordering concentration possess selective layers with the desired nanostructure. In addition to rapidly screening possible polymer solution concentrations, solution SAXS analysis also predicts hexagonal and square pore lattices of the final membrane surface structure. These results suggest solution SAXS as a powerful tool for screening casting solution concentrations and predicting surface structure in the fabrication of asymmetric ultrafiltration membranes from self-assembled block copolymers. (Figure presented) © 2012 American Chemical Society.

  10. Development of small scale soft x-ray lasers

    International Nuclear Information System (INIS)

    Kim, D.; Suckewer, S.; Princeton Univ., NJ; Skinner, C.H.; Voorhees, D.

    1991-05-01

    At present rapid progress is being made in the application of soft x-ray lasers to fields such as microscopy and microlithography. A critical factor in the range of suitable applications is the scale and hence cost of the soft x-ray lasers. At Princeton, gain at 183 angstrom has been obtained with relatively low pump laser energies (as low as 6J) in a ''portable'' small-scale soft x-ray laser system. We will also discuss aspects of data interpretation and pitfalls to be avoided in measurements of gain in such systems. 14 refs., 7 figs

  11. Elasticity of Tantalum to 105 Gpa using a stress and angle-resolved x-ray diffraction

    International Nuclear Information System (INIS)

    Cynn, H; Yoo, C S

    1999-01-01

    Determining the mechanical properties such as elastic constants of metals at Mbar pressures has been a difficult task in experiment. Following the development of anisotropic elastic theory by Singh et al.[l], Mao et a1.[2] have recently developed a novel experimental technique to determine the elastic constants of Fe by using the stress and energy-dispersive x-ray diffraction (SEX). In this paper, we present an improved complementary technique, stress and angle-resolved x-ray diffraction (SAX), which we have applied to determine the elastic constants of tantalum to 105 GPa. The extrapolation of the tantalum elastic data shows an excellent agreement with the low-pressure ultrasonic data[3]. We also discuss the improvement of this SAX method over the previous SEX.[elastic constant, anisotropic elastic theory, angle-dispersive synchrotron x-ray diffraction, mechanical properties

  12. Controlling X-ray beam trajectory with a flexible hollow glass fibre

    Energy Technology Data Exchange (ETDEWEB)

    Tanaka, Yoshihito, E-mail: yotanaka@riken.jp [RIKEN, 1-1-1 Kouto, Sayo-cho, Hyogo 679-5148 (Japan); Kwansei Gakuin University, Gakuen, Sanda, Hyogo 669-1337 (Japan); Nakatani, Takashi; Onitsuka, Rena [Kwansei Gakuin University, Gakuen, Sanda, Hyogo 669-1337 (Japan); Sawada, Kei [RIKEN, 1-1-1 Kouto, Sayo-cho, Hyogo 679-5148 (Japan); Takahashi, Isao [Kwansei Gakuin University, Gakuen, Sanda, Hyogo 669-1337 (Japan)

    2014-01-01

    X-ray beam trajectory control has been performed by using a 1.5 m-long flexible hollow glass fibre. A two-dimensional scan of a synchrotron radiation beam was demonstrated for X-ray absorption mapping. A metre-length flexible hollow glass fibre with 20 µm-bore and 1.5 mm-cladding diameters for transporting a synchrotron X-ray beam and controlling the trajectory has been examined. The large cladding diameter maintains a moderate curvature to satisfy the shallow glancing angle of total reflection. The observed transmission efficiency was more than 20% at 12.4 keV. As a demonstration, a wide-area scan of a synchrotron radiation beam was performed to identify the elements for a fixed metal film through its absorption spectra.

  13. Surface and interface strains studied by x-ray diffraction

    International Nuclear Information System (INIS)

    Akimoto, Koichi; Emoto, Takashi; Ichimiya, Ayahiko

    1998-01-01

    The authors have developed a technique of X-ray diffraction in order to measure strain fields near semiconductor surface and interface. The diffraction geometry is using the extremely asymmetric Bragg-case bulk reflection of a small incident angle to the surface and a large angle exiting from the surface. The incident angle of the X-rays is set near critical angle of total reflection by tuning X-ray energy of synchrotron radiation at the Photon Factory, Japan. For thermally grown-silicon oxide/Si(100) interface, the X-ray intensity of the silicon substrate 311 reflection has been measured. From comparison of the full width at half maxima (FWHM) of X-ray rocking curves of various thickness of silicon oxides, it has been revealed that silicon substrate lattice is highly strained in the thin (less than about 5 nm) silicon oxide/silicon system. In order to know the original silicon surface strain, the authors have also performed the same kind of measurements in the ultra-high vacuum chamber. A clean Si(111) 7x7 surface gives sharper X-ray diffraction peak than that of the native oxide/Si(111) system. From these measurements, it is concluded that the thin silicon oxide film itself gives strong strain fields to the silicon substrates, which may be the reason of the existence of the structural transition layer at the silicon oxide/Si interface

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

    Science.gov (United States)

    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.

  15. Residual stress analysis on materials with steep stress gradient by using X-ray incidence at higher angles

    International Nuclear Information System (INIS)

    Ohya, Shin-ichi; Yoshioka, Yasuo; Maeno, Shigeki

    1996-01-01

    X-ray stress measurements for isotropic polycrystalline are materials are usually carried out by the sin 2 ψ method under the assumption of no stress gradient in X-ray penetration depth. When a steep stress gradient exists in the vicinity of surface layer, however, non-linear sin 2 ψ relation is observed and the sin 2 ψ method cannot be applied on such cases. Although several X-ray stress analyzers have been developed for materials with steep stress gradient in the surface layer, it is desirable to use diffraction data at higher incident angles of ψ 0 as possible as close on 90 degrees in order to determine the both values of surface stress and stress gradient with high accuracy. In the present study, an X-ray stress analyzer based on Ω geometry was fabricated to enable X-ray incidence at higher angle of ψ 0 . The X-ray detector was positioned on -η side against X-ray incident beam. Both of the residual surface stress and stress gradient were determined by use of the COSψ method on shot-peened steel and silicon nitride specimens. This prototype stress analyzer was found effective to perform a biaxial or triaxial stress analysis. (author)

  16. Investigation of the topological shape of bovine serum albumin in solution by small-angle x-ray scattering at Beijing synchrotron radiation facility

    International Nuclear Information System (INIS)

    Dong Shuqiang; Chen Ximeng; Li Liqin; Liu Peng; Dong Yuhui

    2008-01-01

    This paper reports that at a newly constructed small-angle x-ray scattering station of Beijing Synchrotron Radiation Facility, the topological shape of ligand-free bovine serum albumin in solution has been investigated. An appropriate scattering curve is obtained and the calculated value of the gyration radius is 31.2ű0.25A (1Å=0.1 nm) which is coincident with other ones' results. It finds that the low-resolution structure models obtained by making use of ab initio reconstruction methods are fitting the crystal structure of human serum albumin very well. All of these results perform the potential of the beamline to apply to structural biology studies. The characteristics, the defects, and the improving measures of the station in future are also discussed. (condensed matter: structure, thermal and mechanical properties)

  17. Photoelectron and x-ray holography by contrast: enhancing image quality and dimensionality

    Energy Technology Data Exchange (ETDEWEB)

    Fadley, C.S.; Zhao, L. [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA (United States); Department of Physics, University of California, Davis, CA (United States); Hove, M.A. van [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA (United States); Department of Physics, University of California, Davis, CA (United States); Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA (United States); Kaduwela, A.; Marchesini, S. [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA (United States); Omori, S. [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA (United States); Institute of Industrial Science, University of Tokyo, Tokyo (Japan); Sony Corporation Semiconductor Network Company, Asahi-cho, Atsugi, Kanagawa (Japan)

    2001-11-26

    Three forms of electron or x-ray holography 'by contrast' are discussed: they all exploit small changes in diffraction conditions to improve image quality and/or extract additional information. Spin-polarized photoelectron holography subtracts spin-down from spin-up holograms so as to image the relative orientations of atomic magnetic moments around an emitter atom. Differential photoelectron holography subtracts holograms taken at slightly different energies so as to overcome the forward-scattering problem that normally degrades the three-dimensional imaging of atoms, particularly for emitter atoms that are part of a bulk substrate environment. Resonant x-ray fluorescence holography also subtracts holograms at slightly different energies, these being chosen above and below an absorption edge of a constituent atom, thus allowing the selective imaging of that type of atom, or what has been referred to as imaging 'in true colour'. (author)

  18. Two dimensional CCD [charged coupled device] arrays as parallel detectors in electron energy loss and x-ray wavelength dispersive spectroscopy

    International Nuclear Information System (INIS)

    Zaluzec, N.J.

    1988-08-01

    Parallel detection systems for spectroscopy have generally been based upon linear detector arrays. Replacing the linear arrays with two dimensional systems yields more complicated devices; however, there are corresponding benefits which can be realized for both x-ray and electron energy loss spectroscopy. The operational design of these systems, as well as preliminary results from the construction of such a device used for electron spectroscopy, are presented. 10 refs., 8 figs

  19. A small angle X-ray scattering method to investigate the crack tip in metals. Final report of the Marie Curie individual fellowship project

    International Nuclear Information System (INIS)

    Ouytsel, K. van; Boehmert, J.; Mueller, G.

    2003-08-01

    Structural materials, such as ferritic and austenitic steels or aluminium alloys used in the nuclear and aircraft industry, are subjected to external operational loads in different environments. Adopting a damage tolerant design principle, understanding the growth of preexisting or newly formed cracks under these conditions is of prime relevance to prevent extensive crack propagation and failure of the component. Within this framework, the characterization of early stages of the damage processes, as nucleation, growth and coalescence of micro-voids and the evolution of the spatial dislocation distribution (dislocation patterning) is a particularly challenging aspect. It was the objective of the work performed to investigate the damage structure near a crack tip by means of small angle X-ray scattering (SAXS). Pre-cracked fracture mechanics standard specimens from different aluminium alloys and steels were loaded up to different amounts of crack growth. From the crack tip range samples of 100 to 200 μm thickness were prepared and a small region around the crack tip was scanned using a microfocused Synchrotron beam. The SAXS experiments were performed at different Synchrotron sources and equipments with different beam cross section, scan step width and X-ray energy. Additionally, the investigation was completed by other methods like X-ray diffraction, X-ray imaging diffraction technique (MAXIM), transmission electron microscopy, scanning electron microscopy, and positron annihilation spectroscopy. The SAXS intensity pattern shows location-related effects. Potential SAXS parameters to characterize the damage are the integral intensity, a fractal dimension parameter and a value determined from the ratio of the intensity vertical and horizontal to the direction of crack growth. Above all, the last parameter is suitable to depict the damage zone around the crack tip. It is robust and applicable even for a material which exhibits an anisotropic SAXS pattern in the

  20. The methods for detecting multiple small nodules from 3D chest X-ray CT images

    International Nuclear Information System (INIS)

    Hayase, Yosuke; Mekada, Yoshito; Mori, Kensaku; Toriwaki, Jun-ichiro; Natori, Hiroshi

    2004-01-01

    This paper describes a method for detecting small nodules, whose CT values and diameters are more than -600 Hounsfield unit (H.U.) and 2 mm, from three-dimensional chest X-ray CT images. The proposed method roughly consists of two submodules: initial detection of nodule candidates by discriminating between nodule regions and other regions such as blood vessels or bronchi using a shape feature computed from distance values inside the regions and reduction of false positive (FP) regions by using a minimum directional difference filter called minimum directional difference filter (Min-DD) changing its radius suit to the size of the initial candidates. The performance of the proposed method was evaluated by using seven cases of chest X-ray CT images including six abnormal cases where multiple lung cancers are observed. The experimental results for nodules (361 regions in total) showed that sensitivity and FP regions are 71% and 7.4 regions in average per case. (author)

  1. Nanoparticle-Assisted Scanning Focusing X-Ray Therapy with Needle Beam X Rays.

    Science.gov (United States)

    Davidson, R Andrew; Guo, Ting

    2016-01-01

    In this work, we show a new therapeutic approach using 40-120 keV X rays to deliver a radiation dose at the isocenter located many centimeters below the skin surface several hundred times greater than at the skin and how this dose enhancement can be augmented with nanomaterials to create several thousand-fold total dose enhancement effect. This novel approach employs a needle X-ray beam directed at the isocenter centimeters deep in the body while continuously scanning the beam to cover a large solid angle without overlapping at the skin. A Monte Carlo method was developed to simulate an X-ray dose delivered to the isocenter filled with X-ray absorbing and catalytic nanoparticles in a water phantom. An experimental apparatus consisting of a moving plastic phantom irradiated with a stationary 1 mm needle X-ray beam was built to test the theoretical predictions. X-ray films were used to characterize the dose profiles of the scanning X-ray apparatus. Through this work, it was determined that the X-ray dose delivered to the isocenter in a treatment voxel (t-voxel) underneath a 5 cm deep high-density polyethylene (HDPE) phantom was 295 ± 48 times greater than the surface dose. This measured value was in good agreement with the theoretical predicted value of 339-fold. Adding X-ray-absorbing nanoparticles, catalytic nanoparticles or both into the t-voxel can further augment the dose enhancement. For example, we predicted that adding 1 weight percentage (wp) of gold into water could increase the effective dose delivered to the target by onefold. Dose enhancement using 1 mm X-ray beam could reach about 1,600-fold in the t-voxel when 7.5 wp of 88 nm diameter silica-covered gold nanoparticles were added, which we showed in a previously published study can create a dose enhancement of 5.5 ± 0.46-fold without scanning focusing enhancement. Based on the experimental data from that study, mixing 0.02 wp 2.5 nm diameter small tetrakis hydroxymethyl phosphonium chloride (THPC

  2. Structure of a mouse immunoglobulin G that lacks the entire C sub H 1 domain: Protein sequencing and small-angle X-ray scattering studies

    Energy Technology Data Exchange (ETDEWEB)

    Igarashi, Takako; Tanaka, Toshiyuki; Nakanishi, Mamoru; Arata, Yoji (Univ. of Tokyo (Japan)); Sato, Mamoru; Katsube, Yukiteru (Osaka Univ. (Japan)); Takio, Koji (Institute of Physical and Chemical Research, Saitama (Japan))

    1990-06-19

    The structure of a short-chain IgG2a antibody, which is a member of the family of mouse anti-dansyl switch variant antibodies with identical variable regions but different heavy-chain constant regions, is reported. Amino acid sequencing analyses have demonstrated that in the short-chain IgG2a antibody the entire C{sub H}1 domain is deleted whereas the hinge region remains intact. Small-angle X-ray scattering data were collected for the short-chain IgG2a antibody and compared with those for the switch variant IgG1, IgG2a, and IgG2b antibodies with the normal heavy chain. It has been concluded that deletion of the C{sub H}1 domain results in a large structural change and the short-chain IgG2a antibody possesses an elongated molecular shape with a much smaller hinge angle as compared with the normal IgG2a antibody that is a Y-shaped molecule.

  3. A new streaked soft x-ray imager for the National Ignition Facility

    Energy Technology Data Exchange (ETDEWEB)

    Benstead, J., E-mail: james.benstead@awe.co.uk; Morton, J.; Guymer, T. M.; Garbett, W. J.; Rubery, M. S.; Skidmore, J. W. [AWE, Aldermaston, Reading, Berkshire RG7 4PR (United Kingdom); Moore, A. S.; Ahmed, M. F.; Soufli, R.; Pardini, T.; Hibbard, R. L.; Bailey, C. G.; Bell, P. M.; Hau-Riege, S. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Bedzyk, M.; Shoup, M. J.; Reagan, S.; Agliata, T.; Jungquist, R. [Laboratory for Laser Energetics, University of Rochester, Rochester, New York 14623 (United States); Schmidt, D. W. [Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (United States); and others

    2016-05-15

    A new streaked soft x-ray imager has been designed for use on high energy-density (HED) physics experiments at the National Ignition Facility based at the Lawrence Livermore National Laboratory. This streaked imager uses a slit aperture, single shallow angle reflection from a nickel mirror, and soft x-ray filtering to, when coupled to one of the NIF’s x-ray streak cameras, record a 4× magnification, one-dimensional image of an x-ray source with a spatial resolution of less than 90 μm. The energy band pass produced depends upon the filter material used; for the first qualification shots, vanadium and silver-on-titanium filters were used to gate on photon energy ranges of approximately 300–510 eV and 200–400 eV, respectively. A two-channel version of the snout is available for x-ray sources up to 1 mm and a single-channel is available for larger sources up to 3 mm. Both the one and two-channel variants have been qualified on quartz wire and HED physics target shots.

  4. Two-dimensional x-ray magnification based on a monolithic beam conditioner

    Czech Academy of Sciences Publication Activity Database

    Korytár, D.; Mikulík, P.; Ferrari, C.; Hrdý, Jaromír; Baumbach, T.; Freund, A.; Kuběna, A.

    2003-01-01

    Roč. 36, - (2003), s. 1-4 ISSN 0022-3727 R&D Projects: GA AV ČR IAA1010104; GA MŠk OC P7.001 Institutional research plan: CEZ:AV0Z1010914 Keywords : x-ray crystal diffraction * x-ray magnifier Subject RIV: BH - Optics, Masers, Lasers Impact factor: 1.265, year: 2003

  5. Two methods for studying the X-ray variability

    NARCIS (Netherlands)

    Yan, Shu-Ping; Ji, Li; Méndez, Mariano; Wang, Na; Liu, Siming; Li, Xiang-Dong

    2016-01-01

    The X-ray aperiodic variability and quasi-periodic oscillation (QPO) are the important tools to study the structure of the accretion flow of X-ray binaries. However, the origin of the complex X-ray variability from X-ray binaries remains yet unsolved. We proposed two methods for studying the X-ray

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

    International Nuclear Information System (INIS)

    Quiroz, 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 CO 2 and nickel ions to gain access to the nascent active site

  7. A gas microstrip wide angle X-ray detector for application in synchrotron radiation experiments

    CERN Document Server

    Bateman, J E; Derbyshire, G E; Duxbury, D M; Lipp, J; Mir, J A; Simmons, J E; Spill, E J; Stephenson, R; Dobson, B R; Farrow, R C; Helsby, W I; Mutikainen, R; Suni, I

    2002-01-01

    The Gas Microstrip Detector has counting rate capabilities several orders of magnitude higher than conventional wire proportional counters while providing the same (or better) energy resolution for X-rays. In addition the geometric flexibility provided by the lithographic process combined with the self-supporting properties of the substrate offers many exciting possibilities for X-ray detectors, particularly for the demanding experiments carried out on Synchrotron Radiation Sources. Using experience obtained in designing detectors for Particle Physics we have developed a detector for Wide Angle X-ray Scattering studies. The detector has a fan geometry which makes possible a gas detector with high detection efficiency, sub-millimetre spatial resolution and good energy resolution over a wide range of X-ray energy. The detector is described together with results of experiments carried out at the Daresbury Laboratory Synchrotron Radiation Source.

  8. The oblique view for spondylolysis in the growing period. X-ray projection angle to spondylolytic lumbar vertebra based on CT scanning

    Energy Technology Data Exchange (ETDEWEB)

    Kobayashi, Yoshimitsu; Minato, Izumi; Nagano, Junji; Inoue, Yoshiya; Takahashi, Yuji; Saito, Hidehiko [Seirei Hamamatsu General Hospital, Shizuoka (Japan)

    1996-02-01

    In this study, CT images of 239 vertebrae from 227 patients with spondylolysis in the growing period were obtained to analyze x-ray oblique separation images based on the relationship between x-ray incidence angle and CT. The age of the subjects ranged from 5 to 23 years (average 14.8 years), of which 224 patients were 18 years or lower. The CT images obtained were classified into four according to our classification, i.e., Type Ia, 112 vertebrae; Type Ib, 175; Type II, 66; Type III, 67. All patients underwent plain x-ray from 4 directions including 45deg. The angle of separation line and posterior margin of the vertebral body was obtained and the average angle of all slices was determined as separation angle. As a result, depiction level of separation line was better in 30deg oblique images than 45deg oblique images in Ia, Ib, and III groups. It is thus desirable to take the relationship between incidence angle of x-ray, separation angle, and CT classification into consideration. (S.Y.).

  9. The oblique view for spondylolysis in the growing period. X-ray projection angle to spondylolytic lumbar vertebra based on CT scanning

    International Nuclear Information System (INIS)

    Kobayashi, Yoshimitsu; Minato, Izumi; Nagano, Junji; Inoue, Yoshiya; Takahashi, Yuji; Saito, Hidehiko

    1996-01-01

    In this study, CT images of 239 vertebrae from 227 patients with spondylolysis in the growing period were obtained to analyze x-ray oblique separation images based on the relationship between x-ray incidence angle and CT. The age of the subjects ranged from 5 to 23 years (average 14.8 years), of which 224 patients were 18 years or lower. The CT images obtained were classified into four according to our classification, i.e., Type Ia, 112 vertebrae; Type Ib, 175; Type II, 66; Type III, 67. All patients underwent plain x-ray from 4 directions including 45deg. The angle of separation line and posterior margin of the vertebral body was obtained and the average angle of all slices was determined as separation angle. As a result, depiction level of separation line was better in 30deg oblique images than 45deg oblique images in Ia, Ib, and III groups. It is thus desirable to take the relationship between incidence angle of x-ray, separation angle, and CT classification into consideration. (S.Y.)

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

    Science.gov (United States)

    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

  11. Three-dimensional imaging of a complex concaved cuboctahedron copper sulfide crystal by x-ray nanotomography

    International Nuclear Information System (INIS)

    Chen Jie; Tian Jinping; Li Wenjie; Tian Yangchao; Wu Chunyan; Yu Shuhong

    2008-01-01

    By combining Fresnel zone-plate based transmission x-ray microscopy with computed tomography, the nanoscale features in materials with complex shapes can be imaged using synchrotron radiation. The tomographic data sets of a complex copper sulfide crystal were acquired in the angle range ±70 deg. at photon energy of 8.0 keV and then were reconstructed by a standard filtered-back-projection algorithm. This experiment shows the quantifiable three-dimensional information of the copper sulfide crystal, which offers a complete understanding of the concaved cuboctahedron structure with 14 faces comprising of six squares and eight triangles

  12. Dimensional Crossover in a Charge Density Wave Material Probed by Angle-Resolved Photoemission Spectroscopy

    Science.gov (United States)

    Nicholson, C. W.; Berthod, C.; Puppin, M.; Berger, H.; Wolf, M.; Hoesch, M.; Monney, C.

    2017-05-01

    High-resolution angle-resolved photoemission spectroscopy data reveal evidence of a crossover from one-dimensional (1D) to three-dimensional (3D) behavior in the prototypical charge density wave (CDW) material NbSe3 . In the low-temperature 3D regime, gaps in the electronic structure are observed due to two incommensurate CDWs, in agreement with x-ray diffraction and electronic-structure calculations. At higher temperatures we observe a spectral weight depletion that approaches the power-law behavior expected in one dimension. From the warping of the quasi-1D Fermi surface at low temperatures, we extract the energy scale of the dimensional crossover. This is corroborated by a detailed analysis of the density of states, which reveals a change in dimensional behavior dependent on binding energy. Our results offer an important insight into the dimensionality of excitations in quasi-1D materials.

  13. Development of variable-magnification X-ray Bragg optics.

    Science.gov (United States)

    Hirano, Keiichi; Yamashita, Yoshiki; Takahashi, Yumiko; Sugiyama, Hiroshi

    2015-07-01

    A novel X-ray Bragg optics is proposed for variable-magnification of an X-ray beam. This X-ray Bragg optics is composed of two magnifiers in a crossed arrangement, and the magnification factor, M, is controlled through the azimuth angle of each magnifier. The basic properties of the X-ray optics such as the magnification factor, image transformation matrix and intrinsic acceptance angle are described based on the dynamical theory of X-ray diffraction. The feasibility of the variable-magnification X-ray Bragg optics was verified at the vertical-wiggler beamline BL-14B of the Photon Factory. For X-ray Bragg magnifiers, Si(220) crystals with an asymmetric angle of 14° were used. The magnification factor was calculated to be tunable between 0.1 and 10.0 at a wavelength of 0.112 nm. At various magnification factors (M ≥ 1.0), X-ray images of a nylon mesh were observed with an air-cooled X-ray CCD camera. Image deformation caused by the optics could be corrected by using a 2 × 2 transformation matrix and bilinear interpolation method. Not only absorption-contrast but also edge-contrast due to Fresnel diffraction was observed in the magnified images.

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

    Science.gov (United States)

    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.

  15. Level-set reconstruction algorithm for ultrafast limited-angle X-ray computed tomography of two-phase flows.

    Science.gov (United States)

    Bieberle, M; Hampel, U

    2015-06-13

    Tomographic image reconstruction is based on recovering an object distribution from its projections, which have been acquired from all angular views around the object. If the angular range is limited to less than 180° of parallel projections, typical reconstruction artefacts arise when using standard algorithms. To compensate for this, specialized algorithms using a priori information about the object need to be applied. The application behind this work is ultrafast limited-angle X-ray computed tomography of two-phase flows. Here, only a binary distribution of the two phases needs to be reconstructed, which reduces the complexity of the inverse problem. To solve it, a new reconstruction algorithm (LSR) based on the level-set method is proposed. It includes one force function term accounting for matching the projection data and one incorporating a curvature-dependent smoothing of the phase boundary. The algorithm has been validated using simulated as well as measured projections of known structures, and its performance has been compared to the algebraic reconstruction technique and a binary derivative of it. The validation as well as the application of the level-set reconstruction on a dynamic two-phase flow demonstrated its applicability and its advantages over other reconstruction algorithms. © 2015 The Author(s) Published by the Royal Society. All rights reserved.

  16. JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

    Science.gov (United States)

    Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

    2006-01-01

    X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

  17. Three dimensional subsurface elemental identification of minerals using confocal micro-X-ray fluorescence and micro-X-ray computed tomography

    International Nuclear Information System (INIS)

    Cordes, Nikolaus L.; Seshadri, Srivatsan; Havrilla, George J.; Yuan, Xiaoli; Feser, Michael; Patterson, Brian M.

    2015-01-01

    Current non-destructive elemental characterization methods, such as scanning electron microscopy-based energy dispersive spectroscopy (SEM–EDS) and micro-X-ray fluorescence spectroscopy (MXRF), are limited to either elemental identification at the surface (SEM–EDS) or suffer from an inability to discriminate between surface or depth information (MXRF). Thus, a non-destructive elemental characterization of individual embedded particles beneath the surface is impossible with either of these techniques. This limitation can be overcome by using laboratory-based 3D confocal micro-X-ray fluorescence spectroscopy (confocal MXRF). This technique utilizes focusing optics on the X-ray source and detector which allows for spatial discrimination in all three dimensions. However, the voxel-by-voxel serial acquisition of a 3D elemental scan can be very time-intensive (~ 1 to 4 weeks) if it is necessary to locate individual embedded particles of interest. As an example, if each point takes a 5 s measurement time, a small volume of 50 × 50 × 50 pixels leads to an acquisition time of approximately 174 h, not including sample stage movement time. Initially screening the samples for particles of interest using micro-X-ray computed tomography (micro-CT) can significantly reduce the time required to spatially locate these particles. Once located, these individual particles can be elementally characterized with confocal MXRF. Herein, we report the elemental identification of high atomic number surface and subsurface particles embedded in a mineralogical matrix by coupling micro-CT and confocal MXRF. Synergistically, these two X-ray based techniques first rapidly locate and then elementally identify individual subsurface particles. - Highlights: • Coupling of confocal X-ray fluorescence spectroscopy and X-ray computed tomography • Qualitative elemental identification of surface and subsurface mineral particles • Non-destructive particle size measurements • Utilization of

  18. Three dimensional subsurface elemental identification of minerals using confocal micro-X-ray fluorescence and micro-X-ray computed tomography

    Energy Technology Data Exchange (ETDEWEB)

    Cordes, Nikolaus L., E-mail: ncordes@lanl.gov [Polymers and Coatings Group, Material Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Seshadri, Srivatsan, E-mail: srivatsan.seshadri@zeiss.com [Carl Zeiss X-ray Microscopy, Inc., Pleasanton, CA 94588 (United States); Havrilla, George J. [Chemical Diagnostics and Engineering, Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Yuan, Xiaoli [Julius Kruttschnitt Mineral Research Centre, University of Queensland, Indooroopilly, Brisbane, QLD 4068 (Australia); Feser, Michael [Carl Zeiss X-ray Microscopy, Inc., Pleasanton, CA 94588 (United States); Patterson, Brian M. [Polymers and Coatings Group, Material Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2015-01-01

    Current non-destructive elemental characterization methods, such as scanning electron microscopy-based energy dispersive spectroscopy (SEM–EDS) and micro-X-ray fluorescence spectroscopy (MXRF), are limited to either elemental identification at the surface (SEM–EDS) or suffer from an inability to discriminate between surface or depth information (MXRF). Thus, a non-destructive elemental characterization of individual embedded particles beneath the surface is impossible with either of these techniques. This limitation can be overcome by using laboratory-based 3D confocal micro-X-ray fluorescence spectroscopy (confocal MXRF). This technique utilizes focusing optics on the X-ray source and detector which allows for spatial discrimination in all three dimensions. However, the voxel-by-voxel serial acquisition of a 3D elemental scan can be very time-intensive (~ 1 to 4 weeks) if it is necessary to locate individual embedded particles of interest. As an example, if each point takes a 5 s measurement time, a small volume of 50 × 50 × 50 pixels leads to an acquisition time of approximately 174 h, not including sample stage movement time. Initially screening the samples for particles of interest using micro-X-ray computed tomography (micro-CT) can significantly reduce the time required to spatially locate these particles. Once located, these individual particles can be elementally characterized with confocal MXRF. Herein, we report the elemental identification of high atomic number surface and subsurface particles embedded in a mineralogical matrix by coupling micro-CT and confocal MXRF. Synergistically, these two X-ray based techniques first rapidly locate and then elementally identify individual subsurface particles. - Highlights: • Coupling of confocal X-ray fluorescence spectroscopy and X-ray computed tomography • Qualitative elemental identification of surface and subsurface mineral particles • Non-destructive particle size measurements • Utilization of

  19. Preliminary Examination of X-ray Scattering from Human Tissues

    International Nuclear Information System (INIS)

    Desouky, O.S.; Wilkinson, S.; Hall, C.; Rogers, K.; Round, A.

    2008-01-01

    Small Angle x-ray scattering (SAXS) and wide angle x-ray scattering (WAXS) patterns have been recorded from different human soft tissues using x-ray synchrotron radiation.Pathological breast, normal kidney and lung tissues show SAXS peaks at q-values equal to 0.291 nm -1 and 0.481 nm -1 (d 21.6 nm and d =13. nm) which are the 3 r d and 5 t h order of the well known axial D-spacing of collagen fibrils. The diffraction is particularly intense in the meridional direction indicating some febrile alignment. In contrast, the normal tissue of brain, liver and heart shows diffuse scatter.The wide-angle coherent scattering from normal human tissues of brain, liver, heart, lung, and kidney is typical of that for amorphous materials. The scatter of the healthy adipose breast tissue shows a sharp peak at momentum transfer 1.24 nm -1 (d= 0.417 nm). The data of the other tissues appears to consist of a broad scattering peak. The two scattering regimes succeed in differentiating between the two major components of breast tissue, collagen and adipose tissue. The results of this study suggest that the soft tissues may have scattering patterns that are characteristics for the particular tissue types and tissue disease state. These results indicate that it may be possible use the coherent scattering as a diagnostic tool

  20. Wavelet-based feature extraction applied to small-angle x-ray scattering patterns from breast tissue: a tool for differentiating between tissue types

    International Nuclear Information System (INIS)

    Falzon, G; Pearson, S; Murison, R; Hall, C; Siu, K; Evans, A; Rogers, K; Lewis, R

    2006-01-01

    This paper reports on the application of wavelet decomposition to small-angle x-ray scattering (SAXS) patterns from human breast tissue produced by a synchrotron source. The pixel intensities of SAXS patterns of normal, benign and malignant tissue types were transformed into wavelet coefficients. Statistical analysis found significant differences between the wavelet coefficients describing the patterns produced by different tissue types. These differences were then correlated with position in the image and have been linked to the supra-molecular structural changes that occur in breast tissue in the presence of disease. Specifically, results indicate that there are significant differences between healthy and diseased tissues in the wavelet coefficients that describe the peaks produced by the axial d-spacing of collagen. These differences suggest that a useful classification tool could be based upon the spectral information within the axial peaks

  1. Application of space-angle synthesis to two-dimensional neutral-particle transport problems of weapon physics

    International Nuclear Information System (INIS)

    Roberds, R.M.

    1975-01-01

    A space-angle synthesis (SAS) method has been developed for treating the steady-state, two-dimensional transport of neutrons and gamma rays from a point source of simulated nuclear weapon radiation in air. The method was validated by applying it to the problem of neutron transport from a point source in air over a ground interface, and then comparing the results to those obtained by DOT, a state-of-the-art, discrete-ordinates code. In the SAS method, the energy dependence of the Boltzmann transport equation was treated in the standard multigroup manner. The angular dependence was treated by expanding the flux in specially tailored trial functions and applying the method of weighted residuals which analytically integrated the transport equation over all angles. The weighted-residual approach was analogous to the conventional spherical-harmonics (P/sub N/) method with the exception that the tailored expansion allowed for more rapid convergence than a spherical-harmonics P 1 expansion and resulted in a greater degree of accuracy. The trial functions used in the expansion were odd and even combinations of selected trial solutions, the trial solutions being shaped ellipsoids which approximated the angular distribution of the neutron flux in one-dimensional space. The parameters which described the shape of the ellipsoid varied with energy group and the spatial medium, only, and were obtained from a one-dimensional discrete-ordinates calculation. Thus, approximate transport solutions were made available for all two-dimensional problems of a certain class by using tabulated parameters obtained from a single, one-dimensional calculation

  2. X-ray holography. Atoms in three dimensions

    International Nuclear Information System (INIS)

    Tegze, M.

    2005-01-01

    The principles of atomic resolution X-ray holography was elaborated in 1991. X-ray photons scatter thousand times less on atoms than electrons of the same wavelength. As a result, both free path and penetration depth are higher which giver information about the bulk material. X-ray holography is realized by irradiating the single crystal sample with radiation from external X-ray source. The incident radiation is ionizing the atoms of the sample to emit fluorescent radiation. The angle dependence of the fluorescent radiation results an image containing the hologram. The hologram itself is extremely small compared to the background that needs 10 10 capturing photons to recover image. Using Thomas Gog's method and synchrotron radiation the X-ray holography becomes more usable, but the method still needs refining both experimentally and theoretically. (TRA)

  3. Performance verification of the Gravity and Extreme Magnetism Small explorer (GEMS) x-ray polarimeter

    Science.gov (United States)

    Enoto, Teruaki; Black, J. Kevin; Kitaguchi, Takao; Hayato, Asami; Hill, Joanne E.; Jahoda, Keith; Tamagawa, Toru; Kaneko, Kenta; Takeuchi, Yoko; Yoshikawa, Akifumi; Marlowe, Hannah; Griffiths, Scott; Kaaret, Philip E.; Kenward, David; Khalid, Syed

    2014-07-01

    Polarimetry is a powerful tool for astrophysical observations that has yet to be exploited in the X-ray band. For satellite-borne and sounding rocket experiments, we have developed a photoelectric gas polarimeter to measure X-ray polarization in the 2-10 keV range utilizing a time projection chamber (TPC) and advanced micro-pattern gas electron multiplier (GEM) techniques. We carried out performance verification of a flight equivalent unit (1/4 model) which was planned to be launched on the NASA Gravity and Extreme Magnetism Small Explorer (GEMS) satellite. The test was performed at Brookhaven National Laboratory, National Synchrotron Light Source (NSLS) facility in April 2013. The polarimeter was irradiated with linearly-polarized monochromatic X-rays between 2.3 and 10.0 keV and scanned with a collimated beam at 5 different detector positions. After a systematic investigation of the detector response, a modulation factor >=35% above 4 keV was obtained with the expected polarization angle. At energies below 4 keV where the photoelectron track becomes short, diffusion in the region between the GEM and readout strips leaves an asymmetric photoelectron image. A correction method retrieves an expected modulation angle, and the expected modulation factor, ~20% at 2.7 keV. Folding the measured values of modulation through an instrument model gives sensitivity, parameterized by minimum detectable polarization (MDP), nearly identical to that assumed at the preliminary design review (PDR).

  4. Performance Verification of the Gravity and Extreme Magnetism Small Explorer GEMS X-Ray Polarimeter

    Science.gov (United States)

    Enoto, Teruaki; Black, J. Kevin; Kitaguchi, Takao; Hayato, Asami; Hill, Joanne E.; Jahoda, Keith; Tamagawa, Toru; Kanako, Kenta; Takeuchi, Yoko; Yoshikawa, Akifumi; hide

    2014-01-01

    olarimetry is a powerful tool for astrophysical observations that has yet to be exploited in the X-ray band. For satellite-borne and sounding rocket experiments, we have developed a photoelectric gas polarimeter to measure X-ray polarization in the 2-10 keV range utilizing a time projection chamber (TPC) and advanced micro-pattern gas electron multiplier (GEM) techniques. We carried out performance verification of a flight equivalent unit (1/4 model) which was planned to be launched on the NASA Gravity and Extreme Magnetism Small Explorer (GEMS) satellite. The test was performed at Brookhaven National Laboratory, National Synchrotron Light Source (NSLS) facility in April 2013. The polarimeter was irradiated with linearly-polarized monochromatic X-rays between 2.3 and 10.0 keV and scanned with a collimated beam at 5 different detector positions. After a systematic investigation of the detector response, a modulation factor greater than or equal to 35% above 4 keV was obtained with the expected polarization angle. At energies below 4 keV where the photoelectron track becomes short, diffusion in the region between the GEM and readout strips leaves an asymmetric photoelectron image. A correction method retrieves an expected modulation angle, and the expected modulation factor, approximately 20% at 2.7 keV. Folding the measured values of modulation through an instrument model gives sensitivity, parameterized by minimum detectable polarization (MDP), nearly identical to that assumed at the preliminary design review (PDR).

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

    Science.gov (United States)

    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.

  6. Electronic configuration of the c(2 x 2)MnCu two-dimensional alloy in layered structures supported on Cu(100)

    International Nuclear Information System (INIS)

    Gallego, S; Munoz, M C; Huttel, Y; Avila, J; Asensio, M C

    2003-01-01

    The c(2 x 2)MnCu surface alloy on Cu(100) can be considered as a purely two-dimensional magnetic system where the Mn atoms exhibit a large corrugation closely related to their high spin moment. In this paper we investigate the influence of the atomic environment on the electronic and magnetic properties of the two-dimensional alloyed layer, extending our study to the less known multilayered system made of MnCu two-dimensional alloy layers embedded in a Cu crystal. The analysis is based on angle-resolved photoelectron spectroscopy measurements and calculations using the Green function matching method, which allows us to treat exactly the projection of the three-dimensional lattice on the c(2 x 2) plane. A complete study of the valence band is performed along the two-dimensional Brillouin zone in a wide energy range. We show that the presence of Mn results in an important redistribution of the spin-polarized electronic states of the neighbouring Cu atoms. This redistribution is not accompanied by a net charge transfer between different atoms, and also the spin moment of Cu remains small. Most of the new features induced by Mn in the surface alloy are also present in the multilayered system, evidencing that they are specific to the two-dimensional alloyed layer and not surface effects

  7. Unravelling the shape and structural assembly of the photosynthetic GAPDH-CP12-PRK complex from Arabidopsis thaliana by small-angle X-ray scattering analysis.

    Science.gov (United States)

    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.

  8. Method for spatially modulating X-ray pulses using MEMS-based X-ray optics

    Science.gov (United States)

    Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

    2015-03-10

    A method and apparatus are provided for spatially modulating X-rays or X-ray pulses using microelectromechanical systems (MEMS) based X-ray optics. A torsionally-oscillating MEMS micromirror and a method of leveraging the grazing-angle reflection property are provided to modulate X-ray pulses with a high-degree of controllability.

  9. Quantitative X-ray dark-field and phase tomography using single directional speckle scanning technique

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Sawhney, Kawal [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom)

    2016-03-21

    X-ray dark-field contrast tomography can provide important supplementary information inside a sample to the conventional absorption tomography. Recently, the X-ray speckle based technique has been proposed to provide qualitative two-dimensional dark-field imaging with a simple experimental arrangement. In this letter, we deduce a relationship between the second moment of scattering angle distribution and cross-correlation degradation of speckle and establish a quantitative basis of X-ray dark-field tomography using single directional speckle scanning technique. In addition, the phase contrast images can be simultaneously retrieved permitting tomographic reconstruction, which yields enhanced contrast in weakly absorbing materials. Such complementary tomography technique can allow systematic investigation of complex samples containing both soft and hard materials.

  10. Development of x-ray laminography under an x-ray microscopic condition

    International Nuclear Information System (INIS)

    Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa; Suzuki, Yoshio; Yagi, Naoto

    2011-01-01

    An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatial resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.

  11. Simulation study of two-energy X-ray fluorescence holograms reconstruction algorithm to remove twin images

    International Nuclear Information System (INIS)

    Xie Honglan; Hu Wen; Luo Hongxin; Deng Biao; Du Guohao; Xue Yanling; Chen Rongchang; Shi Shaomeng; Xiao Tiqiao

    2008-01-01

    Unlike traditional outside-source holography, X-ray fluorescence holography is carded out with fluorescent atoms in a sample as source light for holographic imaging. With the method, three-dimensional arrangement of atoms into crystals can be observed obviously. However, just like traditional outside-source holography, X-ray fluorescence holography suffers from the inherent twin-image problem, too. With a 27-Fe-atoms cubic lattice as model, we discuss in this paper influence of the photon energy of incident source in removing twin images in reconstructed atomic images by numerical simulation and reconstruction with two-energy X-ray fluorescence holography. The results indicate that incident X-rays of nearer energies have better effect of removing twin images. In the detector of X-ray holography, minimum difference of the two incident energies depends on energy resolution of the monochromator and detector, and for inside source X-ray holography, minimum difference of the two incident energies depends on difference of two neighboring fluorescent energies emitting from the element and energy resolution of detector. The spatial resolution of atomic images increases with the incident energies. This is important for experiments of X-ray fluorescence holography, which is being developed on Shanghai Synchrotron Radiation Facility. (authors)

  12. The neutron small-angle camera D11 at the high-flux reactor, Grenoble

    International Nuclear Information System (INIS)

    Ibel, K.

    1976-01-01

    The neutron small-angle scattering system at the high-flux reactor in Grenoble consists of three major parts: the supply of cold neutrons via bent neutron guides; the small-angle camera D11; and the data handling facilities. The camera D11 has an overall length of 80 m. The effective length of the camera is variable. The full length of the collimator before the fixed sample position can be reduced by movable neutron guides; the second flight path of 40 m full length contains detector sites in various positions. Thus a large range of momentum transfers can be used with the same relative resolution. Scattering angles between 5 x 10 -4 and 0.5 rad and neutron wavelengths from 0.2 to 2.0 nm are available. A large-area position-sensitive detector is used which allows simultaneous recording of intensities scattered at different angles; it is a multiwire proportional chamber. 3808 elements of 1 cm 2 are arranged in a two-dimensional matrix. (Auth.)

  13. Two-dimensional time-resolved X-ray diffraction study of directional solidification in steels

    International Nuclear Information System (INIS)

    Yonemura, Mitsuharu

    2009-01-01

    Full text: The high intensity heat source used for fusion welding creates steep thermal gradients of 100 degree C/s from 1800 degree Celsius. Further, the influence of a preferred orientation is serious for observation of a directional solidification that follows the dendrite growth along the direction toward the moving heat source. Therefore, we observed the rapid solidification of weld metal at a time resolution of 0.01∼0.1seconds by the Two-Dimensional Time-Resolved X-ray Diffraction (2DTRXRD) system for real welding. The diffraction ring was dynamically observed by 2DTRXRD during arc-passing over the irradiation area of X-ray with synchrotron energy of 18 KeV. The arc power output was 10 V - 150 A, and a scan speed of the arc was 1.0 mm/s. The temperature rise of instruments was suppressed by the water-cooled copper plate under the sample. Further, the temperature distribution of the weld metal was measured by the thermocouple and related to the diffraction patterns. Consequently, solidification and solid phase transformation of low carbon steels and stainless steels were observed during rapid cooling by 2DTRXRD. In the low-carbon steel, the microstructure is formed in the 2 step process; (i) formation of crystallites and (ii) increase of crystallinity. In the stainless steel, the irregular interface layer of σ/y in the quenched metal after solidification is expected that it is easy for dendrites to move at the lower temperature. In the carbide precipitation stainless steel, it is easy for NbC to grow on σ phase with a little under cooling. Further, a mist-like pattern, which differs from the halo-pattern, in the fusion zone gave some indication of the possibilities to observe the nucleation and the early solidification by 2DTRXRD. (author)

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

    Science.gov (United States)

    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.

  15. Two-dimensional imaging detectors for structural biology with X-ray lasers.

    Science.gov (United States)

    Denes, Peter

    2014-07-17

    Our ability to harness the advances in microelectronics over the past decade(s) for X-ray detection has resulted in significant improvements in the state of the art. Biology with X-ray free-electron lasers present daunting detector challenges: all of the photons arrive at the same time, and individual high peak power pulses must be read out shot-by-shot. Direct X-ray detection in silicon pixel detectors--monolithic or hybrid--are the standard for XFELs today. For structural biology, improvements are needed for today's 10-100 Hz XFELs, and further improvements are required for tomorrow's 10+ kHz XFELs. This article will discuss detector challenges, why they arise and ways to overcome them, along with the current state of the art. © 2014 The Author(s) Published by the Royal Society. All rights reserved.

  16. Two-dimensional phase separated structures of block copolymers on solids

    Science.gov (United States)

    Sen, Mani; Jiang, Naisheng; Endoh, Maya; Koga, Tadanori; Ribbe, Alexander

    The fundamental, yet unsolved question in block copolymer (BCP) thin films is the self-organization process of BCPs at the solid-polymer melt interface. We here focus on the self-organization processes of cylinder-forming polystyrene-block-poly (4-vinylpyridine) diblock copolymer and lamellar-forming poly (styrene-block-butadiene-block-styrene) triblock copolymer on Si substrates as model systems. In order to reveal the buried interfacial structures, the following experimental protocols were utilized: the BCP monolayer films were annealed under vacuum at T>Tg of the blocks (to equilibrate the melts); vitrification of the annealed BCP films via rapid quench to room temperature; subsequent intensive solvent leaching (to remove unadsorbed chains) with chloroform, a non-selective good solvent for the blocks. The strongly bound BCP layers were then characterized by using atomic force microscopy, scanning electron microscopy, grazing incidence small angle X-ray scattering, and X-ray reflectivity. The results showed that both blocks lie flat on the substrate, forming the two-dimensional, randomly phase-separated structure irrespective of their microdomain structures and interfacial energetics. Acknowledgement of financial support from NSF Grant (CMMI -1332499).

  17. Biological imaging by soft X-ray diffraction microscopy

    Science.gov (United States)

    Shapiro, David

    We have developed a microscope for soft x-ray diffraction imaging of dry or frozen hydrated biological specimens. This lensless imaging system does not suffer from the resolution or specimen thickness limitations that other short wavelength microscopes experience. The microscope, currently situated at beamline 9.0.1 of the Advanced Light Source, can collect diffraction data to 12 nm resolution with 750 eV photons and 17 nm resolution with 520 eV photons. The specimen can be rotated with a precision goniometer through an angle of 160 degrees allowing for the collection of nearly complete three-dimensional diffraction data. The microscope is fully computer controlled through a graphical user interface and a scripting language automates the collection of both two-dimensional and three-dimensional data. Diffraction data from a freeze-dried dwarf yeast cell, Saccharomyces cerevisiae carrying the CLN3-1 mutation, was collected to 12 run resolution from 8 specimen orientations spanning a total rotation of 8 degrees. The diffraction data was phased using the difference map algorithm and the reconstructions provide real space images of the cell to 30 nm resolution from each of the orientations. The agreement of the different reconstructions provides confidence in the recovered, and previously unknown, structure and indicates the three dimensionality of the cell. This work represents the first imaging of the natural complex refractive contrast from a whole unstained cell by the diffraction microscopy method and has achieved a resolution superior to lens based x-ray tomographic reconstructions of similar specimens. Studies of the effects of exposure to large radiation doses were also carried out. It was determined that the freeze-dried cell suffers from an initial collapse, which is followed by a uniform, but slow, shrinkage. This structural damage to the cell is not accompanied by a diminished ability to see small features in the specimen. Preliminary measurements on frozen

  18. Experimental coherent X-ray diffractive imaging: capabilities and limitations of the technique

    International Nuclear Information System (INIS)

    Schropp, Andreas

    2008-08-01

    The investigations pursued during this work were focused on the testing of the applicability of the coherent X-ray diffractive imaging(CXDI)-method in the hard X-ray regime and different measurements were carried out at photon energies between 7 keV and 10 keV. The samples investigated were lithographically prepared two-dimensional gold structures with a size ranging from 3 μm to 10 μm as well as a cluster of gold spheres with a lateral extension of about 3.5 μm. Continuous diffraction patterns were recorded in small angle scattering geometry. In some of the measurements a scattering signal up to the edge of the detector could be measured which corresponds to a lateral resolution of about 30 nm. For certain samples it was possible to reconstruct the object from the measured diffraction data. Since the scattered intensity of non-periodic objects is weak at large scattering angles, the available photon flux is finally the main limitation of the method with regard to the achievable resolution. The experimental data were used to get an estimate of photon flux required for sub-nanometer resolution. The ptychographic iterative phase retrieval algorithm proposed by J. M. Rodenburg et al. (2004) was implemented and tested on simulated diffraction data. Additionally, a genetic algorithm has been developed and implemented for phase retrieval. This algorithm is very different from state-of-the-art algorithms and allows to introduce further experimentally important parameters such as a certain illumination function and partial coherence of the X-ray light. (orig.)

  19. X-Pinch And Its Applications In X-ray Radiograph

    International Nuclear Information System (INIS)

    Zou Xiaobing; Wang Xinxin; Liu Rui; Zhao Tong; Zeng Naigong; Zhao Yongchao; Du Yanqiang

    2009-01-01

    An X-pinch device and the related diagnostics of x-ray emission from X-pinch were briefly described. The time-resolved x-ray measurements with photoconducting diodes show that the x-ray pulse usually consists of two subnanosecond peaks with a time interval of about 0.5 ns. Being consistent with these two peaks of the x-ray pulse, two point x-ray sources of size ranging from 100 μm to 5 μm and depending on cut-off x-ray photon energy were usually observed on the pinhole pictures. The x-pinch was used as x-ray source for backlighting of the electrical explosion of single wire and the evolution of X-pinch, and for phase-contrast imaging of soft biological objects such as a small shrimp and a mosquito.

  20. Pulmonary emphysema diagnosis using a preclinical small-animal X-ray dark-field scanner

    Energy Technology Data Exchange (ETDEWEB)

    Yaroshenko, Andre; Bech, Martin; Tapfer, Arne; Velroyen, Astrid; Pfeiffer, Franz [Department of Physics, Technische Universitaet Muenchen (Germany); Meinel, Felix; Nikolaou, Konstantin; Reiser, Maximilian [Institute of Clinical Radiology, Ludwig-Maximilians-University Hospital Munich, Muenchen (Germany); Bohla, Alexander; Yildirim, Ali Oender; Eickelberg, Oliver [Institute of Lung Biology and Disease, Helmholtz Zentrum Muenchen (Germany)

    2013-07-01

    Pulmonary emphysema is one of the leading causes of morbidity and mortality worldwide that is difficult to detect using conventional x-ray radiographic methods. For emphysematous lungs with enlarged distal airspaces, x-ray scattering decreases and transmission increases, as has been demonstrated by the proof-of-principle experiments with brilliant x-rays from a synchrotron source. Therefore, combination of the transmission and dark-field signals leads to a novel diagnostic approach for pulmonary emphysema. In this study, images of excised murine lungs with pulmonary emphysema and control lungs were acquired using a compact phase- and dark-field scanner with a polychromatic source and a cone-beam geometry. The data analysis revealed a clear distinction between the two groups in the per-pixel scatter plot. The main difference was observed in the angle of the distribution to the vertical. The presented study reveals the high potential of the approach for the pulmonary emphysema diagnosis.

  1. Tuning the Two-Dimensional Electron Gas at Oxide Interfaces with Ti-O Configurations: Evidence from X-ray Photoelectron Spectroscopy

    DEFF Research Database (Denmark)

    Zhang, Yu; Gan, Yulin; Niu, Wei

    2018-01-01

    Chemical redox reaction can lead to a two-dimensional electron gas (2DEG) at the interface between a TiO2-terminated SrTiO3 (STO) substrate and an amorphous LaAlO3 (a-LAO) capping layer. When replacing the STO substrate with rutile and anatase TiO2 substrates, considerable differences...... in interfacial conduction are observed. Based on X-ray photoelectron spectroscopy (XPS) and transport measurements, we conclude that the interfacial conduction comes from redox reactions, and that the differences among the materials systems result mainly from variations in the activation energies...

  2. X-ray imaging system

    International Nuclear Information System (INIS)

    Houston, J.M.

    1980-01-01

    A novel, high-speed apparatus for use in X-ray computerised tomography is described in detail. It consists of a semi-circular array of X-ray sources, collimators and an ion chamber array for detection of the X-rays. The X-ray sources may be pulsed in salvos such that the corresponding detectors in the array are only illuminated by one source. The use of computer controlled salvos speeds up the image processing by at least a factor of two. The ion chamber array is designed to have a constant detection efficiency for varying angles of X-ray incidence. A detailed description of the detector construction and suggested gaseous fillings are given. It is claimed that the present tomographic system allows fast and accurate imaging of internal body organs and is insensitive to the blurring effects which motion of these organs tends to produce. (UK)

  3. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... is repeated. Two or three images (from different angles) will typically be taken. An x-ray may ... RadiologyInfo.org is not a medical facility. Please contact your physician with specific medical questions or for ...

  4. Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders

    Directory of Open Access Journals (Sweden)

    Yifeng Yun

    2015-03-01

    Full Text Available Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED data collection, namely automated diffraction tomography (ADT and rotation electron diffraction (RED, have been developed. Compared with X-ray diffraction (XRD and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni–Se–O–Cl crystals, zeolites, germanates, metal–organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional

  5. Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders.

    Science.gov (United States)

    Yun, Yifeng; Zou, Xiaodong; Hovmöller, Sven; Wan, Wei

    2015-03-01

    Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED) data collection, namely automated diffraction tomography (ADT) and rotation electron diffraction (RED), have been developed. Compared with X-ray diffraction (XRD) and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD) provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni-Se-O-Cl crystals, zeolites, germanates, metal-organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional ED methods

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

    Energy Technology Data Exchange (ETDEWEB)

    Wells, Hannah C.; Sizeland, Katie H.; Kayed, Hanan R.; Haverkamp, Richard G., E-mail: r.haverkamp@massey.ac.nz [School of Engineering and Advanced Technology, Massey University, Private Bag 11222, Palmerston North 4442 (New Zealand); Kirby, Nigel; Hawley, Adrian; Mudie, Stephen T. [Australian Synchrotron, 800 Blackburn Road, Clayton, Victoria 3168 (Australia)

    2015-01-28

    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 from 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.

  7. X-ray Talbot interferometry with capillary plates

    International Nuclear Information System (INIS)

    Momose, Atsushi; Kawamoto, Shinya

    2006-01-01

    An X-ray Talbot interferometer consisting of two capillary plates, which were used as X-ray amplitude gratings, was evaluated for X-ray phase imaging. A theoretical aspect of capillary X-ray Talbot interferometry is presented with a preliminary operation result using synchrotron radiation. A two-dimensional X-ray Talbot effect, or self-imaging effect, which was the basis of Talbot interferometry, was observed with the capillary plate, and moire images formed by the X-ray Talbot interferometer exhibited contrasts corresponding to the differential phase shift caused by phase objects placed in front of the interferometer. Finally, the possibility of quantitative phase measurement with a fringe scanning technique is discussed. (author)

  8. High resolution x-ray stereomicroscopy: True three-dimensional imaging of biological samples

    International Nuclear Information System (INIS)

    Loo, B.W.Jr.; Williams, S.; Meizel, S.; Rothman, S.S.; Univ. of California, Berkeley/San Francisco, CA; Univ. of California, San Francisco, CA

    1993-01-01

    X-ray microscopy has the potential to become a powerful tool for the study of biological samples, allowing the imaging of intact cells and subcellular organelles in an aqueous environment at resolutions previously achievable only by electron microscopy. The ability to examine a relatively thick sample raises the issue of superposition of objects from multiple planes within the sample, making difficult the interpretation of conventional, orthogonally projected images. This paper describes early attempts at developing three-dimensional methods for x-ray microimaging: the first to use x-ray optics, and to the authors' knowledge, the first demonstrating sub-visible resolutions and natural contrast. These studies were performed using the scanning transmission x-ray microscope (STXM) at the National Synchrotron Light Source, Brookhaven National Laboratory

  9. A filter based analyzer for studies of X-ray Raman scattering

    CERN Document Server

    Seidler, G T

    2001-01-01

    Non-resonant X-ray Raman scattering (XRS) with hard X-rays holds the potential for measuring local structure and local electronic properties around low-Z atoms in environments where traditional soft X-ray techniques are inapplicable. However, the small cross-section for XRS requires that experiments must simultaneously achieve high detection efficiency, large collection solid angles, and good energy resolution. We report here that a simple X-ray analyzer consisting of an absorber and a point-focusing spatial filter can be used to study some X-ray Raman near-edge features. This apparatus has greater than 10% detection efficiency, has an energy resolution of 8 eV, and can be readily extended to collection angles of more than 1 sr. We present preliminary measurements of the XRS from the nitrogen 1 s shell in pyrolitic boron nitride.

  10. Fracture mechanics by three-dimensional crack-tip synchrotron X-ray microscopy.

    Science.gov (United States)

    Withers, P J

    2015-03-06

    To better understand the relationship between the nucleation and growth of defects and the local stresses and phase changes that cause them, we need both imaging and stress mapping. Here, we explore how this can be achieved by bringing together synchrotron X-ray diffraction and tomographic imaging. Conventionally, these are undertaken on separate synchrotron beamlines; however, instruments capable of both imaging and diffraction are beginning to emerge, such as ID15 at the European Synchrotron Radiation Facility and JEEP at the Diamond Light Source. This review explores the concept of three-dimensional crack-tip X-ray microscopy, bringing them together to probe the crack-tip behaviour under realistic environmental and loading conditions and to extract quantitative fracture mechanics information about the local crack-tip environment. X-ray diffraction provides information about the crack-tip stress field, phase transformations, plastic zone and crack-face tractions and forces. Time-lapse CT, besides providing information about the three-dimensional nature of the crack and its local growth rate, can also provide information as to the activation of extrinsic toughening mechanisms such as crack deflection, crack-tip zone shielding, crack bridging and crack closure. It is shown how crack-tip microscopy allows a quantitative measure of the crack-tip driving force via the stress intensity factor or the crack-tip opening displacement. Finally, further opportunities for synchrotron X-ray microscopy are explored.

  11. Soft x-ray scanning microtomography with submicron resolution

    International Nuclear Information System (INIS)

    McNulty, I.; Haddad, W.S.; Trebes, J.E.; Anderson, E.H.

    1994-01-01

    Scanning soft x-ray microtomography was used to obtain high-resolution three-dimensional images of a microfabricated test object. Using a special rotation stage mounted on the scanning transmission x-ray microscope at the XIA Beamline at the National Synchrotron Light Source, we recorded nine two-dimensional projections of the 3D test object over an angular range of -50 degrees to +55 degrees. The x-ray wavelength was 3.6 nm and the radiation dose to the object per projection was approximately 2 x 10 6 Gy. The object consisted of two gold patterns supported on transparent silicon nitride membranes, separated by 4.75 Jim, with 100 to 300-nm wide and 65-nm thick features. We reconstructed a volumetric data set of the test object from the two-dimensional projections using an algebraic reconstruction technique algorithm. Features of the test object were resolved to ∼100 nm in transverse and longitudinal extent in three-dimensional images rendered from the volumetric set

  12. Three-dimensional orientation and location-dependent varying rules of radiographic angles of the acetabular cup.

    Science.gov (United States)

    Zhao, Jing-Xin; Su, Xiu-Yun; Zhao, Zhe; Xiao, Ruo-Xiu; Zhang, Li-Cheng; Tang, Pei-Fu

    2018-02-17

    The aim of this study is to demonstrate the varying rules of radiographic angles following varying three-dimensional (3D) orientations and locations of cup using an accurate mathematical model. A cone model is established to address the quantitative relationship between the opening circle of cup and its ellipse projection on radiograph. The varying rules of two-dimensional (2D) radiographic anteversion (RA) and inclination (RI) angles can be analyzed. When the centre of cup is located above X-ray source, with proper 3D RI/RA angles, 2D RA angle can be equal to its 3D counterpart, and 2D RI angle is usually greater than its 3D counterpart. Except for the original point on hip-centered anterior-posterior radiograph, there is no area on radiograph where both 2D RA and RI angles are equal to their 3D counterparts simultaneously. This study proposes an innovative model for accurately explaining how 2D RA/RI angles of cup are varying following different 3D RA/RI angles and location of cup. The analysis results provide clinicians an intuitive grasp of knowledge about 2D RA/RI angles greater or smaller than their 3D counterparts post-operatively. The established model may allow determining the effects of pelvic rotations on 2D radiographic angles of cup.

  13. Healing X-ray scattering images

    Directory of Open Access Journals (Sweden)

    Jiliang Liu

    2017-07-01

    Full Text Available X-ray scattering images contain numerous gaps and defects arising from detector limitations and experimental configuration. 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 structures present in the image, including the identification of diffuse versus sharp 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.

  14. 3D X-Ray Luggage-Screening System

    Science.gov (United States)

    Fernandez, Kenneth

    2006-01-01

    A three-dimensional (3D) x-ray luggage- screening system has been proposed to reduce the fatigue experienced by human inspectors and increase their ability to detect weapons and other contraband. The system and variants thereof could supplant thousands of xray scanners now in use at hundreds of airports in the United States and other countries. The device would be applicable to any security checkpoint application where current two-dimensional scanners are in use. A conventional x-ray luggage scanner generates a single two-dimensional (2D) image that conveys no depth information. Therefore, a human inspector must scrutinize the image in an effort to understand ambiguous-appearing objects as they pass by at high speed on a conveyor belt. Such a high level of concentration can induce fatigue, causing the inspector to reduce concentration and vigilance. In addition, because of the lack of depth information, contraband objects could be made more difficult to detect by positioning them near other objects so as to create x-ray images that confuse inspectors. The proposed system would make it unnecessary for a human inspector to interpret 2D images, which show objects at different depths as superimposed. Instead, the system would take advantage of the natural human ability to infer 3D information from stereographic or stereoscopic images. The inspector would be able to perceive two objects at different depths, in a more nearly natural manner, as distinct 3D objects lying at different depths. Hence, the inspector could recognize objects with greater accuracy and less effort. The major components of the proposed system would be similar to those of x-ray luggage scanners now in use. As in a conventional x-ray scanner, there would be an x-ray source. Unlike in a conventional scanner, there would be two x-ray image sensors, denoted the left and right sensors, located at positions along the conveyor that are upstream and downstream, respectively (see figure). X-ray illumination

  15. Soft x-ray scanning microtomography with submicrometer resolution

    International Nuclear Information System (INIS)

    McNulty, I.; Haddad, W.S.; Trebes, J.E.; Anderson, E.H.

    1995-01-01

    Scanning soft x-ray microtomography was used to obtain high-resolution three-dimensional images of a microfabricated test object. Using a special rotation stage mounted on the scanning transmission x-ray microscope at the X1A beamline at the National Synchrotron Light Source, we recorded nine two-dimensional projections of the 3D test object over an angular range of -50 degree to +55 degree. The x-ray wavelength was 3.6 nm and the radiation dose to the object per projection was approximately 2x10 6 Gy. The object consisted of two gold patterns supported on transparent silicon nitride membranes, separated by 4.75 μm, with 100- to 300-nm-wide and 65-nm-thick features. We reconstructed a volumetric data set of the test object from the two-dimensional projections using an algebraic reconstruction technique algorithm. Features of the test object were resolved to ∼100 nm in transverse and longitudinal extent with low artifact in three-dimensional images rendered from the volumetric set

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

    Energy Technology Data Exchange (ETDEWEB)

    Peyronel, Fernanda; Marangoni, Alejandro G. [Food Science Department, University of Guelph, Guelph, Ontario N1G 2W1 (Canada); Ilavsky, Jan [Advanced Photon Source, Argonne National Laboratory, 9700S Cass Ave., Bldg. 434D, Argonne, Illinois 60439 (United States); Mazzanti, Gianfranco [Department of Process Engineering and Applied Science, Dalhousie University, Halifax, Nova Scotia B3H 4R2 (Canada); Pink, David A. [Food Science Department, University of Guelph, Guelph, Ontario N1G 2W1 (Canada); Physics Department, St. Francis Xavier University, Antigonish, Nova Scotia B2G 2W5 (Canada)

    2013-12-21

    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, R{sub g2} between 1800 Å and 12000 Å and fractal dimensions of either D{sub 2}=1 for case 3 or 1.8≤D{sub 2}≤2.1 for case 1 and case 2. D{sub 2} = 1 is consistent with unaggregated 1-dimensional objects. 1.8 ≤ D{sub 2} ≤ 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 D{sub 3}≈3 while for case 2 and case 3 the fractal dimension was D{sub 3}≈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

  17. Exploring structural variability in X-ray crystallographic models using protein local optimization by torsion-angle sampling

    International Nuclear Information System (INIS)

    Knight, Jennifer L.; Zhou, Zhiyong; Gallicchio, Emilio; Himmel, Daniel M.; Friesner, Richard A.; Arnold, Eddy; Levy, Ronald M.

    2008-01-01

    Torsion-angle sampling, as implemented in the Protein Local Optimization Program (PLOP), is used to generate multiple structurally variable single-conformer models which are in good agreement with X-ray data. An ensemble-refinement approach to differentiate between positional uncertainty and conformational heterogeneity is proposed. Modeling structural variability is critical for understanding protein function and for modeling reliable targets for in silico docking experiments. Because of the time-intensive nature of manual X-ray crystallographic refinement, automated refinement methods that thoroughly explore conformational space are essential for the systematic construction of structurally variable models. Using five proteins spanning resolutions of 1.0–2.8 Å, it is demonstrated how torsion-angle sampling of backbone and side-chain libraries with filtering against both the chemical energy, using a modern effective potential, and the electron density, coupled with minimization of a reciprocal-space X-ray target function, can generate multiple structurally variable models which fit the X-ray data well. Torsion-angle sampling as implemented in the Protein Local Optimization Program (PLOP) has been used in this work. Models with the lowest R free values are obtained when electrostatic and implicit solvation terms are included in the effective potential. HIV-1 protease, calmodulin and SUMO-conjugating enzyme illustrate how variability in the ensemble of structures captures structural variability that is observed across multiple crystal structures and is linked to functional flexibility at hinge regions and binding interfaces. An ensemble-refinement procedure is proposed to differentiate between variability that is a consequence of physical conformational heterogeneity and that which reflects uncertainty in the atomic coordinates

  18. Automatic method for estimation of in situ effective contact angle from X-ray micro tomography images of two-phase flow in porous media.

    Science.gov (United States)

    Scanziani, Alessio; Singh, Kamaljit; Blunt, Martin J; Guadagnini, Alberto

    2017-06-15

    Multiphase flow in porous media is strongly influenced by the wettability of the system, which affects the arrangement of the interfaces of different phases residing in the pores. We present a method for estimating the effective contact angle, which quantifies the wettability and controls the local capillary pressure within the complex pore space of natural rock samples, based on the physical constraint of constant curvature of the interface between two fluids. This algorithm is able to extract a large number of measurements from a single rock core, resulting in a characteristic distribution of effective in situ contact angle for the system, that is modelled as a truncated Gaussian probability density distribution. The method is first validated on synthetic images, where the exact angle is known analytically; then the results obtained from measurements within the pore space of rock samples imaged at a resolution of a few microns are compared to direct manual assessment. Finally the method is applied to X-ray micro computed tomography (micro-CT) scans of two Ketton cores after waterflooding, that display water-wet and mixed-wet behaviour. The resulting distribution of in situ contact angles is characterized in terms of a mixture of truncated Gaussian densities. Crown Copyright © 2017. Published by Elsevier Inc. All rights reserved.

  19. Human thyroid specimen imaging by fluorescent x-ray computed tomography with synchrotron radiation

    Science.gov (United States)

    Takeda, Tohoru; Yu, Quanwen; Yashiro, Toru; Yuasa, Tetsuya; Hasegawa, Yasuo; Itai, Yuji; Akatsuka, Takao

    1999-09-01

    Fluorescent x-ray computed tomography (FXCT) is being developed to detect non-radioactive contrast materials in living specimens. The FXCT system consists of a silicon (111) channel cut monochromator, an x-ray slit and a collimator for fluorescent x ray detection, a scanning table for the target organ and an x-ray detector for fluorescent x-ray and transmission x-ray. To reduce Compton scattering overlapped on the fluorescent K(alpha) line, incident monochromatic x-ray was set at 37 keV. The FXCT clearly imaged a human thyroid gland and iodine content was estimated quantitatively. In a case of hyperthyroidism, the two-dimensional distribution of iodine content was not uniform, and thyroid cancer had a small amount of iodine. FXCT can be used to detect iodine within thyroid gland quantitatively and to delineate its distribution.

  20. The BESSY X-ray microfocus beamline project

    International Nuclear Information System (INIS)

    Erko, A.; Schaefers, F.; Firsov, A.; Peatman, W.B.; Eberhardt, W.; Signorato, R.

    2004-01-01

    The design and construction of a beamline dedicated to X-ray absorption spectroscopy, X-ray fluorescence analysis, X-ray diffraction and X-ray small-angle scattering measurements with micron and submicron spatial resolution in the photon energy range of 1.9-30 keV are reported here. The main feature of the beamline is a combination of all these methods in one experimental station. The source will be a BESSY 7-T wavelength shifter, which is already in operation. Such a wavelength shifter with its continuous spectrum is an optimum source for these experiments. Glass capillaries and the combination of a linear Bragg-Fresnel lens and bimorph mirror were chosen as the special optical components in the beamline. This beamline will open for BESSY users the possibility to perform experiments on the same sample applying a microfocused X-ray beam in combination with advanced experimental methods

  1. Large angle and high linearity two-dimensional laser scanner based on voice coil actuators

    Science.gov (United States)

    Wu, Xin; Chen, Sihai; Chen, Wei; Yang, Minghui; Fu, Wen

    2011-10-01

    A large angle and high linearity two-dimensional laser scanner with an in-house ingenious deflection angle detecting system is developed based on voice coil actuators direct driving mechanism. The specially designed voice coil actuators make the steering mirror moving at a sufficiently large angle. Frequency sweep method based on virtual instruments is employed to achieve the natural frequency of the laser scanner. The response shows that the performance of the laser scanner is limited by the mechanical resonances. The closed-loop controller based on mathematical model is used to reduce the oscillation of the laser scanner at resonance frequency. To design a qualified controller, the model of the laser scanner is set up. The transfer function of the model is identified with MATLAB according to the tested data. After introducing of the controller, the nonlinearity decreases from 13.75% to 2.67% at 50 Hz. The laser scanner also has other advantages such as large deflection mirror, small mechanical structure, and high scanning speed.

  2. Three dimensional characterization of laser ablation craters using high resolution X-ray computed tomography

    Science.gov (United States)

    Galmed, A. H.; du Plessis, A.; le Roux, S. G.; Hartnick, E.; Von Bergmann, H.; Maaza, M.

    2018-01-01

    Laboratory X-ray computed tomography is an emerging technology for the 3D characterization and dimensional analysis of many types of materials. In this work we demonstrate the usefulness of this characterization method for the full three dimensional analysis of laser ablation craters, in the context of a laser induced breakdown spectroscopy setup. Laser induced breakdown spectroscopy relies on laser ablation for sampling the material of interest. We demonstrate here qualitatively (in images) and quantitatively (in terms of crater cone angles, depths, diameters and volume) laser ablation crater analysis in 3D for metal (aluminum) and rock (false gold ore). We show the effect of a Gaussian beam profile on the resulting crater geometry, as well as the first visual evidence of undercutting in the rock sample, most likely due to ejection of relatively large grains. The method holds promise for optimization of laser ablation setups especially for laser induced breakdown spectroscopy.

  3. Multislice imaging of integrated circuits by precession X-ray ptychography.

    Science.gov (United States)

    Shimomura, Kei; Hirose, Makoto; Takahashi, Yukio

    2018-01-01

    A method for nondestructively visualizing multisection nanostructures of integrated circuits by X-ray ptychography with a multislice approach is proposed. In this study, tilt-series ptychographic diffraction data sets of a two-layered circuit with a ∼1.4 µm gap at nine incident angles are collected in a wide Q range and then artifact-reduced phase images of each layer are successfully reconstructed at ∼10 nm resolution. The present method has great potential for the three-dimensional observation of flat specimens with thickness on the order of 100 µm, such as three-dimensional stacked integrated circuits based on through-silicon vias, without laborious sample preparation.

  4. X-ray interferometers

    International Nuclear Information System (INIS)

    Franks, A.

    1980-01-01

    An improved type of amplitude-division x-ray interferometer is described. The wavelength at which the interferometer can operate is variable, allowing the instrument to be used to measure x-ray wavelength, and the angle of inclination is variable for sample investigation. (U.K.)

  5. Photoelectron diffraction from single oriented molecules: Towards ultrafast structure determination of molecules using x-ray free-electron lasers

    Science.gov (United States)

    Kazama, Misato; Fujikawa, Takashi; Kishimoto, Naoki; Mizuno, Tomoya; Adachi, Jun-ichi; Yagishita, Akira

    2013-06-01

    We provide a molecular structure determination method, based on multiple-scattering x-ray photoelectron diffraction (XPD) calculations. This method is applied to our XPD data on several molecules having different equilibrium geometries. Then it is confirmed that, by our method, bond lengths and bond angles can be determined with a resolution of less than 0.1 Å and 10∘, respectively. Differently from any other scenario of ultrafast structure determination, we measure the two- or three-dimensional XPD of aligned or oriented molecules in the energy range from 100 to 200 eV with a 4π detection velocity map imaging spectrometer. Thanks to the intense and ultrashort pulse properties of x-ray free-electron lasers, our approach exhibits the most probable method for obtaining ultrafast real-time structural information on small to medium-sized molecules consisting of light elements, i.e., a “molecular movie.”

  6. Wolter x-ray microscope calibration

    International Nuclear Information System (INIS)

    Gerassimenko, M.

    1986-06-01

    A 22 x Wolter microscope was calibrated after several months of operation in the Lawrence Livermore National laboratory (LLNL) Inertial Confinement Fusion program. Placing a point x-ray source at the microscope focus, I recorded the image plane spectrum, as well as the direct spectrum, and from the ratio of these two spectra derived an accurate estimate of the microscope solid angle in the 1 to 4 keV range. The solid angle was also calculated using the microscope geometry and composition. Comparison of this calculated value with the solid angle that was actually measured suggests contamination of the microscope surface

  7. Wolter x-ray microscope calibration

    International Nuclear Information System (INIS)

    Gerassimenko, M.

    1986-01-01

    A 22 x Wolter microscope was calibrated after several months of operation in the Lawrence Livermore National Laboratory (LLNL) Inertial Confinement Fusion program. Placing a point x-ray source at the microscope focus, I recorded the image plane spectrum, as well as the direct spectrum, and from the ratio of these two spectra derived an accurate estimate of the microscope solid angle in the 1-4 keV range. The solid angle was also calculated using the microscope geometry and composition. Comparison of this calculated value with the solid angle that was actually measured suggests contamination of the microscope surface

  8. Two-dimensional time-resolved x-ray diffraction study of dual phase rapid solidification in steels

    Science.gov (United States)

    Yonemura, Mitsuharu; Osuki, Takahiro; Terasaki, Hidenori; Komizo, Yuichi; Sato, Masugu; Toyokawa, Hidenori; Nozaki, Akiko

    2010-01-01

    The high intensity heat source used for fusion welding creates steep thermal gradients of 100 °C/s from 1800 °C. Further, the influence of preferred orientation is important for the observation of a directional solidification that follows the dendrite growth along the ⟨100⟩ direction toward the moving heat source. In the present study, we observed the rapid solidification of weld metal at a time resolution of 0.01-0.1 s by a two-dimensional time-resolved x-ray diffraction (2DTRXRD) system for real welding. The diffraction rings were dynamically observed by 2DTRXRD with synchrotron energy of 18 keV while the arc passes over the irradiation area of the x-rays. The arc power output was 10 V-150 A, and the scan speed of the arc was 1.0 mm/s. The temperature rise in instruments was suppressed by a water-cooled copper plate under the specimen. Further, the temperature distribution of the weld metal was measured by a thermocouple and correlated with the diffraction patterns. Consequently, solidification and solid phase transformation of low carbon steels and stainless steels were observed during rapid cooling by 2DTRXRD. In the low carbon steel, the microstructure is formed in a two step process, (i) formation of crystallites and (ii) increase of crystallinity. In stainless steel, the irregular interface layer of δ/γ in the quenched metal after solidification is expected to show the easy movement of dendrites at a lower temperature. In carbide precipitation stainless steel, it is easy for NbC to grow on δ phase with a little undercooling. Further, a mistlike pattern, which differs from the halo pattern, in the fusion zone gave some indication of the possibilities to observe the nucleation and the early solidification by 2DTRXRD.

  9. Bacteriophage T7 structure according to the data of small-angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Rol' bin, Yu A; Svergun, D I; Feigin, L A; Gashpar, Sh; Ronto, D [AN SSSR, Moscow. Inst. Kristallografii

    1980-01-01

    An attempt is made to obtain complete data on the form, sizes, weight and hydration of the T7 bacteriophage cultivated on E.coli cells and the peculiarities of phage DNA structure using the method of small-angle scattering.

  10. EFFECTS OF X-RAY BEAM ANGLE AND GEOMETRIC DISTORTION ON WIDTH OF EQUINE THORACOLUMBAR INTERSPINOUS SPACES USING RADIOGRAPHY AND COMPUTED TOMOGRAPHY

    DEFF Research Database (Denmark)

    Djernaes, Julie D.; Nielsen, Jon V.; Berg, Lise C.

    2017-01-01

    The widths of spaces between the thoracolumbar processi spinosi (interspinous spaces) are frequently assessed using radiography in sports horses; however effects of varying X-ray beam angles and geometric distortion have not been previously described. The aim of this prospective, observational...... study was to determine whether X-ray beam angle has an effect on apparent widths of interspinous spaces. Thoracolumbar spine specimens were collected from six equine cadavers and left-right lateral radiographs and sagittal and dorsal reconstructed computed tomographic (CT) images were acquired...... measurements. Effect of geometric distortion was evaluated by comparing the interspinous space in radiographs with sagittal and dorsal reconstructed CT images. A total of 49 interspinous spaces were sampled, yielding 274 measurements. X-ray beam angle significantly affected measured width of interspinous...

  11. Characteristics of angular cross correlations studied by light scattering from two-dimensional microsphere films

    Science.gov (United States)

    Schroer, M. A.; Gutt, C.; Grübel, G.

    2014-07-01

    Recently the analysis of scattering patterns by angular cross-correlation analysis (CCA) was introduced to reveal the orientational order in disordered samples with special focus to future applications on x-ray free-electron laser facilities. We apply this CCA approach to ultra-small-angle light-scattering data obtained from two-dimensional monolayers of microspheres. The films were studied in addition by optical microscopy. This combined approach allows to calculate the cross-correlations of the scattering patterns, characterized by the orientational correlation function Ψl(q), as well as to obtain the real-space structure of the monolayers. We show that CCA is sensitive to the orientational order of monolayers formed by the microspheres which are not directly visible from the scattering patterns. By mixing microspheres of different radii the sizes of ordered monolayer domains is reduced. For these samples it is shown that Ψl(q) quantitatively describes the degree of hexagonal order of the two-dimensional films. The experimental CCA results are compared with calculations based on the microscopy images. Both techniques show qualitatively similar features. Differences can be attributed to the wave-front distortion of the laser beam in the experiment. This effect is discussed by investigating the effect of different wave fronts on the cross-correlation analysis results. The so-determined characteristics of the cross-correlation analysis will be also relevant for future x-ray-based studies.

  12. Determination of the quaternary structural states of bovine casein by small-angle X-ray scattering: submicellar and micellar forms

    International Nuclear Information System (INIS)

    Kumosinski, T.F.; Pessen, H.; Farrell, H.M. Jr.; Brumberger, H.

    1988-01-01

    Whole casein occurs in milk as a spherical colloidal complex of protein and salts called the casein micelle, with approximate average radii of 650 A as determined by electron microscopy. Removal of Ca2+ is thought to result in dissociation into smaller noncolloidal protein complexes called submicelles. Hydrodynamic and light scattering studies on whole casein submicelles suggest that they are predominantly spherical particles with a hydrophobic core. To investigate whether the integrity of a hydrophobically stabilized submicellar structure is preserved in the electrostatically stabilized colloidal micellar structure, small-angle X-ray scattering (SAXS) experiments were undertaken on whole casein from bovine milk under submicellar and micellar conditions. All SAXS results showed multiple Gaussian character and could be analyzed best by nonlinear regression in place of the customary Guinier plot. Analysis of the SAXS data for submicellar casein showed two Gaussian components which could be interpreted in terms of a particle with two concentric regions of different electron density, designated as a compact core and a loose shell, respectively. The submicelle was found to have an average molecular weight of 285,000 +/- 14,600 and a mass fraction of higher electron density core, k, of 0.212 +/- 0.028. The radius of gyration of the core, RC, was 37.98 +/- 0.01 A with an electron density difference, delta rho C, of 0.0148 +/- 0.0014 e-/A3, while the loose region had values of RL = 88.2 +/- 0.8 A with delta rho L = 0.0091 +/- 0.0003 e-/A3. Calculated distance distribution functions and normalized scattering curves also were consistent with an overall spherical particle with a concentric spherical inner core of higher electron density. (Abstract Truncated)

  13. Computed tomographic images using tube source of x rays: interior properties of the material

    Science.gov (United States)

    Rao, Donepudi V.; Takeda, Tohoru; Itai, Yuji; Seltzer, S. M.; Hubbell, John H.; Zeniya, Tsutomu; Akatsuka, Takao; Cesareo, Roberto; Brunetti, Antonio; Gigante, Giovanni E.

    2002-01-01

    An image intensifier based computed tomography scanner and a tube source of x-rays are used to obtain the images of small objects, plastics, wood and soft materials in order to know the interior properties of the material. A new method is developed to estimate the degree of monochromacy, total solid angle, efficiency and geometrical effects of the measuring system and the way to produce monoenergetic radiation. The flux emitted by the x-ray tube is filtered using the appropriate filters at the chosen optimum energy and reasonable monochromacy is achieved and the images are acceptably distinct. Much attention has been focused on the imaging of small objects of weakly attenuating materials at optimum value. At optimum value it is possible to calculate the three-dimensional representation of inner and outer surfaces of the object. The image contrast between soft materials could be significantly enhanced by optimal selection of the energy of the x-rays by Monte Carlo methods. The imaging system is compact, reasonably economic, has a good contrast resolution, simple operation and routine availability and explores the use of optimizing tomography for various applications.

  14. Colliding Stellar Winds Structure and X-ray Emission

    Science.gov (United States)

    Pittard, J. M.; Dawson, B.

    2018-04-01

    We investigate the structure and X-ray emission from the colliding stellar winds in massive star binaries. We find that the opening angle of the contact discontinuity (CD) is overestimated by several formulae in the literature at very small values of the wind momentum ratio, η. We find also that the shocks in the primary (dominant) and secondary winds flare by ≈20° compared to the CD, and that the entire secondary wind is shocked when η ≲ 0.02. Analytical expressions for the opening angles of the shocks, and the fraction of each wind that is shocked, are provided. We find that the X-ray luminosity Lx∝η, and that the spectrum softens slightly as η decreases.

  15. Precise small-angle X-ray scattering evaluation of the pore structures in track-etched membranes: Comparison with other convenient evaluation methods

    Energy Technology Data Exchange (ETDEWEB)

    Miyazaki, Tsukasa, E-mail: t_miyazaki@cross.or.jp [Neutron Science and Technology Center, Comprehensive Research Organization for Science and Society, 162-1, Shirakata, Tokai-mura, Naka-gun, Ibaraki 319-1106 (Japan); Takenaka, Mikihito [Department of Polymer Chemistry, Gradual School of Engineering, Kyoto University, Kyotodaigaku-katsura, Kyoto 615-8510 (Japan)

    2017-03-01

    Poly(ethylene terephthalate) (PET)-based track-etched membranes (TMs) with pore sizes ranging from few nanometers to approximately 1 μm are used in various applications in the biological field, and their pore structures are determined by small-angle X-ray scattering (SAXS). These TMs with the nanometer-sized cylindrical pores aligned parallel to the film thickness direction are produced by chemical etching of the track in the PET films irradiated by heavy ions with the sodium hydroxide aqueous solution. It is well known that SAXS allows us to precisely and statistically estimate the pore size and the pore size distribution in the TMs by using the form factor of a cylinder with the extremely long pore length relative to the pore diameter. The results obtained were compared with those estimated with scanning electron microscopy and gas permeability measurements. The result showed that the gas permeability measurement is convenient to evaluate the pore size of TMs within a wide length scale, and the SEM observation is also suited to estimate the pore size, although SEM observation is usually limited above approximately 30 nm.

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

    Energy Technology Data Exchange (ETDEWEB)

    Chaudhuri, Barnali [University at Buffalo (SUNY); Muñoz, Inés G. [Centro Nacional de Investigaciones Oncológicas Madrid, Madrid, Spain; Urban, Volker S. [ORNL; Qian, Shuo [ORNL

    2017-12-01

    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, 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 helpful for

  17. (an)isotropy of the X-ray sky

    International Nuclear Information System (INIS)

    Shafer, R.A.; Fabian, A.C.

    1983-01-01

    An assessment is made of the extent to which the study of the isotropy of the X-ray sky has contributed to the present understanding of the structure of the universe at moderate redshifts. It is, of course, the anisotropic character of the sky flux that is valuable in this context. Although it is not currently possible to undertake measurements with the precision and small solid angles that are typically achieved in the microwave range, the comparatively crude limits from the X-ray fluctuations place limits on the largest scale structure of the universe. After indicating the nature of measurements made, with the HEAO 1 A-2 experiment, of the X-ray sky and its anisotropies, it is shown how these place limits on the origin of the X-ray sky and on any large scale structure of the universe. 40 references

  18. Geometric estimation method for x-ray digital intraoral tomosynthesis

    Science.gov (United States)

    Li, Liang; Yang, Yao; Chen, Zhiqiang

    2016-06-01

    It is essential for accurate image reconstruction to obtain a set of parameters that describes the x-ray scanning geometry. A geometric estimation method is presented for x-ray digital intraoral tomosynthesis (DIT) in which the detector remains stationary while the x-ray source rotates. The main idea is to estimate the three-dimensional (3-D) coordinates of each shot position using at least two small opaque balls adhering to the detector surface as the positioning markers. From the radiographs containing these balls, the position of each x-ray focal spot can be calculated independently relative to the detector center no matter what kind of scanning trajectory is used. A 3-D phantom which roughly simulates DIT was designed to evaluate the performance of this method both quantitatively and qualitatively in the sense of mean square error and structural similarity. Results are also presented for real data acquired with a DIT experimental system. These results prove the validity of this geometric estimation method.

  19. Compound refractive lenses for novel X-ray sources

    Energy Technology Data Exchange (ETDEWEB)

    Piestrup, M.A. E-mail: melpie@adelphitech.com; Beguiristain, H.R.; Gary, C.K.; Cremer, J.T.; Pantell, R.H.; Tatchyn, R

    2001-01-01

    We have measured the intensity profile of X-rays focused by a linear array of closely spaced spherical lenses fabricated using Mylar (C{sub 5}H{sub 4}O{sub 2}). We have experimentally demonstrated that we can achieve two-dimensional focusing for photon energies between 7 and 9 keV with imaging distances of less than 1 m. For example, using 8-keV X-rays we have achieved full-width-at-half-maximum (FWHM) linewidths down to 27.5 {mu}m at a distance of only 62 cm from the lens. The effective aperture of the lens was measured to be about 390 {mu}m with 38% transmission at 9 keV. A synchrotron source having source-size dimensions of 0.44x1.7 mm{sup 2} was utilized for the experimental work. Such lenses are seen as useful for focusing and increasing the intensity of novel X-ray sources that are directional and have small source size ({sigma}<1 mm)

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

    Science.gov (United States)

    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.

  1. Structural analysis of the yeast exosome Rrp6p–Rrp47p complex by small-angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Dedic, Emil; Seweryn, Paulina; Jonstrup, Anette Thyssen; Flygaard, Rasmus Koch [Centre for mRNP Biogenesis and Metabolism, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Department of Molecular Biology and Genetics, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Fedosova, Natalya U. [Department of Biomedicine, Ole Worms Allé 6, Aarhus University, DK-8000 Aarhus C (Denmark); Hoffmann, Søren Vrønning [Institute for Storage Ring Facilities (ISA), Department of Physics and Astronomy, Ny Munkegade 120, Aarhus University, DK-8000 Aarhus C (Denmark); Boesen, Thomas [Centre for Membrane Pumps in Cells and Disease – PUMPKIN, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Department of Molecular Biology and Genetics, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Brodersen, Ditlev Egeskov, E-mail: deb@mb.au.dk [Centre for mRNP Biogenesis and Metabolism, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Department of Molecular Biology and Genetics, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark)

    2014-07-18

    Highlights: • We show that S. cerevisiae Rrp6p and Rrp47p stabilise each other in vitro. • We determine molecular envelopes of the Rrp6p–Rrp47p complex by SAXS. • Rrp47p binds at the top of the Rrp6p exonuclease domain. • Rrp47p modulates the activity of Rrp6p on a variety of RNA substrates. • Rrp47p does not affect RNA affinity by Rrp6p. - Abstract: The RNase D-type 3′–5′ exonuclease Rrp6p from Saccharomyces cerevisiae is a nuclear-specific cofactor of the RNA exosome and associates in vivo with Rrp47p (Lrp1p). Here, we show using biochemistry and small-angle X-ray scattering (SAXS) that Rrp6p and Rrp47p associate into a stable, heterodimeric complex with an elongated shape consistent with binding of Rrp47p to the nuclease domain and opposite of the HRDC domain of Rrp6p. Rrp47p reduces the exonucleolytic activity of Rrp6p on both single-stranded and structured RNA substrates without significantly altering the affinity towards RNA or the ability of Rrp6p to degrade RNA secondary structure.

  2. Structural analysis of the yeast exosome Rrp6p–Rrp47p complex by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Dedic, Emil; Seweryn, Paulina; Jonstrup, Anette Thyssen; Flygaard, Rasmus Koch; Fedosova, Natalya U.; Hoffmann, Søren Vrønning; Boesen, Thomas; Brodersen, Ditlev Egeskov

    2014-01-01

    Highlights: • We show that S. cerevisiae Rrp6p and Rrp47p stabilise each other in vitro. • We determine molecular envelopes of the Rrp6p–Rrp47p complex by SAXS. • Rrp47p binds at the top of the Rrp6p exonuclease domain. • Rrp47p modulates the activity of Rrp6p on a variety of RNA substrates. • Rrp47p does not affect RNA affinity by Rrp6p. - Abstract: The RNase D-type 3′–5′ exonuclease Rrp6p from Saccharomyces cerevisiae is a nuclear-specific cofactor of the RNA exosome and associates in vivo with Rrp47p (Lrp1p). Here, we show using biochemistry and small-angle X-ray scattering (SAXS) that Rrp6p and Rrp47p associate into a stable, heterodimeric complex with an elongated shape consistent with binding of Rrp47p to the nuclease domain and opposite of the HRDC domain of Rrp6p. Rrp47p reduces the exonucleolytic activity of Rrp6p on both single-stranded and structured RNA substrates without significantly altering the affinity towards RNA or the ability of Rrp6p to degrade RNA secondary structure

  3. X-ray micro-tomography system for small-animal imaging with zoom-in imaging capability

    International Nuclear Information System (INIS)

    Chun, In Kon; Cho, Myung Hye; Lee, Sang Chul; Cho, Min Hyoung; Lee, Soo Yeol

    2004-01-01

    Since a micro-tomography system capable of μm-resolution imaging cannot be used for whole-body imaging of a small laboratory animal without sacrificing its spatial resolution, it is desirable for a micro-tomography system to have local imaging capability. In this paper, we introduce an x-ray micro-tomography system capable of high-resolution imaging of a local region inside a small animal. By combining two kinds of projection data, one from a full field-of-view (FOV) scan of the whole body and the other from a limited FOV scan of the region of interest (ROI), we have obtained zoomed-in images of the ROI without any contrast anomalies commonly appearing in conventional local tomography. For experimental verification of the zoom-in imaging capability, we have integrated a micro-tomography system using a micro-focus x-ray source, a 1248 x 1248 flat-panel x-ray detector, and a precision scan mechanism. The mismatches between the two projection data caused by misalignments of the scan mechanism have been estimated with a calibration phantom, and the mismatch effects have been compensated in the image reconstruction procedure. Zoom-in imaging results of bony tissues with a spatial resolution of 10 lp mm -1 suggest that zoom-in micro-tomography can be greatly used for high-resolution imaging of a local region in small-animal studies

  4. Development of small scale soft x-ray lasers: Aspects of data interpretation

    International Nuclear Information System (INIS)

    Skinner, C.H.; Kim, D.; Voorhees, D.; Suckewer, S.

    1990-02-01

    The widespread application of soft x-ray laser technology is contingent on the development of small scale soft x-ray lasers that do not require large laser facilities. Progress in the development of soft x-ray lasers pumped by a Nd laser of energy 6-12J is reported below. Some aspects of data interpretation and gain measurements in such systems are discussed. 11 refs., 11 figs

  5. X-ray acquisition and electronic digital readout by charge coupled devices

    International Nuclear Information System (INIS)

    Cavailler, C.; Launspach, J.; Mens, A.; Sauneuf, R.

    1985-09-01

    X-ray imaging adapted to laser-matter interaction experiments consists in recording plasma images from its X-ray emission; these phenomena have between 100 ps and some nanoseconds duration. Investigation of the laser-driven plasma may require the formation and the detection of two-dimensional images formed by X-ray microscopes or spectrometers in the soft X-ray range (from about 50 eV to some keV). To reach that purpose, we have developed and tested two opto-electronic chains. The first one is built around a small image converter tube with a soft X-ray photocathode and P20 phosphor screen deposited on a fiber optic plate; the electronic image appearing on the screen is read by a C.C.D. working in the visible spectral range. The second one, designed to work below 100eV is realized with a very thin phosphor screen deposited on the fiber optic input of a visible microchannel image intensifier; the output image is then read by a C.C.D. in the same manner than previously

  6. 13.1 micrometers hard X-ray focusing by a new type monocapillary X-ray optic designed for common laboratory X-ray source

    Science.gov (United States)

    Sun, Xuepeng; zhang, Xiaoyun; Zhu, Yu; Wang, Yabing; Shang, Hongzhong; Zhang, Fengshou; Liu, Zhiguo; Sun, Tianxi

    2018-04-01

    A new type of monocapillary X-ray optic, called 'two bounces monocapillary X-ray optics' (TBMXO), is proposed for generating a small focal spot with high power-density gain for micro X-ray analysis, using a common laboratory X-ray source. TBMXO is consists of two parts: an ellipsoidal part and a tapered part. Before experimental testing, the TBMXO was simulated by the ray tracing method in MATLAB. The simulated results predicted that the proposed TBMXO would produce a smaller focal spot with higher power-density gain than the ellipsoidal monocapillary X-ray optic (EMXO). In the experiment, the TBMXO performance was tested by both an optical device and a Cu target X-ray tube with focal spot of 100 μm. The results indicated that the TBMXO had a slope error of 57.6 μrad and a 13.1 μm focal spot and a 1360 gain in power density were obtained.

  7. X-ray diffraction

    International Nuclear Information System (INIS)

    Vries, J.L. de.

    1976-01-01

    The seventh edition of Philips' Review of literature on X-ray diffraction begins with a list of conference proceedings on the subject, organised by the Philips' organisation at regular intervals in various European countries. This is followed by a list of bulletins. The bibliography is divided according to the equipment (cameras, diffractometers, monochromators) and its applications. The applications are subdivided into sections for high/low temperature and pressure, effects due to the equipment, small angle scattering and a part for stress, texture and phase analyses of metals and quantitative analysis of minerals

  8. Extracting Galaxy Cluster Gas Inhomogeneity from X-Ray Surface Brightness: A Statistical Approach and Application to Abell 3667

    Science.gov (United States)

    Kawahara, Hajime; Reese, Erik D.; Kitayama, Tetsu; Sasaki, Shin; Suto, Yasushi

    2008-11-01

    Our previous analysis indicates that small-scale fluctuations in the intracluster medium (ICM) from cosmological hydrodynamic simulations follow the lognormal probability density function. In order to test the lognormal nature of the ICM directly against X-ray observations of galaxy clusters, we develop a method of extracting statistical information about the three-dimensional properties of the fluctuations from the two-dimensional X-ray surface brightness. We first create a set of synthetic clusters with lognormal fluctuations around their mean profile given by spherical isothermal β-models, later considering polytropic temperature profiles as well. Performing mock observations of these synthetic clusters, we find that the resulting X-ray surface brightness fluctuations also follow the lognormal distribution fairly well. Systematic analysis of the synthetic clusters provides an empirical relation between the three-dimensional density fluctuations and the two-dimensional X-ray surface brightness. We analyze Chandra observations of the galaxy cluster Abell 3667, and find that its X-ray surface brightness fluctuations follow the lognormal distribution. While the lognormal model was originally motivated by cosmological hydrodynamic simulations, this is the first observational confirmation of the lognormal signature in a real cluster. Finally we check the synthetic cluster results against clusters from cosmological hydrodynamic simulations. As a result of the complex structure exhibited by simulated clusters, the empirical relation between the two- and three-dimensional fluctuation properties calibrated with synthetic clusters when applied to simulated clusters shows large scatter. Nevertheless we are able to reproduce the true value of the fluctuation amplitude of simulated clusters within a factor of 2 from their two-dimensional X-ray surface brightness alone. Our current methodology combined with existing observational data is useful in describing and inferring the

  9. X-ray Fluorescence Spectroscopy: the Potential of Astrophysics-developed Techniques

    Science.gov (United States)

    Elvis, M.; Allen, B.; Hong, J.; Grindlay, J.; Kraft, R.; Binzel, R. P.; Masterton, R.

    2012-12-01

    X-ray fluorescence from the surface of airless bodies has been studied since the Apollo X-ray fluorescence experiment mapped parts of the lunar surface in 1971-1972. That experiment used a collimated proportional counter with a resolving power of ~1 and a beam size of ~1degree. Filters separated only Mg, Al and SI lines. We review progress in X-ray detectors and imaging for astrophysics and show how these advances enable much more powerful use of X-ray fluorescence for the study of airless bodies. Astrophysics X-ray instrumentation has developed enormously since 1972. Low noise, high quantum efficiency, X-ray CCDs have flown on ASCA, XMM-Newton, the Chandra X-ray Observatory, Swift and Suzaku, and are the workhorses of X-ray astronomy. They normally span 0.5 to ~8 keV with an energy resolution of ~100 eV. New developments in silicon based detectors, especially individual pixel addressable devices, such as CMOS detectors, can withstand many orders of magnitude more radiation than conventional CCDs before degradation. The capability of high read rates provides dynamic range and temporal resolution. Additionally, the rapid read rates minimize shot noise from thermal dark current and optical light. CMOS detectors can therefore run at warmer temperatures and with ultra-thin optical blocking filters. Thin OBFs mean near unity quantum efficiency below 1 keV, thus maximizing response at the C and O lines.such as CMOS detectors, promise advances. X-ray imaging has advanced similarly far. Two types of imager are now available: specular reflection and coded apertures. X-ray mirrors have been flown on the Einstein Observatory, XMM-Newton, Chandra and others. However, as X-ray reflection only occurs at small (~1degree) incidence angles, which then requires long focal lengths (meters), mirrors are not usually practical for planetary missions. Moreover the field of view of X-ray mirrors is comparable to the incident angle, so can only image relatively small regions. More useful

  10. Bent crystal X-ray optics for the diagnosis and applications of laser-produced plasmas

    International Nuclear Information System (INIS)

    Loetzsch, Robert

    2012-01-01

    The present thesis discussed several aspects of X-ray optics based on bent crystals and a number of applications of these optics. First, a deeper insight into the reflection properties of elastically bent perfect crystal optics was gained by the consideration of all deformation effects. It was shown that the reflection properties depend on the lateral position on the crystal, an effect that was not addressed before, neither experimentally nor theoretically. To investigate this effect, an apparatus for the measurement of Bragg angles of bent crystals with high angular resolution was built. It was measured that the lattice plane distances of two-dimensionally bent crystals vary laterally by up to 10 -4 . This effect has to be considered in high resolution X-ray spectroscopy and imaging with these bent crystals. It can explain discrepancies in theoretical and experimental spectrometer resolution with spherically bent crystals. Besides these principal investigations, in this thesis a number of X-ray optics were presented that demonstrate the application potential of bent crystal optics. This includes two optics that are used in the field of applications of laser-produced plasmas as high repeating hard X-ray sources. It was shown that an X-ray spectrometer based on full cylinder rings of highly oriented pyrolytic graphite is capable to record the rather weak single shot pulses from a high repeating 1 er-plasma X-ray source. This is possible due to the high collection efficiency of the instrument of up to 5.10 -4 . Furthermore, X-ray optics based on toroidally bent crystals that make it possible to spectrally select a bandwidth of ∝1 eV and focus the ultrashort X-ray pulses from such a laser-plasma source, were designed, prepared and characterized. It was shown that these bent crystals provide the calculated integrated reflectivity, the predicted bandwidth and focus to spot sizes smaller than 60 μm. A novel application of toroidally bent crystals was pointed out: a

  11. Method and apparatus for enhanced sensitivity filmless medical x-ray imaging, including three-dimensional imaging

    Science.gov (United States)

    Parker, Sherwood

    1995-01-01

    A filmless X-ray imaging system includes at least one X-ray source, upper and lower collimators, and a solid-state detector array, and can provide three-dimensional imaging capability. The X-ray source plane is distance z.sub.1 above upper collimator plane, distance z.sub.2 above the lower collimator plane, and distance z.sub.3 above the plane of the detector array. The object to be X-rayed is located between the upper and lower collimator planes. The upper and lower collimators and the detector array are moved horizontally with scanning velocities v.sub.1, v.sub.2, v.sub.3 proportional to z.sub.1, z.sub.2 and z.sub.3, respectively. The pattern and size of openings in the collimators, and between detector positions is proportional such that similar triangles are always defined relative to the location of the X-ray source. X-rays that pass through openings in the upper collimator will always pass through corresponding and similar openings in the lower collimator, and thence to a corresponding detector in the underlying detector array. Substantially 100% of the X-rays irradiating the object (and neither absorbed nor scattered) pass through the lower collimator openings and are detected, which promotes enhanced sensitivity. A computer system coordinates repositioning of the collimators and detector array, and X-ray source locations. The computer system can store detector array output, and can associate a known X-ray source location with detector array output data, to provide three-dimensional imaging. Detector output may be viewed instantly, stored digitally, and/or transmitted electronically for image viewing at a remote site.

  12. Analyser-based x-ray imaging for biomedical research

    International Nuclear Information System (INIS)

    Suortti, Pekka; Keyriläinen, Jani; Thomlinson, William

    2013-01-01

    Analyser-based imaging (ABI) is one of the several phase-contrast x-ray imaging techniques being pursued at synchrotron radiation facilities. With advancements in compact source technology, there is a possibility that ABI will become a clinical imaging modality. This paper presents the history of ABI as it has developed from its laboratory source to synchrotron imaging. The fundamental physics of phase-contrast imaging is presented both in a general sense and specifically for ABI. The technology is dependent on the use of perfect crystal monochromator optics. The theory of the x-ray optics is developed and presented in a way that will allow optimization of the imaging for specific biomedical systems. The advancement of analytical algorithms to produce separate images of the sample absorption, refraction angle map and small-angle x-ray scattering is detailed. Several detailed applications to biomedical imaging are presented to illustrate the broad range of systems and body sites studied preclinically to date: breast, cartilage and bone, soft tissue and organs. Ultimately, the application of ABI in clinical imaging will depend partly on the availability of compact sources with sufficient x-ray intensity comparable with that of the current synchrotron environment. (paper)

  13. X-ray phase imaging using a X-ray tube with a small focal spot. Improvement of image quality in mammography

    International Nuclear Information System (INIS)

    Honda, Chika; Ohara, Hiromu; Ishisaka, Akira; Shimada, Fumio

    2002-01-01

    Phase contrast X-ray imaging has been studied intensively using X-rays from synchrotron radiation and micro-focus X-ray tubes. However, these studies have revealed the difficulty of this technique's application to practical medical imaging. We have created a phase contrast imaging technique using a molybdenum X-ray tube with a small focal spot size for mammography. We identified the radiographic conditions in phase contrast magnification mammography with a screen-film system, where edge effect due to phase contrast overcomes geometrical unsharpness caused by the 0.1 mm-focal spot of a molybdenum X-ray tube. The edge enhancement due to phase imaging was observed in an image of a plastic tube, and then geometrical configuration of the X-ray tube, the object and the screen-film system was determined for phase imaging of mammography. In order to investigate a potential for medical application of this method, we conducted evaluation of the images of the American Collage of Radiology (ACR) 156 mammography phantom. We obtained higher scores for phase imaging using high speed screen-film systems without any increase of X-ray dose than the score for contract imaging using a standard speed screen-film system. (author)

  14. Assessment of firing conditions in old fired-clay bricks: The contribution of X-ray powder diffraction with the Rietveld method and small angle neutron scattering

    Energy Technology Data Exchange (ETDEWEB)

    Viani, Alberto, E-mail: viani@itam.cas.cz [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Sotiriadis, Konstantinos [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Len, Adél [Wigner Research Centre for Physics HAS, Konkoly-Thege 29-33, 1121 Budapest (Hungary); Šašek, Petr; Ševčík, Radek [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic)

    2016-06-15

    Full characterization of fired-clay bricks is crucial for the improvement of process variables in manufacturing and, in case of old bricks, for restoration/replacement purposes. To this aim, five bricks produced in a plant in Czech Republic in the past have been investigated with a combination of analytical techniques in order to derive information on the firing process. An additional old brick from another brickyard was also used to study the influence of different raw materials on sample microstructure. The potential of X-ray diffraction with the Rietveld method and small angle neutron scattering technique has been exploited to describe the phase transformations taking place during firing and characterize the brick microstructure. Unit-cell parameter of spinel and amount of hematite are proposed as indicators of the maximum firing temperature, although for the latter, limited to bricks produced from the same raw material. The fractal quality of the surface area of pores obtained from small angle neutron scattering is also suggested as a method to distinguish between bricks produced from different raw clays. - Highlights: • Rietveld method helps in describing microstructure and physical properties of bricks. • XRPD derived cell parameter of spinel is proposed as an indicator of firing temperature. • SANS effectively describes brick micro and nanostructure, including closed porosity. • Fractal quality of pore surface is proposed as ‘fingerprint’ of brick manufacturing.

  15. A summary of the low angle x-ray atomic scattering factors which have been measured by the critical voltage effect in High Energy Electron Diffraction (HEED)

    International Nuclear Information System (INIS)

    Fox, A.G.; Fisher, R.M.

    1987-08-01

    A tabulated summary of all the accurate (/approximately/0.1%) low-angle x-ray atomic scattering (form) factors which have been determined by the systematic critical voltage technique in HEED is presented. For low atomic number elements (Z/approx lt/40) the low angle form factors can be significantly different to best free atom values, and so the best band structure calculated and/or x-ray measured form factors consistent with the critical voltage measurements are also indicated. At intermediate atomic numbers Z≅40→50 only the very low-angle form factors appear to be different to the best free atom values, and even then only by a small amount. For heavy elements (Z/approx lt/70) the best free atom form factors appear to agree very closely with the critical voltage measured values and so, in this case, critical voltage measurements give very accurate measurements of Debye-Waller factors. 48 refs

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

    Science.gov (United States)

    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.

  17. Peculiarities of section topograms for the multiple diffraction of X rays

    Energy Technology Data Exchange (ETDEWEB)

    Kohn, V. G., E-mail: kohnvict@yandex.ru [National Research Centre “Kurchatov Institute” (Russian Federation); Smirnova, I. A. [Russian Academy of Sciences, Institute of Solid State Physics (Russian Federation)

    2016-07-15

    The distortion of interference fringes on the section topograms of single crystal due to the multiple diffraction of X rays has been investigated. The cases of the 220 and 400 reflections in a silicon crystal in the form of a plate with a surface oriented normally to the [001] direction are considered both theoretically and experimentally. The same section topogram exhibits five cases of multiple diffraction at small azimuthal angles for the 400 reflection and MoK{sub α} radiation, while the topogram for the 220 reflection demonstrates two cases of multiple diffraction. All these cases correspond to different combinations of reciprocal lattice vectors. Exact theoretical calculations of section topograms for the aforementioned cases of multiple diffraction have been performed for the first time. The section topograms exhibit two different distortion regions. The distortions in the central region of the structure are fairly complex and depend strongly on the azimuthal angle. In the tails of the multiple diffraction region, there is a shift of two-beam interference fringes, which can be observed even with a laboratory X-ray source.

  18. A novel solid-angle tomosynthesis (SAT) scanning scheme

    International Nuclear Information System (INIS)

    Zhang Jin; Yu, Cedric

    2010-01-01

    Purpose: Digital tomosynthesis (DTS) recently gained extensive research interests in both diagnostic and radiation therapy fields. Conventional DTS images are generated by scanning an x-ray source and flat-panel detector pair on opposite sides of an object, with the scanning trajectory on a one-dimensional curve. A novel tomosynthesis method named solid-angle tomosynthesis (SAT) is proposed, where the x-ray source scans on an arbitrary shaped two-dimensional surface. Methods: An iterative algorithm in the form of total variation regulated expectation maximization is developed for SAT image reconstruction. The feasibility and effectiveness of SAT is corroborated by computer simulation studies using three-dimensional (3D) numerical phantoms including a 3D Shepp-Logan phantom and a volumetric CT image set of a human breast. Results: SAT is able to cover more space in Fourier domain more uniformly than conventional DTS. Greater coverage and more isotropy in the frequency domain translate to fewer artifacts and more accurately restored features in the in-plane reconstruction. Conclusions: Comparing with conventional DTS, SAT allows cone-shaped x-ray beams to project from more solid angles, thus provides more coverage in the spatial-frequency domain, resulting in better quality of reconstructed image.

  19. A more general expression for the average X-ray diffraction intensity of crystals with an incommensurate one-dimensional modulation

    International Nuclear Information System (INIS)

    Lam, E.J.W.; Beurskens, P.T.; Smaalen, S. van

    1994-01-01

    Statistical methods are used to derive an expression for the average X-ray diffraction intensity, as a function of (sinθ)/λ, of crystals with an incommensurate one-dimensional modulation. Displacive and density modulations are considered, as well as a combination of these two. The atomic modulation functions are given by truncated Fourier series that may contain higher-order harmonics. The resulting expression for the average X-ray diffraction intensity is valid for main reflections and low-order satellite reflections. The modulation of individual atoms is taken into account by the introduction of overall modulation amplitudes. The accuracy of this expression for the average X-ray diffraction intensity is illustrated by comparison with model structures. A definition is presented for normalized structure factors of crystals with an incommensurate one-dimensional modulation that can be used in direct-methods procedures for solving the phase problem in X-ray crystallography. A numerical fitting procedure is described that can extract a scale factor, an overall temperature parameter and overall modulation amplitudes from experimental reflection intensities. (orig.)

  20. Progress in small angle neutron scattering activities in Malaysia

    International Nuclear Information System (INIS)

    Mohamed, Abudl Aziz Bin

    2000-01-01

    Research activities by use of small angle neutron scattering in Malaysia are briefly reported. Scattered neutron data are displayed in two or three-dimensional isometric view by the data acquisition system. Visual Basic is utilized for data acquisition and MathCad for data processing and analyses. (Y. Kazumata)

  1. Progress in small angle neutron scattering activities in Malaysia

    Energy Technology Data Exchange (ETDEWEB)

    Mohamed, Abudl Aziz Bin [Industrial Technology Division, Malaysian Institute for Nuclear Technology Research (MINT) (Indonesia)

    2000-10-01

    Research activities by use of small angle neutron scattering in Malaysia are briefly reported. Scattered neutron data are displayed in two or three-dimensional isometric view by the data acquisition system. Visual Basic is utilized for data acquisition and MathCad for data processing and analyses. (Y. Kazumata)

  2. The one- and two-coordinate x-ray detectors

    International Nuclear Information System (INIS)

    Aulchenko, V.M.; Baru, S.E.; Khabakhpashev, A.G.; Savinov, G.A.

    1992-01-01

    The Institute of Nuclear Physics has designed and fabricated one- and two-coordinate x-ray detectors since 1975. For photon detection multiwire proportional chambers that operate in direct pulse count mode are employed. The characteristics of the detectors allow successful use of them for a wide range of diffractive x-ray structure studies, including studies of dynamics of structure variation (x-ray diffractive movies) and measurements at synchrotron radiation channels

  3. X-ray characterization of solid small molecule organic materials

    Science.gov (United States)

    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.

  4. Two digital X-ray imaging systems for applications in X-ray diffraction

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Stephenson, R.; Flesher, A.C.; Bryant, C.J.; Lincoln, A.D.; Tucker, P.A.; Swanton, S.W.

    1986-08-01

    Two digital X-ray imaging systems developed at the Rutherford Appleton Laboratory are described:- the Mark I and the Mark II. Both use a bidimensionally sensitive Multiwire proportional counter as the basic X-ray image transducer coupled to a digital microcomputer system. The Mark I system provides the advantages of high speed, high sensitivity digital imaging directly into the computer with the potential for software control of the sample orientation and environment. The Mark II system adds the novel features of signal averaging and multi-frame exposures. (author)

  5. X-ray microscopy using grazing-incidence reflections optics

    International Nuclear Information System (INIS)

    Price, R.H.

    1983-01-01

    The role of Kirkpatrick-Baez microscopes as the workhorse of the x-ray imaging devices is discussed. This role is being extended with the development of a 22X magnification Kirkpatrick-Baez x-ray microscope with multilayer x-ray mirrors. These mirrors can operate at large angles, high x-ray energies, and have a narrow, well defined x-ray energy bandpass. This will make them useful for numerous experiments. However, where a large solid angle is needed, the Woelter microscope will still be necessary and the technology needed to build them will be useful for many other types of x-ray optics

  6. New insights into nucleation. Pressure trace measurements and the first small angle X-ray scattering experiments in a supersonic laval nozzle

    International Nuclear Information System (INIS)

    Ghosh, D.

    2007-01-01

    Homogeneous nucleation rates of the n-alcohols and the n-alkanes have been determined by combining information from two sets of supersonic Laval nozzle expansion experiments under identical conditions. The nucleation rates J=N/Δt Jmax for the n-alcohols are in the range of 1.10 17 -3 s -1 17 for the temperatures 207≤T/K≤249, the nucleation rates for the n-alkanes lie in the range of 5.10 15 -3 s -1 18 for the temperatures 143 ≤T/K≤215. For the first time it is shown that the nucleation rate is not only a function of the supersaturation and temperature but clearly also sensitive to the expansion rate during supersonic nozzle expansion. A good agreement between the experimental results and those available in literature is found by applying Hale's scaling formalism [Hale, B., Phys. Rev. A 33, 4256 (1986); Hale, B., Metall. Trans. A 23, 1863 (1992)]. The scaling parameters from this work are also in good agreement with those shown by Rusyniak et al. [Rusyniak, M., M. S. El-Shall, J. Phys. Chem. B 105, 11873 (2001)] and Brus et al. [Brus, D., V. Zdimal F. Stratmann, J. Chem Phys. 124, 164306 (2006)]. In the first experiment static pressure measurements were conducted for the n-alkanes to determine the condensible partial pressure, temperature, supersaturation, characteristic time, and the expansion rate corresponding to the maximum nucleation rate. Characteristic times in the range of 13≤Δt Jmax /μs≤34 were found. In the second set of experiments, the first flow rate resolved Small Angle X-ray Scattering experiments are conducted to determine the particle number density for both substance classes. Particle number densities in the range of 1.10 12 -3 12 and 1.10 11 -3 12 for the n-alcohols and n-alkanes are found, respectively. Additionally, by analyzing the radially averaged scattering spectrum, information on the mean radius and the width of the size distribution of the aerosols is obtained. Mean radii for the n-alcohols in the range of 4< left angle r

  7. Six dimensional X-ray Tensor Tomography with a compact laboratory setup

    Science.gov (United States)

    Sharma, Y.; Wieczorek, M.; Schaff, F.; Seyyedi, S.; Prade, F.; Pfeiffer, F.; Lasser, T.

    2016-09-01

    Attenuation based X-ray micro computed tomography (XCT) provides three-dimensional images with micrometer resolution. However, there is a trade-off between the smallest size of the structures that can be resolved and the measurable sample size. In this letter, we present an imaging method using a compact laboratory setup that reveals information about micrometer-sized structures within samples that are several orders of magnitudes larger. We combine the anisotropic dark-field signal obtained in a grating interferometer and advanced tomographic reconstruction methods to reconstruct a six dimensional scattering tensor at every spatial location in three dimensions. The scattering tensor, thus obtained, encodes information about the orientation of micron-sized structures such as fibres in composite materials or dentinal tubules in human teeth. The sparse acquisition schemes presented in this letter enable the measurement of the full scattering tensor at every spatial location and can be easily incorporated in a practical, commercially feasible laboratory setup using conventional X-ray tubes, thus allowing for widespread industrial applications.

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

    Science.gov (United States)

    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.

  9. Aggregation of bovine serum albumin upon cleavage of its disulfide bonds, studied by the time-resolved small-angle X-ray scattering technique with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Ueki, Tatzuo; Inoko, Yoji; Hiragi, Yuzuru; Kataoka, Mikio; Amemiya, Yoshiyuki; Izumi, Yoshinobu; Tagawa, Hiroyuki; Muroga, Yoshio

    1985-11-01

    A rapid mixing system of the stopped-flow type, used with small-angle X-ray scattering equipment using synchrotron radiation, is described. The process of aggregation of bovine serum albumin was traced with a time interval of 50s, initiated upon cleavage of its disulfide bonds by reduction with dithiothreitol. The results indicate that a 218-fold molar excess of dithiothreitol over the number of moles of disulfide bonds in bovine serum albumin is sufficient to initiate the reaction immediately after mixing, which reaches equilibrium in about 15 min. On the other hand, half this amount is not sufficient to initiate the reaction, so that the reaction is delayed by about 150s. Such a single-shot time-resolved experiment showed that experiments with a time interval of 100 ms are possible with repeated multi-shot runs. 26 refs.; 8 figs.

  10. 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

    Energy Technology Data Exchange (ETDEWEB)

    Szymusiak, Magdalena; Kalkowski, Joseph; Luo, Hanying; Donovan, Alexander J.; Zhang, Pin; Liu, Chang; Shang, Weifeng; Irving, Thomas; Herrera-Alonso, Margarita; Liu, Ying (JHU); (IIT); (UIC)

    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. The structural information at this quasi-equilibrium state can also be used as a reference when studying the kinetics of polymer micellization.

  11. 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

    Energy Technology Data Exchange (ETDEWEB)

    Szymusiak, Magdalena [Department; Kalkowski, Joseph [Department; Luo, Hanying [Department; Donovan, Alexander J. [Department; Zhang, Pin [Department; Liu, Chang [Department; Shang, Weifeng [Department; Irving, Thomas [Department; Herrera-Alonso, Margarita [Department; Liu, Ying [Department; Department

    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. The structural information at this quasi-equilibrium state can also be used as a reference when studying the kinetics of polymer micellization.

  12. Aggregation of bovine serum albumin upon cleavage of its disulfide bonds, studied by the time-resolved small-angle X-ray scattering technique with synchrotron radiation

    International Nuclear Information System (INIS)

    Ueki, Tatzuo; Inoko, Yoji; Izumi, Yoshinobu; Tagawa, Hiroyuki; Muroga, Yoshio

    1985-01-01

    A rapid mixing system of the stopped-flow type, used with small-angle X-ray scattering equipment using synchrotron radiation, is described. The process of aggregation of bovine serum albumin was traced with a time interval of 50 s, initiated upon cleavage of its disulfide bonds by reduction with dithiothreitol. The results indicate that a 218-fold molar excess of dithiothreitol over the number of moles of disulfide bonds in bovine serum albumin is sufficient to initiate the reaction immediately after mixing, which reaches equilibrium in about 15 min. On the other hand, half this amount is not sufficient to initiate the reaction, so that the reaction is delayed by about 150 s. Such a single-shot time-resolved experiment showed that experiments with a time interval of 100 ms are possible with repeated multi-shot runs. (Auth.)

  13. Arrangement for X-ray shield

    International Nuclear Information System (INIS)

    1980-01-01

    X-ray screen unit consisting of a light transmissive carrier onto which scintillation material is deposited, which is able to generate light under the influence of incident X-ray irradiation, characterised in that the X-ray screen comprises a number of sectors, wherein the surface with respect to the incident X-radiation is maintained at an acute angle. (G.C.)

  14. Ultrafast x-ray scattering on nanoparticle dynamics

    International Nuclear Information System (INIS)

    Plech, A; Ibrahimkutty, S; Issenmann, D; Kotaidis, V; Siems, A

    2013-01-01

    Pulsed X-ray scattering is used for the determination of structural dynamics of laser-irradiated gold particles. By combining several scattering methods such as powder scattering, small angle scattering and diffuse wide angle scattering it is possible to reconstruct the kinetics of structure evolution on several lengths scales and derive complementary information on the particles and their local environment. A generic structural phase diagram for the reaction as function of delay time after laser excitation and laser fluence can be constructed.

  15. 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)

    International Nuclear Information System (INIS)

    Rawolle, M.; Körstgens, V.; Ruderer, M. A.; Metwalli, E.; Guo, S.; Müller-Buschbaum, P.; Herzog, G.; Benecke, G.; Schwartzkopf, M.; Buffet, A.; Perlich, J.; Roth, S. V.

    2012-01-01

    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 scattered intensity. Therefore, the acquisition time in GISAXS geometry is reduced significantly at beamline P03.

  16. Glancing angle synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cernik, R J [Daresbury Lab., Warrington, WA (United States)

    1996-09-01

    This paper describes in basic detail some of the techniques that can be used to study thin films and surfaces. These are all in the X-ray region and cover reflectivity, diffraction form polycrystalline films, textured films and single crystal films. Other effects such as fluorescence and diffuse scattering are mentioned but not discussed in detail. Two examples of the reflectivity from multilayers and the diffraction from iron oxide films are discussed. The advantages of the synchrotron for these studies is stressed and the experimental geometries that can be employed are described i detail. A brief bibliography is provided at the end to accompany this part of the 1996 Frascati school.

  17. Glancing angle synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Cernik, R.J.

    1996-01-01

    This paper describes in basic detail some of the techniques that can be used to study thin films and surfaces. These are all in the X-ray region and cover reflectivity, diffraction form polycrystalline films, textured films and single crystal films. Other effects such as fluorescence and diffuse scattering are mentioned but not discussed in detail. Two examples of the reflectivity from multilayers and the diffraction from iron oxide films are discussed. The advantages of the synchrotron for these studies is stressed and the experimental geometries that can be employed are described i detail. A brief bibliography is provided at the end to accompany this part of the 1996 Frascati school

  18. Performance of the PRAXyS X-ray polarimeter

    Energy Technology Data Exchange (ETDEWEB)

    Iwakiri, W.B., E-mail: wataru.iwakiri@riken.jp [RIKEN Nishina Center, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Black, J.K. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Rock Creek Scientific, 1400 East-West Hwy, Silver Spring, MD 20910 (United States); Cole, R. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Enoto, T. [The Hakubi Center for Advanced Research, Kyoto University, Kyoto 606-8302 (Japan); Department of Astronomy, Kyoto University, Kitashirakawa-Oiwake-cho, Sakyo-ku, Kyoto 606-8502 (Japan); Hayato, A. [RIKEN Nishina Center, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Hill, J.E.; Jahoda, K. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Kaaret, P. [University of Iowa, Iowa City, IA 52242 (United States); Kitaguchi, T. [Department of Physical Science, Hiroshima University, 1-3-1 Kagamiyama, Higashi-Hiroshima, Hiroshima 739-8526 (Japan); Kubota, M. [Department of Physics, Tokyo University of Science, 3-1 Kagurazaka, Shinjuku-ku, Tokyo 162-8601, Japan. (Japan); RIKEN Nishina Center, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Marlowe, H.; McCurdy, R. [University of Iowa, Iowa City, IA 52242 (United States); Takeuchi, Y. [Department of Physics, Tokyo University of Science, 3-1 Kagurazaka, Shinjuku-ku, Tokyo 162-8601, Japan. (Japan); RIKEN Nishina Center, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Tamagawa, T. [RIKEN Nishina Center, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Department of Physics, Tokyo University of Science, 3-1 Kagurazaka, Shinjuku-ku, Tokyo 162-8601, Japan. (Japan)

    2016-12-01

    The performance of the Time Projection Chamber (TPC) polarimeter for the Polarimeter for Relativistic Astrophysical X-ray Sources (PRAXyS) Small Explorer was evaluated using polarized and unpolarized X-ray sources. The PRAXyS mission will enable exploration of the universe through X-ray polarimetry in the 2–10 keV energy band. We carried out performance tests of the polarimeter at the Brookhaven National Laboratory, National Synchrotron Light Source (BNL-NSLS) and at NASA's Goddard Space Flight Center. The polarimeter was tested with linearly polarized, monochromatic X-rays at 11 different energies between 2.5 and 8.0 keV. At maximum sensitivity, the measured modulation factors at 2.7, 4.5 and 8.0 keV are 27%, 43% and 59%, respectively and the measured angle of polarization is consistent with the expected value at all energies. Measurements with a broadband, unpolarized X-ray source placed a limit of less than 1% on false polarization in the PRAXyS polarimeter.

  19. Performance of the PRAXyS X-ray polarimeter

    Science.gov (United States)

    Iwakiri, W. B.; Black, J. K.; Cole, R.; Enoto, T.; Hayato, A.; Hill, J. E.; Jahoda, K.; Kaaret, P.; Kitaguchi, T.; Kubota, M.; Marlowe, H.; McCurdy, R.; Takeuchi, Y.; Tamagawa, T.

    2016-12-01

    The performance of the Time Projection Chamber (TPC) polarimeter for the Polarimeter for Relativistic Astrophysical X-ray Sources (PRAXyS) Small Explorer was evaluated using polarized and unpolarized X-ray sources. The PRAXyS mission will enable exploration of the universe through X-ray polarimetry in the 2-10 keV energy band. We carried out performance tests of the polarimeter at the Brookhaven National Laboratory, National Synchrotron Light Source (BNL-NSLS) and at NASA's Goddard Space Flight Center. The polarimeter was tested with linearly polarized, monochromatic X-rays at 11 different energies between 2.5 and 8.0 keV. At maximum sensitivity, the measured modulation factors at 2.7, 4.5 and 8.0 keV are 27%, 43% and 59%, respectively and the measured angle of polarization is consistent with the expected value at all energies. Measurements with a broadband, unpolarized X-ray source placed a limit of less than 1% on false polarization in the PRAXyS polarimeter.

  20. X-ray apparatus

    International Nuclear Information System (INIS)

    Bernstein, S.; Stagg, L.; Lambert, T.W.; Griswa, P.J.

    1976-01-01

    A patient support system for X-ray equipment in arteriographic studies of the heart is described in detail. The support system has been designed to overcome many of the practical problems encountered in using previous types of arteriographic X-ray equipment. The support system is capable of horizontal movement and, by a series of shafts attached to the main support system, the X-ray source and image intensifier or detector may be rotated through the same angle. The system is highly flexible and details are given of several possible operational modes. (U.K.)

  1. An optimised set-up for total reflection particle induced X-ray emission

    International Nuclear Information System (INIS)

    Kan, J.A. van; Vis, R.D.

    1997-01-01

    MeV proton beams at small angles of incidence (0-35 mrad) are used to analyse trace elements on flat surfaces such as Si wafers or quartz substrates. In these experiments, the particle induced X-ray emission (PIXE) signal is used in a new optimized set-up. This set-up is constructed in such a way that the X-ray detector can reach very large solid angles, larger than 1 sr. Use of these large detector solid angles, combined with the reduction of bremsstrahlung background, affords limits of detection (LOD) of the order of 10 10 at cm -2 using total reflection particle induced X-ray emission (TPIXE). The LODs from earlier TPIXE measurements in a non-optimized set-up are used to estimate LODs in the new TPIXE set-up. Si wafers with low surface concentrations of V, Ni, Cu and Ag are used as standards to calibrate the LODs found with this set-up. The metal concentrations are determined by total reflection X-ray fluorescence (TXRF). The TPIXE measurements are compared with TXRF measurements on the same wafers. (Author)

  2. Focal spot size reduction using asymmetric collimation to enable reduced anode angles with a conventional angiographic x-ray tube for use with high resolution detectors

    Science.gov (United States)

    Russ, M.; Shankar, A.; Setlur Nagesh, S. V.; Ionita, C. N.; Bednarek, D. R.; Rudin, S.

    2017-03-01

    The high-resolution requirements for neuro-endovascular image-guided interventions (EIGIs) necessitate the use of a small focal-spot size; however, the maximum tube output limits for such small focal-spot sizes may not enable sufficient x-ray fluence after attenuation through the human head to support the desired image quality. This may necessitate the use of a larger focal spot, thus contributing to the overall reduction in resolution. A method for creating a higher-output small effective focal spot based on the line-focus principle has been demonstrated and characterized. By tilting the C-arm gantry, the anode-side of the x-ray field-of-view is accessible using a detector placed off-axis. This tilted central axis diminishes the resultant focal spot size in the anode-cathode direction by the tangent of the effective anode angle, allowing a medium focal spot to be used in place of a small focal spot with minimal losses in resolution but with increased tube output. Images were acquired of two different objects at the central axis, and with the C-arm tilted away from the central axis at 1° increments from 0°-7°. With standard collimation settings, only 6° was accessible, but using asymmetric extended collimation a maximum of 7° was accessed for enhanced comparisons. All objects were positioned perpendicular to the anode-cathode direction and images were compared qualitatively. The increasing advantage of the off-axis focal spots was quantitatively evidenced at each subsequent angle using the Generalized Measured-Relative Object Detectability metric (GM-ROD). This anode-tilt method is a simple and robust way of increasing tube output for a small field-of-view detector without diminishing the overall apparent resolution for neuro-EIGIs.

  3. Modern X-ray spectroscopy 3. X-ray fluorescence holography

    International Nuclear Information System (INIS)

    Hayashi, Kouichi

    2008-01-01

    X-ray fluorescence holography (XFH) provides three dimensional atomic images around specified elements. The XFH uses atoms as a wave source or monitor of interference field within a crystal sample, and therefore it can record both intensity and phase of scattered X-rays. Its current performance makes it possible to apply to ultra thin film, impurity and quasicrystal. In this article, I show the theory including solutions for twin image problem, advanced measuring system, data processing for reconstruction of the atomic images and for obtaining accurate atomic positions, applications using resonant X-ray scattering and X-ray excited optical luminescence, and an example of XFH result on the local structure around copper in silicon steal. (author)

  4. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive medical ...

  5. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small dose ... limitations of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is ...

  6. Bone X-Ray (Radiography)

    Science.gov (United States)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  7. Abdomen X-Ray (Radiography)

    Science.gov (United States)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Abdomen Abdominal x-ray uses a very small ... of an abdominal x-ray? What is abdominal x-ray? An x-ray (radiograph) is a noninvasive medical ...

  8. Small angle scattering of X radiation and slow neutrons in structural analyses of amorphous solids

    International Nuclear Information System (INIS)

    Kostorz, G.

    1980-01-01

    Small angle scattering of x radiation and slow neutrons allows to detect inhomogeneities of the dimension of ten to some thousands of Angstroem by the difference in the scattering length density. The progress made during recent years in the development of apparatusses has created the possibility of solving very complicated problems. A first outline shows that in separation processes as well as in investigating extended defects the method of small angle scattering may provide valuable contributions to the analysis of the non-crystalline state

  9. X-ray microscopy using grazing-incidence reflection optics

    International Nuclear Information System (INIS)

    Price, R.H.

    1981-01-01

    The Kirkpatrick-Baez microscopes are described along with their role as the workhorse of the x-ray imaging devices. This role is being extended with the development of a 22X magnification Kirkpatrick-Baez x-ray microscope with multilayer x-ray mirrors. These mirrors can operate at large angles, high x-ray energies, and have a narrow, well defined x-ray energy bandpass. This will make them useful for numerous experiments. However, where a large solid angle is needed, the Woelter microscope will still be necessary and the technology needed to build them will be useful for many other types of x-ray optics

  10. Chest X-Ray

    Medline Plus

    Full Text Available ... about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed x-ray exams and use a very small dose of ... of the inside of the chest. A chest x-ray is used to evaluate the lungs, heart and ...

  11. Proceedings of the workshop on small angle scattering data analysis. Micelle related topics

    Energy Technology Data Exchange (ETDEWEB)

    Yamaguchi, Toshio [Fukuoka Univ. (Japan). Faculty of Science; Furusaka, Michihiro; Ohtomo, Toshiya [eds.

    1996-02-01

    This workshop was held on December 13 and 14, 1995 at National Laboratory for High Energy Physics. At the workshop, the purpose of the workshop was explained, and lectures were given on the research on superhigh molecular structure by small angle neutron scattering, the verification of the reliability of WINK data (absolute intensity), the analysis of WINK data, the new data program of SAN, small angle X-ray scattering data analysis program (SAXS), the basis of the analysis of micelle system, analysis software manual and practice program Q-I(Q) ver 1.0, various analysis methods for small angle scattering and contrast modulation method and others, the ordering of and the countermeasures to the problems of WINK, and the hereafter of KENS small angle scattering facility. How to treat the analysis related to micelle, how to save WINK and how to install the SAN/reflectometer are the matters to be discussed at the workshop. In this book, the summaries of the lectures are collected. (K.I.)

  12. Angle-resolved X-ray fluorescence spectrometry using synchrotron radiation at ELSA

    International Nuclear Information System (INIS)

    Schmitt, W.; Rothe, J.; Hormes, J.; Gries, W.H.

    1994-01-01

    Measurements on the centroid depth of ion-implanted phosphorus-in-silicon specimen by the method of angle-resolved, self-ratio X-ray fluorescence spectrometry (AR/SR/XFS) have been carried out using 'white' synchrotron radiation (SR). The measurements were performed using a modified wavelength-dispersive fluorescence spectrometer. Problems due to the use of SR, like carbonaceous specimen contamination and sample heating were overcome by flooding the specimen chamber with helium and by pre-absorbing the non-exciting parts of the incident SR with suitable filters, respectively. The decaying primary intensity was monitored by measuring the compensation current of the photoelectrons emitted from a tungsten wire stretched across the primary beam. Results have been obtained for specimen with dose density levels of 10 16 cm -2 and 3x10 15 cm -2 . (orig.)

  13. Energy dependence measurement of small-type optically stimulated luminescence (OSL) dosimeter by means of characteristic X-rays induced with general diagnostic X-ray equipment.

    Science.gov (United States)

    Takegami, Kazuki; Hayashi, Hiroaki; Okino, Hiroki; Kimoto, Natsumi; Maehata, Itsumi; Kanazawa, Yuki; Okazaki, Tohru; Hashizume, Takuya; Kobayashi, Ikuo

    2016-01-01

    For X-ray inspections by way of general X-ray equipment, it is important to measure an entrance-skin dose. Recently, a small optically stimulated luminescence (OSL) dosimeter was made commercially available by Landauer, Inc. The dosimeter does not interfere with the medical images; therefore, it is expected to be a convenient detector for measuring personal exposure doses. In an actual clinical situation, it is assumed that X-rays of different energies will be detected by a dosimeter. For evaluation of the exposure dose measured by a dosimeter, it is necessary to know the energy dependence of the dosimeter. Our aim in this study was to measure the energy dependence of the OSL dosimeter experimentally in the diagnostic X-ray region. Metal samples weighing several grams were irradiated and, in this way, characteristic X-rays having energies ranging from 8 to 85 keV were generated. Using these mono-energetic X-rays, the dosimeter was irradiated. Simultaneously, the fluence of the X-rays was determined with a CdTe detector. The energy-dependent efficiency of the dosimeter was derived from the measured value of the dosimeter and the fluence. Moreover, the energy-dependent efficiency was calculated by Monte-Carlo simulation. The efficiency obtained in the experiment was in good agreement with that of the simulation. In conclusion, our proposed method, in which characteristic X-rays are used, is valuable for measurement of the energy dependence of a small OSL dosimeter in the diagnostic X-ray region.

  14. Three-dimensional cascaded system analysis of a 50 µm pixel pitch wafer-scale CMOS active pixel sensor x-ray detector for digital breast tomosynthesis.

    Science.gov (United States)

    Zhao, C; Vassiljev, N; Konstantinidis, A C; Speller, R D; Kanicki, J

    2017-03-07

    High-resolution, low-noise x-ray detectors based on the complementary metal-oxide-semiconductor (CMOS) active pixel sensor (APS) technology have been developed and proposed for digital breast tomosynthesis (DBT). In this study, we evaluated the three-dimensional (3D) imaging performance of a 50 µm pixel pitch CMOS APS x-ray detector named DynAMITe (Dynamic Range Adjustable for Medical Imaging Technology). The two-dimensional (2D) angle-dependent modulation transfer function (MTF), normalized noise power spectrum (NNPS), and detective quantum efficiency (DQE) were experimentally characterized and modeled using the cascaded system analysis at oblique incident angles up to 30°. The cascaded system model was extended to the 3D spatial frequency space in combination with the filtered back-projection (FBP) reconstruction method to calculate the 3D and in-plane MTF, NNPS and DQE parameters. The results demonstrate that the beam obliquity blurs the 2D MTF and DQE in the high spatial frequency range. However, this effect can be eliminated after FBP image reconstruction. In addition, impacts of the image acquisition geometry and detector parameters were evaluated using the 3D cascaded system analysis for DBT. The result shows that a wider projection angle range (e.g.  ±30°) improves the low spatial frequency (below 5 mm -1 ) performance of the CMOS APS detector. In addition, to maintain a high spatial resolution for DBT, a focal spot size of smaller than 0.3 mm should be used. Theoretical analysis suggests that a pixelated scintillator in combination with the 50 µm pixel pitch CMOS APS detector could further improve the 3D image resolution. Finally, the 3D imaging performance of the CMOS APS and an indirect amorphous silicon (a-Si:H) thin-film transistor (TFT) passive pixel sensor (PPS) detector was simulated and compared.

  15. 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

    Science.gov (United States)

    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.

  16. Soft X-Ray Observations of a Complete Sample of X-Ray--selected BL Lacertae Objects

    Science.gov (United States)

    Perlman, Eric S.; Stocke, John T.; Wang, Q. Daniel; Morris, Simon L.

    1996-01-01

    We present the results of ROSAT PSPC observations of the X-ray selected BL Lacertae objects (XBLs) in the complete Einstein Extended Medium Sensitivity Survey (EM MS) sample. None of the objects is resolved in their respective PSPC images, but all are easily detected. All BL Lac objects in this sample are well-fitted by single power laws. Their X-ray spectra exhibit a variety of spectral slopes, with best-fit energy power-law spectral indices between α = 0.5-2.3. The PSPC spectra of this sample are slightly steeper than those typical of flat ratio-spectrum quasars. Because almost all of the individual PSPC spectral indices are equal to or slightly steeper than the overall optical to X-ray spectral indices for these same objects, we infer that BL Lac soft X-ray continua are dominated by steep-spectrum synchrotron radiation from a broad X-ray jet, rather than flat-spectrum inverse Compton radiation linked to the narrower radio/millimeter jet. The softness of the X-ray spectra of these XBLs revives the possibility proposed by Guilbert, Fabian, & McCray (1983) that BL Lac objects are lineless because the circumnuclear gas cannot be heated sufficiently to permit two stable gas phases, the cooler of which would comprise the broad emission-line clouds. Because unified schemes predict that hard self-Compton radiation is beamed only into a small solid angle in BL Lac objects, the steep-spectrum synchrotron tail controls the temperature of the circumnuclear gas at r ≤ 1018 cm and prevents broad-line cloud formation. We use these new ROSAT data to recalculate the X-ray luminosity function and cosmological evolution of the complete EMSS sample by determining accurate K-corrections for the sample and estimating the effects of variability and the possibility of incompleteness in the sample. Our analysis confirms that XBLs are evolving "negatively," opposite in sense to quasars, with Ve/Va = 0.331±0.060. The statistically significant difference between the values for X-ray

  17. Cone Beam X-Ray Luminescence Tomography Imaging Based on KA-FEM Method for Small Animals.

    Science.gov (United States)

    Chen, Dongmei; Meng, Fanzhen; Zhao, Fengjun; Xu, Cao

    2016-01-01

    Cone beam X-ray luminescence tomography can realize fast X-ray luminescence tomography imaging with relatively low scanning time compared with narrow beam X-ray luminescence tomography. However, cone beam X-ray luminescence tomography suffers from an ill-posed reconstruction problem. First, the feasibility of experiments with different penetration and multispectra in small animal has been tested using nanophosphor material. Then, the hybrid reconstruction algorithm with KA-FEM method has been applied in cone beam X-ray luminescence tomography for small animals to overcome the ill-posed reconstruction problem, whose advantage and property have been demonstrated in fluorescence tomography imaging. The in vivo mouse experiment proved the feasibility of the proposed method.

  18. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  19. Mapping of auroral x-rays from rocket overflights

    International Nuclear Information System (INIS)

    Goldberg, R.A.; Barcus, J.R.; Treinish, L.A.; Vondrak, R.R.

    1982-01-01

    In March 1978, two Nike Tomahawk payloads were launched from Poker Flat, Alaska, to observe the structure of bremsstrhlung x rays and precipitating particles during both nighttime and daytime observe x rays in four spectral ranges (5--10 keV, 10--20 keV, 20--40 keV, and >40 keV). Particle contamination of the detectors was avoided with broom magnet shielding techniques. By virtue of the payloads' approximate 20 0 coning angle (about 10.5-s period), the detectors scanned wide regions on either side of the trajectory paths. This has permitted construction (using computer color graphics) of the time averaged (approx.4 min) x ray source regions near 100 km, a height consistent with Chatanika radar electron density maps obtained during each flight period. X ray image maps for both flights exhibit enhanced source regions well outside the rocket trajectory planes. For the nighttime overflight, Chatanika radar scan data and Fort Yukon riometer data were used to verify the presence of an x ray imaged enhancement of electron precipitation, approximately 30 km to the east of the rocket trajectory plane. The daytime x ray data also exhibited several regions of enhanced emission, but outside the region scanned by Chatanika radar. A comparison of the x ray emissions from the two events shows the daytime x ray spectral distributions to be significantly harder but less intense that the nighttime distributions. Furthermore, for both events, spectra compared within and nearby each enhanced emitting region exhibit characteristics of a two component spectrum, such that the bright regions show an increased flux primarily in the low-energy component. Electron fluxes measured on each of the two flights with Geiger tubes are mainly isotropic over the downward hemisphere at night but show anisotropic pitch angle characteristics by day, consistent with the concept that the enhancement of the low-energy x ray flux component is predominantly induced by electrons filling the loss cone

  20. Bone X-ray absorptiometry using two energies

    International Nuclear Information System (INIS)

    Laval-Jeantet, A.M.; Laval-Jeantet, M.; Bloch, J.

    1979-01-01

    A method of X-ray absorptiometry using two energies (28 and 36 keV) as a means of determining mineralisation of a bone specimen is described. The ratio of coefficients determined at the different energies varies according to the total mineralisation of the bone studied. A model, representing a serie of bone specimens constructed to study this relationship is described. The coefficients of attenuation for a given wavelength were measured. The relation between the coefficients found at two energies for a given specimen of known mineral content was found to vary as a function of the mineralisation. It is possible to determine the coefficient of attenuation characteristic of a bone and hence its mineralisation and thickness by measurements at two different wavelengths using this function. Experimental results show this potential of the method, but also its high sensitivity to small measurements errors [fr