WorldWideScience

Sample records for synchrotron small-angle x-ray

  1. 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.

  2. 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.

  3. The small-angle X-ray scattering beamline of the Brazilian Synchrotron Light Laboratory

    International Nuclear Information System (INIS)

    Kellermann, G.; Vicentin, F.; Tamura, E.; Rocha, M.; Tolentino, H.; Craievich, A.; Barbosa, A.; Torriani, I.

    1997-01-01

    This paper describes the small-angle scattering beamline built at the Brazilian synchrotron light laboratory (LNLS). Vertical focusing of the synchrotron beam is achieved by an elastically bent gold-plated cylindrical mirror. An asymmetric cut curved triangle-shaped silicon single crystal (111 reflection) is used for monochromatization and horizontal focusing. The mirror, monochromator optics and 2θ arm were designed to cover the spectral range between 1.0 and 2.0 A. Three slit sets, a secondary photon shutter, two beam monitors, filters and absorbers, a multi-sample holder, a vacuum path, a beam-stopper and a set of detectors are the basic components of the workstation. The stepping motors are equipped with specially designed encoders. All mechanical and pneumatic movements and detectors can be remotely controlled using a direct panel or a PC. (orig.)

  4. Structural Studies of Bleached Melanin by Synchrotron Small-angle X-ray Scattering¶

    Energy Technology Data Exchange (ETDEWEB)

    Littrell, Kenneth C.; Gallas, James M.; Zajac, Gerry W.; Thiyagarajan, Pappannan

    2003-01-01

    Small-angle X-ray scattering was used to measure the effects of chemical bleaching on the size and morphology of tyrosine-derived synthetic melanin dispersed in aqueous media. The average size as measured by the radius of gyration of the melanin particles in solution, at neutral to mildly basic pH, decreases from 16.5 to 12.5 angstroms with increased bleaching. The melanin particles exhibit scattering characteristic of sheet-like structures with a thickness of approximately 11 angstroms at all but the highest levels of bleaching. The scattering data are well described by the form factor for scattering from a pancake-like circular cylinder. These data are consistent with the hypothesis that unbleached melanin, at neutral to mildly basic pH, is a planar aggregate of 6- to 10-nm-sized melanin protomolecules, hydrogen bonded through their quinone and phenolic perimeters. The observed decrease in melanin particle size with increased bleaching is interpreted as evidence for deaggregation, most probably the result of oxidative disruption of hydrogen bonds and an increase in the number of charged, carboxylic acid groups, whereby the melanin aggregates disassociate into units composed of decreasing numbers of protomolecules.

  5. 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

  6. 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.

  7. Small-angle x-ray scattering/diffraction system for studies of biological and other materials at the Stanford Synchrotron Radiation Laboratory (abstract)

    International Nuclear Information System (INIS)

    Wakatsuki, S.; Hodgson, K.O.; Eliezer, D.; Rice, M.; Hubbard, S.; Gillis, N.; Doniach, S.; Spann, U.

    1992-01-01

    A versatile small-angle x-ray diffraction/scattering system has been developed at Stanford Synchrotron Radiation Laboratory for studies of biological and other materials. The system includes two sets of collimation slits separated by an ionization chamber, a sample holder cooled by a circulation bath, a vacuum/He scattering path after the sample holder and a detector, either a linear one-dimensional position-sensitive proportional counter or a position-sensitive quadrant detector. Data aquisition is controlled by a VAXstation through a CAMAC interface. Menu-driven data acquisition and on-line analysis software has been developed. The system can be used to collect small- to intermediate-angle x-ray scattering and diffraction data. Monochromatic, anomalous, and time-resolved diffraction/scattering experiments are possible. A time-resolved spectrophotometer using photodiode arrays has also been developed for simultaneous measurements of optical absorption spectra and x-ray scattering/diffraction

  8. Effect of additives on distributions of lamellar structures in sheared polymer: a study of synchrotron small-angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Zhu Pengwei; Edward, Graham [Cooperative Research Center for Polymers (Australia); Nichols, Lance [Cooperative Research Centre for Polymers, Vic 3800 (Australia)

    2009-12-21

    The effects of additives on the distributions of lamellar morphology and orientation in sheared isotactic polypropylene were investigated using the small beam of synchrotron small-angle x-ray scattering. The Cu-phthalocyanine can template the lamellar orientation even under low shear rates, whereas the ultramarine blue cannot. The surface contact is suggested to play a role in stabilizing the formation of oriented nuclei which subsequently direct the growth of oriented lamellae. The additives have no notable effects on the long spacing in the shear region. However, at high shear rates, they decrease the thickness of crystalline lamellae or increase the thickness of amorphous lamellae. Since the additives increase the degree of volume crystalline in the shear region, the number of crystalline lamellae should be increased. The results are helpful in designing and selecting suitable additives for controlling lamellar morphology and orientation.

  9. In Situ Lipolysis and Synchrotron Small-Angle X-ray Scattering for the Direct Determination of the Precipitation and Solid-State Form of a Poorly Water-Soluble Drug During Digestion of a Lipid-Based Formulation

    DEFF Research Database (Denmark)

    Khan, Jamal; Hawley, Adrian; Rades, Thomas

    2016-01-01

    In situ lipolysis and synchrotron small-angle X-ray scattering (SAXS) were used to directly detect and elucidate the solid-state form of precipitated fenofibrate from the digestion of a model lipid-based formulation (LBF). This method was developed in light of recent findings that indicate...

  10. 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

  11. 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 ...

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

    Indian Academy of Sciences (India)

    Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400 085, India. *Corresponding author ... ticles dispersed in the matrix was characterized by small angle neutron scattering (SANS) and small angle X-ray ... for scattering from rough pore–mass interfaces, α > 3 and the (surface) fractal dimension Ds = 6 ...

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

    Indian Academy of Sciences (India)

    2015-11-27

    Nov 27, 2015 ... Small angle neutron scattering and small angle X-ray scattering studies of platinum-loaded carbon foams. P U Sastry V K Aswal A G Wagh ... Proceedings of the International Workshop/Conference on Computational Condensed Matter Physics and Materials Science (IWCCMP-2015). Posted on November ...

  14. 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.

  15. Synchrotron X-ray and neutron small-angle scattering of lyotropic lipid mesophases, model biomembranes and proteins in solution at high pressure.

    Science.gov (United States)

    Winter, Roland

    2002-03-25

    In this review we discuss the use of X-ray and neutron diffraction methods for investigating the temperature- and pressure-dependent structure and phase behaviour of lipid and model biomembrane systems. Hydrostatic pressure has been used as a physical parameter for studying the stability and energetics of lipid mesophases, but also because high pressure is an important feature of certain natural membrane environments and because the high pressure phase behaviour of biomolecules is of importance for several biotechnological processes. Using the pressure jump relaxation technique in combination with time-resolved synchrotron X-ray diffraction, the kinetics of different lipid phase transformations was investigated. The techniques can also be applied to the study of other soft matter and biomolecular phase transformations, such as surfactant phase transitions and protein un/refolding reactions. Several examples are given. In particular, we present data on the pressure-induced unfolding and refolding of small proteins, such as Snase. The data are compared with the corresponding results obtained using other trigger mechanisms and are discussed in the light of recent theoretical approaches.

  16. 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

  17. Ultra-small angle X-ray diffraction from muscle

    Energy Technology Data Exchange (ETDEWEB)

    Nave, C.; Diakun, G.P.; Bordas, J.

    1986-05-15

    An ultra-small angle X-ray scattering instrument is described. It uses two channel cut crystals, one to monochromatise and collimate the beam and the other to analyse the scattered radiation. It has been used to collect diffraction data from muscle, in which the physiological unit cell, the sarcomere, has a repeat of 2000 nm or more.

  18. Small angle x-ray scattering and its applications

    International Nuclear Information System (INIS)

    Buckely, C.E.

    2002-01-01

    Full text: Small angle X-ray scattering is an excellent technique to characterise inhomogeneities in materials in the size range from 1 nm - several hundred nm. Ultra small angle X-ray scattering has extended this size range out to 20 μm. SAXS is due to the electron density difference between the matrix and the inhomogeneity. SAXS and small angle neutron scattering have been successfully used to characterise colloidal particles in solution, colloidal powders, macromolecules, glasses and a wide range of solids such as metals, alloys, and natural and synthetic high polymers. Small angle scattering and complementary techniques, such as transmission and scanning electron microscopy are a powerful combination for the investigation of submicron particles. This talk will introduce the small angle scattering technique and its applications, and will also describe the new Nanostar SAXS instrument in the Department of Applied Physics at Curtin University that has been purchased through a 2001 Australian Research Council research infrastructure and equipment fund (2001 ARC RIEF) grant. Copyright (2002) Australian X-ray Analytical Association Inc

  19. 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 ...

  20. 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

  1. 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.

  2. 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.

  3. Studies on polymer thin film structure by X-ray and neutron reflectivity and grazing incidence small angle scattering

    International Nuclear Information System (INIS)

    Ogawa, Hiroki; Kanaya, Toshiji

    2011-01-01

    We have reviewed structure studies of polymer thin films using synchrotron radiation X-ray and neutron reflectivity as well as recently developed grazing incidence small-angle X-ray and neutron scattering, including studies on polymer thin films with embedded ordered nanometer cells, distribution of glass transition temperature Tg in thin polystyrene films, and dewetting process of polymer blend thin films. (author)

  4. 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)

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

    Science.gov (United States)

    Pillon, Monica C; Guarné, Alba

    2017-11-01

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

  6. 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 simultaneous SAXS and ultraviolet absorption measurements during protein dialysis, integrated directly on a SAXS beamline. Microfluidic dialysis can be used for monitoring structural changes in response to buffer exchange or, as demonstrated, protein concentration. By collecting X-ray data during...... the concentration procedure, the risk of inducing protein aggregation due to excessive concentration and storage is eliminated, resulting in reduced sample consumption and improved data quality. The proof of concept demonstrates the effect of halted or continuous flow in the microfluidic device. No sample...

  7. Ultra-small-angle x-ray scattering by single-crystal Al deformed in situ

    Science.gov (United States)

    Long, Gabrielle; Levine, Lyle

    1997-03-01

    Among the earliest small-angle x-ray scattering and small-angle neutron scattering experiments were attempts to study dislocation structures. These structures have proven to be very difficult to measure because of the intrinsically low contrast of the microstructure, and the requirement that multiple Bragg diffraction be strictly avoided. Thus, many attempts to measure dislocation structures have been compromised by these difficulties. We present results from ultra-small-angle x-ray scattering measurements on single-crystal Al, deformed in situ on beam line X23A3 at the National Synchrotron Light Source. Radiographic images, which are in the O-beam position for diffraction, were taken of the scattering volume. The Al crystal was also rotated to ensure that the scattering data would be accumulated in a region sufficiently distant from accidental Bragg diffractions. Stress-strain data were obtained simultaneously with the x-ray scattering data. We report on the evolution of dislocation structures from 0% strain to 18% strain.

  8. Microstructural Investigations by Small Angle Scattering of Neutrons and X-rays

    Science.gov (United States)

    Fiori, F.; Spinozzi, F.

    Small angle scattering techniques [77, 103, 106, 156, 242, 254] (SANS when using neutron beams or SAXS when using conventional X-ray radiation sources or synchrotron radiation) are experimental methods allowing the determination of structural features, such as size and volume fraction, of matrix inhomogeneities in a huge variety of materials, covering studies from biochemistry and biophysics to applied and industrial research. The order of magnitude of the size of objects that can be detected is in the approximate range 1-103 nm, but with special methods (Ultra-SANS) also objects up to tens of micrometerscan be investigated.

  9. 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.

  10. 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)

  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. X-ray fluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Raman, S.; Sparks, C.J. Jr.

    1978-01-01

    An experimental set-up for x-ray fluorescence analysis with synchrotron radiation was built and installed at the Stanford Synchrotron Radiation Project. X-ray spectra were taken from numerous and varied samples in order to assess the potential of synchrotron radiation as an excitation source for multielement x-ray fluorescence analysis. For many applications, the synchrotron radiation technique is shown to be superior to other x-ray fluorescence methods, especially those employing electrons and protons as excitation sources

  13. 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)

  14. 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.

  15. 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

  16. Small-Angle X-ray Scattering Screening Complements Conventional Biophysical Analysis

    DEFF Research Database (Denmark)

    Tian, Xinsheng; Langkilde, Annette Eva; Thorolfsson, Matthias

    2014-01-01

    introduce small-angle X-ray scattering (SAXS) to characterize antibody solution behavior, which strongly complements conventional biophysical analysis. First, we apply a variety of conventional biophysical techniques for the evaluation of structural, conformational, and colloidal stability and report...

  17. 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.

  18. 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.

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

    Science.gov (United States)

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

    2017-04-01

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

  20. Anomalous small-angle X-ray scattering from charged soft matter

    Science.gov (United States)

    Sztucki, M.; Di Cola, E.; Narayanan, T.

    2012-06-01

    A review of recent applications of Anomalous Small-Angle X-ray Scattering (ASAXS) to charged soft matter systems is presented. Although the potential of ASAXS was realized in the eighties [1], applications to soft matter systems became feasible in recent years thanks to the technical developments at the synchrotron sources. Examples include both stiff chain and flexible polyelectrolytes, colloidal brush-like polyelectrolytes, DNA, RNA, and polysaccharides where the counterion profile could be determined with high precision and compared with theoretical models. In addition, ASAXS has also been found useful for microstructure characterization in soft materials. Finally, the present capability for ASAXS studies is illustrated by an example involving a surfactant micellar system.

  1. Small Angle X-ray Scattering: Going Beyond the Bragg Peaks -24 ...

    Indian Academy of Sciences (India)

    This article gives an introduction to the princi- ples of small angle scattering. Some applications of this technique are also briefly discussed. Introduction. Small angle X-ray scattering (SAXS) is a widely used technique to study large scale inhomogeneities in a med- ium, at length scales much larger than the wavelength.

  2. Small angle X-ray scattering studies on the X-ray induced aggregation of malate synthase

    International Nuclear Information System (INIS)

    Zipper, P.; Durchschlag, H.

    1980-01-01

    Malate synthase was investigated by the small-angle X-ray scattering technique in aqueous solution. Measurements extending for several hours revealed a continuous increase of the intensity in the innermost portion of the scattering curve. There is clear evidence that this increase was caused by an X-ray induced aggregation of enzyme particles during the performance of the small-angle X-ray scattering experiment. The monitoring of the aggregation process in situ by means of small-angle X-ray scattering led to a model of the way how the aggregation might proceed. The analysis of the scattering curves of malate synthase taken at various stages of aggregation established the retention of the thickness factor of the native enzyme and the occurrence of one and later on of two cross-section factors. The process of aggregation was also reflected by the increase of extension of the distance distribution function. Measurements of enzymic activity and small-angle X-ray scattering on samples, which had been X-irradiated with a defined dose prior to the measurements, established two different series of efficiency for the protection of the enzyme against aggregation and inactivation. The results showed that there is no direct relation between the extent of aggregation and the loss of enzymic activity. (orig./MG) [de

  3. The Use of Small-Angle X-Ray Diffraction Studies for the Analysis of Structural Features in Archaeological Samples

    DEFF Research Database (Denmark)

    Wess, T. J.; Drakopoulos, M.; Snigirev, A.

    2001-01-01

    the potential of a laboratory source is also described. Specific examples of analysis using X-ray diffraction of historic parchment, archaeological bone, a Central Mexico style pictograph and microdiffraction of calcified tissues are used to show the scope and versatility of the technique. Diffraction data......X-ray diffraction or scattering analysis provides a powerful non-destructive technique capable of providing important information about the state of archaeological samples in the nanometer length scale. Small-angle diffraction facilities are usually found at synchrotron sources, although...

  4. Small-angle X-ray scattering (SAXS) studies of the structure of mesoporous silicas

    Science.gov (United States)

    Zienkiewicz-Strzałka, M.; Skibińska, M.; Pikus, S.

    2017-11-01

    Mesoporous ordered silica nanostructures show strong interaction with X-ray radiation in the range of small-angles. Small-angle X-ray scattering (SAXS) measurements based on the elastically scattered X-rays are important in analysis of condensed matter. In the case of mesoporous silica materials SAXS technique provides information on the distribution of electron density in the mesoporous material, in particular describing their structure and size of the unit cell as well as type of ordered structure and finally their parameters. The characterization of nanopowder materials, nanocomposites and porous materials by Small-Angle X-ray Scattering seems to be valuable and useful. In presented work, the SAXS investigation of structures from the group of mesoporous ordered silicates was performed. This work has an objective to prepare functional materials modified by noble metal ions and nanoparticles and using the small-angle X-ray scattering to illustrate their properties. We report the new procedure for describing mesoporous materials belonging to SBA-15 and MCM-41 family modified by platinum, palladium and silver nanoparticles, based on detailed analysis of characteristic peaks in the small-angle range of X-ray scattering. This procedure allows to obtained the most useful parameters for mesoporous materials characterization and their successfully compare with experimental measurements reducing the time and material consumption with good precision for particles and pores with a size below 10 nm.

  5. 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.)

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

    Science.gov (United States)

    Rambo, Robert P; Tainer, John A

    2010-03-01

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

  7. 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.)

  8. 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.

  9. 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 (Jiaotong); (Peac)

    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.

  10. 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...... 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...

  11. 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.

  12. A simple model for dynamic small-angle X-ray diffraction in colloidal crystals

    NARCIS (Netherlands)

    de Beer, A.G.F.; Petukhov, A.V.

    2007-01-01

    A simple model is presented that allows calculation of the small-angle X-ray diffraction patterns of perfect colloidal crystals. The model is based on the Wentzel–Kramers–Brillouin approximation and permits a straightforward evaluation of multibeam interactions. Results are illustrated by several

  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. Analysis of slit-distored small-angle X-ray scattering intensities without desmearing

    Energy Technology Data Exchange (ETDEWEB)

    Goodisman, J.; Delaglio, F.; Brumberger, H.

    1986-08-01

    Experimental small-angle X-ray scattering intensities, generated from a primary beam of known intensity profile, are often ''desmeared'' to obtain point-collimated intensities. A much simpler way is shown of using the known beam intensity profile to derive, from the experimental scattering intensity, the quantities required for calculation of surface areas.

  15. 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.

  16. 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.

  17. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Sedlak, Steffen M.; Bruetzel, Linda K.; Lipfert, Jan (LMU)

    2017-03-29

    A new model is proposed for the measurement errors incurred in typical small-angle X-ray scattering (SAXS) experiments, which takes into account the setup geometry and physics of the measurement process. The model accurately captures the experimentally determined errors from a large range of synchrotron and in-house anode-based measurements. Its most general formulation gives for the variance of the buffer-subtracted SAXS intensity σ2(q) = [I(q) + const.]/(kq), whereI(q) is the scattering intensity as a function of the momentum transferq;kand const. are fitting parameters that are characteristic of the experimental setup. The model gives a concrete procedure for calculating realistic measurement errors for simulated SAXS profiles. In addition, the results provide guidelines for optimizing SAXS measurements, which are in line with established procedures for SAXS experiments, and enable a quantitative evaluation of measurement errors.

  19. Construction of a two-dimensional ultra-small-angle X-ray scattering apparatus

    International Nuclear Information System (INIS)

    Konishi, T.; Yamahara, E.; Furuta, T.; Ise, N.

    1997-01-01

    A two-dimensional ultra-small-angle X-ray scattering (USAXS) apparatus was constructed using a rotating-anode X-ray generator and a Bonse-Hart camera. In this camera, two sets of two channel-cut single crystals were used to collimate the X-ray beam in both the horizontal and the vertical planes. The measured intensity profile of the direct beam showed a high small-angle resolution in all directions on the detector plane. The full width at half-maximum was 17 '' , indicating that the apparatus can be applied to structural analysis in the range up to 2 μm, even for directionally oriented samples. One- and two-dimensional USAXS profiles from colloidal silica powder agreed well with each other, showing that the desmearing procedure adopted in the previous one-dimensional USAXS experiments were justified. (orig.)

  20. Characterization of nano-structure by small-angle X-ray and neutron scattering

    International Nuclear Information System (INIS)

    Ohnuma, Masato

    2017-01-01

    This paper outlines the cases when small-angle X-ray scattering method and small-angle neutron scattering method in transmission arrangement were applied to heterogeneity with low-volume rate (10% or below), such as nano-sized deposits and trace defects. In particular, it explains not only general analysis, but also the possibility of use of the small angle scattering method as a simple inspection method in nanostructure evaluation, as well as correspondence of small-angle scattering method with powder diffraction method in crystal structure evaluation. From the small-angle scattering profiles of a series of sample groups, we can judge which sample has the smallest nanostructure, by only comparing profiles without analysis. The object to be measured is a heterogeneous structure (void, second phase, crack, etc.) having a diameter of about 1 to several hundred nm present in a material. This paper also outlines the usual small-angle scattering analysis method, as well as further analysis using the difference between X-ray and neutron on scattering length contrast. (A.O.)

  1. 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 X....... 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....

  2. Neutron and x-ray small angle scattering of biological molecules

    International Nuclear Information System (INIS)

    Borso, C.S.; Danyluk, S.S.; Williamson, F.S.; Holmblad, G.L.; DeJong, S.; Pohl, J.

    1981-01-01

    The objectives of this project are to develop instrumentation for small angle x-ray and neutron scattering, and to utilize small angle techniques for study of the structures of the intracellular molecules interacting with the secondary messengers involved in cellular regulation. A unique self-scanning photodiode array has been developed as a linear position sensitive detector for studies of biological structures. A time-of-flight (TOF) small angle neutron instrument was developed and successfully tested at the prototype pulsed neutron facility, ZING-P'. Considerable hardware and software developments were necessary to successfully demonstrate the prototype small angle neutron scattering instrument. A dedicated data acquisition system based on a microprocessor was developed and tested within the short period of approximately 6 months and was interfaced to a biological sample changer and environmental controller. The resolution of the tapered collimation system proved to be adequate

  3. Small-angle X-ray scattering study of conditions for the formation of growth units of protein crystals in lysozyme solutions

    Science.gov (United States)

    Dyakova, Yu. A.; Ilina, K. B.; Konarev, P. V.; Kryukova, A. E.; Marchenkova, M. A.; Blagov, A. E.; Volkov, V. V.; Pisarevsky, Yu. V.; Kovalchuk, M. V.

    2017-05-01

    The structural composition of lysozyme solutions favorable for the formation of the tetragonal form of protein crystals was studied by synchrotron-based small-angle X-ray scattering depending on the protein concentration and the temperature. Along with lysozyme monomers, dimers and octamers are found in crystallization solutions; the octamer content increases with an increase in the protein concentration.

  4. 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

  5. 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)

  6. Small angle x-ray and neutron scattering for materials characterisation

    Energy Technology Data Exchange (ETDEWEB)

    Buckley, C.E. [Curtin University of Technology, Perth, WA (Australia). Department of Applied Physics

    1999-12-01

    Full text: Small angle X-ray and neutron scattering (SAXS and SANS) are excellent techniques to characterise inhomogeneities in materials in the size range from 10 Angstroms to several thousand Angstroms. Ultra small angle neutron and X-ray scattering (USANS and USAXS) have extended this size range out to 20 {mu}m. SAXS is due to the electron density difference between the matrix and the inhomogeneity, whereas SANS is due to the scattering length density difference. SANS and SAXS have been used successfully to characterise colloidal particles in solution, colloidal powders, glasses and a wide range of solids such as metals, alloys, and natural and synthetic high polymers. Small angle scattering and complementary techniques, such transmission and scanning electron microscopy (TEM and SEM) are a powerful combination for the investigation of submicron particles. This paper will introduce the reader to the small angle scattering techniques and will use the aluminium hydrogen (Al-H) system as an example to demonstrate the applicability of each method. Aluminium foils (99.99% purity) and single crystals (99.999% purity) were charged with hydrogen using a gas plasma method (voltage range of 1.0 - 1.2 keV). The results from the SANS, USANS, TEM, SEM, X-ray diffraction and inelastic neutron scattering experiments showed a wide range of H{sub 2} bubbles on the surface and in the bulk of the Al-H sample (< 10 Angstroms up to several microns in size). The volume of the H{sub 2} bubbles was formed by the diffusion of H-vacancy complexes into the bulk. The volume concentration of vacant sites determined from precision density measurements was within experimental error to that calculated from the SANS and USANS experiments. Copyright (1999) Australian X-ray Analytical Association Inc. 5 refs.

  7. Small angle x-ray and neutron scattering for materials characterisation

    International Nuclear Information System (INIS)

    Buckley, C.E.

    1999-01-01

    Full text: Small angle X-ray and neutron scattering (SAXS and SANS) are excellent techniques to characterise inhomogeneities in materials in the size range from 10 Angstroms to several thousand Angstroms. Ultra small angle neutron and X-ray scattering (USANS and USAXS) have extended this size range out to 20 μm. SAXS is due to the electron density difference between the matrix and the inhomogeneity, whereas SANS is due to the scattering length density difference. SANS and SAXS have been used successfully to characterise colloidal particles in solution, colloidal powders, glasses and a wide range of solids such as metals, alloys, and natural and synthetic high polymers. Small angle scattering and complementary techniques, such transmission and scanning electron microscopy (TEM and SEM) are a powerful combination for the investigation of submicron particles. This paper will introduce the reader to the small angle scattering techniques and will use the aluminium hydrogen (Al-H) system as an example to demonstrate the applicability of each method. Aluminium foils (99.99% purity) and single crystals (99.999% purity) were charged with hydrogen using a gas plasma method (voltage range of 1.0 - 1.2 keV). The results from the SANS, USANS, TEM, SEM, X-ray diffraction and inelastic neutron scattering experiments showed a wide range of H 2 bubbles on the surface and in the bulk of the Al-H sample ( 2 bubbles was formed by the diffusion of H-vacancy complexes into the bulk. The volume concentration of vacant sites determined from precision density measurements was within experimental error to that calculated from the SANS and USANS experiments. Copyright (1999) Australian X-ray Analytical Association Inc

  8. 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.

  9. Intercalibration of small-angle X-ray and neutron scattering data

    International Nuclear Information System (INIS)

    Russell, T.P.; Lin, J.S.; Spooner, S.; Wignall, G.D.

    1988-01-01

    Absolute calibration forms a valuable diagnostic tool in small-angle scattering experiments and allows the parameters of a given model to be restricted to the set which reproduces the observed intensity. General methods which are available for absolute scaling of small-angle X-ray scattering (SAXS) data are reviewed along with estimates of the degree of internal consistency which may be achieved between the various standards. In order to minimize the time devoted to calibration in a given experimental program, emphasis is placed on developing a set of precalibrated strongly scattering standards for the SAXS facilities of the National Center for Small-Angle Scattering Research (Oak Ridge). Similar standards have been developed previously for calibration of small-angle neutron scattering (SANS) data. Particular attention is given to standards which can be used for either SAXS or SANS experiments where each sample has been independently calibrated for both types of radiation. These calibrations have been tested via the theoretical relationships between the two cross sections. It has been found that specimens best suited for such intercalibration purposes are a glassy carbon specimen where the scattering arises from voids in a carbon matrix and a perdeuterated polyethylene where the scattering arises from periodic arrangement of the crystalline lamellae. In only these two cases could the identical specimen be used for both the neutron and X-ray scattering experiments. (orig.)

  10. 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

  11. Characterization of porous materials using combined small-angle X-ray and neutron scattering techniques

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Naiping; Borkar, Neha; Kohls, Doug; Schaefer, Dale W. (UCIN)

    2014-09-24

    A combination of ultra small angle X-ray scattering (USAXS) and ultra small angle neutron scattering (USANS) is used to characterize porous materials. The analysis methods yield quantitative information, including the mean skeletal chord length, mean pore chord length, skeletal density, and composition. A mixed cellulose ester (MCE) membrane with a manufacturer-labeled pore size of 0.1 {mu}m was used as a model to elucidate the specifics of the method. Four approaches describing four specific scenarios (different known parameters and form of the scattering data) are compared. Pore chords determined using all four approaches are in good agreement with the scanning electron microscopy estimates but are larger than the manufacturer's nominal pore size. Our approach also gives the average chord of the skeletal solid (struts) of the membrane, which is also consistent for all four approaches. Combined data from USAXS and USANS gives the skeletal density and the strut composition.

  12. Characterization of porous materials using combined small-angle X-ray and neutron scattering techniques

    International Nuclear Information System (INIS)

    Hu, Naiping; Borkar, Neha; Kohls, Doug; Schaefer, Dale W.

    2012-01-01

    A combination of ultra small angle X-ray scattering (USAXS) and ultra small angle neutron scattering (USANS) is used to characterize porous materials. The analysis methods yield quantitative information, including the mean skeletal chord length, mean pore chord length, skeletal density, and composition. A mixed cellulose ester (MCE) membrane with a manufacturer-labeled pore size of 0.1 μm was used as a model to elucidate the specifics of the method. Four approaches describing four specific scenarios (different known parameters and form of the scattering data) are compared. Pore chords determined using all four approaches are in good agreement with the scanning electron microscopy estimates but are larger than the manufacturer's nominal pore size. Our approach also gives the average chord of the skeletal solid (struts) of the membrane, which is also consistent for all four approaches. Combined data from USAXS and USANS gives the skeletal density and the strut composition.

  13. Characterization of Pt/C catalyst by small angle X-ray scattering

    International Nuclear Information System (INIS)

    Xia Qingzhong; Fan Zhijian; Chen Bo

    2007-12-01

    Pt/C catalyst plays an important role in hydrogen-water isotopic exchange reaction. Small Angle X-ray scattering (SAXS) is applied to investigate the structure of three kinds of Pt nanoparticles which were produced by three processes, Glycol synthesis, Soakage-reducing and Microwave heating. The SAXS analysis of size, shape, surface and the aggregates of primary Pt particles is reported here. Additionally, Transmission Electron Microscope (TEM) measurements also carried out, the results of TEM are in agreement with SAXS conclusions. It is shown that three processes produced different sizes and surface area of Pt aggregations. (authors)

  14. Small angle X-ray and neutron scattering on cadmium sulfide nanoparticles in silicate glass

    Science.gov (United States)

    Kuznetsova, Yu. V.; Rempel, A. A.; Meyer, M.; Pipich, V.; Gerth, S.; Magerl, A.

    2016-08-01

    Small angle X-ray and neutron scattering on Cd and S doped glass annealed at 600 °C shows after the first 12 h nucleation and growth of spherical CdS nanoparticles with a radius of up to 34±4 Å. After the nucleation is completed after 24 h, further growth in this amorphous environment is governed by oriented particle attachment mechanism as found for a liquid medium. Towards 48 h the particle shape has changed into spheroidal with short and long axis of 40±2 Å and 120±2 Å, respectively.

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

    DEFF Research Database (Denmark)

    Stovgaard, Kasper; Andreetta, Christian; Ferkinghoff-Borg, Jesper

    2010-01-01

    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...

  16. 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.

  17. Synchrotron X-ray magnetic scattering

    CERN Document Server

    Stirling, W G

    2003-01-01

    Research on magnetic materials constitutes an increasingly important part of the programmes of most major synchrotron radiation centres. The extremely high brilliance and small spot size of advanced synchrotron beamlines, combined with element-specific resonant effects at certain absorption edges, provide a powerful probe of magnetic structures and phase transitions, with excellent wavevector resolution. Over the last decade a variety of experimental techniques have been developed, exploiting these effects for the study of thin film, multilayer and bulk magnetic materials. In this paper the basic concepts of X-ray magnetic scattering will be introduced, followed by recent examples taken from work at Daresbury Laboratory (UK), the European Synchrotron Radiation Facility (Grenoble, France) and the National Synchrotron Light Source (Brookhaven National Laboratory, USA). Investigations of domain patterns in thin magnetic films employing X-ray resonant magnetic scattering (XRMS) will be described, followed by a se...

  18. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    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/sup 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/sup 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.

  20. Light-Induced Structural Flexibility of Thylakoid Membranes - Investigated using Small-Angle X-ray and Neutron Scattering

    OpenAIRE

    Aagaard, Thomas Helverskov

    2005-01-01

    Using small-angle x-ray and neutron scattering the light-induced structural changes in pea thylakoids have been investigated. It is shown that light-induced shinkage in the thylakoids is connected to photosynthetic electron transduction. Using small-angle x-ray and neutron scattering the light-induced structural changes in pea thylakoids have been investigated. It is shown that light-induced shinkage in the thylakoids is connected to photosynthetic electron transduction.

  1. Ultra-small angle neutron scattering and X-ray tomography studies of caseinate-hydroxyapatite microporous materials

    Energy Technology Data Exchange (ETDEWEB)

    Ritzoulis, C., E-mail: critzou@food.teithe.gr [ATEI of Thessaloniki, PO Box 141, 57400 Thessaloniki (Greece); Strobl, M. [Ruprecht-Karls-University Heidelberg, Physikalisch-Chemisches Institut, Im Neuenheimer Feld 229, 69120 Heidelberg (Germany); Helmholtz Centre Berlin for Materials and Energy (former Hahn-Meitner Institute), SF1, Glienicker Str. 100, 14109 Berlin (Germany); Panayiotou, C. [Aristotle University of Thessaloniki, University Campus (Greece); Choinka, G. [Helmholtz Centre Berlin for Materials and Energy (former Hahn-Meitner Institute), SF1, Glienicker Str. 100, 14109 Berlin (Germany); Tsioptsias, C. [Aristotle University of Thessaloniki, University Campus (Greece); Vasiliadou, C. [KEPAMAH, 22nd April 1, 63100 Polygyros, Chalkidiki (Greece); Vasilakos, V. [University of Crete, Department of Biology, 71409 Heraklion, Crete (Greece); Beckmann, F.; Herzen, J.; Donath, T. [Institute for Materials Research, GKSS-Research Center, 21502 Geesthacht (Germany)

    2010-09-01

    Microporous hydroxyapatite-protein composite materials of bimodal pore size distribution, intended for utilization as bone regeneration scaffolds, have been prepared by means of milk caseinate emulsion droplet templating. Ultra-small angle neutron scattering (USANS) has been utilized in order to obtain information on the size distribution of the smaller pores (less than tens of micrometers), as compared to the emulsions that have been initially used as templates. The samples were subsequently visualized in 3 dimensions using synchrotron radiation X-ray tomography, where information concerning the larger pores has been obtained. The examination of the samples confirmed a strong correlation between the size of the templating droplets and the produced pores. In addition, 1 {mu}m-sized pores appear to adhere to the surface of 20-70 {mu}m pores, providing an irregular surface on the large pore walls, a desirable feature in bone-mimicking materials.

  2. Small-angle X-ray scattering on extracellular oxygen binding proteins and on one phosphorylase

    International Nuclear Information System (INIS)

    Krebs, A.

    1996-02-01

    The extracellular hemoglobins (Hbs) and Chlorocruorins (Chls) of annelids are giant multisubunit proteins of up to ∼ 200 polypeptide chains with molecular masses of about 3.500 kDa. They differ from all other Hbs in having both O 2 -binding chains and 'linker' chains. The latter are required for assembly and structural integrity of the proteins and are deficient in or lack heme. In this work the influence of O 2 binding on the overall structure of Lumbricus terrestris hemoglobin, Eudistylia vancouverii Chlorocruorin and Lumbricus terrestris hemoglobin dodecamer (assembly of 12 polypeptide chains) was investigated using the method of small-angle X-ray scattering. No dramatic effects were observed, although a tendency to smaller values of the radius of gyration, maximal intraparticle distance and volume upon deoxygenation of the samples was observed. Models of the three dimensional structures of the above mentioned proteins and of Macrobdella decora hemoglobin are proposed. Furthermore a detailed model of Lumbricus terrestris hemoglobin is proposed, wherein 12 models of the dodecamer subunit and additional linker chains build up the whole model, thus supporting the 'bracelet-model'. Small-angle X-ray scattering experiments of the α-glucan phosphorylase of Corynebacterium callunae led to a model of its quartenary structure with an axial ratio of about 1:0.95:0.41. (author)

  3. A gradient method for anomalous small-angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Jemian, P.R. [Argonne National Lab., IL (United States); Weertman, J.R. [Northwestern Univ., Evanston, IL (United States). Dept. of Materials Science and Engineering; Long, G.G. [National Institute of Standards and Technology, Gaithersburg, MD (United States). Ceramics Div.

    1992-09-15

    A new method of general applicability for analyzing data from anomalous dispersion small-angle X-ray scattering (ASAXS) measurements is described. ASAXS is used as a contrast variation method to label the scattering from a single element in a complex material containing several types of scatterers. The contrast variation is achieved through the anomalous dispersion of X-rays. Thus only one sample is required for a complete analysis. To label a scatterer by ASAXS, the atomic scattering factor of an element in the sample is varied by the selection of photon energies near the absorption edge of the element. Careful selection of the photon energies allows the contrast of only the labeled scatterer to change. Data from several small-angle scattering measurements, each conducted at a fixed energy, are combined in a single analysis. The gradient method, used as an extension to a standard SAXS data analysis method, is demonstrated by isolating the volume fraction size distribution of Cr{sub 23}C{sub 6} in 9Cr-1 MoVNb steel.

  4. In situ small angle x-ray studies of coal gasification

    Energy Technology Data Exchange (ETDEWEB)

    Jensen, K F

    1983-01-01

    This report summarizes the progress made the first 12 months of a planned 36 month project on small angle x-ray studies of coal and char pore structure. Model carbon studies have been employed to demonstrate the usefulness of small angle x-ray scattering (SAXS) in monitoring the structural changes in porous carbonaceous materials during gasification. Scattering data from particles gasified to varying levels of conversion show increases in the micropore sizes with conversion. This is also supported by surface area measurements by SAXS showing a maximum at intermediate conversion in agreements with previous studies by conventional means. The application of SAXS to PSOC coal samples is also demonstrated. Existing models for the porous structure have been reviewed and percolation theory has been selected as a consistent framework for both the modelling and the data analysis. This theory will make it possible to describe the porous structure in terms of its geometry and connectivity, rather than being limited to a fixed geometry as in conventional approaches. Two graduate students and the PI have been trained in SAXS and the associated theory. Results from the model carbon studies have been published. 18 references, 9 figures, 2 tables.

  5. 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.

  6. 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.

  7. Composite material characterisation using an advanced small angle x-ray (SAXS) technique

    Science.gov (United States)

    Yazid, Hafizal; Murshidi, Julie A.; Jamro, Rafhayudi; Megat Harun, M. A.; Aziz Mohamed, Abdul

    2018-01-01

    Materials development in the field of composite material spurs the use of advanced characterization technique. As the fillers become in the nanoscale range in size, the effect of agglomeration become apparent and cannot be avoided. The use of Small Angle X-Ray (SAXS) Scattering technique revealed the information on agglomeration based on the value of specific surface (m2/g). Thermoplastic natural rubber composite was found isotropic based on 2D saxs scattering pattern. As the amount of fillers increased from 2-10% wt., the value of specific surface dropped accordingly. This indicated the higher the amount of filler used, the higher the degree of agglomeration. The SAXS system was also tested by Alumina (BAM) powder and yield result which was in good agreement with BET technique.

  8. Collimation effects in small-angle X-ray and neutron scattering

    International Nuclear Information System (INIS)

    Schmidt, P.W.

    1988-01-01

    To obtain adequate intensity in small-angle X-ray and neutron scattering measurements, the apertures that define the incident and scattered beams often must be made so large that the measured intensity is an average over an appreciable interval of scattering angles. Allowance must frequently be made for the resulting distortion of the measured scattering curve. A technique previously developed by Hendricks and Schmidt for describing collimation effects is outlined. This method makes use of a function called the ''weighting function'', which specifies the width of the interval over which the intensity is averaged and indicates the emphasis given to scattering angles within this interval. A new calculation of the weighting function for pinhole collimating systems, which employ circularly symmetric apertures instead of long narrow slits, is presented. Several techniques for performing collimation corrections are described, and a review is given of results that several workers have recently obtained in studies of collimation effects in pinhole systems. (orig.)

  9. 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...... of the dosimeter. When omitting gelatin, ellipsoidal micelles of SDS were formed with a core radius near 15 Å, an eccentricity of 1.6, and a head-group shell thickness near 7 Å. Gelatin significantly changed the micelles to a cylindrical shape with around three times lower core radius and four times larger shell...... thickness, which shows that the gelatin is present in the shell and the outer part of the core. Insight into the detailed structure might help to improve the dosimeter performance and increase the dose response to clinically relevant dose levels....

  10. Nucleation and growth of gold nanoparticles studied via in situ small angle X-ray scattering at millisecond time resolution.

    Science.gov (United States)

    Polte, Jörg; Erler, Robert; Thünemann, Andreas F; Sokolov, Sergey; Ahner, T Torsten; Rademann, Klaus; Emmerling, Franziska; Kraehnert, Ralph

    2010-02-23

    Gold nanoparticles (AuNP) were prepared by the homogeneous mixing of continuous flows of an aqueous tetrachloroauric acid solution and a sodium borohydride solution applying a microstructured static mixer. The online characterization and screening of this fast process ( approximately 2 s) was enabled by coupling a micromixer operating in continuous-flow mode with a conventional in-house small angle X-ray scattering (SAXS) setup. This online characterization technique enables the time-resolved investigation of the growth process of the nanoparticles from an average radius of ca. 0.8 nm to about 2 nm. To the best of our knowledge, this is the first demonstration of a continuous-flow SAXS setup for time-resolved studies of nanoparticle formation mechanisms that does not require the use of synchrotron facilities. In combination with X-ray absorption near edge structure microscopy, scanning electron microscopy, and UV-vis spectroscopy the obtained data allow the deduction of a two-step mechanism of gold nanoparticle formation. The first step is a rapid conversion of the ionic gold precursor into metallic gold nuclei, followed by particle growth via coalescence of smaller entities. Consequently it could be shown that the studied synthesis serves as a model system for growth driven only by coalescence processes.

  11. 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.

  12. 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.

  13. Quantifying radiation damage in biomolecular small-angle X-ray scattering.

    Science.gov (United States)

    Hopkins, Jesse B; Thorne, Robert E

    2016-06-01

    Small-angle X-ray scattering (SAXS) is an increasingly popular technique that provides low-resolution structural information about biological macromolecules in solution. Many of the practical limitations of the technique, such as minimum required sample volume, and of experimental design, such as sample flow cells, are necessary because the biological samples are sensitive to damage from the X-rays. Radiation damage typically manifests as aggregation of the sample, which makes the collected data unreliable. However, there has been little systematic investigation of the most effective methods to reduce damage rates, and results from previous damage studies are not easily compared with results from other beamlines. Here a methodology is provided for quantifying radiation damage in SAXS to provide consistent results between different experiments, experimenters and beamlines. These methods are demonstrated on radiation damage data collected from lysozyme, glucose isomerase and xylanase, and it is found that no single metric is sufficient to describe radiation damage in SAXS for all samples. The radius of gyration, molecular weight and integrated SAXS profile intensity constitute a minimal set of parameters that capture all types of observed behavior. Radiation sensitivities derived from these parameters show a large protein dependence, varying by up to six orders of magnitude between the different proteins tested. This work should enable consistent reporting of radiation damage effects, allowing more systematic studies of the most effective minimization strategies.

  14. 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.

  15. 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.

  16. Techniques for materials research with synchrotron radiation x-rays

    International Nuclear Information System (INIS)

    Bowen, D.K.

    1983-01-01

    A brief introductory survey is presented of the properties and generation of synchrotron radiation and the main techniques developed so far for its application to materials problems. Headings are:synchrotron radiation; X-ray techniques in synchrotron radiation (powder diffraction; X-ray scattering; EXAFS (Extended X-ray Absorption Fine Structure); X-ray fluorescent analysis; microradiography; white radiation topography; double crystal topography); future developments. (U.K.)

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

    Science.gov (United States)

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

    2012-04-01

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

  18. Analysis of heterogeneity of polymer systems from the data of small angle X-ray and neutron scattering

    International Nuclear Information System (INIS)

    Agamalyan, M.M.

    1989-01-01

    The possibility of determination of the chemical composition of supermolecular formations in blocks of polymer systems by comparison of squares of relative contrasts measured experimentally using small-angle X-ray and neutron scattering with theoretically calculated ones is discussed. The efficiency of this technique is related with large difference in the scattering capacity of density heterogeneities of hydrogen-containing media towards X-ray and neutrons. The technique is illustrated with some examples

  19. 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...... cycle can be performed in less than 3 min. Bovine serum albumin was used as a model protein to characterize the mixing efficiency and sample consumption of the system. The N2 fragment of an adaptor protein (p120-RasGAP) was used to demonstrate how the device can be used to survey the structural space...

  20. Synchrotron radiation X-ray microfluorescence techniques

    Indian Academy of Sciences (India)

    Synchrotron X-ray imaging systems with fluorescence techniques was developed for biomedical researches in Brazilian Synchrotron Laboratory. An X-ray fluorescence microtomography system was implemented to analyse human prostate and breast samples and an X-ray microfluorescence system was implemented to ...

  1. Synchrotron radiation X-ray microfluorescence techniques and ...

    Indian Academy of Sciences (India)

    Synchrotron X-ray imaging systems with fluorescence techniques was developed for biomedical researches in Brazilian Synchrotron Laboratory. An X-ray fluorescence microtomography system was implemented to analyse human prostate and breast samples and an X-ray microfluorescence system was implemented to ...

  2. 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

  3. 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.

  4. Nano-scale morphology of melanosomes revealed by small-angle X-ray scattering.

    Directory of Open Access Journals (Sweden)

    Thomas Gorniak

    Full Text Available Melanosomes are highly specialized organelles that produce and store the pigment melanin, thereby fulfilling essential functions within their host organism. Besides having obvious cosmetic consequences--determining the color of skin, hair and the iris--they contribute to photochemical protection from ultraviolet radiation, as well as to vision (by defining how much light enters the eye. Though melanosomes can be beneficial for health, abnormalities in their structure can lead to adverse effects. Knowledge of their ultrastructure will be crucial to gaining insight into the mechanisms that ultimately lead to melanosome-related diseases. However, due to their small size and electron-dense content, physiologically intact melanosomes are recalcitrant to study by common imaging techniques such as light and transmission electron microscopy. In contrast, X-ray-based methodologies offer both high spatial resolution and powerful penetrating capabilities, and thus are well suited to study the ultrastructure of electron-dense organelles in their natural, hydrated form. Here, we report on the application of small-angle X-ray scattering--a method effective in determining the three-dimensional structures of biomolecules--to whole, hydrated murine melanosomes. The use of complementary information from the scattering signal of a large ensemble of suspended organelles and from single, vitrified specimens revealed a melanosomal sub-structure whose surface and bulk properties differ in two commonly used inbred strains of laboratory mice. Whereas melanosomes in C57BL/6J mice have a well-defined surface and are densely packed with 40-nm units, their counterparts in DBA/2J mice feature a rough surface, are more granular and consist of 60-nm building blocks. The fact that these strains have different coat colors and distinct susceptibilities to pigment-related eye disease suggest that these differences in size and packing are of biological significance.

  5. A triple axis double crystal multiple reflection camera for ultra small angle X-ray scattering

    Science.gov (United States)

    Lambard, Jacques; Lesieur, Pierre; Zemb, Thomas

    1992-06-01

    To extend the domain of small angle X-ray scattering requires multiple reflection crystals to collimate the beam. A double crystal, triple axis X-ray camera using multiple reflection channel cut crystals is described. Procedures for measuring the desmeared scattering cross-section on absolute scale are described as well as the measurement from several typical samples : fibrils of collagen, 0.3 μm diameter silica spheres, 0.16 μm diameter interacting latex spheres, porous lignite coal, liquid crystals in a surfactant-water system, colloidal crystal of 0.32 μm diameter silica spheres. L'extension du domaine de diffusion des rayons-X vers les petits angles demande l'emploi de cristaux à réflexions multiples pour collimater le faisceau. Nous décrivons une caméra à rayons-X à trois axes où les réflexions multiples sont réalisées dans deux cristaux à gorge. Nous donnons ensuite les procédures de déconvolution pour obtenir la section efficace de diffusion en échelle absolue, ainsi que les résultats des mesures effectuées avec plusieurs échantillons typiques : fibres de collagène, sphères de silice de 0,3 μm de diamètre, sphères de latex de 0,16 μm de diamètre en interaction, charbon lignite poreux, cristaux liquides formés dans un système eau-tensioactif, solution colloïdale de sphères de silice de 0,32 μm de diamètre.

  6. Recent improvements in small angle x-ray diffraction for the study of muscle physiology

    Science.gov (United States)

    Reconditi, Massimo

    2006-10-01

    The molecular mechanism of muscle contraction is one of the most important unresolved problems in biology and biophysics. Notwithstanding the great advances of recent years, it is not yet known in detail how the molecular motor in muscle, the class II myosin, converts the free energy of ATP hydrolysis into work by interacting with its track, the actin filament; neither is it understood how the high efficiency in energy conversion depends on the cooperative action of myosin motors working in parallel along the actin filament. Research in muscle contraction involves the combination of mechanical, biochemical and structural methods in studies that span from tissue to single molecule. Therefore, more than for any other research field, progress in the comprehension of muscle contraction at the molecular level is related to, and in turn contributes to, the advancement of methods in biophysics. This review will focus on the progress achieved by time-resolved small angle x-ray scattering (SAXS) from muscle, an approach made possible by the highly ordered arrangement of both the contractile proteins myosin and actin in the ca 2 µm long structural unit, the sarcomere, that repeats along the whole length of the muscle cell. Among time-resolved structural techniques, SAXS has proved to be the most powerful method of investigation, as it allows the molecular motor to be studied in situ, in intact single muscle cells, where it is possible to combine the structural study with fast mechanical methods that synchronize the action of the molecular motors. The latest development of this technique allows Angstrom-scale measurements of the axial movement of the motors that pull the actin filament towards the centre of the sarcomere, by exploiting the x-ray interference between the two arrays of myosin motors in the two halves of the sarcomere.

  7. Small angle X-ray studies of protein-polymer interactions

    International Nuclear Information System (INIS)

    Torriani, Iris; Oliveira, Cristiano L.P. de; Almeida, Nara L.; Loh, Watson

    2003-01-01

    Full text: The interaction between biological macromolecules and non-adsorbing polymers is considered of utmost importance in the study of protein crystallization processes and in the study of a large number of protein-polymer systems or artificial surfaces used in medical procedures, in which polymeric materials are in contact with blood proteins. The structural information furnished by small angle X-ray scattering (SAXS) experiments can be used to describe protein-polymer interaction in solution mixtures considering the dispersion as a two-component system. In this work, two proteins, lysozyme and bovine serum albumin (BSA), were studied in the presence of Poly(ethylene oxide) (PEO), various EO/PO copolymers of varied composition and Poly(ethylene glycol) (PEG). Thermal stability of both lysozyme and BSA was studied in the presence of these polymers. X-ray scattering experiments were performed at the SAXS beamline of the Laboratorio Nacional de Luz Sincrotron, Campinas, SP, using the facility available for liquid dispersions under controlled temperature. Room temperature measurements were aimed at detecting possible polymer-protein interactions. Thermal denaturation processes were studied in some of these systems in order to check the stabilizing effect of some of the polymers used, at fixed temperatures of 25, 50, 60 and 70 deg C. At 80 deg C, using a real time data acquisition system, structural changes could be followed as a function of time in a sequence of frames that show denaturation and aggregation of the proteins. Real space analysis of the intensity functions was performed using a mathematical expression derived for the form factor of a system of particles of different shapes. The pair distance distribution functions of each component of the system could be calculated separately. The possibility of complex formation in the case of the proteins studied is not supported by our results. The presence of polymers may affect the protein-protein interaction

  8. Recent improvements in small angle x-ray diffraction for the study of muscle physiology

    Energy Technology Data Exchange (ETDEWEB)

    Reconditi, Massimo [Universita di Firenze, Lab di Fisiologia - DBAG, c/o Dip. di Fisica, via Sansone 1, I-50019 Sesto Fiorentino (Italy)

    2006-10-15

    The molecular mechanism of muscle contraction is one of the most important unresolved problems in biology and biophysics. Notwithstanding the great advances of recent years, it is not yet known in detail how the molecular motor in muscle, the class II myosin, converts the free energy of ATP hydrolysis into work by interacting with its track, the actin filament; neither is it understood how the high efficiency in energy conversion depends on the cooperative action of myosin motors working in parallel along the actin filament. Research in muscle contraction involves the combination of mechanical, biochemical and structural methods in studies that span from tissue to single molecule. Therefore, more than for any other research field, progress in the comprehension of muscle contraction at the molecular level is related to, and in turn contributes to, the advancement of methods in biophysics. This review will focus on the progress achieved by time-resolved small angle x-ray scattering (SAXS) from muscle, an approach made possible by the highly ordered arrangement of both the contractile proteins myosin and actin in the ca 2 {mu}m long structural unit, the sarcomere, that repeats along the whole length of the muscle cell. Among time-resolved structural techniques, SAXS has proved to be the most powerful method of investigation, as it allows the molecular motor to be studied in situ, in intact single muscle cells, where it is possible to combine the structural study with fast mechanical methods that synchronize the action of the molecular motors. The latest development of this technique allows Angstrom-scale measurements of the axial movement of the motors that pull the actin filament towards the centre of the sarcomere, by exploiting the x-ray interference between the two arrays of myosin motors in the two halves of the sarcomere.

  9. 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

  10. 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.

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

    Science.gov (United States)

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

    2012-11-01

    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.

  12. Structural variations in lignite coal: a small angle X-ray scattering investigation

    Science.gov (United States)

    Sastry, P. U.; Sen, D.; Mazumder, S.; Chandrasekaran, K. S.

    2000-04-01

    The structural morphology of raw and processed lignite coal specimens from Neyveli (Tamil Nadu, India) is characterized over a length scale of 5-100 nm by small angle X-ray scattering (SAXS). The scattering profile from the unprocessed lignite specimen exhibits two distinct power laws indicating different fractal morphologies over different length scales: a pore fractal (dimension Dp˜2.7) for the pore-coal interface below 17 nm and a surface fractal (dimension Ds˜2.3) above 17 nm. As a result of industrial processing at different temperature, pressure and carbonization, significant changes in the structure are noticed as indicated by the scattering profiles. The fractal roughness of the pore-coal interface becomes smooth (average Ds˜2) for a large window of the length scale, whereas a part of the pore fractal transforms to a surface ( Ds˜2.8). The specimen treated at relatively higher temperature exhibits further variation from the fractal geometry with a tendency to form a new non-fractal micropore structure for the length scale ≤8 nm.

  13. 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.

  14. Lysozyme crystal growth, as observed by small angle X-ray scattering, proceeds without crystallization intermediates

    International Nuclear Information System (INIS)

    Finet, S.; Bonnete, F.; Frouin, J.; Provost, K.; Tardieu, A.

    1998-01-01

    A combination of small angle X-ray scattering and gel techniques was used to follow the kinetics of protein crystal growth as a function of time. Hen egg white lysozyme, at different protein concentrations, was used as a model system. A new sample holder was designed, in which supersaturation is induced in the presence of salt by decreasing the temperature. It had been shown previously that a decrease in temperature and/or an increase in crystallizing agent induces an increase in the attractive interactions present in the lysozyme solutions, the lysozyme remaining monomeric. In the present paper we show that similar behaviour is observed in NaCl when agarose gels are used. During crystal growth, special attention was paid to determine whether oligomers were formed as the protein in solution was incorporated in the newly formed crystals. From these first series of experiments, we did not find any indication of oligomer formation between monomer in solution and crystal. The results obtained are in agreement with the hypothesis that lysozyme crystals in NaCl grow by addition of monomeric particles. (orig.)

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

    Science.gov (United States)

    Eicher, Barbara; Heberle, Frederick A; Marquardt, Drew; Rechberger, Gerald N; Katsaras, John; Pabst, Georg

    2017-04-01

    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 palmitoyl-oleoyl phosphatidyl-choline (POPC) vesicles, compared to the inner leaflet. 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.

  16. Characterization of Physically and Chemically Separated Athabasca Asphaltenes Using Small-Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Amundaraín Hurtado, Jesús Leonardo; Chodakowski, Martin; Long, Bingwen; Shaw, John M. (Alberta)

    2012-02-07

    Athabasca asphaltenes were characterized using small-angle X-ray scattering (SAXS). Two methods were used to separate asphaltenes from the Athabasca bitumen: namely, chemical separation by precipitation with n-pentane and physical separation by nanofiltration using a zirconia membrane with a 20 nm average pore size. The permeate and chemically separated samples were diluted in 1-methylnaphtalene and n-dodecane prior to SAXS measurements. The temperature and asphaltene concentration ranges were 50-310 C and 1-10.4 wt %, respectively. Model-independent analysis of SAXS data provided the radius of gyration and the scattering coefficients. Model-dependent fits provided size distributions for asphaltenes assuming that they are dense and spherical. Model-independent analysis for physically and chemically separated asphaltenes showed significant differences in nominal size and structure, and the temperature dependence of structural properties. The results challenge the merits of using chemically separated asphaltene properties as a basis for asphaltene property prediction in hydrocarbon resources. While the residuals for model-dependent fits are small, the results are inconsistent with the structural parameters obtained from model-independent analysis.

  17. 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.

  18. 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)

  19. 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

  20. Small-angle X-ray scattering: a high-throughput technique for investigating archaeological bone preservation

    NARCIS (Netherlands)

    Hiller, J.C.; Collins, M.J.; Chamberlain, A.T.; Wess, T.J.

    2004-01-01

    Diagenetic alteration to archaeological bone can cause significant disruption to both the biogenic mineral structure and the preservation of biomolecular resources such as protein and DNA over archaeological time. We report here the use of a technique, small-angle X-ray scattering, which makes it

  1. 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 st...

  2. Small-Angle X-ray Scattering Data in Combination with RosettaDock Improves the Docking Energy Landscape

    DEFF Research Database (Denmark)

    Sønderby, Pernille; Rinnan, Åsmund; Madsen, Jesper J.

    2017-01-01

    We have performed a benchmark to evaluate the relative success of using small-angle X-ray scattering (SAXS) data as constraints (hereafter termed SAXSconstrain) in the RosettaDock protocol (hereafter termed RosettaDockSAXS). For this purpose, we have chosen 38 protein complex structures, calculat...

  3. Self-assembly of designed coiled coil peptides studied by small-angle X-ray scattering and analytical ultracentrifugation

    DEFF Research Database (Denmark)

    Malik, Leila; Nygaard, Jesper; Christensen, Niels Johan

    2013-01-01

    , they are promising tools for the construction of nanomaterials. Small-angle X-ray scattering (SAXS) has emerged as a new biophysical technique for elucidation of protein topology. Here, we describe a systematic study of the self-assembly of a small ensemble of coiled coil sequences using SAXS and analytical...

  4. 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...

  5. 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.

  6. 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

  7. 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.)

  8. 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.

  9. Synchrotron x-ray microbeam characteristics for x-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Iida, Atsuo; Noma, Takashi

    1995-01-01

    X-ray fluorescence analysis using a synchrotron x-ray microprobe has become an indispensable technique for non-destructive micro-analysis. One of the most important parameters that characterize the x-ray microbeam system for x-ray fluorescence analysis is the beam size. For practical analysis, however, the photon flux, the energy resolution and the available energy range are also crucial. Three types of x-ray microbeam systems, including monochromatic and continuum excitation systems, were compared with reference to the sensitivity, the minimum detection limit and the applicability to various types of x-ray spectroscopic analysis. 16 refs., 5 figs

  10. 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.

  11. 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.

  12. Detection of short range order in SiO{sub 2} thin-films by grazing-incidence wide and small-angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Nagata, Kohki, E-mail: nagata.koki@iri-tokyo.jp [Tokyo Metropolitan Industrial Technology Research Institute, 2-4-10 Aomi, Koto-ku, Tokyo 135-0064 (Japan); School of Science and Technology, Meiji University, 1-1-1 Higashimita, Tama-ku, Kawasaki, Kanagawa 214-8571 (Japan); Ogura, Atsushi [School of Science and Technology, Meiji University, 1-1-1 Higashimita, Tama-ku, Kawasaki, Kanagawa 214-8571 (Japan); Hirosawa, Ichiro [Japan Synchrotron Radiation Research Institute (JASRI), 1-1-1, Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198 (Japan); Suwa, Tomoyuki; Teramoto, Akinobu; Ohmi, Tadahiro [New Industry Creation Hatchery Center, Tohoku University, 6-6-10 Aramakiazaaoba, Aoba-ku, Sendai, Miyagi 980-8579 (Japan)

    2016-04-21

    The effects of the fabrication process conditions on the microstructure of silicon dioxide thin films of <10 nm thickness are presented. The microstructure was investigated using grazing-incidence wide and small-angle X-ray scattering methods with synchrotron radiation. The combination of a high brilliance light source and grazing incident configuration enabled the observation of very weak diffuse X-ray scattering from SiO{sub 2} thin films. The results revealed different microstructures, which were dependent on oxidizing species or temperature. The micro-level properties differed from bulk properties reported in the previous literature. It was indicated that these differences originate from inner stress. The detailed structure in an amorphous thin film was not revealed owing to detection difficulties.

  13. Gas gain operations with single photon resolution using an integrating ionization chamber in small-angle X-ray scattering experiments

    CERN Document Server

    Menk, R H; Besch, H J; Walenta, Albert H; Amenitsch, H; Bernstorff, S

    2000-01-01

    In this work a combination of an ionization chamber with one-dimensional spatial resolution and a MicroCAT structure will be presented. Initially, MicroCAT was thought of as a shielding grid (Frisch-grid) but later was used as an active electron amplification device that enables single X-ray photon resolution measurements at low fluxes even with integrating readout electronics. Moreover, the adjustable gas gain that continuously covers the entire range from pure ionization chamber mode up to high gas gains (30000 and more) provides stable operation yielding a huge dynamic range of about 10 sup 8 and more. First measurements on biological samples using small angle X-ray scattering techniques with synchrotron radiation will be presented.

  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. 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

  16. Analysis of mesoporous thin films by X-ray reflectivity, optical reflectivity and grazing incidence small angle X-ray scattering

    International Nuclear Information System (INIS)

    Gibaud, A.; Dourdain, S.; Vignaud, G.

    2006-01-01

    It is well-established that X-ray reflectivity (XR) is an invaluable tool to investigate the structure of thin films. Indeed, this technique provides under correct analysis, the electron density profile of thin films in the direction perpendicular to the substrate. For thin films that exhibit lateral ordering at the nanometer scale, grazing incidence small angle X-ray scattering (GISAXS) ideally complements the XR technique to measure the scattering in off-specular directions. As typical examples, XR and GISAXS data of mesoporous silica thin films and porous materials are presented. The analysis of the XR curve allows to determine the porosity of the film. We also show that the combination of X-ray and visible optical reflection provides information about the index of refraction of thin films. Finally we report how capillary condensation of water can be monitored by XR and GISAXS

  17. 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)

  18. 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.

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

    Science.gov (United States)

    Jääskeläinen, Pentti; Engelhardt, Peter; Hynönen, Ulla; Torkkeli, Mika; Palva, Airi; Serimaa, Ritva

    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 Å and 435 Å.

  20. Optoelectronic Picosecond Detection of Synchrotron X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Durbin, Stephen M. [Purdue Univ., West Lafayette, IN (United States)

    2017-08-04

    The goal of this research program was to develop a detector that would measure x-ray time profiles with picosecond resolution. This was specifically aimed for use at x-ray synchrotrons, where x-ray pulse profiles have Gaussian time spreads of 50-100 ps (FWHM), so the successful development of such a detector with picosecond resolution would permit x-ray synchrotron studies to break through the pulse width barrier. That is, synchrotron time-resolved studies are currently limited to pump-probe studies that cannot reveal dynamics faster than ~50 ps, whereas the proposed detector would push this into the physically important 1 ps domain. The results of this research effort, described in detail below, are twofold: 1) the original plan to rely on converting electronic signals from a semiconductor sensor into an optical signal proved to be insufficient for generating signals with the necessary time resolution and sensitivity to be widely applicable; and 2) an all-optical method was discovered whereby the x-rays are directly absorbed in an optoelectronic material, lithium tantalate, which can then be probed by laser pulses with the desired picosecond sensitivity for detection of synchrotron x-rays. This research program has also produced new fundamental understanding of the interaction of x-rays and optical lasers in materials that has now created a viable path for true picosecond detection of synchrotron x-rays.

  1. Bacteriophage T7 structure according to the data of small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Rol'bin, Yu.A.; Svergun, D.I.; Fejgin, L.A.; Gashpar, Sh.; Ronto, D.

    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

  2. Magnetic X-Ray Scattering with Synchrotron Radiation

    DEFF Research Database (Denmark)

    Moncton, D. E.; Gibbs, D.; Bohr, Jakob

    1986-01-01

    With the availability of high-brilliance synchrotron radiation from multiple wigglers, magnetic X-ray scattering has become a powerful new probe of magnetic structure and phase transitions. Similar to the well-established magnetic neutron scattering technique, magnetic X-ray scattering methods have...

  3. Study on microstructures of advanced metallic materials by small-angle X-ray and neutron scattering

    International Nuclear Information System (INIS)

    Ohnuma, Masato; Suzuki, Jun-ichi

    2006-01-01

    The microstructure of metal-nonmetal nano-granular soft magnetic films, precipitation hardened stainless steel and Al-Mg-Si alloys, have been studied by small-angle X-ray/neutron scattering (SAXS/SANS). Quantitative evaluation of average scale of their microstructures in nanometer scale has been accomplished by SAXS and SANS. Using this information, the contribution of the microstructures in nanometer scale has been accomplished by SAXS and SANS. Using this information, the contribution of the microstructures to the magnetic and mechanical properties are discussed in this paper. (author)

  4. Anomalous grazing incidence small-angle x-ray scattering studies of Pt nanoparticles formed by cluster deposition

    International Nuclear Information System (INIS)

    Lee, B.; Seifert, S.; Riley, S.J.; Tikhonov, G.Y.; Tomczyk, N.A.; Vajda, S.; Winans, R.E.

    2005-01-01

    The size evolution of platinum nanoparticles formed on a SiO2/Si(111) substrate as a function of the level of surface coverage with deposited clusters has been investigated. The anisotropic shapes of sub-nanometer-size nanoparticles are changed to isotropic on the amorphous substrate as their sizes increased. Using anomalous grazing incidence small-angle x-ray scattering (AGISAXS), the scattering from nanoparticles on the surface of a substrate is well separated from that of surface roughness and fluorescence. We show that AGISAXS is a very effective method to subtract the background and can provide unbiased information about particle sizes of less than 1 nm.

  5. 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.

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

    Science.gov (United States)

    2016-12-01

    Natick, MA, USA), which were then sealed using “5 Minute” epoxy. The epoxy was allowed to cure overnight. The samples were then placed on the sample...of X-ray and neutron scattering in polymer science. New York (NY): Oxford University Press; 2000. 3. Strobl G. The physics of polymers: concepts for...understanding their structures and behavior. 3rd ed. Berlin Heidelberg (Germany): Springer; 2006. 4. Hamley IW. The physics of block copolymers. 1st

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

    Science.gov (United States)

    2016-12-01

    Natick, MA, USA), which were then sealed using “5 Minute” epoxy. The epoxy was allowed to cure overnight. The samples were then placed on the sample...of X-ray and neutron scattering in polymer science. New York (NY): Oxford University Press; 2000. 3. Strobl G. The physics of polymers: concepts for...understanding their structures and behavior. 3rd ed. Berlin Heidelberg (Germany): Springer; 2006. 4. Hamley IW. The physics of block copolymers. 1st

  8. Small angle X-ray and neutron scattering from solutions of biological macromolecules

    CERN Document Server

    Svergun, Dmitri I; May, Roland P; Timmins, Peter A

    2013-01-01

    In this book, following the presentation of the basics of scattering from isotropic macromolecular solutions, modern instrumentation, experimental practice and advanced analysis techniques are explained. Advantages of X-rays (rapid data collection, small sample volumes) and of neutrons (contrast variation by hydrogen/deuterium exchange) are specifically highlighted. Examples of applications of the technique to different macromolecular systems are considered with specific emphasis on the synergistic use of SAXS/SANS with other structural, biophysical and computational techniques.

  9. 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

  10. Synchrotron X-Ray Radiation and Deformation Studies

    DEFF Research Database (Denmark)

    Fæster Nielsen, Søren

    In the present thesis two different synchrotron X-ray diffraction techniques capable of producing non-destructive information from the bulk of samples, have been investigated. Traditionally depth resolu-tion in diffraction experiments is obtained by inserting pinholes in both the incoming...... machining. The conical slit has six 25µm thick conically shaped openings matching six of the Debye-Scherrer cones from a fcc powder. By combining the conical slit with a micro-focused incoming beam of hard X-rays an embedded gauge volume is defined. Using a 2D detector, fast and complete information can...... boundary morphology. Another X-ray diffraction technique was applied on the three-dimensional X-ray diffraction (3DXRD) microscope at the ESRF synchrotron. The microscope uses a new technique based on ray tracing of diffracted high energy X-rays, providing a fast and non-destructive scheme for mapping...

  11. Synchrotron-Radiation Induced X-Ray Emission (SRIXE)

    Energy Technology Data Exchange (ETDEWEB)

    Jones, Keith W.

    1999-09-01

    Elemental analysis using emission of characteristic x rays is a well-established scientific method. The success of this analytical method is highly dependent on the properties of the source used to produce the x rays. X-ray tubes have long existed as a principal excitation source, but electron and proton beams have also been employed extensively. The development of the synchrotron radiation x-ray source that has taken place during the past 40 years has had a major impact on the general field of x-ray analysis. Even tier 40 years, science of x-ray analysis with synchrotron x-ray beams is by no means mature. Improvements being made to existing synchrotron facilities and the design and construction of new facilities promise to accelerate the development of the general scientific use of synchrotron x-ray sources for at least the next ten years. The effective use of the synchrotron source technology depends heavily on the use of high-performance computers for analysis and theoretical interpretation of the experimental data. Fortunately, computer technology has advanced at least as rapidly as the x-ray technology during the past 40 years and should continue to do so during the next decade. The combination of these technologies should bring about dramatic advances in many fields where synchrotron x-ray science is applied. It is interesting also to compare the growth and rate of acceptance of this particular research endeavor to the rates for other technological endeavors. Griibler [1997] cataloged the time required for introduction, diffusion,and acceptance of technological, economic, and social change and found mean values of 40 to 50 years. The introduction of the synchrotron source depends on both technical and non-technical factors, and the time scale at which this seems to be occurring is quite compatible with what is seen for other major innovations such as the railroad or the telegraph. It will be interesting to see how long the present rate of technological change

  12. 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.

  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

    2016-11-01

    Small-angle X-ray scattering (SAXS) and small-angle neutron scattering (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. 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 be pure and monodisperse for the duration of the experiment. This protocol outlines the basic physics of SAXS and SANS, and it 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 (SEC) and light scattering. Also included are procedures that are specific to X-rays (in-line SEC-SAXS) and neutrons, specifically preparing samples for contrast matching or variation experiments and deuterium labeling of proteins.

  14. 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.

  15. 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.)

  16. A synchrotron radiation facility for x-ray astronomy

    DEFF Research Database (Denmark)

    Hall, C.J.; Lewis, R.A.; Christensen, Finn Erland

    1997-01-01

    A proposal for an x-ray optics test facility based at a synchrotron radiation source is presented. The facility would incorporate a clean preparation area, and a large evacuable test area. The advantages of using a synchrotron as the source of the test radiation are discussed. These include the a...

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

    Directory of Open Access Journals (Sweden)

    Norbert Kučerka

    2015-09-01

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

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

    Science.gov (United States)

    Kučerka, Norbert; Heberle, Frederick A; Pan, Jianjun; Katsaras, John

    2015-09-21

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

  19. Facilitating model reconstruction for single-particle scattering using small-angle X-ray scattering methods.

    Science.gov (United States)

    Ma, Shufen; Liu, Haiguang

    2016-04-01

    X-ray free-electron lasers generate intense femtosecond X-ray pulses, so that high-resolution structure determination becomes feasible from noncrystalline samples, such as single particles or single molecules. At the moment, the orientation of sample particles cannot be precisely controlled, and consequently the unknown orientation needs to be recovered using computational algorithms. This delays the model reconstruction until all the scattering patterns have been re-oriented, which often entails a long elapse of time and until the completion of the experiment. The scattering patterns from single particles or multiple particles can be summed to form a virtual powder diffraction pattern, and the low-resolution region, corresponding to the small-angle X-ray scattering (SAXS) regime, can be analysed using existing SAXS methods. This work presents a pipeline that converts single-particle data sets into SAXS data, from which real-time model reconstruction is achieved using the model retrieval approach implemented in the software package SASTBX [Liu, Hexemer & Zwart (2012). J. Appl. Cryst. 45 , 587-593]. To illustrate the applications, two case studies are presented with real experimental data sets collected at the Linac Coherent Light Source.

  20. Nano materials Characterization by Small-angle X-ray Scattering Applied on a Multi-purpose X-ray Diffractometer Platform

    International Nuclear Information System (INIS)

    Bolze, J.

    2011-01-01

    We present the application of the small-angle X-ray scattering (SAXS) technique for the structural characterization of nano materials. This technique has become available in the laboratory on a multipurpose X-ray diffractometer platform and yields information that is complementary to what can be deduced from XRD (or WAXS) data. Among others SAXS is used for the determination of the size distribution, shape, specific surface area, inner structure and aggregation behavior of nanoparticles. It may also be applied to investigate pore size distributions in meso porous materials as well as ordered nano structures. Several application examples dealing with the characterization of photo catalytic nano powders, porous materials, polymer nano composites, colloidal dispersions, surfactants and related samples will be given. Furthermore, the SAXS technique will be compared and contrasted to complementary experimental techniques, such as dynamic light scattering, ultracentrifugation, electron microscopy, BET measurements and mercury intrusion porosimetry. Whereas this presentation focuses on the application examples of the SAXS technique, a more fundamental and practical introduction will be given within the workshop. (author)

  1. The nanomechanics of feather keratin studied by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Pabisch, Silvia; Puchegger, Stephan; Peterlik, Herwig; Weiss, Ingrid; Kirchner, Helmut

    2012-01-01

    Full text: Feather keratin is a highly conserved protein of 98 amino acids synthesized intracellularly in aves. In the cortex of the tail covert feathers of the peacock it forms a crystalline structure, held together by disulfide bonds between the nine cysteines of the molecule. Despite the biological importance of the molecule, its spatial structure has not yet been determined. Fraser and Parry proposed a crystallographic arrangement of beta-barrels and relegate the N-terminus and the C-terminus to an amorphous matrix, akin to the situation in silk. Therefore, in-situ tension and compression tests were made to investigate the changes in axial and lateral direction. Nanoscopically a pronounced structural asymmetry between tension and compression rules out a dihedral axis normal to the fibril direction, and indicates a strong clip-like polarization of the molecule. Based on these X-ray diffraction data from Pavo cristatus feathers, a model is presented for the axial and lateral arrangement of the molecule in feather keratin, which integrates biochemical structure and mechanical experiments. (author)

  2. Synchrotron X-ray induced solution precipitation of nanoparticles

    CERN Document Server

    Lee, H J; Hwu, Y; Tsai, W L

    2003-01-01

    By irradiating a solution in electroless Ni deposition using synchrotron X-rays, Ni composite was found to nucleate homogeneously and eventually precipitate in the form of nanoparticles. The size of the nanoparticles precipitated is rather uniform (100-300 nm depending on the applied temperature). By the addition of an organic acid, well-dispersed nanoparticles could be effectively deposited on glass substrate. The hydrated electrons (e sub a sub q sup -), products of radiolysis of water molecules by synchrotron X-rays, may be responsible for the effective reduction of the metal ions, resulting in homogeneous nucleation and nanoparticle formation. Our results suggest that synchrotron X-ray can be used to induce solution precipitation of nanoparticles and therefore lead to a new method of producing nanostructured particles and coating.

  3. Micromirror-based manipulation of synchrotron x-ray beams

    Science.gov (United States)

    Walko, D. A.; Chen, Pice; Jung, I. W.; Lopez, D.; Schwartz, C. P.; Shenoy, G. K.; Wang, Jin

    2017-08-01

    Synchrotron beamlines typically use macroscopic, quasi-static optics to manipulate x-ray beams. We present the use of dynamic microelectromechanical systems-based optics (MEMS) to temporally modulate synchrotron x-ray beams. We demonstrate this concept using single-crystal torsional MEMS micromirrors oscillating at frequencies of 75 kHz. Such a MEMS micromirror, with lateral dimensions of a few hundred micrometers, can interact with x rays by operating in grazing-incidence reflection geometry; x rays are deflected only when an x-ray pulse is incident on the rotating micromirror under appropriate conditions, i.e., at an angle less than the critical angle for reflectivity. The time window for such deflections depends on the frequency and amplitude of the MEMS rotation. We demonstrate that reflection geometry can produce a time window of a few microseconds. We further demonstrate that MEMS optics can isolate x rays from a selected synchrotron bunch or group of bunches. With ray-trace simulations we explain the currently achievable time windows and suggest a path toward improvements.

  4. Small-angle neutron and X-ray scattering studies of supraatomic structure of synthetic quartz irradiated by fast neutrons

    International Nuclear Information System (INIS)

    Lebedev, V.M.; Lebedev, V.T.; Orlov, S.P.; Golubkov, V.V.; Pevzner, B.Z.; Tolstikhin, I.N.

    2008-01-01

    Quartz nanostructures have been simulated for the investigation into diffusion of gases in the Earth crust. The nanostructure of synthetic quartz irradiated by fast neutrons with energy E n >0.1 MeV was studied by neutron and X-ray small-angle scattering. The range of neutron fluence is of 10 17 cm -2 up to 2x10 -2 0 cm -2 . In the irradiated samples the different kinds of defects such as point-like, extended linear (dislocations) and globular (size ∼100 nm, amorphous phase nuclei) were observed. The density of highly irradiated quartz (fluence 2x10 20 cm -2 ) is shown to decrease by 0.39 g/cm 2 and reach the magnitude of 2.260 g/cm 2 corresponding to 100% metamict phase. The first results of model structures helium saturation have been received [ru

  5. Investigating the Effect of Adding Drug (Lidocaine) to a Drug Delivery System Using Small-Angle X-Ray Scattering

    Science.gov (United States)

    Balogh, Joakim; Pedersen, Jan Skov

    The effect on a model drug delivery system when adding a drug, lidocaine, has been studied. Temperature and concentration dependence of a nonionic microemulsion with part of the oil, 1 and %[vol.]10, substituted with drug has been investigated. A nonionic oil-in-water microemulsion consisting of CH3(CH2)11(OCH2CH2)5OH, (C12E5), decane, water and the drug (lidocaine) that has been used to substitute part of the oil was studied. The microscopic differences have been derived from small-angle X-ray scattering (SAXS) data and the results are compared with light scattering data. Using these results together with the macroscopic differences, as observed in the phase diagram (lowering of phase boundaries), between the systems with and without lidocaine can be explained.

  6. 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.

  7. 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

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

    Science.gov (United States)

    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 Julián Fernández, C; García, M A

    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 x 10(-4) was found at the Au L3 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.

  9. Quantifying "Softness" of Organic Coatings on Gold Nanoparticles Using Correlated Small-Angle X-ray and Neutron Scattering.

    Science.gov (United States)

    Diroll, Benjamin T; Weigandt, Katie M; Jishkariani, Davit; Cargnello, Matteo; Murphy, Ryan J; Hough, Lawrence A; Murray, Christopher B; Donnio, Bertrand

    2015-12-09

    Small-angle X-ray and neutron scattering provide powerful tools to selectively characterize the inorganic and organic components of hybrid nanomaterials. Using hydrophobic gold nanoparticles coated with several commercial and dendritic thiols, the size of the organic layer on the gold particles is shown to increase from 1.2 to 4.1 nm. A comparison between solid-state diffraction from self-assembled lattices of nanoparticles and the solution data from neutron scattering suggests that engineering softness/deformability in nanoparticle coatings is less straightforward than simply increasing the organic size. The "dendritic effect" in which higher generations yield increasingly compact molecules explains changes in the deformability of organic ligand shells.

  10. 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.

  11. 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.

  12. 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.

  13. Light source for synchrotron radiation x-ray topography study at Beijing Synchrotron Radiation Laboratory (BSRL)

    International Nuclear Information System (INIS)

    Zhao Jiyong; Jiang Jianhua; Tian Yulian

    1992-01-01

    Characteristics of the synchrotron radiation source for X-ray topography study at Beijing Synchrotron Radiation Laboratory (BSRL) is described, local geometrical resolution of topographies is discussed, and the diffracting intensities of white beam topography is given

  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. A combined small-angle X-ray and neutron scattering study of the structure of purified soluble gastrointestinal mucins.

    Science.gov (United States)

    Georgiades, Pantelis; di Cola, Emanuela; Heenan, Richard K; Pudney, Paul D A; Thornton, David J; Waigh, Thomas A

    2014-12-01

    The structures of purified soluble porcine gastric (Muc5ac) and duodenal (Muc2) mucin solutions at neutral and acidic pH were examined using small-angle X-ray scattering and small-angle neutron scattering experiments. We provide evidence for the morphology of the network above the semidilute overlap concentration and above the entanglement concentration. Furthermore, we investigated the gelation of both types of mucin solutions in response to a reduction in pH, where we observed the formation of large-scale heterogeneities within the polymer solutions, typical of microphase-separated gels. The concentration dependence of the inhomogeneity length scale (Ξ) and the amplitude of the excess scattering intensity [I(ex) (0)] are consistent with previously studied gelled synthetic polymeric systems. The persistence lengths of the chains were found to be similar for both Muc5ac and Muc2 from Kratky plots of the neutron data (8 ± 2 nm). © 2014 Wiley Periodicals, Inc.

  16. [Clinical applications of synchrotron radiation X-ray].

    Science.gov (United States)

    Uyama, C

    1994-09-01

    Synchrotron Radiation X-ray (SR X-ray) is an extremely strong X-ray source with a photon number more than 10(4) compared with that of the current X-ray tube. X-rays obtained by monochromatizing SR X-ray have been applied to new techniques for medical diagnosis. Several studies are now being conducted at the beam site for medical use at the Accumulation Ring of the High Energy Physics Research Institute, Tsukuba. Applications being studied include (1) energy subtraction coronary angiography. (2) microdetection of metas in samples excised from subjects. (3) monochromatic X-ray computed tomography and so on. Energy subtraction coronary angiography might have a safety advantage over the current selective coronary angiography. Microdetection of mandatory metals and poisonous heavy metals in in vivo samples contributes to the development of pathologic knowledge and clinical treatment of cancer and heavy metal toxications. Monochromatic X-ray CT is expected to detect diseases in the early stage due to increased accuracy in CT values.

  17. High-intensity laser synchrotron x-ray source

    International Nuclear Information System (INIS)

    Pogorelsky, I.V.

    1995-10-01

    A laser interacting with a relativistic electron beam behaves like a virtual wiggler of an extremely short period equal to half of the laser wavelength. This approach opens a route to relatively compact, high-brightness x-ray sources alternative or complementary to conventional synchrotron light sources. Although not new, the Laser Synchrotron Light Source (LSLS) concept is still waiting for a convincing demonstration. Available at the BNL's Accelerator Test Facility (ATF), a high-brightness electron beam and the high-power C0 2 laser may be used as prototype LSLS brick stones. In a feasible demonstration experiment, 10-GW, 100-ps C0 2 laser beam will be brought to a head-on collision with a 10-ps, 0.5-nC, 70 MeV electron bunch. Flashes of well-collimated, up to 9.36-keV (∼ Angstrom) x-rays of 10-ps pulse duration, with a flux of ∼10 19 photons/sec will be produced via linear Compton backscattering. The x-ray spectrum is tunable proportionally to a variable e-beam energy. A natural short-term extension of the proposed experiment would be further enhancement of the x-ray flux to a 10 21 -10 22 photons/sec level, after the ongoing ATF CO 2 laser upgrade to 1 TW peak power and electron bunch shortening to 3 ps. The ATF LSLS x-ray beamline, exceeding by orders of magnitude the peak fluxes attained at the National Synchrotron Light Source (NSLS) x-ray storage ring, may become attractive for certain users, e.g., for biological x-ray microscopy. In addition, a terawatt CO 2 laser will enable harmonic multiplication of the x-ray spectrum via nonlinear Compton scattering

  18. 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.

  19. 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.)

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

    International Nuclear Information System (INIS)

    Li, Denghua; Du, Sujun; Lu, Chunxiang; Wu, Gangping; Yang, Yu; Wang, Lina

    2016-01-01

    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.)

  1. 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

  2. Quantitative X-ray microtomography with synchrotron radiation

    International Nuclear Information System (INIS)

    Donath, T.

    2007-01-01

    Synchrotron-radiation-based computed microtomography (SR μ CT) is an established method for the examination of volume structures. It allows to measure the x-ray attenuation coefficient of a specimen three-dimensionally with a spatial resolution of about one micrometer. In contrast to conventional x-ray sources (x-ray tubes), the unique properties of synchrotron radiation enable quantitative measurements that do not suffer from beam-hardening artifacts. During this work the capabilities for quantitative SR μ CT measurements have been further improved by enhancements that were made to the SR μ CT apparatus and to the reconstruction chain. For high-resolution SR μ CT an x-ray camera consisting of luminescent screen (x-ray phosphor), lens system, and CCD camera was used. A significant suppression of blur that is caused by reflections inside the luminescent screen could be achieved by application of an absorbing optical coating to the screen surface. It is shown that blur and ring artifacts in the tomographic reconstructions are thereby drastically reduced. Furthermore, a robust and objective method for the determination of the center of rotation in projection data (sinograms) is presented that achieves sub-pixel precision. By implementation of this method into the reconstruction chain, complete automation of the reconstruction process has been achieved. Examples of quantitative SR μ CT studies conducted at the Hamburger Synchrotronstrahlungslabor HASYLAB at the Deutsches Elektronen-Synchrotron DESY are presented and used for the demonstration of the achieved enhancements. (orig.)

  3. 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.

  4. 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

  5. X-ray diffraction microtomography using synchrotron radiation

    CERN Document Server

    Barroso, R C; Jesus, E F O; Oliveira, L F

    2001-01-01

    The X-ray diffraction computed tomography technique is based on the interference phenomena of the coherent scatter. For low-momentum transfer, it is most probable that the scattering interaction will be coherent. A selective discrimination of a given element in a scanned specimen can be realized by fixing the Bragg angle which produces an interference peak and then, to carry out the computed tomography in the standard mode. The image reconstructed exalts the presence of this element with respect to other ones in a sample. This work reports the feasibility of a non-destructive synchrotron radiation X-ray diffraction imaging technique. This research was performed at the X-ray Diffraction beam line of the National Synchrotron Light Laboratory (LNLS) in Brazil. The coherent scattering properties of different tissue and bone substitute materials were evaluated. Furthermore, diffraction patterns of some polycrystalline solids were studied due to industrial and environmental human exposure to these metals. The obtai...

  6. Structure and property characterization of low-k dielectric porous thin films determined by x-ray reflectivity and small-angle neutron scattering

    International Nuclear Information System (INIS)

    Lin, Eric K.; Lee, Hae-jeong; Wang, Howard; Wu Wenli

    2001-01-01

    A novel methodology using a combination of high energy ion scattering, x-ray reflectivity, and small angle neutron scattering is developed to characterize the structure and properties of porous thin films for use as low-k dielectric materials. Ion scattering is used to determine the elemental composition of the film. X-ray reflectivity is used to measure the average electron density, film thickness, and electron density depth profile. Small angle neutron scattering is used to determine the pore structure and pore connectivity. Combining information from all three techniques, the film porosity and matrix material density can be uniquely determined

  7. Hard X-ray Sources for the Mexican Synchrotron Project

    Science.gov (United States)

    Reyes-Herrera, Juan

    2016-10-01

    One of the principal tasks for the design of the Mexican synchrotron was to define the storage ring energy. The main criteria for choosing the energy come from studying the electromagnetic spectrum that can be obtained from the synchrotron, because the energy range of the spectrum that can be obtained will determine the applications available to the users of the future light source. Since there is a public demand of hard X-rays for the experiments in the synchrotron community users from Mexico, in this work we studied the emission spectra from some hard X-ray sources which could be the best options for the parameters of the present Mexican synchrotron design. The calculations of the flux and the brightness for one Bending Magnet and four Insertion Devices are presented; specifically, for a Superconducting Bending Magnet (SBM), a Superconducting Wiggler (SCW), an In Vacuum Short Period Undulator (IV-SPU), a Superconducting Undulator (SCU) and for a Cryogenic Permanent Magnet Undulator (CPMU). Two commonly available synchrotron radiation programs were used for the computation (XOP and SRW). From the results, it can be concluded that the particle beam energy from the current design is enough to have one or more sources of hard X-rays. Furthermore, a wide range of hard X-ray region can be covered by the analyzed sources, and the choice of each type should be based on the specific characteristics of the X-ray beam to perform the experiments at the involved beamline. This work was done within the project Fomix Conacyt-Morelos ”Plan Estrategico para la construccion y operación de un Sincrotron en Morelos” (224392).

  8. Small-Angle X-Ray Scattering for Imaging of Surface Layers on Intact Bacteria in the Native Environment

    Science.gov (United States)

    Sekot, Gerhard; Schuster, David; Messner, Paul; Pum, Dietmar

    2013-01-01

    Crystalline cell surface layers (S-layers) represent a natural two-dimensional (2D) protein self-assembly system with nanometer-scale periodicity that decorate many prokaryotic cells. Here, we analyze the S-layer on intact bacterial cells of the Gram-positive organism Geobacillus stearothermophilus ATCC 12980 and the Gram-negative organism Aquaspirillum serpens MW5 by small-angle X-ray scattering (SAXS) and relate it to the structure obtained by transmission electron microscopy (TEM) after platinum/carbon shadowing. By measuring the scattering pattern of X rays obtained from a suspension of bacterial cells, integral information on structural elements such as the thickness and lattice parameters of the S-layers on intact, hydrated cells can be obtained nondestructively. In contrast, TEM of whole mounts is used to analyze the S-layer lattice type and parameters as well as the physical structure in a nonaqueous environment and local information on the structure is delivered. Application of SAXS to S-layer research on intact bacteria is a challenging task, as the scattering volume of the generally thin (3- to 30-nm) bacterial S-layers is low in comparison to the scattering volume of the bacterium itself. For enhancement of the scattering contrast of the S-layer in SAXS measurement, either silicification (treatment with tetraethyl orthosilicate) is used, or the difference between SAXS signals from an S-layer-deficient mutant and the corresponding S-layer-carrying bacterium is used for determination of the scattering signal. The good agreement of the SAXS and TEM data shows that S-layers on the bacterial cell surface are remarkably stable. PMID:23504021

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

    Science.gov (United States)

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

    2017-04-01

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

  10. Low energy X-ray grating interferometry at the Brazilian Synchrotron

    Science.gov (United States)

    Koch, F. J.; O'Dowd, F. P.; Cardoso, M. B.; Da Silva, R. R.; Cavicchioli, M.; Ribeiro, S. J. L.; Schröter, T. J.; Faisal, A.; Meyer, P.; Kunka, D.; Mohr, J.

    2017-06-01

    Grating based X-ray differential phase contrast imaging has found a large variety of applications in the last decade. Different types of samples call for different imaging energies, and efforts have been made to establish the technique all over the spectrum used for conventional X-ray imaging. Here we present a two-grating interferometer working at 8.3 keV, implemented at the bending magnet source of the IMX beamline of the Brazilian Synchrotron Light Laboratory. The low design energy is made possible by gratings fabricated on polymer substrates, and makes the interferometer mainly suited to the investigation of light and thin samples. We investigate polymer microspheres filled with Fe2O3 nanoparticles, and find that these particles give rise to a significant visibility reduction due to small angle scattering.

  11. An X-ray microprobe facility using synchrotron radiation

    International Nuclear Information System (INIS)

    Gordon, B.M.; Jones, K.W.; Hanson, A.L.; Pounds, J.G.; Rivers, M.L.; Sutton, S.R.; Spanne, P.

    1990-01-01

    An X-ray microprobe for trace elemental analysis at micrometer spatial resolutions, using synchrotron radiation (SR), is under development. The facility consists of two beamlines, one including a 1:1 focusing mirror and the other an 8:1 ellipsoidal mirror. At present, open-quotes white lightclose quotes is used for excitation of the characteristic X-ray fluorescence lines. Sensitivities in thin biological samples are in the range of 2-20 fg in 100 μm 2 areas in 5 min irradiation times. Scanning techniques, as well as microtomography and chemical speciation, are discussed. Application to a specific biomedical study is included

  12. 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

  13. 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.

  14. Molecular structures of fluid phase phosphatidylglycerol bilayers as determined by small angle neutron and X-ray scattering

    Science.gov (United States)

    Pan, Jianjun; Heberle, Frederick A.; Tristram-Nagle, Stephanie; Szymanski, Michelle; Koepfinger, Mary; Katsaras, John; Kučerka, Norbert

    2013-01-01

    We have determined the molecular structures of commonly used phosphatidylglycerols (PGs) in the commonly accepted biologically relevant fluid phase. This was done by simultaneously analyzing small angle neutron and X-ray scattering data, with the constraint of measured lipid volumes. We report the temperature dependence of bilayer parameters obtained using the one-dimensional scattering density profile model – which was derived from molecular dynamics simulations – including the area per lipid, the overall bilayer thickness, as well as other intrabilayer parameters (e.g., hydrocarbon thickness). Lipid areas are found to be larger than their phosphatidylcholine (PC) counterparts, a result likely due to repulsive electrostatic interactions taking place between the charged PG headgroups even in the presence of sodium counterions. In general, PG and PC bilayers show a similar response to changes in temperature and chain length, but differ in their response to chain unsaturation. For example, compared to PC bilayers, the inclusion of a first double bond in PG lipids results in a smaller incremental change to the area per lipid and bilayer thickness. However, the extrapolated lipid area of saturated PG lipids to infinite chain length is found to be similar to that of PCs, an indication of the glycerol–carbonyl backbone's pivotal role in influencing the lipid–water interface. PMID:22583835

  15. 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.

  16. 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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Emanuela Di Cola

    2016-03-01

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

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

    Science.gov (United States)

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

    2016-03-28

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

  20. 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.

  1. 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)

  2. Temperature-dependent atomic models of detergent micelles refined against small-angle X-ray scattering data.

    Science.gov (United States)

    Ivanovic, Milos T; Bruetzel, Linda K; Lipfert, Jan; Hub, Jochen S

    2018-03-13

    Surfactants have found a wide range of industrial and scientific applications. In particular, detergent micelles are used as lipid membrane mimics to solubilize membrane proteins for functional and structural characterisation. However, an atomic-level understanding of surfactants remains limited because many experiments provide only low-resolution structural information on surfactant aggregates. Here, we combine small-angle X-ray scattering with molecular dynamics simulations to derive fully atomic models of two maltoside micelles, at temperatures between 10°C and 70°C. We find that the micelles take the shape of general tri-axial ellipsoids and decrease in size and aggregation number with increasing temperature. Density profiles of hydrophobic groups and water along the three principal axes reveal that the minor micelle axis closely mimics lipid membranes. Our results suggest that coupling atomic simulations with low-resolution data allows for a structural characterisation of surfactant aggregates. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. A small-angle X-ray scattering study of the lyotropic nematic phase of vanadium pentoxide gels

    Energy Technology Data Exchange (ETDEWEB)

    Davidson, P. [Universite de Paris-Sud, Orsay (France). Lab. de Phys. des Solides; Bourgaux, C.; Sergot, P.; Livage, J.

    1997-10-01

    Aqueous suspensions of vanadium pentoxide (V{sub 2}O{sub 5}) ribbons, also called Zocher phases, are known to display a lyotropic nematic phase. In this paper, it is shown how the small-angle X-ray scattering (SAXS) technique can provide useful information on the building blocks and their organization in this phase. SAXS experiments were performed either on unoriented samples or on samples aligned by a magnetic field or by shear flow. The scattering is comparable to that of the other classic lyotropic nematic phases displayed by stiff organic rod-like particles such as the tobacco mosaic virus. Scattering studies show that the building blocks have a ribbon shape, that their thickness is 9(1) A and indirectly that their width is several 100 A. Their length is known to be around a few thousand A and therefore could not be measured by SAXS. By following the average distance between the ribbons as a function of concentration, it is shown that the swelling of the phase is one-dimensional at large concentrations and two-dimensional at low concentrations. Finally, estimates of the nematic order parameter of a single domain sample and of samples sheared in a Couette cell have been obtained. (orig.). 24 refs.

  4. Particle evolution of Composition B-3 studied by time-resolved small angle x-ray scattering

    Science.gov (United States)

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

    Accessing various pressures and temperatures of the carbon phase diagram through high explosive (HE) detonations, as a means of synthesis, provides an exciting opportunity to study new carbon allotropes. Carbon allotropes in HE detonations are thought to form through collision of free carbon within the detonation cloud; however direct confirmation of real-time product formation is limited due to experimental restraints. Time-resolved small angle x-ray scattering (TRSAXS) of in-line detonations provides information about particle formation behind the detonation front on the 100's of nanoseconds timescale. The only set-up of its kind in the United States is at Argonne National Laboratory at the Advanced Photon Source in the Dynamic Compression Sector (DCS). Through empirical and analytical analysis of the TRSAXS data, parameters such as particle size and morphology can be deduced with respect to time. In the case of Composition B-3 (40% TNT/60% RDX) particle formation morphs from spherical core-shell structure to an elongated structure at long times ( 2 us) under vacuum. To complete the timeline of carbon formation, the post detonation soot is also analyzed to confirm this elongated structure as the majority carbon product. LA-UR-16-28691

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

    Science.gov (United States)

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

    2018-04-11

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

  6. Synchrotron x-ray reflectivity study of oxidation/passivation of copper and silicon.

    Energy Technology Data Exchange (ETDEWEB)

    Chu, Y.; Nagy, Z.; Parkhutik, V.; You, H.

    1999-07-21

    Synchrotron x-ray-scattering technique studies of copper and silicon electrochemical interfaces are reported. These two examples illustrate the application of synchrotron x-ray techniques for oxidation, passivation, and dissolution of metals and semiconductors.

  7. In Operando Monitoring of the Pore Dynamics in Ordered Mesoporous Electrode Materials by Small Angle X-ray Scattering.

    Science.gov (United States)

    Park, Gwi Ok; Yoon, Jeongbae; Park, Eunjun; Park, Su Bin; Kim, Hyunchul; Kim, Kyoung Ho; Jin, Xing; Shin, Tae Joo; Kim, Hansu; Yoon, Won-Sub; Kim, Ji Man

    2015-05-26

    To monitor dynamic volume changes of electrode materials during electrochemical lithium storage and removal process is of utmost importance for developing high performance lithium storage materials. We herein report an in operando probing of mesoscopic structural changes in ordered mesoporous electrode materials during cycling with synchrotron-based small angel X-ray scattering (SAXS) technique. In operando SAXS studies combined with electrochemical and other physical characterizations straightforwardly show how porous electrode materials underwent volume changes during the whole process of charge and discharge, with respect to their own reaction mechanism with lithium. This comprehensive information on the pore dynamics as well as volume changes of the electrode materials will not only be critical in further understanding of lithium ion storage reaction mechanism of materials, but also enable the innovative design of high performance nanostructured materials for next generation batteries.

  8. 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...

  9. 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...

  10. 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...

  11. Diamond detectors for synchrotron radiation X-ray applications

    International Nuclear Information System (INIS)

    De Sio, A.; Pace, E.; Cinque, G.; Marcelli, A.; Achard, J.; Tallaire, A.

    2007-01-01

    Due to its unique physical properties, diamond is a very appealing material for the development of electronic devices and sensors. Its wide band gap (5.5 eV) endows diamond based devices with low thermal noise, low dark current levels and, in the case of radiation detectors, high visible-to-X-ray signal discrimination (visible blindness) as well as high sensitivity to energies greater than the band gap. Furthermore, due to its radiation hardness diamond is very interesting for applications in extreme environments, or as monitor of high fluency radiation beams. In this work the use of diamond based detectors for X-ray sensing is discussed. On purpose, some photo-conductors based on different diamond types have been tested at the DAFNE-L synchrotron radiation laboratory at Frascati. X-ray sensitivity spectra, linearity and stability of the response of these diamond devices have been measured in order to evidence the promising performance of such devices

  12. Soft X-ray microscopy and lithography with synchrotron radiation

    International Nuclear Information System (INIS)

    Gudat, W.

    1977-12-01

    Considerable progress in the technique microscopy with soft X-ray radiation has been achieved in particular through the application of synchrotron radiation. Various methods which are currently being studied theoretically or already being used practically will be described briefly. Attention is focussed on the method of contact microscopy. Various biological specimens have been investigated by this method with a resolution as good as 100 A. X-ray lithography which in the technical procedure is very similar to contact microscopy gives promise for the fabrication of high quality submicron structures in electronic device production. Important factors limiting the resolution and determining the performance of contact microscopy and X-ray lithography will be discussed. (orig.) [de

  13. Quantitative X-ray microtomography with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Donath, T. [GKSS-Forschungszentrum Geesthacht GmbH (Germany). Inst. fuer Materialforschung

    2007-07-01

    Synchrotron-radiation-based computed microtomography (SR{sub {mu}}CT) is an established method for the examination of volume structures. It allows to measure the x-ray attenuation coefficient of a specimen three-dimensionally with a spatial resolution of about one micrometer. In contrast to conventional x-ray sources (x-ray tubes), the unique properties of synchrotron radiation enable quantitative measurements that do not suffer from beam-hardening artifacts. During this work the capabilities for quantitative SR{sub {mu}}CT measurements have been further improved by enhancements that were made to the SR{sub {mu}}CT apparatus and to the reconstruction chain. For high-resolution SR{sub {mu}}CT an x-ray camera consisting of luminescent screen (x-ray phosphor), lens system, and CCD camera was used. A significant suppression of blur that is caused by reflections inside the luminescent screen could be achieved by application of an absorbing optical coating to the screen surface. It is shown that blur and ring artifacts in the tomographic reconstructions are thereby drastically reduced. Furthermore, a robust and objective method for the determination of the center of rotation in projection data (sinograms) is presented that achieves sub-pixel precision. By implementation of this method into the reconstruction chain, complete automation of the reconstruction process has been achieved. Examples of quantitative SR{sub {mu}}CT studies conducted at the Hamburger Synchrotronstrahlungslabor HASYLAB at the Deutsches Elektronen-Synchrotron DESY are presented and used for the demonstration of the achieved enhancements. (orig.)

  14. Applications of synchrotron X-rays in microelectronics industry research

    International Nuclear Information System (INIS)

    Jordan-Sweet, Jean L.; Detavernier, Christophe; Lavoie, Christian; Mooney, Patricia M.; Toney, Michael F.

    2005-01-01

    The high flux and density of X-rays produced at synchrotrons provide the microelectronics industry with a powerful probe of the structure and behavior of a wide array of solid materials that are being developed for use in devices of the future. They also are of great use in determining why currently-used materials and processes sometimes fail. This paper describes the X20 X-ray beamline facility operated by IBM at the National Synchrotron Light Source, and presents a series of three industry challenges and results that illustrate the variety of techniques used and problems addressed. The value of this research ranges from solving short-term, technically specific problems to increasing our academic understanding of materials in general. Techniques discussed include high-resolution diffraction, time-resolved diffraction, texture measurements, and grazing-incidence diffraction

  15. Application of X-ray synchrotron microscopy instrumentation in biology

    Energy Technology Data Exchange (ETDEWEB)

    Gasperini, F. M. [Medical Science Program, Fluminense Federal Univ., Niteroi (Brazil); Pereira, G. R. [Dept. of Metallurgical and Materials Engineering, Federal Univ. of Rio de Janeiro (Brazil); Granjeiro, J. M. [Molecular and Cell Biology Dept., Fluminense Federal Univ., Niteroi, Rio de Janeiro (Brazil); Calasans-Maia, M. D. [Oral Surgery Dept., Fluminense Federal Univ., Niteroi, Rio de Janeiro (Brazil); Rossi, A. M. [Biomaterials Laboratory, Brazilian Center of Physics Research, Rio de Janeiro (Brazil); Perez, C. A. [Brazilian Synchrotron Laboratory, Campinas, Sao Paulo (Brazil); Lopes, R. T.; Lima, I. [Nuclear Engineering Laboratory, Federal Univ. of Rio de Janeiro (Brazil)

    2011-07-01

    X-ray micro-fluorescence imaging technique has been used as a significant tool in order to investigate minerals contents in some kinds of materials. The aim of this study was to evaluate the elemental distribution of calcium and zinc in bone substitute materials (nano-hydroxyapatite spheres) and cortical bones through X-Ray Micro-fluorescence analysis with the increment of Synchrotron Radiation in order to evaluate the characteristics of the newly formed bone and its interface, the preexisting bone and biomaterials by the arrangement of collagen fibers and its birefringence. The elemental mapping was carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo, Brazil working at D09-XRF beam line. Based on this study, the results suggest that hydroxyapatite-based biomaterials are biocompatible, promote osteo-conduction and favored bone repair. (authors)

  16. Insights into Surface Interactions between Metal Organic Frameworks and Gases during Transient Adsorption and Diffusion by In-Situ Small Angle X-ray Scattering

    Directory of Open Access Journals (Sweden)

    Ludovic F. Dumée

    2016-09-01

    Full Text Available The fabrication of molecular gas sieving materials with specific affinities for a single gas species and able to store large quantities of materials at a low or atmospheric pressure is desperately required to reduce the adverse effects of coal and oil usage in carbon capture. Fundamental understanding of the dynamic adsorption of gas, the diffusion mechanisms across thin film membranes, and the impact of interfaces play a vital role in developing these materials. In this work, single gas permeation tests across micro-porous membrane materials, based on metal organic framework crystals grown on the surface of carbon nanotubes (ZiF-8@CNT, were performed for the first time in-situ at the Australian Synchrotron on the small angle X-ray scattering beamline in order to reveal molecular sieving mechanisms and gas adsorption within the material. The results show that specific chemi-sorption of CO2 across the ZiF-8 crystal lattices affected the morphology and unit cell parameters, while the sieving of other noble or noble like gases across the ZiF-8@CNT membranes was found to largely follow Knudsen diffusion. This work demonstrates for the first time a novel and effective technique to assess molecular diffusion at the nano-scale across sub-nano-porous materials by probing molecular flexibility across crystal lattice and single cell units.

  17. 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.

  18. Chemical crystallography with pulsed neutrons and synchrotron x-rays

    International Nuclear Information System (INIS)

    Carrondo, M.A.; Jeffrey, G.A.

    1988-01-01

    Solid-state chemists and physicists, crystallographers and molecular biologists who are using or who plan to use the special properties of pulsed neutron spallation and synchrotron X-ray sources will find this book invaluable. Those scientists who have not yet gained experience in working with such sources will find the basic physics of the radiations, their production and their scattering properties explained, together with descriptions of the different types of diffraction experiments which use them

  19. Calcified-tissue investigations using synchrotron x-ray microscopy

    International Nuclear Information System (INIS)

    Jones, K.W.; Spanne, P.; Schidlovsky, G.; Dejun, X.; Bockman, R.S.; Hammond, P.B.; Bornschein, R.L.; Hoeltzel, D.A.

    1990-10-01

    Synchrotron x-ray microscopy (SXRM) in both emission and absorption modes has been used to examine elemental distributions in specimens of rat tibia, human deciduous teeth, and an orthopedic implant phantom. The work was performed with a spatial resolution of 8 μm for the emission work and 25 μm for the absorption work. The results illustrate the usefulness of SXRM for measurements of different types of calcified tissue. 3 figs

  20. Small-angle X-ray scattering study of the influence of solvent replacement (from H2O to D2O) on the initial crystallization stage of tetragonal lysozyme

    Science.gov (United States)

    Boikova, A. S.; D'yakova, Yu. A.; Il'ina, K. B.; Konarev, P. V.; Kryukova, A. E.; Marchenkova, M. A.; Blagov, A. E.; Pisarevskii, Yu. V.; Koval'chuk, M. V.

    2017-11-01

    The composition of lysozyme solutions in D2O under conditions favorable for the formation of tetragonal crystals has been investigated at different protein concentrations by small-angle X-ray scattering using the synchrotron radiation. In addition to lysozyme monomers, dimeric and octameric species are found in the crystallization solutions; the octamer content increases with an increase in the protein concentration. A comparison of the data with those obtained under similar conditions but with H2O used as a solvent has shown that the replacement of light water with heavy one leads to increase of octamer volume fraction in solution.

  1. Mesoscopic structures of triglyceride nanosuspensions studied by small-angle X-ray and neutron scattering and computer simulations.

    Science.gov (United States)

    Schmiele, Martin; Schindler, Torben; Westermann, Martin; Steiniger, Frank; Radulescu, Aurel; Kriele, Armin; Gilles, Ralph; Unruh, Tobias

    2014-07-24

    Aqueous suspensions of platelet-like shaped tripalmitin nanocrystals are studied here at high tripalmitin concentrations (10 wt % tripalmitin) for the first time by a combination of small-angle X-ray and neutron scattering (SAXS and SANS). The suspensions are stabilized by different lecithins, namely, DLPC, DOPC, and the lecithin blend S100. At such high concentrations the platelets start to self-assemble in stacks, which causes interference maxima at low Q-values in the SAXS and SANS patterns, respectively. It is found that the stack-related interference maxima are more pronounced for the suspension stabilized with DOPC and in particular DLPC, compared to suspensions stabilized by S100. By use of the X-ray and neutron powder pattern simulation analysis (XNPPSA), the SAXS and SANS patterns of the native tripalmitin suspensions could only be reproduced simultaneously when assuming the presence of both isolated nanocrystals and stacks of nanocrystals of different size in the simulation model of the dispersions. By a fit of the simulated SAXS and SANS patterns to the experimental data, a distribution of the stack sizes and their volume fractions is determined. The volume fraction of stacklike platelet assemblies is found to rise from 70% for S100-stabilized suspensions to almost 100% for the DLPC-stabilized suspensions. The distribution of the platelet thicknesses could be determined with molecular resolution from a combined analysis of the SAXS and SANS patterns of the corresponding diluted tripalmitin (3 wt %) suspensions. In accordance with microcalorimetric data, it could be concluded that the platelets in the suspensions stabilized with DOPC, and in particular DLPC, are significantly thinner than those stabilized with S100. The DLPC-stabilized suspensions exhibit a significantly narrower platelet thickness distribution compared to DOPC- and S100-stabilized suspensions. The smaller thicknesses for the DLPC- and DOPC-stabilized platelets explain their higher

  2. 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

  3. 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.

  4. In situ anomalous small-angle X-ray scattering studies of platinum nanoparticle fuel cell electrocatalyst degradation.

    Science.gov (United States)

    Gilbert, James A; Kariuki, Nancy N; Subbaraman, Ram; Kropf, A Jeremy; Smith, Matt C; Holby, Edward F; Morgan, Dane; Myers, Deborah J

    2012-09-12

    Polymer electrolyte fuel cells (PEFCs) are a promising high-efficiency energy conversion technology, but their cost-effective implementation, especially for automotive power, has been hindered by degradation of the electrochemically active surface area (ECA) of the Pt nanoparticle electrocatalysts. While numerous studies using ex situ post-mortem techniques have provided insight into the effect of operating conditions on ECA loss, the governing mechanisms and underlying processes are not fully understood. Toward the goal of elucidating the electrocatalyst degradation mechanisms, we have followed Pt nanoparticle growth during potential cycling of the electrocatalyst in an aqueous acidic environment using in situ anomalous small-angle X-ray scattering (ASAXS). ASAXS patterns were analyzed to obtain particle size distributions (PSDs) of the Pt nanoparticle electrocatalysts at periodic intervals during the potential cycling. Oxide coverages reached under the applied potential cycling protocols were both calculated and determined experimentally. Changes in the PSD, mean diameter, and geometric surface area identify the mechanism behind Pt nanoparticle coarsening in an aqueous environment. Over the first 80 potential cycles, the dominant Pt surface area loss mechanism when cycling to 1.0-1.1 V was found to be preferential dissolution or loss of the smallest particles with varying extents of reprecipitation of the dissolved species onto existing particles, resulting in particle growth, depending on potential profile. Correlation of ASAXS-determined particle growth with both calculated and voltammetrically determined oxide coverages demonstrates that the oxide coverage is playing a key role in the dissolution process and in the corresponding growth of the mean Pt nanoparticle size and loss of ECA. This understanding potentially reduces the complex changes in PSD and ECA resulting from various voltage profiles to a response dependent on oxide coverage.

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

    Energy Technology Data Exchange (ETDEWEB)

    Bagge-Hansen, M. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Lauderbach, L. M. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Hodgin, R. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Bastea, S. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Fried, L. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Jones, A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); van Buuren, T. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Hansen, D. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Benterou, J. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); May, C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Graber, T. [Washington State Univ., Pullman, WA (United States); Jensen, B. J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Ilavsky, J. [Argonne National Lab. (ANL), Argonne, IL (United States); Willey, T. M. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2015-06-24

    The dynamics of carboncondensation in detonating high explosives remains controversial. Detonation model validation requires data for processes occurring at nanometer length scales on time scales ranging from nanoseconds to microseconds. A new detonation endstation has been commissioned to acquire and provide time-resolved small-angle x-ray scattering (SAXS) from detonating explosives. Hexanitrostilbene (HNS) was selected as the first to investigate due to its ease of initiation using exploding foils and flyers, vacuum compatibility, high thermal stability, and stoichiometric carbon abundance that produces high carbon condensate yields. The SAXS data during detonation, collected with 300 ns time resolution, provide unprecedented signal fidelity over a broad q-range. This fidelity permits the first analysis of both the Guinier and Porod/power-law regions of the scattering profile during detonation, which contains information about the size and morphology of the resultant carbon condensate nanoparticles. To bolster confidence in these data, the scattering angle and intensity were additionally cross-referenced with a separate, highly calibrated SAXS beamline. The data show that HNS produces carbon particles with a radius of gyration of 2.7 nm in less than 400 ns after the detonation front has passed, and this size and morphology are constant over the next several microseconds. These data directly contradict previous pioneering work on RDX/TNT mixtures and TATB, where observations indicate significant particle growth (50% or more) continues over several microseconds. As a result, the power-law slope is about –3, which is consistent with a complex disordered, irregular, or folded sp2 sub-arrangement within a relatively monodisperse structure possessing radius of gyration of 2.7 nm after the detonation of HNS.

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

    Science.gov (United States)

    Doutch, James; Gilbert, Elliot P

    2013-01-02

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

  7. Small-angle x-ray scattering of calpain-5 reveals a highly open conformation among calpains

    Science.gov (United States)

    Gakhar, Lokesh; Bassuk, Alexander G.; Velez, Gabriel; Khan, Saif; Yang, Jing; Tsang, Stephen H.; Mahajan, Vinit B.

    2016-01-01

    Calpain-5 is a calcium-activated protease expressed in the retina. Mutations in calpain-5 cause autosomal dominant neovascular inflammatory vitreoretinopathy (ADNIV, OMIM#193235). The structure of calpain-5 has not been determined, thus hindering the investigation of its proteolytic targets and pathological role in ADNIV. Herein, we report models of the proteolytic core of calpain-5 (mini-calpain-5) containing two globular domains (termed DIIa-IIb) connected by a short, flexible linker, consistent with small-angle x-ray scattering (SAXS) data. Structural modeling in the absence of calcium suggests that mini-calpain-5 adopts a more open conformation when compared to previously determined structures of other calpain cores. This open conformation, achieved by a rotation of DIIa and DIIb with respect to each other, prevents formation of the active site and constrains the enzyme in an inactivated form. The relative domain rotation of 60-100°we found for mini-calpain-5 (a non-classical calpain) is significantly greater than the largest rotation previously observed for a classical calpain (i.e., 55.0°for mini-calpain-9). Together with our prediction that, in the full-length form, a long loop in DIIb (loop C1), a few residues downstream of the inter-domain linker, likely interacts with the shorter, acidic, inactivating loop on domain-III (DIII), these structural insights illuminate the complexity of calpain regulation. Moreover, our studies argue that pursuing higher resolution structural studies are necessary to understand the complex activity regulation prevalent in the calpain family and for the design of specific calpain inhibitors. PMID:27474374

  8. EXPRESSION, PURIFICATION, AND SMALL ANGLE X-RAY SCATTERING OF DNA REPLICATION AND REPAIR PROTEINS FROM THE HYPERTHERMOPHILE SULFOLOBUS SOLFATARICUS

    Energy Technology Data Exchange (ETDEWEB)

    Patterson, S.M.; Hatherill, J.R.; Hammel, M.; Hura, G.L.; Tainer, J.A.; Yannone, S.M.

    2008-01-01

    Vital molecular processes such as DNA replication, transcription, translation, and maintenance occur through transient protein interactions. Elucidating the mechanisms by which these protein complexes and interactions function could lead to treatments for diseases related to DNA damage and cell division control. In the recent decades since its introduction as a third domain, Archaea have shown to be simpler models for complicated eukaryotic processes such as DNA replication, repair, transcription, and translation. Sulfolobus solfataricus is one such model organism. A hyperthermophile with an optimal growth temperature of 80°C, Sulfolobus protein-protein complexes and transient protein interactions should be more stable at moderate temperatures, providing a means to isolate and study their structure and function. Here we provide the initial steps towards characterizing three DNA-related Sulfolobus proteins with small angle X-ray scattering (SAXS): Sso0257, a cell division control and origin recognition complex homolog, Sso0768, the small subunit of the replication factor C, and Sso3167, a Mut-T like protein. SAXS analysis was performed at multiple concentrations for both short and long exposure times. The Sso0257 sample was determined to be either a mixture of monomeric and dimeric states or a population of dynamic monomers in various conformational states in solution, consistent with a fl exible winged helix domain. Sso0768 was found to be a complex mixture of multimeric states in solution. Finally, molecular envelope reconstruction from SAXS data for Sso3167 revealed a novel structural component which may function as a disordered to ordered region in the presence of its substrates and/or protein partners.

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

    Energy Technology Data Exchange (ETDEWEB)

    Pessen, H.; Kumosinski, T.F.; Farrell, H.M. Jr.; Brumberger, H. (Dept. of Agriculture, Eastern Regional Research Center, Philadelphia, PA (USA))

    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.

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

    Science.gov (United States)

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

    2018-04-11

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

  11. A New Insight into Growth Mechanism and Kinetics of Mesoporous Silica Nanoparticles by in Situ Small Angle X-ray Scattering.

    Science.gov (United States)

    Yi, Zhifeng; Dumée, Ludovic F; Garvey, Christopher J; Feng, Chunfang; She, Fenghua; Rookes, James E; Mudie, Stephen; Cahill, David M; Kong, Lingxue

    2015-08-04

    The growth mechanism and kinetics of mesoporous silica nanoparticles (MSNs) were investigated for the first time by using a synchrotron time-resolved small-angle X-ray scattering (SAXS) analysis. The synchrotron SAXS offers unsurpassed time resolution and the ability to detect structural changes of nanometer sized objects, which are beneficial for the understanding of the growth mechanism of small MSNs (∼20 nm). The Porod invariant was used to quantify the conversion of tetraethyl orthosilicate (TEOS) in silica during MSN formation, and the growth kinetics were investigated at different solution pH and temperature through calculating the scattering invariant as a function of reaction time. The growth of MSNs was found to be accelerated at high temperature and high pH, resulting in a higher rate of silica formation. Modeling SAXS data of micelles, where a well-defined electrostatic interaction is assumed, determines the size and shape of hexadecyltrimethylammonium bromide (CTAB) micelles before and after the addition of TEOS. The results suggested that the micelle size increases and the micelle shape changes from ellipsoid to spherical, which might be attributed to the solubilization of TEOS in the hydrophobic core of CTAB micelles. A new "swelling-shrinking" mechanism is proposed. The mechanism provides new insights into understanding MSN growth for the formation of functional mesoporous materials exhibiting controlled morphologies. The SAXS analyses were correlated to the structure of CTAB micelles and chemical reaction of TEOS. This study has provided critical information to an understanding of the growth kinetics and mechanism of MSNs.

  12. K-Edge Subtraction Angiography with Synchrotron X-Rays

    CERN Document Server

    Giacomini, J C

    1996-01-01

    The purpose of this project was to utilize dual energy, monochromatic X-rays produced from synchrotrons radiation in order to obtain noninvasive medical imaging. The application of synchrotrons radiation to medical imaging is based on the principle of iodine dichromography, first described by Bertil Jacobson of the Karolinska Institute in 1953. Medical imaging using synchrotrons radiation and K-edge dichromography was pioneered at Stanford University under the leadership of Dr. Ed Rubenstein, and the late Nobel Laureate in Physics, Dr. Robert Hofstadter. With progressive refinements in hardware, clinical-quality images were obtained of human coronary arteries utilizing peripheral injections of iodinated contrast agent. These images even now are far superior to those being presented by investigators using MRI as an imaging tool for coronary arteries. However, new supplies and instruments in the cardiac catheterization laboratory have served to transform coronary angiography into an outpatient procedure, with r...

  13. A multiple CCD X-ray detector and its first operation with synchrotron radiation X-ray beam

    International Nuclear Information System (INIS)

    Suzuki, Masayo; Yamamoto, Masaki; Kumasaka, Takashi; Sato, Kazumichi; Toyokawa, Hidenori; Aries, Ian F.; Jerram, Paul A.; Ueki, Tatzuo

    1999-01-01

    A 4x4 array structure of 16 identical CCD X-ray detector modules, called the multiple CCD X-ray detector system (MCCDX), was submitted to its first synchrotron radiation experiment at the protein crystallography station of the RIKEN beamline (BL45XU) at the SPring-8 facility. An X-ray diffraction pattern of cholesterol powder was specifically taken in order to investigate the overall system performance

  14. A multiple CCD X-ray detector and its first operation with synchrotron radiation X-ray beam

    CERN Document Server

    Suzuki, M; Kumasaka, T; Sato, K; Toyokawa, H; Aries, I F; Jerram, P A; Ueki, T

    1999-01-01

    A 4x4 array structure of 16 identical CCD X-ray detector modules, called the multiple CCD X-ray detector system (MCCDX), was submitted to its first synchrotron radiation experiment at the protein crystallography station of the RIKEN beamline (BL45XU) at the SPring-8 facility. An X-ray diffraction pattern of cholesterol powder was specifically taken in order to investigate the overall system performance.

  15. Internal structures of thermosensitive hybrid microgels investigated by means of small-angle X-ray scattering.

    Science.gov (United States)

    Suzuki, Daisuke; Nagase, Yasuhisa; Kureha, Takuma; Sato, Takaaki

    2014-02-27

    Internal structures of thermosensitive microgels and their hybrid counterparts that contain Au nanoparticles are investigated by means of small-angle X-ray scattering (SAXS). Thermosensitive cationic microgels were synthesized by aqueous free radical precipitation polymerization from N-isopropylacrylamide and 3-(methacrylamino) propyltrimethylammonium chloride used as monomers. Using the microgels as templates, Au nanoparticles were synthesized in situ, using the cationic sites in the microgel to nucleate particle growth. To obtain different types of the hybrid microgels, Au nanoparticles were synthesized in the presence of the microgels by changing the reduction conditions of the precursor ions, such as temperature and species of reducing reagent. The hybrid microgels were characterized mainly by TEM and SAXS. For SAXS investigation, the hybrid microgels were analyzed in the wide q-range of 0.07 nm(-1) < q < 20 nm(-1), where q is the magnitude of the scattering vector. A quantitative description of the scattering intensities, I(q), for the nonhybrid microgels requires a sum of five components having different physical origins. An upturn increase of the forward intensity originates from the interface of microgels, obeying the Porod law, I(q) ∝ q(-4). An additional Guinier term found in q < 0.2 nm(-1) seems to arise from solidlike density fluctuation due to the inhomogeneities of chemical cross-links. The power-law behavior manifested in the low- to intermediate-q range is directly linked with the fractal nature of the swollen (coil) polymer networks and well described by the Ornstein-Zernike equation. Two interference peaks centered at q ≈ 5 nm (-1) and q ≈ 15 nm(-1) are likely to reflect inter- and intrachain correlations of pNIPAm, respectively, which are formally fitted by pseudo-Voigt equations. As for the hybrid microgels, a pronounced new contribution from the Au nanoparticles emerges, which calls for an additional scattering component describing

  16. Direct Evidence of Confined Water in Room-Temperature Ionic Liquids by Complementary Use of Small-Angle X-ray and Neutron Scattering.

    Science.gov (United States)

    Abe, Hiroshi; Takekiyo, Takahiro; Shigemi, Machiko; Yoshimura, Yukihiro; Tsuge, Shu; Hanasaki, Tomonori; Ohishi, Kazuki; Takata, Shinichi; Suzuki, Jun-Ichi

    2014-04-03

    The direct evidence of confined water ("water pocket") inside hydrophilic room-temperature ionic liquids (RTILs) was obtained by complementary use of small-angle X-ray scattering and small-angle neutron scattering (SAXS and SANS). A large contrast in X-ray and neutron scattering cross-section of deuterons was used to distinguish the water pocket from the RTIL. In addition to nanoheterogeneity of pure RTILs, the water pocket formed in the water-rich region. Both water concentration and temperature dependence of the peaks in SANS profiles confirmed the existence of the hidden water pocket. The size of the water pocket was estimated to be ∼3 nm, and D2O aggregations were well-simulated on the basis of the observed SANS data.

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

    Energy Technology Data Exchange (ETDEWEB)

    Babushkina, T. A.; Klimova, T. P. [Russian Academy of Sciences, Nesmeyanov Institute of Organoelement Compounds (Russian Federation); Shtykova, E. V.; Dembo, K. A.; Volkov, V. V. [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation); Khripunov, A. K. [Russian Academy of Sciences, Institute of Macromolecular Compounds (Russian Federation); Klechkovskaya, V. V., E-mail: klechvv@ns.crys.ras.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2010-03-15

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

  18. Study of moire fringes using synchrotron X-rays

    International Nuclear Information System (INIS)

    Yoshimura, Jun-ichi

    1992-01-01

    It has recently been shown that X-ray moire fringes are not exactly the projection of the intensity distribution of the wave field on the exit surface of the crystal, but do oscillate along the beam path behind the crystal. Such nonprojectiveness of moire fringes is inexplicable by the conventional understanding of moire fringes, and therefore is of interest from a fundamental viewpoint as well as practical one. In this paper the phenomena of the nonprojectiveness are described on the basis of the latest experimental data obtained by synchrotron radiation. (author)

  19. Oxides neutron and synchrotron X-ray diffraction studies

    CERN Document Server

    Sosnowska, I M

    1999-01-01

    We review some results from several areas of oxide science in which neutron scattering and X-ray synchrotron scattering exercise a complementary role to high-resolution transmission electron microscopy. The very high-resolution time-of-flight neutron diffraction technique and its role in studies of the magnetic structure of oxides is especially reviewed. The selected topics of structural studies for the chosen oxides are: crystal and magnetic structure of the so-called cellular random systems, magnetic structure and phase transitions in ferrites and the behaviour of water in non-stoichiometric protonic conductors and in the opal silica-water system. (40 refs).

  20. Synchrotron X-ray diffraction using triple-axis spectrometry

    International Nuclear Information System (INIS)

    Als-Nielsen, J.

    1980-12-01

    High resolution X-ray diffraction studies of (i) monolayers of the noble gases Kr and Ar physiosorbed on graphite (ii) smectic A fluctuations in the nematic and the smectic A phases of liquid crystals are described. The apparatus used is a triple axis spectrometer situated at the storage ring DORIS at Hasylab, DESY, Hamburg. A monochromatic, well collimated beam is extracted from the synchrotron radiation spectrum by Bragg reflection from perfect Si or Ge crystals. The direction of the beam scattered from the sample is determined by Bragg reflection from a perfect Si or Ge crystal. High intensities even with resolution extending beyond the wavelength of visible light can be obtained. (Auth.)

  1. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Lavisse, L.; Jouvard, J.-M.; Girault, M.; Potin, V.; Andrzejewski, H.; Marco de Lucas, M. C.; Bourgeois, S. [Laboratoire Interdisciplinaire Carnot de Bourgogne (ICB), UMR 6303 CNRS-Universite de Bourgogne, 9 Avenue A. Savary, BP 47870-21078 Dijon Cedex (France); Le Garrec, J.-L.; Carles, S.; Mitchell, J. B. A. [Institut de Physique de Rennes, UMR 6251 CNRS-Universite de Rennes 1, 35042 Rennes Cedex (France); Hallo, L. [CEA CESTA, 15 Avenue des Sablieres CS 60001, 33116 Le Barp Cedex (France); Perez, J. [Synchrotron SOLEIL, L' Orme des Merisiers, Saint-Aubin, F-91192 Gif-sur-Yvette Cedex (France); Decloux, J. [Kaluti System, Optique et Laser, Centre Scientifique d' Orsay, 91400 Orsay (France)

    2012-04-16

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

  3. Microstructure of amorphous-silicon-based solar cell materials by small-angle x-ray scattering. Annual subcontract report, 6 April 1994--5 April 1995

    Energy Technology Data Exchange (ETDEWEB)

    Williamson, D.L. [Colorado School of Mines, Golden, CO (United States)

    1995-08-01

    The general objective of this research is to provide detailed microstructural information on the amorphous-silicon-based, thin-film materials under development for improved multijunction solar cells. The experimental technique used is small-angle x-ray scattering (SAXS) providing microstructural data on microvoid fractions, sizes, shapes, and their preferred orientations. Other microstructural features such as alloy segregation, hydrogen-rich clusters and alloy short-range order are probed.

  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. Precise stress measurements with white synchrotron x rays

    International Nuclear Information System (INIS)

    Weidner, Donald J.; Vaughan, Michael T.; Wang Liping; Long, Hongbo; Li Li; Dixon, Nathaniel A.; Durham, William B.

    2010-01-01

    In situ measurement of stress in polycrystalline samples forms the basis for studies of the mechanical properties of materials with very broad earth science and materials science applications. Synchrotron x rays have been used to define the local elastic strain in these samples, which in turn define stress. Experimental work to date has been carried out on a prototype detection system that provided a strain measurement precision >10 -4 , which corresponds to a stress resolution >50 MPa for silicate minerals. Here we report operation of a new, permanent, energy dispersive detection system for white radiation, which has been developed at the National Synchrotron Light Source. The new system provides differential strain measurements with a precision of 3x10 -5 for volumes that are 50x50x500 μm 3 . This gives a stress precision of about 10 MPa for silicate minerals.

  6. Probing deformation substructure by synchrotron X-ray diffraction and dislocation dynamics modelling.

    Science.gov (United States)

    Korsunsky, Alexander M; Hofmann, Felix; Song, Xu; Eve, Sophie; Collins, Steve P

    2010-09-01

    Materials characterization at the nano-scale is motivated by the desire to resolve the structural aspects and deformation behavior at length scales relevant to those mechanisms that define the novel and unusual properties of nano-structured materials. A range of novel techniques has recently become accessible with the help of synchrotron X-ray beams that can be focused down to spot sizes of less than a few microns on the sample. The unique combination of tunability (energy selection), parallelism and brightness of synchrotron X-ray beams allows their use for high resolution diffraction (determination of crystal structure and transformations, analysis of dislocation sub-structures, orientation and texture analysis, strain mapping); small angle X-ray scattering (analysis of nano-scale voids and defects; orientation analysis) and imaging (radiography and tomography). After a brief review of the state-of-the-art capabilities for monochromatic and white beam synchrotron diffraction, we consider the usefulness of these techniques for the task of bridging the gap between experiment and modeling. Namely, we discuss how the experiments can be configured to provide information relevant to the validation and improvement of modeling approaches, and also how the results of various simulations can be post-processed to improve the possibility of (more or less) direct comparison with experiments. Using the example of some recent experiments carried out on beamline 116 at Diamond Light Source near Oxford, we discuss how such experimental results can be interpreted in view and in conjunction with numerical deformation models, particularly those incorporating dislocation effects, e.g., finite-element based pseudo-continuum strain gradient formulations, and discrete dislocation simulations. Post-processing of FE and discrete dislocation simulations is described, illustrating the kind of information that can be extracted from comparisons between modeling and experimental data.

  7. Structural and magnetic properties of inverse opal photonic crystals studied by x-ray diffraction, scanning electron microscopy, and small-angle neutron scattering

    NARCIS (Netherlands)

    Grigoriev, S.V.; Napolskii, K.S.; Grigoryeva, N.A.; Vasilieva, A.V.; Mistonov, A.A.; Chernyshov, D.Y.; Petukhov, A.V.; Belov, D.V.; Eliseev, A.A.; Lukashin, A.V.; Tretyakov, Y.D.; Sinitskii, A.S.; Eckerlebe, H.

    2009-01-01

    The structural and magnetic properties of nickel inverse opal photonic crystal have been studied by complementary experimental techniques, including scanning electron microscopy, wide-angle and small-angle diffraction of synchrotron radiation, and polarized neutrons. The sample was fabricated by

  8. Application of X-rays and Synchrotron X Rays to Residual Stress Evaluation Near Surfaces

    International Nuclear Information System (INIS)

    Pyzalla, Anke

    1999-01-01

    A nondestructive residual stress analysis can be performed using diffraction methods. The easiest accessible radiation is characteristic X radiation that has a penetration depth of ∼10 microm suitable for the determination of the residual stresses in near-surface layers. Special techniques have been developed, e.g., with respect to in situ analyses of the stress state in oxide layers and the residual stress analysis in coarse grained zones of steel welds or annealed Ni-base alloys. Depending on the size of the gauge volume, neutron diffraction can provide information at depths of tens of millimetres of steel and many tens of millimetres of Al. An alternative to the use of the characteristic synchrotron radiation is the use of a high-energy polychromatic beam in an energy dispersive arrangement, which gives access to higher penetration depths at still gauge volumes as small as 100 microm x 100 microm x 1 mm in steel rods of 15-mm diameter. The combination of neutrons with conventional X rays and monochromatic and polychromatic synchrotron radiation allows for a comprehensive investigation of the phase composition, the texture, and the residual stresses

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

    Czech Academy of Sciences Publication Activity Database

    Kontro, I.; Svedström, K.; Duša, Filip; Ahvenainen, P.; Ruokonen, S. K.; Witos, J.; Wiedmer, S. K.

    2016-01-01

    Roč. 201, DEC (2016), s. 59-66 ISSN 0009-3084 Institutional support: RVO:68081715 Keywords : phospholipids * x-ray scattering Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.361, year: 2016

  10. Synchrotron X-ray tomographic microscopy of fossil embryos.

    Science.gov (United States)

    Donoghue, Philip C J; Bengtson, Stefan; Dong, Xi-ping; Gostling, Neil J; Huldtgren, Therese; Cunningham, John A; Yin, Chongyu; Yue, Zhao; Peng, Fan; Stampanoni, Marco

    2006-08-10

    Fossilized embryos from the late Neoproterozoic and earliest Phanerozoic have caused much excitement because they preserve the earliest stages of embryology of animals that represent the initial diversification of metazoans. However, the potential of this material has not been fully realized because of reliance on traditional, non-destructive methods that allow analysis of exposed surfaces only, and destructive methods that preserve only a single two-dimensional view of the interior of the specimen. Here, we have applied synchrotron-radiation X-ray tomographic microscopy (SRXTM), obtaining complete three-dimensional recordings at submicrometre resolution. The embryos are preserved by early diagenetic impregnation and encrustation with calcium phosphate, and differences in X-ray attenuation provide information about the distribution of these two diagenetic phases. Three-dimensional visualization of blastomere arrangement and diagenetic cement in cleavage embryos resolves outstanding questions about their nature, including the identity of the columnar blastomeres. The anterior and posterior anatomy of embryos of the bilaterian worm-like Markuelia confirms its position as a scalidophoran, providing new insights into body-plan assembly among constituent phyla. The structure of the developing germ band in another bilaterian, Pseudooides, indicates a unique mode of germ-band development. SRXTM provides a method of non-invasive analysis that rivals the resolution achieved even by destructive methods, probing the very limits of fossilization and providing insight into embryology during the emergence of metazoan phyla.

  11. 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.

  12. Microfocussing of synchrotron X-rays using X-ray refractive lens ...

    Indian Academy of Sciences (India)

    2014-07-02

    Jul 2, 2014 ... ring (black) is fixed from polyimide side and (g) finally the metal substrate is etched to prepare the X-ray mask. standardized for the present X-ray lithography beamline. X-ray exposures are carried out in 3–10 keV region selected using two X-ray mirrors kept at grazing incidence angles. The total power ...

  13. Microfocussing of synchrotron X-rays using X-ray refractive lens

    Indian Academy of Sciences (India)

    X-ray lenses are fabricated in polymethyl methacrylate using deep X-ray lithography beamline of Indus-2. The focussing performance of these lenses is evaluated using Indus-2 and Diamond Light Source Ltd. The process steps for the fabrication of X-ray lenses and microfocussing at 10 keV at moderate and low emittance ...

  14. Microfocussing of synchrotron X-rays using X-ray refractive lens ...

    Indian Academy of Sciences (India)

    2014-07-02

    Jul 2, 2014 ... Abstract. X-ray lenses are fabricated in polymethyl methacrylate using deep X-ray lithography beamline of Indus-2. The focussing performance of these lenses is evaluated using Indus-2 and Dia- mond Light Source Ltd. The process steps for the fabrication of X-ray lenses and microfocussing at 10 keV at ...

  15. Microfocussing of synchrotron X-rays using X-ray refractive lens ...

    Indian Academy of Sciences (India)

    X-ray lenses are fabricated in polymethyl methacrylate using deep X-ray lithography beamline of Indus-2. The focussing performance of these lenses is evaluated using Indus-2 and Diamond Light Source Ltd. The process steps for the fabrication of X-ray lenses and microfocussing at 10 keV at moderate and low emittance ...

  16. GENFIT: software for the analysis of small-angle X-ray and neutron scattering data of macro-molecules in solution.

    Science.gov (United States)

    Spinozzi, Francesco; Ferrero, Claudio; Ortore, Maria Grazia; De Maria Antolinos, Alejandro; Mariani, Paolo

    2014-06-01

    Many research topics in the fields of condensed matter and the life sciences are based on small-angle X-ray and neutron scattering techniques. With the current rapid progress in source brilliance and detector technology, high data fluxes of ever-increasing quality are produced. In order to exploit such a huge quantity of data and richness of information, wider and more sophisticated approaches to data analysis are needed. Presented here is GENFIT , a new software tool able to fit small-angle scattering data of randomly oriented macromolecular or nanosized systems according to a wide list of models, including form and structure factors. Batches of curves can be analysed simultaneously in terms of common fitting parameters or by expressing the model parameters via physical or phenomenological link functions. The models can also be combined, enabling the user to describe complex heterogeneous systems.

  17. X-ray and neutron small-angle scattering analysis of the complex formed by the Met receptor and the Listeria monocytogenes invasion protein InlB.

    Science.gov (United States)

    Niemann, Hartmut H; Petoukhov, Maxim V; Härtlein, Michael; Moulin, Martine; Gherardi, Ermanno; Timmins, Peter; Heinz, Dirk W; Svergun, Dmitri I

    2008-03-21

    The Listeria monocytogenes surface protein InlB binds to the extracellular domain of the human receptor tyrosine kinase Met, the product of the c-met proto-oncogene. InlB binding activates the Met receptor, leading to uptake of Listeria into normally nonphagocytic host cells. The N-terminal half of InlB (InlB(321)) is sufficient for Met binding and activation. The complex between this Met-binding domain of InlB and various constructs of the Met ectodomain was characterized by size exclusion chromatography and dynamic light scattering, and structural models were built using small-angle X-ray scattering and small-angle neutron scattering. Although most receptor tyrosine kinase ligands induce receptor dimerization, InlB(321) consistently binds the Met ectodomain with a 1:1 stoichiometry. A construct comprising the Sema and PSI domains of Met, although sufficient to bind the physiological Met ligand hepatocyte growth factor/scatter factor, does not form a complex with InlB(321) in solution, highlighting the importance of Met Ig domains for InlB binding. Small-angle X-ray scattering and small-angle neutron scattering measurements of ligand and receptor, both free and in complex, reveal an elongated shape for the receptor. The four Ig domains form a bent, rather than a fully extended, conformation, and InlB(321) binds to Sema and the first Ig domain of Met, in agreement with the recent crystal structure of a smaller Met fragment in complex with InlB(321). These results call into question whether receptor dimerization is the basic underlying event in InlB(321)-mediated Met activation and demonstrate differences in the mechanisms by which the physiological ligand hepatocyte growth factor/scatter factor and InlB(321) bind and activate the Met receptor.

  18. Synchrotron x-ray sources and new opportunities in the soil and environmental sciences

    Energy Technology Data Exchange (ETDEWEB)

    Schulze, D. (Purdue Univ., Lafayette, IN (USA)); Anderson, S. (Michigan State Univ., East Lansing, MI (USA)); Mattigod, S. (Pacific Northwest Lab., Richland, WA (USA))

    1990-07-01

    This report contains the following papers: characteristics of the advanced photon source and comparison with existing synchrotron facilities; x-ray absorption spectroscopy: EXAFS and XANES -- A versatile tool to study the atomic and electronic structure of materials; applications of x-ray spectroscopy and anomalous scattering experiments in the soil and environmental sciences; X-ray fluorescence microprobe and microtomography.

  19. X-ray and synchrotron methods in studies of cultural heritage sites

    Science.gov (United States)

    Koval'chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.; Tereshchenko, E. Yu.; Prosekov, P. A.; Dyakova, Yu. A.

    2016-09-01

    X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.

  20. X-ray and synchrotron methods in studies of cultural heritage sites

    International Nuclear Information System (INIS)

    Koval’chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.; Tereshchenko, E. Yu.; Prosekov, P. A.; Dyakova, Yu. A.

    2016-01-01

    X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.

  1. X-ray and synchrotron methods in studies of cultural heritage sites

    Energy Technology Data Exchange (ETDEWEB)

    Koval’chuk, M. V.; Yatsishina, E. B.; Blagov, A. E.; Tereshchenko, E. Yu., E-mail: elenatereschenko@yandex.ru; Prosekov, P. A.; Dyakova, Yu. A. [National Research Centre “Kurchatov Institute” (Russian Federation)

    2016-09-15

    X-ray and synchrotron methods that are most widely used in studies of cultural heritage objects (including archaeological sites)—X-ray diffraction analysis, X-ray spectroscopy, and visualization techniques— have been considered. The reported examples show high efficiency and informativeness of natural science studies when solving most diverse problems of archaeology, history, the study of art, museology, etc.

  2. Synchrotron x-ray sources and new opportunities in the soil and environmental sciences

    International Nuclear Information System (INIS)

    Schulze, D.; Anderson, S.; Mattigod, S.

    1990-07-01

    This report contains the following papers: characteristics of the advanced photon source and comparison with existing synchrotron facilities; x-ray absorption spectroscopy: EXAFS and XANES -- A versatile tool to study the atomic and electronic structure of materials; applications of x-ray spectroscopy and anomalous scattering experiments in the soil and environmental sciences; X-ray fluorescence microprobe and microtomography

  3. White Beam, X-Ray, Energy-Dispersive Diffractometry using Synchrotron Radiation

    DEFF Research Database (Denmark)

    Gerward, Leif; Buras, B.; Olsen, J. Staun

    1978-01-01

    The special features of left double quote white right double quote beam X-ray energy-dispersive diffractometry using synchrotron radiation are discussed on the basis of experiments performed at the Deutsches Electronen-Synchrotron, DESY.......The special features of left double quote white right double quote beam X-ray energy-dispersive diffractometry using synchrotron radiation are discussed on the basis of experiments performed at the Deutsches Electronen-Synchrotron, DESY....

  4. Utilization of synchrotron radiation in analytical chemistry. Soft X-ray emission and absorption spectroscopy

    International Nuclear Information System (INIS)

    Muramatsu, Yasuji

    2015-01-01

    Synchrotron soft X-ray spectroscopy includes three major types of spectroscopy such as X-ray absorption spectroscopy (XAS), X-ray emission spectroscopy (XES), and X-ray photoelectron spectroscopy (XPS). This paper takes up XAS and XES of soft X-rays, and briefly describes the principle. XAS is roughly classified into XANES (X-ray absorption near-edge structure) and EXAFS (extended X-ray absorption fine structure), and XANES is mainly used in the analysis based on XAS of soft X-rays. As the examples of the latest soft X-ray analyses, the following are introduced: (1) bandgap of boron implantation diamond and the local structure of boron, (2) catalytic sites in solid fuel cell carbon electrode, and (3) soft X-ray analysis under atmospheric pressure. (A.O.)

  5. Structure of PEP-PEO block copolymer micelles: Exploiting the complementarity of small-angle X-ray scattering and static light scattering

    DEFF Research Database (Denmark)

    Jensen, Grethe Vestergaard; Shi, Qing; Hernansanz, María J.

    2011-01-01

    . The present work shows that the same information can be obtained by combining static light scattering (SLS) and small-angle X-ray scattering (SAXS), which provide information on, respectively, large and short length scales. Micelles of a series of block copolymers of poly(ethylene propylene)-b-poly(ethylene...... oxide) (PEP-PEO) in a 70% ethanol solution are investigated. The polymers have identical PEP blocks of 5.0 kDa and varying PEO blocks of 2.8-49 kDa. The SLS contrasts of PEP and PEO are similar, providing a homogeneous contrast, making SLS ideal for determining the overall micelle morphology. The SAXS...

  6. Salt Dependence of the Radius of Gyration and Flexibility of Single-stranded DNA in Solution probed by Small-angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Sim, Adelene Y.L.; Lipfert, Jan; Herschlag, Daniel; Doniach, Sebastian

    2012-07-06

    Short single-stranded nucleic acids are ubiquitous in biological processes and understanding their physical properties provides insights to nucleic acid folding and dynamics. We used small angle x-ray scattering to study 8-100 residue homopolymeric single-stranded DNAs in solution, without external forces or labeling probes. Poly-T's structural ensemble changes with increasing ionic strength in a manner consistent with a polyelectrolyte persistence length theory that accounts for molecular flexibility. For any number of residues, poly-A is consistently more elongated than poly-T, likely due to the tendency of A residues to form stronger base-stacking interactions than T residues.

  7. Actinide science with soft x-ray synchrotron radiation

    International Nuclear Information System (INIS)

    Shuh, D.

    2002-01-01

    Several workshops, some dating back more than fifteen years, recognised both the potential scientific impact and opportunities that would be made available by the capability to investigate actinide materials in the vacuum ultraviolet (VUV)/soft X-ray region of the synchrotron radiation (SR) spectrum. This spectral region revolutionized the approach to surface materials chemistry and physics nearly two decades ego. The actinide science community was unable to capitalize on these SR methodologies for the study of actinide materials until recently because of radiological safety concerns. ,The Advanced Light Source (ALS) at LBNL is a third-generation light source providing state-of-the-art performance in the VUV/soft X-ray region. Along with corresponding improvements in detector and vacuum technology, the ALS has rendered experiments with small amounts of actinide materials possible. In particular, it has been the emergence and development of micro-spectroscopic techniques that have enabled investigations of actinide materials at the ALS. The primary methods for the experimental investigation of actinide materials in the VUV/soft X-ray region are the complementary photoelectron spectroscopies, near-edge X-ray absorption fine structure (NEXAFS) and X-ray emission spectroscopy (XES) techniques. Resonant photo-emission is capable of resolving the 5f electron contributions to actinide bonding and can be used to characterise the electronic structure of actinide materials. This technique is clearly a most important methodology afforded by the tunable SR source. Core level and valence band photoelectron spectroscopies are valuable for the characterisation of the electronic properties of actinide materials, as well as for general analytical purposes. High-resolution core-level photo-emission and resonant photo-emission measurements from the a (monoclinic) and δ (FCC) allotropic phases of plutonium metal have been collected on beam line 7.0 at the ALS and the spectra show

  8. 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).

  9. Trace element characterization using a synchrotron radiation X-ray microprobe

    OpenAIRE

    早川, 慎二郎

    1996-01-01

    A scanning X-ray microprobe using synchrotron radiation was developed employing an X-ray focusing system with total reflection mirrors. Utilizing a Wolter mirror system, a hard X-ray microbeam was first realized. With an energy tunable X-ray microprobe, sensitivity in X-ray fluorescence (XRF) analysis can be optimized for the element of interest at less than 1 ppm in relative concentration. Moreover, small area X-ray absorption fine structure (XAFS) measurements with XRF detection can provide...

  10. Geoscience Applications of Synchrotron X-ray Computed Microtomography

    Science.gov (United States)

    Rivers, M. L.

    2009-05-01

    Computed microtomography is the extension to micron spatial resolution of the CAT scanning technique developed for medical imaging. Synchrotron sources are ideal for the method, since they provide a monochromatic, parallel beam with high intensity. High energy storage rings such as the Advanced Photon Source at Argonne National Laboratory produce x-rays with high energy, high brilliance, and high coherence. All of these factors combine to produce an extremely powerful imaging tool for earth science research. Techniques that have been developed include: - Absorption and phase contrast computed tomography with spatial resolution approaching one micron - Differential contrast computed tomography, imaging above and below the absorption edge of a particular element - High-pressure tomography, imaging inside a pressure cell at pressures above 10GPa - High speed radiography, with 100 microsecond temporal resolution - Fluorescence tomography, imaging the 3-D distribution of elements present at ppm concentrations. - Radiographic strain measurements during deformation at high confining pressure, combined with precise x- ray diffraction measurements to determine stress. These techniques have been applied to important problems in earth and environmental sciences, including: - The 3-D distribution of aqueous and organic liquids in porous media, with applications in contaminated groundwater and petroleum recovery. - The kinetics of bubble formation in magma chambers, which control explosive volcanism. - Accurate crystal size distributions in volcanic systems, important for understanding the evolution of magma chambers. - The equation-of-state of amorphous materials at high pressure using both direct measurements of volume as a function of pressure and also by measuring the change x-ray absorption coefficient as a function of pressure. - The formation of frost flowers on Arctic sea-ice, which is important in controlling the atmospheric chemistry of mercury. - The distribution of

  11. Novel Melt-Spun Polymer-Optical Poly(methyl methacrylate Fibers Studied by Small-Angle X-ray Scattering

    Directory of Open Access Journals (Sweden)

    Markus Beckers

    2017-02-01

    Full Text Available The structural properties of novel melt-spun polymer optical fibers (POFs are investigated by small-angle X-ray scattering. The amorphous PMMA POFs were subjected to a rapid cooling in a water quench right after extrusion in order to obtain a radial refractive index profile. Four fiber samples were investigated with small-angle X-ray scattering (SAXS. The resulting distance-distribution functions obtained from the respective equatorial and meridional SAXS data exhibit a real-space correlation peak indicative of periodic cross-sectional and axial variations in the scattering density contrast. Simple model calculations demonstrate how the structural information contained particularly in the equatorial distance distribution function can be interpreted. The respective results are qualitatively verified for one of the fiber samples by comparison of the model curve with the measured SAXS data. Eventually, the study confirms that the cross-sectional variation of the (scattering- density is the main reason for the formation of radial refractive-index profiles in the POFs.

  12. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  14. K-Edge Subtraction Angiography with Synchrotron X-Rays

    International Nuclear Information System (INIS)

    Giacomini, John C.

    1996-01-01

    The purpose of this project was to utilize dual energy, monochromatic X-rays produced from synchrotrons radiation in order to obtain noninvasive medical imaging. The application of synchrotrons radiation to medical imaging is based on the principle of iodine dichromography, first described by Bertil Jacobson of the Karolinska Institute in 1953. Medical imaging using synchrotrons radiation and K-edge dichromography was pioneered at Stanford University under the leadership of Dr. Ed Rubenstein, and the late Nobel Laureate in Physics, Dr. Robert Hofstadter. With progressive refinements in hardware, clinical-quality images were obtained of human coronary arteries utilizing peripheral injections of iodinated contrast agent. These images even now are far superior to those being presented by investigators using MRI as an imaging tool for coronary arteries. However, new supplies and instruments in the cardiac catheterization laboratory have served to transform coronary angiography into an outpatient procedure, with relatively little morbidity. We extended the principles learned with coronary angiography to noninvasive imaging of the human bronchial tree. For these images, we utilized xenon as the contrast agent, as it has a K-edge very similar to that of iodine. In this case, there is no true competing diagnostic test, and pulmonary neoplasm is an enormous public health concern. In early experiments, we demonstrated remarkably clear images of the human bronchial tree. These images have been shown internationally; however, funding difficulties primarily with the Department of Energy have not allowed for progression of this promising avenue of research. One potential criticism of the project is that in order to obtain these images, we utilized national laboratories. Some have questioned whether this would lead to a practical imaging modality. However, we have shown that the technology exists to allow for construction of a miniature storage ring, with a superconducting

  15. A modular reactor design for in situ synchrotron x-ray investigation of atomic layer deposition processes

    Science.gov (United States)

    Klug, Jeffrey A.; Weimer, Matthew S.; Emery, Jonathan D.; Yanguas-Gil, Angel; Seifert, Sönke; Schlepütz, Christian M.; Martinson, Alex B. F.; Elam, Jeffrey W.; Hock, Adam S.; Proslier, Thomas

    2015-11-01

    Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present in situ results for (1) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, (2) grazing-incidence small angle scattering of MnO nucleation on silicon, and (3) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er2O3 ALD on amorphous ALD alumina and single crystalline sapphire.

  16. 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.

  17. SAXSANA: an interactive program for the analysis and monitoring of static and time-resolved small-angle X-ray solution scattering measurements.

    Science.gov (United States)

    Hiragi, Yuzuru; Sano, Yoh; Matsumoto, Tomoharu

    2003-03-01

    An interactive analytical program, SAXSANA, for small-angle X-ray scattering measurements of solutions is described. The program processes scattered data without disciplined knowledge of small-angle scattering. SAXSANA also assists in finding the best experimental conditions, thus avoiding blind runs of experiments. SAXSANA consists of the following procedures: (i) determination of the centre of scattered X-rays and moment transfer Q (Q = 4pisintheta/lambda, where 2theta is the scattering angle and lambda is the wavelength) for each measured channel; (ii) conversion of the data format to the format of Q versus scattered intensities J(Q); (iii) truncation of unnecessary data and smoothing of scattering curves by cubic-spline function; (iv) correction of the absorption effect and subtraction of the scattered intensity of the buffer (solvent) solution from that of the sample solution; (v) creation of a data file for a three-dimensional representation of time-resolved scattering curves; (vi) determination of radii of gyration by Guinier plots; (vii) determination of persistent lengths by Kratky plots; (viii) extrapolation of the small-angle part by Guinier plots; (ix) extrapolation of the wide-angle part by Porod's & Luzzati's laws for the Hankel transformation in order to obtain the distance distribution function p(r); (x) calculation of p(r) and computation of the invariant, the chord length, the Volume, the spherical radius, the maximum dimension D(max) and the radius of gyration (Rg). SAXSANA also serves as an on-site monitor for the validity of an experimental result during the measurements.

  18. Soft X-ray diffractometer for synchrotron radiation

    CERN Document Server

    Gau, T S; Liu, K Y; Chung, C H; Chen, C K; Lai, S C; Shu, C H; Huang, Y S; Chao, C H; Lee, Y R; Chen, C T; Chang, S L

    2001-01-01

    An ultra-high vacuum soft X-ray diffractometer has been constructed and commissioned at the Synchrotron Radiation Research Center (SRRC) to investigate materials structures in mesoscale. The diffractometer, housed in a UHV tank, consists of a 6-circle goniometer, together with the systems for beam-collimation, signal detection, vacuum, and control panels. The kappa-phi (cursive,open) Greek-psi goniostat is adopted for the sample orientation. Crystal samples can be rotated along a given reciprocal lattice vector by using psi scan. Two orthogonal axes, gamma (or 2 theta) and delta, are used to move the detector. The detector is a semiconductor pin diode, which can be used in UHV ambient. This 6-circle goniometer allows for sample scanning of a wide range in the momentum space. The motors used for goniometer rotation and slit selection are UHV compatible. The UHV tank is placed on an XYZ table capable of positioning the center of the goniometer onto the incident beam. Test experiments have been carried on the 1-...

  19. Synchrotron radiation X-ray powder diffraction techniques applied in hydrogen storage materials - A review

    OpenAIRE

    Honghui Cheng; Chen Lu; Jingjing Liu; Yongke Yan; Xingbo Han; Huiming Jin; Yu Wang; Yi Liu; Changle Wu

    2017-01-01

    Synchrotron radiation is an advanced collimated light source with high intensity. It has particular advantages in structural characterization of materials on the atomic or molecular scale. Synchrotron radiation X-ray powder diffraction (SR-XRPD) has been successfully exploited to various areas of hydrogen storage materials. In the paper, we will give a brief introduction on hydrogen storage materials, X-ray powder diffraction (XRPD), and synchrotron radiation light source. The applications of...

  20. Small-Angle X-ray and Neutron Scattering Study on Microphase Separation Induced by Non-Solvent in a Semi-Dilute Solution of an Ultra-High-Molecular-Weight Block Copolymer

    International Nuclear Information System (INIS)

    Okamoto, Shigeru

    2009-01-01

    Full text: A block copolymer consists of immiscible different polymers covalently connected to each other and form micro domain structures such as lamellae, cylinders, spheres, gyroids, etc of the size of their own molecular size. Utilization of an ultra-high-molecular-weight block copolymer enables us to create micro domains on the order of several hundred nanometers. However, such large molecules have high viscosity due to the large number of entanglements per chain. Therefore the structures usually contain a lot of defects or distortion and are far from the equilibrated state. Here, We found a very interesting phenomenon that a microphase separation is induced by addition of a non-solvent into a semi dilute solution of an ultra-high-molecular-weight block copolymer. The solvent mixture of the common solvent and the non-solvent act as a highly selective solvent and are selectively introduced into one phase of the phase-separated state. We investigated the structures by the small-angle x-ray scattering (SAXS) technique using synchrotron radiation and the small-angle neutron scattering (SANS) technique. The results showed that micro domain structures were highly ordered and the grain size was gigantic because block copolymers in a semi dilute solution has high mobility due to the dilution effect by solvents. The SANS results showed there was not the composition fluctuation of constituent different solvent molecules in both phases. In other words, the results means the common good solvent was also selectively introduced into one phase. (author)

  1. Microbial biofilm study by synchrotron X-ray microscopy

    International Nuclear Information System (INIS)

    Pennafirme, S.; Lima, I.; Bitencourt, J.A.; Crapez, M.A.C.; Lopes, R.T.

    2015-01-01

    Microbial biofilm has already being used to remove metals and other pollutants from wastewater. In this sense, our proposal was to isolate and cultivate bacteria consortia from mangrove’s sediment resistant to Zn (II) and Cu (II) at 50 mg L −1 and to observe, through synchrotron X-ray fluorescence microscopy (microXRF), whether the biofilm sequestered the metal. The biofilm area analyzed was 1 mm 2 and a 2D map was generated (pixel size 20×20 μm 2 , counting time 5 s/point). The biofilm formation and retention followed the sequence Zn>Cu. Bacterial consortium zinc resistant formed dense biofilm and retained 63.83% of zinc, while the bacterial consortium copper resistant retained 3.21% of copper, with lower biofilm formation. Dehydrogenase activity of Zn resistant bacterial consortium was not negatively affect by 50 mg ml −1 zinc input, whereas copper resistant bacterial consortium showed a significant decrease on dehydrogenase activity (50 mg mL −1 of Cu input). In conclusion, biofilm may protect bacterial cells, acting as barrier against metal toxicity. The bacterial consortia Zn resistant, composed by Nitratireductor spp. and Pseudomonas spp formed dense biofilm and sequestered metal from water, decreasing the metal bioavailability. These bacterial consortia can be used in bioreactors and in bioremediation programs. - Highlights: • We studied bacterial bioremediation by microXRF. • Dense biofilm may act sequestering metal while protecting bacterial metabolism. • Nitratireductor spp. and Pseudomonas spp decreased seawater metal bioavailability. • Bacterial consortia from polluted areas may be used in bioremediation programs.

  2. 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.

  3. 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......-dimensional data in terms of the indirect Fourier transform using the objective Bayesian approach to obtain the pair-distance distribution function, PDDF, and is thereby a free and open-source alternative to existing PDDF estimation software. Apart from the TIFF input format, the program also accepts ASCII...

  4. Chaperone-client interactions between Hsp21 and client proteins monitored in solution by small angle X-ray scattering and captured by crosslinking mass spectrometry

    DEFF Research Database (Denmark)

    Rutsdottir, Gudrun; I Rasmussen, Morten; Hojrup, Peter

    2018-01-01

    and six inwardly-facing. Here, we investigated the interactions between Hsp21 and thermosensitive model substrate client proteins in solution, by small-angle X-ray scattering (SAXS) and crosslinking mass spectrometry. The chaperone-client complexes were monitored and the Rg-values were found to increase......The small heat shock protein (sHsp) chaperones are important for stress survival, yet the molecular details of how they interact with client proteins are not understood. All sHsps share a folded middle domain to which is appended flexible N- and C-terminal regions varying in length and sequence...... continuously during 20 min at 45°, which could reflect binding of partially unfolded clients to the flexible N-terminal arms of the Hsp21 dodecamer. No such increase in Rg-values was observed with a mutational variant of Hsp21, which is mainly dimeric and has reduced chaperone activity. Crosslinking data...

  5. 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

  6. Solution structure of variant H2A.Z.1 nucleosome investigated by small-angle X-ray and neutron scatterings.

    Science.gov (United States)

    Sugiyama, Masaaki; Horikoshi, Naoki; Suzuki, Yuya; Taguchi, Hiroyuki; Kujirai, Tomoya; Inoue, Rintaro; Oba, Yojiro; Sato, Nobuhiro; Martel, Anne; Porcar, Lionel; Kurumizaka, Hitoshi

    2015-12-01

    Solution structures of nucleosomes containing a human histone variant, H2A.Z.1, were measured by small-angle X-ray and neutron scatterings (SAXS and SANS). SAXS revealed that the outer shape, reflecting the DNA shape, of the H2A.Z.1 nucleosome is almost the same as that of the canonical H2A nucleosome. In contrast, SANS employing a contrast variation technique revealed that the histone octamer of the H2A.Z.1 nucleosome is smaller than that of the canonical nucleosome. The DNA within the H2A.Z.1 nucleosome was more susceptible to micrococcal nuclease than that within the canonical nucleosome. These results suggested that the DNA is loosely wrapped around the histone core in the H2A.Z.1 nucleosome.

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

    Science.gov (United States)

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

    2017-05-01

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

  8. Agglomeration and sintering in annealed FePt nanoparticle assemblies studied by small angle neutron scattering and x-ray diffraction

    International Nuclear Information System (INIS)

    Thomson, T.; Lee, S.L.; Oates, C.J.; Toney, M.F.; Dewhurst, C.D.; Ogrin, F.Y.; Sun, S.

    2005-01-01

    In this work we give a detailed account of complementary small angle neutron scattering and x-ray diffraction studies of polymer mediated, self-assembled FePt nanoparticle arrays as a function of annealing temperature. The combination of these two techniques provides significantly greater physical insight than is available using either individually. Since both methods integrate over a large number of particles statistically meaningful data can be obtained in contrast to imaging techniques where typically only small areas are analyzed. The data show that the median particle size increases with annealing at temperatures of 580 deg. C and above. The data also demonstrate that the distribution of particle diameters is significant and increases with annealing temperature. These results allow a comprehensive structural model of the annealed assemblies to be developed in terms of particle sintering and agglomeration. This enhanced understanding will allow new strategies to be pursued in realizing the potential of nanoparticle assemblies as a monodispersed data storage medium

  9. Agglomeration and Sintering in Annealed FePt Nanoparticle Assemblies Studied by Small Angle Neutron Scattering and X-Ray Diffraction

    International Nuclear Information System (INIS)

    Thomson, T.

    2005-01-01

    In this work we give a detailed account of the use of small angle neutron scattering to study the properties of polymer mediated, self assembled nanoparticle arrays as a function of annealing temperature. The results from neutron scattering are compared with those obtained from x-ray diffraction. Both techniques show that particle size increases with annealing temperatures of 580 C and above. They also show that the distribution of particle diameters is significant and increases with annealing temperature. The complementary nature of the two measurements allows a comprehensive structural model of the assemblies to be developed in terms of particle sintering and agglomeration. To realize the potential of nanoparticle assemblies as a monodispersed data storage medium the problem of particle separation necessary to avoid sintering and agglomeration during annealing must be addressed

  10. A small-angle X-ray scattering study of complexes formed in mixtures of a cationic polyelectrolyte and an anionic surfactant

    DEFF Research Database (Denmark)

    Bergström, M.; Kjellin, U.R.M.; Claesson, P.M.

    2002-01-01

    The internal structure of the solid phase formed in mixtures of the anionic surfactant sodium dodecyl sulfate (SDS) and a range of oppositely charged polyelectrolytes with different side chains and charge density has been investigated using small-angle X-ray scattering. Polyelectrolytes with short....... The hexagonal structure of MAPTAC is retained either when a neutral monomer (acrylamide, AM) is included in the polymer backbone to reduce the charge density or when a nonionic surfactant is admixed to the SDS/polyelctrolyte complex.. The unit cell length of AM-MAPTAC increases with decreasing charge density...... structure and the bilayers in the lamellar structure are based on self-assembled surfactant aggregates with the polyelectrolyte mainly located in the aqueous region adjacent to the charged surfactant headgroups....

  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; 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.

  12. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Jeffries, J. R.; Hammons, J. A.; Willey, T. M.; Wall, M. A.; Ruddle, D.; Ilavsky, J.; Allen, P. G.; van Buuren, T.

    2018-01-01

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

  14. In situ small-angle X-ray scattering observations of Pt/NaY catalysts during processing: sintering of Pt

    Energy Technology Data Exchange (ETDEWEB)

    Brumberger, H. [Syracuse Univ., NY (United States). Dept. of Chemistry; Goodisman, J. [Syracuse Univ., NY (United States). Dept. of Chemistry; Ramaya, R. [Syracuse Univ., NY (United States). Dept. of Chemistry; Ciccariello, S. [Padua Univ. (Italy). Dipt. di Fisica

    1996-10-01

    Small-angle X-ray scattering observations on Pt/NaY catalysts, made in situ during calcination and reduction stages of processing, demonstrate the usefulness of this technique in following morphological changes. Observations show that the same platinum species (Pt{sup 0} under the preparation conditions used) is present in the early stages of calcination, carried out at relatively high heating rates, as after reduction, and that the ultimate dispersity of the metal is already reached within 0.5 h of the start of calcination. Increasing aggregation of metal particles occurs at calcination temperatures higher than 573 K, leading to average particle sizes too large to fit the supercages of the zeolite framework. With the assumption that the metal is a Maxwellian distribution of spheres, values of the distribution parameters giving the best fit to the scattering for each catalyst sample are found; from these parameters, average particle radii are calculated. (orig.).

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

    Science.gov (United States)

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

    2012-11-28

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

  16. UV-Visible Absorption Spectroscopy Enhanced X-ray Crystallography at Synchrotron and X-ray Free Electron Laser Sources.

    Science.gov (United States)

    Cohen, Aina E; Doukov, Tzanko; Soltis, Michael S

    2016-01-01

    This review describes the use of single crystal UV-Visible Absorption micro-Spectrophotometry (UV-Vis AS) to enhance the design and execution of X-ray crystallography experiments for structural investigations of reaction intermediates of redox active and photosensitive proteins. Considerations for UV-Vis AS measurements at the synchrotron and associated instrumentation are described. UV-Vis AS is useful to verify the intermediate state of an enzyme and to monitor the progression of reactions within crystals. Radiation induced redox changes within protein crystals may be monitored to devise effective diffraction data collection strategies. An overview of the specific effects of radiation damage on macromolecular crystals is presented along with data collection strategies that minimize these effects by combining data from multiple crystals used at the synchrotron and with the X-ray free electron laser.

  17. 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.

  18. 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

    International Nuclear Information System (INIS)

    Viani, Alberto; Sotiriadis, Konstantinos; Len, Adél; Šašek, Petr; Ševčík, Radek

    2016-01-01

    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.

  19. 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.

  20. Scanning soft x-ray microscopy with a fresnel zoneplate at the National Synchrotron Light Source

    International Nuclear Information System (INIS)

    Kenney, J.M.; Kirz, J.; Rarback, H.; Feder, R.; Sayre, D.; Howells, M.

    1983-01-01

    We have built a scanning transmission soft x-ray microscope located at the National Synchrotron Light Source (NSLS). Images of biological specimens have been formed with submicron resolution. A Fresnel zoneplate serves as the focusing element

  1. Recent trends of X-ray detectors in synchrotron radiation science

    CERN Document Server

    Suzuki, M

    2003-01-01

    This article attempts to describe the recent trends of X-ray detectors in synchrotron radiation science in the light of not only the advance but also the stagnation of which are seriously dependent upon the current semiconductor technology. (author)

  2. Time-resolved materials science opportunities using synchrotron x-ray sources

    International Nuclear Information System (INIS)

    Larson, B.C.; Tischler, J.Z.

    1995-06-01

    The high brightness, high intensity, and pulsed time-structure of synchrotron sources provide new opportunities for time-resolved x-ray diffraction investigations. With third generation synchrotron sources coming on line, high brilliance and high brightness are now available in x-ray beams with the highest flux. In addition to the high average flux, the instantaneous flux available in synchrotron beams is greatly enhanced by the pulsed time structure, which consists of short bursts of x-rays that are separated by ∼tens to hundreds of nanoseconds. Time-resolved one- and two-dimensional position sensitive detection techniques that take advantage of synchrotron radiation for materials science x-ray diffraction investigations are presented, and time resolved materials science applications are discussed in terms of recent diffraction and spectroscopy results and materials research opportunities

  3. Report of the workshop on transferring X-ray Lithography Synchrotron (XLS) technology to industry

    Energy Technology Data Exchange (ETDEWEB)

    Marcuse, W.

    1987-01-01

    This paper reports on plans to develop an x-ray synchrotron for use in lithography. The primary concern of the present paper is technology transfer from national laboratories to private industry. (JDH)

  4. Iron overload of human colon adenocarcinoma cells studied by synchrotron-based X-ray techniques

    NARCIS (Netherlands)

    Mihucz, Victor G.; Meirer, Florian; Polgári, Zsófia; Réti, Andrea; Pepponi, Giancarlo; Ingerle, Dieter; Szoboszlai, Norbert; Streli, Christina

    2016-01-01

    Fast- and slow-proliferating human adenocarcinoma colorectal cells, HT-29 and HCA-7, respectively, overloaded with transferrin (Tf), Fe(III) citrate, Fe(III) chloride and Fe(II) sulfate were studied by synchrotron radiation total-reflection X-ray spectrometry (TXRF), TXRF-X-ray absorption near edge

  5. Antiferroelectric surface layers in a liquid crystal as observed by synchrotron x-ray scattering

    DEFF Research Database (Denmark)

    Gramsbergen, E. F.; de Jeu, W. H.; Als-Nielsen, Jens Aage

    1986-01-01

    The X-ray reflectivity form the surface of a liquid crystal with terminally polar (cyano substituted) molecules has been studied using a high-resolution triple-axis X-ray spectrometer in combination with a synchrotron source. It is demonstrated that at the surface of the smectic Al phase a few...

  6. 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.

  7. Solution structure of human plasma fibronectin using small-angle X-ray and neutron scattering at physiological pH and ionic strength

    International Nuclear Information System (INIS)

    Sjoeberg, B.P.; Pap, S.; Osterlund, E.; Osterlund, K.; Vuento, M.; Kjems, J.

    1987-01-01

    Human plasma fibronectin has been investigated at physiological pH and ionic strength, by using small-angle X-ray and neutron scattering techniques. The results indicate that the molecule is disc shaped with an axial ratio of about 1:10. In fact, an ellipsoid of revolution with semiaxes a = 1.44 nm and b = c = 13.8 nm is in agreement with the experimental scattering data, and can also fully explain the rather extreme hydrodynamic parameters reported for fibronectin. The X-ray data gave a radius of gyration of 8.9 nm and a molecular weight of 510,000, whereas the neutron data gave slightly larger values, 9.5 nm and 530,000, respectively. From the volume of the best fitting ellipsoid we obtain a degree of hydration of 0.61 g H 2 O/g protein (dry weight). Neutron data, recorded at different D 2 O concentrations in the solvent, gave a match point of 43% D 2 O, which indicates that approximately 80% of the hydrogens bound to oxygen and nitrogen are exchangeable

  8. 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.

  9. 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.

  10. X-ray spectrometry with synchrotron radiation; Roentgenspektrometrie mit Synchrotronstrahlung

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, Matthias [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany). Arbeitsgruppe ' Roentgen- und IR-Spektrometrie' ; Gerlach, Martin; Holfelder, Ina; Hoenicke, Philipp; Lubeck, Janin; Nutsch, Andreas; Pollakowski, Beatrix; Streeck, Cornelia; Unterumsberger, Rainer; Weser, Jan; Beckhoff, Burkhard

    2014-12-15

    The X-ray spectrometry of the PTB at the BESSY II storage ring with radiation in the range from 78 eV to 10.5 keV is described. After a description of the instrumentation development reference-sample free X-ray fluorescence analysis, the determination of fundamental atomic parameters, X-ray fluorescence analysis under glance-angle incidence, highly-resolving absorption spectrometry, and emission spectrometry are considered. Finally liquid cells and in-situ measurement techniques are described. (HSI)

  11. Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera

    Energy Technology Data Exchange (ETDEWEB)

    Fittschen, Ursula Elisabeth Adriane, E-mail: ursula.fittschen@chemie.uni-hamburg.de [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Menzel, Magnus [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Scharf, Oliver [IfG Institute for Scientific Instruments GmbH, Berlin (Germany); Radtke, Martin; Reinholz, Uwe; Buzanich, Günther [BAM Federal Institute of Materials Research and Testing, Berlin (Germany); Lopez, Velma M.; McIntosh, Kathryn [Los Alamos National Laboratory, Los Alamos, NM (United States); Streli, Christina [Atominstitut, TU Wien, Vienna (Austria); Havrilla, George Joseph [Los Alamos National Laboratory, Los Alamos, NM (United States)

    2014-09-01

    Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by “drop on demand” technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation. - Highlights: • Use of a color X-ray camera and drop on demand printing to diagnose X-ray shading • Specimens were obtained uniform and well-defined in shape and concentration by printing. • Direct visualization and determination of shading in such specimens using the camera.

  12. The capability of measuring cross-sectional profile for hole patterns in nanoimprint templates using small-angle x-ray scattering

    Science.gov (United States)

    Hagihara, Kazuki; Taniguchi, Rikiya; Yamanaka, Eiji; Omote, Kazuhiko; Ito, Yoshiyasu; Ogata, Kiyoshi; Hayashi, Naoya

    2017-07-01

    Nanoimprint lithography (NIL) is one of the highest potential candidates for next generation lithography in semiconductors. NIL is very useful technology for pattern fabrication in high resolution compared to conventional optical lithography. NIL technology makes use of replication from quartz templates. The cross-sectional profile of the template is directly transferred to the resist profile on a wafer. Accordingly, the management of the cross-sectional profile on the template pattern is much more important than on each photomask. In our previous report, we had studied the performance of measuring cross-sectional profiles using grazing-incidence small-angle X-ray scattering (GISAXS). GISAXS has made it possible to analyze the repeated nanostructure patterns with a 2D X-ray scattering pattern. After various researches, we found the application is very effective in the method of cross-sectional profiling of sub-20 nm half-pitch lines-and-spaces (LS) patterns. In this report, we investigated the capabilities of measuring cross-sectional profiles for hole patterns using GISAXS. Since the pattern density of hole patterns is much lower than that of LS patterns, the intensity of X-ray scattering in hole measurements is much lower. We optimized some measurement conditions to build the hole measurement system. Finally, the results suggested that 3D profile measurement of hole pattern using GISAXS has sufficient performance to manage the cross-sectional profile of template. The measurement system using GISAXS for measuring 3D profiles establishes the cross-sectional profile management essential for the production of high quality quartz hole templates.

  13. Synchrotron x-ray diffraction study of liquid surfaces

    DEFF Research Database (Denmark)

    Als-Nielsen, Jens Aage; Pershan, P.S.

    1983-01-01

    A spectrometer for X-ray diffraction and refraction studies of horizontal, free surfaces of liquids is described. As an illustration smetic-A layering at the surface of a liquid crystal is presented.......A spectrometer for X-ray diffraction and refraction studies of horizontal, free surfaces of liquids is described. As an illustration smetic-A layering at the surface of a liquid crystal is presented....

  14. Synchrotron radiation sources: their properties and applications for VUV and X-ray spectroscopy

    International Nuclear Information System (INIS)

    Koch, E.E.

    1976-09-01

    Synchrotron radiation from accelerators and storage rings offers far reaching possibilities for many fields of basic and applied physics. The properties of synchrotron radiation, existing and planned synchrotron radiation facilities, as well as instrumental aspects are discussed. In order to illustrate the usefulness of the synchrotron radiation sources a few highlights from atomic, molelucar, and solid state spectroscopy are presented and examples from x-ray experiments and from the field of applied physics are given. (orig.) [de

  15. Data and videos for ultrafast synchrotron X-ray imaging studies of metal solidification under ultrasound

    Directory of Open Access Journals (Sweden)

    Bing Wang

    2018-04-01

    Full Text Available The data presented in this article are related to the paper entitled ‘Ultrafast synchrotron X-ray imaging studies of microstructure fragmentation in solidification under ultrasound’ [Wang et al., Acta Mater. 144 (2018 505-515]. This data article provides further supporting information and analytical methods, including the data from both experimental and numerical simulation, as well as the Matlab code for processing the X-ray images. Six videos constructed from the processed synchrotron X-ray images are also provided.

  16. Total reflection X-ray fluorescence analysis of light elements with synchrotron radiation and special X-ray tubes

    International Nuclear Information System (INIS)

    Streli, C.; Wobrauschek, P.; Bauer, V.; Kregsamer, P.; Goergl, R.; Pianetta, P.; Ryon, R.; Pahlke, S.; Fabry, L.

    1997-01-01

    Total reflection X-ray fluorescence analysis (TXRF) of light elements, such as C, O and Al (atomic numbers 5-13) generally has poor sensitivity and detection limits due to poor excitation and low fluorescent yields. Special excitation sources are necessary to compensate for these physical limitations. Synchrotron radiation is the ideal source for TXRF due to its high intensity and wide spectral range extending into the low energy region required for light elements. For more routine use, special X-ray tubes can be constructed. Experiments have been performed at the Standford Synchrotron Radiation Laboratory (SSRL) using beamline III-4, which is specially designed for the sue of low energy photons. Light elements on Si wafers have been analyzed, leading to detection limits below 100 fg for Na, Mg and Al, which corresponds to about 10 9 atoms. A new vacuum chamber is introduced meeting the requirements of wafer handling without the risk of contamination and offering the possibility of scanning a certain area of the wafer. Boron was detected on a wafer with 10 14 atoms cm -2 implanted in the surface layer. A special windowless X-ray tube with Mo, Al and Si as anode materials was also tested. With the optimization of anode geometry, beam path and excitation conditions, a detection limit of 5 pg (corresponds to 10 11 atoms) for Al was achieved. (Author)

  17. Total reflection X-ray fluorescence analysis of light elements with synchrotron radiation and special X-ray tubes

    Energy Technology Data Exchange (ETDEWEB)

    Streli, C.; Wobrauschek, P.; Bauer, V.; Kregsamer, P.; Goergl, R. [Atominstitut der Oesterreichischen Universitaeten, Wien (Austria); Pianetta, P. [Stanford Synchrotron Radiation Lab. (Canada); Ryon, R. [Lawrence Livermore National Lab. CA (United States); Pahlke, S.; Fabry, L. [Wacker Siltronic AG, Burghausen (Germany)

    1997-06-20

    Total reflection X-ray fluorescence analysis (TXRF) of light elements, such as C, O and Al (atomic numbers 5-13) generally has poor sensitivity and detection limits due to poor excitation and low fluorescent yields. Special excitation sources are necessary to compensate for these physical limitations. Synchrotron radiation is the ideal source for TXRF due to its high intensity and wide spectral range extending into the low energy region required for light elements. For more routine use, special X-ray tubes can be constructed. Experiments have been performed at the Standford Synchrotron Radiation Laboratory (SSRL) using beamline III-4, which is specially designed for the sue of low energy photons. Light elements on Si wafers have been analyzed, leading to detection limits below 100 fg for Na, Mg and Al, which corresponds to about 10{sup 9}atoms. A new vacuum chamber is introduced meeting the requirements of wafer handling without the risk of contamination and offering the possibility of scanning a certain area of the wafer. Boron was detected on a wafer with 10{sup 14} atoms cm{sup -2} implanted in the surface layer. A special windowless X-ray tube with Mo, Al and Si as anode materials was also tested. With the optimization of anode geometry, beam path and excitation conditions, a detection limit of 5 pg (corresponds to 10{sup 11} atoms) for Al was achieved. (Author).

  18. Thermal management of next-generation contact-cooled synchrotron x-ray mirrors

    Energy Technology Data Exchange (ETDEWEB)

    Khounsary, A.

    1999-10-29

    In the past decade, several third-generation synchrotrons x-ray sources have been constructed and commissioned around the world. Many of the major problems in the development and design of the optical components capable of handling the extremely high heat loads of the generated x-ray beams have been resolved. It is expected, however, that in the next few years even more powerful x-ray beams will be produced at these facilities, for example, by increasing the particle beam current. In this paper, the design of a next generation of synchrotron x-ray mirrors is discussed. The author shows that the design of contact-cooled mirrors capable of handing x-ray beam heat fluxes in excess of 500 W/mm{sup 2} - or more than three times the present level - is well within reach, and the limiting factor is the thermal stress rather then thermally induced slope error.

  19. Combination of acoustic levitation with small angle scattering techniques and synchrotron radiation circular dichroism. Application to the study of protein solutions.

    Science.gov (United States)

    Cristiglio, Viviana; Grillo, Isabelle; Fomina, Margarita; Wien, Frank; Shalaev, Evgenyi; Novikov, Alexey; Brassamin, Séverine; Réfrégiers, Matthieu; Pérez, Javier; Hennet, Louis

    2017-01-01

    The acoustic levitation technique is a useful sample handling method for small solid and liquids samples, suspended in air by means of an ultrasonic field. This method was previously used at synchrotron sources for studying pharmaceutical liquids and protein solutions using x-ray diffraction and small angle x-ray scattering (SAXS). In this work we combined for the first time this containerless method with small angle neutron scattering (SANS) and synchrotron radiation circular dichroism (SRCD) to study the structural behavior of proteins in solutions during the water evaporation. SANS results are also compared with SAXS experiments. The aggregation behavior of 45μl droplets of lysozyme protein diluted in water was followed during the continuous increase of the sample concentration by evaporating the solvent. The evaporation kinetics was followed at different drying stage by SANS and SAXS with a good data quality. In a prospective work using SRCD, we also studied the evolution of the secondary structure of the myoglobin protein in water solution in the same evaporation conditions. Acoustic levitation was applied for the first time with SANS and the high performances of the used neutron instruments made it possible to monitor fast container-less reactions in situ. A preliminary work using SRCD shows the potentiality of its combination with acoustic levitation for studying the evolution of the protein structure with time. This multi-techniques approach could give novel insights into crystallization and self-assembly phenomena of biological compound with promising potential applications in pharmaceutical, food and cosmetics industry. This article is part of a Special Issue entitled "Science for Life" Guest Editor: Dr. Austen Angell, Dr. Salvatore Magazù and Dr. Federica Migliardo. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    Fukasawa, Toshiko; Sato, Takaaki

    2011-02-28

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

  1. Synchrotron X-ray studies of liquid-vapor interfaces

    DEFF Research Database (Denmark)

    Als-Nielsen, Jens Aage

    1986-01-01

    The density profile ρ(z) across a liquid-vapor interface may be determined by the reflectivity R(θ) of X-rays at grazing angle incidence θ. The relation between R(θ) and ρ(z) is discussed, and experimental examples illustrating thermal roughness of simple liquids and smectic layering of liquid...

  2. Report on the fifth workshop on synchrotron x ray lithography

    Science.gov (United States)

    Williams, G. P.; Godel, J. B.; Brown, G. S.; Liebmann, W.

    Semiconductors comprise a greater part of the United States economy than the aircraft, steel, and automobile industries combined. In future the semiconductor manufacturing industry will be forced to switch away from present optical manufacturing methods in the early to mid 1990s. X ray lithography has emerged as the leading contender for continuing production below the 0.4 micron level. Brookhaven National Laboratory began a series of workshops on x ray lithography in 1986 to examine key issues and in particular to enable United States industry to take advantage of the technical base established in this field. Since accelerators provide the brightest sources for x ray lithography, most of the research and development to date has taken place at large accelerator-based research centers such as Brookhaven, the University of Wisconsin, and Stanford. The goals of this Fifth Brookhaven Workshop were to review progress and goals since the last workshop and to establish a blueprint for the future. The meeting focused on the exposure tool, that is, a term defined as the source plus beamline and stepper. In order to assess the appropriateness of schedules for the development of this tool, other aspects of the required technology such as masks, resists and inspection and repair were also reviewed. To accomplish this, two working groups were set up, one to review the overall aspects of x ray lithography and set a time frame, the other to focus on sources.

  3. Synchrotron radiation X-ray microfluorescence techniques and ...

    Indian Academy of Sciences (India)

    raphy system was implemented to analyse human prostate and breast samples and an X-ray mi- crofluorescence system was .... at the lumbar vertebral body of Wistar rat which are trabecular regions with dimensions smaller than those found in human femora, as can be seen in figure 4. Similar behaviour. (a). (b). Figure 5.

  4. Small-angle X-ray scattering studies of the oligomeric state and quaternary structure of the trifunctional proline utilization A (PutA) flavoprotein from Escherichia coli.

    Science.gov (United States)

    Singh, Ranjan K; Larson, John D; Zhu, Weidong; Rambo, Robert P; Hura, Greg L; Becker, Donald F; Tanner, John J

    2011-12-16

    The trifunctional flavoprotein proline utilization A (PutA) links metabolism and gene regulation in Gram-negative bacteria by catalyzing the two-step oxidation of proline to glutamate and repressing transcription of the proline utilization regulon. Small-angle x-ray scattering (SAXS) and domain deletion analysis were used to obtain solution structural information for the 1320-residue PutA from Escherichia coli. Shape reconstructions show that PutA is a symmetric V-shaped dimer having dimensions of 205 × 85 × 55 Å. The particle consists of two large lobes connected by a 30-Å diameter cylinder. Domain deletion analysis shows that the N-terminal DNA-binding domain mediates dimerization. Rigid body modeling was performed using the crystal structure of the DNA-binding domain and a hybrid x-ray/homology model of residues 87-1113. The calculations suggest that the DNA-binding domain is located in the connecting cylinder, whereas residues 87-1113, which contain the two catalytic active sites, reside in the large lobes. The SAXS data and amino acid sequence analysis suggest that the Δ(1)-pyrroline-5-carboxylate dehydrogenase domains lack the conventional oligomerization flap, which is unprecedented for the aldehyde dehydrogenase superfamily. The data also provide insight into the function of the 200-residue C-terminal domain. It is proposed that this domain serves as a lid that covers the internal substrate channeling cavity, thus preventing escape of the catalytic intermediate into the bulk medium. Finally, the SAXS model is consistent with a cloaking mechanism of gene regulation whereby interaction of PutA with the membrane hides the DNA-binding surface from the put regulon thereby activating transcription.

  5. Small-angle X-ray Scattering Studies of the Oligomeric State and Quaternary Structure of the Trifunctional Proline Utilization A (PutA) Flavoprotein from Escherichia coli*

    Science.gov (United States)

    Singh, Ranjan K.; Larson, John D.; Zhu, Weidong; Rambo, Robert P.; Hura, Greg L.; Becker, Donald F.; Tanner, John J.

    2011-01-01

    The trifunctional flavoprotein proline utilization A (PutA) links metabolism and gene regulation in Gram-negative bacteria by catalyzing the two-step oxidation of proline to glutamate and repressing transcription of the proline utilization regulon. Small-angle x-ray scattering (SAXS) and domain deletion analysis were used to obtain solution structural information for the 1320-residue PutA from Escherichia coli. Shape reconstructions show that PutA is a symmetric V-shaped dimer having dimensions of 205 × 85 × 55 Å. The particle consists of two large lobes connected by a 30-Å diameter cylinder. Domain deletion analysis shows that the N-terminal DNA-binding domain mediates dimerization. Rigid body modeling was performed using the crystal structure of the DNA-binding domain and a hybrid x-ray/homology model of residues 87–1113. The calculations suggest that the DNA-binding domain is located in the connecting cylinder, whereas residues 87–1113, which contain the two catalytic active sites, reside in the large lobes. The SAXS data and amino acid sequence analysis suggest that the Δ1-pyrroline-5-carboxylate dehydrogenase domains lack the conventional oligomerization flap, which is unprecedented for the aldehyde dehydrogenase superfamily. The data also provide insight into the function of the 200-residue C-terminal domain. It is proposed that this domain serves as a lid that covers the internal substrate channeling cavity, thus preventing escape of the catalytic intermediate into the bulk medium. Finally, the SAXS model is consistent with a cloaking mechanism of gene regulation whereby interaction of PutA with the membrane hides the DNA-binding surface from the put regulon thereby activating transcription. PMID:22013066

  6. Analysis of InGaN nanodots grown by droplet heteroepitaxy using grazing incidence small-angle X-ray scattering and electron microscopy

    Science.gov (United States)

    Woodward, J. M.; Nikiforov, A. Yu.; Ludwig, K. F.; Moustakas, T. D.

    2017-08-01

    We present a detailed structural investigation of self-assembled indium gallium nitride nanodots grown on c-plane aluminum nitride templates by the droplet heteroepitaxy technique in a plasma-assisted molecular beam epitaxy reactor. Various growth parameters, including the total coverage of the metal species, relative and total metal effusion fluxes, and nitridation temperature were investigated. Analyses of in situ reflection high-energy electron diffraction patterns and comparison with simulations showed that the resulting crystal structure was a mixture of wurtzite and twinned zinc blende phases, with the zinc blende phase increasingly dominant for lower metal coverages and lower nitridation temperatures, and the wurtzite phase increasingly dominant for higher nitridation temperature. Studies by field emission scanning electron microscopy and atomic force microscopy revealed that the nanodots exhibit trimodal size distributions, with the dot morphologies of the intermediate size mode often resembling aggregations of distinct clusters. Nanodots grown at higher nitridation temperatures had larger inter-dot spacings, with hexagonal in-plane ordering observable at a sufficiently high temperature. Using grazing incidence small angle X-ray scattering, we determined the nanodots to be approximately truncated cone shaped, and extracted the mean radius, height, and inter-dot distance for each distribution. Microstructural investigations of the nanodots by cross-sectional transmission electron microscopy indicated that the majority of the dots were formed in dislocation-free regions, and confirmed that the intermediate size dots were approximately truncated cone shaped and consisted of both zinc blende and wurtzite regions. Mapping of the elemental distributions by energy dispersive X-ray spectroscopy in scanning transmission electron microscopy mode indicated highly nonuniform indium distributions within both small and intermediate size dots which are potentially

  7. Simulations of X-ray synchrotron beams using the EGS4 code system in medical applications

    International Nuclear Information System (INIS)

    Orion, I.; Henn, A.; Sagi, I.; Dilmanian, F.A.; Pena, L.; Rosenfeld, A.B.

    2001-01-01

    X-ray synchrotron beams are commonly used in biological and medical research. The availability of intense, polarized low-energy photons from the synchrotron beams provides a high dose transfer to biological materials. The EGS4 code system, which includes the photoelectron angular distribution, electron motion inside a magnetic field, and the LSCAT package, found to be the appropriate Monte Carlo code for synchrotron-produced X-ray simulations. The LSCAT package was developed in 1995 for the EGS4 code to contain the routines to simulate the linear polarization, the bound Compton, and the incoherent scattering functions. Three medical applications were demonstrated using the EGS4 Monte Carlo code as a proficient simulation code system for the synchrotron low-energy X-ray source. (orig.)

  8. 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.

  9. 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.

  10. 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.

  11. Dimyristoylphosphatidylcholine/C16 : 0-ceramide binary liposomes studied by differential scanning calorimetry and wide- and small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Holopainen, J. M.; Lemmich, Jesper; Richter, F.

    2000-01-01

    hysteresis in the thermal phase behavior of ceramide-containing membranes. A partial phase diagram was constructed based on results from a combination of these two methods. DSC heating scans show that with increased X-cer the pretransition temperature T-P first increases, whereafter at X-cer > 0.06 it can...... of the studied compositions there is an endotherm in the region close to the T-m for DMPC. At X-cer greater than or equal to 0.03 a second endotherm is evident at higher temperatures, starting at 32.1 degrees C and reaching 54.6 degrees C at X-cer = 0.30. X-ray small-angle reflection heating scans reveal...... a lamellar phase within the temperature range of 15-60 degrees C, regardless of composition. The pretransition is observed up to X-cer repeat distance d increases from similar to 61 Angstrom at X-cer = 0.03, to 67 Angstrom at X-cer = 0...

  12. The model resolution function - a technique for estimating the quality of approximation of particles by models in small-angle X-ray or neutron scattering

    International Nuclear Information System (INIS)

    Mueller, J.J.; Damaschun, G.; Schmidt, P.W.

    1985-01-01

    Although the quality of a structure model obtained from small-angle X-ray or neutron scattering curves for polymers can be determined qualitatively by comparing the isotropic scattering curve calculated for the model with the experimental scattering data for a solution of polymer molecules, other methods are needed for a more precise evaluation. A model resolution function has been defined to permit quantitative comparisons. With this function, the quality of the approximation can be assessed, and the structure resolution can be determined. An overinterpretation of scattering curves by use of complex but uniform-density models can thus be avoided. Furthermore, the value of the Porod volume calculated from the scattering data has been found to depend strongly on the interval in which the scattering data are recorded or selected for evaluation. The calculations with the atomic model curves showed that it is impossible to compute physically meaningful values of the hydration of the molecules from the Porod volume and the dry volume by use of extrapolated scattering curves with an insufficient resolution. The theory of the model resolution function and the interpretation of the Porod volume have been verified and tested with experimental scattering curves from solutions of RNA molecules. (orig.)

  13. 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.

  14. Small-Angle X-ray Scattering Study on Internal Microscopic Structures of Poly(N-isopropylacrylamide-co-tris(2,2'-bipyridyl))ruthenium(II) Complex Microgels.

    Science.gov (United States)

    Matsui, Shusuke; Kureha, Takuma; Nagase, Yasuhisa; Okeyoshi, Kosuke; Yoshida, Ryo; Sato, Takaaki; Suzuki, Daisuke

    2015-07-07

    Internal microscopic structures of poly(N-isopropylacrylamide-co-tris(2,2'-bipyridyl))ruthenium(II) complex microgels were investigated using small-angle X-ray scattering (SAXS) in the extended q-range of 0.07 ≤ q/nm(-1) ≤ 20. The microgels were prepared by aqueous free-radical precipitation polymerization, resulting in formation of monodispersed, submicrometer-sized microgels, which was confirmed by transmission electron microscopy and dynamic light scattering. To reveal the changes in the microscopic structures of the microgels during swelling/deswelling or dispersing/flocculating oscillation, the redox state of Ru(bpy)3 complexes was fixed in the microgels using Ce(IV) or Ce(III) ions under high ionic strength (1.5 M) during the SAXS measurements. The scattering intensity of the microgels manifested five different structural features. In particular, the correlation length (ξ), which was obtained from the fitting analysis using the Ornstein-Zernike equation, of the microgels both in the reduced and oxidized Ru(bpy)3 states exhibited divergent-like behavior. In addition, a low-q peak centered at q ≈ 5 nm(-1) did not appear clearly in both the reduced [Ru(bpy)3](2+) and oxidized [Ru(bpy)3](3+) states, indicating that the formation of a polymer-rich domain was suppressed; thus, Ru(bpy)3 complexes can be active even though the microgels are deswollen or flocculated during the oscillation reaction.

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

    Science.gov (United States)

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

    2015-12-01

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

  16. Evolution of Helium with Temperature in Neutron-Irradiated 10B-Doped Aluminum by Small-Angle X-Ray Scattering

    Directory of Open Access Journals (Sweden)

    Chaoqiang Huang

    2014-01-01

    Full Text Available Helium status is the primary effect of material properties under radiation. 10B-doped aluminum samples were prepared via arc melting technique and rapidly cooled with liquid nitrogen to increase the boron concentration during the formation of compounds. An accumulated helium concentration of ~6.2 × 1025 m−3 was obtained via reactor neutron irradiation with the reaction of 10B(n, α7Li. Temperature-stimulated helium evolution was observed via small-angle X-ray scattering (SAXS and was confirmed via transmission electron microscopy (TEM. The SAXS results show that the volume fraction of helium bubbles significantly increased with temperature. The amount of helium bubbles reached its maximum at 600°C, and the most probable diameter of the helium bubbles increased with temperature until 14.6 nm at 700°C. A similar size distribution of helium bubbles was obtained via TEM after in situ SAXS measurement at 700°C, except that the most probable diameter was 3.9 nm smaller.

  17. Small angle X-ray scattering data and structure factor fitting for the study of the quaternary structure of the spermidine N-acetyltransferase SpeG.

    Science.gov (United States)

    Weigand, Steven; Filippova, Ekaterina V; Kiryukhina, Olga; Anderson, Wayne F

    2016-03-01

    Here we describe the treatment of the small-angle X-ray Scattering (SAXS) data used during SpeG quaternary structure study as part of the research article "Substrate induced allosteric change in the quaternary structure of the spermidine N-acetyltransferase SpeG" published in Journal of Molecular Biology [1]. These data were collected on two separate area detectors as separate dilution series of the SpeG and the SpeG with spermine samples along with data from their companion buffers. The data were radially integrated, corrected for incident beam variation, and scaled to absolute units. After subtraction of volume-fraction scaled buffer scattering and division by the SpeG concentration, multiple scattering curves free of an inter-molecular structure factor were derived from the dilution series. Rather than extrapolating to infinite dilution, the structure factor contribution was estimated by fitting to the full set of data provided by dividing the scattering curves of a dilution series by the curve from the most dilute sample in that series.

  18. Effect of urea on bovine serum albumin in aqueous and reverse micelle environments investigated by small angle X-ray scattering, fluorescence and circular dichroism

    International Nuclear Information System (INIS)

    Itri, Rosangela; Caetano, Wilker; Barbosa, Leandro R.S.; Baptista, Mauricio S.

    2004-01-01

    The influence that urea has on the conformation of water-soluble globular protein, bovine serum albumin (BSA), exposed directly to the aqueous solution as compared to the condition where the macromolecule is confined in the Aerosol-OT (AOT - sodium bis-2-ethylhexyl sulfosuccinate)/n-hexane/water reverse micelle (RM) is addressed. Small angle X-ray scattering (SAXS), tryptophan (Trp) fluorescence emission and circular dichroism (CD) spectra of aqueous BSA solution in the absence and in the presence of urea (3M and 5M) confirm the known denaturing effect of urea in proteins. The loss of the globular native structure is observed by the increase in the protein maximum dimension and gyration radius, through the Trp emission increase and maximum red-shift as well as the decrease in helix content. In RMs, the Trp fluorescence and CD spectra show that BSA is mainly located in its interfacial region independently of the micellar size. Addition of urea in this BSA/RM system also causes changes in the Trp fluorescence (emission decrease and maximum red-shift) and in the BSA CD spectra (decrease in helix content), which are compatible with the denaturation of the protein and Trp exposition to a more apolar environment in the RM. The fact that urea causes changes in the protein structure when it is located in the interfacial region (evidenced by CD) is interpreted as an indication that the direct interaction of urea with the protein is the major factor to explain its denaturing effect. (author)

  19. Structure of immune stimulating complex matrices and immune stimulating complexes in suspension determined by small-angle x-ray scattering.

    Science.gov (United States)

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

    2012-05-16

    Immune stimulating complex (ISCOM) particles consisting of a mixture of Quil-A, cholesterol, and phospholipids were structurally characterized by small-angle x-ray scattering (SAXS). The ISCOM particles are perforated vesicles of very well-defined structures. We developed and implemented a novel (to our knowledge) modeling method based on Monte Carlo simulation integrations to describe the SAXS data. This approach is similar to the traditional modeling of SAXS data, in which a structure is assumed, the scattering intensity is calculated, and structural parameters are optimized by weighted least-squares methods when the model scattering intensity is fitted to the experimental data. SAXS data from plain ISCOM matrix particles in aqueous suspension, as well as those from complete ISCOMs (i.e., with an antigen (tetanus toxoid) incorporated) can be modeled as a polydisperse distribution of perforated bilayer vesicles with icosahedral, football, or tennis ball structures. The dominating structure is the tennis ball structure, with an outer diameter of 40 nm and with 20 holes 5-6 nm in diameter. The lipid bilayer membrane is 4.6 nm thick, with a low-electron-density, 2.0-nm-thick hydrocarbon core. Surprisingly, in the ISCOMs, the tetanus toxoid is located just below the membrane inside the particles. Copyright © 2012 Biophysical Society. Published by Elsevier Inc. All rights reserved.

  20. Measuring the molecular dimensions of wine tannins: comparison of small-angle X-ray scattering, gel-permeation chromatography and mean degree of polymerization.

    Science.gov (United States)

    McRae, Jacqui M; Kirby, Nigel; Mertens, Haydyn D T; Kassara, Stella; Smith, Paul A

    2014-07-23

    The molecular size of wine tannins can influence astringency, and yet it has been unclear as to whether the standard methods for determining average tannin molecular weight (MW), including gel-permeation chromatography (GPC) and depolymerization reactions, are actually related to the size of the tannin in wine-like conditions. Small-angle X-ray scattering (SAXS) was therefore used to determine the molecular sizes and corresponding MWs of wine tannin samples from 3 and 7 year old Cabernet Sauvignon wine in a variety of wine-like matrixes: 5-15% and 100% ethanol; 0-200 mM NaCl and pH 3.0-4.0, and compared to those measured using the standard methods. The SAXS results indicated that the tannin samples from the older wine were larger than those of the younger wine and that wine composition did not greatly impact on tannin molecular size. The average tannin MWs as determined by GPC correlated strongly with the SAXS results, suggesting that this method does give a good indication of tannin molecular size in wine-like conditions. The MW as determined from the depolymerization reactions did not correlate as strongly with the SAXS results. To our knowledge, SAXS measurements have not previously been attempted for wine tannins.

  1. Small-angle x-ray scattering studies of microvoids in amorphous-silicon-based semiconductors. Annual subcontract report, February 1, 1992--January 31, 1993

    Energy Technology Data Exchange (ETDEWEB)

    Williamson, D L; Jones, S J; Chen, Y [Colorado School of Mines, Golden, CO (United States)

    1994-05-01

    Our general objectives are to provide new details of the microstructure for the size scale from about 1 to 30 nm in high-quality a-Si:H and related alloys prepared by current state-of-the-art deposition methods as well as by new and emerging deposition technologies and thereby help determine the role of microvoids and other density fluctuations in controlling the opto-electronic properties. More specifically, the objectives are to determine whether the presence of microstructure as detected by small-angle x-ray scattering (SAXS) (1) limits the photovoltaic properties of device-quality a-Si:H, (2) plays a role in determining the photo-stability of a-Si:H, and (3) is responsible for degradation of the photovoltaic properties due to alloying with Ge, C and other constituents. The approach involves collaboration with several groups that can supply relevant systematic sets of samples and the associated opto-electronic data to help address these issues. Since the SAXS technique has not been a standard characterization technique for thin-film materials, and was recently set up at CSM with support by NREL, the project involves considerable development of the method with regard to standardizing the procedures, minimizing substrate influences and implementing improved data reduction and modeling methodology. Precise, highly reproducible, and accurate results are being sought in order to allow useful, reliable, and sensitive comparisons of materials deposited under different conditions, by different methods, and by different systems that represent the same nominal method.

  2. 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.

  3. Small-angle x-ray scattering studies of microvoids in amorphous-silicon-based semiconductors. Final subcontract report, 1 February 1991--31 January 1994

    Energy Technology Data Exchange (ETDEWEB)

    Williamson, D.L.; Jone, S.J.; Chen, Y. [Colorado School of Mines, Golden, CO (United States)

    1994-07-01

    This report describes work performed to provide new details of the microstructure for the size scale from about 1 nm to 30 nm in high-quality hydrogenated amorphous-silicon and related alloys prepared by current state-of-the-art deposition methods as well as by new and emerging deposition technologies. The purpose of this work is to help determine the role of microvoids and other density fluctuations in controlling the opto-electronic and photovoltaic properties. The approach involved collaboration with several groups that supplied relevant systematic sets of samples and the associated opto-electronic/photovoltaic data to help address particular issues. The small-angle X-ray scattering (SAXS) technique, as developed during this project, was able to provide microstructural information with a high degree of sensitivity not available from other methods. It is particularly sensitive to microvoids or H-rich microdomains and to the presence of oriented microstructures. The latter is readily associated with columnar-type growth and can even be observed in premature stages not detectable by transmission electron microscopy. Flotation density measurements provided important complementary data. Systematic correlations demonstrated that material with more SAXS-detected microstructure has to-electronic and photovoltaic properties and increased degradation under light soaking. New results related to alloy randomness emerged from our ability to measure the difffuse scattering component of the SAXS.

  4. Neutron and Synchrotron X-Ray Scattering Studies of Superconductors

    International Nuclear Information System (INIS)

    Tranquada, J.M.

    2008-01-01

    Superconductors hold the promise for a more stable and efficient electrical grid, but new isotropic, high-temperature superconductors are needed in order to reduce cable manufacturing costs. The effort to understand high-temperature superconductivity, especially in the layered cuprates, provides guidance to the search for new superconductors. Neutron scattering has long provided an important probe of the collective excitations that are involved in the pairing mechanism. For the cuprates, neutron and x-ray diffraction techniques also provide information on competing types of order, such as charge and spin stripes, that appear to be closely connected to the superconductivity. Recently, inelastic x-ray scattering has become competitive for studying phonons and may soon provide valuable information on electronic excitations. Examples of how these techniques contribute to our understanding of superconductivity are presented

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

    Directory of Open Access Journals (Sweden)

    Matthias Schwartzkopf

    2016-12-01

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

  6. X-ray Synchrotron Radiation in a Plasma Wiggler

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Shuoquin; /UCLA /SLAC, SSRL

    2005-09-27

    A relativistic electron beam can radiate due to its betatron motion inside an ion channel. The ion channel is induced by the electron bunch as it propagates through an underdense plasma. In the theory section of this thesis the formation of the ion channel, the trajectories of beam electrons inside the ion channel, the radiation power and the radiation spectrum of the spontaneous emission are studied. The comparison between different plasma wiggler schemes is made. The difficulties in realizing stimulated emission as the beam traverses the ion channel are investigated, with particular emphasis on the bunching mechanism, which is important for the ion channel free electron laser. This thesis reports an experiment conducted at the Stanford Linear Accelerator Center (SLAC) to measure the betatron X-ray radiations for the first time. They first describe the construction and characterization of the lithium plasma source. In the experiment, the transverse oscillations of the SLAC 28.5 GeV electron beam traversing through a 1.4 meter long lithium plasma source are clearly seen. These oscillations lead to a quadratic density dependence of the spontaneously emitted betatron X-ray radiation. The divergence angle of the X-ray radiation is measured. The absolute photon yield and the spectral brightness at 14.2 KeV photon energy are estimated and seen to be in reasonable agreement with theory.

  7. Characterization of Polycrystalline Materials Using Synchrotron X-ray Imaging and Diffraction Techniques

    DEFF Research Database (Denmark)

    Ludwig, Wolfgang; King, A.; Herbig, M.

    2010-01-01

    propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray......The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using...... diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure...

  8. Noninvasive 3D Structural Analysis of Arthropod by Synchrotron X-Ray Phase Contrast Tomography

    Directory of Open Access Journals (Sweden)

    Shengkun Yao

    2015-01-01

    Full Text Available X-ray imaging techniques significantly advanced our understanding of materials and biology, among which phase contrast X-ray microscopy has obvious advantages in imaging biological specimens which have low contrast by conventional absorption contrast microscopy. In this paper, three-dimensional microstructure of arthropod with high contrast has been demonstrated by synchrotron X-ray in-line phase contrast tomography. The external morphology and internal structures of an earthworm were analyzed based upon tomographic reconstructions with and without phase retrieval. We also identified and characterized various fine structural details such as the musculature system, the digestive system, the nervous system, and the circulatory system. This work exhibited the high efficiency, high precision, and wide potential applications of synchrotron X-ray phase contrast tomography in nondestructive investigation of low-density materials and biology.

  9. Noninvasive 3D Structural Analysis of Arthropod by Synchrotron X-Ray Phase Contrast Tomography

    International Nuclear Information System (INIS)

    Yao, S.; Zong, Y.; Fan, J.; Sun, Z.; Jiang, H.

    2015-01-01

    X-ray imaging techniques significantly advanced our understanding of materials and biology, among which phase contrast X-ray microscopy has obvious advantages in imaging biological specimens which have low contrast by conventional absorption contrast microscopy. In this paper, three-dimensional microstructure of arthropod with high contrast has been demonstrated by synchrotron X-ray in-line phase contrast tomography. The external morphology and internal structures of an earthworm were analyzed based upon tomographic reconstructions with and without phase retrieval. We also identified and characterized various fine structural details such as the musculature system, the digestive system, the nervous system, and the circulatory system. This work exhibited the high efficiency, high precision, and wide potential applications of synchrotron X-ray phase contrast tomography in nondestructive investigation of low-density materials and biology.

  10. Characterization of Polycrystalline Materials Using Synchrotron X-ray Imaging and Diffraction Techniques

    DEFF Research Database (Denmark)

    Ludwig, Wolfgang; King, A.; Herbig, M.

    2010-01-01

    The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using...... propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X......-ray diffraction contrast tomography provides access to the 3-D shape, orientation, and elastic strain state of the individual grains from polycrystalline sample volumes containing up to thousand grains. Combining both imaging modalities, one obtains a comprehensive description of the materials microstructure...

  11. Model experiment of in vivo synchrotron X-ray diffraction of human kidney stones

    Energy Technology Data Exchange (ETDEWEB)

    Ancharov, A.I. [Institute of Solid State Chemistry and Mechanochemistry SB RAS, Novosibirsk (Russian Federation)]. E-mail: ancharov@mail.ru; Potapov, S.S. [Institute of Mineralogy UB RAS, Miass (Russian Federation); Moiseenko, T.N. [The State Regional Clinical Hospital, Novosibirsk (Russian Federation); Feofilov, I.V. [The State Regional Clinical Hospital, Novosibirsk (Russian Federation); Nizovskii, A.I. [Boreskov Institute of Catalysis SB RAS, Novosibirsk (Russian Federation)

    2007-05-21

    The diffraction of synchrotron radiation (SR) was used to explore the phase composition of kidney stones placed into a specific object phantom, which imitated the human body. As an imitation of the patient breath, the kidney stone was moved vertically and rotated to an angle of 15{sup o} during the recording of the X-ray pattern. It was shown that rotation and displacement did not distort the X-ray pattern.

  12. DEVELOPMENTS IN SYNCHROTRON X-RAY COMPUTED MICROTOMOGRAPHY AT THE NATIONAL SYNCHROTRON LIGHT SOURCE.

    Energy Technology Data Exchange (ETDEWEB)

    DOWD,B.A.

    1999-07-23

    Last year, the X27A beamline at the National Synchrotron Light Source (NSLS) became dedicated solely to X-Ray Computed Microtomography (XCMT). This is a third-generation instrument capable of producing tomographic volumes of 1-2 micron resolution over a 2-3mm field of view. Recent enhancements will be discussed. These have focused on two issues: the desire for real-time data acquisition and processing and the need for highly monochromatic beam (.1 % energy bandpass). The latter will permit k-edge subtraction studies and will provide improved image contrast from below the Cr (6 keV) up to the Cs (36 keV) k-edge. A range of applications that benefit from these improvements will be discussed as well. These two goals are somewhat counterproductive, however; higher monochromaticity yields a lower flux forcing longer data acquisition times. To balance the two, a more efficient scintillator for X-ray conversion is being developed. Some testing of a prototype scintillator has been performed; preliminary results will be presented here. In the meantime, data reconstruction times have been reduced, and the entire tomographic acquisition, reconstruction and volume rendering process streamlined to make efficient use of synchrotron beam time. A Fast Filtered Back Transform (FFBT) reconstruction program recently developed helped to reduce the time to reconstruct a volume of 150 x 150 x 250 pixels{sup 3} (over 5 million voxels) from the raw camera data to 1.5 minutes on a dual R10,000 CPU. With these improvements, one can now obtain a ''quick look'' of a small tomographic volume ({approximately}10{sup 6}voxels) in just over 15 minutes from the start of data acquisition.

  13. 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.

  14. Report of the second workshop on synchrotron radiation sources for x-ray lithography

    Energy Technology Data Exchange (ETDEWEB)

    Barton, M.Q.; Craft, B.; Williams, G.P. (eds.)

    1986-01-01

    The reported workshop is part of an effort to implement a US-based x-ray lithography program. Presentations include designs for three storage rings (one superconducting and two conventional) and an overview of a complete lithography program. The background of the effort described, the need for synchrotron radiation, and the international competition in the area are discussed briefly. The technical feasibility of x-ray lithography is discussed, and synchrotron performance specifications and construction options are given, as well as a near-term plan. It is recommended that a prototype synchrotron source be built as soon as possible, and that a research and development plan on critical technologies which could improve cost effectiveness of the synchrotron source be established. It is further recommended that a small number of second generation prototype synchrotrons be distributed to IC manufacturing centers to expedite commercialization. (LEW)

  15. Report of the second workshop on synchrotron radiation sources for x-ray lithography

    International Nuclear Information System (INIS)

    Barton, M.Q.; Craft, B.; Williams, G.P.

    1986-01-01

    The reported workshop is part of an effort to implement a US-based x-ray lithography program. Presentations include designs for three storage rings (one superconducting and two conventional) and an overview of a complete lithography program. The background of the effort described, the need for synchrotron radiation, and the international competition in the area are discussed briefly. The technical feasibility of x-ray lithography is discussed, and synchrotron performance specifications and construction options are given, as well as a near-term plan. It is recommended that a prototype synchrotron source be built as soon as possible, and that a research and development plan on critical technologies which could improve cost effectiveness of the synchrotron source be established. It is further recommended that a small number of second generation prototype synchrotrons be distributed to IC manufacturing centers to expedite commercialization

  16. Synchrotron X-ray PIV Technique for Measurement of Blood Flow Velocity

    International Nuclear Information System (INIS)

    Kim, Guk Bae; Lee, Sang Joon; Je, Jung Ho

    2007-01-01

    Synchrotron X-ray micro-imaging method has been used to observe internal structures of various organisms, industrial devices, and so on. However, it is not suitable to see internal flows inside a structure because tracers typically employed in conventional optical flow visualization methods cannot be detectable with the X-ray micro-imaging method. On the other hand, a PIV (particle image velocimetry) method which has recently been accepted as a reliable quantitative flow visualization technique can extract lots of flow information by applying digital image processing techniques However, it is not applicable to opaque fluids such as blood. In this study, we combined the PIV method and the synchrotron X-ray micro-imaging technique to compose a new X-ray PIV technique. Using the X-ray PIV technique, we investigated the optical characteristics of blood for a coherent synchrotron X-ray beam and quantitatively visualized real blood flows inside an opaque tube without any contrast media. The velocity field information acquired would be helpful for investigating hemorheologic characteristics of the blood flow

  17. Effect of toroidal mirror on spatial coherence of synchrotron hard X-ray beams

    International Nuclear Information System (INIS)

    Wang Hua; Yan Shuai; Yan Fen; Mao Chengwen; Liang Dongxun; He Yan; Jiang Sheng; Li Aiguo; Yu Xiaohan

    2012-01-01

    The Gaussian Schell-model source theory is used to describe the hard X-ray micro focusing beamline with an undulator of the Shanghai Synchrotron Radiation Facility. Based on the model and general Huygens-Fresnel principle, propagation of cross-spectral density function in free space is studied. Equivalent source hypothesis is proposed and the effect of toroidal mirror on spatial coherence of the hard X-ray beams is studied. The theoretical results are consistent with the experimental results. Only divergence angles of the incident and outgoing X-rays are considered in the equivalent source hypothesis, hence an easy extension of the hypothesis to other beamline optical elements. (authors)

  18. A new miniature microchannel plate X-ray detector for synchrotron radiation

    International Nuclear Information System (INIS)

    Rosemeier, R.G.; Green, R.E. Jr.

    1982-01-01

    A state-of-the-art microchannel plate detector has been developed which allows real time X-ray imaging of X-ray diffraction as well as radiographic phenomenon. Advantages of the device include a 50 mm X-ray input, length less than 4'', and a weight of less than 1 lb. Since the use of synchrotron radiation is greatly facilitated by the capability of remote viewing of X-ray diffraction or radiographic images in real time, a prototype electro-optical system has been designed which couples the X-ray microchannel plate detector with a solid state television camera. Advantages of the miniature, lightweight, X-ray synchrotron camera include a large 50 mm X-ray input window, an output signal that is available in both analog format for display on a television monitor and in digital format for computer processing, and a completely modular design which allows all the components to be exchanged for other components optimally suited for the desired applications. (orig.)

  19. Thermal, structural, and fabrication aspects of diamond windows for high power synchrotron x-ray beamlines

    International Nuclear Information System (INIS)

    Khounsary, A.M.; Phillips, W.

    1992-01-01

    Recent advances in chemical vapor deposition (CVD) technology have made it possible to produce thin free-standing diamond foils that can be used as the window material in high heat load, synchrotron beamlines. Numerical simulations suggest that these windows can offer an attractive and at times the only altemative to beryllium windows for use in third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, as are the microstructure characteristics bearing on diamond's performance in this role. Analytic and numerical results are also presented to provide a basis for the design and testing of such windows

  20. A CCD-based area detector for X-ray crystallography using synchrotron and laboratory sources

    International Nuclear Information System (INIS)

    Phillips, W.C.; Li Youli; Stanton, M.; Xie Yuanhui; O'Mara, D.; Kalata, K.

    1993-01-01

    The design and characteristics of a CCD-based area detector suitable for X-ray crystallographic studies using both synchrotron and laboratory sources are described. The active area is 75 mm in diameter, the FWHM of the point response function is 0.20 mm, and for Bragg peaks the dynamic range is 900 and the DQE ∼0.3. The 1320x1035-pixel Kodak CCD is read out into an 8 Mbyte memory system in 0.14 s and digitized to 12 bits. X-ray crystallographic data collected at the NSLS synchrotron from cubic insulin crystals are presented. (orig.)

  1. Effects of synchrotron x-rays on PVD deposited and ion implanted α-Si

    International Nuclear Information System (INIS)

    Yu, K.M.; Wang, L.; Walukiewicz, W.; Muto, S.; McCormick, S.; Abelson, J.R.

    1997-01-01

    The authors have studied the effects of intense X-ray irradiation on the structure of amorphous Si films. The films were obtained by either physical vapor deposition or by implantation of high energy ions into crystalline Si. They were exposed to different total doses of synchrotron X-rays. From the EXAFS and EXELFS measurements they find that an exposure to X-rays increases the Si coordination number. Also in the PVD films a prolonged X-ray exposure enlarges, by about 2%, the Si-Si bond length. Raman spectroscopy shows that Si amorphized with high energy ions contains small residual amounts of crystalline material. Irradiation of such films with X-rays annihilates those crystallites resulting in homogeneously amorphous layer with a close to four-fold coordination of Si atoms. This rearrangement of the local structure has a pronounced effect on the crystallization process of the amorphous films. Thermal annealing of X-ray irradiated ion amorphized films leads to nearly defect free solid phase epitaxy at 500 C. Also they observe a delay in the onset of the crystallization process in X-ray irradiated PVD films. They associate this with a reduced concentration of nucleation centers in the x-ray treated materials

  2. Investigation of the effect of sugar stereochemistry on biologically relevant lyotropic phases from branched-chain synthetic glycolipids by small-angle X-ray scattering.

    Science.gov (United States)

    Zahid, N Idayu; Conn, Charlotte E; Brooks, Nicholas J; Ahmad, Noraini; Seddon, John M; Hashim, Rauzah

    2013-12-23

    Synthetic branched-chain glycolipids are suitable as model systems in understanding biological cell membranes, particularly because certain natural lipids possess chain branching. Herein, four branched-chain glycopyranosides, namely, 2-hexyl-decyl-α-D-glucopyranoside (α-Glc-OC10C6), 2-hexyl-decyl-β-D-glucopyranoside (β-Glc-OC10C6), 2-hexyl-decyl-α-D-galactopyranoside (α-Gal-OC10C6), and 2-hexyl-decyl-β-D-galactopyranoside (β-Gal-OC10C6), with a total alkyl chain length of 16 carbon atoms have been synthesized, and their phase behavior has been studied. The partial binary phase diagrams of these nonionic surfactants in water were investigated by optical polarizing microscopy (OPM) and small-angle X-ray scattering (SAXS). The introduction of chain branching in the hydrocarbon chain region is shown to result in the formation of inverse structures such as inverse hexagonal and inverse bicontinuous cubic phases. A comparison of the four compounds showed that they exhibited different polymorphism, especially in the thermotropic state, as a result of contributions from anomeric and epimeric effects according to their stereochemistry. The neat α-Glc-OC10C6 compound exhibited a lamellar (Lα) phase whereas dry α-Gal-OC10C6 formed an inverse bicontinuous cubic Ia3d (QII(G)) phase. Both β-anomers of glucoside and galactoside adopted the inverse hexagonal phase (HII) in the dry state. Generally, in the presence of water, all four glycolipids formed inverse bicontinuous cubic Ia3d (QII(G)) and Pn3m (QII(D)) phases over wide temperature and concentration ranges. The formation of inverse nonlamellar phases by these Guerbet branched-chain glycosides confirms their potential as materials for novel biotechnological applications such as drug delivery and crystallization of membrane proteins.

  3. Small angle X-ray scattering and cross-linking for data assisted protein structure prediction in CASP 12 with prospects for improved accuracy

    KAUST Repository

    Ogorzalek, Tadeusz L.

    2018-01-04

    Experimental data offers empowering constraints for structure prediction. These constraints can be used to filter equivalently scored models or more powerfully within optimization functions toward prediction. In CASP12, Small Angle X-ray Scattering (SAXS) and Cross-Linking Mass Spectrometry (CLMS) data, measured on an exemplary set of novel fold targets, were provided to the CASP community of protein structure predictors. As HT, solution-based techniques, SAXS and CLMS can efficiently measure states of the full-length sequence in its native solution conformation and assembly. However, this experimental data did not substantially improve prediction accuracy judged by fits to crystallographic models. One issue, beyond intrinsic limitations of the algorithms, was a disconnect between crystal structures and solution-based measurements. Our analyses show that many targets had substantial percentages of disordered regions (up to 40%) or were multimeric or both. Thus, solution measurements of flexibility and assembly support variations that may confound prediction algorithms trained on crystallographic data and expecting globular fully-folded monomeric proteins. Here, we consider the CLMS and SAXS data collected, the information in these solution measurements, and the challenges in incorporating them into computational prediction. As improvement opportunities were only partly realized in CASP12, we provide guidance on how data from the full-length biological unit and the solution state can better aid prediction of the folded monomer or subunit. We furthermore describe strategic integrations of solution measurements with computational prediction programs with the aim of substantially improving foundational knowledge and the accuracy of computational algorithms for biologically-relevant structure predictions for proteins in solution. This article is protected by copyright. All rights reserved.

  4. Structure of the bifunctional aminoglycoside-resistance enzyme AAC(6')-Ie-APH(2'')-Ia revealed by crystallographic and small-angle X-ray scattering analysis.

    Science.gov (United States)

    Smith, Clyde A; Toth, Marta; Weiss, Thomas M; Frase, Hilary; Vakulenko, Sergei B

    2014-10-01

    Broad-spectrum resistance to aminoglycoside antibiotics in clinically important Gram-positive staphylococcal and enterococcal pathogens is primarily conferred by the bifunctional enzyme AAC(6')-Ie-APH(2'')-Ia. This enzyme possesses an N-terminal coenzyme A-dependent acetyltransferase domain [AAC(6')-Ie] and a C-terminal GTP-dependent phosphotransferase domain [APH(2'')-Ia], and together they produce resistance to almost all known aminoglycosides in clinical use. Despite considerable effort over the last two or more decades, structural details of AAC(6')-Ie-APH(2'')-Ia have remained elusive. In a recent breakthrough, the structure of the isolated C-terminal APH(2'')-Ia enzyme was determined as the binary Mg2GDP complex. Here, the high-resolution structure of the N-terminal AAC(6')-Ie enzyme is reported as a ternary kanamycin/coenzyme A abortive complex. The structure of the full-length bifunctional enzyme has subsequently been elucidated based upon small-angle X-ray scattering data using the two crystallographic models. The AAC(6')-Ie enzyme is joined to APH(2'')-Ia by a short, predominantly rigid linker at the N-terminal end of a long α-helix. This α-helix is in turn intrinsically associated with the N-terminus of APH(2'')-Ia. This structural arrangement supports earlier observations that the presence of the intact α-helix is essential to the activity of both functionalities of the full-length AAC(6')-Ie-APH(2'')-Ia enzyme.

  5. Small Angle X-ray Scattering and Electron Spin Resonance Spectroscopy Study on Fragrance Infused Cationic Vesicles Modeling Scent-Releasing Fabric Softeners.

    Science.gov (United States)

    Ogura, Taku; Sato, Takaaki; Abe, Masahiko; Okano, Tomomichi

    2018-02-01

    Industrially relevant systems for household and personal-care products often involve a large number of components. Such multiple component formulations are indispensable and effective for functionalization of the products, but may simultaneously provide more complex structural features compared to those in ideal systems comprising a smaller number of highly pure substances. Using cryogenic transmission electron microscopy (cryo-TEM), small angle X-ray scattering (SAXS), and electron spin resonance (ESR) spectroscopy, we have investigated effects of fragrance-incorporation into cationic vesicles on their bilayer structures and membrane-membrane interactions. Cationic vesicles were prepared from TEQ surfactant, whose major component was di(alkyl fatty ester) quaternary ammonium methosulfate, and fragrance components, l-menthol, linalool, and d-limonene, were infused into the vesicle membranes to model scent-releasing fabric softeners. The cryo-TEM images confirm formation of multilamellar vesicles (MLVs). Generalized indirect Fourier transformation (GIFT) analysis of the SAXS intensities based on the modified Caillé structure factor model reveals that incorporation of a more hydrophobic fragrance component leads to a more pronounced increase of the surface separation (water layer thickness). Furthermore, the fragrance-infused systems show longer-range order of the bilayer correlations and enhanced undulation fluctuation of the membranes than those in the TEQ alone system. The spin-label ESR results indicate different restricted molecular motions in the TEQ bilayers depending on the labeled position and their marked changes upon addition of the fragrance components, suggesting different mixing schemes and solubilization positions of the fragrance molecules in the TEQ bilayers. The present data have demonstrated how the infused fragrance molecules having different hydrophobicity and molecular architectures into the cationic vesicles affect the membrane structures and

  6. Combining NMR and small angle X-ray and neutron scattering in the structural analysis of a ternary protein-RNA complex

    International Nuclear Information System (INIS)

    Hennig, Janosch; Wang, Iren; Sonntag, Miriam; Gabel, Frank; Sattler, Michael

    2013-01-01

    Many processes in the regulation of gene expression and signaling involve the formation of protein complexes involving multi-domain proteins. Individual domains that mediate protein-protein and protein-nucleic acid interactions are typically connected by flexible linkers, which contribute to conformational dynamics and enable the formation of complexes with distinct binding partners. Solution techniques are therefore required for structural analysis and to characterize potential conformational dynamics. Nuclear magnetic resonance spectroscopy (NMR) provides such information but often only sparse data are obtained with increasing molecular weight of the complexes. It is therefore beneficial to combine NMR data with additional structural restraints from complementary solution techniques. Small angle X-ray/neutron scattering (SAXS/SANS) data can be efficiently combined with NMR-derived information, either for validation or by providing additional restraints for structural analysis. Here, we show that the combination of SAXS and SANS data can help to refine structural models obtained from data-driven docking using HADDOCK based on sparse NMR data. The approach is demonstrated with the ternary protein-protein-RNA complex involving two RNA recognition motif (RRM) domains of Sex-lethal, the N-terminal cold shock domain of Upstream-to-N-Ras, and msl-2 mRNA. Based on chemical shift perturbations we have mapped protein-protein and protein-RNA interfaces and complemented this NMR-derived information with SAXS data, as well as SANS measurements on subunit-selectively deuterated samples of the ternary complex. Our results show that, while the use of SAXS data is beneficial, the additional combination with contrast variation in SANS data resolves remaining ambiguities and improves the docking based on chemical shift perturbations of the ternary protein-RNA complex.

  7. Small angle X-ray scattering and cross-linking for data assisted protein structure prediction in CASP 12 with prospects for improved accuracy.

    Science.gov (United States)

    Ogorzalek, Tadeusz L; Hura, Greg L; Belsom, Adam; Burnett, Kathryn H; Kryshtafovych, Andriy; Tainer, John A; Rappsilber, Juri; Tsutakawa, Susan E; Fidelis, Krzysztof

    2018-03-01

    Experimental data offers empowering constraints for structure prediction. These constraints can be used to filter equivalently scored models or more powerfully within optimization functions toward prediction. In CASP12, Small Angle X-ray Scattering (SAXS) and Cross-Linking Mass Spectrometry (CLMS) data, measured on an exemplary set of novel fold targets, were provided to the CASP community of protein structure predictors. As solution-based techniques, SAXS and CLMS can efficiently measure states of the full-length sequence in its native solution conformation and assembly. However, this experimental data did not substantially improve prediction accuracy judged by fits to crystallographic models. One issue, beyond intrinsic limitations of the algorithms, was a disconnect between crystal structures and solution-based measurements. Our analyses show that many targets had substantial percentages of disordered regions (up to 40%) or were multimeric or both. Thus, solution measurements of flexibility and assembly support variations that may confound prediction algorithms trained on crystallographic data and expecting globular fully-folded monomeric proteins. Here, we consider the CLMS and SAXS data collected, the information in these solution measurements, and the challenges in incorporating them into computational prediction. As improvement opportunities were only partly realized in CASP12, we provide guidance on how data from the full-length biological unit and the solution state can better aid prediction of the folded monomer or subunit. We furthermore describe strategic integrations of solution measurements with computational prediction programs with the aim of substantially improving foundational knowledge and the accuracy of computational algorithms for biologically-relevant structure predictions for proteins in solution. © 2018 Wiley Periodicals, Inc.

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

    Science.gov (United States)

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

    2014-12-07

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

  9. In-Situ Monitoring of the Microstructure of TATB-based Explosive Formulations During Temperature Cycling using Ultra-small Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Willey, T M; Hoffman, D M; van Buuren, T; Lauderbach, L; Ilavsky, J; Gee, R H; Maiti, A; Overturf, G; Fried, L

    2008-02-06

    TATB (1,3,5 triamino-2,4,6-trinitrobenzene), an extremely insensitive explosive, is used both in plastic-bonded explosives (PBXs) and as an ultra-fine pressed powder (UFTATB). With both PBXs and UFTATB, an irreversible expansion occurs with temperature cycling known as ratchet growth. In TATB-based explosives using Kel-F 800 as binder (LX-17 and PBX-9502), additional voids, sizes hundreds of nanometers to a few microns account for much of the volume expansion caused by temperature cycling. These voids are in the predicted size regime for hot-spot formation during ignition and detonation, and thus an experimental measure of these voids is important feedback for hot-spot theory and for determining the relationship between void size distributions and detonation properties. Also, understanding the mechanism of ratchet growth allows future choice of explosive/binder mixtures to minimize these types of changes to explosives, further extending PBX shelf life. This paper presents the void size distributions of LX-17, UFTATB, and PBXs using commercially available Cytop M, Cytop A, and Hyflon AD60 binders during temperature cycling between -55 C and 70 C. These void size distributions are derived from ultra-small angle x-ray scattering (USAXS), a technique sensitive to structures from about 10 nm to about 2 mm. Structures with these sizes do not appreciably change in UFTATB, indicating voids or cracks larger than a few microns appear in UFTATB during temperature cycling. Compared to Kel-F 800 binders, Cytop M and Cytop A show relatively small increases in void volume from 0.9% to 1.3% and 0.6% to 1.1%, respectively, while Hyflon fails to prevent irreversible volume expansion (1.2% to 4.6%). Computational mesoscale models of ratchet growth and binder wetting and adhesion properties point to mechanisms of ratchet growth, and are discussed in combination with the experimental results.

  10. Adsorption of bovine hemoglobin onto spherical polyelectrolyte brushes monitored by small-angle X-ray scattering and Fourier transform infrared spectroscopy.

    Science.gov (United States)

    Henzler, Katja; Wittemann, Alexander; Breininger, Eugenia; Ballauff, Matthias; Rosenfeldt, Sabine

    2007-11-01

    The adsorption of bovine hemoglobin (BHb) onto colloidal spherical polyelectrolyte brushes (SPBs) is studied by a combination of small-angle X-ray scattering (SAXS) and Fourier transform infrared spectroscopy (FTIR). The SPBs consist of a polystyrene core onto which long chains of poly(styrene sulfonic acid) are grafted. Hemoglobin is a tetrameric protein that disassembles at low pH's and high ionic strengths. The protein is embedded into the brush layer composed of strong polyacids. Thus, the protein is subjected to a pH and ionic strength that largely differs from the bulk solution. At low ionic strengths up to 650 mg of BHb per gram of SPB could be immobilized. The analysis of the particles loaded with protein by SAXS demonstrates that the protein enters deeply into the brush. A large fraction of hemoglobin is bound at the surface of the polystyrene core. We attribute this strong affinity to hydrophobic interactions between the protein and the polystyrene core. The other protein molecules are closely correlated with the polyelectrolyte chains. The secondary structure of the protein within the brush was studied by FTIR spectroscopy. The analysis revealed a significant disturbance of the secondary structure of the tetrameric protein. The content of alpha-helix is significantly lowered compared to the native conformation. Moreover, there is an increase of beta-sheet structure as compared to the native conformation. The partial loss of the structural integrity of the hydrophobic protein is due to hydrophobic interactions with the hydrophobic polystyrene core. Hydrophobic interactions with the phenyl groups of the poly(styrene sulfonate) chains influence the secondary structure as well. These findings indicate that changes of the secondary structure play a role in the uptake of hemoglobin into the poly(styrene sulfonate) brushes.

  11. Time-resolved small-angle x-ray scattering study of the early stage of amyloid formation of an apomyoglobin mutant

    Science.gov (United States)

    Ortore, Maria Grazia; Spinozzi, Francesco; Vilasi, Silvia; Sirangelo, Ivana; Irace, Gaetano; Shukla, Anuj; Narayanan, Theyencheri; Sinibaldi, Raffaele; Mariani, Paolo

    2011-12-01

    The description of the fibrillogenesis pathway and the identification of “on-pathway” or “off-pathway” intermediates are key issues in amyloid research as they are concerned with the mechanism for onset of certain diseases and with therapeutic treatments. Recent results on the fibril formation process revealed an unexpected complexity both in the number and in the types of species involved, but the early aggregation events are still largely unknown, mainly because of their experimental inaccessibility. To provide information on the early stage events of self-assembly of an amyloidogenic protein, during the so-called lag phase, stopped-flow time-resolved small angle x-ray scattering (SAXS) experiments were performed. Using a global fitting analysis, the structural and aggregation properties of the apomyoglobin W7FW14F mutant, which is monomeric and partly folded at acidic pH but forms amyloid fibrils after neutralization, were derived from the first few milliseconds onward. SAXS data indicated that the first aggregates appear in less than 20 ms after the pH jump to neutrality and further revealed the simultaneous presence of diverse species. In particular, worm-like unstructured monomers, very large assemblies, and elongated particles were detected, and their structural features and relative concentrations were derived as a function of time on the basis of our model. The final results show that, during the lag phase, early assembling occurs due to the presence of transient monomeric species very prone to association and through successive competing aggregation and rearrangement processes leading to coexisting on-pathway and off-pathway transient species.

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

    KAUST Repository

    Yu, Hsiu-Yu

    2014-09-15

    © the Partner Organisations 2014. We investigate the static structure factor S(q) of solvent-free nanoparticle-organic hybrid materials consisting of silica nanocores and space-filling polyethylene glycol coronas using a density-functional theory and small angle X-ray scattering measurements. The theory considers a bidisperse suspension of hard spheres with different radii and tethered bead-spring oligomers with different grafting densities to approximate the polydispersity effects in experiments. The experimental systems studied include pure samples with different silica core volume fractions and the associated mean corona grafting densities, and blends with different mixing ratios of the pure samples, in order to introduce varying polydispersity of corona grafting density. Our scattering experiments and theory show that, compared to the hard-sphere suspension with the same core volume fraction, S(q) for pure samples exhibit both substantially smaller values at small q and stronger particle correlations corresponding to a larger effective hard core at large q, indicating that the tethered incompressible oligomers enforce a more uniform particle distribution, and the densely grafted brush gives rise to an additional exclusionary effect between the nanoparticles. According to the theory, polydispersity in the oligomer grafting density controls the deviation of S(q) from the monodisperse system at smaller q, and the interplay of the enhanced effective core size and the entropic attraction among the particles is responsible for complex variations in the particle correlations at larger q. The successful comparison between the predictions and the measurements for the blends further suggests that S(q) can be used to assess the uniformity of grafting density in polymer-grafted nanoparticle materials. This journal is

  13. Determination of the quaternary structural states of bovine casein by small-angle X-ray scattering: submicellar and micellar forms

    Energy Technology Data Exchange (ETDEWEB)

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

    1988-11-01

    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)

  14. Synchrotron X-ray Scattering from Self-organized Soft Nanostructures in Clays

    Science.gov (United States)

    Fossum, J. O.

    2009-04-01

    . Gog, C. Venkataraman, Observations of orientational ordering in aqueous suspensions of a nano-layered silicate, ENERGY The International Journal 30, 873 (2005). 2. D. M. Fonseca, Y. Méheust, J. O. Fossum, K. D. Knudsen, K. J. Måløy and K. P. S. Parmar, Phase behavior of platelet-shaped nanosilicate colloids in saline solutions: A small-angle X-ray scattering study J. Appl. Cryst. 40 292 (2007) 3. E. N. de Azevedo, M. Engelsberg, J. O. Fossum, R. E. de Souza, Anisotropic water diffusion in nematic self-assemblies of clay nano-platelets suspended in water, Langmuir 23, 5100 (2007) 4. Nils Ivar Ringdal, Master thesis, Department of Physics, NTNU (2008) 5. J.O. Fossum, Y. Meheust, K.P.S. Parmar, K.D. Knudsen, K.J. Maloy, D.d.M. Fonseca, Intercalation-enhanced electric polarization and chain formation of nano-layered particles, Europhys. Lett., 74, 438 (2006), and in the Scientific Highlights 2006 of the European Synchrotron Radiation Facility - ESRF (2007) 6. K.P.S. Parmar, Y. Meheust, B. Schelderupsen and J.O. Fossum, Electrorheological suspensions of laponite in oil: rheometry studies, Langmuir 24,1814 (2008) 7. F. Bergaya, B. K. G. Theng, and G. Lagaly, editors. Handbook of Clay Science. Elsevier (2006)

  15. Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera

    Science.gov (United States)

    Fittschen, Ursula Elisabeth Adriane; Menzel, Magnus; Scharf, Oliver; Radtke, Martin; Reinholz, Uwe; Buzanich, Günther; Lopez, Velma M.; McIntosh, Kathryn; Streli, Christina; Havrilla, George Joseph

    2014-09-01

    Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by “drop on demand” technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation.

  16. Beryllium window flange for synchrotron radiation X-ray beamline fabricated by hot isostatic press method

    International Nuclear Information System (INIS)

    Asaoka, Seiji; Maezawa, Hideki; Nishida, Kiyotoshi; Sakamoto, Naoki.

    1995-01-01

    The synchrotron radiation experimental facilities in National Laboratory for High Energy Physics are the experimental facilities for joint utilization, that possess the positron storage ring of 2.5 GeV exclusively used for synchrotron radiation. Synchrotron radiation is led through a mainstay beam channel to the laboratory, and in the beam line of X-ray, it is used for experiment through the taking-out window made of beryllium. At this time, the function of the taking-out window is to shut off between the ultrahigh vacuum in the mainstay beam channel and the atmosphere, and to cut the low energy component of synchrotron radiation spectra. The experiment using X-ray is carried out mostly in the atmosphere. The design of the efficient cooling water channel which is compatible with the flange construction is important under the high thermal load of synchrotron radiation. The beryllium window flange for synchrotron radiation X-ray was made by HIP method, and the ultrahigh vacuum test, the high pressure water flow test and the actual machine test were carried out by heat cycle. The properties required for the window material, the requirement of the construction, the new development of HIP method, and the experiments for evaluating the manufactured beryllium window are described. (K.I.)

  17. Structural Analysis on Reduced Graphene Oxide Prepared from Old Coconut Shell by Synchrotron X-Ray Scattering

    Science.gov (United States)

    Yogi Nugraheni, Ananda; Jayanti, Dwi Noor; Kurniasari; Soontaranon, Siriwat; Giri Rachman Putra, Edy; Darminto

    2017-05-01

    This work is aimed to identify the distribution of size and structure of the reduced graphene oxide (rGO) particles before and after the mechanical exfoliation process from coconut shell. The burnt sample was heated at 400°C in ambient air, followed by sonication and centrifugation method for various concentration. The characterization were performed by using wide angle X-ray scattering (WAXS) and synchrotron small angle X-ray scattering (SAXS). Based on SAXS result, the structure of rGO showed that in low range of momentum transfer (Q), the particle size was too big to be measured using SAXS. In the high Q, the graph shown the apparent absence of change in curvature which indicates that the small particles are typically seen on high Q range, having aggregate with a new shape and big particles. The average fitting slope is -3.3, implying that the particles structure tends to be fractal (rough) surface, where the particles form aggregates to become bigger size and irregular structure. Further, the WAXS characterization shows that the exfoliation step has not affected the rGO phase formed.

  18. High-energy synchrotron X-ray radiography of shock-compressed materials

    Science.gov (United States)

    Rutherford, Michael E.; Chapman, David J.; Collinson, Mark A.; Jones, David R.; Music, Jasmina; Stafford, Samuel J. P.; Tear, Gareth R.; White, Thomas G.; Winters, John B. R.; Drakopoulos, Michael; Eakins, Daniel E.

    2015-06-01

    This presentation will discuss the development and application of a high-energy (50 to 250 keV) synchrotron X-ray imaging method to study shock-compressed, high-Z samples at Beamline I12 at the Diamond Light Source synchrotron (Rutherford-Appleton Laboratory, UK). Shock waves are driven into materials using a portable, single-stage gas gun designed by the Institute of Shock Physics. Following plate impact, material deformation is probed in-situ by white-beam X-ray radiography and complimentary velocimetry diagnostics. The high energies, large beam size (13 x 13 mm), and appreciable sample volumes (~ 1 cm3) viable for study at Beamline I12 compliment existing in-house pulsed X-ray capabilities and studies at the Dynamic Compression Sector. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

  19. Synchrotron radiation and free-electron lasers principles of coherent X-ray generation

    CERN Document Server

    Kim, Kwang-Je; Lindberg, Ryan

    2017-01-01

    Learn about the latest advances in high-brightness X-ray physics and technology with this authoritative text. Drawing upon the most recent theoretical developments, pre-eminent leaders in the field guide readers through the fundamental principles and techniques of high-brightness X-ray generation from both synchrotron and free-electron laser sources. A wide range of topics is covered, including high-brightness synchrotron radiation from undulators, self-amplified spontaneous emission, seeded high-gain amplifiers with harmonic generation, ultra-short pulses, tapering for higher power, free-electron laser oscillators, and X-ray oscillator and amplifier configuration. Novel mathematical approaches and numerous figures accompanied by intuitive explanations enable easy understanding of key concepts, whilst practical considerations of performance-improving techniques and discussion of recent experimental results provide the tools and knowledge needed to address current research problems in the field. This is a comp...

  20. On diamond windows for high power synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Khounsary, A.M.; Kuzay, T.M.

    1991-01-01

    Recent advances in chemical vapor deposition (CVD) technology has made available thin, free-standing polycrystalline diamond foils that can be used as the window material on high heat load synchrotron x-ray beamlines. Diamond windows have many advantages that stem from the exceptionally attractive thermal, structural, and physical properties of diamond. Numerical simulations indicate that diamond windows can offer an attractive and at times the only alternative to beryllium windows for use on the third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, and analytical and numerical results are presented to provide a basis for the design and testing of such windows

  1. A microfocus X-ray fluorescence beamline at Indus-2 synchrotron radiation facility.

    Science.gov (United States)

    Tiwari, M K; Gupta, P; Sinha, A K; Kane, S R; Singh, A K; Garg, S R; Garg, C K; Lodha, G S; Deb, S K

    2013-03-01

    A microfocus X-ray fluorescence spectroscopy beamline (BL-16) at the Indian synchrotron radiation facility Indus-2 has been constructed with an experimental emphasis on environmental, archaeological, biomedical and material science applications involving heavy metal speciation and their localization. The beamline offers a combination of different analytical probes, e.g. X-ray fluorescence mapping, X-ray microspectroscopy and total-external-reflection fluorescence characterization. The beamline is installed on a bending-magnet source with a working X-ray energy range of 4-20 keV, enabling it to excite K-edges of all elements from S to Nb and L-edges from Ag to U. The optics of the beamline comprises of a double-crystal monochromator with Si(111) symmetric and asymmetric crystals and a pair of Kirkpatrick-Baez focusing mirrors. This paper describes the performance of the beamline and its capabilities with examples of measured results.

  2. Progress in X-ray synchrotron diffraction studies of muscle contraction. Ch. 19

    International Nuclear Information System (INIS)

    Wakabayashi, Katsuzo

    1991-01-01

    This chapter provides a review of applications of synchrotron radiation (SR) to X-ray diffraction studies on the dynamic aspects of muscle contraction and is, at the same time, a progress report on the technical developments specifically related to muscle research. The introduction of SR as an intense X-ray source and the development of high ability detectors have led to enormous improvement in the quality of data from time-resolved X-ray diffraction studies of muscle contraction. The X-ray diffraction pattern taken during contraction shows that the force generation of a muscle proceeds upon interaction of the incommensurate structures of the thin and thick filaments. In this framework a distinct intensity change of the weaker reflections from the thin filaments was detected. However, there was still no strong evidence of direct physical attachment of myosin heads to actin during contraction. (author). 170 refs.; 52 figs.; 3 tabs

  3. 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.

  4. High counting rates of x-ray photon detection using APD detectors on synchrotron machines

    Energy Technology Data Exchange (ETDEWEB)

    Kakuno, E. M.; Giacomolli, B. A.; Scorzato, C. R. [Universidade Federal do Pampa - UNIPAMPA-Bage, 96413-170 (Brazil); Laboratorio Nacional de Luz Sincrotron - LNLS, 13086-100 (Brazil)

    2012-05-17

    In this work we show the results of 10 x 10 mm{sup 2} Si-APD detector's test with guard ring detecting x-rays. The result of mapping surface is also exhibited. We show and discuss the difficulty of single photon detection in high counting rate experiments in synchrotrons machines.

  5. Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron ...

    Indian Academy of Sciences (India)

    Abstract. An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from var- ious elemental metals and standard ...

  6. High-pressure phases of uranium monophosphide studied by synchrotron x-ray diffraction

    DEFF Research Database (Denmark)

    Olsen, J. Staun; Gerward, Leif; Benedict, U.

    1988-01-01

    X-ray diffraction studies have been performed on UP powder for pressures up to 51 GPa using synchrotron radiation and a diamond-anvil cell. At ambient pressure UP has the rocksalt structure. The bulk modulus has been determined to B0=102(4) GPa and its pressure derivative to B0’=4.0(8). The cubic...

  7. Synchrotron-based X-ray microscopic studies for bioeffects of nanomaterials.

    Science.gov (United States)

    Zhu, Ying; Cai, Xiaoqing; Li, Jiang; Zhong, Zengtao; Huang, Qing; Fan, Chunhai

    2014-04-01

    There have been increasing interests in studying biological effects of nanomaterials, which are nevertheless faced up with many challenges due to the nanoscale dimensions and unique chemical properties of nanomaterials. Synchrotron-based X-ray microscopy, an advanced imaging technology with high spatial resolution and excellent elemental specificity, provides a new platform for studying interactions between nanomaterials and living systems. In this article, we review the recent progress of X-ray microscopic studies on bioeffects of nanomaterials in several living systems including cells, model organisms, animals and plants. We aim to provide an overview of the state of the art, and the advantages of using synchrotron-based X-ray microscopy for characterizing in vitro and in vivo behaviors and biodistribution of nanomaterials. We also expect that the use of a combination of new synchrotron techniques should offer unprecedented opportunities for better understanding complex interactions at the nano-biological interface and accounting for unique bioeffects of nanomaterials. Synchrotron-based X-ray microscopy is a non-destructive imaging technique that enables high resolution spatial mapping of metals with elemental level detection methods. This review summarizes the current use and perspectives of this novel technique in studying the biology and tissue interactions of nanomaterials. Copyright © 2014 Elsevier Inc. All rights reserved.

  8. A Spectrometer for X-Ray Energy-Dispersive Diffraction using Synchrotron Radiation

    DEFF Research Database (Denmark)

    Staun Olsen, Janus; Buras, B; Gerward, Leif

    1981-01-01

    Describes a white-beam X-ray energy-dispersive diffractometer built for Hasylab in Hamburg, FRG, using the synchrotron radiation from the electron storage ring DORIS. The following features of the instrument are discussed: horizontal or vertical scattering plane, collimators, sample environment, ...

  9. Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron ...

    Indian Academy of Sciences (India)

    An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from various elemental metals and standard inorganic ...

  10. CCD [charge-coupled device] sensors in synchrotron x-ray detectors

    International Nuclear Information System (INIS)

    Strauss, M.G.; Naday, I.; Sherman, I.S.; Kraimer, M.R.; Westbrook, E.M.; Zaluzec, N.J.

    1987-01-01

    The intense photon flux from advanced synchrotron light sources, such as the 7-GeV synchrotron being designed at Argonne, require integrating-type detectors. Charge-coupled devices (CCDs) are well suited as synchrotron x-ray detectors. When irradiated indirectly via a phosphor followed by reducing optics, diffraction patterns of 100 cm 2 can be imaged on a 2 cm 2 CCD. With a conversion efficiency of ∼1 CCD electron/x-ray photon, a peak saturation capacity of >10 6 x rays can be obtained. A programmable CCD controller operating at a clock frequency of 20 MHz has been developed. The readout rate is 5 x 10 6 pixels/s and the shift rate in the parallel registers is 10 6 lines/s. The test detector was evaluated in two experiments. In protein crystallography diffraction patterns have been obtained from a lysozyme crystal using a conventional rotating anode x-ray generator. Based on these results we expect to obtain at a synchrotron diffraction images at the rate of ∼1 frame/s or a complete 3-dimensional data set from a single crystal in ∼2 min. 16 refs., 16 figs., 2 tabs

  11. Atomic physics with hard X-rays from high brilliance synchrotron light sources

    International Nuclear Information System (INIS)

    Southworth, S.; Gemmell, D.

    1996-08-01

    A century after the discovery of x rays, the experimental capability for studying atomic structure and dynamics with hard, bright synchrotron radiation is increasing remarkably. Tempting opportunities arise for experiments on many-body effects, aspects of fundamental photon-atom interaction processes, and relativistic and quantum-electrodynamic phenomena. Some of these possibilities are surveyed in general terms

  12. Fabrication of nested elliptical KB mirrors using profile coating for synchrotron radiation X-ray focusing

    International Nuclear Information System (INIS)

    Liu Chian; Ice, G.E.; Liu, W.; Assoufid, L.; Qian, J.; Shi, B.; Khachatryan, R.; Wieczorek, M.; Zschack, P.; Tischler, J.Z.

    2012-01-01

    This paper describes fabrication methods used to demonstrate the advantages of nested or Montel optics for micro/nanofocusing of synchrotron X-ray beams. A standard Kirkpatrick-Baez (KB) mirror system uses two separated elliptical mirrors at glancing angles to the X-ray beam and sequentially arranged at 90° to each other to focus X-rays successively in the vertical and horizontal directions. A nested KB mirror system has the two mirrors positioned perpendicular and side-by-side to each other. Compared to a standard KB mirror system, Montel optics can focus a larger divergence and the mirrors can have a shorter focal length. As a result, nested mirrors can be fabricated with improved demagnification factor and ultimately smaller focal spot, than with a standard KB arrangement. The nested system is also more compact with an increased working distance, and is more stable, with reduced complexity of mirror stages. However, although Montel optics is commercially available for laboratory X-ray sources, due to technical difficulties they have not been used to microfocus synchrotron radiation X-rays, where ultra-precise mirror surfaces are essential. The main challenge in adapting nested optics for synchrotron microfocusing is to fabricate mirrors with a precise elliptical surface profile at the very edge where the two mirrors meet and where X-rays scatter. For example, in our application to achieve a sub-micron focus with high efficiency, a surface figure root-mean-square (rms) error on the order of 1 nm is required in the useable area along the X-ray footprint with a ∼0.1 mm-diameter cross section. In this paper we describe promising ways to fabricate precise nested KB mirrors using our profile coating technique and inexpensive flat Si substrates.

  13. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources

    International Nuclear Information System (INIS)

    Rutherford, Michael E.; Chapman, David J.; White, Thomas G.; Drakopoulos, Michael; Rack, Alexander; Eakins, Daniel E.

    2016-01-01

    Scintillator performance in time-resolved, hard, indirect detection X-ray studies on the sub-microsecond timescale at synchrotron light sources is reviewed, modelled and examined experimentally. LYSO:Ce is found to be the only commercially available crystal suitable for these experiments. The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits)

  14. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources

    Energy Technology Data Exchange (ETDEWEB)

    Rutherford, Michael E.; Chapman, David J.; White, Thomas G. [Imperial College London, London (United Kingdom); Drakopoulos, Michael [Diamond Light Source, I12 Joint Engineering, Environmental, Processing (JEEP) Beamline, Didcot, Oxfordshire (United Kingdom); Rack, Alexander [European Synchrotron Radiation Facility, Grenoble (France); Eakins, Daniel E., E-mail: d.eakins@imperial.ac.uk [Imperial College London, London (United Kingdom)

    2016-03-24

    Scintillator performance in time-resolved, hard, indirect detection X-ray studies on the sub-microsecond timescale at synchrotron light sources is reviewed, modelled and examined experimentally. LYSO:Ce is found to be the only commercially available crystal suitable for these experiments. The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits)

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

    Science.gov (United States)

    Pan, Jianjun; Cheng, Xiaolin; Sharp, Melissa; Ho, Chian-Sing; Khadka, Nawal; Katsaras, John

    2015-01-07

    The detailed structural and mechanical properties of a tetraoleoyl cardiolipin (TOCL) bilayer were determined using neutron spin echo (NSE) spectroscopy, small angle neutron and X-ray scattering (SANS and SAXS, respectively), and molecular dynamics (MD) simulations. We used MD simulations to develop a scattering density profile (SDP) model, which was then utilized to jointly refine SANS and SAXS data. In addition to commonly reported lipid bilayer structural parameters, component distributions were obtained, including the volume probability, electron density and neutron scattering length density. Of note, the distance between electron density maxima DHH (39.4 Å) and the hydrocarbon chain thickness 2DC (29.1 Å) of TOCL bilayers were both found to be larger than the corresponding values for dioleoyl phosphatidylcholine (DOPC) bilayers. Conversely, TOCL bilayers have a smaller overall bilayer thickness DB (36.7 Å), primarily due to their smaller headgroup volume per phosphate. SDP analysis yielded a lipid area of 129.8 Å(2), indicating that the cross-sectional area per oleoyl chain in TOCL bilayers (i.e., 32.5 Å(2)) is smaller than that for DOPC bilayers. Multiple sets of MD simulations were performed with the lipid area constrained at different values. The calculated surface tension versus lipid area resulted in a lateral area compressibility modulus KA of 342 mN m(-1), which is slightly larger compared to DOPC bilayers. Model free comparison to experimental scattering data revealed the best simulated TOCL bilayer from which detailed molecular interactions were determined. Specifically, Na(+) cations were found to interact most strongly with the glycerol hydroxyl linkage, followed by the phosphate and backbone carbonyl oxygens. Inter- and intra-lipid interactions were facilitated by hydrogen bonding between the glycerol hydroxyl and phosphate oxygen, but not with the backbone carbonyl. Finally, analysis of the intermediate scattering functions from NSE

  16. Structural analysis and characterization of synthesized ordered mesoporous silicate (MCM-41) using small angle X-rays scattering and complementary techniques

    Science.gov (United States)

    Akinlalu, Ademola V.

    Mesoporous silicate have widespread potential applications, such as drug delivery, supports for catalysis, selective adsorption and host to guest molecules. Most important in the area of scientific research and industrial applications is their demand due to its extremely high surface areas (> 800m 2g-1) and larger pores with well defined structures. Mesoporous silicate (MCM-41) samples were prepared by hydrothermal method under various chemo-physical conditions and various experimental methods such as small angle X-rays scattering (SAXS), Nitrogen adsorption-desorption analysis at 77 K, Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) were employed to investigate the changes in the structural morphology and subtle lattice parameter changes. With regards to the subtle changes in the structural characteristics of the synthesized mesoporous silicate, we seek to understand the electron density function changes as the synthesis parameter are varied from low molar concentration of ATAB/Si to higher concentration, the system becoming more acidity due to increase in the hydrolysis time of pH regulator as a result of increased production of ethanol and acetic acid and the changes due to extended reaction time. This Ph.D. research tries to understand the influence of various parameters like surfactant-Si molar ratio, reaction time, and the hydrolysis of the pH regulator on the orderliness/disorderliness of the lattice order, lattice spacing and electron density function. The stages during synthesis are carefully selected to better understand where the greater influence on the overall structural morphology exist so as to be able to ne tune this parameter for any desired specification and application. The SAXS measurement were conducted on a HECUS S3-Micro X-ray system at Rensselaer Polytechnic Institute, Troy, NY. while the data evaluation and visualization were carried in 3DView 4.2 and EasySWAXS software. The electron density functions

  17. Synchrotron radiation X-ray powder diffraction techniques applied in hydrogen storage materials - A review

    Directory of Open Access Journals (Sweden)

    Honghui Cheng

    2017-02-01

    Full Text Available Synchrotron radiation is an advanced collimated light source with high intensity. It has particular advantages in structural characterization of materials on the atomic or molecular scale. Synchrotron radiation X-ray powder diffraction (SR-XRPD has been successfully exploited to various areas of hydrogen storage materials. In the paper, we will give a brief introduction on hydrogen storage materials, X-ray powder diffraction (XRPD, and synchrotron radiation light source. The applications of ex situ and in situ time-resolved SR-XRPD in hydrogen storage materials, are reviewed in detail. Future trends and proposals in the applications of the advanced XRPD techniques in hydrogen storage materials are also discussed.

  18. A powerful flare from Sgr A* confirms the synchrotron nature of the X-ray emission

    Science.gov (United States)

    Ponti, G.; George, E.; Scaringi, S.; Zhang, S.; Jin, C.; Dexter, J.; Terrier, R.; Clavel, M.; Degenaar, N.; Eisenhauer, F.; Genzel, R.; Gillessen, S.; Goldwurm, A.; Habibi, M.; Haggard, D.; Hailey, C.; Harrison, F.; Merloni, A.; Mori, K.; Nandra, K.; Ott, T.; Pfuhl, O.; Plewa, P. M.; Waisberg, I.

    2017-06-01

    We present the first fully simultaneous fits to the near-infrared (NIR) and X-ray spectral slope (and its evolution) during a very bright flare from Sgr A*, the supermassive black hole at the Milky Way's centre. Our study arises from ambitious multiwavelength monitoring campaigns with XMM-Newton, NuSTAR and SINFONI. The average multiwavelength spectrum is well reproduced by a broken power law with ΓNIR = 1.7 ± 0.1 and ΓX = 2.27 ± 0.12. The difference in spectral slopes (ΔΓ = 0.57 ± 0.09) strongly supports synchrotron emission with a cooling break. The flare starts first in the NIR with a flat and bright NIR spectrum, while X-ray radiation is detected only after about 103 s, when a very steep X-ray spectrum (ΔΓ = 1.8 ± 0.4) is observed. These measurements are consistent with synchrotron emission with a cooling break and they suggest that the high-energy cut-off in the electron distribution (γmax) induces an initial cut-off in the optical-UV band that evolves slowly into the X-ray band. The temporal and spectral evolution observed in all bright X-ray flares are also in line with a slow evolution of γmax. We also observe hints for a variation of the cooling break that might be induced by an evolution of the magnetic field (from B ˜ 30 ± 8 G to B ˜ 4.8 ± 1.7 G at the X-ray peak). Such drop of the magnetic field at the flare peak would be expected if the acceleration mechanism is tapping energy from the magnetic field, such as in magnetic reconnection. We conclude that synchrotron emission with a cooling break is a viable process for Sgr A*'s flaring emission.

  19. On diamond windows for high power synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Khounsary, A.M.; Kuzay, T.M.

    1992-01-01

    X-ray windows are often used on the front end of synchrotron beamlines to isolate the ultra high vacuum of the storage ring from the downstream environment. The windows are usually made of low atomic number materials, such as beryllium, for maximum x-ray transmission, and they must survive and remain vacuum tight during repeated thermal cycles. The intense x-ray beams generated by the wigglers and undulators at high energy storage rings can deposit substantial amounts of localized heat in the (actively cooled) windows leading to high temperatures, and vacuum or structural failure. Thermal filters upstream of the windows can be used to reduce the radiation absorbed in the windows. This solution has limitations, however, since a small amount of filtering may still leave an unacceptable amount of heat to be absorbed in the windows, while substantial filtering will absorb a large amount of the useful photons. Recent advances in chemical vapor deposition (CVD) technology has made available thin, free-standing polycrystalline diamond films that can be used as the window material on high heat load synchrotron x-ray beamlines. Diamond windows have many advantages that stem from the exceptional thermal, structural, and physical properties of diamond. Numerical simulation indicates that diamond windows offer an attractive alternative to beryllium windows for use on the third generation x-ray synchrotron radiation beamlines. Utilization, design, and fabrication aspects of diamond windows for high heat load x-ray beamlines are discussed, and analytical results are presented to provide a basis for design and testing of such windows

  20. X-ray phase contrast imaging: From synchrotrons to conventional sources

    International Nuclear Information System (INIS)

    Olivo, A.; Castelli, E.

    2014-01-01

    Phase-based approaches can revolutionize X-ray imaging and remove its main limitation: poor image contrast arising from low attenuation differences. They exploit the unit decrement of the real part of the refractive index, typically 1000 times larger than the imaginary part driving attenuation. This increases the contrast of all details, and enables the detection of features classically considered 'X-ray invisible'. Following pioneering experiments dating back to the mid-sixties, X-ray phase contrast imaging 'exploded' in the mid-nineties, when third generation synchrotron sources became more widely available. Applications were proposed in fields as diverse as material science, palaeontology, biology, food science, cultural heritage preservation, and many others. Among these applications, medicine has been constantly considered the most important; among medical applications, mammography is arguably the one that attracted most attention. Applications to mammography were pioneered by the SYRMEP (SYnchrotron Radiation for MEdical Physics) group in Trieste, which was already active in the area through a combination of innovative ways to do imaging at synchrotrons and development of novel X-ray detectors. This pioneering phase led to the only clinical experience of phase contrast mammography on human patients, and spawned a number of ideas as to how these advances could be translated into clinical practice.

  1. Synchrotron X-ray adaptative monochromator: study and realization of a prototype

    International Nuclear Information System (INIS)

    Dezoret, D.

    1995-01-01

    This work presents a study of a prototype of a synchrotron X-ray monochromator. The spectral qualities of this optic are sensitive to the heat loads which are particularly important on third synchrotron generation like ESRF. Indeed, powers generated by synchrotron beams can reach few kilowatts and power densities about a few tens watts per square millimeters. The mechanical deformations of the optical elements of the beamlines issue issue of the heat load can damage their spectral efficiencies. In order to compensate the deformations, wa have been studying the transposition of the adaptive astronomical optics technology to the x-ray field. First, we have considered the modifications of the spectral characteristics of a crystal induced by x-rays. We have established the specifications required to a technological realisation. Then, thermomechanical and technological studies have been required to transpose the astronomical technology to an x-ray technology. After these studies, we have begun the realisation of a prototype. This monochromator is composed by a crystal of silicon (111) bonded on a piezo-electric structure. The mechanical control is a loop system composed by a infrared light, a Shack-Hartmann CDD and wave front analyser. This system has to compensate the deformations of the crystal in the 5 kcV to 60 kcV energy range with a power density of 1 watt per square millimeters. (authors)

  2. X-ray detectors for diffraction studies and their use with synchrotron radiation

    International Nuclear Information System (INIS)

    Milch, J.

    1976-02-01

    All techniques for X-ray diffraction studies on biological materials exhibit certain limitations. The characteristics of several X-ray detection systems, namely film, multiwire proportional counter and image intensified TV, are discussed and compared for application to specific biological studies. For the high count-rate situation existing at a synchrotron, it is shown that film is a good choice, but that the image intensified TV exhibits significant advantages. The details of such a system now being used at Princeton with a low intensity source are given and current results presented

  3. Antiferroelectric surface layers in a liquid crystal as observed by synchrotron x-ray scattering

    DEFF Research Database (Denmark)

    Gramsbergen, E. F.; de Jeu, W. H.; Als-Nielsen, Jens Aage

    1986-01-01

    The X-ray reflectivity form the surface of a liquid crystal with terminally polar (cyano substituted) molecules has been studied using a high-resolution triple-axis X-ray spectrometer in combination with a synchrotron source. It is demonstrated that at the surface of the smectic Al phase a few...... antiferroelectric double layers develop that can be distinguished from the bulk single layer structure. A model is developed that separates the electron density in a contribution from the molecular form factor, and from the structure factor of the mono- and the bilayers, respectively. It shows that (i) the first...

  4. A Furnace for Diffraction Studies using Synchrotron X-Ray Radiation

    DEFF Research Database (Denmark)

    Buras, B.; Lebech, Bente; Kofoed, W.

    1984-01-01

    A furnace for diffraction studies using synchrotron X-ray radiation is described. The furnace can be operated between ambient temperature and 1 800 °C with a temperature stability better than 5 °C for temperatures above 300 °C. Kapton windows allow almost 360° access for the X-ray beam in the hor...... in the horizontal scattering plane and the furnace may be used in both conventional monochromatic beam angle-dispersive and white-beam energy-dispersive diffraction experiments. Details of the furnace windows, heating element, thermometry and sample mount are given....

  5. Synchrotron X-ray and neutron diffraction studies in solid-state chemistry

    International Nuclear Information System (INIS)

    Cheetham, A.K.; Wilkinson, A.P.

    1992-01-01

    Since the scatterers are different - X-rays are scattered by the electrons of an atom, neutrons by the nuclei - the questions addressed by the two diffraction experiments have been complementary. For example, neighboring elements of the periodic table could be distinguished formerly only by neutron diffraction. Now, however, this is also partly possible with high-energy synchrotron radiation. This review describes recent applications of X-ray and neutron diffraction methods in solid-state chemistry and how the maximal information can be extracted by a combination of techniques. (orig.)

  6. X-ray fluorescence in Member States: Austria. Synchrotron radiation induced TXRF-XANES

    International Nuclear Information System (INIS)

    Meirer, Florian; Wobrauschek, Peter; Streli, Christina; Pepponi, Giancarlo

    2009-01-01

    X ray Absorption Near Edge Structure (XANES) analysis was used in combination with Total reflection X ray Fluorescence (TXRF) at different Synchrotron Radiation (SR) facilities to perform elemental analysis and speciation at trace levels. TXRF-XANES was used to perform analysis of contaminations on Silicon wafer surfaces and determine the oxidation state of Fe. Urban aerosols were sampled size fractioned and the oxidation state of Fe was determined for each impactor stage again using TXRF-XANES. The feasibility of XANES analysis at trace element levels using different SR-XRF setups was demonstrated. (author)

  7. Advanced Nanoscale Characterization of Cement Based Materials Using X-Ray Synchrotron Radiation: A Review

    KAUST Repository

    Chae, Sejung R.

    2013-05-22

    We report various synchrotron radiation laboratory based techniques used to characterize cement based materials in nanometer scale. High resolution X-ray transmission imaging combined with a rotational axis allows for rendering of samples in three dimensions revealing volumetric details. Scanning transmission X-ray microscope combines high spatial resolution imaging with high spectral resolution of the incident beam to reveal X-ray absorption near edge structure variations in the material nanostructure. Microdiffraction scans the surface of a sample to map its high order reflection or crystallographic variations with a micron-sized incident beam. High pressure X-ray diffraction measures compressibility of pure phase materials. Unique results of studies using the above tools are discussed-a study of pores, connectivity, and morphology of a 2,000 year old concrete using nanotomography; detection of localized and varying silicate chain depolymerization in Al-substituted tobermorite, and quantification of monosulfate distribution in tricalcium aluminate hydration using scanning transmission X-ray microscopy; detection and mapping of hydration products in high volume fly ash paste using microdiffraction; and determination of mechanical properties of various AFm phases using high pressure X-ray diffraction. © 2013 The Author(s).

  8. Energy Dependence of Synchrotron X-Ray Rims in Tycho's Supernova Remnant

    Science.gov (United States)

    Tran, Aaron; Williams, Brian J.; Petre, Robert; Ressler, Sean M.; Reynolds, Stephen P.

    2015-01-01

    Several young supernova remnants exhibit thin X-ray bright rims of synchrotron radiation at their forward shocks. Thin rims require strong magnetic field amplification beyond simple shock compression if rim widths are only limited by electron energy losses. But, magnetic field damping behind the shock could produce similarly thin rims with less extreme field amplification. Variation of rim width with energy may thus discriminate between competing influences on rim widths. We measured rim widths around Tycho's supernova remnant in 5 energy bands using an archival 750 ks Chandra observation. Rims narrow with increasing energy and are well described by either loss-limited or damped scenarios, so X-ray rim width-energy dependence does not uniquely specify a model. But, radio counterparts to thin rims are not loss-limited and better reflect magnetic field structure. Joint radio and X-ray modeling favors magnetic damping in Tycho's SNR with damping lengths approximately 1-5% of remnant radius and magnetic field strengths approximately 50-400 micron G assuming Bohm diffusion. X-ray rim widths are approximately 1% of remnant radius, somewhat smaller than inferred damping lengths. Electron energy losses are important in all models of X-ray rims, suggesting that the distinction between loss-limited and damped models is blurred in soft X-rays. All loss-limited and damping models require magnetic fields approximately greater than 20 micron G, arming the necessity of magnetic field amplification beyond simple compression.

  9. Optimizing a synchrotron based x-ray lithography system for IC manufacturing

    Science.gov (United States)

    Kovacs, Stephen; Speiser, Kenneth; Thaw, Winston; Heese, Richard N.

    1990-05-01

    The electron storage ring is a realistic solution as a radiation source for production grade, industrial X-ray lithography system. Today several large scale plans are in motion to design and implement synchrotron storage rings of different types for this purpose in the USA and abroad. Most of the scientific and technological problems related to the physics, design and manufacturing engineering, and commissioning of these systems for microlithography have been resolved or are under extensive study. However, investigation on issues connected to application of Synchrotron Orbit Radiation (SOR ) in chip production environment has been somewhat neglected. In this paper we have filled this gap pointing out direct effects of some basic synchrotron design parameters and associated subsystems (injector, X-ray beam line) on the operation and cost of lithography in production. The following factors were considered: synchrotron configuration, injection energy, beam intensity variability, number of beam lines and wafer exposure concept. A cost model has been worked out and applied to three different X-ray Lithography Source (XLS) systems. The results of these applications are compared and conclusions drawn.

  10. Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries.

    Science.gov (United States)

    Lin, Feng; Liu, Yijin; Yu, Xiqian; Cheng, Lei; Singer, Andrej; Shpyrko, Oleg G; Xin, Huolin L; Tamura, Nobumichi; Tian, Chixia; Weng, Tsu-Chien; Yang, Xiao-Qing; Meng, Ying Shirley; Nordlund, Dennis; Yang, Wanli; Doeff, Marca M

    2017-11-08

    Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancement of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allow for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy, and imaging) and their successful applications (ex situ, in situ, and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools and are also discussed toward the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution, because a sole

  11. Microfocussing of synchrotron X-rays using X-ray refractive lens developed at Indus-2 deep X-ray lithography beamline

    International Nuclear Information System (INIS)

    Dhamgaye, V.P.; Tiwari, M.K.; Lodha, G.S.; Sawhney, K.J.S.

    2014-01-01

    X-ray lenses are fabricated in polymethyl methacrylate using deep X-ray lithography beamline of Indus-2. The focussing performance of these lenses is evaluated using Indus-2 and Diamond Light Source Ltd. The process steps for the fabrication of X-ray lenses and microfocussing at 10 keV at moderate and low emittance sources are compared. (author)

  12. A new high-resolution small-angle X-ray scattering apparatus using a fine-focus rotating anode, point-focusing collimation and a position-sensitive proportional counter

    International Nuclear Information System (INIS)

    Yoda, O.

    1984-01-01

    A high-resolution small-angle X-ray scattering camera has been built, which has the following features. (i) The point collimation optics employed allows the scattering cross section of the sample to be directly measured without corrections for desmearing. (ii) A small-angle resolution better than 0.5 mrad is achieved with a camera length of 1.6 m. (iii) A high photon flux of 0.9 photons μs -1 is obtained on the sample with the rotating-anode X-ray generator operated at 40 kV-30 mA. (iv) Incident X-rays are monochromatized by a bent quartz crystal, which makes the determination of the incident X-ray intensity simple and unambiguous. (v) By rotation of the position-sensitive proportional counter around the direct beam, anisotropic scattering patterns can be observed without adjusting the sample. Details of the design and performance are presented with some applications. (Auth.)

  13. ORNL-SAS: Versatile software for calculation of small-angle x-ray and neutron scattering intensity profiles from arbitrary structures

    International Nuclear Information System (INIS)

    Heller, William T; Tjioe, Elina

    2007-01-01

    ORNL-SAS is software for calculating solution small-angle scattering intensity profiles from any structure provided in the Protein Data Bank format and can also compare the results with experimental data

  14. Phase-contrast computed microtomography with 50 keV synchrotron x-rays

    International Nuclear Information System (INIS)

    Raven, C.; Snigirev, A.; Snigireva, I.; Spanne, P.; Suvorov, A.

    1996-01-01

    The possibilities to determine the internal structure of low density materials by a simple microtomography setup with high energy synchrotron x-rays are demonstrated experimentally. The coherent properties of a 50 keV x-ray beam at the ESRF wiggler beamline are used to observe phase-contrast images of a boron fiber, which has negligible absorption in this energy range. Images of the boron fiber are recorded with a high-resolution x-ray film at various distances up to 2 m. For microtomography studies, 61 images are taken over an angular range of 180 degrees. In the reconstructed cross sections, the hollow, 15-mm-diameter core of the fiber is clearly visible. copyright 1996 American Institute of Physics

  15. Diamond monochromator for high heat flux synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Khounsary, A.M.; Smither, R.K.; Davey, S.; Purohit, A.

    1992-12-01

    Single crystal silicon has been the material of choice for x-ray monochromators for the past several decades. However, the need for suitable monochromators to handle the high heat load of the next generation synchrotron x-ray beams on the one hand and the rapid and on-going advances in synthetic diamond technology on the other make a compelling case for the consideration of a diamond mollochromator system. In this Paper, we consider various aspects, advantage and disadvantages, and promises and pitfalls of such a system and evaluate the comparative an monochromator subjected to the high heat load of the most powerful x-ray beam that will become available in the next few years. The results of experiments performed to evaluate the diffraction properties of a currently available synthetic single crystal diamond are also presented. Fabrication of diamond-based monochromator is within present technical means

  16. Characterisation of microfocused beam for synchrotron powder diffraction using a new X-ray camera

    International Nuclear Information System (INIS)

    Thomas, C; Potter, J; Tang, C C; Lennie, A R

    2012-01-01

    The powder diffraction beamline I11, Diamond Light Source, is being continually upgraded as requirements of the user community evolve. Intensities of X-rays from the I11 in-vacuum electron undulator in the 3 GeV synchrotron fall off at higher energies. By focusing higher energy X-rays, we can overcome flux limitations, and open up new diffraction experiments. Here, we describe characterisation of microfocusing using compound refractive lenses (CRL). For a relatively modest outlay, we have developed an experimental setup and a novel X-ray camera with good sensitivity and a resolution specification suitable for characterising these focusing optics. We show that vertical oscillations in the focused beam compromise resolution of the source imaged by the CRL. Nevertheless, we have measured CRL focusing properties, and demonstrate the use of energy scanning to determine lens alignment. Real benefits of the intensity gain are illustrated.

  17. Synchrotron-Radiation X-Ray Investigation of Li+/Na+ Intercalation into Prussian Blue Analogues

    Directory of Open Access Journals (Sweden)

    Yutaka Moritomo

    2013-01-01

    Full Text Available Prussian blue analogies (PBAs are promising cathode materials for lithium ion (LIB and sodium ion (SIB secondary batteries, reflecting their covalent and nanoporous host structure. With use of synchrotron-radiation (SR X-ray source, we investigated the structural and electronic responses of the host framework of PBAs against Li+ and Na+ intercalation by means of the X-ray powder diffraction (XRD and X-ray absorption spectroscopy (XAS. The structural investigation reveals a robust nature of the host framework against Li+ and Na+ intercalation, which is advantageous for the stability and lifetime of the batteries. The spectroscopic investigation identifies the redox processes in respective plateaus in the discharge curves. We further compare these characteristics with those of the conventional cathode materials, such as, LiCoO2, LiFePO4, and LiMn2O4.

  18. Optimizing Monocapillary Optics for Synchrotron X-ray Diffraction, Fluorescence Imaging, and Spectroscopy Applications

    International Nuclear Information System (INIS)

    Bilderback, Donald H.; Kazimirov, Alexander; Gillilan, Richard; Cornaby, Sterling; Woll, Arthur; Zha, Chang-Sheng; Huang Rong

    2007-01-01

    A number of synchrotron x-ray applications such as powder diffraction in diamond anvil cells, microbeam protein crystallography, x-ray fluorescence imaging, etc. can benefit from using hollow glass monocapillary optics to improve the flux per square micron on a sample. We currently draw glass tubing into the desired elliptical shape so that only one-bounce under total reflection conditions is needed to bring the x-ray beam to a focus at a 25 to 50 mm distance beyond the capillary tip. For modest focal spot sizes of 10 to 20 microns, we can increase the intensity per square micron by factors of 10 to 1000. We show some of the results obtained at CHESS and Hasylab with capillaries focusing 5 to 40 keV radiation, their properties, and how even better the experimental results could be if more ideal capillaries were fabricated in the future

  19. New insights into nucleation. Pressure trace measurements and the first small angle X-ray scattering experiments in a supersonic laval nozzle

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, D.

    2007-07-01

    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/{delta}t{sub Jmax} for the n-alcohols are in the range of 1.10{sup 17}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{sup 12}

  20. 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

  1. 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

  2. Beer analysis by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Recursos Hidricos]. E-mail: silvana@fec.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br; Zucchi, Orgheda L.D.A. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas de Ribeirao Preto]. E-mail: olzucchi@fcfrp.usp.br

    2005-07-01

    In this work the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian Legislation and the nutritive values established by National Agricultural Library (NAL). The measurements were performed at the X-ray Fluorescence Beamline at Synchrotron Light Source Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 {mu}L of sample beers containing just an internal standard, used to correct geometry effects, were analyzed without any pre-treatment. The measuring time was 100 s and the detection limits obtained varied from 1{mu}g.L{sup -1} for Mn and Fe to 15{mu}g.L{sup -1} for P. (author)

  3. Beer analysis by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF)

    International Nuclear Information System (INIS)

    Moreira, Silvana; Vives, Ana Elisa S. de; Nascimento Filho, Virgilio F.; Zucchi, Orgheda L.D.A.

    2005-01-01

    In this work the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian Legislation and the nutritive values established by National Agricultural Library (NAL). The measurements were performed at the X-ray Fluorescence Beamline at Synchrotron Light Source Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 μL of sample beers containing just an internal standard, used to correct geometry effects, were analyzed without any pre-treatment. The measuring time was 100 s and the detection limits obtained varied from 1μg.L -1 for Mn and Fe to 15μg.L -1 for P. (author)

  4. Analysis of beers from Brazil with synchrotron radiation total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Moreira, S.; Vives, A.E.S.; Brienza, S.M.B.; Zucchi, O.L.A.D.; Jesus, E.F.O. de; Nascimento Filho, V.F.

    2006-01-01

    In this study the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian legislation and the nutritional values established by National Agricultural Library (NAL, USA). The measurements were performed at the X-Ray Fluorescence Beamline at Brazilian National Synchrotron Light Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 μl of beers containing an internal standard used to correct geometry effects was analyzed without pretreatment. The measuring time was 100 seconds and the detection limits obtained varied from 1 μg x l -1 for Mn and Fe to 15 μg x l -1 for P. (author)

  5. National Synchrotron Light Source users manual: Guide to the VUV and x-ray beam lines

    International Nuclear Information System (INIS)

    Gmuer, N.F.; White-DePace, S.M.

    1987-08-01

    The success of the National Synchrotron Light Source in the years to come will be based, in large part, on the size of the users community and the diversity of the scientific disciplines represented by these users. In order to promote this philosophy, this National Synchrotron Light Source (NSLS) Users Manual: Guide to the VUV and X-Ray Beam Lines, has been published. This manual serves a number of purposes. In an effort to attract new research, it will present to the scientific community-at-large the current and projected architecture and capabilities of the various VUV and x-ray beam lines and storage rings. We anticipate that this publication will be updated periodically in order to keep pace with the constant changes at the NSLS

  6. Nondestructive analysis of silver in gold foil using synchrotron radiation X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Kasamatsu, Masaaki; Suzuki, Yasuhiro; Suzuki, Shinichi; Nakanishi, Toshio; Shimoda, Osamu; Nishiwaki, Yoshinori; Miyamoto, Naoki

    2005-01-01

    Small particles of gold foil detached from an indoor decoration might be important evidence to associate a suspect with a crime scene. We have investigated the application of elemental analysis using synchrotron radiation X-ray fluorescence spectrometry to discriminate small particles of gold foil. Eight kinds of gold foil samples collected in Japan were used in the experiments. As a result of synchrotron radiation X-ray fluorescence spectrometry, only two elements, gold and silver, were detected from all gold foil samples. The intensity ratios of AgK α /AuL α showed good correlation with the content ratios of Ag/Au. The variation of intensity ratio within a same sample was sufficiently small compared with those of different samples. Therefore the comparison of this intensity ratio can be an effective method to discriminate small particles originating from different types of gold foil. (author)

  7. Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

    Science.gov (United States)

    Boggon, T. J.; Helliwell, J. R.; Judge, Russell A.; Siddons, D. P.; Snell, Edward H.; Stojanoff, V.

    2000-01-01

    A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

  8. Synchrotron X-ray CT of rose peduncles. Evaluation of tissue damage by radiation

    Energy Technology Data Exchange (ETDEWEB)

    Herppich, Werner B. [Leibniz-Institut fuer Agrartechnik Potsdam-Bornim e.V., Potsdam (Germany). Abt. Technik im Gartenbau; Matsushima, Uzuki [Iwate Univ., Morioka (Japan). Faculty of Agriculture; Graf, Wolfgang [Association for Technology and Structures in Agriculture (KTBL), Darmstadt (Germany); Zabler, Simon [Fraunhofer-Institut fuer Integrierte Schaltungen (IIS), Wuerzburg (Germany). Project group NanoCT Systems (NCTS); Dawson, Martin [Salford Univ., Greater Manchester (United Kingdom); Choinka, Gerard; Manke, Ingo [Helmholtz Center Berlin for Materials and Energy (HZB), Berlin (Germany)

    2015-02-01

    ''Bent-neck'' syndrome, an important postharvest problem of cut roses, is probably caused by water supply limitations and/or the structural weakness of vascular bundles of the peduncle tissue. For this reason, advanced knowledge about the microstructures of rose peduncles and their cultivar specific variations may lead to a better understanding of the underlying mechanisms. Synchrotron X-ray computed tomography (SXCT), especially phase-based CT, is a highly suitable technique to nondestructively investigate plants' micro anatomy. SXCT with monochromatic X-ray beams of 30, 40 and 50 keV photon energy was used to evaluate the three-dimensional inner structures of the peduncles of 3 rose cultivars that differ greatly in their bent-neck susceptibility. Results indicated that this technique achieves sufficiently high spatial resolution to investigate complex tissues. However, further investigations with chlorophyll fluorescence analysis (CFA) and optical microscope imagery reveal different kinds of heavy damage of the irradiated regions induced by synchrotron X-rays; in a cultivar-specific manner, partial destruction of cell walls occurred a few hours after X-ray irradiation. Furthermore, a delayed inhibition of photosynthesis accompanied by the degradation of chlorophyll was obvious from CFA within hours and days after the end of CT measurements. Although SXCT is certainly well suited for three-dimensional anatomical analysis of rose peduncles, the applied technique is not nondestructive.

  9. Electron density measurement with dual-energy x-ray CT using synchrotron radiation

    International Nuclear Information System (INIS)

    Torikoshi, Masami; Tsunoo, Takanori; Sasaki, Makoto; Endo, Masahiro; Noda, Yutaka; Ohno, Yumiko; Kohno, Toshiyuki; Hyodo, Kazuyuki; Uesugi, Kentaro; Yagi, Naoto

    2003-01-01

    Monochromatic x-ray computed tomography (CT) at two different energies provides information about electron density of human tissue without ambiguity due to the beam hardening effect. This information makes the treatment planning for proton and heavy-ion radiotherapy more precise. We have started a feasibility study on dual energy x-ray CT by using synchrotron radiation. A translation-rotation scanning CT system was developed for quantitative measurement in order to clarify what precision in the measurement was achieved. Liquid samples of solutions of K 2 HPO 4 and solid samples of tissue equivalent materials were used to simulate human tissue. The experiments were carried out using monochromatic x-rays with energies of 40, 70 and 80 keV produced by monochromatizing synchrotron radiation. The solid samples were also measured in a complementary method using high-energy carbon beams to evaluate the electron densities. The measured electron densities were compared with the theoretical values or the values measured in the complementary method. It was found that these values were in agreement in 0.9% on average. Effective atomic numbers were obtained as well from dual-energy x-ray CT. The tomographic image based on each of the electron densities and the effective atomic number presents a different feature of the material, and its contrast drastically differs from that in a conventional CT image

  10. High resolution hard x-ray microscope on a second generation synchrotron source

    International Nuclear Information System (INIS)

    Tian Yangchao; Li Wenjie; Chen Jie; Liu Longhua; Liu Gang; Tian Jinping; Xiong Ying; Tkachuk, Andrei; Gelb, Jeff; Hsu, George; Yun Wenbing

    2008-01-01

    A full-field, transmission x-ray microscope (TXM) operating in the energy range of 7-11 keV has been installed at the U7A beamline at the National Synchrotron Radiation Laboratory, a second generation synchrotron source operating at 0.8 GeV. Although the photon flux at sample position in the operating energy range is significantly low due to its relatively large emittance, the TXM can get high quality x-ray images with a spatial resolution down to 50 nm with acceptable exposure time. This TXM operates in either absorption or Zernike phase contrast mode with similar resolution. This TXM is a powerful analytical tool for a wide range of scientific areas, especially studies on nanoscale phenomena and structural imaging in biology, materials science, and environmental science. We present here the property of the x-ray source, beamline design, and the operation and key optical components of the x-ray TXM. Plans to improve the throughput of the TXM will be discussed.

  11. Synchrotron X-ray Investigations of Mineral-Microbe-Metal Interactions

    International Nuclear Information System (INIS)

    Kemner, Kenneth M.; O'Loughlin, Edward J.; Kelly, Shelly D.; Boyanov, Maxim I.

    2005-01-01

    Interactions between microbes and minerals can play an important role in metal transformations (i.e. changes to an element's valence state, coordination chemistry, or both), which can ultimately affect that element's mobility. Mineralogy affects microbial metabolism and ecology in a system; microbes, in turn, can affect the system's mineralogy. Increasingly, synchrotron-based X-ray experiments are in routine use for determining an element's valence state and coordination chemistry, as well as for examining the role of microbes in metal transformations.

  12. Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines

    International Nuclear Information System (INIS)

    Alcock, Simon G.; Nistea, Ioana; Sutter, John P.; Sawhney, Kawal; Fermé, Jean-Jacques; Thellièr, Christophe; Peverini, Luca

    2015-01-01

    A next-generation bimorph mirror with piezos bonded to the side faces of a monolithic substrate was created. When replacing a first-generation bimorph mirror suffering from the junction effect, the new type of mirror significantly improved the size and shape of the reflected synchrotron X-ray beam. No evidence of the junction effect was observed even after eight months of continuous beamline usage. Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the ‘junction effect’: a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts

  13. Synchrotron radiation phase-contrast X-ray CT imaging of acupuncture points

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Dongming; Yan, Xiaohui; Zhang, Xinyi [Fudan University, Synchrotron Radiation Research Center, State Key Laboratory of Surface Physics and Department of Physics, Shanghai (China); Liu, Chenglin [Physics Department of Yancheng Teachers' College, Yancheng (China); Dang, Ruishan [The Second Military Medical University, Shanghai (China); Xiao, Tiqiao [Chinese Academy of Sciences, Shanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Shanghai (China); Zhu, Peiping [Chinese Academy of Sciences, Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, Beijing (China)

    2011-08-15

    Three-dimensional (3D) topographic structures of acupuncture points were investigated by using synchrotron radiation in-line X-ray phase contrast computerized tomography. Two acupuncture points, named Zhongji (RN3) and Zusanli (ST36), were studied. We found an accumulation of microvessels at each acupuncture point region. Images of the tissues surrounding the acupuncture points do not show such kinds of structure. This is the first time that 3D images have revealed the specific structures of acupuncture points. (orig.)

  14. Synchrotron radiation phase-contrast X-ray CT imaging of acupuncture points

    International Nuclear Information System (INIS)

    Zhang, Dongming; Yan, Xiaohui; Zhang, Xinyi; Liu, Chenglin; Dang, Ruishan; Xiao, Tiqiao; Zhu, Peiping

    2011-01-01

    Three-dimensional (3D) topographic structures of acupuncture points were investigated by using synchrotron radiation in-line X-ray phase contrast computerized tomography. Two acupuncture points, named Zhongji (RN3) and Zusanli (ST36), were studied. We found an accumulation of microvessels at each acupuncture point region. Images of the tissues surrounding the acupuncture points do not show such kinds of structure. This is the first time that 3D images have revealed the specific structures of acupuncture points. (orig.)

  15. Parallel beam microradiography of dental hard tissue using synchrotron radiation and X-ray image magnification

    International Nuclear Information System (INIS)

    Takagi, S.; Chow, L.C.; Brown, W.E.; Dobbyn, R.C.; Kuriyama, M.

    1984-01-01

    A novel technique utilizing a highly parallel beam of monochromatic synchrotron radiation combined with X-ray image magnification has been used to obtain microradiographs of caries lesions in relatively thick tooth sections. Preliminary results reveal structural features not previously reported. This technique holds the promise of allowing one to follow the structural changes accompanying the formation, destruction and chemical repair of mineralized tissue in real time. (orig.)

  16. A method for measuring the time structure of synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Moses, W.W.; Derenzo, S.E.

    1989-08-01

    We describe a method employing a plastic scintillator coupled to a fast photomultiplier tube to generate a timing pulse from the x-ray bursts emitted from a synchrotron radiation source. This technique is useful for performing synchrotron experiments where detailed knowledge of the timing distribution is necessary, such as time resolved spectroscopy or fluorescence lifetime experiments. By digitizing the time difference between the timing signal generated on one beam crossing with the timing signal generated on the next beam crossing, the time structure of a synchrotron beam can be analyzed. Using this technique, we have investigated the single bunch time structure at the National Synchrotron Light Source (NSLS) during pilot runs in January, 1989, and found that the majority of the beam (96%) is contained in one rf bucket, while the remainder of the beam (4%) is contained in satellite rf buckets preceeding and following the main rf bucket by 19 ns. 1 ref., 4 figs

  17. High-energy synchrotron radiation x-ray microscopy: Present status and future prospects

    International Nuclear Information System (INIS)

    Jones, K.W.; Gordon, B.M.; Spanne, P.; Rivers, M.L.; Sutton, S.R.

    1991-01-01

    High-energy radiation synchrotron x-ray microscopy is used to characterize materials of importance to the chemical and materials sciences and chemical engineering. The x-ray microscope (XRM) forms images of elemental distributions fluorescent x rays or images of mass distributions by measurement of the linear attenuation coefficient of the material. Distributions of sections through materials are obtained non-destructively using the technique of computed microtomography. The energy range of the x rays used for the XRM ranges from a few keV at the minimum value to more than 100 keV, which is sufficient to excite the K-edge of all naturally occurring elements. The work in progress at the Brookhaven NSLS X26 and X17 XRM is described in order to show the current status of the XRM. While there are many possible approaches to the XRM instrumentation, this instrument gives state-of-the-art performance in most respects and serves as a reasonable example of the present status of the instrumentation in terms of the spatial resolution and minimum detection limits obtainable. The examples of applications cited give an idea of the types of research fields that are currently under investigation. They can be used to illustrate how the field of x-ray microscopy will benefit from the use of bending magnets and insertion devices at the Advanced Photon Source. 8 refs., 5 figs

  18. Versatile, reprogrammable area pixel array detector for time-resolved synchrotron x-ray applications

    Energy Technology Data Exchange (ETDEWEB)

    Gruner, Sol [Cornell Univ., Ithaca, NY (United States)

    2010-05-01

    The final technical report for DOE grant DE-SC0004079 is presented. The goal of the grant was to perform research, development and application of novel imaging x-ray detectors so as to effectively utilize the high intensity and brightness of the national synchrotron radiation facilities to enable previously unfeasible time-resolved x-ray research. The report summarizes the development of the resultant imaging x-ray detectors. Two types of detector platforms were developed: The first is a detector platform (called a Mixed-Mode Pixel Array Detector, or MM-PAD) that can image continuously at over a thousand images per second while maintaining high efficiency for wide dynamic range signals ranging from 1 to hundreds of millions of x-rays per pixel per image. Research on an even higher dynamic range variant is also described. The second detector platform (called the Keck Pixel Array Detector) is capable of acquiring a burst of x-ray images at a rate of millions of images per second.

  19. Apparatus development for high-pressure X-ray diffraction using synchrotron radiation

    International Nuclear Information System (INIS)

    Martinez, L.G.; Orlando, M.T.D.; Rossi, J.L.; Passamai Junior, J.L.; Melo, F.C.L.; Ferreira, F.F.

    2006-01-01

    Some phenomena in the field of condensed matter physics can be studied when the matter is submitted to extreme conditions of pressure, magnetic fields or temperatures. Once submitted to these conditions it is generally necessary to measure the properties of the matter in situ. The existence of a synchrotron light laboratory in Brazil opens up the chance of studying materials in extreme conditions by techniques like X-ray diffraction and absorption. However, when compared to high-energy synchrotrons accelerators, the Brazilian source offers a narrower energy range and lower flux. These facts impose limitation to perform diffraction experiments by energy dispersion and, consequently, the use of pressure cells with denser anvils like diamond. However, for a lower-pressure range, preliminary studies showed the viability of measurements in an angular dispersion configuration. This allows the use of silicon carbide anvils B 4C . In this work it is described the development of a hydrostatic pressure cell suitable for X-rays diffraction measurements in the Brazilian Synchrotron Light Laboratory using materials and technologies developed by the institutions and researchers involved in this project (IPEN, UFES, CTA and LNLS). This development can provide the scientific community with the possibility of performing X-ray diffraction measurements under hydrostatic pressure, initially up to 2 GPa, with possibilities of increasing the maximum pressure to higher values, with or without application of magnetic fields and high or low temperatures. (author)

  20. Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines.

    Science.gov (United States)

    Alcock, Simon G; Nistea, Ioana; Sutter, John P; Sawhney, Kawal; Fermé, Jean Jacques; Thellièr, Christophe; Peverini, Luca

    2015-01-01

    Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the `junction effect': a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼ 0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts.

  1. Use of a synchrotron radiation x-ray microprobe for elemental analysis at the National Synchrotron Light Source

    International Nuclear Information System (INIS)

    Gordon, B.M.

    1980-01-01

    The National Synchrotron Light Source (NSLS) is a facility consisting of a 700 MeV and a 2.5 GeV electron storage ring and dedicated to providing synchrotron radiation in the energy range from the vacuum ultraviolet to high energy x rays. Some of the properties of synchrotron radiation that contribute to its usefulness for x-ray fluorescence are: a continuous, tunable energy spectrum, strong collimation in the horizontal plane, high polarization in the storage ring plane, and relatively low energy deposition. The highest priority is for the development of an x-ray microprobe beam line capable of trace analysis in the parts per million range with spatial resolution as low as one micrometer. An eventual capability for bulk sample analysis is also planned with sensitivities in the more favorable cases beings low as 50 parts per billion in dry biological tissue. The microprobe technique has application to a variety of fields including the geological, medical, materials and environmental sciences. Examples of investigations include multielemental trace analysis across grain boundaries for the study of diffusion and cooling processes in geological and materials sciences samples; in leukocytes and other types of individual cells for studying the relationship between trace element concentrations and disease or nutrition; and in individual particles in air pollution samples

  2. High-speed X-ray imaging pixel array detector for synchrotron bunch isolation

    International Nuclear Information System (INIS)

    Philipp, Hugh T.; Tate, Mark W.; Purohit, Prafull; Shanks, Katherine S.; Weiss, Joel T.; Gruner, Sol M.

    2016-01-01

    A high-speed pixel array detector for time-resolved X-ray imaging at synchrotrons has been developed. The ability to isolate single synchrotron bunches makes it ideal for time-resolved dynamical studies. A wide-dynamic-range imaging X-ray detector designed for recording successive frames at rates up to 10 MHz is described. X-ray imaging with frame rates of up to 6.5 MHz have been experimentally verified. The pixel design allows for up to 8–12 frames to be stored internally at high speed before readout, which occurs at a 1 kHz frame rate. An additional mode of operation allows the integration capacitors to be re-addressed repeatedly before readout which can enhance the signal-to-noise ratio of cyclical processes. This detector, along with modern storage ring sources which provide short (10–100 ps) and intense X-ray pulses at megahertz rates, opens new avenues for the study of rapid structural changes in materials. The detector consists of hybridized modules, each of which is comprised of a 500 µm-thick silicon X-ray sensor solder bump-bonded, pixel by pixel, to an application-specific integrated circuit. The format of each module is 128 × 128 pixels with a pixel pitch of 150 µm. In the prototype detector described here, the three-side buttable modules are tiled in a 3 × 2 array with a full format of 256 × 384 pixels. The characteristics, operation, testing and application of the detector are detailed

  3. Evaluating scintillator performance in time-resolved hard X-ray studies at synchrotron light sources.

    Science.gov (United States)

    Rutherford, Michael E; Chapman, David J; White, Thomas G; Drakopoulos, Michael; Rack, Alexander; Eakins, Daniel E

    2016-05-01

    The short pulse duration, small effective source size and high flux of synchrotron radiation is ideally suited for probing a wide range of transient deformation processes in materials under extreme conditions. In this paper, the challenges of high-resolution time-resolved indirect X-ray detection are reviewed in the context of dynamic synchrotron experiments. In particular, the discussion is targeted at two-dimensional integrating detector methods, such as those focused on dynamic radiography and diffraction experiments. The response of a scintillator to periodic synchrotron X-ray excitation is modelled and validated against experimental data collected at the Diamond Light Source (DLS) and European Synchrotron Radiation Facility (ESRF). An upper bound on the dynamic range accessible in a time-resolved experiment for a given bunch separation is calculated for a range of scintillators. New bunch structures are suggested for DLS and ESRF using the highest-performing commercially available crystal LYSO:Ce, allowing time-resolved experiments with an interframe time of 189 ns and a maximum dynamic range of 98 (6.6 bits).

  4. Effects of synchrotron radiation spectrum energy on polymethyl methacrylate photosensitivity to deep x-ray lithography

    CERN Document Server

    Mekaru, H; Hattori, T

    2003-01-01

    Since X-ray lithography requires a high photon flux to achieve deep resist exposure, a synchrotron radiation beam, which is not monochromatized, is generally used as a light source. If the synchrotron radiation beam is monochromatized, photon flux will decrease rapidly. Because of this reason, the wavelength dependence of the resist sensitivity has not been investigated for deep X-ray lithography. Measuring the spectrum of a white beam with a Si solid-state detector (SSD) is difficult because a white beam has a high intensity and an SSD has a high sensitivity. We were able to measure the spectrum and the photocurrent of a white beam from a beam line used for deep X-ray lithography by keeping the ring current below 0.05 mA. We evaluated the characteristics of the output beam based on the measured spectrum and photocurrent, and used them to investigate the relationship between the total exposure energy and the dose-processing depth with polymethyl methacrylate (PMMA). We found that it is possible to guess the p...

  5. Conical geometry for sagittal focusing as applied to X rays from synchrotrons

    International Nuclear Information System (INIS)

    Ice, G.E.; Sparks, C.J.

    1993-06-01

    The authors describe a method for simultaneously focusing and monochromatization of X rays from a fan of radiation having up to 15 mrad divergence in one dimension. This geometry is well suited to synchrotron radiation sources at magnifications of one-fifth to two and is efficient for X-ray energies between 3 and 40 keV (0.48 and 6.4 fJ). The method uses crystals bent to part of a cone for sagittal focusing and allows for the collection of a larger divergence with less mixing of the horizontal into the vertical divergence than is possible with X-ray mirrors. They describe the geometry required to achieve the highest efficiency when a conical crystal follows a flat crystal in a nondispersive two-crystal monochromator. At a magnification of one-third, the geometry is identical to a cylindrical focusing design described previously. A simple theoretical calculation is shown to agree well with ray-tracing results. Minimum aberrations are observed at magnifications near one. Applications of the conical focusing geometry to existing and future synchrotron radiation facilities are discussed

  6. Heat transfer issues in high-heat-load synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Khounsary, A.M.; Mills, D.M.

    1994-09-01

    In this paper, a short description of the synchrotron radiation x-ray sources and the associated power loads is given, followed by a brief description of typical synchrotron components and their heat load. It is emphasized that the design goals for most of these components is to limit (a) temperature, (b) stresses, or (c) strains in the system. Each design calls for a different geometry, material selection, and cooling scheme. Cooling schemes that have been utilized so far are primarily single phase and include simple macrochannel cooling, microchannel cooling, contact cooling, pin-post cooling, porous-flow cooling, jet cooling, etc. Water, liquid metals, and various cryogenic coolants have been used. Because the trend in x-ray beam development is towards brighter (i.e., more powerful) beams and assuming that no radical changes in the design of x-ray generating machines occurs in the next few years, it is fair to state that the utilization of various effective cooling schemes and, in particular, two-phase flow (e.g., subcooled boiling) warrants further investigation. This, however, requires a thorough examination of stability and reliability of two-phase flows for high-heat-flux components operating in ultrahigh vacuum with stringent reliability requirements

  7. Diffraction measurements of residual macrostress and microstress using x-rays, synchrotron and neutrons

    International Nuclear Information System (INIS)

    Tanaka, Keisuke; Akiniwa, Yoshiaki

    2004-01-01

    The present paper reviews some recent developments of the measurements of the macrostress and microstress by diffraction using X-rays, synchrotron and neutrons especially in Japan. These three methods are based on the same principle of the diffraction of crystals, and have different advantages. The conventional X-rays detect the stress very near the surface, while the neutron diffraction takes the stress in the interior of the materials. High-energy X-rays from synchrotron sources have the penetration depth in between and are suitable for the measurement of subsurface stresses. After describing the developments of the fundamentals of the methods, the paper covers the recent applications of the diffraction methods to the residual stress analysis in textured thin films, the nondestructive determination of the subsurface distribution of residual stress in shot-peened materials, local stress measurements near the crack tip, the stress measurements of single crystals, macrostress and microstress measurements in composites, and the determination of the internal distribution of the residual stress in welded joints. (author)

  8. Synthesis of nanoparticles through x-ray radiolysis using synchrotron radiation

    Science.gov (United States)

    Yamaguchi, A.; Okada, I.; Fukuoka, T.; Ishihara, M.; Sakurai, I.; Utsumi, Y.

    2016-09-01

    The synthesis and deposition of nanoparticles consisting of Cu and Au in a CuSO4 solution with some kinds of alcohol and electroplating solution containing gold (I) trisodium disulphite under synchrotron X-ray radiation was investigated. The functional group of alcohol plays an important in nucleation, growth and aggregation process of copper and cupric oxide particles. We found that the laboratory X-ray source also enables us to synthesize the NPs from the metallic solution. As increasing X-ray exposure time, the full length at half width of particle size distribution is broader and higher-order nanostructure containing NPs clusters is formed. The surface-enhanced Raman scattering (SERS) of 4, 4'-bipyridine (4bpy) in aqueous solution was measured using higher-order nanostructure immobilized on silicon substrates under systematically-varied X-ray exposure. This demonstration provide a clue to develop a three-dimensional printing and sensor for environmental analyses and molecular detection through simple SERS measurements.

  9. X-ray absorption spectroscopy investigations on radioactive matter using MARS beamline at SOLEIL synchrotron

    Energy Technology Data Exchange (ETDEWEB)

    Llorens, Isabelle; Solari, Pier Lorenzo; Sitaud, Bruno [Synchrotron SOLEIL - l' Orme des Merisiers Saint Aubin, Gif-sur-Yvette (France); and others

    2014-07-01

    The MARS beamline at the SOLEIL synchrotron is dedicated to the characterization of radioactive material samples. One great advantage of the beamline is the possibility to characterize about 380 radionuclides by different X-ray techniques in the same place. This facility is unique in Europe. A wide energy range from around 3.5 keV to 36 keV K-edges from K to Cs, and L3 edges from Cd to Am and beyond can be used. The MARS beamline is optimized for X-ray absorption spectroscopy techniques (XANES/EXAFS), powder diffraction (XRD) but X-ray fluorescence (XRF) analysis, High Energy Resolution Fluorescence Detected-XAS (HERFD-XAS), X-ray Emission (XES) and μ-XAS/XRD are also possible. A description of the beamline as well as its performances are given in a first part. Then some scientific examples of XAS studies from users are presented which cover a wide variety of topics in radiochemistry and nuclear materials.

  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. Small-angle scattering, topography and radiography

    International Nuclear Information System (INIS)

    Schelten, J.

    1978-01-01

    A table is given showing scattering and imaging methods for X-rays and neutrons, followed, by a discussion of such topics as 1. Radiography 2. Topography 3. Small-angle scattering 3.1. The differential cross section 3.2. Comparison of X-ray and neutron small-angle scattering 3.3. Examples of small-angle scattering. (orig.) [de

  12. Application of X-ray and neutron small angle scattering techniques to study the hierarchical structure of plant cell walls: a review.

    Science.gov (United States)

    Martínez-Sanz, Marta; Gidley, Michael J; Gilbert, Elliot P

    2015-07-10

    Plant cell walls present an extremely complex structure of hierarchically assembled cellulose microfibrils embedded in a multi-component matrix. The biosynthesis process determines the mechanism of cellulose crystallisation and assembly, as well as the interaction of cellulose with other cell wall components. Thus, a knowledge of cellulose microfibril and bundle architecture, and the structural role of matrix components, is crucial for understanding cell wall functional and technological roles. Small angle scattering techniques, combined with complementary methods, provide an efficient approach to characterise plant cell walls, covering a broad and relevant size range while minimising experimental artefacts derived from sample treatment. Given the system complexity, approaches such as component extraction and the use of plant cell wall analogues are typically employed to enable the interpretation of experimental results. This review summarises the current research status on the characterisation of the hierarchical structure of plant cell walls using small angle scattering techniques. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

  13. Development of confocal X-ray fluorescence (XRF) microscopy at the Cornell high energy synchrotron source

    International Nuclear Information System (INIS)

    Woll, A.R.; Huang, R.; Mass, J.; Bisulca, C.; Bilderback, D.H.; Gruner, S.; Gao, N.

    2006-01-01

    A confocal X-ray fluorescence microscope was built at the Cornell High Energy Synchrotron Source (CHESS) to obtain compositional depth profiles of historic paintings. The microscope consists of a single-bounce, borosilicate monocapillary optic to focus the incident beam onto the painting and a commercial borosilicate polycapillary lens to collect the fluorescent X-rays. The resolution of the microscope was measured by scanning a variety of thin metal films through this confocal volume while monitoring the fluorescence signal. The capabilities of the technique were then probed using test paint microstructures with up to four distinct layers, each having a thickness in the range of 10-80 microns. Results from confocal XRF were compared with those from stand-alone XRF and visible light microscopy of the paint cross-sections. A large area, high-resolution scanner is currently being built to perform 3D scans on moderately sized paintings. (orig.)

  14. Source assemblage types for cratonic diamonds from X-ray synchrotron diffraction

    Science.gov (United States)

    Nestola, F.; Alvaro, M.; Casati, M. N.; Wilhelm, H.; Kleppe, A. K.; Jephcoat, A. P.; Domeneghetti, M. C.; Harris, J. W.

    2016-11-01

    Three single crystals of clinopyroxene trapped within three different gem-quality diamonds from the Udachnaya kimberlite (Siberia, Russia) were analysed in situ by single-crystal synchrotron X-ray diffraction in order to obtain information on their chemical composition and infer source assemblage type. A non-destructive approach was used with high-energy (≈ 60 keV; λ ≈ 0.206 Å) at I15, the extreme-conditions beamline at Diamond Light Source. A dedicated protocol was used to center the mineral inclusions located deep inside the diamonds in the X-ray beam. Our results reveal that two of the inclusions can be associated with peridotitic paragenesis whereas the third is eclogitic. This study also demonstrates that this non-destructive experimental approach is extremely efficient in evaluating the origin of minerals trapped in their diamond hosts.

  15. Synchrotron hard X-ray imaging of shock-compressed metal powders

    Science.gov (United States)

    Rutherford, Michael E.; Chapman, David J.; Collinson, Mark A.; Jones, David R.; Music, Jasmina; Stafford, Samuel J. P.; Tear, Gareth R.; White, Thomas G.; Winters, John B. R.; Drakopoulos, Michael; Eakins, Daniel E.

    2015-06-01

    This poster will present the application of a new, high-energy (50 to 250 keV) synchrotron X-ray radiography technique to the study of shock-compressed granular materials. Following plate-impact loading, transmission radiography was used to quantitatively observe the compaction and release processes in a range of high-Z metal powders (e.g. Fe, Ni, Cu). By comparing the predictions of 3D numerical models initialized from X-ray tomograms-captured prior to loading-with experimental results, this research represents a new approach to refining mesoscopic compaction models. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

  16. Metals determination in wood treated by synchrotron radiation X-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Vives, Ana Elisa Sirito de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Silva, Richard Maximiliano da Cunha [Centro de Energia Nuclear na Agricultura, Piracicaba, SP (Brazil)]. E-mail: maxcunha@cena.usp.br; Medeiros, Jean Gabriel da Silva; Tomazello Filho, Mario [Sao Paulo Univ., Piracicaba, SP (Brazil). Escola Superior de Agricultura Luiz de Queiroz]. E-mail: jeangm@esalq.usp.br; mtomazel@esalq.usp.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Zucchi, Orgheda Luiza Araujo Domingues [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Barroso, Regina Cely [Universidade do Estado, Rio de Janeiro, RJ (Brazil)]. E-mail: cely@uerj.br

    2005-07-01

    The paper describes the use of X-Ray fluorescence analysis for distribution and quantification of metals in the hardwood (Eucalyptus sp) and softwood (Pinus sp) treated with CCA (copper-chromium-arsenic). The sapwood/heartwood for hardwood sample and the growth-rings for softwood sample were analyzed. The samples were scanned in 320 mm steps in the vertical direction. For excitation of the elements a white beam synchrotron radiation of {approx} 320 x 180 mm was employed and for the X-ray detection a Si(Li) semiconductor detector. The elements K, Ca, Cr, Mn, Cu, Zn and As were determined. Fundamental parameters were used to quantify the elements concentrations. (author)

  17. Metals determination in wood treated by synchrotron radiation X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Vives, Ana Elisa Sirito de; Medeiros, Jean Gabriel da Silva; Tomazello Filho, Mario

    2005-01-01

    The paper describes the use of X-Ray fluorescence analysis for distribution and quantification of metals in the hardwood (Eucalyptus sp) and softwood (Pinus sp) treated with CCA (copper-chromium-arsenic). The sapwood/heartwood for hardwood sample and the growth-rings for softwood sample were analyzed. The samples were scanned in 320 mm steps in the vertical direction. For excitation of the elements a white beam synchrotron radiation of ∼ 320 x 180 mm was employed and for the X-ray detection a Si(Li) semiconductor detector. The elements K, Ca, Cr, Mn, Cu, Zn and As were determined. Fundamental parameters were used to quantify the elements concentrations. (author)

  18. High-resolution X-ray scattering topography using synchrotron radiation microbeam

    International Nuclear Information System (INIS)

    Chikaura, Yoshinori; Suzuki, Yoshifumi; Kii, Hideki

    1994-01-01

    Although spatial resolution is the most essential factor determining the function of X-ray topography, it has not been improved in 30 years in spite of increasing requirements for highly-resolvable topography in materials science. X-ray scattering topography using a microbeam is a method capable of overcoming this resolution problem. Because the maximum resolution of an apparatus using a sealed-off tube is limited to 20μm, we designed and constructed scattering topography equipment using a synchrotron radiation microbeam. In the experiment, the slit system forms the microbeam 7 μm in diameter. We observed a cellulose distribution in bamboo as a testing material. When the scanning step was 2 μm, we attained spatial resolution less than 5 μm. (author)

  19. Optics for protein microcrystallography using synchrotron and laboratory X-ray sources

    International Nuclear Information System (INIS)

    Varghese, J.N.; Van Donkelaar, A.; Balaic, D.X.; Barnea, Z.

    2000-01-01

    Full text: For protein crystallography, a highly-intense focused beam overcomes a serious constraint in current biological research: the inability of many protein molecules to form crystals larger than a few tens of microns in size. High structure-resolution X-ray diffraction analysis of microcrystals is currently only being studied at synchrotron X-ray sources. We shall examine how this is being carried out, and also report the development of a novel tapered glass monocapillary toroidal-mirror optic, which achieves a high-intensity, low-divergence focused beam from a rotating-anode Xray generator. We have used this optic, which demonstrates an ∼28x intensity gain at the beam focus to solve the structure of a plant exoglucanse/inhibtor complex microcrystal to 2.8 Angstroms, with volume equivalent to a 30-micron-edge cube

  20. X-rays from synchrotron: A new challenge for neutron scattering

    International Nuclear Information System (INIS)

    Shirane, G.

    1983-01-01

    A brief review is given of current developments in X-ray scattering techniques at synchrotron radiation facilities. Highly collimated, intense sources of white radiation open up new areas of research in condensed matter physics and challenge the traditional domains of neutron scattering. These include energy dispersive scattering, the use of anomalous dispersion, magnetic diffraction and direct energy analysis by backscattering. The relative merits of X-ray and neutron scattering techniques will be discussed. The unique advantage of neutron scattering is the capability of performing polarization analysis. We will discuss in some detail the current developments at Brookhaven inelastic scattering of polarized neutrons. In addition, we will also discuss special technical problems associated with the search for phasons utilizing a high-resolution triple axis spectrometer. (orig.)

  1. Nanostructure of protective rust layer on weathering steel examined using synchrotron radiation x-rays

    International Nuclear Information System (INIS)

    Yamashita, Masato; Uchida, Hitoshi; Konishi, Hiroyuki; Mizuki, Jun'ichiro

    2004-01-01

    The X-ray absorption fine structure (XAFS) spectrum of pure goethite around the Fe K absorption edge and that of the protective rust layer formed on weathering steel exposed for 17 years in an atmospheric environment around the Cr K edge, have been examined using synchrotron radiation X-rays. It was found that the rust layer on the weathering steel mainly consisted of Cr-goethite. By examining the fine structure at the Cr K edge and the Fe K edge, we concluded that Cr 3+ in the rust layer is coordinated with O 2- and is positioned in the double chains of vacant sites in the network of FeO 3 (OH) 3 octahedra in the goethite crystal. This Cr 3+ site indicates that the protective effect of the rust layer is due to the dense aggregation of fine crystals of Cr-goethite with cation selectivity. (author)

  2. Development of a speckle-based portable device for in situ metrology of synchrotron X-ray mirrors.

    Science.gov (United States)

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-09-01

    A portable device for in situ metrology of synchrotron X-ray mirrors based on the near-field speckle scanning technique has been developed. Ultra-high angular sensitivity is achieved by scanning a piece of abrasive paper or filter membrane in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that optimizing active X-ray mirrors is simple and fast. The functionality and feasibility of this device have been demonstrated by characterizing and optimizing X-ray mirrors.

  3. CCD-based detector for protein crystallography with synchrotron X-rays

    International Nuclear Information System (INIS)

    Strauss, M.G.; Westbrook, E.M.; Naday, I.; Coleman, T.A.; Westbrook, M.L.; Travis, D.J.; Sweet, R.M.; Pflugrath, J.W.; Stanton, M.

    1990-01-01

    A detector with a 114 mm aperture, based on a charge-coupled device (CCD), has been designed for X-ray diffraction studies in protein crystallography. The detector was tested at the National Synchrotron Light Source with a beam intensity, through a 0.3 mm collimator, of greater than 10 9 X-ray photons/s. A fiberoptic taper, an image intensifier, and a lens demagnify, intensity, and focus the image onto a CCD having 512x512 pixels. The statistical uncertainty in the detector output was evaluated as a function of conversion gain. From this, a detective quantum efficiency (DQE) of 0.36 was derived. The dynamic range of 4x4 pixel resolution element, comparable in size to a diffraction peak, was 10 4 . The point-spread function shows FWHM resolution of approximately 1 pixel, where a pixel is 160 μm on the detector face. A data set collected from a chicken egg-white lysozyme crystal, consisting of 495 0.1deg frames, was processed by the MADNES data reduction program. The symmetry R-factors for the data were 3.2-3.5%. In a separate experiment a complete lysozyme data set consisting of 45 1deg frames was obtained in just 36 s of X-ray exposure. Diffraction images from crystals of the myosin S1 head (a=275 A) were also recorded; the Bragg spots, only 5 pixels apart, were separated but not fully resolved. Changes in the detector design that will improve the DQE and spatial resolution are outlined. The overall performance showed that this type of detector is well suited for X-ray scattering investigations with synchrotron sources. (orig.)

  4. CCD-based detector for protein crystallography with synchrotron X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Strauss, M.G.; Westbrook, E.M.; Naday, I.; Coleman, T.A.; Westbrook, M.L.; Travis, D.J. (Argonne National Lab., IL (USA)); Sweet, R.M. (Brookhaven National Lab., Upton, NY (USA)); Pflugrath, J.W. (Cold Spring Harbor Lab., NY (USA)); Stanton, M. (Brandeis Univ., Waltham, MA (USA))

    1990-11-15

    A detector with a 114 mm aperture, based on a charge-coupled device (CCD), has been designed for X-ray diffraction studies in protein crystallography. The detector was tested at the National Synchrotron Light Source with a beam intensity, through a 0.3 mm collimator, of greater than 10{sup 9} X-ray photons/s. A fiberoptic taper, an image intensifier, and a lens demagnify, intensity, and focus the image onto a CCD having 512x512 pixels. The statistical uncertainty in the detector output was evaluated as a function of conversion gain. From this, a detective quantum efficiency (DQE) of 0.36 was derived. The dynamic range of 4x4 pixel resolution element, comparable in size to a diffraction peak, was 10{sup 4}. The point-spread function shows FWHM resolution of approximately 1 pixel, where a pixel is 160 {mu}m on the detector face. A data set collected from a chicken egg-white lysozyme crystal, consisting of 495 0.1deg frames, was processed by the MADNES data reduction program. The symmetry R-factors for the data were 3.2-3.5%. In a separate experiment a complete lysozyme data set consisting of 45 1deg frames was obtained in just 36 s of X-ray exposure. Diffraction images from crystals of the myosin S1 head (a=275 A) were also recorded; the Bragg spots, only 5 pixels apart, were separated but not fully resolved. Changes in the detector design that will improve the DQE and spatial resolution are outlined. The overall performance showed that this type of detector is well suited for X-ray scattering investigations with synchrotron sources. (orig.).

  5. CCD-based detector for protein crystallography with synchrotron X-rays

    Science.gov (United States)

    Strauss, M. G.; Westbrook, E. M.; Naday, I.; Coleman, T. A.; Westbrook, M. L.; Travis, D. J.; Sweet, R. M.; Pflugrath, J. W.; Stanton, M.

    1990-11-01

    A detector with a 114 mm aperture, based on a charge-coupled device (CCD), has been designed for X-ray diffraction studies in protein crystallography. The detector was tested at the National Synchrotron Light Source with a beam intensity, through a 0.3 mm collimator, of greater than 109 X-ray photons/s. A fiberoptic taper, an image intensifier, and a lens demagnify, intensify, and focus the image onto a CCD having 512×512 pixels. The statistical uncertainty in the detector output was evaluated as a function of conversion gain. From this, a detective quantum efficiency (DQE) of 0.36 was derived. The dynamic range of a 4×4 pixel resolution element, comparable in size to a diffraction peak, was 104. The point-spread function shows FWHM resolution of approximately 1 pixel, where a pixel is 160 μm on the detector face. A data set collected from a chicken egg-white lysozyme crystal, consisting of 495 0.1° frames, was processed by the MADNES data reduction program. The symmetry R-factors for the data were 3.2-3.5%. In a separate experiment a complete lysozyme data set consisting of 45 1° frames was obtained in just 36 s of X-ray exposure. Diffraction images from crystals of the myosin S1 head (a = 275 Å) were also recorded; the Bragg spots, only 5 pixels apart, were separated but not fully resolved. Changes in the detector design that will improve the DQE and spatial resolution are outlined. The overall performance showed that this type of detector is well suited for X-ray scattering investigations with synchrotron sources.

  6. Synchrotron x-ray methods in studies of thin organic film structure

    International Nuclear Information System (INIS)

    Gentle, I.

    2002-01-01

    Full text: In recent years, the study of the structures of organic films as thin as a single monolayer has been revolutionized by methods that take advantage of the characteristics of synchrotron radiation. In particular, the methods of grazing incidence X-ray diffraction (GIXD) and X-ray reflectivity have led to a number of valuable insights into structural aspects of thin films at molecular resolution. Our group has been studying films formed at the air/water interface as insoluble monolayers and subsequently transferred to solid substrates using either the vertical (Langmuir-Blodgett) or horizontal (Langmuir-Schaeffer) methods. The main aim of these experiments is to exert control over film structure in the direction parallel to the substrate surface. This is highly desirable in order to design devices that exploit the optical and electrooptical properties of functional materials, but is difficult to do. By varying the chemical structure of the film materials and controlling deposition conditions a degree of control is possible, but only using synchrotron methods can it be easily verified. We have also developed a novel method of rapidly collecting data from GIXD measurements by the application of area detection (imaging plates), which has made possible measurements of dynamic processes such as in-situ annealing. Such measurements are not possible using traditional scanning methods. One area of current interest is films composed of porphyrins as functional materials, either alone or as mixed films with fatty acids. We have been investigating ways of assembling porphyrins in such a way as to overcome the tendency to aggregate, and to produce patterning and ordered structures in the plane of the interface. Examples will be given of how film composition and deposition method affects the final structure, and of how X-ray methods can be used to elucidate both the structures and the mechanisms. Copyright (2002) Australian X-ray Analytical Association Inc

  7. DOE/DMS workshop on future synchrotron VUV and x-ray beam Lines

    International Nuclear Information System (INIS)

    Green, P.H.

    1992-03-01

    This document contains an overview of the participating DOE Laboratory beam line interests and the projected science to be addressed on these beam lines, both at new and existing synchrotron facilities. The scientific programs associated with present and planned synchrotron research by DOE Laboratories are discussed in chapters titled ''VUV and Soft X-Ray Research'' and ''Hard X-Ray Research.'' This research encompasses a broad range of the nation's scientific and technical research needs from fundamental to applied, in areas including environmental, biological, and physical sciences; new materials; and energy-related technologies. The projected cost of this proposed construction has been provided in tabular form using a uniform format so that anticipated DOE and outside funding agency contributions for construction and for research and development can be determined. The cost figures are, of course, subject to uncertainties of detailed design requirements and the availability of facility-designed generic components and outside vendors. The report also contains a compendium (as submitted by the beam line proposers) of the design capabilities, the anticipated costs, and the scientific programs of projected beam line construction at the four synchrotron facilities. A summary of the projected cost of these beam lines to be requested of DOE is compiled

  8. X-ray beam splitting design for concurrent imaging at hard X-ray FELs and synchrotron facilities

    Czech Academy of Sciences Publication Activity Database

    Oberta, Peter; Mokso, R.

    2013-01-01

    Roč. 729, NOV (2013), s. 85-89 ISSN 0168-9002 R&D Projects: GA MPO FR-TI1/412 Institutional research plan: CEZ:AV0Z10100522 Keywords : diffractive-refractive optics * hard X-ray FEL * X-ray imaging Subject RIV: BH - Optics, Masers, Lasers Impact factor: 1.316, year: 2013 http://www.sciencedirect.com/science/article/pii/S0168900213009613

  9. Iron overload of human colon adenocarcinoma cells studied by synchrotron-based X-ray techniques.

    Science.gov (United States)

    Mihucz, Victor G; Meirer, Florian; Polgári, Zsófia; Réti, Andrea; Pepponi, Giancarlo; Ingerle, Dieter; Szoboszlai, Norbert; Streli, Christina

    2016-04-01

    Fast- and slow-proliferating human adenocarcinoma colorectal cells, HT-29 and HCA-7, respectively, overloaded with transferrin (Tf), Fe(III) citrate, Fe(III) chloride and Fe(II) sulfate were studied by synchrotron radiation total-reflection X-ray spectrometry (TXRF), TXRF-X-ray absorption near edge structure (TXRF-XANES), and micro-X-ray fluorescence imaging to obtain information on the intracellular storage of overloaded iron (Fe). The determined TfR1 mRNA expression for the investigated cells correlated with their proliferation rate. In all cases, the Fe XANES of cells overloaded with inorganic Fe was found to be similar to that of deliquescent Fe(III) sulfate characterized by a distorted octahedral geometry. A fitting model using a linear combination of the XANES of Tf and deliquescent Fe(III) sulfate allowed to explain the near edge structure recorded for HT-29 cells indicating that cellular overload with inorganic Fe results in a non-ferritin-like fast Fe storage. Hierarchical cluster analysis of XANES spectra recorded for Fe overloaded HT-29 and HCA-7 cells was able to distinguish between Fe treatments performed with different Fe species with a 95% hit rate, indicating clear differences in the Fe storage system. Micro-X-ray fluorescence imaging of Fe overloaded HT-29 cells revealed that Fe is primarily located in the cytosol of the cells. By characterizing the cellular Fe uptake, Fe/S content ratios were calculated based on the X-ray fluorescence signals of the analytes. These Fe/S ratios were dramatically lower for HCA-7 treated with organic Fe(III) treatments suggesting dissimilarities from the Tf-like Fe uptake.

  10. Reference-free total reflection X-ray fluorescence analysis of semiconductor surfaces with synchrotron radiation.

    Science.gov (United States)

    Beckhoff, Burkhard; Fliegauf, Rolf; Kolbe, Michael; Müller, Matthias; Weser, Jan; Ulm, Gerhard

    2007-10-15

    Total reflection X-ray fluorescence (TXRF) analysis is a well-established method to monitor lowest level contamination on semiconductor surfaces. Even light elements on a wafer surface can be excited effectively when using high-flux synchrotron radiation in the soft X-ray range. To meet current industrial requirements in nondestructive semiconductor analysis, the Physikalisch-Technische Bundesanstalt (PTB) operates dedicated instrumentation for analyzing light element contamination on wafer pieces as well as on 200- and 300-mm silicon wafer surfaces. This instrumentation is also suited for grazing incidence X-ray fluorescence analysis and conventional energy-dispersive X-ray fluorescence analysis of buried and surface nanolayered structures, respectively. The most prominent features are a high-vacuum load-lock combined with an equipment front end module and a UHV irradiation chamber with an electrostatic chuck mounted on an eight-axis manipulator. Here, the entire surface of a 200- or a 300-mm wafer can be scanned by monochromatized radiation provided by the plane grating monochromator beamline for undulator radiation in the PTB laboratory at the electron storage ring BESSY II. This beamline provides high spectral purity and high photon flux in the range of 0.078-1.86 keV. In addition, absolutely calibrated photodiodes and Si(Li) detectors are used to monitor the exciting radiant power respectively the fluorescence radiation. Furthermore, the footprint of the excitation radiation at the wafer surface is well-known due to beam profile recordings by a CCD during special operation conditions at BESSY II that allow for drastically reduced electron beam currents. Thus, all the requirements of completely reference-free quantitation of TXRF analysis are fulfilled and are to be presented in the present work. The perspectives to arrange for reference-free quantitation using X-ray tube-based, table-top TXRF analysis are also addressed.

  11. Structural Studies on Plasmodium falciparum Erythrocyte Membrane Protein 1 (PfEMP1) Malaria Antigens Using Small Angle X-Ray Scattering (SAXS)

    DEFF Research Database (Denmark)

    Christoffersen, Stig

    Infection with the pathogenic Plasmodium falciparum parasite causes the potentially deadly Malaria disease which leads to over 1 million fatalities each year according to the WHO (World Health Organization). Individuals subjected to multiple infections gradually become immune to the disease...... purposes. Macromolecular crystallography is typically the biophysical method of choice for obtaining detailed structural information but it unfortunately requires the formation of X-ray scattering protein crystals. The protein crystallization step remains a major bottleneck for X-ray protein...... crystallography. While conducting the SAXS experiments on PfEMP1 protein solutions, I alongside performed crystallization experiments using these solutions and found that the purified proteins showed very poor aptitude towards crystals formation. On the other hand, the SAXS method proved itself as a valuable tool...

  12. Computer simulation of small-angle X-ray reflection from finite size samples with accounting for the instrumental errors of a diffractometer

    International Nuclear Information System (INIS)

    Zorina, M.V.; Mironov, V.L.; Mironov, S.V.

    2005-01-01

    A model is developed, which enables computation of the the angular dependences of X-ray reflection, with taking into account the finiteness of sample sizes and the diffractometer alignment errors. It is shown that the angular dependences of refraction for glass and quartz wafers calculated with account of possible errors of the diffractometer optical system alignment are in good agreement with the experimental curves in the entire range of angles [ru

  13. Microscopy and elemental analysis in tissue samples using computed microtomography with synchrotron x-rays

    International Nuclear Information System (INIS)

    Spanne, P.; Rivers, M.L.

    1988-01-01

    The initial development shows that CMT using synchrotron x-rays can be developed to μm spatial resolution and perhaps even better. This creates a new microscopy technique which is of special interest in morphological studies of tissues, since no chemical preparation or slicing of the sample is necessary. The combination of CMT with spatial resolution in the μm range and elemental mapping with sensitivity in the ppM range results in a new tool for elemental mapping at the cellular level. 7 refs., 1 fig

  14. Raphide crystal structure in agave tequilana determined by x-ray originating from synchrotron radiation

    International Nuclear Information System (INIS)

    Tadokoro, Makoto; Ozawa, Yoshiki; Mitsumi, Minoru; Toriumi, Kohshiro; Ogura, Tetsuya

    2005-01-01

    The first single crystal structure of small natural raphides in an agave plant is completely determined using an intense X-ray originating from a synchrotron radiation. The SEM image shows that the tip of the crystal is approximately hundreds of nanometer in width sharply grow to stick to the tissue of herbivorous vermin. Furthermore, the crystal develops cracks that propagate at an inclination of approximately 45deg towards the direction of crystal growth such that the crystal easily splits into small pieces in the tissue. (author)

  15. Porosity characterization of fiber-reinforced ceramic matrix composite using synchrotron X-ray computed tomography

    Science.gov (United States)

    Zou, C.; Marrow, T. J.; Reinhard, C.; Li, B.; Zhang, C.; Wang, S.

    2016-03-01

    The pore structure and porosity of a continuous fiber reinforced ceramic matrix composite has been characterized using high-resolution synchrotron X-ray computed tomography (XCT). Segmentation of the reconstructed tomograph images reveals different types of pores within the composite, the inter-fiber bundle open pores displaying a "node-bond" geometry, and the intra-fiber bundle isolated micropores showing a piping shape. The 3D morphology of the pores is resolved and each pore is labeled. The quantitative filtering of the pores measures a total porosity 8.9% for the composite, amid which there is about 7.1~ 9.3% closed micropores.

  16. An x-ray fluorescence study of lake sediments from ancient Turkey using synchrotron radiation.

    Energy Technology Data Exchange (ETDEWEB)

    Alatas, A.; Alp, E. E.; Friedman, E. S.; Jennings, G.; Johnson, C. E.; Lai, B.; Mini, S. M.; Sato, Y.; Wilkinson, T. J.; Yener, K. A.

    1999-03-10

    Sediments from relic Lake Golbasi were analyzed by X-ray fluorescence with synchrotrons radiation to determine changes in element concentrations over time with selected elements serving as proxies for environmental change. Increases in Ca and Sr suggest soil formation during a dry period, from ca. 4500 BC to ca. 200 AD at which point K, Rb, Zr, Ti, and Y increase, indicating the return of a wet environment. Soil erosion, represented by Cr and Ni, increases ca. 7000 BC, probably as a consequence of environmental change, prior to suggested exploitation of natural resources by the newly urbanized society of the third millennium BC.

  17. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    Science.gov (United States)

    Tiwari, M. K.; Singh, A. K.; Das, Gangadhar; Chowdhury, Anupam; Lodha, G. S.

    2014-04-01

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  18. Non-destructive synchrotron X-ray diffraction mapping of a Roman painting

    International Nuclear Information System (INIS)

    Dooryhee, E.; Anne, M.; Hodeau, J.-L.; Martinetto, P.; Rondot, S.; Bardies, I.; Salomon, J.; Walter, P.; Vaughan, G.B.M.

    2005-01-01

    The history and the properties of materials are deduced not only from their elemental and molecular signatures, but also from their exact phase compositions, and from the structures and the defects of their constituents. Here we implement a non-destructive synchrotron X-ray based method, which combines both the quantitative structural content of diffraction and the imaging mode. As a demonstration case, the pigments of a Roman wall painting are examined. The joined elemental and mineral maps mimic the major features of the painting. Different structural phases made of common atomic elements are differentiated. Textures and graininess are measured and related to the artist's know-how. (orig.)

  19. X-ray photoelectron spectroscopy study of synchrotron radiation irradiation of a polytetrafluoroethylene surface

    CERN Document Server

    Haruyama, Y; Matsui, S; Ideta, T; Ishigaki, H

    2003-01-01

    The effect of synchrotron radiation (SR) irradiation of a polytetrafluoroethylene (PTFE) surface was investigated using X-ray photoelectron spectroscopy (XPS). After the SR irradiation, the relative intensity of the F ls peak to the C ls peak decreased markedly. The chemical composition ratio to the F atoms to C atoms was estimated to be 0.29. From the curve fitting analysis of C ls and F ls XPS spectra, the chemical components and their intensity ratio were determined. The reason for the chemical composition change by the SR irradiation was discussed. (author)

  20. Electron multiplier as a detector for soft x rays from synchrotron and laser plasma sources

    Science.gov (United States)

    Buckley, Christopher J.; Dermody, Geraint; Khaleque, Naz I.; Michette, Alan G.; Pfauntsch, Slawka J.; Turcu, I. C. Edmond; Allott, Ric M.

    1998-11-01

    An electron-tubes-LTD 129EM electron multiplier tube has been modified to act as a detector of soft x-rays. the first dynode was coated with 100 nm of CsI and the assembly was mounted in a small vacuum chamber with 100 nm thick silicon nitride entrance window. Initial tests show the detector is linear up to an input flux of approximately 1MHz on a synchrotron source and has proved effective in providing pulse height discrimination when used on a pulsed laser plasma source.

  1. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    Energy Technology Data Exchange (ETDEWEB)

    Tiwari, M. K., E-mail: mktiwari@rrcat.gov.in; Singh, A. K., E-mail: mktiwari@rrcat.gov.in; Das, Gangadhar, E-mail: mktiwari@rrcat.gov.in; Chowdhury, Anupam, E-mail: mktiwari@rrcat.gov.in; Lodha, G. S., E-mail: mktiwari@rrcat.gov.in [Indus Synchrotrons Utilisation Division, Raja Ramanna Centre for Advanced Technology, Indore-452013 (India)

    2014-04-24

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  2. Total and available metal contents in sediments by synchrotron radiation total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Sobrinho, Gilmar A. [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil]. E-mail: silvana@fecf.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), SP (Brazil); Jesus, Edgar F.O. de; Lopes, Ricardo T. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia

    2002-07-01

    In this work the total and available contents of Al, Si, Cl, K, Mn, Fe, Co, Ni, Cu, Zn, Sr, Zr, Ba, Ce and Pb in sediments from river Atibaia were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence technique. The detection limits for K series varies from 200 ng.mL{sup -1} for Al to 2 ng.mL{sup -1} for Zn while for L series the value varies from 20 ng.mL{sup -1} for Ba to 10 ng.mL{sup -1} for Pb. The samples were submitted to two different processes, in order to obtain the total and biological available metal contents. The information about metal content is a important parameter for a correct evaluation about the hydrologic cycle in Piracicaba basin. All the measure were carried out at the National Synchrotron Light Laboratory, Campinas, SP, Brazil, using a white beam for excitation. (author)

  3. Extending the possibilities in phase space analysis of synchrotron radiation x-ray optics.

    Science.gov (United States)

    Ferrero, Claudio; Smilgies, Detlef-Matthias; Riekel, Christian; Gatta, Gilles; Daly, Peter

    2008-08-01

    A simple analytical approach to phase space analysis of the performance of x-ray optical setups (beamlines) combining several elements in position-angle-wavelength space is presented. The mathematical description of a large class of optical elements commonly used on synchrotron beamlines has been reviewed and extended with respect to the existing literature and is reported in a revised form. Novel features are introduced, in particular, the possibility to account for imperfections on mirror surfaces and to incorporate nanofocusing devices like refractive lenses in advanced beamline setups using the same analytical framework. Phase space analysis results of the simulation of an undulator beamline with focusing optics at the European Synchrotron Radiation Facility compare favorably with results obtained by geometric ray-tracing methods and, more importantly, with experimental measurements. This approach has been implemented into a simple and easy-to-use program toolkit for optical calculations based on the Mathematica software package.

  4. Investigation of mineral distribution in bone by synchrotron X-ray fluorescence microscopy after tibolone therapy

    Energy Technology Data Exchange (ETDEWEB)

    Lima, I. [Rio de Janeiro State Univ., Nova Friburgo, RJ (Brazil). Dept. of Mechanical Engineering and Energy; Federal Univ. of Rio de Janeiro, RJ (Brazil). Nuclear Instrumentation Lab. - COPPE; Carvalho, A.C.B.; Henriques, H.N.; Guzman-Silva, M.A. [Fluminense Federal Univ., Niteroi, RJ (Brazil). Lab. of Experimental Pathology; Sales, E.; Lopes, R.T. [Federal Univ. of Rio de Janeiro, RJ (Brazil). Nuclear Instrumentation Lab. - COPPE; Granjeiro, J.M. [Fluminense Federal Univ., Niteroi, RJ (Brazil). Dept. of Cellular and Molecular Biology

    2011-07-01

    Tibolone is a synthetic steroid with estrogenic, androgenic, and progestagenic properties used for the prevention of postmenopausal osteoporosis and treatment of climacteric symptoms. Tibolone shows almost no action on breast and endometrium, which are target-organs for estrogens and progesterone activity. The aim of this work was to investigate the spatial distribution of calcium and zinc minerals in the femoral head of ovariectomized rat in order to evaluate the effects of the long-term administration of tibolone. For that purpose X-ray microfluorescence was used with synchrotron radiation imaging technique which was performed at Brazilian Light Synchrotron Laboratory, Campinas, SP. Minerals were not homogeneously distributed in trabecular bone areas; a higher concentration of calcium in the trabecular regions at femoral heads was found in ovariectomized and tibolone-treated rats compared to ovariectomized and control groups. (orig.)

  5. Multielemental analysis in Brazilian cigarettes using total reflection X-ray fluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T.; Moreira, Silvana

    2005-01-01

    In order to identify major and trace elements in conventional and light Brazilian cigarettes, Total Reflection X-Ray Fluorescence with Synchrotron Radiation (SR-TXRF) was used. The fluorescence measurements were carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo. This technique enables detection limit is in the ngg -1 range, which is very useful in elemental tobacco smoke analysis, since it presents most of its elements at a trace level. The major elements identified in tobacco samples were: S, Cl, K, Ca, Mn, Fe and Cd, and the trace elements were: Ti, Cr, Ni, Cu, Zn, Br, Rb, Sr and Ba. However in tobacco smoke samples, there were only two major elements: K and Ca, the others were present a trace level. The rate transfer of tobacco to tobacco smoke was about 2.5 % for all elements studied. (author)

  6. Online monitoring the detector calibration process at a synchrotron X-ray source

    Science.gov (United States)

    Li, Huapng; Zhao, Yidong; Zheng, Lei; Tang, Kun; Liu, Shuhu; Zhao, Xiaoliang; Zhao, Yashuai; Li, Fan

    2017-12-01

    This paper describes an online noble gas monitor used for the detector calibration process with a cryogenic radiometer. The process is implemented under a high-flux synchrotron radiation X-ray source in the energy range from 2100 to 6000 eV at the Beijing Synchrotron Radiation Facility (BSRF). This online monitoring system aims to lower the uncertainty of the calibration results caused by electron beam decay in the storage ring during the detector calibration process. Because the calibration process is performed under the high vacuum condition, an ionization chamber with adjustable Kr gas pressure is chosen as the monitoring device. To decrease the electronic noise, a method for obtaining the signal by collecting the counts within a specified time has been applied. Under the properly controlled conditions, the uncertainty of the calibration results introduced by the online monitoring system is estimated to be better than 0.15%, which can meet the demands of various high-precision calibration processes.

  7. Synchrotron radiation based micro X-ray fluorescence analysis of the calibration samples used in surface sensitive total reflection and grazing emission X-ray fluorescence techniques

    Science.gov (United States)

    Kubala-Kukuś, A.; Banaś, D.; Pajek, M.; Szlachetko, J.; Jagodziński, P.; Susini, J.; Salomé, M.

    2013-12-01

    Total reflection X-ray fluorescence (TXRF) and grazing emission X-ray fluorescence (GEXRF) are surface sensitive techniques and can be used for detailed surface studies of different materials, including ultra-low concentration contamination or the lateral and depth distributions of elements. The calibration procedure typically used involves placing a micro-droplet (˜μl) of the standard solution onto a silicon wafer (or quartz backing). After evaporation of the solvent, the residual amount of elements is used as a reference standard. Knowledge of the distribution of residue material on the substrate surface is crucial for precise quantification. In the present work the investigation of the lateral distribution of elements in the multielemental calibrating samples, containing the 23 most commonly studied elements, by using the synchrotron radiation based micro X-ray fluorescence is presented. The goal of this project was the study of a uniformity of the elemental distributions and determination of the residual elements morphology depending on the temperature of the drying process. The X-ray images were compared with optical and SEM images. Paper presents in details the experimental setup, sample preparation procedures, measurements and results. In the analysis of the X-ray images of the sample dried in high temperature the censoring approach was applied improving the quality of statistical analysis. The information on the elements distribution in the calibrating samples can be useful for developing more accurate calibration procedures applied in quantitative analysis of surface sensitive TXRF and GEXRF techniques.

  8. STEADY X-RAY SYNCHROTRON EMISSION IN THE NORTHEASTERN LIMB OF SN 1006

    International Nuclear Information System (INIS)

    Katsuda, Satoru; Petre, Robert; Mori, Koji; Reynolds, Stephen P.; Long, Knox S.; Winkler, P. Frank; Tsunemi, Hiroshi

    2010-01-01

    We investigate time variations and detailed spatial structures of X-ray synchrotron emission in the northeastern limb of SN 1006, using two Chandra observations taken in 2000 and 2008. We extract spectra from a number of small (∼10'') regions. After taking account of proper motion and isolating the synchrotron from the thermal emission, we study time variations in the synchrotron emission in the small regions. We find that there are no regions showing strong flux variations. Our analysis shows an apparent flux decline in the overall synchrotron flux of ∼4% at high energies, but we suspect that this is mostly a calibration effect, and that flux is actually constant to ∼1%. This is much less than the variation found in other remnants where it was used to infer magnetic-field strengths up to 1 mG. We attribute the lack of variability to the smoothness of the synchrotron morphology, in contrast to the small-scale knots found to be variable in other remnants. The smoothness is to be expected for a Type Ia remnant encountering uniform material. Finally, we find a spatial correlation between the flux and the cutoff frequency in synchrotron emission. The simplest interpretation is that the cutoff frequency depends on the magnetic-field strength. This would require that the maximum energy of accelerated electrons is not limited by synchrotron losses, but by some other effect. Alternatively, the rate of particle injection and acceleration may vary due to some effect not yet accounted for, such as a dependence on shock obliquity.

  9. Advancements and Application of Microsecond Synchrotron X-ray Footprinting at the Advanced Light Source

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, Sayan; Celestre, Rich; Feng, Jun; Ralston, Corie

    2016-01-02

    The method of synchrotron X-ray protein footprinting (XF-MS) is used to determine protein conformational changes, folding, protein-protein and protein-ligand interactions, providing information which is often difficult to obtain using X-ray crystallography and other common structural biology methods [1 G. Xu and M.R. Chance, Chemical Reviews 107, 3514–3543 (2007). [CrossRef], [PubMed], [Web of Science ®], [Google Scholar] –3 V.N. Bavro, Biochem Soc Trans 43, 983–994 (2015). [CrossRef], [PubMed], [Web of Science ®], [Google Scholar] ]. The technique uses comparative in situ labeling of solvent-accessible side chains by highly reactive hydroxyl radicals (•OH) in buffered aqueous solution under different assay conditions. In regions where a protein is folded or binds a partner, these •OH susceptible sites are inaccessible to solvent, and therefore protected from labeling. The •OH are generated by the ionization of water using high-flux-density X-rays. High-flux density is a key factor for XF-MS labeling because obtaining an adequate steady-state concentration of hydroxyl radical within a short irradiation time is necessary to minimize radiation-induced secondary damage and also to overcome various scavenging reactions that reduce the yield of labeled side chains.

  10. Absorption and Phase Contrast X-Ray Imaging in Paleontology Using Laboratory and Synchrotron Sources

    Energy Technology Data Exchange (ETDEWEB)

    Bidola, Pidassa; Stockmar, Marco; Achterhold, Klaus; Pfeiffer, Franz; Pacheco, Mirian L.A.F.; Soriano, Carmen; Beckmann, Felix; Herzen, Julia

    2015-10-01

    X-ray micro-computed tomography (CT) is commonly used for imaging of samples in biomedical or materials science research. Owing to the ability to visualize a sample in a nondestructive way, X-ray CT is perfectly suited to inspect fossilized specimens, which are mostly unique or rare. In certain regions of the world where important sedimentation events occurred in the Precambrian geological time, several fossilized animals are studied to understand questions related to their origin, environment, and life evolution. This article demonstrates the advantages of applying absorption and phase-contrast CT on the enigmatic fossil Corumbella werneri, one of the oldest known animals capable of building hard parts, originally discovered in Corumba (Brazil). Different tomographic setups were tested to visualize the fossilized inner structures: a commercial laboratory-based CT device, two synchrotron-based imaging setups using conventional absorption and propagation-based phase contrast, and a commercial X-ray microscope with a lens-coupled detector system, dedicated for radiography and tomography. Based on our results we discuss the strengths and weaknesses of the different imaging setups for paleontological studies.

  11. Synchrotron Vacuum Ultraviolet Light and Soft X-Ray Radiation Effects on Aluminized Teflon FEP Investigated

    Science.gov (United States)

    Dever, Joyce A.; Townsend, Jacqueline A.; Gaier, James R.; Jalics, Alice I.

    1999-01-01

    Since the Hubble Space Telescope (HST) was deployed in low Earth orbit in April 1990, two servicing missions have been conducted to upgrade its scientific capabilities. Minor cracking of second-surface metalized Teflon FEP (DuPont; fluorinated ethylene propylene) surfaces from multilayer insulation (MLI) was first observed upon close examination of samples with high solar exposure retrieved during the first servicing mission, which was conducted 3.6 years after deployment. During the second HST servicing mission, 6.8 years after deployment, astronaut observations and photographic documentation revealed significant cracks in the Teflon FEP layer of the MLI on both the solar- and anti-solar-facing surfaces of the telescope. NASA Goddard Space Flight Center directed the efforts of the Hubble Space Telescope MLI Failure Review Board, whose goals included identifying the low-Earth-orbit environmental constituent(s) responsible for the cracking and embrittling of Teflon FEP which was observed during the second servicing mission. The NASA Lewis Research Center provided significant support to this effort. Because soft x-ray radiation from solar flares had been considered as a possible cause for the degradation of the mechanical properties of Teflon FEP (ref. 1), the effects of soft xray radiation and vacuum ultraviolet light on Teflon FEP were investigated. In this Lewisled effort, samples of Teflon FEP with a 100-nm layer of vapor-deposited aluminum (VDA) on the backside were exposed to synchrotron radiation of various vacuum ultraviolet and soft x-ray wavelengths between 18 nm (69 eV) and 0.65 nm (1900 eV). Synchrotron radiation exposures were conducted using the National Synchrotron Light Source at Brookhaven National Laboratory. Samples of FEP/VDA were exposed with the FEP surface facing the synchrotron beam. Doses and fluences were compared with those estimated for the 20-yr Hubble Space Telescope mission.

  12. Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

    Science.gov (United States)

    Post, J. E.; Bish, D. L.; Heaney, P. J.

    2006-05-01

    Sepiolite is a hydrous Mg-silicate clay mineral with fibrous morphology that typically occurs as fine-grained, poorly crystalline masses. It occurs in a wide variety of geological environments and has been mined for centuries because of its many uses, e.g. in the pharmaceutical, fertilizer, and pesticide industries. Its versatile functionality derives from the large surface area and microporosity that are characteristic of the material. In recent years, sepiolite has received considerable attention with regard to the adsorption of organics, for use as a support for catalysts, as a molecular sieve, and as an inorganic membrane for ultrafiltration. Because of its fine-grained and poorly crystalline nature, it has not been possible to study sepiolite's crystal structure using single-crystal X-ray diffraction methods, and consequently many details of the structure are still not well known. In this study, Rietveld refinements using synchrotron powder X-ray diffraction data were used to investigate the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room- temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic water site. The RT structure under vacuum retained only ~1/8 of the zeolitic water and the volume decreased 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic water is lost by ~390 K, accompanied by a decrease in the a and c unit-cell parameters. Above ~600 K the sepiolite structure folds as one-half of the crystallographically bound water is lost. Rietveld refinements of the "anhydrous" sepiolite structure reveal that, in general, unit-cell parameters a, b, â and volume steadily decrease with increasing temperature; there is an obvious change in slope at ~820 K suggesting a phase

  13. Proceedings of the 10. International conference on small-angle scattering; Workshop on synchrotron radiation and neutron SAS: instrumentation and industrial applications. Abstracts

    International Nuclear Information System (INIS)

    Craievich, Aldo

    1996-01-01

    This publication contains the abstracts of the papers presented during the 10. International conference on small-angle scattering (SAS-96) and also during the Workshop on synchrotron radiation and neutron SAS: instrumentation and industrial applications. Works on the areas of inorganic materials, polymers, biology and liquid crystals are presented

  14. Mapping Metal Elements of Shuangbai Dinosaur Fossil by Synchrotron X-ray Fluorescence Microprobe

    International Nuclear Information System (INIS)

    Wang, Y.; Qun, Y.; Ablett, J.

    2008-01-01

    The metal elements mapping of Shuangbai dinosaur fossil, was obtained by synchrotron x-ray fluorescence (SXRF). Eight elements, Ca, Mn, Fe, Cu, Zn, As, Y and Sr were determined. Elements As and Y were detected for the first time in the dinosaur fossil. The data indicated that metal elements are asymmetrical on fossil section. This is different from common minerals. Mapping metals showed that metal element As is few. The dinosaur most likely belongs to natural death. This is different from Zigong dinosaurs which were found dead from poisoning. This method has been used to find that metals Fe and Mn are accrete, and the same is true for Sr and Y. This study indicated that colloid granule Fe and Mn, as well as Sr and Y had opposite electric charges in lithification process of fossils. By this analysis, compound forms can be ascertained. Synchrotron light source x-ray fluorescence is a complementary method that shows mapping of metal elements at the dinosaur fossil, and is rapid, exact and intuitionist. This study shows that dinosaur fossil mineral imaging has a potential in reconstructing the paleoenvironment and ancient geology.

  15. Analysis of synchrotron X-ray diffraction patterns from fluorotic enamel samples

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Ana P.G.; Braz, Delson, E-mail: anapaulagalmeida@gmail.co [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Lab. de Instrumentacao Nuclear; Colaco, Marcos V.; Barroso, Regina C., E-mail: cely@uerj.b [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Inst. de Fisica; Porto, Isabel M., E-mail: belporto@ig.com.b [Universidade Estadual de Campinas (UNICAMP), Piracicaba, SP (Brazil). Faculdade de Odontologia; Gerlach, Raquel F., E-mail: rfgerlach@forp.usp.b [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Odontologia; Droppa Junior, Roosevelt, E-mail: rdroppa@lnls.b [Associacao Brasileira de Tecnologia de Luz Sincrotron (ABTLuS), Campinas, SP (Brazil)

    2009-07-01

    With the introduction of fluoride as the main anticaries agent used in preventive dentistry, and perhaps an increase in fluoride in our food chain, dental fluorosis has become an increasing world-wide problem. Visible signs of fluorosis begin to become obvious on the enamel surface as opacities, implying some porosity in the tissue. The mechanisms that conduct the formation of fluorotic enamel are unknown, but should involve modifications in the basics physical-chemistry reactions of demineralisation and remineralisation of the enamel of the teeth, which is the same reaction of formation of the enamel's hydroxyapatite (HAp) in the maturation phase. The increase of the amount of fluoride inside of the apatite will result in gradual increase of the lattice parameters. The hexagonal symmetry seems to work well with the powder diffraction data, and the crystal structure of HAp is usually described in space group P63/m. The aim of this work is to characterize the healthy and fluorotic enamel in human tooth using technique Synchrotron X-ray diffraction in order to determine the crystal structure and crystallinity of on fluoroapatite (FAp) crystal present in fluoritic enamel. All the scattering profile measurements was carried out at the X-ray diffraction beamline (XRD1) at the National Synchrotron Light Laboratory - LNLS, Campinas, Brazil. (author)

  16. Evaluation of osteoporotic bone structure through synchrotron radiation X-ray microfluorescence images

    Energy Technology Data Exchange (ETDEWEB)

    Lima, I. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil)], E-mail: inaya@lin.ufrj.br; Anjos, M.J. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil); Physics Institute, UERJ (Brazil); Farias, M.L.F. [University Hospital, UFRJ (Brazil); Pantaleao, T.U.; Correa da Costa, V.M. [Biophysics Institute, UFRJ (Brazil); Lopes, R.T. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil)

    2008-12-15

    The abnormal accumulation or deficiency of trace elements may theoretically impair the formation of bone and contribute to osteoporosis. In this context, the knowledge of major and trace elements is very important in order to clarify many issues regarding diseases of the bone, such as osteoporosis, that remain unresolved. Several kinds of imaging techniques can be useful to access morphology and the minerals present in osteoporotic bones. In this work, synchrotron radiation X-ray microfluorescence was used as an X-ray imaging technique to investigate bone structures. Therefore, this research aims to improve the knowledge about some aspects of bone quality. The measurements were carried out at the Brazilian Synchrotron Laboratory Light Laboratory, in Brazil. A white beam with an energy range of 4-23 keV, a 45 deg./45 deg. geometry and a capillary optics were used. It was demonstrated that bone quality can and must be evaluated not only by considering the architecture of bones but also by taking into account the concentration and the distribution of minerals. Our results showed that the elemental distributions in bone zones on a micron scale were very helpful to understand functions in those structures.

  17. ENDIX. A computer program to simulate energy dispersive X-ray and synchrotron powder diffraction diagrams

    International Nuclear Information System (INIS)

    Hovestreydt, E.; Karlsruhe Univ.; Parthe, E.; Benedict, U.

    1987-01-01

    A Fortran 77 computer program is described which allows the simulation of energy dispersive X-ray and synchrotron powder diffraction diagrams. The input consists of structural data (space group, unit cell dimensions, atomic positional and displacement parameters) and information on the experimental conditions (chosen Bragg angle, type of X-ray tube and applied voltage or operating power of synchrotron radiation source). The output consists of the normalized intensities of the diffraction lines, listed by increasing energy (in keV), and of an optional intensity-energy plot. The intensities are calculated with due consideration of the wave-length dependence of both the anomalous dispersion and the absorption coefficients. For a better agreement between observed and calculated spectra provision is made to optionally superimpose, on the calculated diffraction line spectrum, all additional lines such as fluorescence and emission lines and escape peaks. The different effects which have been considered in the simulation are discussed in some detail. A sample calculation of the energy dispersive powder diffraction pattern of UPt 3 (Ni 3 Sn structure type) is given. Warning: the user of ENDIX should be aware that for a successful application it is necessary to adapt the program to correspond to the actual experimental conditions. Even then, due to the only approximately known values of certain functions, the agreement between observed and calculated intensities will not be as good as for angle dispersive diffraction methods

  18. Synchrotron X-ray measurement techniques for thermal barrier coated cylindrical samples under thermal gradients.

    Science.gov (United States)

    Siddiqui, Sanna F; Knipe, Kevin; Manero, Albert; Meid, Carla; Wischek, Janine; Okasinski, John; Almer, Jonathan; Karlsson, Anette M; Bartsch, Marion; Raghavan, Seetha

    2013-08-01

    Measurement techniques to obtain accurate in situ synchrotron strain measurements of thermal barrier coating systems (TBCs) applied to hollow cylindrical specimens are presented in this work. The Electron Beam Physical Vapor Deposition coated specimens with internal cooling were designed to achieve realistic temperature gradients over the TBC coated material such as that occurring in the turbine blades of aeroengines. Effects of the circular cross section on the x-ray diffraction (XRD) measurements in the various layers, including the thermally grown oxide, are investigated using high-energy synchrotron x-rays. Multiple approaches for beam penetration including collection, tangential, and normal to the layers, along with variations in collection parameters are compared for their ability to attain high-resolution XRD data from the internal layers. This study displays the ability to monitor in situ, the response of the internal layers within the TBC, while implementing a thermal gradient across the thickness of the coated sample. The thermal setup maintained coating surface temperatures in the range of operating conditions, while monitoring the substrate cooling, for a controlled thermal gradient. Through variation in measurement location and beam parameters, sufficient intensities are obtained from the internal layers which can be used for depth resolved strain measurements. Results are used to establish the various techniques for obtaining XRD measurements through multi-layered coating systems and their outcomes will pave the way towards goals in achieving realistic in situ testing of these coatings.

  19. X-ray diffraction studies on single and mixed confectionery fats using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    MacMillan, S.C.; Roberts, K.J.; Wells, M.; Polgreen, M.; Smith, I. [Heriot-Watt University, Edinburgh, (United Kingdom). Department of Mechanical and Chemical Engineering, Centre for Molecular and Interface Engineering

    1999-12-01

    and stirring rate (shear rate). The X-rays used are from a high intensity synchrotron radiation source, enabling polymorphic phase transformations for a variety of fat mixtures to observed. Copyright (1999) Australian X-ray Analytical Association Inc.

  20. X-ray diffraction studies on single and mixed confectionery fats using synchrotron radiation

    International Nuclear Information System (INIS)

    MacMillan, S.C.; Roberts, K.J.; Wells, M.; Polgreen, M.; Smith, I.

    1999-01-01

    and stirring rate (shear rate). The X-rays used are from a high intensity synchrotron radiation source, enabling polymorphic phase transformations for a variety of fat mixtures to observed. Copyright (1999) Australian X-ray Analytical Association Inc