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Sample records for anomalous small-angle x-ray

  1. 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.

  2. 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.

  3. 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.

  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. 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.

  6. Anomalous and resonance small-angle scattering

    International Nuclear Information System (INIS)

    Epperson, J.E.; Thiyagarajan, P.

    1988-01-01

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

  7. Anomalous and resonance small angle scattering

    International Nuclear Information System (INIS)

    Epperson, J.E.; Thiyagarajan, P.

    1987-11-01

    Significant changes in the small angle scattered intensity can be induced by making measurements with radiation close to an absorption edge of an appropriate atomic species contained in the sample. These changes can be related quantitatively to the real and imaginary anomalous dispersion terms for the scattering factor (x-rays) or scattering length (neutrons). The physics inherent in these anomalous dispersion terms is first discussed before considering how they enter the relevant scattering theory. Two major areas of anomalous scattering research have emerged; macromolecules in solution and unmixing of metallic alloys. Research in each area is reviewed, illustrating both the feasibility and potential of these techniques. All the experimental results reported to date have been obtained with x-rays. However, it is pointed out that the formalism is the same or the analogue experiment with neutrons, and a number of suitable isotopes exist which exhibit resonance in an accessible range of energy. Potential applications of resonance small-angle neutron scatterings are discussed. 8 figs

  8. 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 ...

  9. 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 ...

  10. 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 ...

  11. A comparison of the merits of isotopic substitution in neutron small-angle scattering and anomalous X-ray scattering for the evaluation of partial structure functions in a ternary alloy

    International Nuclear Information System (INIS)

    Simon, J.P.; Grenoble-1 Univ., 38; Lyon, O.; Paris-11 Univ., 91 - Orsay; Fontaine, D. de

    1985-01-01

    Solute partitioning during decomposition of a ternary alloy may be evaluated through the inversion of a system of linear equations, obtained by performing at least three independent small-angle scattering experiments. The merits of neutron scattering (with isotopic contrast) and of anomalous X-ray scattering (near the absorption edges) are compared. It appears that neutron scattering, although having good contrast, is not suited to these studies since slight structural differences between the three samples may lead to erroneous results. On the other hand, the use of the same sample in anomalous scattering avoids this problem, but with the drawback of a more ill-conditioned system. Nevertheless, the possibility of performing more than three anomalous experiments may improve the results and a new analysis of data is proposed. (orig.)

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

    International Nuclear Information System (INIS)

    Vollet, D.

    1983-01-01

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

  13. 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.

  14. 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

  15. 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

  16. Dietary iron-loaded rat liver haemosiderin and ferritin: in situ measurement of iron core nanoparticle size and cluster structure using anomalous small-angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Bovell, Eliza; Buckley, Craig E.; Chua-anusorn, Wanida; Cookson, David; Kirby, Nigel; Saunders, Martin; St. Pierre, Timothy G. ((UWA)); ((Curtin U.)); ((ASRP))

    2009-03-16

    The morphology, particle size distribution and cluster structure of the hydrated iron(III) oxyhydroxide particles associated with haemosiderin and ferritin in dietary iron-loaded rat liver tissue have been investigated using transmission electron microscopy (TEM) and anomalous small-angle x-ray scattering (ASAXS). Rat liver tissue was removed from a series of female Porton rats which had been fed an iron-rich diet until sacrifice at various ages from 2-24 months. Hepatic iron concentrations ranged from 1 to 65 mg Fe g{sup -1} dry tissue. TEM studies showed both dispersed and clustered iron-containing nanoparticles. The dispersed particles were found to have mean sizes ({+-}standard deviation) of 54 {+-} 8 {angstrom} for the iron-loaded animals and 55 {+-} 7 {angstrom} for the controls. Superposition of particles in TEM images prevented direct measurement of nanoparticulate size in the clusters. The ASAXS data were modelled to provide a quantitative estimate of both the size and spacing of iron oxyhydroxide particles in the bulk samples. The modelling yielded close-packed particles with sizes of 60 to 78 {angstrom} which when corrected for anomalous scattering suggests sizes from 54 to 70 {angstrom}. Particle size distributions are of particular importance since they determine the surface iron to core iron ratios, which in turn are expected to be related to the molar toxicity of iron deposits in cells.

  17. 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)

  18. 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.

  19. 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)

  20. 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)

  1. 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

  2. Anomalous X-Ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Wendin, G.

    1979-01-01

    The availability of tunable synchrotron radiation has made it possible systematically to perform x-ray diffraction studies in regions of anomalous scattering near absorption edges, e.g., in order to derive phase information for crystal structure determination. An overview is given of recent experimental and theoretical work and discussion of the properties of the anomalous atomic scattering factor, with emphasis on threshold resonances and damping effects. The results are applied to a discussion of the very strong anomalous dispersion recently observed near the L3 edge in a cesium complex. Also given is an overview of elements and levels where similar behavior can be expected. Finally, the influence of solid state and chemical effects on the absorption edge structure is discussed. 64 references.

  3. Anomalous x-ray scattering

    International Nuclear Information System (INIS)

    Wendin, G.

    1979-01-01

    The availability of tunable synchrotron radiation has made it possible systematically to perform x-ray diffraction studies in regions of anomalous scattering near absorption edges, e.g. in order to derive phase information for crystal structure determination. An overview is given of recent experimental and theoretical work and discuss the properties of the anomalous atomic scattering factor, with emphasis on threshold resonances and damping effects. The results are applied to a discussion of the very strong anomalous dispersion recently observed near the L 3 edge in a cesium complex. Also given is an overview of elements and levels where similar behavior can be expected. Finally, the influence of solid state and chemical effects on the absorption edge structure is discussed. 64 references

  4. 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...

  5. 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.

  6. 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

  7. 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.

  8. 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.)

  9. 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

  10. 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.

  11. 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.

  12. 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...

  13. 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.

  14. 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

  15. 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 ...

  16. 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 ...

  17. 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.

  18. 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.)

  19. 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.)

  20. 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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  2. 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.

  3. 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

  4. 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.

  5. 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.)

  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. 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

  8. 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.

  9. 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.

  10. 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)

  11. 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.

  12. 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.

  13. 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...

  14. 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.

  15. 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.

  16. 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

  17. 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.

  18. 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.

  19. 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)

  20. 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)

  1. 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.

  2. 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.

  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. 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.

  5. 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.

  6. 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.

  7. 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.)

  8. 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.

  9. 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.

  10. 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....

  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. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.)

  18. 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.

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. 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

  6. 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

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  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. 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.

  15. 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.)

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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)

  1. 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

  2. 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

  3. 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...

  4. 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.

  5. 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...

  6. 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...

  7. Diffraction anomalous fine structure using X-ray anomalous dispersion

    International Nuclear Information System (INIS)

    Soejima, Yuji; Kuwajima, Shuichiro

    1998-01-01

    A use of X-ray anomalous dispersion effects for structure investigation has recently been developed by using synchrotron radiation. One of the interesting method is the observation of anomalous fine structure which arise on diffraction intensity in energy region of incident X-ray at and higher than absorption edge. The phenomenon is so called Diffraction Anomalous Fine Structure (DAFS). DAFS originates in the same physical process an that of EXAFS: namely photoelectric effect at the corresponding atom and the interaction of photoelectron waves between the atom and neighboring atoms. In contrast with EXAFS, the method is available for only the crystalline materials, but shows effective advantages of the structure investigations by a use of diffraction: one is the site selectivity and the other is space selectivity. In the present study, demonstrations of a use of X-ray anomalous dispersion effect for the superstructure determination will be given for the case of PbZrO 3 , then recent trial investigations of DAFS in particular on the superlattice reflections will be introduced. In addition, we discuss about Forbidden Reflection near Edge Diffraction (FRED) which is more recently investigated as a new method of the structure analysis. (author)

  8. 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

  9. 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.

  10. 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.)

  11. 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.

  12. 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.

  13. 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.

  14. 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

  15. 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...

  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 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

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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

  5. 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)

  6. 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.

  7. 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

  8. 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

  9. 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

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.)

  15. 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..

  16. 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.).

  17. 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.)

  18. 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.

  19. Structure investigation of metal ions clustering in dehydrated gel using x-ray anomalous dispersion effect

    CERN Document Server

    Soejima, Y; Sugiyama, M; Annaka, M; Nakamura, A; Hiramatsu, N; Hara, K

    2003-01-01

    The structure of copper ion clusters in dehydrated N-isopropylacrylamide/sodium acrylate (NIPA/SA) gel has been studied by means of small angle X-ray scattering (SAXS) method. In order to distinguish the intensity scattered by Cu ions, the X-ray anomalous dispersion effect around the Cu K absorption edge has been coupled with SAXS. It is found that the dispersion effect dependent on the incident X-ray energy is remarkable only at the momentum transfer q = 0.031 A sup - sup 1 , where a SAXS peak is observed. The results indicate that copper ions form clusters in the dehydrated gel, and that the mean size of clusters is the same as that of SA clusters produced by microphase separation. It is therefore naturally presumed that copper ions are adsorbed into the SA molecules. On the basis of the presumption, a mechanism is proposed for microphase-separation and clustering of Cu ions.

  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. 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

  3. 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.

  4. 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.

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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)

  13. 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.

  14. 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.

  15. 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.)

  16. 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.)

  17. 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.

  18. 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

  19. 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

  20. 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....

  1. 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.

  2. 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

  3. 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.

  4. 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

  5. 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.

  6. 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...

  7. 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

  8. 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.

  9. 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

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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)

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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...

  1. 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...

  2. 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.

  3. 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...

  4. 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

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. 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.

  11. 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.

  12. 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

  13. 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.

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

    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.

  15. 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

  16. 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.

  17. 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.

  18. 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...

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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...

  4. 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.

  5. 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.

  6. 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.

  7. 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).

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Understanding the X-ray spectrum of anomalous X-ray pulsars and soft gamma-ray repeaters

    Science.gov (United States)

    Guo, Yan-Jun; Dai, Shi; Li, Zhao-Sheng; Liu, Yuan; Tong, Hao; Xu, Ren-Xin

    2015-04-01

    Hard X-rays above 10 keV are detected from several anomalous X-ray pulsars (AXPs) and soft gamma-ray repeaters (SGRs), and different models have been proposed to explain the physical origin within the frame of either a magnetar model or a fallback disk system. Using data from Suzaku and INTEGRAL, we study the soft and hard X-ray spectra of four AXPs/SGRs: 1RXS J170849-400910, 1E 1547.0-5408, SGR 1806-20 and SGR 0501+4516. It is found that the spectra could be well reproduced by the bulk-motion Comptonization (BMC) process as was first suggested by Trümper et al., showing that the accretion scenario could be compatible with X-ray emission from AXPs/SGRs. Simulated results from the Hard X-ray Modulation Telescope using the BMC model show that the spectra would have discrepancies from the power-law, especially the cutoff at ˜200 keV. Thus future observations will allow researchers to distinguish different models of the hard X-ray emission and will help us understand the nature of AXPs/SGRs. Supported by the National Natural Science Foundation of China.

  13. 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.

  14. 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.

  15. 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

  16. 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...

  17. 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...

  18. 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

  19. 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.

  20. 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.

  1. 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

  2. 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

  3. 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....

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.).

  9. Methods in the determination of partial structure factors of disordered matter by neutron and anomalous X-ray diffraction

    International Nuclear Information System (INIS)

    Suck, J.B.; Chieux, P.; Raoux, D.; Riekel, C.

    1993-01-01

    A general introduction into all possible binary correlations (nuclear-nuclear correlations, mass-mass, charge-charge, nuclear-magnetic, nuclear-electronic, etc.), is followed by methods used in connection with neutron diffraction (and also to neutron inelastic scattering) like isotopic substitution, first and second order difference methods, isomorphic substitution and anomalous neutron diffraction. Then the X-ray anomalous scattering methods used specifically in connection with synchrotron radiation are presented. For both radiation methods and results for wide angle and small angle diffraction are included. Applications of both methods to special systems and problems inherent in these combinations are discussed. Methods and results obtained by computer simulations, Reverse Monte Carlo calculations and a new regularization method used in context with an optimization of compatible data obtained with different methods on the same system, are presented. A translation kit is proposed for semantic purposes between the two domains

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Discovery of Hard Nonthermal Pulsed X-Ray Emission from the Anomalous X-Ray Pulsar 1E 1841-045

    NARCIS (Netherlands)

    Kuiper, L.; Hermsen, W.; Méndez, R.M.

    2004-01-01

    We report the discovery of nonthermal pulsed X-ray/soft gamma-ray emission up to ~150 keV from the anomalous 11.8 s X-ray pulsar AXP 1E 1841-045 located near the center of supernova remnant Kes 73 using Rossi X-Ray Timing Explorer (RXTE) Proportional Counter Array and High Energy X-Ray Timing

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. Macromolecular X-ray structure determination using weak, single-wavelength anomalous data

    Energy Technology Data Exchange (ETDEWEB)

    Bunkóczi, Gábor; McCoy, Airlie J.; Echols, Nathaniel; Grosse-Kunstleve, Ralf W.; Adams, Paul D.; Holton, James M.; Read, Randy J.; Terwilliger, Thomas C.

    2014-12-22

    We describe a likelihood-based method for determining the substructure of anomalously scattering atoms in macromolecular crystals that allows successful structure determination by single-wavelength anomalous diffraction (SAD) X-ray analysis with weak anomalous signal. With the use of partial models and electron density maps in searches for anomalously scattering atoms, testing of alternative values of parameters and parallelized automated model-building, this method has the potential to extend the applicability of the SAD method in challenging cases.

  3. 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

  4. 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.

  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

    2011-12-16

    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.

  6. 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

  7. 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

  8. Determination of X-ray anomalous scattering in silicon

    International Nuclear Information System (INIS)

    Cusatis, C.

    1987-01-01

    The linear attenuation coeficient for X-ray in silicon was measured with approximately 0,1% accuracy, for 6 diferent wavelenghts of caracteristic radiation. From these result the imaginary parts of the atomic scattering factors, for silicon and for those wavelenghts, were obtained with the same accuracy. The results are compared with the most recent published values. The proposed method to avoid Rayleigh scattering can be used for any type of ''perfect'' crystal. (author) [pt

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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...

  14. 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.)

  15. Precise small-angle X-ray scattering evaluation of the pore structures in track-etched membranes: Comparison with other convenient evaluation methods

    Energy Technology Data Exchange (ETDEWEB)

    Miyazaki, Tsukasa, E-mail: t_miyazaki@cross.or.jp [Neutron Science and Technology Center, Comprehensive Research Organization for Science and Society, 162-1, Shirakata, Tokai-mura, Naka-gun, Ibaraki 319-1106 (Japan); Takenaka, Mikihito [Department of Polymer Chemistry, Gradual School of Engineering, Kyoto University, Kyotodaigaku-katsura, Kyoto 615-8510 (Japan)

    2017-03-01

    Poly(ethylene terephthalate) (PET)-based track-etched membranes (TMs) with pore sizes ranging from few nanometers to approximately 1 μm are used in various applications in the biological field, and their pore structures are determined by small-angle X-ray scattering (SAXS). These TMs with the nanometer-sized cylindrical pores aligned parallel to the film thickness direction are produced by chemical etching of the track in the PET films irradiated by heavy ions with the sodium hydroxide aqueous solution. It is well known that SAXS allows us to precisely and statistically estimate the pore size and the pore size distribution in the TMs by using the form factor of a cylinder with the extremely long pore length relative to the pore diameter. The results obtained were compared with those estimated with scanning electron microscopy and gas permeability measurements. The result showed that the gas permeability measurement is convenient to evaluate the pore size of TMs within a wide length scale, and the SEM observation is also suited to estimate the pore size, although SEM observation is usually limited above approximately 30 nm.

  16. 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.

  17. 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.

  18. 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.

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

    Science.gov (United States)

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

    2017-10-01

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

  20. 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.

  1. 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)

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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...

  8. 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.

  9. 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

  10. Charge and orbital ordered states studied by using x-ray anomalous scattering terms

    CERN Document Server

    Nakao, H

    2002-01-01

    Recently, the studies utilizing anomalous scattering term of atomic scattering factor near absorption edge, so called x-ray anomalous scattering and resonant x-ray scattering, have been rapidly developed. This technique has especially contributed to the determination of the charge-orbital ordered structure in strongly correlated electron system. In this paper, we present the typical examples - the charge ordering of V sup 4 sup + and V sup 5 sup + in NaV sub 2 O sub 5 and the antiferro-quadrupole ordering (orbital ordering) of Ge sup 3 sup + ions in CeB sub 6 (author)

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. 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)

  5. Anomalous X-ray scattering studies of short-, intermediate- and extended-range order in glasses

    International Nuclear Information System (INIS)

    Price, D.L.; Saboungi, M.L.; Armand, P.; Cox, D.E.

    1998-01-01

    The authors present the formalism of anomalous x-ray scattering as applied to partial structure analysis of disordered materials, and give an example of how the technique has been applied, together with that of neutron diffraction, to investigate short-, intermediate- and extended-range order in vitreous germania and rubidium germanate

  6. 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

  7. 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

  8. On the Casimir scaling violation in the cusp anomalous dimension at small angle

    Science.gov (United States)

    Grozin, Andrey; Henn, Johannes; Stahlhofen, Maximilian

    2017-10-01

    We compute the four-loop n f contribution proportional to the quartic Casimir of the QCD cusp anomalous dimension as an expansion for small cusp angle ϕ. This piece is gauge invariant, violates Casimir scaling, and first appears at four loops. It requires the evaluation of genuine non-planar four-loop Feynman integrals. We present results up to O({φ}^4) . One motivation for our calculation is to probe a recent conjecture on the all-order structure of the cusp anomalous dimension. As a byproduct we obtain the four-loop HQET wave function anomalous dimension for this color structure.

  9. 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.)

  10. 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

  11. 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}

  12. 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

  13. 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

  14. 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

  15. 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...

  16. 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

  17. 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.

  18. 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.

  19. Amorphous CuZr alloy investigated by anomalous X-ray scattering

    International Nuclear Information System (INIS)

    Bionducci, M.; Buffa, F.; Licheri, G.; Navarra, G.

    1993-01-01

    Cu Zr amorphous powder was prepared by a mechano-chemical reaction in order to state a comparison with corresponding samples prepared by different amorphization processes. The structure of the alloyed powder is studied by anomalous X-ray scattering method. Starting from a suitable set of total and differential structure factors and using a regularization algorithm, a set of partial structure factors is obtained, which compares well with those previously obtained for a sample prepared by rapid solidification of the melt. (authors) 1 fig., 1 tab., 14 refs

  20. 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...

  1. 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

  2. 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.

  3. 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.

  4. Introduction to the application and limits of anomalous X-ray diffraction in the determination of partial structure factors

    International Nuclear Information System (INIS)

    Bienenstock, A.

    1993-01-01

    The use of anomalous X-ray scattering to obtain the first differences and partial structure factors normally obtained with isotopic substitution neutron diffraction is described and compared with the neutron technique. Both the problems associated with the X-ray technique (low-Z problems, scattering factor problems, Compton scattering problems, fluorescence problems, storage ring stability problems) and the situations in which it is highly valuable are discussed. 12 refs

  5. Small-angle x-ray scattering studies of the porosity of coals and chars. Quarterly progress report, July 1-September 30, 1980

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, P.W.

    1980-09-01

    Considerable effort has been devoted to checking and verifying some of the preliminary data reported previously. The technique employed in the past for measuring the x-ray transmission of the samples has been modified to provide more accurate values of the transmission. These transmission measurements are important for quantitative interpretation of the scattering data both because they are needed to determine the amount of background scattering that must be subtracted from a measured scattering curve and also because the value of the transmission is required for calculating the specific surface from the scattering data. Previous determinations of the specific surface have been checked and modified when corrected transmission values made recalculation necessary. Evaluation of the specific surface from the scattering data also requires a measurement of the absolute scattered intensity, or scattering cross section. In other words, the fraction of the incident radiation which is scattered must be known. For this scattering investigation of coals, the absolute intensity for the scattering system was determined by measurement of the scattering from a colloidal silica suspension. The details of this technique are described by I.S. Patel and P.W. Schmidt, J. Appl. Cryst. 4, 50 to 55. (1971).

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

    Energy Technology Data Exchange (ETDEWEB)

    Volkov, V. V.; Klechkovskaya, V. V., E-mail: klechvv@ns.crys.ras.ru; Shtykova, E. V.; Dembo, K. A.; Arkharova, N. A.; Ivakin, G. I. [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation); Smyslov, R. Yu. [Russian Academy of Sciences, Institute of Macromolecular Compounds (Russian Federation)

    2009-03-15

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

  7. 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)

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Science.gov (United States)

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

    2018-03-01

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

  10. The roles of the RIIβ linker and N-terminal cyclic nucleotide-binding domain in determining the unique structures of the type IIβ protein kinase A: a small angle x-ray and neutron scattering study.

    Science.gov (United States)

    Blumenthal, Donald K; Copps, Jeffrey; Smith-Nguyen, Eric V; Zhang, Ping; Heller, William T; Taylor, Susan S

    2014-10-10

    Protein kinase A (PKA) is ubiquitously expressed and is responsible for regulating many important cellular functions in response to changes in intracellular cAMP concentrations. The PKA holoenzyme is a tetramer (R2:C2), with a regulatory subunit homodimer (R2) that binds and inhibits two catalytic (C) subunits; binding of cAMP to the regulatory subunit homodimer causes activation of the catalytic subunits. Four different R subunit isoforms exist in mammalian cells, and these confer different structural features, subcellular localization, and biochemical properties upon the PKA holoenzymes they form. The holoenzyme containing RIIβ is structurally unique in that the type IIβ holoenzyme is much more compact than the free RIIβ homodimer. We have used small angle x-ray scattering and small angle neutron scattering to study the solution structure and subunit organization of a holoenzyme containing an RIIβ C-terminal deletion mutant (RIIβ(1-280)), which is missing the C-terminal cAMP-binding domain to better understand the structural organization of the type IIβ holoenzyme and the RIIβ domains that contribute to stabilizing the holoenzyme conformation. Our results demonstrate that compaction of the type IIβ holoenzyme does not require the C-terminal cAMP-binding domain but rather involves large structural rearrangements within the linker and N-terminal cyclic nucleotide-binding domain of the RIIβ homodimer. The structural rearrangements are significantly greater than seen previously with RIIα and are likely to be important in mediating short range and long range interdomain and intersubunit interactions that uniquely regulate the activity of the type IIβ isoform of PKA. © 2014 by The American Society for Biochemistry and Molecular Biology, Inc.

  11. Probing the surface microstructure of layer-by-layer self-assembly chitosan/poly(L-glutamic acid) multilayers: A grazing-incidence small-angle X-ray scattering study

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Nie; Yang, Chunming, E-mail: yangchunming@sinap.ac.cn; Wang, Yuzhu; Zhao, Binyu; Bian, Fenggang; Li, Xiuhong; Wang, Jie, E-mail: wangjie@sinap.ac.cn

    2016-01-01

    This study characterized the surface structure of layer-by-layer self-assembly chitosan/poly(L-glutamic acid) multilayers through grazing-incidence small-angle X-ray scattering (GISAXS), X-ray reflectivity (XRR), and atomic force microscopy (AFM). A weakly long-period ordered structure along the in-plane direction was firstly observed in the polyelectrolyte multilayer by the GISAXS technique. This structure can be attributed to the specific domains on the film surface. In the domain, nanodroplets that were formed by polyelectrolyte molecules were orderly arranged along the free surface of the films. This ordered structure gradually disappeared with the increasing bilayer number because of the complex merging behavior of nanodroplets into large islands. Furthermore, resonant diffuse scattering became evident in the GISAXS patterns as the number of bilayers in the polyelectrolyte multilayer was increased. Notably, the lateral cutoff length of resonant diffuse scattering for these polyelectrolyte films was comparable with the long-period value of the ordered nanodroplets in the polyelectrolyte multilayer. Therefore, the nanodroplets could be considered as a basic transmission unit for structure propagation from the inner interface to the film surface. It suggests that the surface structure with length scale larger than the size of nanodroplets was partially complicated from the interface structure near the substrate, but surface structure smaller than the cutoff length was mainly depended on the conformation of nanodroplets. - Highlights: • The growth of ordered nanodroplets in PEMs was characterized by the GISAXS technique. • The basic transmission units for structure propagation within PEMs were nanodroplets. • High-performance of wave-guiding devices prepared by PEMs was predicted.

  12. Small-angle X-ray scattering analysis reveals the ATP-bound monomeric state of the ATPase domain from the homodimeric MutL endonuclease, a GHKL phosphotransferase superfamily protein.

    Science.gov (United States)

    Iino, Hitoshi; Hikima, Takaaki; Nishida, Yuya; Yamamoto, Masaki; Kuramitsu, Seiki; Fukui, Kenji

    2015-05-01

    DNA mismatch repair is an excision system that removes mismatched bases chiefly generated by replication errors. In this system, MutL endonucleases direct the excision reaction to the error-containing strand of the duplex by specifically incising the newly synthesized strand. Both bacterial homodimeric and eukaryotic heterodimeric MutL proteins belong to the GHKL ATPase/kinase superfamily that comprises the N-terminal ATPase and C-terminal dimerization regions. Generally, the GHKL proteins show large ATPase cycle-dependent conformational changes, including dimerization-coupled ATP binding of the N-terminal domain. Interestingly, the ATPase domain of human PMS2, a subunit of the MutL heterodimer, binds ATP without dimerization. The monomeric ATP-bound state of the domain has been thought to be characteristic of heterodimeric GHKL proteins. In this study, we characterized the ATP-bound state of the ATPase domain from the Aquifex aeolicus MutL endonuclease, which is a homodimeric GHKL protein unlike the eukaryotic MutL. Gel filtration, dynamic light scattering, and small-angle X-ray scattering analyses clearly showed that the domain binds ATP in a monomeric form despite its homodimeric nature. This indicates that the uncoupling of dimerization and ATP binding is a common feature among bacterial and eukaryotic MutL endonucleases, which we suggest is closely related to the molecular mechanisms underlying mismatch repair.

  13. Assessment of data-assisted prediction by inclusion of crosslinking/mass-spectrometry and small angle X-ray scattering data in the 12th Critical Assessment of protein Structure Prediction experiment.

    Science.gov (United States)

    Tamò, Giorgio E; Abriata, Luciano A; Fonti, Giulia; Dal Peraro, Matteo

    2018-03-01

    Integrative modeling approaches attempt to combine experiments and computation to derive structure-function relationships in complex molecular assemblies. Despite their importance for the advancement of life sciences, benchmarking of existing methodologies is rather poor. The 12 th round of the Critical Assessment of protein Structure Prediction (CASP) offered a unique niche to benchmark data and methods from two kinds of experiments often used in integrative modeling, namely residue-residue contacts obtained through crosslinking/mass-spectrometry (CLMS), and small-angle X-ray scattering (SAXS) experiments. Upon assessment of the models submitted by predictors for 3 targets assisted by CLMS data and 11 targets by SAXS data, we observed no significant improvement when compared to the best data-blind models, although most predictors did improve relative to their own data-blind predictions. Only for target Tx892 of the CLMS-assisted category and for target Ts947 of the SAXS-assisted category, there was a net, albeit mild, improvement relative to the best data-blind predictions. We discuss here possible reasons for the relatively poor success, which point rather to inconsistencies in the data sources rather than in the methods, to which a few groups were less sensitive. We conclude with suggestions that could improve the potential of data integration in future CASP rounds in terms of experimental data production, methods development, data management and prediction assessment. © 2017 Wiley Periodicals, Inc.

  14. Effects of blending poly(D,L-lactide) with poly(ethylene glycol) on the higher-order crystalline structures of poly(ethylene glycol) as revealed by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Tien, N D; Kimura, G; Yamashiro, Y; Fujiwara, H; Sasaki, S; Sakurai, S; Hoa, T P; Mochizuki, M

    2011-01-01

    Effects of blending poly(lactic acid) (PLA) with poly(ethylene glycol) (PEG) on higher-order crystalline structures of PEG were examined using small-angle X-ray scattering (SAXS). For this purpose, the fact that two polymers are both crystalline makes situtation much complicated. To simplify, non-crystalline PLA is suitable. Thus, we used poly(D,L-lactic acid) (DLPLA), which is random copolymer comprising D- and L-lactic acid moieties. Multiple scattering peaks arising from the regular crystalline lamellar structure were observed for the PEG homopolymer and the blends. Surprisingly, the structure is much more regular for the blend DLPLA/PEG at composition of 20/80 wt.% than for the PEG homopolymer. Also for this blend sample as well as for a PEG homopolymer, very peculiar SAXS profiles were observed just 1 deg. C below T m of PEG. This is found to be a particle scattering of plate-like objects, which has never been reported for polymer blends or crystalline polymers. Futhermore, it was found that there was strong hysteresis of the higher-order structure formation.

  15. Structural dynamics and ssDNA binding activity of the three N-terminal domains of the large subunit of Replication Protein A from small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Pretto, Dalyir I.; Tsutakawa, Susan; Brosey, Chris A.; Castillo, Amalchi; Chagot, Marie-Eve; Smith, Jarrod A.; Tainer, John A.; Chazin, Walter J.

    2010-03-11

    Replication Protein A (RPA) is the primary eukaryotic ssDNA binding protein utilized in diverse DNA transactions in the cell. RPA is a heterotrimeric protein with seven globular domains connected by flexible linkers, which enable substantial inter-domain motion that is essential to its function. Small angle X-ray scattering (SAXS) experiments on two multi-domain constructs from the N-terminus of the large subunit (RPA70) were used to examine the structural dynamics of these domains and their response to the binding of ssDNA. The SAXS data combined with molecular dynamics simulations reveal substantial interdomain flexibility for both RPA70AB (the tandem high affinity ssDNA binding domains A and B connected by a 10-residue linker) and RPA70NAB (RPA70AB extended by a 70-residue linker to the RPA70N protein interaction domain). Binding of ssDNA to RPA70NAB reduces the interdomain flexibility between the A and B domains, but has no effect on RPA70N. These studies provide the first direct measurements of changes in orientation of these three RPA domains upon binding ssDNA. The results support a model in which RPA70N remains structurally independent of RPA70AB in the DNA bound state and therefore freely available to serve as a protein recruitment module.

  16. Anomalous scattering and isomorphous replacement in X-ray diffuse scattering holography

    Czech Academy of Sciences Publication Activity Database

    Kopecký, Miloš; Kub, Jiří; Busetto, E.; Lausi, A.; Fábry, Jan; Šourek, Zbyněk

    2007-01-01

    Roč. 204, č. 8 (2007), s. 2572-2577 ISSN 1862-6300 R&D Projects: GA AV ČR IAA100100529; GA MŠk LA 287 Institutional research plan: CEZ:AV0Z10100523; CEZ:AV0Z10100520 Keywords : x-ray difuse scattering * x-ray holography Subject RIV: BM - Solid Matter Physics ; Magnetism

  17. Modelling of cation displacements in SrTiO.sub.3./sub. by means of multi-energy anomalous X-ray diffuse scattering

    Czech Academy of Sciences Publication Activity Database

    Kopecký, Miloš; Fábry, Jan; Kub, Jiří

    2016-01-01

    Roč. 49, Jun (2016), 1016-1020 ISSN 1600-5767 R&D Projects: GA ČR GA15-04121S Institutional support: RVO:68378271 Keywords : X-ray diffuse scattering * atomic displacements * anomalous X-ray scattering * SrTiO 3 Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.495, year: 2016

  18. 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.

    2014-01-01

    Broad-spectrum resistance to aminoglycoside antibiotics in clinically important Gram-positive staphylococcal and entero­coccal pathogens is primarily conferred by the bifunctional enzyme AAC(6′)-Ie-APH(2′′)-Ia. This enzyme possesses an N-terminal coenzyme A-dependent acetyltransferase domain [AAC(6′)-Ie] and a C-terminal GTP-dependent phosphotransferase domain [APH(2′′)-Ia], and together they produce resistance to almost all known aminoglycosides in clinical use. Despite considerable effort over the last two or more decades, structural details of AAC(6′)-Ie-APH(2′′)-Ia have remained elusive. In a recent breakthrough, the structure of the isolated C-terminal APH(2′′)-Ia enzyme was determined as the binary Mg2GDP complex. Here, the high-resolution structure of the N-terminal AAC(6′)-Ie enzyme is reported as a ternary kanamycin/coenzyme A abortive complex. The structure of the full-length bifunctional enzyme has subsequently been elucidated based upon small-angle X-ray scattering data using the two crystallographic models. The AAC(6′)-Ie enzyme is joined to APH(2′′)-Ia by a short, predominantly rigid linker at the N-terminal end of a long α-helix. This α-helix is in turn intrinsically associated with the N-terminus of APH(2′′)-Ia. This structural arrangement supports earlier observations that the presence of the intact α-helix is essential to the activity of both functionalities of the full-length AAC(6′)-Ie-APH(2′′)-Ia enzyme. PMID:25286858

  19. Structural effects of insulin-loading into HII mesophases monitored by electron paramagnetic resonance (EPR), small angle X-ray spectroscopy (SAXS), and attenuated total reflection Fourier transform spectroscopy (ATR-FTIR).

    Science.gov (United States)

    Mishraki, Tehila; Ottaviani, Maria Francesca; Shames, Alexander I; Aserin, Abraham; Garti, Nissim

    2011-06-30

    Insulin entrapment within a monoolein-based reverse hexagonal (H(II)) mesophase was investigated under temperature-dependent conditions at acidic (pH 3) and basic (pH 8) conditions. Studying the structure of the host H(II) system and the interactions of insulin under temperature-dependent conditions has great impact on the enhancement of its thermal stabilization and controlled release for the purposes of transdermal delivery. Small angle X-ray spectroscopy (SAXS) measurements show that pH variation and/or insulin entrapment preserve the hexagonal structure and do not influence the lattice parameter. Attenuated total reflection Fourier transform spectroscopy (ATR-FTIR) spectra indicate that, although insulin interacts with hydroxyl groups of GMO in the interface region, it is not affected by pH variations. Hence different microenvironments within the H(II) mesophase were monitored by a computer-aided electron paramagnetic resonance (EPR) analysis using 5-doxylstearic acid (5-DSA) as a pH-dependent probe. The microviscosity, micropolarity, order of systems, and distribution of the probes in different microenvironments were influenced by three factors: temperature, pH, and insulin solubilization. When the temperature is increased, microviscosity and order parameters decreased at both pH 3 and 8, presenting different decrease trends. It was found that, at pH 3, the protein perturbs the lipid structure while "pushing aside" the un-ionized 5-DSA probe to fit into the narrow water cylinders. At the interface region (pH 8), the probe was distributed in two differently structured environments that significantly modifies by increasing temperature. Insulin loading within the H(II) mesophase decreased the order and microviscosity of both the microenvironments and increased their micropolarity. Finally, the EPR analysis also provides information about the unfolding/denaturation of insulin within the channel at high temperatures.

  20. Suzaku X-Ray Study of an Anomalous Source XSS J12270-4859

    Science.gov (United States)

    Saitou, Kei; Tsujimoto, Masahiro; Ebisawa, Ken; Ishida, Manabu

    2009-08-01

    We report on the results of a Suzaku X-ray observation of XSSJ12270-4859, one of the hard X-ray sources in the INTEGRAL catalogue. This object has been classified as an intermediate polar (IP) by its optical spectra, and a putative X-ray period of ˜860s. With a 30ks exposure by Suzaku, we obtained a well-exposed spectrum in the 0.2--70keV band. We conclude against a previous IP classification based on a lack of Fe Kα emission features in the spectrum and a failure to confirm the previously reported X-ray period. Instead, the X-ray light curve is filled with exotic phenomena, including repetitive flares lasting for ˜100s, occasional dips with no apparent periodicities, spectral hardening after some flares, and bimodal changes pivoting between quiet and active phases. The rapid flux changes, the dips, and the power-law spectrum point toward an interpretation that this is a low-mass X-ray binary. Some temporal characteristics are similar to those in the Rapid Burster and GRO J1744-28, making XSS J12270-4859 a very rare object.

  1. ON THE EVOLUTION OF ANOMALOUS X-RAY PULSARS AND SOFT GAMMA-RAY REPEATERS WITH FALL BACK DISKS

    International Nuclear Information System (INIS)

    Ertan, Ue.; Alpar, M. A.; Eksi, K. Y.; Erkut, M. H.

    2009-01-01

    We show that the period clustering of anomalous X-ray pulsars (AXPs) and soft gamma-ray repeaters (SGRs), their X-ray luminosities, ages, and statistics can be explained with fall back disks with large initial specific angular momentum. The disk evolution models are developed by comparison to self-similar analytical models. The initial disk mass and angular momentum set the viscous timescale. An efficient torque, with (1 - ω 2 * ) dependence on the fastness parameter ω * , leads to period clustering in the observed AXP-SGR period range under a wide range of initial conditions. The timescale t 0 for the early evolution of the fall back disk, and the final stages of fall back disk evolution, when the disk becomes passive, are the crucial determinants of the evolution. The disk becomes passive at temperatures around 100 K, which provides a natural cutoff for the X-ray luminosity and defines the end of evolution in the observable AXP and SGR phase. This low value for the minimum temperature for active disk turbulence indicates that the fall back disks are active up to a large radius, ∼>10 12 cm. We find that transient AXPs and SGRs are likely to be older than their persistent cousins. A fall back disk with mass transfer rates corresponding to the low quiescent X-ray luminosities of the transient sources in early evolutionary phases would have a relatively lower initial mass, such that the mass-flow rate in the disk is not sufficient for the inner disk to penetrate into the light cylinder of the young neutron star, making mass accretion onto the neutron star impossible. The transient AXP phase therefore must start later. The model results imply that the transient AXP/SGRs, although older, are likely to be similar in number to persistent sources. This is because the X-ray luminosities of AXPs and SGRs are found to decrease faster at the end of their evolution, and the X-ray luminosities of transient AXP and SGRs in quiescence lie in the luminosity range of X-ray

  2. Observation of parametric X-ray radiation in an anomalous diffraction region

    Energy Technology Data Exchange (ETDEWEB)

    Alexeyev, V.I., E-mail: vial@x4u.lebedev.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation); Eliseyev, A.N., E-mail: elisseev@pluton.lpi.troitsk.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation); Irribarra, E., E-mail: esteban.irribarra@epn.edu.ec [Escuela Politécnica Nacional, Ladrón de Guevara E11-253, Quito (Ecuador); Kishin, I.A., E-mail: ivan.kishin@mail.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation); Kubankin, A.S., E-mail: kubankin@bsu.edu.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation); Nazhmudinov, R.M., E-mail: fizeg@bk.ru [P.N. Lebedev Physical Institute RAS, 53 Leninskiy prospect, Moscow (Russian Federation); Belgorod National Research University, 85 Pobedy st., Belgorod (Russian Federation)

    2016-08-19

    A new possibility to expand the energy region of diffraction processes based on the interaction of relativistic charged particles with crystalline structures is presented. Diffracted photons related to parametric X-ray radiation produced by relativistic electrons are detected below the low energy threshold for the X-ray diffraction mechanism in crystalline structures for the first time. The measurements were performed during the interaction of 7 MeV electrons with a textured polycrystalline tungsten foil and a highly oriented pyrolytic graphite crystal. The experiment results are in good agreement with a developed model based on the PXR kinematical theory. The developed experimental approach can be applied to separate the contributions of real and virtual photons to the total diffracted radiation generated during the interaction of relativistic charged particles with crystalline targets. - Highlights: • Parametric X-ray radiation below the low energy threshold for diffraction of free X-rays. • Experimental separation of the contributions from different radiation mechanisms. • PXR from relativistic electrons in mosaic crystals and textured polycrystlas.

  3. Effect of temperature on self-assembly of bovine beta-casein above and below isoelectric pH. Structural analysis by cryogenic-transmission electron microscopy and small-angle X-ray scattering.

    Science.gov (United States)

    Moitzi, Christian; Portnaya, Irina; Glatter, Otto; Ramon, Ory; Danino, Dganit

    2008-04-01

    beta-Casein is one of the main proteins in milk, recently classified as an intrinsically unstructured protein. At neutral pH, it is composed of a highly polar N-terminus domain and a hydrophobic C-terminus tail. This amphiphilic block-copolymer-like structure leads to self-organization of the protein monomers into defined micelles. Recently, it has been shown that at room temperature, beta-casein also self-organizes into micelles in an acidic environment, but the effect of temperature on the micelles' formation and properties at the low pH regime were not explored. In the present study, we used two complementary techniques, cryogenic-transmission electron microscopy (cryo-TEM) and small-angle X-ray scattering (SAXS), to characterize at high-resolution the micelles' shape, dimensions, and aggregation numbers and to determine how these properties are affected by temperature between 1 and 40 degrees C. Two different regimes were studied: highly acidic pH where the protein is cationic, and neutral pH, where it is anionic. We found that flat disk-like micelles with low aggregation numbers formed at low temperature in the two pH regimes. Close to neutral pH increase in temperature involves a transition in the micelles' shape and dimensions from flat disks to bulky, almost spheroidal micelles, coupled with a sharp increase in the micelles' aggregation number. In contrast, no effects on the micelles' morphology or aggregation number were detected in the acidic environment within the entire temperature range studied. The self-organization into disk micelles and the lack of effect of temperature in the acidic environment are linked to the unstructured character of the protein and to the charge distribution map. The latter indicates that below the isoelectric pH (pI), beta-casein loses the distinct separation of hydrophobic and hydrophilic domains, thereby suggesting that it may no longer be considered as a classical head-tail block-copolymer amphiphile as in neutral pH.

  4. Simulations de la croissance de sphérolites de polymère et de spectres de diffusion centrale des rayons X Simulations of Polymer Spherulites Growth and Small-Angle X-Ray Scattering Spectra

    Directory of Open Access Journals (Sweden)

    Jarrin J.

    2006-11-01

    épend fortement du désordre d'empilement des lamelles; différentes situations sont envisagées. Mechanical properties of semi-crystalline polymers are closely related to material microstructure. The latter is usually made of spherulites, within which are radially disposed crystalline lamellae, separated by amorphous regions. A better description of this structure is necessary to predict more accuretely mechanical properties. Various physical and chemical characterization techniques can be used, such as scanning electronic microscopy or small-angle X-ray scattering (SAXS. Microscopy will give a spherulite picture, whereas diffusion technique will be more specific about the average organization of crystalline lamellae from the interference peak observed on spectrum. In order to relate informations given by these two techniques, a modelling approach was adopted, i. e. writing of a spherulite growth simulation software, the base unit being the lamellae, and a SAXS spectra computing program, based on given structural models. The SAXS computing program has been adapted from existing IFP (Institut Français du Pétrole softwares, allowing computing of wide-angle X-ray scattering spectra. Several spherulite growth parameters have been adjusted, so as to obtain a good agreement with scanning electronic micrographs. Also, the simultaneous growth of several spherulitic entities has been simulated, in both instantaneous and homogeneous nucleation cases. The boundaries between spherulites at the end of the growth are very similar to those observed in optical microscopy. The relative orientations and positions of nuclei are of great importance for impingement, interlocking and organization of spherulites, and therefore for mechanical properties. The diffusion spectrum of simulated spherulitic structures did not present an interference peak. Some spherulite branches are in fact composed of a set of crystalline lamellae, which explains the presence of the interference peak. Intensity of the

  5. Small-angle scattering on soft materials

    International Nuclear Information System (INIS)

    Mortensen, K.

    1994-01-01

    Small angle x-ray and neutron scattering provides tools for investigation of structures on the length scale 10 to 1000 A. This is the length scale which is relevant for many topics within soft materials, like biological macromolecules, polymers, colloids, etc. The very large difference between the scattering amplitude of neutrons by regular hydrogen and deuterium makes neutron scattering a very important technique within soft condensed matter. The basic theory for small angle scattering is reviewed. Experimental results obtained by small angle scattering are shown, with emphasis on soft materials. (author). 33 refs, 6 figs, 1 tab

  6. Characterization of materials of industrial importance using small-angle scattering techniques

    International Nuclear Information System (INIS)

    Thiyagarajan, P.

    2003-01-01

    Small angle scattering (SAS) techniques using either X-rays or neutrons are versatile tools for deriving information on the size, morphology and dispersion of colloidal systems in complex materials of industrial importance. The processes such as self-assembly, aggregation, crystallization and phase separation can be studied using SAS techniques at relevant conditions. The difference in the interaction of X-rays and neutrons with matter enables complementary contrast variation studies using SANS and anomalous SAXS (in the presence of metals) on multi-component materials with hierarchical structures. In this paper we present results from small angle scattering studies on a number of systems of industrial importance including, temperature/pressure/shear dependent phase behaviour of pluronics in aqueous media, solution structures of aggregates/polymers of metal-extractant complexes, third phase formation of metal-extractant complexes in organic phase, encapsulation of lanthanides and actinides in porous silica and phase separation and nanocrystallization in bulk metallic glasses. (orig.)

  7. A WHITE DWARF MERGER AS PROGENITOR OF THE ANOMALOUS X-RAY PULSAR 4U 0142+61?

    International Nuclear Information System (INIS)

    Rueda, J. A.; Boshkayev, K.; Izzo, L.; Ruffini, R.; Lorén-Aguilar, P.; Külebi, B.; Aznar-Siguán, G.; García-Berro, E.

    2013-01-01

    It has been recently proposed that massive, fast-rotating, highly magnetized white dwarfs could describe the observational properties of some of soft gamma-ray repeaters and anomalous X-ray pulsars (AXPs). Moreover, it has also been shown that high-field magnetic white dwarfs can be the outcome of white dwarf binary mergers. The products of these mergers consist of a hot central white dwarf surrounded by a rapidly rotating disk. Here we show that the merger of a double degenerate system can explain the characteristics of the peculiar AXP 4U 0142+61. This scenario accounts for the observed infrared excess. We also show that the observed properties of 4U 0142+6 are consistent with an approximately 1.2 M ☉ white dwarf, remnant of the coalescence of an original system made of two white dwarfs of masses 0.6 M ☉ and 1.0 M ☉ . Finally, we infer a post-merging age τ WD ≈ 64 kyr and a magnetic field B ≈ 2 × 10 8 G. Evidence for such a magnetic field may come from the possible detection of the electron cyclotron absorption feature observed between the B and V bands at ≈10 15 Hz in the spectrum of 4U 0142+61

  8. The Chemically-Specific Structure of an Amorphous Molybdenum Germanium Alloy by Anomalous X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Ishii, H. A.

    2002-06-11

    Since its inception in the late 1970s, anomalous x-ray scattering (AXS) has been employed for chemically-specific structure determination in a wide variety of noncrystalline materials. These studies have successfully produced differential distribution functions (DDFs) which provide information about the compositionally-averaged environment of a specific atomic species in the sample. Despite the wide success in obtaining DDFs, there are very few examples of successful extraction of the fully-chemically-specific partial pair distribution functions (PPDFs), the most detailed description of an amorphous sample possible by x-ray scattering. Extracting the PPDFs is notoriously difficult since the matrix equation involved is ill-conditioned and thus extremely sensitive to errors present in the experimental quantities that enter the equation. Instead of addressing this sensitivity by modifying the data through mathematical methods, sources of error have been removed experimentally: A focusing analyzer crystal was combined with a position-sensitive linear detector to experimentally eliminate unwanted inelastic scattering intensity over most of the reciprocal space range probed. This instrumentation has been used in data collection for the extraction of PPDFs from amorphous (a)-MoGe{sub 3}. This composition arises as a phase separation endpoint in the Ge-rich region of the vapor-deposited Mo-Ge amorphous alloy system but is not present at equilibrium. Since the first Ge-rich compound in the Mo-Ge equilibrium system is MoGe{sub 2}, previous workers have speculated that perhaps a unique MoGe{sub 3} compound exists in the amorphous system. Rather than indicating a distinct MoGe{sub 3} compound with definitive local structure, however, the coordination results are more consistent with a densely-packed alloy having a wide range of solid solubility. Significant improvement in the quality and reliability of experimental PPDFs from a-MoGe{sub 3} by AXS has been achieved solely

  9. Determination of transition metal ion distribution in cubic spinel Co1.5Fe1.5O4 using anomalous x-ray diffraction

    Directory of Open Access Journals (Sweden)

    M. N. Singh

    2015-08-01

    Full Text Available We report anomalous x-ray diffraction studies on Co ferrite with composition Co1.5Fe1.5O4 to obtain the distribution of transition metal ions in tetrahedral and octahedral sites. We synthesize spinel oxide (Co1.5Fe1.5O4 through co-precipitation and subsequent annealing route. The imaginary part (absorption of the energy dependent anomalous form factor is measured and the real part is calculated theoretically through Kramers–Krönig transformation to analyze anomalous x-ray diffraction peak intensities. Fe and Co K-edge x-ray absorption near edge structure (XANES spectra are used to estimate charge states of transition metals. Our analysis, within experimental errors, suggests 44% of the tetrahedral sites contain Co in +2 oxidation state and the rest 56% sites contain Fe in +2 and +3 oxidation states. Similarly, 47% of the octahedral sites contain Fe in +3 oxidation states, whereas, the rest of the sites contain Co in +2 and +3 oxidation states. While a distinct pre-edge feature in the Fe K-edge XANES is observed, Co pre-edge remains featureless. Implications of these results to magnetism are briefly discussed.

  10. Introduction to small-angle scattering

    International Nuclear Information System (INIS)

    Gilbert, E.

    2003-01-01

    Full text: Small angle neutron and X-ray scattering (SANS and SAXS) are ideal tools for studying the structure of materials in the size range between 10 and 1000 Angstrom. While imaging methods such as transmission electron microscopy (TEM) also have this capability, they provide images in real space, for instance individual grains in a nanocrystalline material. SANS and SAXS, on the other hand, provide (generally) a non-destructive method yielding structural information averaged over all grains with high statistical accuracy due to averaging over the whole sample volume. The use of neutrons and X-rays is also implicitly complementary due to their sensitivity to either nuclear or electron density respectively. This provides several further advantages over real-space techniques such as isotopic sensitivity and contrast variation. In this talk, I will provide an introduction to the technique with a minimum number of equations, emphasising what structural information may be obtained from small-angle scattering

  11. Small-Angle Scattering on Magnetoferritin Nanoparticles

    Science.gov (United States)

    Balejčíková Petrenko, L., VI; Avdeev, MV; Garamus, VM; Almásy, L.; Kopčanský, P.

    2017-05-01

    Magnetoferritin is a synthetically prepared magnetic bio-complex, consisting of apoferritin shell and iron-based nanoparticles. Superparamagnetic behaviour, nanoscale size (about 12 nm) and biological origin allow to use magnetoferritin in various applications. In this report, we present a general overview about basic physicochemical properties of magnetoferritin, as determined by small-angle X-ray and neutron scattering experiments and some interesting references on their potential bio-applications.

  12. Ultra small angle scattering versus diffraction

    Science.gov (United States)

    Ebrahimi, O.; Treimer, W.; Strobl, M.; Feye-Treimer, U.; Beul, N.; Jericha, E.; Seidel, S. O.

    2010-11-01

    In the case of ultra small angle (neutron or x-ray) scattering (USANS, USAXS) it may happen that structures under investigations are not fully coherently illuminated by the incident wave. Despite this fact interference effects are observed similar to SAS data. In this case the measured scattering patterns must be different interpreted. We propose a procedure to calculate and adapt such scattering patterns to experimental data.

  13. Ultra small angle scattering versus diffraction

    International Nuclear Information System (INIS)

    Ebrahimi, O; Treimer, W; Strobl, M; Feye-Treimer, U; Beul, N; Jericha, E; Seidel, S O

    2010-01-01

    In the case of ultra small angle (neutron or x-ray) scattering (USANS, USAXS) it may happen that structures under investigations are not fully coherently illuminated by the incident wave. Despite this fact interference effects are observed similar to SAS data. In this case the measured scattering patterns must be different interpreted. We propose a procedure to calculate and adapt such scattering patterns to experimental data.

  14. Anomalous lattice behavior of vanadium pentaoxide (V2O5): X-ray diffraction, inelastic neutron scattering and ab initio lattice dynamics.

    Science.gov (United States)

    Singh, Baltej; Gupta, Mayanak Kumar; Mishra, Sanjay Kumar; Mittal, Ranjan; Sastry, P U; Rols, Stephane; Chaplot, Samrath Lal

    2017-07-21

    We present structural and dynamical studies of layered vanadium pentaoxide (V 2 O 5 ). The temperature dependent X-ray diffraction measurements reveal highly anisotropic and anomalous thermal expansion from 12 K to 853 K. The results do not show any evidence of structural phase transition or decomposition of α-V 2 O 5 , contrary to the previous transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS) experiments. The inelastic neutron scattering measurements performed up to 673 K corroborate the result of our X-ray diffraction measurements. The analysis of the experimental data is carried out using ab initio lattice dynamics calculations. The important role of van der Waals dispersion and Hubbard interactions in the structure and dynamics is revealed through ab initio calculations. The calculated anisotropic thermal expansion behavior agrees well with temperature dependent X-ray diffraction. The mechanism of anisotropic thermal expansion and anisotropic linear compressibility is discussed in terms of calculated anisotropy in the Grüneisen parameters and elastic coefficients. The calculated Gibbs free energy in various phases of V 2 O 5 is used to understand the high pressure and temperature phase diagram of the compound.

  15. Small angle neutron scattering

    International Nuclear Information System (INIS)

    Gupta, Sanjay

    1982-01-01

    The technique of small angle neutron scattering was first used in Germany less than two decades ago. Since then it has developed very rapidly, and today it is regarded as one of the most powerful techniques in materials, chemical and biological research. During the last decade the combination of high flux reactors and sophisticated instrumentation has revolutionized the technique. This paper endeavours to present a brief but comprehensive review of small angle scattering of neutrons and its applications in solid state research. The domain in which small angle neutron scattering is particularly useful is delineated and some of the methods used in the analysis of data are discussed with special emphasis on recent developments. Typical small angle neutron scattering cameras are described. Finally some experimental results on heterogeneities in metallic systems (both static and dynamic studies), radiation damage in materials, superconductivity, magnetic materials and the technologically very important area of non-destructive testing are reviewed in order to illustrate the wide range of applicability of this technique to problems in solid state research. (author)

  16. Structural analysis of Fe-Mn-O nanoparticles in glass ceramics by small angle scattering

    Science.gov (United States)

    Raghuwanshi, Vikram Singh; Harizanova, Ruzha; Tatchev, Dragomir; Hoell, Armin; Rüssel, Christian

    2015-02-01

    Magnetic nanocrystals containing Fe and Mn were obtained by annealing of silicate glasses with the composition 13.6Na2O-62.9SiO2-8.5MnO-15.0Fe2O3-x (mol%) at 580 °C for different periods of time. Here, we present Small Angle Neutron Scattering using Polarized neutrons (SANSPOL) and Anomalous Small Angle X-ray Scattering (ASAXS) investigation on these glass ceramic samples. Analysis of scattering data from both methods reveals the formation of spherical core-shell type of nanoparticles with mean sizes between 10 nm and 100 nm. ASAXS investigation shows the particles have higher concentration of iron atoms and the shell like region surrounding the particles is enriched in SiO2. SANSPOL investigation shows the particles are found to be magnetic and are surrounded by a non-magnetic shell-like region.

  17. Time-Resolved Small-Angle X-Ray Scattering

    NARCIS (Netherlands)

    ten Elshof, Johan E.; Besselink, R.; Stawski, Tomasz; Castricum, H.L.; Levy, D.; Zayat, M.

    2015-01-01

    This chapter focuses on time-resolved studies of nanostructure development in sol-gel liquids, that is, diluted sols, wet gels, and drying thin fffilms. The most commonly investigated classes of sol-gel materials are silica, organically modified silica, template-directed mesostructured silica,

  18. Synchrotron X-ray diffraction investigation of the anomalous behavior of ice during freezing of aqueous systems.

    Science.gov (United States)

    Varshney, Dushyant B; Elliott, James A; Gatlin, Larry A; Kumar, Satyendra; Suryanarayanan, Raj; Shalaev, Evgenyi Y

    2009-05-07

    Simple aqueous systems, i.e., phosphate-glycine buffers and pure water, were studied at subambient temperatures by X-ray difractometry using a high-intensity synchrotron radiation source at the Advanced Photon Source of Argonne National Laboratory. Complex X-ray diffraction (XRD) patterns, with two or more poorly resolved peaks in place of each of the four diagnostic peaks of hexagonal ice, 100, 002, 101, and 102, referred as "splitting", were observed in the majority of cases. The splitting of up to 0.05 A (d-spacing) was detected for 100, 002, and 101 peaks, whereas 102 peak was less affected. Deformation of the lattice of hexagonal ice, probably due to local stress created on the ice/ice or ice/container interface during water-to-ice transformation, is proposed as a possible mechanism for the observed splitting of XRD peaks. Using molecular modeling, it was estimated that the observed shifts in the peak positions are equivalent to applying a hydrostatic pressure of 2-3 kbars. The splitting can be used to quantify stresses during freezing, which could improve our understanding of the role of water-to-ice transformation on the destabilization of proteins and other biological systems.

  19. X-ray diffraction

    International Nuclear Information System (INIS)

    Vries, J.L. de.

    1976-01-01

    The seventh edition of Philips' Review of literature on X-ray diffraction begins with a list of conference proceedings on the subject, organised by the Philips' organisation at regular intervals in various European countries. This is followed by a list of bulletins. The bibliography is divided according to the equipment (cameras, diffractometers, monochromators) and its applications. The applications are subdivided into sections for high/low temperature and pressure, effects due to the equipment, small angle scattering and a part for stress, texture and phase analyses of metals and quantitative analysis of minerals

  20. X-ray Excitation Triggers Ytterbium Anomalous Emission in CaF 2 :Yb but Not in SrF 2 :Yb

    Energy Technology Data Exchange (ETDEWEB)

    Hughes-Currie, Rosa B.; Ivanovskikh, Konstantin V.; Wells, Jon-Paul R.; Reid, Michael F.; Gordon, Robert A.; Seijo, Luis; Barandiarán, Zoila

    2017-02-27

    Materials that luminesce after excitation with ionizing radiation are extensively applied in physics, medicine, security, and industry. Lanthanide dopants are known to trigger crystal scintillation through their fast d–f emissions; the same is true for other important applications as lasers or phosphors for lighting. However, this ability can be seriously compromised by unwanted anomalous emissions often found with the most common lanthanide activators. We report high-resolution X-ray-excited optical (IR to UV) luminescence spectra of CaF2:Yb and SrF2:Yb samples excited at 8949 eV and 80 K. Ionizing radiation excites the known anomalous emission of ytterbium in the CaF2 host but not in the SrF2 host. Wave function-based ab initio calculations of host-to-dopant electron transfer and Yb2+/Yb3+ intervalence charge transfer explain the difference. The model also explains the lack of anomalous emission in Yb-doped SrF2 excited by VUV radiation.

  1. An introduction to small-angle neutron scattering

    International Nuclear Information System (INIS)

    Windsor, C.G.

    1988-01-01

    Neutron and X-ray small-angle scattering provide, along with electron microscopy and diffraction, the principal techniques for the microscopic characterization of materials. Neutron, X-ray and electron beams each have quite different properties. In fact, each has unique advantages. The penetration of neutrons through most materials is responsible for many applications. The ever-increasing intensity of available X-ray beams is opening new fields. The advantage of electron beams is their ability to work in both real and reciprocal space. The problems of transforming the results of an experiment in reciprocal space to give an interpretation in real space are central to small-angle scattering, and are discussed. Several examples will be given of the successful use of small-angle neutron scattering applied to problems where other techniques have failed to make a decisive contribution. (orig.)

  2. Long-range structure of Cu(InxGa1-x)3Se5: A complementary neutron and anomalous x-ray diffraction study

    Science.gov (United States)

    Lehmann, S.; Marrón, D. fürtes; León, M.; Feyerherm, R.; Dudzik, E.; Friedrich, E. J.; Tovar, M.; Tomm, Y.; Wolf, C.; Schorr, S.; Schedel-Niedrig, Th.; Lux-Steiner, M. Ch.; Merino, J. M.

    2011-01-01

    Distinguishing the scattering contributions of isoelectronic atomic species by means of conventional x-ray- and/or electron diffraction techniques is a difficult task. Such a problem occurs when determining the crystal structure of compounds containing different types of atoms with equal number of electrons. We propose a new structural model of Cu(InxGa1-x)3Se5 which is valid for the entire compositional range of the CuIn3Se5-CuGa3Se5 solid solution. Our model is based on neutron and anomalous x-ray diffraction experiments. These complementary techniques allow the separation of scattering contributions of the isoelectronic species Cu+ and Ga3+, contributing nearly identically in monoenergetic x-ray diffraction experiments. We have found that CuIII3Se5 (III=In,Ga) in its room temperature near-equilibrium modification exhibits a modified stannite structure (space group I4¯2m). Different occupation factors of the species involved, Cu+, In3+, Ga3+, and vacancies have been found at three different cationic positions of the structure (Wyckoff sites 2a, 2b, and 4d) depending on the composition of the compound. Significantly, Cu+ does not occupy the 2b site for the In-free compound, but does for the In-containing case. Structural parameters, including lattice constants, tetragonal distortions, and occupation factors are given for samples covering the entire range of the CuIn3Se5-CuGa3Se5 solid solution. At the light of the result, the denotation of Cu-poor 1:3:5 compounds as chalcopyrite-related materials is only valid in reference to their composition.

  3. Crystal structure determination of solar cell materials: Cu2ZnSnS4 thin films using X-ray anomalous dispersion

    International Nuclear Information System (INIS)

    Nozaki, Hiroshi; Fukano, Tatsuo; Ohta, Shingo; Seno, Yoshiki; Katagiri, Hironori; Jimbo, Kazuo

    2012-01-01

    Highlights: ► Cu 2 ZnSnS 4 thin films as a solar cell material were synthesized. ► The wavelength dependences of the diffraction intensity were measured. ► The crystal structures were clearly identified as kesterite structure for all samples. ► Crystal structure analysis revealed that the atomic compositions were Cu/(Zn + Sn) = 0.97 and Zn/Sn = 1.42 for the sample synthesized using stoichiometric amount of starting materials. - Abstract: The crystal structure of Cu 2 ZnSnS 4 (CZTS) thin films fabricated by vapor-phase sulfurization was determined using X-ray anomalous dispersion. High statistic synchrotron radiation X-ray diffraction data were collected from very small amounts of powder. By analyzing the wavelength dependencies of the diffraction peak intensities, the crystal structure was clearly identified as kesterite. Rietveld analysis revealed that the atomic composition deviated from stoichiometric composition, and the compositions were Cu/(Zn + Sn) = 0.97, and Zn/Sn = 1.42.

  4. Neutron small angle scattering

    International Nuclear Information System (INIS)

    Ibel, K.

    1975-01-01

    The neutron small-angle scattering system at the High-Flux Reactor in Grenoble consists of three major parts: the supply of cold neutrons via bent neutron guides; the small angle camera D11; and the data handling facilities. The camera D11 has an overall length of 80 m. The effective length of the camera is variable. The length of the collimator before the fixed sample position can be reduced by movable neutron guides; the secondary flight path of 40 m full length contains detector sites in various positions. Thus, a large domain of momentum transfers can be exploited. Scattering angles between 5.10 -4 and 0.5 rad and neutron wavelengths from 0.2 to 2.0 nm are available with the same instrument and the same relative resolution. A large-area position-sensitive detector is used which allows simultaneous recording of intensities scattered into different angles; it is a multiwire proportional chamber. 3808 elements of 1 cm 2 are arranged in a two-dimensional matrix. Future development comprises an increase of the limit in the count rate due to the electronic interface between the detector and on-line computer, actually at 5.10 4 per sec. by one order of magnitude

  5. Small angle neutron scattering

    International Nuclear Information System (INIS)

    Dasannacharya, B.A.; Goyal, P.S.

    1997-01-01

    Small angle neutron scattering (SANS) is one of the most popular neutron scattering technique both for the basic research and as a tool in the hands of applied scientist. SANS is used for studying the structure of a material on a length scale of 10 - 1000 A. SANS is a diffraction experiment that involves scattering of a monocromatic beam of neutrons in order to obtain structural information about macromolecules and heterogeneities. This paper will discuss the design of SANS spectrometers with a special emphasis on the instruments which are better suited for medium flux reactors. The design of several different types of SANS spectrometers will be given. The optimization procedures and appropriate modifications to suit the budget and the space will be discussed. As an example, the design of a SANS spectrometer at CIRUS reactor Trombay will be given. (author)

  6. Strain, size and composition of InAs quantum sticks, embedded in InP, determined via X-ray anomalous diffraction and diffraction anomalous fine structure in grazing incidence

    International Nuclear Information System (INIS)

    Letoublon, A.; Favre-Nicolin, V.; Renevier, H.; Proietti, M.G.; Monat, C.; Gendry, M.; Marty, O.; Priester, C.

    2005-01-01

    We report on the study of strain, size and composition of small-size encapsulated semiconductor nanostructures. We show that the partial structure factor of As atoms in InAs stick-like nanostructures (quantum sticks), embedded in InP, can be directly extracted from grazing incidence anomalous X-ray diffraction maps at the As K-edge. We have recovered the average height and strain of the islands and determined their composition. The average height of the quantum sticks (QSs), as deduced from the width of the structure factor profile is 2.54 nm. The InAs out of plane deformation, relative to InP, is equal to 6.1%. Fixed-Q anomalous diffraction spectra, measured at the As K-edge, in grazing incidence provide clear evidence of pure InAs QSs. This is confirmed by the analysis of the diffraction anomalous fine structure (DAFS) that also gives a direct way to recover the strain accomodation inside the quantum sticks. Finite difference method calculations reproduce well the diffraction data. Chemical mixing at interfaces is at most 1 ML. This paper shows that ultimate application of anomalous diffraction and DAFS together with reciprocal space maps is a powerful method to sudy the structural properties of nanostructures

  7. X-ray diagnostic in gas discharge

    International Nuclear Information System (INIS)

    Chen Suhe; Wang Dalun; Cui Gaoxian; Wang Mei; Fu Yibei; Zhang Xinwei; Zhang Wushou

    1995-01-01

    X rays were observed when the anomalous phenomenon in the metal loaded with deuterium studied by the gas-discharge method. Therefore the X-ray energy spectra were measured by the absorption method, the specific X-ray approach and the NaI scintillation counter, while X-ray intensity was estimated by using 7 Li thermoluminescent foils. The X-ray average energy measured by the absorption method is 27.6 +- 2.1 keV, which is fitted within the error extent to 26.0 +-2.4 keV monoenergetic X rays measured by the NaI scintillation counter

  8. Small angle neutron scattering

    Directory of Open Access Journals (Sweden)

    Cousin Fabrice

    2015-01-01

    Full Text Available Small Angle Neutron Scattering (SANS is a technique that enables to probe the 3-D structure of materials on a typical size range lying from ∼ 1 nm up to ∼ a few 100 nm, the obtained information being statistically averaged on a sample whose volume is ∼ 1 cm3. This very rich technique enables to make a full structural characterization of a given object of nanometric dimensions (radius of gyration, shape, volume or mass, fractal dimension, specific area… through the determination of the form factor as well as the determination of the way objects are organized within in a continuous media, and therefore to describe interactions between them, through the determination of the structure factor. The specific properties of neutrons (possibility of tuning the scattering intensity by using the isotopic substitution, sensitivity to magnetism, negligible absorption, low energy of the incident neutrons make it particularly interesting in the fields of soft matter, biophysics, magnetic materials and metallurgy. In particular, the contrast variation methods allow to extract some informations that cannot be obtained by any other experimental techniques. This course is divided in two parts. The first one is devoted to the description of the principle of SANS: basics (formalism, coherent scattering/incoherent scattering, notion of elementary scatterer, form factor analysis (I(q→0, Guinier regime, intermediate regime, Porod regime, polydisperse system, structure factor analysis (2nd Virial coefficient, integral equations, characterization of aggregates, and contrast variation methods (how to create contrast in an homogeneous system, matching in ternary systems, extrapolation to zero concentration, Zero Averaged Contrast. It is illustrated by some representative examples. The second one describes the experimental aspects of SANS to guide user in its future experiments: description of SANS spectrometer, resolution of the spectrometer, optimization of

  9. Studies in small angle scattering techniques

    International Nuclear Information System (INIS)

    Moellenbach, K.

    1980-03-01

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

  10. Complementary information on CdSe/ZnSe quantum dot local structure from extended X-ray absorption fine structure and diffraction anomalous fine structure measurements

    International Nuclear Information System (INIS)

    Piskorska-Hommel, E.; Holý, V.; Caha, O.; Wolska, A.; Gust, A.; Kruse, C.; Kröncke, H.; Falta, J.; Hommel, D.

    2012-01-01

    The extended X-ray absorption fine structure (EXAFS) and diffraction anomalous fine structure (DAFS) have been applied to investigate a local structure for the CdSe/ZnSe quantum dots grown by molecular beam epitaxy (MBE) and migration-enhanced epitaxy (MEE). The aim was to study the intermixing of Cd and Zn atoms, chemical compositions and strain induced by cap-layer. The EXAFS at the Cd K-edge and DAFS at the Se K-edge proved the intermixing of Cd and Zn atoms. The distances Cd–Se (2.61 Å) found from EXAFS and DAFS analysis for h 1 region is closer to that in bulk CdSe (2.62 Å). The DAFS analysis revealed the differences in the local structure in two investigated regions (i.e. different iso-strain volumes) on the quantum dots. It was found that the investigated areas differ in the Cd concentration. To explain the experimental results the theoretical calculation based on a full valence-force field (VFF) model was performed. The theoretical VFF model fully explains the experimental data.

  11. Skull x-ray

    Science.gov (United States)

    X-ray - head; X-ray - skull; Skull radiography; Head x-ray ... There is low radiation exposure. X-rays are monitored and regulated to provide the minimum amount of radiation exposure needed to produce the image. Most ...

  12. Neck x-ray

    Science.gov (United States)

    X-ray - neck; Cervical spine x-ray; Lateral neck x-ray ... There is low radiation exposure. X-rays are monitored so that the lowest amount of radiation is used to produce the image. Pregnant women and ...

  13. Small-angle neutron scattering in materials science

    International Nuclear Information System (INIS)

    Fratzl, P.

    1999-01-01

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

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

    CERN Document Server

    Benediktovitch, Andrei; Ulyanenkov, Alexander

    2013-01-01

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

  15. Grazing incident small angle neutron scattering. Analysis of self-assembly of softmatters in thin films

    International Nuclear Information System (INIS)

    Yokoyama, Hideaki

    2009-01-01

    Grazing incident small angle scattering has been used for the analysis of surface and thin film structures. X-ray in particular is widely used for such analysis and called grazing incident small angle X-ray scattering (GISAXS). However, a very limited number of studied has been done using grazing incident small angle neutron scattering (GISANS) primarily due to low intensity of neutron beam. The arising JPARC neutron source will enable us to use GISANS to analyze thin film structures of softmatter. This report provides a basic concept of GISAS using an example of the analysis of nanocellular thin films fabricated by block copolymer template with supercritical carbon dioxide (BSTSC). (author)

  16. Competitive adsorption of strontium and fulvic acid at the muscovite-solution interface observed with resonant anomalous X-ray reflectivity

    Science.gov (United States)

    Lee, Sang Soo; Park, Changyong; Fenter, Paul; Sturchio, Neil C.; Nagy, Kathryn L.

    2010-03-01

    Molecular-scale distributions of Sr 2+ and fulvic acid (FA) adsorbed on the muscovite (0 0 1) surface were investigated using in situ specular X-ray reflectivity (XR) and resonant anomalous X-ray reflectivity (RAXR). The total amount of Sr 2+ adsorbed from a 1 × 10 -2 mol/kg SrCl 2 and 100 mg/kg Elliott Soil Fulvic Acid II (ESFA II) solution at pH 5.5 compensated 81 ± 5% of the muscovite surface charge, less than previously measured (118 ± 5%) in an ESFA II-free solution with the same Sr concentration and pH. Inner-sphere (IS) and outer-sphere (OS) Sr 2+ constituted 87% of the total adsorbed species in IS:OS proportions of 19:81 compared to 42:58 in the solution without FA, suggesting that adsorbed FA competes with the IS Sr 2+ for surface sites. The coverage of both IS and OS Sr 2+ decreased even more in a pH 3.5 solution containing the same concentration of FA and 0.5 × 10 -2 mol/kg Sr(NO 3) 2, whereas a significant amount of Sr 2+ accumulated farther from the surface in the FA layer. The amount of Sr 2+ incorporated in the ˜10 Å thick FA layer decreased by 79% with decreasing FA concentration (100 → 1 mg/kg) and increasing Sr 2+ concentration (0.5 × 10 -2 → 1 × 10 -2 mol/kg) and pH (3.5 → 3.6). These results indicate not only that adsorbed FA molecules (and perhaps also H 3O +) displace Sr 2+ near the muscovite surface, but also that the sorbed FA film provides binding sites for additional Sr 2+ away from the surface. When a muscovite crystal pre-coated with FA after reaction in a 100 mg/kg ESFA II solution for 50 h was subsequently reacted with a 0.5 × 10 -2 mol/kg Sr(NO 3) 2 and 100 mg/kg ESFA II solution at pH 3.7, a significant fraction of Sr 2+ was distributed in the outer part of the FA film similar to that observed on fresh muscovite reacted at pH 3.5 with a pre-mixed Sr-FA solution at the same concentrations. However, this Sr 2+ sorbed in the pre-adsorbed organic film was more widely distributed and had a lower coverage, suggesting that

  17. The National Facility for Small-Angle Neutron Scattering

    International Nuclear Information System (INIS)

    Koehler, W.C.

    1986-01-01

    On this occasion honoring Professor C.G.Shull, the 30-m small-angle neutron scattering (SANS) instrument of the National Center for Small-Angle Scattering Research (NCSASR) will have been in routine user-mode operation for five years. Professor Shull served the Center as chairman of its first Advisory Committee and in that capacity contributed his expertise to the construction phase of the 30-m machine and to the formulation of operating policy. He has had a long and varied interest in the scientific application of small-angle scattering of X-rays and of neutrons. It is a pleasure for me to dedicate this review to him on his 70th birthday. (orig.)

  18. Cosmic x ray physics

    Science.gov (United States)

    Mccammon, Dan; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1991-01-01

    The annual progress report on Cosmic X Ray Physics for the period 1 Jan. to 31 Dec. 1990 is presented. Topics studied include: soft x ray background, new sounding rocket payload: x ray calorimeter, and theoretical studies.

  19. X-Ray

    Science.gov (United States)

    ... enema. What you can expect During the X-ray X-rays are performed at doctors' offices, dentists' offices, ... as those using a contrast medium. Your child's X-ray Restraints or other techniques may be used to ...

  20. Chest x-ray

    Science.gov (United States)

    Chest radiography; Serial chest x-ray; X-ray - chest ... There is low radiation exposure. X-rays are monitored and regulated to provide the minimum amount of radiation exposure needed to produce the image. Most ...

  1. Abdominal x-ray

    Science.gov (United States)

    Abdominal film; X-ray - abdomen; Flat plate; KUB x-ray ... There is low radiation exposure. X-rays are monitored and regulated to provide the minimum amount of radiation exposure needed to produce the image. Most ...

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

    Energy Technology Data Exchange (ETDEWEB)

    Raghuwanshi, Vikram Singh, E-mail: vikram.raghuwanshi@helmholtz-berlin.de [Helmholtz Zentrum Berlin für Materialien und Energie, Hahn-Meitner Platz 1, D-14109 Berlin (Germany); Harizanova, Ruzha [University of Chemical Technology and Metallurgy, 8 Kl. Ohridski Blvd, 1756 Sofia (Bulgaria); Tatchev, Dragomir [Institute of Physical Chemistry, Bulgarian Academy of Sciences, Acad. G. Bonchev Str. Bl. 11, 1113 Sofia (Bulgaria); Hoell, Armin [Helmholtz Zentrum Berlin für Materialien und Energie, Hahn-Meitner Platz 1, D-14109 Berlin (Germany); Rüssel, Christian [Friedrich Schiller University, Fraunhoferstr. 6, 07743 Jena (Germany)

    2015-02-15

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

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

    International Nuclear Information System (INIS)

    Raghuwanshi, Vikram Singh; Harizanova, Ruzha; Tatchev, Dragomir; Hoell, Armin; Rüssel, Christian

    2015-01-01

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

  4. X-ray astronomy

    International Nuclear Information System (INIS)

    Giacconi, R.; Gursky, H.

    1974-01-01

    This text contains ten chapters and three appendices. Following an introduction, chapters two through five deal with observational techniques, mechanisms for the production of x rays in a cosmic setting, the x-ray sky and solar x-ray emission. Chapters six through ten include compact x-ray sources, supernova remnants, the interstellar medium, extragalactic x-ray sources and the cosmic x-ray background. Interactions of x rays with matter, units and conversion factors and a catalog of x-ray sources comprise the three appendices. (U.S.)

  5. Small-angle scattering studies on clathrin-coated vesicles

    International Nuclear Information System (INIS)

    Bauer, R.; Hansen, S.; Oegendal, L.; Behan, M.; Jones, G.; Mortensen, K.; Saermark, T.

    1991-01-01

    Structural information of clathrin-coated vesicles has been achieved by small-angle X-ray, neutron and dynamic light scattering studies. A characteristic peak in the X-ray and neutron scattering profile (in D 2 O) from intact coated vesicles is consistent with the polygonic structure of the clathrin coat. Neutron as well as dynamic light scattering gives a coated vesicle size close to 1000A. Dynamic light scattering detects a distribution of sizes for the coated vesicles demonstrating polydispersity of the samples. Quick freezing and slow thawing cause breakdown of the polygonic coat and production of large aggregates, as observed by dynamic light scattering and the reduction of the peak in the X-ray scattering profile as well as an increase in the scattering intensity at the lowest angles in the neutron scattering profile. (orig.)

  6. Near edge x-ray spectroscopy theory

    International Nuclear Information System (INIS)

    1994-01-01

    We propose to develop a quantitative theory of x-ray spectroscopies in the near edge region, within about 100 eV of threshold. These spectroscopies include XAFS (X-ray absorption fine structure), photoelectron diffraction (PD), and diffraction anomalous fine structure (DAFS), all of which are important tools for structural studies using synchrotron radiation x-ray sources. Of primary importance in these studies are many-body effects, such as the photoelectron self-energy, and inelastic losses. A better understanding of these quantities is needed to obtain theories without adjustable parameters. We propose both analytical and numerical calculations, the latter based on our x-ray spectroscopy codes FEFF

  7. Chest X-Ray

    Medline Plus

    Full Text Available ... about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed x-ray exams and use a very small dose of ... of the inside of the chest. A chest x-ray is used to evaluate the lungs, heart and ...

  8. X-ray sky

    International Nuclear Information System (INIS)

    Gruen, M.; Koubsky, P.

    1977-01-01

    The history is described of the discoveries of X-ray sources in the sky. The individual X-ray detectors are described in more detail, i.e., gas counters, scintillation detectors, semiconductor detectors, and the principles of X-ray spectrometry and of radiation collimation aimed at increased resolution are discussed. Currently, over 200 celestial X-ray sources are known. Some were identified as nebulae, in some pulsations were found or the source was identified as a binary star. X-ray bursts of novae were also observed. The X-ray radiation is briefly mentioned of spherical star clusters and of extragalactic X-ray sources. (Oy)

  9. Chandra ACIS-S imaging spectroscopy of anomalously faint X-ray emission from Comet 103P/Hartley 2 during the EPOXI encounter

    Science.gov (United States)

    Lisse, C. M.; Christian, D. J.; Wolk, S. J.; Dennerl, K.; Bodewits, D.; Combi, M. R.; Lepri, S. T.; Zurbuchen, T. H.; Li, J. Y.; Dello-Russo, N.; Belton, M. J. S.; Knight, M. M.

    2013-02-01

    We present results from the Chandra X-ray Observatory's characterization of the X-ray emission from Comet 103P/Hartley 2, in support of NASA's Deep Impact Extended close flyby of the comet on 04 November 2010. The comet was observed 4 times for a total on target time of ˜60 ks between the 17th of October and 16th of November 2010, with two of the visits occurring during the EPOXI close approach on 04 November and 05 November 2010. X-ray emission from 103P was qualitatively similar to that observed for collisionally thin Comets 2P/Encke (Lisse, C.M. et al. [2005]. Astrophys. J. 635, 1329-1347) and 9P/Tempel 1 (Lisse, C.M. et al. [2007]. Icarus 190, 391-405). Emission morphology offset sunward but asymmetrical from the nucleus and emission lines produced by charge exchange between highly stripped C, N, and O solar wind minor ions and coma neutral gas species were found. The comet was very under-luminous in the X-ray at all times, representing the 3rd faintest comet ever detected (LX = 1.1 ± 0.3 × 1014 erg s-1). The coma was collisionally thin to the solar wind at all times, allowing solar wind ions to flow into the inner coma and interact with the densest neutral coma gas. Localization of the X-ray emission in the regions of the major rotating gas jets was observed, consistent with the major source of cometary neutral gas species being icy coma dust particles. Variable spectral features due to changing solar wind flux densities and charge states were also seen. Modeling of the Chandra observations from the first three visits using observed gas production rates and ACE solar wind ion fluxes with a charge exchange mechanism for the emission is consistent with the temporal and spectral behavior expected for a slow, hot wind typical of low latitude emission from the solar corona interacting with the comet's neutral coma. The X-ray emission during the 4th visit on 16 November 2010 is similar to the unusual behavior seen for Comet 17P/Holmes in 2007 (Christian, D.J. et

  10. Phase sensitive small angle neutron scattering

    Science.gov (United States)

    Brok, Erik; Majkrzak, Charles F.; Krycka, Kathryn

    It is a well-known problem that information about the scattered wave is lost in scattering experiments because the measured quantity is the modulus squared of the complex wave function. This ''phase problem'' leads to ambiguity in determining the physical properties of the scattering sample. Small angle neutron scattering (SANS) is a useful technique for determining the structure of biomolecules, in particular proteins that cannot be crystallized and studied with x-ray crystallography. However, because the biomolecules are usually suspended in a liquid the observed scattering is an average of all possible orientations, making it difficult to obtain three dimensional structural information. In a proposed method polarized SANS and magnetic nanoparticle references attached to the sample molecules is used to obtain phase sensitive structural information and simultaneously circumvent the problem of orientational averaging (Majkrzak et al. J. Appl. Cryst. 47, 2014) If realized and perfected the technique is very promising for unambiguous determination of the three dimensional structure of biomolecules. We demonstrate the principles of our method and show the first experimental data obtained on a simple test system consisting of core shell magnetic nanoparticles.

  11. X-ray diffraction computed tomography

    International Nuclear Information System (INIS)

    Harding, G.; Kosanetzky, J.; Neitzel, U.

    1987-01-01

    Coherent scattering of x-ray photons leads to the phenomenon of x-ray diffraction, which is widely used for determining atomic structure in materials science. A technique [x-ray diffraction computed tomography (CT)] is described, analogous to conventional CT, in which the x-ray diffraction properties of a stack of two-dimensional object sections may be imaged. The technique has been investigated using a first generation (single pencil beam) CT scanner to measure small angle coherent scatter, in addition to the customary transmitted radiation. Diffraction data from a standard CT performance phantom obtained with this new technique and with an x-ray diffractometer are compared. The agreement is satisfactory bearing in mind the poor momentum resolution of our apparatus. The dose and sensitivity of x-ray diffraction CT are compared with those of conventional transmission CT. Diffraction patterns of some biological tissues and plastics presented in a companion paper indicate the potential of x-ray diffraction CT for tissue discrimination and material characterization. Finally, possibilities for refinement of the technique by improving the momentum resolution are discussed

  12. Small angle scattering and polymers

    Energy Technology Data Exchange (ETDEWEB)

    Cotton, J.P. [Laboratoire Leon Brillouin (LLB) - Centre d`Etudes de Saclay, 91 - Gif-sur-Yvette (France)

    1996-12-31

    The determination of polymer structure is a problem of interest for both statistical physics and industrial applications. The average polymer structure is defined. Then, it is shown why small angle scattering, associated with isotopic substitution, is very well suited to the measurement of the chain conformation. The corresponding example is the old, but pedagogic, measurement of the chain form factor in the polymer melt. The powerful contrast variation method is illustrated by a recent determination of the concentration profile of a polymer interface. (author) 12 figs., 48 refs.

  13. Small angle neutron scattering study of disordered and crystalline iron nanoparticle assemblies

    International Nuclear Information System (INIS)

    Farrell, D.F.; Ijiri, Y.; Kelly, C.V.; Borchers, J.A.; Rhyne, J.J.; Ding, Y.; Majetich, S.A.

    2006-01-01

    Monodisperse surfactant-coated iron nanoparticles are used to form both disordered nanoparticle assemblies and ordered face-centered cubic nanoparticle crystals. The structural order is probed by small angle X-ray scattering, and the magnetic scattering is studied using small angle neutron scattering. The magnetic scattering corresponding to different length scales is interpreted in terms of collective correlations among the particles within the assemblies

  14. Anomalous metallic state with strong charge fluctuations in BaxTi8O16 +δ revealed by hard x-ray photoemission spectroscopy

    Science.gov (United States)

    Dash, S.; Kajita, T.; Okawa, M.; Saitoh, T.; Ikenaga, E.; Saini, N. L.; Katsufuji, T.; Mizokawa, T.

    2018-04-01

    We have studied a charge-orbital driven metal-insulator transition (MIT) in hollandite-type BaxTi8O16 +δ by means of hard x-ray photoemission spectroscopy (HAXPES). The Ti 2 p HAXPES indicates strong Ti3 +/Ti4 + charge fluctuation in the metallic phase above the MIT temperature. The metallic phase is characterized by a power-law spectral function near the Fermi level which would be a signature of bad metal with non-Drude polaronic behavior. The power-law spectral shape is associated with the large Seebeck coefficient of the metallic phase in BaxTi8O16 +δ .

  15. X-ray apparatus

    International Nuclear Information System (INIS)

    Sell, L.J.

    1981-01-01

    A diagnostic x-ray device, readily convertible between conventional radiographic and tomographic operating modes, is described. An improved drive system interconnects and drives the x-ray source and the imaging device through coordinated movements for tomography

  16. X-ray - skeleton

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003381.htm X-ray - skeleton To use the sharing features on this ... Degenerative bone conditions Osteomyelitis Risks There is low radiation exposure. X-rays machines are set to provide the smallest ...

  17. Dental x-rays

    Science.gov (United States)

    X-ray - teeth; Radiograph - dental; Bitewings; Periapical film; Panoramic film; Digital image ... dentist's office. There are many types of dental x-rays. Some of them are: Bitewing. Shows the crown ...

  18. Chest X-Ray

    Medline Plus

    Full Text Available ... some concerns about chest x-rays. However, it’s important to consider the likelihood of benefit to your health. While a chest x-ray use a ... posted: How to Obtain and Share ...

  19. X-ray (image)

    Science.gov (United States)

    X-rays are a form of ionizing radiation that can penetrate the body to form an image on ... will be shades of gray depending on density. X-rays can provide information about obstructions, tumors, and other ...

  20. Chest X-Ray

    Medline Plus

    Full Text Available ... by Image/Video Gallery Your Radiologist Explains Chest X-ray Transcript Welcome to Radiology Info dot org! Hello, ... you about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed ...

  1. Modelling small-angle scattering data from complex protein-lipid systems

    DEFF Research Database (Denmark)

    Kynde, Søren Andreas Røssell

    as carriers of membrane proteins. Together they form monodisperse soluble aggregates of about 10 nm in size. Chapter 2 introduces the method of small-angle scattering. Small-angle X-ray and neutron scattering are well suited for studying particles in solution on length scales from 1 to 100 nm. This makes...... describes a protein system that has successfully been measured with small-angle scattering methods and subsequently analysed using the hybrid approach. Paper I governs the transmembrane protein bacteriorhodopsin embedded into a phospholipid nanodisc. The modelling is based on a crystal structure...

  2. Flash X-ray

    International Nuclear Information System (INIS)

    Sato, Eiichi

    2003-01-01

    Generation of quasi-monochromatic X-ray by production of weakly ionized line plasma (flash X-ray), high-speed imaging by the X-ray and high-contrast imaging by the characteristic X-ray absorption are described. The equipment for the X-ray is consisted from the high-voltage power supply and condenser, turbo molecular pump, and plasma X-ray tube. The tube has a long linear anticathode to produce the line plasma and flash X-ray at 20 kA current at maximum. X-ray spectrum is measured by the imaging plate equipped in the computed radiography system after diffracted by a LiF single crystal bender. Cu anticathode generates sharp peaks of K X-ray series. The tissue images are presented for vertebra, rabbit ear and heart, and dog heart by X-ray fluoroscopy with Ce anticathode. Generation of K-orbit characteristic X-ray with extremely low bremsstrahung is to be attempted for medical use. (N.I.)

  3. The use of anomalous scattering of uranium for the determination of biological macromolecules structures - From hard to soft X-rays

    International Nuclear Information System (INIS)

    Chesne-Seck, M.L.

    2002-01-01

    In order to solve biological macromolecules structures, structure factor phases must be derived from the intensities diffracted by the crystal. The SAD and the MAD methods make use of variations in scattering factors measured at specific absorption edges of heavy atoms, bound to the protein. The phasing power depends on the occupancy of the binding sites and on the variations of the scattering factors at the absorption edge that is used. With uranyl, numerous sites with low occupancies are usually obtained. We used new colored uranyl complexes, which give higher occupancies, to solve de novo the lysozyme structure and an unknown structure. We have developed the use of the My absorption edge of uranium (λ = 3,5 Angstroms), where a variation of 120 electrons is observed in the scattering factors. With a helium atmosphere to limit the X-rays absorption, we have collected three data sets, on a single image. Data were processed both with 'classical' and specific programs. (author) [fr

  4. X-ray can do more; ''Roentgen'' kann noch mehr

    Energy Technology Data Exchange (ETDEWEB)

    Spiess, Lothar [Technische Univ. Ilmenau (Germany). Inst. fuer Werkstofftechnik; Teichert, Gerd [Technische Univ. Ilmenau (Germany). MFPA Weimar Pruefzentrum Schicht- und Materialeigenschaften

    2013-07-01

    Radiography is not the only technology for characterising components and materials. Other methods which make use of X-ray radiation to characterise materials include X-ray fluorescence analysis (RFA) and, a technique still neglected to date, X-ray diffractometry (XRD) including small-angle X-ray scattering (SAXS) and X-ray reflectometry (XRR, GISAXS). This paper presents the capabilities, limits and application areas of these other X-ray techniques, which add to the range of nondestructive material characterisation methods beside classical radiography. Material analyses of brass materials are used as examples.

  5. Characterization of nano-size heterogeneities by small-angle-scattering

    International Nuclear Information System (INIS)

    Ohnuma, Masato

    2012-01-01

    Techniques of Small-Angle Neutron and X-ray Scattering (SANS and SAXS) are overviewed from principle to applications. Importance of characterizing composition of nano-size heterogeneity is explained based on the results obtained by combination of SANS and SAXS. (author)

  6. X-ray holography

    CERN Document Server

    Faigel, G; Belakhovsky, M; Marchesini, S; Bortel, G

    2003-01-01

    In the last decade holographic methods using hard X-rays were developed. They are able to resolve atomic distances, and can give the 3D arrangement of atoms around a selected element. Therefore, hard X-ray holography has potential applications in chemistry, biology and physics. In this article we give a general description of these methods and discuss the developments in the experimental technique. The capabilities of hard X-ray holography are demonstrated by examples.

  7. X-ray holography

    International Nuclear Information System (INIS)

    Faigel, G.; Tegze, M.; Belakhovsky, M.; Marchesini, S.; Bortel, G.

    2003-01-01

    In the last decade holographic methods using hard X-rays were developed. They are able to resolve atomic distances, and can give the 3D arrangement of atoms around a selected element. Therefore, hard X-ray holography has potential applications in chemistry, biology and physics. In this article we give a general description of these methods and discuss the developments in the experimental technique. The capabilities of hard X-ray holography are demonstrated by examples

  8. Providing x-rays

    International Nuclear Information System (INIS)

    Mallozzi, P.J.; Epstein, H.M.

    1985-01-01

    This invention provides an apparatus for providing x-rays to an object that may be in an ordinary environment such as air at approximately atmospheric pressure. The apparatus comprises: means (typically a laser beam) for directing energy onto a target to produce x-rays of a selected spectrum and intensity at the target; a fluid-tight enclosure around the target; means for maintaining the pressure in the first enclosure substantially below atmospheric pressure; a fluid-tight second enclosure adjoining the first enclosure, the common wall portion having an opening large enough to permit x-rays to pass through but small enough to allow the pressure reducing means to evacuate gas from the first enclosure at least as fast as it enters through the opening; the second enclosure filled with a gas that is highly transparent to x-rays; the wall of the second enclosure to which the x-rays travel having a portion that is highly transparent to x-rays (usually a beryllium or plastic foil), so that the object to which the x-rays are to be provided may be located outside the second enclosure and adjacent thereto and thus receive the x-rays substantially unimpeded by air or other intervening matter. The apparatus is particularly suited to obtaining EXAFS (extended x-ray fine structure spectroscopy) data on a material

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

    International Nuclear Information System (INIS)

    Borbely, S.; Rosta, L.

    1999-04-01

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

  10. Modeling the amorphous structure of mechanically alloyed Ti{sub 50}Ni{sub 25}Cu{sub 25} using anomalous wide-angle x-ray scattering and reverse Monte Carlo simulation

    Energy Technology Data Exchange (ETDEWEB)

    Lima, J.C. de, E-mail: fsc1jcd@fisica.ufsc.br [Departamento de Física, Universidade Federal de Santa Catarina, Campus Universitário Trindade, S/N, C.P. 476, 88040-900 Florianópolis, Santa Catarina (Brazil); Poffo, C.M. [Departamento de Engenharia Mecânica, Universidade Federal de Santa Catarina, Campus Universitário Trindade, S/N, C.P. 476, 88040-900 Florianópolis, Santa Catarina (Brazil); Departamento de Física, Universidade Federal do Amazonas, 3000 Japiim, 69077-000 Manaus, Amazonas (Brazil); Souza, S.M. [Departamento de Física, Universidade Federal do Amazonas, 3000 Japiim, 69077-000 Manaus, Amazonas (Brazil); Machado, K.D. [Departamento de Física, Centro Politécnico, Universidade Federal do Paraná, 81531-990 Curitiba, Paraná (Brazil); Trichês, D.M. [Departamento de Física, Universidade Federal do Amazonas, 3000 Japiim, 69077-000 Manaus, Amazonas (Brazil); Grandi, T.A. [Departamento de Física, Universidade Federal de Santa Catarina, Campus Universitário Trindade, S/N, C.P. 476, 88040-900 Florianópolis, Santa Catarina (Brazil); Biasi, R.S. de [Seção de Engenharia Mecânica e de Materiais, Instituto Militar de Engenharia, 22290-270 Rio de Janeiro, RJ (Brazil)

    2013-09-01

    An amorphous Ti{sub 50}Ni{sub 25}Cu{sub 25} alloy was produced by 19 h of mechanical alloying. Anomalous wide angle x-ray scattering data were collected at six energies and six total scattering factors were obtained. By considering the data collected at two energies close to the Ni and Cu K edges, two differential anomalous scattering factors about the Ni and Cu atoms were obtained, showing that the chemical environments around these atoms are different. Eight factors were used as input data to the reverse Monte Carlo method used to compute the partial structure factors S{sub Ti3Ti}(K), S{sub Ti–Cu}(K), S{sub Ti–Ni}(K), S{sub Cu3Cu}(K), S{sub Cu–Ni}(K) and S{sub Ni–Ni}(K) and the partial pair distribution functions G{sub Ti3Ti}(r), G{sub Ti–Cu}(r), G{sub Ti–Ni}(r), G{sub Cu3Cu}(r), G{sub Cu–Ni}(r) and G{sub Ni–Ni}(r). From the RMC final atomic configuration and G{sub ij}(r) functions, the coordination numbers and interatomic atomic distances for the first neighbors were determined.

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

    Energy Technology Data Exchange (ETDEWEB)

    Chaudhuri, Barnali [University at Buffalo (SUNY); Muñoz, Inés G. [Centro Nacional de Investigaciones Oncológicas Madrid, Madrid, Spain; Urban, Volker S. [ORNL; Qian, Shuo [ORNL

    2017-12-01

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

  12. Extremity x-ray

    Science.gov (United States)

    ... page: //medlineplus.gov/ency/article/003461.htm Extremity x-ray To use the sharing features on this page, ... in the body Risks There is low-level radiation exposure. X-rays are monitored and regulated to provide the ...

  13. Chest X-Ray

    Medline Plus

    Full Text Available ... loose, comfortable clothing. You may be asked to change into a gown. You may have some concerns about chest x-rays. However, it’s important to consider the likelihood of benefit to your health. While a chest x-ray use a tiny ...

  14. Chest X-Ray

    Medline Plus

    Full Text Available ... by Image/Video Gallery Your Radiologist Explains Chest X-ray Transcript Welcome to Radiology Info dot org! Hello, ... d like to talk with you about chest radiography also known as chest x-rays. Chest x- ...

  15. Insights from soft X-rays

    DEFF Research Database (Denmark)

    Raaf, Jennifer; Issinger, Olaf-Georg; Niefind, Karsten

    2008-01-01

    The diffraction pattern of a protein crystal is normally a product of the interference of electromagnetic waves scattered by electrons of the crystalline sample. The diffraction pattern undergoes systematic changes in case additionally X-ray absorption occurs, meaning if the wavelength of the pri......The diffraction pattern of a protein crystal is normally a product of the interference of electromagnetic waves scattered by electrons of the crystalline sample. The diffraction pattern undergoes systematic changes in case additionally X-ray absorption occurs, meaning if the wavelength...... of the primary X-ray beam is relatively close to the absorption edge of selected elements of the sample. The resulting effects are summarized as "anomalous dispersion" and can be always observed with "soft" X-rays (wavelength around 2 A) since they match the absorption edges of sulfur and chlorine...

  16. X-ray generator

    International Nuclear Information System (INIS)

    Dawson, J.M.

    1976-01-01

    An apparatus and a method are described for producing coherent secondary x-rays that are controlled as to direction by illuminating a mixture of high z and low z gases with an intense burst of primary x-rays. The primary x-rays are produced with a laser activated plasma, and these x-rays strip off the electrons of the high z atoms in the lasing medium, while the low z atoms retain their electrons. The neutral atoms transfer electrons to highly excited states of the highly stripped high z ions giving an inverted population which produces the desired coherent x-rays. In one embodiment, a laser, light beam provides a laser spark that produces the intense burst of coherent x-rays that illuminates the mixture of high z and low z gases, whereby the high z atoms are stripped while the low z ones are not, giving the desired mixture of highly ionized and neutral atoms. Means for magnetically confining and stabilizing the plasma are disclosed for controlling the direction of the x-rays

  17. X-ray crystallography

    Science.gov (United States)

    2001-01-01

    X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

  18. X-ray apparatus

    International Nuclear Information System (INIS)

    Bernstein, S.; Stagg, L.; Lambert, T.W.; Griswa, P.J.

    1976-01-01

    A patient support system for X-ray equipment in arteriographic studies of the heart is described in detail. The support system has been designed to overcome many of the practical problems encountered in using previous types of arteriographic X-ray equipment. The support system is capable of horizontal movement and, by a series of shafts attached to the main support system, the X-ray source and image intensifier or detector may be rotated through the same angle. The system is highly flexible and details are given of several possible operational modes. (U.K.)

  19. X-ray detector

    International Nuclear Information System (INIS)

    Whetten, N.R.; Houston, J.M.

    1977-01-01

    An ionization chamber for use in determining the spatial distribution of x-ray photons in tomography systems comprises a plurality of substantially parallel, planar anodes separated by parallel, planar cathodes and enclosed in a gas of high atomic weight at a pressure from approximately 10 atmospheres to approximately 50 atmospheres. The cathode and anode structures comprise metals which are substantially opaque to x-ray radiation and thereby tend to reduce the resolution limiting effects of x-ray fluoresence in the gas. In another embodiment of the invention the anodes comprise parallel conductive bars disposed between two planar cathodes. Guard rings eliminate surface leakage currents between adjacent electrodes. 8 figures

  20. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive medical ...

  1. Panoramic Dental X-Ray

    Science.gov (United States)

    ... Resources Professions Site Index A-Z Panoramic Dental X-ray Panoramic dental x-ray uses a very small ... limitations of Panoramic X-ray? What is Panoramic X-ray? Panoramic radiography , also called panoramic x-ray , is ...

  2. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  3. Bone X-Ray (Radiography)

    Science.gov (United States)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  4. Abdomen X-Ray (Radiography)

    Science.gov (United States)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Abdomen Abdominal x-ray uses a very ... of an abdominal x-ray? What is abdominal x-ray? An x-ray (radiograph) is a noninvasive medical ...

  5. X-Ray Exam: Hip

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Hip KidsHealth / For Parents / X-Ray Exam: ... darker. An X-ray technician takes the X-rays. An X-ray technician in the radiology department of a ...

  6. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small dose ... limitations of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is ...

  7. Lumbosacral spine x-ray

    Science.gov (United States)

    X-ray - lumbosacral spine; X-ray - lower spine ... The test is done in a hospital x-ray department or your health care provider's office by an x-ray technician. You will be asked to lie on the x-ray table ...

  8. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  9. Spectroscopic Studies of X-Ray Binary Pulsars

    Indian Academy of Sciences (India)

    R. Narasimhan (Krishtel eMaging) 1461 1996 Oct 15 13:05:22

    ... those X-ray sources. A merit of investigating soft excess feature using XBP spectra is that it allows us to search pulse modulation of the soft component. Anomalous X-ray pulsars (AXPs) are also known to have a two component spectra, a steep power law and blackbody emission model (e.g., Mereghetti & Stella 1995).

  10. Chest X-Ray

    Medline Plus

    Full Text Available ... Radiology and You Take our survey Sponsored by Image/Video Gallery Your Radiologist Explains Chest X-ray ... posted: How to Obtain and Share Your Medical Images Movement Disorders Video: The Basketball Game: An MRI ...

  11. X-ray tubes

    International Nuclear Information System (INIS)

    Young, R.W.

    1979-01-01

    A form of x-ray tube is described which provides satisfactory focussing of the electron beam when the beam extends for several feet from gun to target. Such a tube can be used for computerised tomographic scanning. (UK)

  12. Chest X-Ray

    Medline Plus

    Full Text Available ... Site Index A-Z Spotlight February is American Heart Month Recently posted: Carotid Intima-Media Thickness Test ... x-ray is used to evaluate the lungs, heart and chest wall and may be used to ...

  13. Chest X-Ray

    Medline Plus

    Full Text Available ... Abdominal Ultrasound Video: Pelvic Ultrasound Medical Imaging Costs Radiology and You Take our survey Sponsored by Image/ ... Radiologist Explains Chest X-ray Transcript Welcome to Radiology Info dot org! Hello, I’m Dr. Geoffrey ...

  14. Chest X-Ray

    Medline Plus

    Full Text Available ... exams and use a very small dose of ionizing radiation to produce pictures of the inside of the ... chest x-ray use a tiny dose of ionizing radiation, the benefit of an accurate diagnosis far outweighs ...

  15. Chest X-Ray

    Medline Plus

    Full Text Available ... accurate diagnosis far outweighs any risk. For more information about chest x-rays, visit Radiology Info dot ... Inc. (RSNA). To help ensure current and accurate information, we do not permit copying but encourage linking ...

  16. Chest X-Ray

    Medline Plus

    Full Text Available ... and You Take our survey Sponsored by Image/Video Gallery Your Radiologist Explains Chest X-ray Transcript ... Carotid Intima-Media Thickness Test Medical Imaging Costs Video: Abdominal Ultrasound Video: Pelvic Ultrasound Radiology and You ...

  17. Chest X-Ray

    Medline Plus

    Full Text Available ... However, it’s important to consider the likelihood of benefit to your health. While a chest x-ray use a tiny dose of ionizing radiation, the benefit of an accurate diagnosis far outweighs any risk. ...

  18. Chest X-Ray

    Medline Plus

    Full Text Available ... chest x-ray is used to evaluate the lungs, heart and chest wall and may be used ... diagnose and monitor treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A ...

  19. Chest X-Ray

    Medline Plus

    Full Text Available ... and use a very small dose of ionizing radiation to produce pictures of the inside of the ... x-ray use a tiny dose of ionizing radiation, the benefit of an accurate diagnosis far outweighs ...

  20. Chest X-Ray

    Medline Plus

    Full Text Available ... Index A-Z Spotlight March is National Colorectal Cancer Awareness Month Recently posted: Carotid Intima-Media Thickness ... of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray requires no special preparation. ...

  1. Chest X-Ray

    Medline Plus

    Full Text Available ... Index A-Z Spotlight March is National Colorectal Cancer Awareness Month Recently posted: How to Obtain and ... of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray requires no special preparation. ...

  2. Chest X-Ray

    Medline Plus

    Full Text Available ... Index A-Z Spotlight March is National Colorectal Cancer Awareness Month Recently posted: Video: The Basketball Game: ... of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray requires no special preparation. ...

  3. X-Ray Lasers

    Science.gov (United States)

    Eder, David C.

    1998-05-01

    We provide an overview of the status of x-ray laser development worldwide with particular attention given to activities at LLNL. Since the demonstration of x-ray lasing 14 years ago there has been major progress in achieving shorter wavelengths, higher energies per pulse, higher efficiency, shorter pulse durations, etc. Original x-ray lasers used large kJ class lasers to achieve lasing in mid-Z materials with electron collisional pumping in the highly stripped ion being the most successful process for populating the upper-laser state. The two most common electron configurations for these collisional x-ray lasers are Ne-like and Ni-like ions. Through the use of prepulses and short picosecond driving pulses, transient collisional x-ray lasing schemes have been demonstrated using lasers with only a few Joules per pulse. An interesting aspect of these lasers is the time lag in reaching ionization equilibrium helps in obtaining high gain coefficients. A different approach to x-ray lasing is also being studied where lasing occurs in a singly ionized ion following innershell photoionization. The major requirement of the driving laser in this case is an ultrashort pulse duration (rise time to achieve lasing prior to collisional ionization of outershell electrons. In the area of applications, most of the work has been for single pulse experiments such as plasma and biological imaging. However, many of the new x-ray lasers achieve high average power by having a reasonable repetition rate of order 10 Hz and we briefly discuss relevant applications for these x-ray lasers. This work performed under the auspices of US DOE by LLNL under Contract No. W-7405-Eng-48.

  4. X-Ray Optics

    Science.gov (United States)

    1990-01-01

    samples. Another exciting application of microbeam of x-rays is in that of high pressure x-ray diffraction from small samples. Along this line, Yan...will be presented by Jonathan in February at the Physics and Chemistry of Semiconductor Interfaces conference and in March at the American Physical...VUV9 conference this summer. Jeff has also worked on developing software that makes use of the scattering factor tables for both microvax and IBM PC

  5. Low Mass X-ray Binary 4U1705-44 Exiting an Extended High X-ray State

    Science.gov (United States)

    Phillipson, Rebecca; Boyd, Patricia T.; Smale, Alan P.

    2017-09-01

    The neutron-star low-mass X-ray binary 4U1705-44, which exhibited high amplitude long-term X-ray variability on the order of hundreds of days during the 16-year continuous monitoring by the RXTE ASM (1995-2012), entered an anomalously long high state in July 2012 as observed by MAXI (2009-present).

  6. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... drawer under the table holds the x-ray film or image recording plate . Sometimes the x-ray ... extended over the patient while an x-ray film holder or image recording plate is placed beneath ...

  7. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... of knee x-rays. A portable x-ray machine is a compact apparatus that can be taken ... of the body being examined, an x-ray machine produces a small burst of radiation that passes ...

  8. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... are the limitations of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray ( ... leg (shin), ankle or foot. top of page What are some common uses of the procedure? A ...

  9. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... holds the x-ray film or image recording plate . Sometimes the x-ray is taken with the ... an x-ray film holder or image recording plate is placed beneath the patient. top of page ...

  10. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose ... Medicine Radiation Safety How to Read Your Radiology Report Images related to X-ray (Radiography) - Bone Sponsored ...

  11. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... that might interfere with the x-ray images. Women should always inform their physician and x-ray ... Safety page for more information about radiation dose. Women should always inform their physician or x-ray ...

  12. Small-angle scattering applications to materials science

    International Nuclear Information System (INIS)

    Gerold, V.

    1978-01-01

    The review describes results of the last three or four years from the application of both X-ray and neutron small-angle scattering (SAS) to problems in the general field of materials science. A wide range of topics has been covered including phase separation in binary and ternary systems (early stages as well as the determination of the metastable miscibility gap), density and concentration fluctuations in single-phase systems, and studies of various structural defects such as voids, radiation damage, dislocations, and surfaces and interfaces. The interaction between magnetic moments and neutrons has made possible SAS research on the long-range interaction of spins in complicated magnetic systems and flux-line studies in type-II superconductors, and this work is also reviewed. (Auth.)

  13. Small-angle neutron scattering instrument at MINT

    International Nuclear Information System (INIS)

    Mohd Ali Sufi; Yusof Abdullah; Razali Kassim; Hamid; Shahidan Radiman; Mohammad Deraman; Abdul Ghaffar Ramli

    1996-01-01

    The Small Angle Neutron Scattering (SANS) Instrument has been developed at Malaysian Institute for Nuclear Technology Research (MINT) for studying structural properties of materials on the length scale 1 nm to 100 nm. This is the length scale which is relevant for many topics within soft condensed matter, like polymers, colloids, biological macromolecules, etc. The SANS is a complementary technique to X-ray and electron scattering. However, while these later techniques give information on structures near surface, SANS concerns the structure of the bulk. Samples studied by SANS technique are typically bulk materials of the sizes mm's to cm's, or materials dissolved in a liquid. This paper described the general characteristics of SANS instrument as well as the experimental formulation in neutron scattering. The preliminary results obtained by this instrument are shown

  14. Field study of nanoparticles by small angle neutron scattering

    International Nuclear Information System (INIS)

    Mirebeau, I.; Hennion, M.; Bellouard, C.

    1994-01-01

    In nanometric iron particles, magnetic correlations are determined by small angle neutron scattering and compared to their values calculated in a simple superparamagnetic model. The introduction of a Lorentzian shape for the magnetic form factor is necessary to obtain a good fit of the data. This reveals two extra features: a spin disorder at the surface of the particles which persists in applied field, and a distribution in the particle sizes not probed by X-rays. The field alignment becomes easier with decreasing temperature. This is no longer true for samples with bigger and closer-packed particles, where strong dipolar interactions develop at low temperatures and oppose to the external field. 4 figs., 3 refs

  15. Small-angle neutron-scattering experiments

    International Nuclear Information System (INIS)

    Hardy, A.D.; Thomas, M.W.; Rouse, K.D.

    1981-04-01

    A brief introduction to the technique of small-angle neutron scattering is given. The layout and operation of the small-angle scattering spectrometer, mounted on the AERE PLUTO reactor, is also described. Results obtained using the spectrometer are presented for three materials (doped uranium dioxide, Magnox cladding and nitrided steel) of interest to Springfields Nuclear Power Development Laboratories. The results obtained are discussed in relation to other known data for these materials. (author)

  16. X-Ray Absorption with Transmission X-Ray Microscopes

    NARCIS (Netherlands)

    de Groot, F.M.F.

    2016-01-01

    In this section we focus on the use of transmission X-ray microscopy (TXM) to measure the XAS spectra. In the last decade a range of soft X-ray and hard X-ray TXM microscopes have been developed, allowing the measurement of XAS spectra with 10–100 nm resolution. In the hard X-ray range the TXM

  17. Small-Angle Scattering from Nanoscale Fat Fractals.

    Science.gov (United States)

    Anitas, E M; Slyamov, A; Todoran, R; Szakacs, Z

    2017-12-01

    Small-angle scattering (of neutrons, x-ray, or light; SAS) is considered to describe the structural characteristics of deterministic nanoscale fat fractals. We show that in the case of a polydisperse fractal system, with equal probability for any orientation, one obtains the fractal dimensions and scaling factors at each structural level. This is in agreement with general results deduced in the context of small-angle scattering analysis of a system of randomly oriented, non-interacting, nano-/micro-fractals. We apply our results to a two-dimensional fat Cantor-like fractal, calculating analytic expressions for the scattering intensities and structure factors. We explain how the structural properties can be computed from experimental data and show their correlation to the variation of the scaling factor with the iteration number. The model can be used to interpret recorded experimental SAS data in the framework of fat fractals and can reveal structural properties of materials characterized by a regular law of changing of the fractal dimensions. It can describe successions of power-law decays, with arbitrary decreasing values of the scattering exponents, and interleaved by regions of constant intensity.

  18. Characterization of porous materials by small-angle scattering

    International Nuclear Information System (INIS)

    Mazumder, S.; Sen, D.; Patra, A.K.

    2004-01-01

    Characterization of porous materials by small-angle scattering has been extensively pursued for several years now as the pores are often of mesoscopic size and compatible with the length scale accessible by the technique using both neutrons and X-rays as probing radiation. With the availability of ultra small-angle scattering instruments, one can investigate porous materials in the sub-micron length scale. Because of the increased accessible length scale vis-a-vis the multiple scattering effect, conventional data analysis procedures based on single scattering approximation quite often fail. The limitation of conventional data analysis procedures is also pronounced in the case of thick samples and long wavelength of the probing radiation. Effect of multiple scattering is manifested by broadening the scattering profile. Sample thickness for some technologically important materials is often significantly high, as the experimental samples have to replicate all its essential properties in the bulk material. Larger wavelength of the probing radiation is used in some cases to access large length scale and also to minimize the effect of double Bragg reflections. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-01

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

  20. 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

    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, Torus...

  1. Study of particles in solution by small angle x-ray scattering

    International Nuclear Information System (INIS)

    Itri, R.

    1986-01-01

    The implantation of SAXS technique is presented, and mycellas in solution of the dodecyl sodium sulfate SLS/water system are studied. A synthesis of SAXS theory to study parameters such as, volume, radii of gyration and specific surface and distribution function of the distance of homogenous and inhomogeneous particles is also presented. The technique was implanted by the study of a vitreous coal sample with voids in amorphous matrix. Computer programs were used for data treatment. It was concluded that the void configuration must be an oblate ellipsoid with rippled external surface and radii of gyration of ∼20A . The study of mycellas in solution of the SLL/H 2 O binary system showed spherical mycellas with paraffinic radii of 16A and total radii of 25.5 A. Interaction effects start to appear in 15% SLS concentrations. The change in the scattering curve occurs due to the interactions between mycellas. The isotropic-nematic transition in the ternary system by decanol addition was also investigated. (M.C.K.) [pt

  2. Small angle neutron and X-ray studies of carbon structures with metal atoms

    Science.gov (United States)

    Lebedev, V. T.; Szhogina, A. A.; Bairamukov, V. Yu

    2017-05-01

    Encapsulation of metal atoms inside carbon single-wall cages or within multi-layer cells has been realized using molecular precursors and high temperature processes transforming them into desirable structures. Endohedral fullerenols Fe@C60(OH)X with 3d-metal (iron) have been studied by SANS in aqueous solutions where they form stable globular clusters with radii R C ∼ 10-12 nm and aggregation numbers N C ∼ 104. This self-assembly is a crucial feature of paramagnetic fullerenols as perspective contrast agents for Magneto-Resonance Imaging in medicine. Cellular carbon-metal structures have been created by the pyrolysis of diphthalocyanines of lanthanides and actinides. It was established that these ultra porous matrices consist of globular cells of molecular precursor size (∼ 1 nm) which are aggregated into superstructures. This provides retain of metal atoms inside matrices which may serve for safety storage of spent fuel of nuclear power plants.

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

    CSIR Research Space (South Africa)

    Jonah, EO

    2012-10-01

    Full Text Available 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...

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

    Energy Technology Data Exchange (ETDEWEB)

    Howell, Steven C. [George Washington Univ., Washington, DC (United States)

    2016-01-31

    We set out to determine quantitative information regarding the dynamic conformation of nucleosome arrays in solution using experimental SAXS. Toward this end, we developed a CG simulation algorithm for dsDNA which rapidly generates ensembles of structures through Metropolis MC sampling of a Markov chain.

  5. Small angle neutron and X-ray studies of carbon structures with metal atoms

    International Nuclear Information System (INIS)

    Lebedev, V T; Szhogina, A A; Yu Bairamukov, V

    2017-01-01

    Encapsulation of metal atoms inside carbon single-wall cages or within multi-layer cells has been realized using molecular precursors and high temperature processes transforming them into desirable structures. Endohedral fullerenols Fe@C 60 (OH) X with 3d-metal (iron) have been studied by SANS in aqueous solutions where they form stable globular clusters with radii R C ∼ 10-12 nm and aggregation numbers N C ∼ 10 4 . This self-assembly is a crucial feature of paramagnetic fullerenols as perspective contrast agents for Magneto-Resonance Imaging in medicine. Cellular carbon-metal structures have been created by the pyrolysis of diphthalocyanines of lanthanides and actinides. It was established that these ultra porous matrices consist of globular cells of molecular precursor size (∼ 1 nm) which are aggregated into superstructures. This provides retain of metal atoms inside matrices which may serve for safety storage of spent fuel of nuclear power plants. (paper)

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

    Indian Academy of Sciences (India)

    To prevent oxidation upon exposure to atmo-. (leminej@yahoo.com) sphere, the sample was over-coated with 140 Å amorphous silicon. Thermal annealing .... Tappert J, Keune W, Brand R A, Vulliet P, Sanchez J-P and Shinjo. T 1996 J. Appl. Phys. 80 4503. Tappert J, Neumann S, Brand R A, Keune W, Klose F and Maletta.

  7. Small angle scatter imaging from wide beam diffraction patterns

    International Nuclear Information System (INIS)

    Wilkinson, Steven J; Rogers, Keith D; Hall, Chris J; Round, Adam R

    2007-01-01

    In this paper we report on the extension of the technique of mapping small angle x-ray scatter (SAXS) across a soft material specimen several millimetres square. In the conventional SAXS mapping technique a pencil beam of x-rays is raster scanned over the specimen with the scatter pattern recorded from each point in the raster. In our technique a wide, parallel beam is used, speeding up the data collection time considerably. An image processing algorithm is used to separate the scatter pattern features from individual points along the line of the beam. To test the efficacy of the technique a phantom was constructed using gelatin and rat tail tendon collagen. Collagen fibres in the phantom were arranged in quarters horizontally, diagonally and vertically leaving one quarter with just gelatin. The phantom was used to collect both raster scanned sets of SAXS patterns spaced at 0.25 mm horizontally and vertically and also a wide beam data set. The width of the beam in this case was approximately 7 mm. Using the third-order diffraction of rat tail tendon intensity data were gathered from each SAXS pattern and used to construct a map. Data from the raster scan image and that from the wide beam are compared. Finally using a phantom made from dehydrated rat tail tendon and paraffin wax a tomographic slice constructed using data from SAXS patterns is shown

  8. X-ray astronomy

    International Nuclear Information System (INIS)

    Giacconi, R.; Setti, G.

    1980-01-01

    This book contains the lectures, and the most important seminars held at the NATO meeting on X-Ray astronomy in Erice, July 1979. The meeting was an opportune forum to discuss the results of the first 8-months of operation of the X-ray satellite, HEAO-2 (Einstein Observatory) which was launched at the end of 1978. Besides surveying these results, the meeting covered extragalactic astronomy, including the relevant observations obtained in other portions of the electromagnetic spectrum (ultra-violet, optical, infrared and radio). The discussion on galactic X-ray sources essentially covered classical binaries, globular clusters and bursters and its significance to extragalactic sources and to high energy astrophysics was borne in mind. (orig.)

  9. X-ray tube

    International Nuclear Information System (INIS)

    Webley, R.S.

    1975-01-01

    The object of the invention described is to provide an X-ray tube providing a scanned X-ray output which does not require a scanned electron beam. This is obtained by an X-ray tube including an anode which is rotatable about an axis, and a source of a beam of energy, for example an electron beam, arranged to impinge on a surface of the anode to generate X-radiation substantially at the region of incidence on the anode surface. The anode is rotatable about the axis to move the region of incidence over the surface. The anode is so shaped that the rotation causes the region of incidence to move in a predetermined manner relative to fixed parts of the tube so that the generated X-radiation is scanned in a predetermined manner relative to the tube. (UK)

  10. X-Ray Exam: Pelvis

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Pelvis KidsHealth / For Parents / X-Ray Exam: ... Ray Exam: Hip Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  11. X-Ray Exam: Forearm

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Forearm KidsHealth / For Parents / X-Ray Exam: ... Muscles, and Joints Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  12. X-Ray Exam: Foot

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Foot KidsHealth / For Parents / X-Ray Exam: ... Muscles, and Joints Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  13. X-Ray Exam: Wrist

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Wrist KidsHealth / For Parents / X-Ray Exam: ... Muscles, and Joints Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  14. Thoracic spine x-ray

    Science.gov (United States)

    Vertebral radiography; X-ray - spine; Thoracic x-ray; Spine x-ray; Thoracic spine films; Back films ... There is low radiation exposure. X-rays are monitored and regulated to provide the minimum amount of radiation exposure needed to produce the image. Most ...

  15. X-Ray Exam: Finger

    Science.gov (United States)

    ... Staying Safe Videos for Educators Search English Español X-Ray Exam: Finger KidsHealth / For Parents / X-Ray Exam: ... Muscles, and Joints Broken Bones Getting an X-ray (Video) X-Ray (Video) View more Partner Message About Us ...

  16. Subluminous X-ray binaries

    NARCIS (Netherlands)

    Armas Padilla, M.

    2013-01-01

    The discovery of the first X-ray binary, Scorpius X-1, by Giacconi et al. (1962), marked the birth of X-ray astronomy. Following that discovery, many additional X-ray sources where found with the first generation of X-ray rockets and observatories (e.g., UHURU and Einstein). The short-timescale

  17. X-ray detector

    International Nuclear Information System (INIS)

    Houston, J.M.; Whetten, N.R.

    1981-01-01

    An ionization chamber for use in determining the spatial distribution of x-ray photons in tomography systems comprises a plurality of substantially parallel, planar anodes separated by parallel, planar cathodes and enclosed in a gas of high atomic weight at a pressure from approximately 10 atmospheres to approximately 50 atmospheres. The cathode and anode structures comprise metals which are substantially opaque to x-ray radiation and thereby tend to reduce the resolution limiting effects of xray fluoresence in the gas. In another embodiment of the invention the anodes comprise parallel conductive bars disposed between two planar cathodes. Guard rings eliminate surface leakage currents between adjacent electrodes

  18. X-ray masks

    International Nuclear Information System (INIS)

    Greenwood, J.C.; Satchell, D.W.

    1984-01-01

    In semiconductor manufacture, where X-ray irradiation is used, a thin silicon membrane can be used as an X-ray mask. This membrane has areas on which are patterns to define the regions to be irradiated. These regions are of antireflection material. With the thin, in the order of 3 microns, membranes used, fragility is a problem. Hence a number of ribs of silicon are formed integral with the membrane, and which are relatively thick, 5 to 10 microns. The ribs may be formed by localised deeper boron deposition followed by a selective etch. (author)

  19. Flash x-ray

    International Nuclear Information System (INIS)

    Johnson, Q.; Pellinen, D.

    1976-01-01

    The complementary techniques of flash x-ray radiography (FXR) and flash x-ray diffraction (FXD) provide access to a unique domain in nondestructive materials testing. FXR is useful in studies of macroscopic properties during extremely short time intervals, and FXD, the newer technique, is used in studies of microscopic properties. Although these techniques are similar in many respects, there are some substantial differences. FXD generally requires low-voltage, line-radiation sources and extremely accurate timing; FXR is usually less demanding. Phenomena which can be profitably studied by FXR often can also be studied by FXD to permit a complete materials characterization

  20. CRL X-ray tube

    International Nuclear Information System (INIS)

    Kolchevsky, N.N.; Petrov, P.V.

    2015-01-01

    A novel types of X-ray tubes with refractive lenses are proposed. CRL-R X-ray tube consists of Compound Refractive Lens- CRL and Reflection X-ray tube. CRL acts as X-ray window. CRL-T X-ray consists of CRL and Transmission X-ray tube. CRL acts as target for electron beam. CRL refractive lens acts as filter, collimator, waveguide and focusing lens. Properties and construction of the CRL X-ray tube are discussed. (authors)

  1. CRL X-RAY TUBE

    OpenAIRE

    Kolchevsky, N. N.; Petrov, P. V.

    2015-01-01

    A novel types of X-ray tubes with refractive lenses are proposed. CRL-R X-ray tube consists of Compound Refractive Lens- CRL and Reflection X-ray tube. CRL acts as X-ray window. CRL-T X-ray consists of CRL and Transmission X-ray tube. CRL acts as target for electron beam. CRL refractive lens acts as filter, collimator, waveguide and focusing lens. Properties and construction of the CRL X-ray tube are discussed.

  2. X rays and condensed matter

    International Nuclear Information System (INIS)

    Daillant, J.

    1997-01-01

    After a historical review of the discovery and study of X rays, the various interaction processes between X rays and matter are described: Thomson scattering, Compton scattering, X-photon absorption through photoelectric effect, and magnetic scattering. X ray sources such as the European Synchrotron Radiation Facility (ESRF) are described. The various X-ray applications are presented: imagery such as X tomography, X microscopy, phase contrast; X-ray photoelectron spectroscopy and X-ray absorption spectroscopy; X-ray scattering and diffraction techniques

  3. X-ray beam generator

    International Nuclear Information System (INIS)

    Koller, T.J.; Randmer, J.A.

    1977-01-01

    A method of minimizing the preferential angular absorption of the divergent beam from an X-ray generator is described. The generator consists of an X-ray shielded housing with an X-ray transmissive window symmetrically placed in radial alignment with a focal spot area on a sloped target surface of an X-ray tube in the housing. The X-ray tube may be of the stationary anode type or of the rotating anode type. (U.K.)

  4. Chest X-Ray

    Medline Plus

    Full Text Available ... Test/Treatment Patient Type Screening/Wellness Disease/Condition Safety En Español More Info Images/Videos About Us ... to consider the likelihood of benefit to your health. While a chest x-ray use a tiny ...

  5. Small Angle Scattering for Pharmaceutical Applications: From Drugs to Drug Delivery Systems.

    Science.gov (United States)

    Alford, Aaron; Kozlovskaya, Veronika; Kharlampieva, Eugenia

    2017-01-01

    The sub-nanometer scale provided by small angle neutron and X-ray scattering is of special importance to pharmaceutical and biomedical investigators. As drug delivery devices become more functionalized and continue decreasing in size, the ability to elucidate details on size scales smaller than those available from optical techniques becomes extremely pertinent. Information gathered from small angle scattering therefore aids the endeavor of optimizing pharmaceutical efficacy at its most fundamental level. This chapter will provide some relevant examples of drug carrier technology and how small angle scattering (SAS) can be used to solve their mysteries. An emphasis on common first-step data treatments is provided which should help clarify the contents of scattering data to new researchers. Specific examples of pharmaceutically relevant research on novel systems and the role SAS plays in these studies will be discussed. This chapter provides an overview of the current applications of SAS in drug research and some practical considerations for selecting scattering techniques.

  6. Modelling small-angle scattering data from complex protein-lipid systems

    DEFF Research Database (Denmark)

    Kynde, Søren Andreas Røssell

    the techniques very well suited for the study of the nanodisc system. Chapter 3 explains two different modelling approaches that can be used in the analysis of small-angle scattering data from lipid-protein complexes. These are the continuous approach where the system of interest is modelled as a few regular...... are particularly interesting to study because they are common targets for pharmaceutical drugs. At the same time they are unfortunately unstable in solution which make them challenging to study. Phospholipid nanodiscs are small patches of lipid membrane stabilised by a belt of amphipathic helices. They can act...... as carriers of membrane proteins. Together they form monodisperse soluble aggregates of about 10 nm in size. Chapter 2 introduces the method of small-angle scattering. Small-angle X-ray and neutron scattering are well suited for studying particles in solution on length scales from 1 to 100 nm. This makes...

  7. 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.

  8. 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

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

    Directory of Open Access Journals (Sweden)

    Emmanuel Kentzinger

    2016-03-01

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

  10. X-ray filter for x-ray powder diffraction

    Science.gov (United States)

    Sinsheimer, John Jay; Conley, Raymond P.; Bouet, Nathalie C. D.; Dooryhee, Eric; Ghose, Sanjit

    2018-01-23

    Technologies are described for apparatus, methods and systems effective for filtering. The filters may comprise a first plate. The first plate may include an x-ray absorbing material and walls defining first slits. The first slits may include arc shaped openings through the first plate. The walls of the first plate may be configured to absorb at least some of first x-rays when the first x-rays are incident on the x-ray absorbing material, and to output second x-rays. The filters may comprise a second plate spaced from the first plate. The second plate may include the x-ray absorbing material and walls defining second slits. The second slits may include arc shaped openings through the second plate. The walls of the second plate may be configured to absorb at least some of second x-rays and to output third x-rays.

  11. Experimental technique of small angle neutron scattering

    International Nuclear Information System (INIS)

    Xia Qingzhong; Chen Bo

    2006-03-01

    The main parts of Small Angle Neutron Scattering (SANS) spectrometer, and their function and different parameters are introduced from experimental aspect. Detailed information is also introduced for SANS spectrometer 'Membrana-2'. Based on practical experiments, the fundamental requirements and working condition for SANS experiments, including sample preparation, detector calibration, standard sample selection and data preliminary process are described. (authors)

  12. Small Angle Light Scattering by Biological Objects

    International Nuclear Information System (INIS)

    Berdzenishvili, L.; Melikishvili, Z.

    2005-01-01

    In this paper the small angle laser radiation scattering by the particles of different shape and size is analyzed. Experimental results and theoretical calculations show that after ejection from bacteriophage DNA forms the scattering medium consisted of quasi-spherical elements with radius of R⁓10λ 0 . (author)

  13. A small angle neutron scattering study

    Indian Academy of Sciences (India)

    Nanocrystalline nickel oxide powders were calcined at 300, 600 and 900°C and pore structure evolution was followed by small angle neutron scattering (SANS). Pore size distributions at two widely separated size ranges have been revealed. Shrinkage of larger-sized pore with reduction in polydispersity has been observed ...

  14. SANS-1: Small angle neutron scattering

    Directory of Open Access Journals (Sweden)

    André Heinemann

    2015-08-01

    Full Text Available The new small angle scattering instrument SANS-1, jointly operated by the Technische Universität München and GEMS, Helmholtz-Zentrum Geesthacht, has completed commissioning and is in regular user service (Gilles et al., 2006. SANS-1 is located at the end of neutron guide NL4a in the Neutron Guide Hall West.

  15. SANS-1: Small angle neutron scattering

    OpenAIRE

    Heinemann, André; Mühlbauer, Sebastian

    2015-01-01

    The new small angle scattering instrument SANS-1, jointly operated by the Technische Universität München and GEMS, Helmholtz-Zentrum Geesthacht, has completed commissioning and is in regular user service (Gilles et al., 2006). SANS-1 is located at the end of neutron guide NL4a in the Neutron Guide Hall West.

  16. A small-angle neutron scattering investigation

    Indian Academy of Sciences (India)

    Hence, the steel is used in aircraft, nuclear reactor, petrochemical plants and many other industries. However, presence of carbide formers such as Mo and Cr war- rants the possibility of carbide precipitates in the structure and in turn affects the mechanical properties. Small-angle neutron scattering (SANS) is an important ...

  17. Structural study of polymers under stretch using a new X-ray TV detector

    International Nuclear Information System (INIS)

    Ohishi, Yasuo; Uemura, Akio; Amemiya, Yoshiyuki.

    1994-01-01

    Time-resolved synchrotron radiation small angle X-ray scattering experiment to investigate the structural change of polyethylene during stretching have been made by utilizing a new X-ray TV detector installed at the Photon Factory. This X-ray TV detector specially developed for real-time measurements of diffraction patterns employs an X-ray image intensifier with a Be-window of a 150 mm diameter. The TV detector has a sensitivity and a time resolution of 30 frames per second. This capability allows us to observe weak SAXS patterns in a time-resolved mode. (author)

  18. X-ray refractometer

    International Nuclear Information System (INIS)

    Tur'yanskij, A.G.; Pirshin, I.V.

    2001-01-01

    Paper introduces a new circuit of X-ray refractometer to study angular and spectral features of refracted radiation within hard X-ray range. Refractometer incorporates two goniometers, two crystal-analyzers and three radiation detectors. The maximum distance between radiation source focal point and a receiving slit of the second goniometer is equal to 1.4 m. For the first time one obtained refraction patterns of fine-film specimens including C/Si stressed structure. Paper describes a new technique of refractometry via specimen oscillation at fixed position of a detecting device. Paper presents the measurement results of oscillation refraction patterns for specimens of melted quartz and ZnSe single crystal [ru

  19. X-ray microtomography

    International Nuclear Information System (INIS)

    Dunsmuir, J.H.; Ferguson, S.R.; D'Amico, K.L.; Stokes, J.P.

    1991-01-01

    In this paper the authors describe the application of a new high-resolution X-ray tomographic microscope to the study of porous media. The microscope was designed to exploit the properties of a synchrotron X-ray source to perform three dimensional tomography on millimeter sized objects with micron resolution and has been used in materials science studies with both synchrotron and conventional and synchrotron sources will be compared. In this work the authors have applied the microscope to measure the three dimensional structure of fused bead packs and berea sandstones with micron resolution and have performed preliminary studies of flow in these media with the microscope operated in a digital subtraction radiography mode. Computer graphics techniques have been applied to the data to visually display the structure of the pore body system. Tomographic imaging after flow experiments should detect the structure of the oil-water interface in the pore network and this work is ongoing

  20. X-ray Ordinance

    International Nuclear Information System (INIS)

    Kramer, R.; Zerlett, G.

    1983-01-01

    This commentary, presented as volume 2 of the Deutsches Strahlenschutzrecht (German legislation on radiation protection) deals with the legal provisions of the ordinance on the protection against harmful effects of X-radiation (X-ray Ordinance - RoeV), of March 1, 1973 (announced in BGBl.I, page 173), as amended by the ordinance on the protection against harmful effects of ionizing radiation, of October 13, 1976 (announced in BGBl. I, page 2905). Thus volume 2 completes the task started with volume 1, namely to present a comprehensive view and account of the body of laws governing radiation protection, a task which was thought useful as developments in the FRG led to regulations being split up into the X-ray Ordinance, and the Radiation Protection Ordinance. In order to present a well-balanced commentary on the X-ray Ordinance, it was necessary to discuss the provisions both from the legal and the medical point of view. This edition takes into account the Fourth Public Notice of the BMA (Fed. Min. of Labour and Social Affairs) concerning the implementation of the X-ray Ordinance of January 4, 1982, as well as court decisions and literature published in this field, until September 1982. In addition, the judgment of the Federal Constitutional Court, dated October 19, 1982, concerning the voidness of the law on government liability, and two decisions by the Federal High Court, dated November 23, 1982, concerning the right to have insight into medical reports - of great significance in practice - have been considered. This commentary therefore is up to date with current developments. (orig.) [de

  1. X-ray diffraction

    International Nuclear Information System (INIS)

    Einstein, J.R.; Wei, C.H.

    1982-01-01

    We have been interested in structural elucidation by x-ray diffraction of compounds of biological interest. Understanding exactly how atoms are arranged in three-dimensional arrays as molecules can help explain the relationship between structure and functions. The species investigated may vary in size and shape; our recent studies included such diverse substances as antischistosomal drugs, a complex of cadmium with nucleic acid base, nitrate salts of adenine, and proteins

  2. X-ray apparatus

    International Nuclear Information System (INIS)

    Tomita, Chuji.

    1980-01-01

    A principal object of the present invention is to provide an X-ray apparatus which is such that the distance between the surface of the patient's table and the floor on which the apparatus is installed is sufficiently small in the horizontal position of the patient's table of the roentgenographical pedestal and that the rotation of the pedestal from the horizontal position to a tilted position and further to the vertical position of the table can be carried out smoothly. (auth)

  3. Producing x-rays

    International Nuclear Information System (INIS)

    Mallozzi, P.J.; Epstein, H.M.; Jung, R.G.; Applebaum, D.C.; Fairand, B.P.; Gallagher, W.J.

    1977-01-01

    A method of producing x-rays by directing radiant energy from a laser onto a target is described. Conversion efficiency of at least about 3 percent is obtained by providing the radiant energy in a low-power precursor pulse of approximately uniform effective intensity focused onto the surface of the target for about 1 to 30 nanoseconds so as to generate an expanding unconfined coronal plasma having less than normal solid density throughout and comprising a low-density (underdense) region wherein the plasma frequency is less than the laser radiation frequency and a higher-density (overdense) region wherein the plasma frequency is greater than the laser radiation frequency and, about 1 to 30 nanoseconds after the precursor pulse strikes the target, a higher-power main pulse focused onto the plasma for about 10 -3 to 30 nanoseconds and having such power density and total energy that the radiant energy is absorbed in the underdense region and conducted into the overdense region to heat it and thus to produce x-rays therefrom with the plasma remaining substantially below normal solid density and thus facilitating the substantial emission of x-rays in the form of spectral lines arising from nonequilibrium ionization states

  4. Ultrafast x-ray scattering on nanoparticle dynamics

    International Nuclear Information System (INIS)

    Plech, A; Ibrahimkutty, S; Issenmann, D; Kotaidis, V; Siems, A

    2013-01-01

    Pulsed X-ray scattering is used for the determination of structural dynamics of laser-irradiated gold particles. By combining several scattering methods such as powder scattering, small angle scattering and diffuse wide angle scattering it is possible to reconstruct the kinetics of structure evolution on several lengths scales and derive complementary information on the particles and their local environment. A generic structural phase diagram for the reaction as function of delay time after laser excitation and laser fluence can be constructed.

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

    Science.gov (United States)

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

    2018-03-12

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

  6. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... position possible that still ensures x-ray image quality. top of page Who interprets the results and ...

  7. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... tissue shows up in shades of gray and air appears black. Until recently, x-ray images were ... position possible that still ensures x-ray image quality. top of page Who interprets the results and ...

  8. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Videos About Us News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x- ... x-ray machine is a compact apparatus that can be taken to the patient in a hospital ...

  9. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... shades of gray and air appears black. Until recently, x-ray images were maintained on large film ... assist you in finding the most comfortable position possible that still ensures x-ray image quality. top ...

  10. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... position possible that still ensures x-ray image quality. top of page Who interprets the results and ... ray examination. X-rays usually have no side effects in the typical diagnostic range for this exam. ...

  11. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... the body. X-rays are the oldest and most frequently used form of medical imaging. A bone ... bones. top of page How should I prepare? Most bone x-rays require no special preparation. You ...

  12. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... can be taken to the patient in a hospital bed or the emergency room. The x-ray ... position possible that still ensures x-ray image quality. top of page Who interprets the results and ...

  13. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... wrist, arm, elbow, shoulder, spine, pelvis, hip, thigh, knee, leg (shin), ankle or foot. top of page ... the patient standing upright, as in cases of knee x-rays. A portable x-ray machine is ...

  14. X-ray detector array

    International Nuclear Information System (INIS)

    Houston, J.M.

    1980-01-01

    The object of the invention (an ionization chamber X-ray detector array for use with high speed computerised tomographic imaging apparatus) is to reduce the time required to produce a tomographic image. The detector array described determines the distribution of X-ray intensities in one or more flat, coplanar X-ray beams. It comprises three flat anode sheets parallel to the X-ray beam, a plurality of rod-like cathodes between the anodes, a detector gas between the electrodes and a means for applying a potential between the electrodes. Each of the X-ray sources is collimated to give a narrow, planar section of X-ray photons. Sets of X-ray sources in the array are pulsed simultaneously to obtain X-ray transmission data for tomographic image reconstruction. (U.K.)

  15. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... evaluation. National and international radiology protection organizations continually review and update the technique standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose ...

  16. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... patient. top of page How does the procedure work? X-rays are a form of radiation like ... Safety page for more information about radiation dose. Women should always inform their physician or x-ray ...

  17. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... image on photographic film or a special detector. Different parts of the body absorb the x-rays ... process is repeated. Two or three images (from different angles) will typically be taken. An x-ray ...

  18. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose control methods to minimize stray (scatter) radiation. This ensures ...

  19. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... up in shades of gray and air appears black. Until recently, x-ray images were maintained on ... Safety page for more information about radiation dose. Women should always inform their physician or x-ray ...

  20. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... tissues around or in bones. top of page How should I prepare? Most bone x-rays require ... is placed beneath the patient. top of page How does the procedure work? X-rays are a ...