WorldWideScience

Sample records for angle x-ray studies

  1. X-ray absorption spectroscopy and small-angle x-ray scattering studies of metal nanoparticles using synchrotron radiation

    International Nuclear Information System (INIS)

    The synchrotron-radiation-based techniques of x-ray absorption spectroscopy and small-angle x-ray scattering are ideally suited to the characterisation of nanoparticles. Their combined application to study the structural and vibrational properties of elemental metal nanoparticles embedded in silica is described here

  2. 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)

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

    International Nuclear Information System (INIS)

    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. (

  4. Precipitation study in thin layers by grazing small-angle scattering of X-rays

    OpenAIRE

    Slimani, T.; Thoft, N.; Naudon, A.

    1993-01-01

    Studies of thin layer by small-angle scattering of X-rays in the transmission mode give weak intensities because the X-ray path is short. Grazing-incidence X-ray scattering circumvents this difficulty for the analysis of a thin layer deposited on a substrate. Furthermore, for a bulk sample, grazing incidence is the only way to study the surface layer, and the penetration depth can be controlled by the incidence angle of the X-ray beam. In this study, we report on krypton and xenon bubbles whi...

  5. Feasibility Study on Anomalous Small-Angle X-ray Scattering near Sulphur K-edge

    International Nuclear Information System (INIS)

    Anomalous small-angle X-ray scattering (ASAXS) is expected to be a powerful and vital tool for the structural study of soft matter. We investigated feasibility of ASAXS near sulphur K absorption edge at SPring-8. Scattering pattern was successfully obtained and the dependence of scattering intensity on the energy of X-ray well agreed with the calculated one. This study can be the basis of structural study of soft matter using ASAXS, especially non-crystalline/amorphous materials.

  6. Small-angle scattering studies of meso-scopic structures with synchrotron X-rays

    Science.gov (United States)

    Dore, J. C.; North, A. N.; Rigden, J. S.

    1995-03-01

    The use of small-angle X-ray scattering techniques for the study of spatial inhomogeneities over the range 20 Å to 2 μm is reviewed. The basic formalism for scattering by an inhomogeneous medium is developed with particular reference to liquid suspensions, porous solids and solid aggregates. The instrumentation available on the Synchrotron Radiation Source at the Daresbury Laboratory is briefly presented and the use of the Bonse-Hart method for studies at ultra-low scattering angles described. The extraction of structural information for a range of natural and synthetic materials is presented with particular reference to microemulsions, porous silicas, clays and composites. The complementarity of X-ray and neutron techniques is critically reviewed and prospects for future developments, particularly for the study of anisotropic systems, are discussed.

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

    International Nuclear Information System (INIS)

    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)

  8. 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.

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

    International Nuclear Information System (INIS)

    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

    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.

  11. Neighborite Under High Pressure: In Situ Angle Dispersive X-ray Diffraction Study Using Synchrotron Radiation

    Science.gov (United States)

    Liu, H.; Chen, J.; Weidner, D.; Hu, J.; Meng, Y.; Mao, H.

    2003-12-01

    The neighborite (NaMgF3) is an ideal analogue model for silicate perovskite (MgSiO3) due to the similarities between their crystal and electronic structures. The advantage of the analogue study is that the weaker bonding feature of neighborite grants us the opportunity to simulate behavior of silicate perovskite at lower mantlei. e.high pressure and high temperature condition, at relatively lower P-T conditions. The previous high pressure studies for neighborite were reported by Zhao et al [1, 2]. Energy dispersive x-ray diffraction data were achieved within 10GPa and 1000oC, while angle dispersive x-ray diffraction data were obtained only at 4.9GPa and room temperature.More information of atomic position change is required to reveal the role of MgF6 octahedral framework tilting during its phase transition process responding to heating andcompressing. Thus the high-resolution monochromatic x-ray powder diffraction studies on NaMgF3 perovskite at high pressure were carried out using diamond anvil cell at X17C of National Synchrotron Light Source (Brookhaven) and HPCAT of Advance Photon Source (Argonne). The orthorhombic structure keeps stable under pressure up to 30 GPa, and the crystal structure is refined using Rietveld method. The result indicates that tilting angle of the MgF6 octahedral framework increases continually while the octahedral Mg-F bond length decreases slightly with increasing pressure.Difference between the tilting angles derived from macro-structure (lattice parameters) and from micro-structure (atomic positions), as well as the trend of change in the tilting angle with temperature and pressureare discussed. [1]. Zhao YS, Weidner DJ, Ko JD, Leinenweber K, Liu X, Li BS, Meng Y,Pacalo REG, Vaughan MT, Wang YB, Yeganehhaeri A,J.Geophys. Res. Solid Earth, 99 (1994) 2871. [2]. Zhao YS, Parise JB, Wang YB, Kusaba K, Vaughan MT, Weidner DJ, Kikegawa T, Chen J, Shimomura O,Am.Miner., 79 (1994) 615.

  12. Colloidal crystallite suspensions studied by high pressure small angle x-ray scattering

    Science.gov (United States)

    Schroer, M. A.; Westermeier, F.; Lehmkühler, F.; Conrad, H.; Schavkan, A.; Zozulya, A. V.; Fischer, B.; Roseker, W.; Sprung, M.; Gutt, C.; Grübel, G.

    2016-02-01

    We report on high pressure small angle x-ray scattering on suspensions of colloidal crystallites in water. The crystallites made out of charge-stabilized poly-acrylate particles exhibit a complex pressure dependence which is based on the specific pressure properties of the suspending medium water. The dominant effect is a compression of the crystallites caused by the compression of the water. In addition, we find indications that also the electrostatic properties of the system, i.e. the particle charge and the dissociation of ions, might play a role for the pressure dependence of the samples. The data further suggest that crystallites in a metastable state induced by shear-induced melting can relax to a similar structural state upon the application of pressure and dilution with water. X-ray cross correlation analysis of the two-dimensional scattering patterns indicates a pressure-dependent increase of the orientational order of the crystallites correlated with growth of these in the suspension. This study underlines the potential of pressure as a very relevant parameter to understand colloidal crystallite systems in aqueous suspension.

  13. Small angle X-ray scattering study of oxygen precipitation in silicon

    International Nuclear Information System (INIS)

    Czochralski-grown dislocation-free silicon is used in the semiconductor industry almost exclusively for manufacturing VLSI devices. Such material contains small quantities (∼20 ppm) of dissolved oxygen, which can have a crucial effect on the properties of produced devices. Therefore it is of great importance to study its precipitation in a silicon matrix after given thermal treatment. The small angle X-ray scattering (SAXS) technique was used to study oxygen precipitation in monocrystalline silicon samples. We used 8 and 16 keV radiation to overcome the high absorption at low energies. A series of samples has been prepared with controlled sequence of oxygen nucleation and precipitation phase and measured with SAXS. It is shown that this low contrast changes in standard wafers can be investigated using synchrotron radiation

  14. Small angle neutron/x-ray scattering study of microtubules and polycations

    International Nuclear Information System (INIS)

    Microtubules (MTs) are hollow cylindrical protein nanotubes with 25 nm diameter, composed of α/β-tubulin heterodimers with surface charge density ~ e/nm2. They are involved in many cellular functions such as cell division, maintaining cell shape, and intracellular trafficking. There have been studies about higher-order assemblies of MTs (e.g. Hexagonal bundle of MTs, inverted tubulin tubes, etc) in the presence of multivalent cations (e.g. Ca2+, spermine, etc). We show our recent findings on the assembly structures of MTs and cationic polymers, which have different structures as the concentration of the polycations changes. Various assemblies are studied both in real and reciprocal spaces using small angle Neutron/X-ray scattering and transmission electron microscopy.

  15. Small angle x ray scattering studies of aggregation in supercritical fluid solutions

    Science.gov (United States)

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

    1994-10-01

    Small-angle x ray scattering (SAXS) can be used to derive structural information on molecular aggregates having sizes from 2 to 200 nm. Not only is the technique useful for probing fluid structure in pure and simple binary supercritical fluid systems, but the technique is also well suited to investigate a range of much more complex multi-molecular aggregates that form when surfactants are added to supercritical fluids. The authors describe the experimental apparatus that was constructed for these studies and the experimental approach used to collect the scattering data. They present scattering results for pure fluids and for fluids containing various types of microemulsion phases, including reverse micelle and normal micelle phases. These results demonstrate that SAXS is a powerful technique for probing various types of molecular aggregation in supercritical fluid solutions.

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

    International Nuclear Information System (INIS)

    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

  17. Study of human blood and hemocomponents irradiated by low angle x ray scattering (LAXS)

    International Nuclear Information System (INIS)

    Irradiation of blood and blood components is currently practiced in developed and in a few developing countries. The main purpose of this process is the prevention of graft versus host disease in immunodeficient patients. The Food and Drug Administration recommends a dose range of 15 Gy to 25 Gy for these blood components. When x-ray photons are scattered from biological samples, their angular distribution shows one or more peaks in the forward direction of scattering. These peaks are characteristic for the investigated samples. Due to its wide range of biological and medical applications, low-angle x-ray scattering has attracted the attention of many authors. Thus in this present work was studied the possible variations in scattering profiles due to the irradiation when the gender of patients was considered. Fresh blood specimens were obtained from volunteers using vacutainer tubes containing EDTA, at the Dr. Eliel Figueiredo Laboratory, Rio de Janeiro. All the samples were lyophilized for 48 hours in a freeze drier in order to remove the water. The scattering measurements were carried out in e-2e reflection geometry using a powder diffractometer Shimadzu XRD- 6000. The measured characterization parameters for LAXS were associated with epidemiological data (gender). The mean values of the different parameters were compared using the Students's t-test for each characterization parameters. The scattering profiles from plasma and formed elements are characterized by the presence of two peaks in the forward direction of scattering. For epidemiological data (gender) analyzed was not found significant changes in the mostly of characterization parameters (p>0.05). (author)

  18. Study of human blood and hemocomponents irradiated by low angle x ray scattering (LAXS)

    Energy Technology Data Exchange (ETDEWEB)

    Pinto, Nivia G. Villela; Barroso, Regina C. [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Inst. de Fisica. Dept. de Fisica Aplicada e Termodinamica], e-mail: nitatag@gmail.com; Mota, Carla L.S.; Almeida, Andre P.; Azeredo, Soraia R.; Braz, Delson [Coordenacao dos Programas de Pos-graduacao em Engenharia (COPPE/UFRJ), RJ (Brazil). Lab. de Instrumentacao Nuclear], e-mail: delson@lin.ufrj.br

    2009-07-01

    Irradiation of blood and blood components is currently practiced in developed and in a few developing countries. The main purpose of this process is the prevention of graft versus host disease in immunodeficient patients. The Food and Drug Administration recommends a dose range of 15 Gy to 25 Gy for these blood components. When x-ray photons are scattered from biological samples, their angular distribution shows one or more peaks in the forward direction of scattering. These peaks are characteristic for the investigated samples. Due to its wide range of biological and medical applications, low-angle x-ray scattering has attracted the attention of many authors. Thus in this present work was studied the possible variations in scattering profiles due to the irradiation when the gender of patients was considered. Fresh blood specimens were obtained from volunteers using vacutainer tubes containing EDTA, at the Dr. Eliel Figueiredo Laboratory, Rio de Janeiro. All the samples were lyophilized for 48 hours in a freeze drier in order to remove the water. The scattering measurements were carried out in e-2e reflection geometry using a powder diffractometer Shimadzu XRD- 6000. The measured characterization parameters for LAXS were associated with epidemiological data (gender). The mean values of the different parameters were compared using the Students's t-test for each characterization parameters. The scattering profiles from plasma and formed elements are characterized by the presence of two peaks in the forward direction of scattering. For epidemiological data (gender) analyzed was not found significant changes in the mostly of characterization parameters (p>0.05). (author)

  19. Synaptic vesicles studied by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    The heterogeneous structure of synaptic vesicles isolated from rat brain is investigated considering solution small-angle X-ray scattering data in combination with data obtained by cryogenic electron microscopy, dynamic light scattering and biochemical analysis. Overall low resolution structural models of the entire functional synaptic vesicle are proposed, elucidating details on the density profile of the membrane, including contributions from the lipids and the proteins, as well as addressing the average conformation and overall lateral organization of proteins in micro-domains on the average synaptic vesicle under quasi-physiological conditions. Entropic contributions to free energy due to possible protein cluster formation and disintegration on the synaptic vesicle are investigated. Further, cell free fusion systems are characterized employing dynamic light scattering and applicability of small-angle X-ray scattering is considered for investigating membrane fusion processes.

  20. Location of two antioxidants in oriented model membranes. Small-angle x-ray diffraction study.

    OpenAIRE

    Katsaras, J.; Stinson, R H; Davis, J H; Kendall, E J

    1991-01-01

    Small-angle x-ray diffraction has been applied in locating either butylated hydroxytoluene (BHT) or delta-tocopherol and their brominated analogues at a concentration of 40 mol% in oriented bilayers of dipalmitoylphosphatidylcholine (DPPC) or DPPC + 15 mol% cholesterol at 20 degrees C. Phases were determined using swelling experiments with structure factors plotted in reciprocal space, creating a relatively smooth curve as the amount of water between the bilayers was changed. Continuous Fouri...

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

    DEFF Research Database (Denmark)

    Stribeck, Norbert; Schneider, Konrad; Zeinolebadi, Ahmad;

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Lingling

    1996-04-01

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

  3. Small angle x-ray scattering study of the porosity in coals

    Science.gov (United States)

    Schmidt, P. W.; Kalliat, M.; Kwak, C. Y.

    1981-02-01

    Small-angle scattering curves have bee obtained for some Pennsylvania State University PSOC coal samples and for several other coals. The x-ray scattering data provide information about the porosity in the coals and suggest that there are three classes of pores, which have average dimensions of the order of 1000 A˚, 30 A˚, and less than 5 A˚, corresponding to the macropores, transition pores and micropores discussed by Dubinin. The principal factor determining the form of the scattering curves has been found to be the rank of the coal. In coals of all ranks, the specific surface associated with the macropores is about 1 to 10 m2/gm. The micropores are most highly developed in high-rank coals. Comparison of the x-ray and adsorption results suggests that x-ray scattering and nitrogen adsorption detect only the specific surface of the macropores and transition pores, while carbon dioxide adsorption measures the total porosity from the micropores. Scattering data have also been recorded for a series of coals which had been tested for their suitability for conversion to liquid fuels. All the coals which were well-suited for producing liquid fuels were found to have a well-developed transition pore structure, while coals which were not especially good for coal liquefaction processes had almost no transition pores.

  4. New reactor dedicated to in operando studies of model catalysts by means of surface x-ray diffraction and grazing incidence small angle x-ray scattering

    International Nuclear Information System (INIS)

    A new experimental setup has been developed to enable in situ studies of catalyst surfaces during chemical reactions by means of surface x-ray diffraction (SXRD) and grazing incidence small angle x-ray scattering. The x-ray reactor chamber was designed for both ultrahigh-vacuum (UHV) and reactive gas environments. A laser beam heating of the sample was implemented; the sample temperature reaches 1100 K in UHV and 600 K in the presence of reactive gases. The reactor equipment allows dynamical observations of the surface with various, perfectly mixed gases at controlled partial pressures. It can run in two modes: as a bath reactor in the pressure range of 1-1000 mbars and as a continuous flow cell for pressure lower than 10-3 mbar. The reactor is connected to an UHV preparation chamber also equipped with low energy electron diffraction and Auger spectroscopy. This setup is thus perfectly well suited to extend in situ studies to more complex surfaces, such as epitaxial films or supported nanoparticles. It offers the possibility to follow the chemically induced changes of the morphology, the structure, the composition, and growth processes of the model catalyst surface during exposure to reactive gases. As an example the Pd8Ni92(110) surface structure was followed by SXRD under a few millibars of hydrogen and during butadiene hydrogenation while the reaction was monitored by quadrupole mass spectrometry. This experiment evidenced the great sensitivity of the diffracted intensity to the subtle interaction between the surface atoms and the gas molecules

  5. Small angle neutron scattering and small angle X-ray scattering studies of platinum-loaded carbon foams

    Indian Academy of Sciences (India)

    P U Sastry; V K Aswal; A G Wagh

    2008-11-01

    The morphology of carbon nanofoam samples comprising platinum nanoparticles 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 and the average radius of the platinum particles is about 2.5 nm. The fractal dimension as well as the size distribution parameters of platinum particles varies markedly with the platinum content and annealing temperature. Transmission electron micrographs of the samples corroborate the SANS and SAXS results.

  6. Radiation embrittlement studies using anomalous small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Anomalous small angle x-ray scattering (ASAXS) was performed on an Fe-O.9 wt.% Cu-1.0 wt.% Mn alloy subjected to annealing or electron irradiation. ASAXS takes advantage of natural variations in the atomic scattering factor which exist at energies very near an element's x-ray absorption edge. By performing systematic SAXS experiments at energies near these absorption edges of the constituent alloy elements it is possible to vary the contrast of scattering centers containing the elements and in doing so quantify scatterer composition. The results of such an analysis for the samples in this work indicate the presence of Cu-rich, Cu85Mn15 precipitates in the alloy. By applying the maximum entropy technique to the scattering data, it was possible to extract size distributions of scattering centers fog the different treatments. The results demonstrate the ability to detect and characterize small (11 A radius) scatterers at quite low irradiation damage levels (5x10-4 displacements per atom)

  7. Radiation embrittlement studies using anomalous small-angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Alexander, D. E.; Kestel, B. J.; Seifert, S.; Jemian, P. R.; Odette, G. R.; Klingensmith, D.; Gragg, D.

    1999-12-06

    Anomalous small angle x-ray scattering (ASAXS) was performed on an Fe-O.9 wt.% Cu-1.0 wt.% Mn alloy subjected to annealing or electron irradiation. ASAXS takes advantage of natural variations in the atomic scattering factor which exist at energies very near an element's x-ray absorption edge. By performing systematic SAXS experiments at energies near these absorption edges of the constituent alloy elements it is possible to vary the contrast of scattering centers containing the elements and in doing so quantify scatterer composition. The results of such an analysis for the samples in this work indicate the presence of Cu-rich, Cu{sub 85}Mn{sub 15} precipitates in the alloy. By applying the maximum entropy technique to the scattering data, it was possible to extract size distributions of scattering centers fog the different treatments. The results demonstrate the ability to detect and characterize small (11 {angstrom} radius) scatterers at quite low irradiation damage levels (5x10{sup {minus} 4} displacements per atom).

  8. DMSO-Induced Dehydration of DPPC Membranes Studied by X-ray Diffraction, Small-Angle Neutron Scattering, and Calorimetry

    OpenAIRE

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

    2001-01-01

    The influence of dimethyl sulfoxide (DMSO) on membrane thickness, multilamellar repeat distance, and phase transitions of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC) was investigated by X-ray diffraction and small-angle neutron scattering (SANS). The differential scanning calorimetry (DSC) study of water freezing and ice melting was performed in the ternary DPPC /DMSO /water and binary DMSO /water systems. The methods applied demonstrated the differences in membrane structure in t...

  9. Spatially-resolved small-angle x-ray scattering studies of soot inception and growth

    International Nuclear Information System (INIS)

    The high spectral brilliance of x-rays produced at the Basic Energy Sciences Synchrotron Radiation Center of Argonne's Advanced Photon Source allows us to perform small-angle x-ray scattering (SAXS) measurements of the distributions of soot particles in flames. SAXS provides an in situ probe of the size and distribution of particles in the region between 1 and 100 nm. Detailed measurements on a propylene/air diffusion flame allow us to extract a spatially dependent background, which occurs in gas-phase combustion systems, and to perform Abel inversions, which provide the radial dependence of the scattering intensity. A bimodal distribution of soot particles is needed to describe our results. The radial behavior of the two modes of this distribution implies that the chemistry and fluid dynamics are strongly coupled in this simple diffusion flame. The larger particles of this distribution correspond to the previously observed primary particles, which have a relatively complex radial dependence. Midway between the fuel source and the widest part of the flame the primary particles have a mean radius of 6 nm or less and their concentration is symmetrically distributed about the flame front. At the widest part of the flame, two distinct distributions of primary particles are observed. Near the center of the flame the particles have a mean radius of 10 nm and a polydispersity of 0.3 and beyond a transition region they have a mean radius of 21 nm and a polydispersity of 0.2. The smaller particles, which require additional experiments before they can be identified, correspond either to soot nuclei, PAH species such as naphthalene, and/or disordered carbons with graphitic basal planes

  10. 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..

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

    Science.gov (United States)

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

    2013-11-01

    The disordered structure of commercially available CXV activated carbon produced from finely powdered wood-based carbon has been studied using the wide-angle x-ray scattering technique, molecular dynamics and density functional theory simulations. The x-ray scattering data has been converted to the real space representation in the form of the pair correlation function via the Fourier transform. Geometry optimizations using classical molecular dynamics based on the reactive empirical bond order potential and density functional theory at the B3LYP/6-31g* level have been performed to generate nanoscale models of CXV carbon consistent with the experimental data. The final model of the structure comprises four chain-like and buckled graphitic layers containing a small percentage of four-fold coordinated atoms (sp3 defects) in each layer. The presence of non-hexagonal rings in the atomic arrangement has been also considered.

  12. Angle-dependent hard X-ray photoemission study of Nb hydride formation in high-pressure supercritical water

    Energy Technology Data Exchange (ETDEWEB)

    Soda, Kazuo, E-mail: j45880a@cc.nagoya-u.ac.jp [Department of Quantum Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8603 (Japan); Kondo, Hiroki; Yamaguchi, Kanta; Kato, Masahiko [Department of Quantum Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8603 (Japan); Shiraki, Tatsuhito; Niwa, Ken; Kusaba, Keiji; Hasegawa, Masashi [Department of Crystalline Materials Science, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8603 (Japan); Xeniya, Kozina; Ikenaga, Eiji [Japan Synchrotron Radiation Research Institute, 1-1-1, Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198 (Japan)

    2015-09-15

    Highlights: • Nb hydrides in 10-GPa supercritical water are studied by photoelectron spectroscopy. • The hydride components of the Nb 3d core-level spectra are increased with the depth. • The bulk valence-band spectrum shows a split band due to the Nb–H bond formation. • The hydrides are formed in the bulk and their surfaces are covered with Nb oxides. - Abstract: Nb hydrides formation in 10-GPa supercritical water has been investigated by angle-dependent micro-beam hard X-ray photoemission spectroscopy. In the Nb 3d core-level spectra, Nb hydride components are found in the slightly high binding energy side of the metallic components, and the oxide ones are observed even though little oxides are recognized in X-ray diffraction patterns. Obtained emission-angle dependence of the Nb 3d core-level spectra of Nb hydride specimens shows that the Nb hydride components increase with the emission angle decreased i.e. the sampling depth increased, while the oxide ones decrease. The bulk valence-band spectrum is obtained by decomposing the measured valence-band spectra into a bulk and surface components with use of the emission-angle dependence of the core-level and valence-band spectra; it consists of two bands. This implies the Nb–H chemical bond formation and Nb in an oxidation state, consistent with reported band structure calculations and the observed core-level chemical shifts. Thus it is confirmed by valence-band and core-level photoelectron spectroscopy that the Nb hydrides are formed inside the specimen, irrespective to the well-known high oxidation ability of supercritical water.

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

    International Nuclear Information System (INIS)

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-01

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

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

    Science.gov (United States)

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

    2007-01-01

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

  16. Small-Angle X-ray Study of the Three-Dimensional Collagen/Mineral Superstructure in Intramuscular Fish Bone

    International Nuclear Information System (INIS)

    Synchrotron small-angle X-ray scattering (SAXS) was conducted on native intramuscular shad/herring bone samples. Two-dimensional SAXS patterns were quantitatively analyzed with special consideration for preferred orientation effects, leading to new insights into the three-dimensional superstructure of mineralized collagen fibrils in shad/herring bone

  17. 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

    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 the...... capable of giving fundamental structural information as well as quantifying the remodelling of structures influenced by environmental factors....

  18. Structure of Carbon Nanotube Porins in Lipid Bilayers: An in Situ Small-Angle X-ray Scattering (SAXS) Study.

    Science.gov (United States)

    Tran, Ich C; Tunuguntla, Ramya H; Kim, Kyunghoon; Lee, Jonathan R I; Willey, Trevor M; Weiss, Thomas M; Noy, Aleksandr; van Buuren, Tony

    2016-07-13

    Carbon nanotube porins (CNTPs), small segments of carbon nanotubes capable of forming defined pores in lipid membranes, are important future components for bionanoelectronic devices as they could provide a robust analog of biological membrane channels. In order to control the incorporation of these CNT channels into lipid bilayers, it is important to understand the structure of the CNTPs before and after insertion into the lipid bilayer as well as the impact of such insertion on the bilayer structure. Here we employed a noninvasive in situ probe, small-angle X-ray scattering, to study the integration of CNT porins into dioleoylphosphatidylcholine bilayers. Our results show that CNTPs in solution are stabilized by a monolayer of lipid molecules wrapped around their outer surface. We also demonstrate that insertion of CNTPs into the lipid bilayer results in decreased bilayer thickness with the magnitude of this effect increasing with the concentration of CNTPs. PMID:27322135

  19. A study of mixtures of nanometer sized Fe and Cu crystallites by anomalous small angle X-ray scattering (ASAXS)

    International Nuclear Information System (INIS)

    Mixtures of Fe crystallites and Cu crystallites with diameters of about 6-14 nm, have been prepared by inert gas condensation and subsequent compaction of the crystallites. Small angle X-ray scattering experiments using synchrotron radiation have been carried out to study the microstructure of the compacts on a nanometer scale. By variation of the atomic scattering factors near the K absorption edge of Fe, partial intensities have been obtained which provide separate information about the environment of the Fe or the Cu atoms, respectively. The partial intensities are interpreted in terms of scattering contributions of particles with different sizes. The resulting size distribution functions not only indicate the presence of Fe and Cu crystallites but also give evidence for correlations between the crystallites. These correlations between Fe and Cu crystals are interpreted in terms of a mixture of the chemically different crystallites on a nanometer scale. (orig.)

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

    International Nuclear Information System (INIS)

    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)

  1. Glancing angle synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    This paper describes in basic detail some of the techniques that can be used to study thin films and surfaces. These are all in the X-ray region and cover reflectivity, diffraction form polycrystalline films, textured films and single crystal films. Other effects such as fluorescence and diffuse scattering are mentioned but not discussed in detail. Two examples of the reflectivity from multilayers and the diffraction from iron oxide films are discussed. The advantages of the synchrotron for these studies is stressed and the experimental geometries that can be employed are described i detail. A brief bibliography is provided at the end to accompany this part of the 1996 Frascati school

  2. Glancing angle synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cernik, R.J. [Daresbury Lab., Warrington, WA (United States)

    1996-09-01

    This paper describes in basic detail some of the techniques that can be used to study thin films and surfaces. These are all in the X-ray region and cover reflectivity, diffraction form polycrystalline films, textured films and single crystal films. Other effects such as fluorescence and diffuse scattering are mentioned but not discussed in detail. Two examples of the reflectivity from multilayers and the diffraction from iron oxide films are discussed. The advantages of the synchrotron for these studies is stressed and the experimental geometries that can be employed are described i detail. A brief bibliography is provided at the end to accompany this part of the 1996 Frascati school.

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

    International Nuclear Information System (INIS)

    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/H2O 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.)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-15

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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

    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

  7. DMSO-Induced Dehydration of DPPC Membranes Studied by X-ray Diffraction, Small-Angle Neutron Scattering, and Calorimetry

    CERN Document Server

    Kiselev, M A; Kisselev, A M; Grabielle-Madelmond, C; Ollivon, M

    1999-01-01

    The influence of dimethyl sulfoxide (DMSO) on membrane thickness, multilamellar repeat distance, and phase transitions of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC) was investigated by X-ray diffraction and small-angle neutron scattering (SANS). The differential scanning calorimetry (DSC) study of water freezing and ice melting was performed in the ternary DPPC /DMSO /water and binary DMSO /water systems. The methods applied demonstrated the differences in membrane structure in three sub-regions of the DMSO mole fraction (X_dmso): from 0.0 to 0.3 for the first, from 0.3 to 0.8 for the second, and from 0.9 to 1.0 for the third sub-region. The thickness of the intermembrane solvent at T =20C decreases from 14.4 +/- 1.8 A at X_dmso =0.0 to 7.8 +/- 1.8 A at X_dmso =0.1. The data were used to determine the number of free water molecules in the intermembrane space in the presence of DMSO. The results for 0.0 < X_dmso < 0.3 were explained in the framework of DMSO-induced dehydration of the interme...

  8. Short-range order in Fe-based metallic glasses: Wide-angle X-ray scattering studies

    International Nuclear Information System (INIS)

    The local atomic structure of the Fe80B20, Fe70Nb10B20 and Fe62Nb8B30 glasses prepared in the form of ribbons has been studied by wide-angle X-ray scattering. Structural information about the amorphous ribbons has been derived from analysis of the radial distribution functions using the least-squares curve-fitting method. The obtained structural parameters indicate that Fe–Fe, Fe–B, Fe–Nb and Nb–B contributions are involved in the near-neighbor coordination spheres. The possible similarities of the local atomic arrangement in the investigated glasses and the crystalline Fe3B, Fe23B6 and bcc Fe structures are also discussed. - Graphical abstract: Pair distribution functions (a) and best-fit model and experimental radial distribution functions for Fe80B20 (b), Fe70Nb10B20 (c) and Fe62Nb8B30 (d) metallic glasses. - Highlights: • The short-range ordering in the Fe-based metallic glasses is presented. • The results of RDF function have been analyzed using the least-squares method. • The Fe–Fe, Fe–B, Fe–Nb or Nb–B contributions are involved in coordination spheres. • The structural unit is distorted triangular prism containing B, Fe or Nb atoms. • Similarities of atomic arrangement in glassy and crystalline structures are discussed

  9. Ultrahigh vacuum/high-pressure flow reactor for surface x-ray diffraction and grazing incidence small angle x-ray scattering studies close to conditions for industrial catalysis

    International Nuclear Information System (INIS)

    A versatile instrument for the in situ study of catalyst surfaces by surface x-ray diffraction and grazing incidence small angle x-ray scattering in a 13 ml flow reactor combined with reaction product analysis by mass spectrometry has been developed. The instrument bridges the so-called ''pressure gap'' and ''materials gap'' at the same time, within one experimental setup. It allows for the preparation and study of catalytically active single crystal surfaces and is also equipped with an evaporator for the deposition of thin, pure metal films, necessary for the formation of small metal particles on oxide supports. Reactions can be studied in flow mode and batch mode in a pressure range of 100-1200 mbar and temperatures up to 950 K. The setup provides a unique combination of sample preparation, characterization, and in situ experiments where the structure and reactivity of both single crystals and supported nanoparticles can be simultaneously determined.

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

    International Nuclear Information System (INIS)

    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 stacks. In the NCs the discrete SAXS of arranged crystalline PP domains is limited to a skin zone of 300 μm thickness. Even there only frozen-in primary lamellae are detected. The core of the NCs is dominated by diffuse scattering from crystalline domains placed at random. The SAXS of the MMT flakes exhibits a complex skin–core gradient. Both the direction of the symmetry axis and the apparent perfection of flake-orientation are varying. Thus there is no local fiber symmetry, and the structure gradient cannot be reconstructed from a scan across the full rod. To overcome the problem the rods are machined. Scans across the residual webs are performed. For the first time webs have been carved out in two principal directions. Comparison of the corresponding two sets of SAXS patterns demonstrates the complexity of the MMT orientation. Close to the surface (< 1 mm) the flakes cling to the wall. The variation of the orientation distribution widths indicates the presence of both MMT flakes and grains. The grains have not been oriented in the flowing melt. An empirical equation is presented which describes the variation from skin to core of one component of the inclination angle of flake-shaped phyllosilicate filler particles. (paper)

  11. Anomalous Small-angle X-ray Scattering Study on Aggregation of a Block Copolymer in a Selective Solvent

    International Nuclear Information System (INIS)

    Anomalous small-angle X-ray Scattering (ASAXS) analysis for poly(4-vinylphenol)-b-poly(4-bromostyrene) (PVPh-b-PBrS) in N,N,N',N'-tetramethyl ethylene diamine (TMEDA) solution was examined. The ASAXS measurements, executed at three different energies, provided the separation of the scattering of the Br atoms from whole system. The energy-dependent term in the SAXS profile, which is corresponding to the form factor of PBrS domain, sufficiently agree with the SAXS profile calculated for hard sphere with 41 nm radius. Therefore, the PBrS chains assemble into spherical core with 41 nm radius in TMEDA solution.

  12. Comparative anomalous small-angle X-ray scattering study of hotwire and plasma grown amorphous silicon-germanium alloys

    OpenAIRE

    Goerigk, G.; Williamson, D. L.

    2001-01-01

    The nanostructure of hydrogenated amorphous silicon-germanium alloys, a-Si1-xGex:H, prepared by the hotwire deposition technique (x=0.06-0.79) and by the plasma enhanced chemical vapor deposition technique (x=0 and 0.50) was analyzed by anomalous small-angle x-ray scattering experiments. For all alloys with x >0 the Ge component was found to be inhomogeneously distributed with correlation lengths of about 1 nm. A systematic increase of the separated scattering was found due to the increasing ...

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

    Institute of Scientific and Technical Information of China (English)

    柳义; 陈东风; 王洪立; 陈娜; 李丹; 韩布兴; 荣利霞; 赵辉; 王俊; 董宝中

    2002-01-01

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

  14. Small angle x-ray scattering and electron paramagnetic resonance studies of nucleation and crystallisation in basalt glasses

    International Nuclear Information System (INIS)

    We report here small angle x-ray scattering, wide angle x-ray diffraction, and electron paramagnetic resonance measurements on glasses of the same origin but prepared under various tholeitic basalt redox conditions and melted at 16000C for 16 h. The spatial correlation between growing particles is associated with interference effects observed on the scattering curves. These were completely smoothed out for reduced samples. For crystallisation temperatures of 720, 740, and 7600C the growth stage was around 5, 5, and 1 min respectively. At longer times volume diffusion controlled Ostwald ripening occurs. The resonance spectra at 9 GHz of the oxidised and reduced samples were similar and consisted of isolated paramagnetic Fe3+ with g = 4.26 and a broad asymmetric absorption ΔH (300 K) > 500 G with a peak at g = 2.0. The temperature dependence of the linewidth and intensity in fused samples and samples treated at 6350C were such as would be expected for small (of the order of 100 A) ferrimagnetic particles, and in the spectrum of a sample treated at 635 and 7050C was characteristic of a magnetic phase transition. Ferrimagnetic particles are present in quenched samples and increase in size with thermal treatment, but are not affected by fusion under the oxidising and reducing conditions used in these experiments. (author)

  15. Small-angle X-ray scattering of solutions

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

    Gilbert, James Andrew

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

  18. 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. PMID:22857132

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

    International Nuclear Information System (INIS)

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

  20. 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.

  1. 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.

  2. 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.

  3. In Situ Synchrotron X-Ray Diffraction and Small Angle X-Ray Scattering Studies on Rapidly Heated and Cooled Ti-Al and Al-Cu-Mg Alloys Using Laser-Based Heating

    Science.gov (United States)

    Kenel, C.; Schloth, P.; Van Petegem, S.; Fife, J. L.; Grolimund, D.; Menzel, A.; Van Swygenhoven, H.; Leinenbach, C.

    2016-03-01

    Beam-based additive manufacturing (AM) typically involves high cooling rates in a range of 103-104 K/s. Therefore, new techniques are required to understand the non-equilibrium evolution of materials at appropriate time scales. Most technical alloys have not been optimized for such rapid solidification, and microstructural, phase, and elemental solubility behavior can be very different. In this work, the combination of complementary in situ synchrotron micro-x-ray diffraction (microXRD) and small angle x-ray scattering (SAXS) studies with laser-based heating and rapid cooling is presented as an approach to study alloy behavior under processing conditions similar to AM techniques. In rapidly solidified Ti-48Al, the full solidification and phase transformation sequences are observed using microXRD with high temporal resolution. The high cooling rates are achieved by fast heat extraction. Further, the temperature- and cooling rate-dependent precipitation of sub-nanometer clusters in an Al-Cu-Mg alloy can be studied by SAXS. The sensitivity of SAXS on the length scales of the newly formed phases allows their size and fraction to be determined. These techniques are unique tools to help provide a deeper understanding of underlying alloy behavior and its influence on resulting microstructures and properties after AM. Their availability to materials scientists is crucial for both in-depth investigations of novel alloys and also future production of high-quality parts using AM.

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

    International Nuclear Information System (INIS)

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

  5. Nano-structural study of microfibrils in acacia mangium wood using small- angle x-ray scattering (SAXS)

    International Nuclear Information System (INIS)

    Small-angle X-ray scattering (SAXS) was used to investigate the nanostructure of the microfibrils of cell wall in Acacia Mangium wood. Parameters, such as the fibre length (L), surface area of the single fibre (S), the correspondence distance from the center of the fibre to the center of its neighbor and the shape of the fibre were determined as a function to the distance from pith towards the bark The results indicate that the fibre length ranged from 53.44 mm to 13.72 mm from pith to bark. Surface area of the single fibre varied from 0.65 nm?2 to 4.36 nm?2, the highest being found at the end of bark region. The mean value of the correspondence distance is 13.95 nm. Surface structure analysis from scattering graph showed a rod shape off fibre in the pith region of Acacia Mangium wood. The use of SAXS technique and scanning electron microscope (SEM) micrographs gives the most reliable dimensions values. (Author)

  6. 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

  7. Structure of diglycerol monomyristate reverse micelles in styrene: a small-angle X-ray scattering (SAXS) study.

    Science.gov (United States)

    Shrestha, Lok Kumar; Shrestha, Rekha Goswami; Aramaki, Kenji; Ariga, Katsuhiko

    2011-08-01

    Structure of diglycerol monomyristate (designated as C14G2) nonionic surfactant reverse micelles in aromatic solvent styrene has been investigated as a function of surfactant concentration, temperature, and water addition by using small-angle X-ray scattering (SAXS) technique. Structure of micelles in real-space so called pair-distance distribution function, p(r), was obtained by the generalized indirect fourier transformation (GIFT) evaluation of SAXS data. It was found that C14G2 spontaneously self-assembles into spheroid reverse micelles with maximum diameter approximately 3.0 nm when added into styrene under ambient condition. The micellar shape and size remained essentially the same despite a wide variation in surfactant concentration (5 to 30%) but an opposite trend was observed with the rise of temperature; size decreased by approximately 25% with increase in temperature from 25 to 75 degrees C. Addition of traces water favored micellar growth and eventually ellipsoid prolate type micelles were formed, whose scenario is understood in terms of decrease in the critical packing parameter (cpp); water hydrates the surfactant's headgroup and decreases cpp. At a particular concentration of water, increasing temperature decreased the micellar size due to dehydration of headgroup. It is interesting to note that size of 1.57% water incorporated micelle is approximately 2.5 times bigger than the empty micelles. PMID:22103110

  8. Mass-fractal growth in niobia/silsesquioxane mixtures: a small-angle X-ray scattering study

    Science.gov (United States)

    Besselink, Rogier; ten Elshof, Johan E.

    2014-01-01

    The nucleation and growth of niobium pentaethoxide (NPE)-derived clusters in ethanol, through acid-catalyzed hydrolysis/condensation in the presence and absence of the silsesquioxane 1,2-bis(triethoxysilyl)ethane (BTESE), was monitored at 298–333 K by small-angle X-ray scattering. The data were analyzed with a newly derived model for polydisperse mass-fractal-like structures. At 298–313 K in the absence of BTESE the data indicated the development of relatively monodisperse NPE-derived structures with self-preserving polydispersity during growth. The growth exponent was consistent with irreversible diffusion-limited cluster agglomeration. At 333 K the growth exponent was characteristic for fast-gelling reaction-limited cluster agglomeration. The reaction yielded substantially higher degrees of polydispersity. In the presence of BTESE the growth exponents were substantially smaller. The smaller growth exponent in this case is not consistent with irreversible Smoluchowski-type agglomeration. Instead, reversible Lifshitz–Slyozov-type agglomeration seems to be more consistent with the experimental data. PMID:25294980

  9. ``Ordered'' structure in dilute solutions of sodium polystyrenesulfonates as studied by small-angle x-ray scattering

    Science.gov (United States)

    Ise, Norio; Okubo, Tsuneo; Kunugi, Shigeru; Matsuoka, Hideki; Yamamoto, K.; Ishii, Yasuo

    1984-10-01

    The small angle x-ray scattering measurements were performed for aqueous solutions of sodium polystyrenesulfonates having relatively narrow molecular weight distributions. As was observed for other synthetic macroions, polynucleotide and proteins, a single, broad peak was observed. The scattering vector at the peak position (Sm) was shifted toward larger values with increasing polymer concentration and toward lower values with increasing salt concentration, which confirmed earlier observations with polyacrylate and poly-L-lysine. The molecular weight dependence of the scattering behavior, which was earlier observed, was confirmed to be true for samples with Mw of 74 000, 18 000, and 4600. The mixture of two fractions with different Mw's gave a scattering curve which was again different from the composite curve obtained with the parent curves before mixing. A similar situation was observed for the mixture of polystyrenesulfonate and polyacrylate. Thus, it was concluded that the observed single peak indicates the presence of an intermolecular ordering, not an intramolecular ordering. The intermacroion distance (2Dexp) was thus calculated by using the Bragg equation. 2Dexp decreased with increasing polymer concentration and increased (not decreased) with increasing concentration of added salt and Mw. The 2Dexp values thus obtained were smaller beyond the experimental error than 2D0, a theoretical distance calculated from the concentration by assuming the uniform distribution of the macroions throughout the solution and the 2D0/2Dexp value amounted to 3.5 for high molecular weight samples. This fact indicates the presence of an intermacroion attractive interaction. When two fractions with different Mw's were compared at a given number concentration of macroions, the 2Dexp value for the sample of a larger Mw was smaller than that for the fraction of a smaller Mw. This implies that the attraction must be intensified, though unexpectedly, with increasing valency of the

  10. Low angle X-ray scattering

    International Nuclear Information System (INIS)

    The theoretical and experimental problems appearing in diffraction experiments at very low angles by several kinds of materials are discussed. The importance of synchrotron radiation in such problems is shown. (L.C.)

  11. Small-Angle X-Ray Scattering on the ChemMatCARS Beamline at the Advanced Photon Source: A Study of Shear-Induced Crystallisation in Polypropylene

    Energy Technology Data Exchange (ETDEWEB)

    Sutton, D.; Hanley, T.; Knott, R.; Cookson, D. (CRC); (ANSTO)

    2008-09-08

    The first ever time-resolved small-angle X-ray scattering (SAXS) data from the undulator 15-ID-D beamline (ChemMatCARS) are presented. A 1.3 {angstrom} (9.54 keV) X-ray beam was selected to study the structure development in a polypropylene sample during shear-induced crystallization. A Linkam CSS450 shear cell provided the temperature and shear control. The polypropylene was first melted and then quenched to the crystallization temperature, where a step shear was applied. The SAXS data were collected using a Bruker 6000 CCD detector, which provided images of excellent resolution. The SAXS images (with 180{sup o} rotational symmetry) indicated that the polypropylene crystallizes with a high degree of anisotropy, and the lamellae are oriented perpendicular to the flow direction.

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

    International Nuclear Information System (INIS)

    We present synchrotron-based time-resolved small-angle x-ray scattering (SAXS) measurements of spinodal decomposition in a covalently cross-linked N-isopropylacrylamide gel. The range of wave numbers examined is well beyond the position of the maximum in the structure factor S(q,t). The equilibrium structure factor is described by the sum of a Lorentzian and a Gaussian. Following a temperature jump into the two phase region, the scattered intensity increases with time and eventually saturates. For early times the linear Cahn-Hilliard-Cook (CHC) theory can be used to describe the time evolution of the scattered intensity. From this analysis we found that the growth rate R(q) is linearly dependent on q2, in agreement with mean-field theoretical predictions. However the Onsager transport coefficient Λ(q)∼q-4, which is stronger than the q dependence predicted by the mean-field theory. We found that the growth rate R(q)>0, even though the wave numbers q probed by SAXS are greater than √ (2) qm where qm is the position of the peak of S(q,t), also in agreement with the mean-field predictions for a deep quench. We have also examined the range of validity of the linear CHC theory, and found that its breakdown occurs earlier at higher wave numbers. At later times, a pinning of the structure was observed. The relaxation to a final, microphase-separated morphology is faster and occurs earlier at the highest wave numbers, which probe length scales comparable to the average distance between crosslinks. copyright 1999 The American Physical Society

  13. Small-angle X-ray scattering study of the growth kinetics of CuCl nanocrystals in NaCl

    OpenAIRE

    Kranold, R.; Kriesen, S.; Haselhoff, M.; Weber, H.-J.; Goerigk, G.

    2003-01-01

    The precipitation of CuCl nanocrystals in a NaCl matrix has been studied by time-resolved small-angle X-ray scattering. The experimental results suggest that the nucleation process is accelerated by lattice defects of the matrix remaining in the NaCl lattice after the dissolution of previous nanocrystals at high temperature. The evolution of structural parameters calculated from the scattering curves, such as volume fraction, mean radius and particle number density of the nanocrystals, is dis...

  14. Small-angle x-ray scattering and differential scanning calorimetry studies of DPPC multilamellar structures containing membranotropic agents of different chemical nature

    International Nuclear Information System (INIS)

    Multilamellar structures formed in DPPC/water/glycerol and DPPC/water/oxyethylated glycerol systems are studied by small-angle X-ray scattering (SAXS) and differential scanning calorimetry (DSC) methods. The effects of glycerol, oxyethylated glycerol, and other membranotropic agents (MTAs) on the lamellar repeat distance D are compared in gel, ripple, and high-temperature (Lα) liquid crystal phases of the hydrated phospholipids. It is noted that the introduction of MTAs could lead to different types of 'D vs. temperature' behavior in the Lα phase, which is correlated with changes in D caused by the introduction of these substances to the DPPC/water reference system

  15. Small Angle X-ray Scattering Study of Palladium Nanoparticle Growth on Genetically Engineered Tobacco Mosaic Virus Nanotemplates

    Science.gov (United States)

    Manocchi, Amy K.

    Transition metal nanoparticles possess valuable specific size dependent properties that arise at the nanoscale, and differ significantly from their bulk properties. However, the fabrication of these nanoparticles is often difficult to predict and control due to harsh reaction conditions and effects of capping agents or surfactants. Therefore, there is a critical need for facile routes toward controllable nanoparticle fabrication. Biological supramolecules, such as viruses, offer attractive templates for nanoparticle synthesis, due to their precise size and shape. In addition, simple genetic modifications can be employed to confer additional functionality with a high number of precisely spaced functional groups. In this work we exploit the specificity of genetically modified Tobacco Mosaic Virus (TMV1cys) for readily controllable palladium (Pd) nanoparticle synthesis via simple electroless deposition. TMV1cys, engineered to display one cysteine residue on the surface of each of over 2000 identical coat proteins, provides high density precisely spaced thiol groups for the preferential nucleation and growth of Pd nanoparticles. Small-Angle X-ray Scattering (SAXS) was employed to provide a statistically meaningful route to the investigation of Pd nanoparticle size ranges formed on the viral-nanotemplates. Specifically, we examine the size range and thermal stability of Pd nanoparticles formed on surface assembled TMV1cys. Further, we investigate the growth of Pd nanoparticles on TMV1cys in solution using in situ SAXS to better understand and predict nanoparticle growth on these nanotemplates. Lastly, we compare TMV1cys templated particle growth to Pd nanoparticle growth in the absence of TMV1cys to elucidate the role of TMV in particle formation. We show that Pd nanoparticles form preferentially on surface assembled TMV1cys in high density in a broad particle size range (4-18nm). Further, we show that Pd nanoparticles are significantly smaller and more uniform when

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

  18. Small-angle subgrain boundaries emanating from dislocation pile-ups in multicrystalline silicon studied with synchrotron white-beam X-ray topography

    International Nuclear Information System (INIS)

    The formation of dislocation pile-ups and related small-angle subgrain boundaries in block-cast multicrystalline silicon for photovoltaic applications has been studied by means of white-beam X-ray topography (WB-XRT). For this purpose, samples sliced perpendicular and parallel to the growth direction have been investigated in reflection and transmission geometry, respectively. During the growth process of the silicon ingot, the dislocation density increases. WB-XRT measurements revealed the formation of small-angle subgrain boundaries. The subgrains have a slightly changed orientation related to a rotation of ∼0.07–0.80° around an axis parallel to the growth direction. This tilt results from the high number of dislocations forming dislocation pile-ups and walls. The spacings between dislocations in such subgrain boundaries were found to be between 297 and 28 nm. A qualitative model for the formation of dislocation pile-ups is proposed

  19. Microfluidics for small angle x-ray scattering experiments

    International Nuclear Information System (INIS)

    Full text: Small Angle X-ray Scattering (SAXS) is a powerful technique which provides structural information on samples with characteristic size between ten and few thousand Angstroms. Therefore, it can be successfully employed in various fields such as material science (e.g. design of new nano-structured materials) or biology (e.g. structural characterization of biological processes). Recent developments in this method and novel x-ray detectors made it possible to conduct measurements in the regime of very short time-scales, very broad resolution range and to work with nanometer beam sizes. Micro and nano fabrication techniques permit the design and fabrication of new microfluidic devices and systems relying on different physical principles than on the macroscale, enabling to precisely control biological and chemical entities. Moreover, microfluidics lead to reduced sample and reagent consumption. By creating a strong synergy between state of the art microtechnology and advanced measurement and manipulation techniques is thus possible to access new fields of investigation. Our activity aims at the design, fabrication and test of microfluidic prototypes focusing on a versatile, modular set-up to be adopted in various research areas, i.e. chemistry and biology. In this communication, two microfluidic devices will be presented. The first is a rapid mixing device with a free jet flow for studying ultrafast chemical reactions by SAXS. The second is a microfluidic cell for the study of localized biological nanostructures by means of SAXS and laser tweezers which are a scientific instrument using a focused laser beam to provide an attractive or repulsive force, to physically hold and move microscopic objects. (author)

  20. 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, J.; Richter, F.; Mouritsen, O.G.; Rapp, G.; Kinnunen, P.K.J.

    2000-01-01

    hydrated binary membranes composed of dimyristoylphosphatidylcholine (DMPC) and N-palmitoyl-ceramide (C16:0-ceramide, up to a mole fraction X-cer = 0.35) were resolved in further detail by high-sensitivity differential scanning calorimetry (DSC) and x-ray diffraction. Both methods reveal very strong...... 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 < 0.18, together with an increase in T-p. In the gel phase the lamellar repeat distance d increases from similar to 61 Angstrom at X-cer = 0.03, to 67 Angstrom at X-cer = 0...

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

    DEFF Research Database (Denmark)

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

    2010-01-01

    Combined in situ small- and wide-angle X-ray scattering (SAXS/WAXS) studies were performed in a recently developed laboratory setup to investigate the dynamical properties of dry oleic acid-capped titanium dioxide nanorods during annealing in an inert gas stream in a temperature interval of 298......-1023 K. Aggregates formed by the titanium dioxide particles exhibit a continuous growth as a function of temperature. The particle size determined with SAXS and the crystallite size refined from WAXS show a correlated growth at temperatures above 673 K, where the decomposition of the surfactant is...... microscopy studies of the sample. Transmission electron microscopy shows a transformation from a rod to a spherical particle shape; the WAXS data indicate that the shape change occurs in a temperature interval of 773-923 K. The highly crystalline titanium dioxide particles remain in the metastable anatase...

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

    Science.gov (United States)

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

    2016-08-01

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

  3. MgATP-induced conformational changes in the iron protein from Azotobacter vinelandii, as studied by small-angle x-ray scattering.

    Science.gov (United States)

    Chen, L; Gavini, N; Tsuruta, H; Eliezer, D; Burgess, B K; Doniach, S; Hodgson, K O

    1994-02-01

    Small angle x-ray scattering experiments have been carried out on the purified iron proteins of nitrogenase from wild-type Azotobacter vinelandii and from a Nif- mutant strain, A. vinelandii UW91 (which has an A157S mutation). This study was designed to investigate the influence of MgATP and MgADP binding on the protein structure in solution. For the wild-type protein, the binding of MgATP induces a significant conformational change that is observed as a decrease of about 2.0 A in the radius of gyration. In contrast, the binding of MgADP to the wild-type iron protein does not detectably affect the radius of gyration. In the absence of nucleotides, the radius of gyration for the UW91 mutant is indistinguishable from that of the wild-type. However, unlike for the wild-type protein, the radius of gyration of the UW91 iron protein is unaffected by the addition of MgATP. We have previously shown that the UW91 iron protein has a normal [4Fe-4S] cluster and MgATP binding ability but that it is completely blocked for electron transfer and MgATP hydrolysis (Gavini, N., and Burgess, B. K. (1992) J. Biol. Chem. 267, 21179-21186). These x-ray scattering measurements suggest that a conformation different from that of the native state is therefore required for the iron protein to perform electron transfer to the MoFe protein. These results also support the hypothesis that Ala-157 is crucial for the iron protein to establish the electron-transfer-favored conformation induced by MgATP binding. PMID:8106367

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

    International Nuclear Information System (INIS)

    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 Se0 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. 1H NMR cryoporometry allowed us to reveal the details of changes in the sizes of small aqueous pores during modifications.

  5. THE MEDIUM RANGE STRUCTURE OF HYDROGENATED Cu-Ti AMORPHOUS ALLOYS STUDIED BY ANOMALOUS SMALL-ANGLE SCATTERING OF X-RAYS AND NEUTRON DIFFRACTION

    OpenAIRE

    Goudeau, P.; Naudon, A.; Rodmacq, B.; Mangin, P; Chamberod, A.

    1985-01-01

    Amorphous Cu-Ti alloys, when hydrogenated, reveal a strong small-angle scattered intensity. The anomalous X-ray scattering effect is used to analyse this SAS intensity on both copper and titanium edges. It allows to assert the presence of very small clusters of titanium hydride having the TiH2 composition. These results are in good agreement with those obtained by neutron scattering experiments when using either hydrogen (b 0) for the hydrogenation of the samples.

  6. Soft x rays for radiobiological studies

    International Nuclear Information System (INIS)

    Lethal effects and chromosome aberrations induced in cells exposed to low energy (soft) X rays demonstrated that these relatively low energy X rays are just as effective as those of higher energy for radiobiological studies, and even more effective for irradiating cultured mammalian cells than laboratory animals. (author)

  7. Dynamic angle selection in X-ray computed tomography

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-04-01

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

  8. X-ray scattering studies of lignocellulosic biomass: a review.

    Science.gov (United States)

    Xu, Feng; Shi, Yong-Cheng; Wang, Donghai

    2013-05-15

    The high processing cost of lignocellulosic ethanol is one of the most important barriers to its profitable commercialization. Pretreatments have been used to change the structure of biomass significantly and to improve sugar and ethanol yield. Great efforts have been made to understand the structural changes of biomass during these processes, including the molecular assembly of crystalline cellulose. Wide-angle and small-angle X-ray scattering are powerful techniques in studying the biomass structure at a molecular level. In this review, after we introduce the basic structure of lignocellulosic biomass, the effects of commonly used pretreatment methods on biomass structure, and the principle of X-ray scattering technique, the application of X-ray scattering, including studies of crystallinity, crystallite size, orientation distribution, and pore structure, and the related results in biomass conversion are summarized and discussed. Future study of biomass with X-ray scattering also is proposed. PMID:23544649

  9. Small-angle X-ray scattering of filled rubber

    International Nuclear Information System (INIS)

    The addition of fillers such as carbon black and silica in rubber shows reinforcement effects, which increase modulus of elasticity, tensile strength, and cracking resistance. The mechanism of the reinforcement has not yet been understood. A filter composes a hierarchical structure in rubber, where primary particles form aggregates and the aggregates from agglomerates. The structures of the aggregates and agglomerates, on a size of 100 μm∼10 μm, are considered to be the origins of the reinforcement. A two-dimensional ultra-small-angle x-ray scattering (2D-USAXS) system is a promising tool for the observation of the structural change on a size of 100 nm∼10 μm and has been installed in the SPring-8 storage ring. The combination of 2D-USAXS and viscoelastic measurements for styrene-butadiene rubber reveals the relationship between the aggregate structure and reinforcement. The energy dissipation mechanism of fillers will be resolved on the basis of the fluctuation-dissipation theorem from the observation of the fluctuation of fillers by the time-resolved spectra of the coherent microbeam x-ray small angle scattering. (Y.K.)

  10. How Large is an α-Helix? Studies of the Radii of Gyration of Helical Peptides by Small-angle X-ray Scattering and Molecular Dynamics

    International Nuclear Information System (INIS)

    Using synchrotron radiation and the small-angle X-ray scattering technique we have measured the radii of gyration of a series of alanine-based alpha-helix-forming peptides of the composition Ace-(AAKAA)(n)-GY-NH(2), n=2-7, in aqueous solvent at 10(+/-1) degrees C. In contrast to other techniques typically used to study alpha-helices in isolation (such as nuclear magnetic resonance and circular dichroism), small-angle X-ray scattering reports on the global structure of a molecule and, as such, provides complementary information to these other, more sequence-local measuring techniques. The radii of gyration that we measure are, except for the 12-mer, lower than the radii of gyration of ideal alpha-helices or helices with frayed ends of the equivalent sequence-length. For example, the measured radius of gyration of the 37-mer is 14.2(+/-0.6)A, which is to be compared with the radius of gyration of an ideal 37-mer alpha-helix of 17.6A. Attempts are made to analyze the origin of this discrepancy in terms of the analytical Zimm-Bragg-Nagai (ZBN) theory, as well as distributed computing explicit solvent molecular dynamics simulations using two variants of the AMBER force-field. The ZBN theory, which treats helices as cylinders connected by random walk segments, predicts markedly larger radii of gyration than those measured. This is true even when the persistence length of the random walk parts is taken to be extremely short (about one residue). Similarly, the molecular dynamics simulations, at the level of sampling available to us, give inaccurate values of the radii of gyration of the molecules (by overestimating them by around 25% for longer peptides) and/or their helical content. We conclude that even at the short sequences examined here (< or =37 amino acid residues), these alpha-helical peptides behave as fluctuating semi-broken rods rather than straight cylinders with frayed ends.

  11. Preparation of metal oxide nanoparticles of different sizes and morphologies, their characterization using small angle X-ray scattering and study of thermal properties

    International Nuclear Information System (INIS)

    In an effort to shed light into the role of surface morphology of nanoparticles on their thermal properties, we have prepared Fe3O4 and CuO nanoparticles of different sizes and morphologies using co-precipitation and precipitation approach, respectively. The prepared particles are characterized using Small Angle X-ray Scattering (SAXS) and the results are compared with X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM), and Dynamic Light Scattering (DLS). The results show that the size distribution and surface morphologies of nanoparticles can be quite accurately measured by using SAXS with the aid of appropriate models. The thermal conductivity of spherical Fe3O4 nanofluids follows effective medium theory whereas the CuO nanorod based dispersions show a much larger thermal conductivity beyond the effective medium theory. The abnormal thermal conductivity in CuO is attributed to effective conduction of heat through nanorods of higher aspect ratio. These finding are useful for engineering efficient nanofluids for thermal management. - Highlights: • Fe3O4 and CuO nanoparticles of different sizes and morphologies were prepared. • The morphological evaluation was done using Small Angle X-ray Scattering (SAXS). • Thermal conductivity (k) of Fe3O4 nanofluids follows effective medium theory (EMT). • CuO nanorod based dispersions show a k enhancement beyond the EMT. • Abnormal k in CuO is due to the effective conduction of heat through nanorods

  12. Novel in situ setup to study the formation of nanoparticles in the gas phase by small angle x-ray scattering

    International Nuclear Information System (INIS)

    An in-house built aerosol generator setup for in situ gas phase studies of aerosol and nanoparticles is described. The aerosol generator with an ultrasonic ceramic disk mist maker provides high enough particle concentrations for structural gas phase analysis by synchrotron small angle x-ray scattering (for water ∼4x108 droplets/s with a droplet size of ∼2.5 μm). The working principle was proved by scattering of gold nanoparticles. For evaporation induced self-assembly studies of nanostructured particles, an additional thermal treatment chamber was included in the setup. The first on-line gas phase data with our setup for mesostructured silica particles are presented for different thermal treatments. Scanning electron microscope imaging revealed the average particle size to be ∼1 μm. Furthermore, to quantify their internal nanostructure, diffraction experiments of deposited silica aerosols were carried out and the corresponding electron density map indicates a silica wall thickness of about 1 nm

  13. Cell survival studies using ultrasoft x rays

    International Nuclear Information System (INIS)

    Cell survival was studied for V79 hamster, 10T1/2 mouse, and human skin fibroblast cell lines, using carbon K (0.28 keV), copper K (8.0 keV), and 250 kVp x rays. Because of the rapid attenuation of the carbon x rays, cellular dimensions at the time of exposure were measured using optical and electron microscopy, and frequency distributions of mean dose absorbed by the cell nucleus were obtained. The results indicate that the differences in cell killing between ultra-soft and hard x rays may depend on the nuclear thickness of the cells. Studies of the effects of hypoxia on V79 and 10T1/2 cells using carbon K, aluminum K (1.5 keV), and copper K x rays show decreasing OER values with decreasing x-ray energy and no difference between the two cell lines. Age response studies with V79 cells show similar cell-cycle variation of survival for carbon K and aluminum K x rays as for hard x rays

  14. Diffractometer for small angle resonant soft x-ray scattering under magnetic field

    International Nuclear Information System (INIS)

    There has been a recent increasing interest in a topological spin texture, so-called skyrmion crystal, stimulated by small-angle neutron scattering and Lorentz-TEM studies. For the purpose of measuring the resonant soft x-ray magnetic scattering to characterize the distribution of magnetic moments with long-wavelength in range of a few tens to hundreds nm, we have developed a diffractometer for small angle soft x-ray scattering. The principle features of the diffractometer and the initial experimental results are presented.

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

    Science.gov (United States)

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

    2012-07-28

    We study the structure and reorientation dynamics of nanometer-sized water droplets inside nonionic reverse micelles (water/Igepal-CO-520/cyclohexane) with time-resolved mid-infrared pump-probe spectroscopy and small angle x-ray scattering. In the time-resolved experiments, we probe the vibrational and orientational dynamics of the O-D bonds of dilute HDO:H(2)O mixtures in Igepal reverse micelles as a function of temperature and micelle size. We find that even small micelles contain a large fraction of water that reorients at the same rate as water in the bulk, which indicates that the polyethylene oxide chains of the surfactant do not penetrate into the water volume. We also observe that the confinement affects the reorientation dynamics of only the first hydration layer. From the temperature dependent surface-water dynamics, we estimate an activation enthalpy for reorientation of 45 ± 9 kJ mol(-1) (11 ± 2 kcal mol(-1)), which is close to the activation energy of the reorientation of water molecules in ice. PMID:22852627

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

    Science.gov (United States)

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

    2012-07-01

    We study the structure and reorientation dynamics of nanometer-sized water droplets inside nonionic reverse micelles (water/Igepal-CO-520/cyclohexane) with time-resolved mid-infrared pump-probe spectroscopy and small angle x-ray scattering. In the time-resolved experiments, we probe the vibrational and orientational dynamics of the O-D bonds of dilute HDO:H2O mixtures in Igepal reverse micelles as a function of temperature and micelle size. We find that even small micelles contain a large fraction of water that reorients at the same rate as water in the bulk, which indicates that the polyethylene oxide chains of the surfactant do not penetrate into the water volume. We also observe that the confinement affects the reorientation dynamics of only the first hydration layer. From the temperature dependent surface-water dynamics, we estimate an activation enthalpy for reorientation of 45 ± 9 kJ mol-1 (11 ± 2 kcal mol-1), which is close to the activation energy of the reorientation of water molecules in ice.

  17. Study of pore structure in grafted polymer membranes using slow positron beam and small-angle X-ray scattering techniques

    International Nuclear Information System (INIS)

    Pore structure in polypropylene membranes has been investigated using slow positron beam and small-angle X-ray scattering (SAXS) studies. The pore structure has been modified by chemically grafting methylmethacrylate in polypropylene. Depth-resolved Doppler lineshape S-parameter and positronium (Ps) fraction (3γ/2γ ratio) measurements have been carried out using a variable low energy positron beam. Lineshape S-parameter and Ps fraction are found to decrease with the extent of grafting. The deduced positron diffusion length is also seen to decrease with the extent of pore grafting. The power law dependence of SAXS intensity over a wide range of the wave vector transfer reveals the fractal nature of the pore-membrane surface and, the surface fractal dimensions are seen to increase with amount of pore grafting. The value of the negative exponent of the power law size distribution of the pores has been found to be increasing with increase in grafting revealing reduction in the pore size and narrower pore size distribution. The deduced pore size from SAXS measurements is correlated with positron diffusion length and S-parameter from the positron beam measurements

  18. X-ray tubes study and design

    International Nuclear Information System (INIS)

    This thesis contain both theoretical and experimental works. Theoretical aspect includes X-Ray tubes case study and design principles, in the introduced design process, anode-cathode distance, vacuum needed, filament size, anode face angle and shape and size of focusing electrodes can be found. A method for specification of tungsten lager thickness on anode is also introduced. Using computer simulation, electron trajectory between cathode-anode is obtained, This work is presented in the first International Conference on Control and Modeling, Tehran, 1990. Experimental work contains manufacturing more than 10 tubes and test each of them. One of these tubes can with stand up to 50 KV. Filament can be heated by passing a 2.1 A current. In these conditions anode current is 1.2 m A. Using this tube, some radiographs have been taken

  19. Low-angle X-ray scattering from spices

    Science.gov (United States)

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

    2002-07-01

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

  20. Low-angle X-ray scattering from spices

    International Nuclear Information System (INIS)

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

  1. Low-angle X-ray scattering from spices

    Energy Technology Data Exchange (ETDEWEB)

    Desouky, O.S. E-mail: omardesouky@yahoo.com; Ashour, Ahmed H.; Abdullah, Mohamed I.; Elshemey, Wael M

    2002-07-01

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

  2. Evolution and change of He bubbles in He-containing Ti films upon thermal treatment studied by small-angle X-ray scattering and transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Guangai [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Wu, Erdong, E-mail: ewu@imr.ac.cn [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Huang, Chaoqiang [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Cheng, Chun [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Yan, Guanyun [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Wang, Xiaolin [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); College of Nuclear Science and Technology, University of Science and Technology of China, Hefei, 230029 (China); Liu, Shi [National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016 (China); Tian, Qiang; Chen, Bo [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Wu, Zhonghua [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Liu, Yi; Wang, Jie [Institute of Shanghai Apply Physics, Chinese Academy of Sciences, Shanghai 201800 (China)

    2014-05-02

    Evolution and change of He bubbles in magnetron sputtering prepared He-containing Ti films under thermal treatment are studied by small-angle X-ray scattering (SAXS), transmission electron microscopy (TEM) and X-ray diffraction. Incorporation of He introduces a large number of He-vacancy clusters and some voids in the films, and significantly increases SAXS intensity and causes anisotropic scattering. The change of He induced defects during annealing is affected by thermal diffusion and migration of trapped He to the surface and between interfaces of He induced defects within the films. Annealing at 200 and 400 °C reduces intensity and anisotropy of SAXS, in accord with observed shrinking and disappearance of the voids. The simultaneous growth of non-uniformly distributed He bubbles to the sizes of 1–2 nm and a population level of 10{sup 5}/μm{sup 3} are detected in the temperature range. The changes are explained by migration and coalescence mechanisms, which requires low apparent activation energy. Inconsistence between TEM and SAXS observations is noted and attributed to thinning induced internal stress relaxation of TEM specimen. Remarkable enlargement of He bubbles, associated with increased SAXS intensity and fractal dimension, is observed after 600 °C annealing, indicating involvement of Ostwald Ripening (OR) mechanism. The OR process dominates at 800 °C, where the high temperature provides activation energy for accelerated He dissociation from small bubbles into larger ones, and generating textured microstructure and agglomerated bubble clusters. The inhomogeneous bubble size distribution observed at this temperature covers a broad range of about 10–50 nm and possessing a population density level of 10{sup 3}/μm{sup 3}. - Highlights: • Change of He bubbles in thermally treated Ti–He films is studied by SAXS and TEM. • SAXS reveals size distribution and fractional population of He bubbles in films. • He-vacancy clusters in Ti–He film

  3. Evolution and change of He bubbles in He-containing Ti films upon thermal treatment studied by small-angle X-ray scattering and transmission electron microscopy

    International Nuclear Information System (INIS)

    Evolution and change of He bubbles in magnetron sputtering prepared He-containing Ti films under thermal treatment are studied by small-angle X-ray scattering (SAXS), transmission electron microscopy (TEM) and X-ray diffraction. Incorporation of He introduces a large number of He-vacancy clusters and some voids in the films, and significantly increases SAXS intensity and causes anisotropic scattering. The change of He induced defects during annealing is affected by thermal diffusion and migration of trapped He to the surface and between interfaces of He induced defects within the films. Annealing at 200 and 400 °C reduces intensity and anisotropy of SAXS, in accord with observed shrinking and disappearance of the voids. The simultaneous growth of non-uniformly distributed He bubbles to the sizes of 1–2 nm and a population level of 105/μm3 are detected in the temperature range. The changes are explained by migration and coalescence mechanisms, which requires low apparent activation energy. Inconsistence between TEM and SAXS observations is noted and attributed to thinning induced internal stress relaxation of TEM specimen. Remarkable enlargement of He bubbles, associated with increased SAXS intensity and fractal dimension, is observed after 600 °C annealing, indicating involvement of Ostwald Ripening (OR) mechanism. The OR process dominates at 800 °C, where the high temperature provides activation energy for accelerated He dissociation from small bubbles into larger ones, and generating textured microstructure and agglomerated bubble clusters. The inhomogeneous bubble size distribution observed at this temperature covers a broad range of about 10–50 nm and possessing a population density level of 103/μm3. - Highlights: • Change of He bubbles in thermally treated Ti–He films is studied by SAXS and TEM. • SAXS reveals size distribution and fractional population of He bubbles in films. • He-vacancy clusters in Ti–He film transfer to bubbles and

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

    NARCIS (Netherlands)

    Abramova, V.V.; Sinitskii, A.S.; Grigoryeva, N.A.; Grigoriev, S.V.; Belov, D.V.; Petukhov, A.V.; Mistonov, A.A.; Vasilieva, A.V.; Tretyakov, Y.D.

    2009-01-01

    The results of an ultrasmall angle X ray scattering study of iron(III) oxide inverse opal thin films are presented. The photonic crystals examined are shown to have fcc structure with amount of stacking faults varying among the samples. The method used in this study makes it possible to easily disti

  5. X-ray imaging based on small-angle X-ray scattering using spatial coherence of parametric X-ray radiation

    International Nuclear Information System (INIS)

    X-ray imaging based on small-angle X-ray scattering (SAXS) was carried out using the parametric X-ray radiation (PXR) source at the Laboratory for Electron Beam Research and Application (LEBRA) of Nihon University. The experimental setup employed in this novel imaging approach is the same as that employed in diffraction-enhanced imaging (DEI), a kind of X-ray phase-contrast imaging method. In SAXS-based imaging, the image contrast is correlated with the broadening of the rocking curve peak due to the scattering from micron- or sub-micron-sized grains in the sample material. An experiment using the 25.5-keV PXR beam demonstrated that SAXS-based imaging with PXR provides a substantially strong contrast for granular materials despite the extremely low density of the material.

  6. 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...

  7. Preparation of metal oxide nanoparticles of different sizes and morphologies, their characterization using small angle X-ray scattering and study of thermal properties

    Energy Technology Data Exchange (ETDEWEB)

    Gopinath, S.; Philip, John, E-mail: philip@igcar.gov.in

    2014-05-01

    In an effort to shed light into the role of surface morphology of nanoparticles on their thermal properties, we have prepared Fe{sub 3}O{sub 4} and CuO nanoparticles of different sizes and morphologies using co-precipitation and precipitation approach, respectively. The prepared particles are characterized using Small Angle X-ray Scattering (SAXS) and the results are compared with X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM), and Dynamic Light Scattering (DLS). The results show that the size distribution and surface morphologies of nanoparticles can be quite accurately measured by using SAXS with the aid of appropriate models. The thermal conductivity of spherical Fe{sub 3}O{sub 4} nanofluids follows effective medium theory whereas the CuO nanorod based dispersions show a much larger thermal conductivity beyond the effective medium theory. The abnormal thermal conductivity in CuO is attributed to effective conduction of heat through nanorods of higher aspect ratio. These finding are useful for engineering efficient nanofluids for thermal management. - Highlights: • Fe{sub 3}O{sub 4} and CuO nanoparticles of different sizes and morphologies were prepared. • The morphological evaluation was done using Small Angle X-ray Scattering (SAXS). • Thermal conductivity (k) of Fe{sub 3}O{sub 4} nanofluids follows effective medium theory (EMT). • CuO nanorod based dispersions show a k enhancement beyond the EMT. • Abnormal k in CuO is due to the effective conduction of heat through nanorods.

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

    Directory of Open Access Journals (Sweden)

    Changizi V

    2008-01-01

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

  9. Small-angle X-ray scattering study of the structural evolution of the drying of teos-derived sonogels with the liquid phase exchanged by acetone

    International Nuclear Information System (INIS)

    Full text: The structural evolution on the drying of wet sonogels of silica with the liquid phase exchanged by acetone, obtained from tetraethoxisilane sonohydrolysis, was studied 'in situ' by small-angle X-ray scattering (SAXS). The SAXS measurements were carried out using synchrotron radiation with a wavelength λ = 0.1608 nm and a pin-hole geometry collimated beam. The periods associated to the structural evolution as determined by SAXS are in agreement with those classical ones established on basis of the features of the evaporation rate of the liquid phase in the obtaining of xerogels. The SAXS data were analyzed on basis of the fractal characteristics of the sonogels. The wet gel can be described as formed by primary particles (microclusters), with characteristic length a ∼ 0.67 nm and surface which is fractal, linking together to form mass fractal structures with mass fractal dimension D = 2.24 in a length scale ξ ∼ 6.7 nm. As the network collapses while the liquid/vapor meniscus is kept out of the gel volume, the mass fractal structure becomes more compacted by increasing D and decreasing ξ, with smoothing of the fractal surface of the microclusters. The time evolution of the density of the wet gels was evaluated exclusively from the SAXS parameters ξ, D and a. The final dried acetone-exchanged gel presents Porod's inhomogeneity length of about 2.8 nm and apparently exhibits an interesting singularity D → 3, as determined by the mass fractal modeling used to t the SAXS intensity data for the obtaining of the parameters ξ and D. (author)

  10. Structural model and stability studies of the extracellular domain of the human amyloid precursor protein obtained using small angle X-ray scattering

    International Nuclear Information System (INIS)

    Full text: The amyloid precursor protein (APP) is the precursor of the β-amyloid peptide (Aβ), which is centrally related to the genesis of Alzheimer's disease (AD). In addition, APP has been suggested to mediate and/or participate in events that lead to neuronal degeneration in AD. Human APP exists in various isoforms, of which the major ones contain 695, 751 and 770 aminoacids. Proteolytic cleavage of APP by α- or β-secretases releases the extracellular soluble fragments sAPPα and sAPPβ, respectively. Despite the fact that sAPPα plays important roles in both physiological and pathological processes in the brain, very little is known about the structure and stability of this protein. We have recently presented a structural model of sAPPα695 obtained from small-angle X-ray scattering (SAXS) measurements (Gralle et al., Biophys. J. 83,3513-3524). The elongated shape of the reported model is in agreement with the circular dichroism and secondary structure predictions based on the aminoacid sequence of APP. This suggests that a significant fraction of APP (30% of the aminoacid residues) is not involved in standard secondary structure elements. We now report high resolution SAXS models and studies of folding and stabilities of both sAPPα695 and sAPPα770. These high resolution measurements allows the calculation of models up to subdomain structure (4 angstrom resolution). These models enable the prediction of hydrodynamic parameters of these proteins which can be compared with measured values. SAXS measurements of the denaturation of sAPPα695 and sAPPα770 by GdnHCl and urea revealed a multi-step folding pathway for both sAPPα isoforms. The stepwise denaturation process can be correlated to the three-dimensional models. (author)

  11. Characterization of angle – dependent Focal spot in a miniature X-ray tube

    International Nuclear Information System (INIS)

    Miniature x-ray tube can be used to obtain important images easily due to its small size and movability. Because the miniature x-ray tube discussed in this paper is a transmission type, it can emit x-rays in all directions, making it possible to take angle-dependent images. Focal spot is essential in an x-ray tube because it affects the quality of images taken by the x-ray tube. The size of the focal spot is equivalent to that of the x-ray generation region located at the x-ray tube target. If the size of focal spot is too large, images produced will be blurry. In other words, smaller focal spots produce clearer images. Currently common x-ray tubes have a relatively thick target, causing them to emit x-rays in one direction with uniform focal spot size. This type of x-ray produced is called reflection x-ray. However, unlike the conventional, miniature x-ray tubes, that this paper focuses on, have thin beryllium targets, allowing for both reflection x-ray and transmission x-ray to be generated at the targets. And since both types can affect the size of focal spots, these miniature x-ray tubes can emit x-rays, which is a crucial property when taking angle-dependent images. By measuring the physical characteristics of the focal spots, methods of improving the qualities of angle-dependent images can be determined. Thus, this experiment, which deals with measuring these physical characteristics will substantially help in the improvement of the qualities of angle-dependent images. The result was obtained by analyzing the image with procedure provided by EN-12543-5 Focal spots increase with increase in angle from 0 degree to 90 degrees

  12. What can be obtained by bringing together small angle X-ray scattering and deep X-ray lithography?

    International Nuclear Information System (INIS)

    Full text: Micro-nanotechnology has melted away the borders between material science and biology. In fact, the miniaturization of chemical and biological assays, promoted by micro-nanofluidics, requires both a careful selection of the fabrication methods and the development of tailored materials for the specific applications. As a consequence, interdisciplinary is becoming fundamental also in the combination of microfabrication and characterization techniques both aimed at the construction of new devices and at the development of novel materials for chemistry and biology applications. In this communication, we want to underline the advantages obtainable by combining two techniques: Deep X-ray Lithography (DXRL) for microfabrication and Small and Wide Angle X-ray Scattering (SAXS/WAXS) for investigation. On one hand DXRL makes it possible for SAXS to improve time resolution and create new sample environments. On the other hand SAXS permits the investigation of the nanostructural morphology of the microstructures fabricated by DXRL in order to tune the morphology for specific applications like nanosensors and biosensors or to determine the effect of irradiation on new materials. Examples will be presented to highlight both. First, microdevices fabricated for time resolved experiments of fast biological and chemical reactions, or for the study of the effect of confinement on crystal growth will be discussed. Then, the combination of bottom-up and top-down approaches for the development of new functionalized materials for which characterization with SAXS/WAXS is fundamental will be described. (author)

  13. In-situ study of precipitates in Al–Zn–Mg–Cu alloys using anomalous small-angle x-ray scattering

    Science.gov (United States)

    Chun-Ming, Yang; Feng-Gang, Bian; Bai-Qing, Xiong; Dong-Mei, Liu; Yi-Wen, Li; Wen-Qiang, Hua; Jie, Wang

    2016-06-01

    In the present work, the precipitate compositions and precipitate amounts of these elements (including the size distribution, volume fraction, and inter-precipitate distance) on the Cu-containing 7000 series aluminum alloys (7150 and 7085 Al alloys), are investigated by anomalous small-angle x-ray scattering (ASAXS) at various energies. The scattering intensity of 7150 alloy with T6 aging treatment decreases as the incident x-ray energy approaches the Zn absorption edge from the lower energy side, while scattering intensity does not show a noticeable energy dependence near the Cu absorption edge. Similar results are observed in the 7085 alloy in an aging process (120 °C) by employing in-situ ASAXS measurements, indicating that the precipitate compositions should include Zn element and should not be strongly related to Cu element at the early stage after 10 min. In the aging process, the precipitate particles with an initial average size of ∼ 8 Å increase with aging time at an energy of 9.60 keV, while the increase with a slower rate is observed at an energy of 9.65 keV as near the Zn absorption edge. Project supported by the National Natural Science Foundation of China (Grant Nos. 11005143, 11405259, and 51274046) and the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry of China (Grant No. [2014]1685).

  14. High-performance permanent magnetic circuit designed for small-angle X-ray scattering using synchrotron radiation source

    International Nuclear Information System (INIS)

    A new type of permanent magnetic circuit with several prominent characteristics was developed and applied to the studies of oriented macromolecular assemblies by small-angle X-ray scattering using synchrotron radiation source. (orig.)

  15. In-Situ Small-Angle X-Ray Scattering Study of Simple Shear Oriented Poly(ethylene Terephthalate) during Heating

    Science.gov (United States)

    Wang, Zhigang; Xia, Zhiyong; Hsiao, Benjamin; Sue, Hj; Han, Charles

    2002-03-01

    An equal channel angular extrusion (ECAE) process was used to prepare poly(ethylene terephthalate) samples with segmental lamellar orientations. In-situ small-angle X-ray scattering measurements were carried out to follow the structure changes during heating of sections of equal-channel-angular-extruded PET samples before and after the transition line. The total scattering power, fractions of anisotropic and isotropic scattering, orientation factors and long periods along the flow directions were obtained. The changes in these parameters revealed the processes of lamellar relaxation, recrystallization and melting during heating in specimens of different orientation and morphology. Acknowledgements. The financial support of this work is provided by a grant from NIST and NSF (DMR 0098104). The Advanced Polymers Beamline is supported by DOE (DE-FG02-99ER 45760).

  16. Aggregation of bovine serum albumin upon cleavage of its disulfide bonds, studied by the time-resolved small-angle X-ray scattering technique with synchrotron radiation

    International Nuclear Information System (INIS)

    A rapid mixing system of the stopped-flow type, used with small-angle X-ray scattering equipment using synchrotron radiation, is described. The process of aggregation of bovine serum albumin was traced with a time interval of 50 s, initiated upon cleavage of its disulfide bonds by reduction with dithiothreitol. The results indicate that a 218-fold molar excess of dithiothreitol over the number of moles of disulfide bonds in bovine serum albumin is sufficient to initiate the reaction immediately after mixing, which reaches equilibrium in about 15 min. On the other hand, half this amount is not sufficient to initiate the reaction, so that the reaction is delayed by about 150 s. Such a single-shot time-resolved experiment showed that experiments with a time interval of 100 ms are possible with repeated multi-shot runs. (Auth.)

  17. Weak self-interactions of globular proteins studied by small-angle X-ray scattering and structure-based modeling

    CERN Document Server

    Kaieda, Shuji; Plivelic, Tomás S; Halle, Bertil

    2014-01-01

    We investigate protein-protein interactions in solution by small-angle X-ray scattering (SAXS) and theoretical modeling. The structure factor for solutions of bovine pancreatic trypsin inhibitor (BPTI), myoglobin (Mb), and intestinal fatty acid-binding protein (IFABP) is determined from SAXS measurements at multiple concentrations, from Monte Carlo simulations with a coarse-grained structure-based interaction model, and from analytic approximate solutions of two idealized colloidal interaction models without adjustable parameters. By combining these approaches, we find that the structure factor is essentially determined by hard-core and screened electrostatic interactions. Other soft short-ranged interactions (van der Waals and solvation-related) are either individually insignificant or tend to cancel out. The structure factor is also not significantly affected by charge fluctuations. For Mb and IFABP, with small net charge and relatively symmetric charge distribution, the structure factor is well described b...

  18. 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.; Pedersen, J.S.; Nielsen, Martin Meedom

    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...... side chains ([3-(2-methylpropionamido)propyl]trimethylammonium chloride, MAPTAC, and poly{[(2-propionyloxy)ethyl]-trimethylammonium chloride}, PCMA) form a 2-dimensional hexagonal structure with SDS, whereas a polyelectrolyte without side chains (poly(vinlyamine), PVAm) forms a lamellar structure. The...... from a=47.7 Angstrom (MAPTAC, 100% charge density) to 58.5 Angstrom (AM-MAPTAC, 30% charge density). The unit cell length in the lamellar SDS/PVAm complex (a=36.1 Angstrom) is significantly smaller than for the different hexagonal structures. It is conjectured that the cylinders in the hexagonal...

  19. In situ synchrotron study of liquid phase separation process in Al-10 wt.% Bi immiscible alloys by radiography and small angle X-ray scattering

    Science.gov (United States)

    Lu, W. Q.; Zhang, S. G.; Li, J. G.

    2016-03-01

    Liquid phase separation process of immiscible alloys has been repeatedly tuned to create special structure for developing materials with unique properties. However, the fundamental understanding of the liquid phase separation process is still under debate due to the characteristics of immiscible alloys in opacity and high temperature environment of alloy melt. Here, the liquid phase separation process in solidifying Al-Bi immiscible alloys was investigated by synchrotron radiography and small angle X-ray scattering. We provide the first direct evidence of surface segregation prior to liquid decomposition and present that the time dependence on the number of Bi droplets follows Logistic curve. The liquid decomposition results from a nucleation and growth process rather than spinodal decomposition mechanism because of the positive deviation from Porod's law. We also found that the nanometer-sized Bi-rich droplets in Al matrix melt present mass fractal characteristics.

  20. Radiobiological studies using gamma and x rays.

    Energy Technology Data Exchange (ETDEWEB)

    Potter, Charles Augustus; Longley, Susan W.; Scott, Bobby R. [Lovelace Respiratory Research Institute, Albuquerque, NM; Lin, Yong [Lovelace Respiratory Research Institute, Albuquerque, NM; Wilder, Julie [Lovelace Respiratory Research Institute, Albuquerque, NM; Hutt, Julie A. [Lovelace Respiratory Research Institute, Albuquerque, NM; Padilla, Mabel T. [Lovelace Respiratory Research Institute, Albuquerque, NM; Gott, Katherine M. [Lovelace Respiratory Research Institute, Albuquerque, NM

    2013-02-01

    There are approximately 500 self-shielded research irradiators used in various facilities throughout the U.S. These facilities use radioactive sources containing either 137Cs or 60Co for a variety of biological investigations. A report from the National Academy of Sciences[1] described the issues with security of particular radiation sources and the desire for their replacement. The participants in this effort prepared two peer-reviewed publications to document the results of radiobiological studies performed using photons from 320-kV x rays and 137Cs on cell cultures and mice. The effectiveness of X rays was shown to vary with cell type.

  1. X-ray studies of multilayer semiconductors using synchrotron radiation

    Science.gov (United States)

    Huang, Shiwen

    X-ray scattering and absorption techniques utilizing synchrotron radiation have been used to study a variety of multilayer semiconductors. The angular-dependent x-ray scattering at grazing incidence angles (grazing incidence x-ray scattering, GIXS) provides structural information of interfaces in these materials, such as rms interfacial roughness, cross- and lateral-correlation lengths, etc. Long-range order structures in material are probed by large-angle scattering (x-ray diffraction), in which strain and lattice constant as well as crystallinity of the epilayers are measured. Local structural variations in materials including local bond length, coordination number, and local disorder are obtained quantitatively by examining the modulation in the x-ray absorption spectrum some 40 eV above the absorption edge (extended x-ray absorption fine structure, EXAFS). Materials studied in the present work are SiGe/Si heterostructures, MnAs/GaAs ferromagnetic-semiconductor films, solar cell films, ZnSe-based II-VI semiconductor thin films, InGaAs/GaAs and GaAs/AlAs superlattices. Results obtained have shown (i) evidence for strain-induced surface/interface morphology variations in SiGe/Si heterostructures, (ii) template-dependent microstructures in MnAs/GaAs, (iii) changes in interface structures for films of different formations in solar cell films, (iv) differences between samples prepared by different epitaxial growth methods in II-VI semiconductor films, (v) observation of lateral structural ordering in one of the InGaAs/GaAs superlattices, (vi) differences in interfacial microstructures between MBE-grown samples with different interrupts in GaAs/AlAs superlattices. Most of all, x- rays are found to be a very useful nondestructive tool for probing microscopic structures in various multilayer semiconductor materials.

  2. A small-angle X-ray scattering study of the effect of chain architecture on the shear-induced crystallization of branched and linear poly(ethylene terephthalate)

    OpenAIRE

    Hanley, T.; Sutton, D.; Heeley, E; Moad, G.; KNOTT, R.

    2007-01-01

    The synchrotron-based small-angle X-ray scattering (SAXS) technique was used to investigate the shear-induced crystallization kinetics of branched/unbranched poly(ethylene terephthalate) (PET). Reactive extrusion of bottle-grade PET with the branching and chain-extension agents pyromellitic dianhydride and pentaerythritol results in enhanced rheological properties, such as higher melt strength and higher viscosity. In this study, six samples of PET were investigated: linear PET [intrinsic vis...

  3. The filament forming reactions of vimentin tetramers studied in a serial-inlet microflow device by small angle x-ray scattering.

    Science.gov (United States)

    Saldanha, Oliva; Brennich, Martha E; Burghammer, Manfred; Herrmann, Harald; Köster, Sarah

    2016-03-01

    The structural organization of metazoan cells and their shape are established through the coordinated interaction of a composite network consisting of three individual filament systems, collectively termed the cytoskeleton. Specifically, microtubules and actin filaments, which assemble from monomeric globular proteins, provide polar structures that serve motor proteins as tracks. In contrast, intermediate filaments (IFs) assemble from highly charged, extended coiled coils in a hierarchical assembly mechanism of lateral and longitudinal interaction steps into non-polar structures. IF proteins are expressed in a distinctly tissue-specific way and thereby serve to generate the precise plasticity of the respective cells and tissues. Accordingly, in the cell, numerous parameters such as pH and salt concentration are adjusted such that the generation of functional networks is ensured. Here, we transfer the problem for the mesenchymal IF protein vimentin to an in vitro setting and combine small angle x-ray scattering with microfluidics and finite element method simulations. Our approach is adapted to resolve the early assembly steps, which take place in the sub-second to second range. In particular, we reveal the influence of ion species and concentrations on the assembly. By tuning the flow rates and thus concentration profiles, we find a minimal critical salt concentration for the initiation of the assembly. Furthermore, our analysis of the surface sensitive Porod regime in the x-ray data reveals that the formation of first assembly intermediates, so-called unit length filaments, is not a one-step reaction but consists of distinct consecutive lateral association steps followed by radial compaction as well as smoothening of the surface of the full-width filament. PMID:27042250

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-05-01

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

  5. Arbutin: Isolation, X-ray structure and computional studies

    Science.gov (United States)

    Nycz, Jacek E.; Malecki, Grzegorz; Morag, Monika; Nowak, Gerard; Ponikiewski, Lukasz; Kusz, Joachim; Switlicka, Anna

    2010-09-01

    Arbutin, an active component originated from Serratula quinquefolia for skin-whitening use and treating skin related allergic inflammation, was characterized by microanalysis, FTIR, UV-Vis, multinuclear NMR spectroscopy, and single crystal X-ray diffraction method. The geometries of the studied compound were optimized in singlet states using the density functional theory (DFT) method with B3LYP functional. Electronic spectra were calculated by TDDFT method. In general, the predicted bond lengths and angles are in a good agreement with the values based on the X-ray crystal structure data.

  6. Laser-based X-ray and electron source for X-ray fluorescence studies

    Science.gov (United States)

    Valle Brozas, F.; Crego, A.; Roso, L.; Peralta Conde, A.

    2016-08-01

    In this work, we present a modification to conventional X-rays fluorescence using electrons as excitation source and compare it with the traditional X-ray excitation for the study of pigments. For this purpose, we have constructed a laser-based source capable to produce X-rays as well as electrons. Because of the large penetration depth of X-rays, the collected fluorescence signal is a combination of several material layers of the artwork under study. However, electrons are stopped in the first layers, allowing a more superficial analysis. We show that the combination of both excitation sources can provide extremely valuable information about the structure of the artwork.

  7. [Diffuse x-ray wide-angle scattering of polyglutamic acid in solution].

    Science.gov (United States)

    Fedorov, B A; Becker, M; Damaschun, G; Damaschun, H; Gedicke, C; Zirwer, D

    1977-01-01

    The diffuse wide angle x-ray scattering (WAXS) of polyglutamic acid (PGA) in solution was studied using an x-ray diffractometer with small aperture of the primary beam. The scattering curve was recorded at an angular interval from (article: see text). The experimental scattering intensity of PGA with alpha-helical CD spectrum showed a maximum at 14.4 nm-1. Unordered PGA in solution yielded no maximum at this scattering angle. The studies have proved that the scattering theory can be applied to globular proteins in solution as well as to chain molecules in solution in this angular interval. The differences between the calculated scattering curves and the experimental curves indicate minor movements of the side chains of PGA in solutions and slight structuring of the solvent at the surface of the polypeptide chain. PMID:25547

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

    OpenAIRE

    Stovgaard Kasper; Andreetta Christian; Ferkinghoff-Borg Jesper; Hamelryck Thomas

    2010-01-01

    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 ac...

  9. Small angle X-ray scattering study of poly(N-isopropyl acrylamide) based cryogels near the volume-phase transition temperature

    International Nuclear Information System (INIS)

    The structural modifications induced by changes in temperature are investigated by Small-Angle X-ray Scattering (SAXS) over a broad range of q-values (3.5x10-2 - 12 nm-1) in cryogels based on N-isopropylacrylamide (NIPA) and/or 2-Hydroxyethyl methacrylate-L-Lactide-Dextran (HEMA-LLA-D) macromer. Various copolymeric cryogels of these two monomers are prepared by cryopolymerization yielding macroporous gels (cryogels). For the plain pNIPA cryogel, the SAXS curves obtained at each temperature are well fitted by a sum of four equations describing respectively the scattering resulting from the gel surface (power law), from the solid-like (Guinier equation) and liquid-like (Ornstein-Zernike equation) heterogeneities and from the chain-chain correlation yielding a broad peak (pseudo-Voigt equation) in the high-q domain. The temperature dependence of the parameters obtained from the fit is analyzed and discussed. It is shown that the existence of an isoscattering (or isosbestic) point observed in pNIPA gels and in some copolymers is related to features observed by Differential Scanning Calorimetry and swelling ratio measurements.

  10. Time-resolved small-angle X-ray scattering studies of polymer-silica nanocomposite particles: initial formation and subsequent silica redistribution.

    Science.gov (United States)

    Balmer, Jennifer A; Mykhaylyk, Oleksandr O; Armes, Steven P; Fairclough, J Patrick A; Ryan, Anthony J; Gummel, Jeremie; Murray, Martin W; Murray, Kenneth A; Williams, Neal S J

    2011-02-01

    Small angle X-ray scattering (SAXS) is a powerful characterization technique for the analysis of polymer-silica nanocomposite particles due to their relatively narrow particle size distributions and high electron density contrast between the polymer core and the silica shell. Time-resolved SAXS is used to follow the kinetics of both nanocomposite particle formation (via silica nanoparticle adsorption onto sterically stabilized poly(2-vinylpyridine) (P2VP) latex in dilute aqueous solution) and also the spontaneous redistribution of silica that occurs when such P2VP-silica nanocomposite particles are challenged by the addition of sterically stabilized P2VP latex. Silica adsorption is complete within a few seconds at 20 °C and the rate of adsorption strongly dependent on the extent of silica surface coverage. Similar very short time scales for silica redistribution are consistent with facile silica exchange occurring as a result of rapid interparticle collisions due to Brownian motion; this interpretation is consistent with a zeroth-order Smoluchowski-type calculation. PMID:21171624

  11. Small angle X-ray scattering study of poly(N-isopropyl acrylamide) based cryogels near the volume-phase transition temperature

    Science.gov (United States)

    Chalal, Mohand; Ehrburger-Dolle, Françoise; Morfin, Isabelle; Aguilar de Armas, Maria-Rosa; López, Maria-Luisa; Bley, Françoise

    2010-10-01

    The structural modifications induced by changes in temperature are investigated by Small-Angle X-ray Scattering (SAXS) over a broad range of q-values (3.5×10-2 - 12 nm-1) in cryogels based on N-isopropylacrylamide (NIPA) and/or 2-Hydroxyethyl methacrylate-L-Lactide-Dextran (HEMA-LLA-D) macromer. Various copolymeric cryogels of these two monomers are prepared by cryopolymerization yielding macroporous gels (cryogels). For the plain pNIPA cryogel, the SAXS curves obtained at each temperature are well fitted by a sum of four equations describing respectively the scattering resulting from the gel surface (power law), from the solid-like (Guinier equation) and liquid-like (Ornstein-Zernike equation) heterogeneities and from the chain-chain correlation yielding a broad peak (pseudo-Voigt equation) in the high-q domain. The temperature dependence of the parameters obtained from the fit is analyzed and discussed. It is shown that the existence of an isoscattering (or isosbestic) point observed in pNIPA gels and in some copolymers is related to features observed by Differential Scanning Calorimetry and swelling ratio measurements.

  12. Probing the extent of the Sr2+ ion condensation to anionic polyacrylate coils: A quantitative anomalous small-angle x-ray scattering study

    Science.gov (United States)

    Goerigk, G.; Huber, K.; Schweins, R.

    2007-10-01

    The shrinking process of anionic sodium polyacrylate (NaPA) chains in aqueous solution induced by Sr2+ counterions was analyzed by anomalous small-angle x-ray scattering. Scattering experiments were performed close to the precipitation threshold of strontium polyacrylate. The pure-resonant scattering contribution, which is related to the structural distribution of the Sr2+ counterions, was used to analyze the extent of Sr2+ condensation onto the polyacrylate coils. A series of four samples with different ratios [Sr2+]/[NaPA] (between 0.451 and 0.464) has been investigated. From the quantitative analysis of the resonant invariant, the amount of Sr cations localized in the collapsed phase was calculated with concentrations v¯ between 0.94×1017 and 2.01×1017cm-3 corresponding to an amount of Sr cations in the collapsed phase between 9% and 23% of the total Sr2+ cations in solution. If compared to the concentration of polyacrylate expressed in moles of monomers [NaPA], a degree of site binding of r =[Sr2+]/[NaPA] between 0.05 and 0.11 was estimated. These values clearly differ from r =0.25, which was established from former light scattering experiments, indicating that the counterion condensation starts before the phase border is reached and increases rather sharply at the border.

  13. Wide-angle incidence x-ray waveguides prepared by micro-/nano-technology using crystal surface diffraction

    Science.gov (United States)

    Chen, Sung-Yu; Shen, Yu-Chi; Chiu, Mau-Sen; Chu, Chia-Hung; Stetsko, Yuriy P.; Shew, Bo-Yuan; Chang, Shih-Lin

    2008-03-01

    Grazing incidence x-ray waveguides have been most studied because of its simple geometry and its applicability for all photon energies. However, wide-angle incidence waveguides are also essential for modern x-ray optics, as far as coupling/guiding x-ray beams into given directions are concerned. To investigate this possibility we have prepared waveguides on silicon wafers by x-ray lithographic technique. The waveguides are 100μm high and 1cm long with different widths and the distance between the adjacent waveguides is 2.5 mm. Both the top and bottom surface of a waveguide are plated with gold. With this type of waveguides we have actually observed the effects of guiding x-rays in both lateral and vertical directions using (113) surface diffraction in Au/Si waveguide systems.

  14. Liquid structure of acetic acid-water and trifluoroacetic acid-water mixtures studied by large-angle X-ray scattering and NMR.

    Science.gov (United States)

    Takamuku, Toshiyuki; Kyoshoin, Yasuhiro; Noguchi, Hiroshi; Kusano, Shoji; Yamaguchi, Toshio

    2007-08-01

    The structures of acetic acid (AA), trifluoroacetic acid (TFA), and their aqueous mixtures over the entire range of acid mole fraction xA have been investigated by using large-angle X-ray scattering (LAXS) and NMR techniques. The results from the LAXS experiments have shown that acetic acid molecules mainly form a chain structure via hydrogen bonding in the pure liquid. In acetic acid-water mixtures hydrogen bonds of acetic acid-water and water-water gradually increase with decreasing xA, while the chain structure of acetic acid molecules is moderately ruptured. Hydrogen bonds among water molecules are remarkably formed in acetic acid-water mixtures at xATFA molecules form not a chain structure but cyclic dimers through hydrogen bonding in the pure liquid. In TFA-water mixtures O...O hydrogen bonds among water molecules gradually increase when xA decreases, and hydrogen bonds among water molecules are significantly formed in the mixtures at xATFA molecules are considerably dissociated to hydrogen ions and trifluoroacetate in the mixtures. 1H, 13C, and 19F NMR chemical shifts of acetic acid and TFA molecules for acetic acid-water and TFA-water mixtures have indicated strong relationships between a structural change of the mixtures and the acid mole fraction. On the basis of both LAXS and NMR results, the structural changes of acetic acid-water and TFA-water mixtures with decreasing acid mole fraction and the effects of fluorination of the methyl group on the structure are discussed at the molecular level. PMID:17628099

  15. Small angle X-ray scattering mapping and kinetics study of sub-critical CO{sub 2} sorption by two Australian coals

    Energy Technology Data Exchange (ETDEWEB)

    Radlinski, Andrzej P. [Geoscience Australia, Symonston, Australian Capital Territory 2609 (Australia)]|[Cooperative Research Centre for Greenhouse Gas Technologies, Canberra, Australian Capital Territory 2601 (Australia)]|[Nanoscale Science and Technology Centre, Griffith University, Brisbane, Queensland 4111 (Australia); Busbridge, Tara L.; Gray, Evan Mac A.; Blach, Tomasz P. [Nanoscale Science and Technology Centre, Griffith University, Brisbane, Queensland 4111 (Australia); Cookson, David J. [Australian Synchrotron, Clayton, Victoria 3168 (Australia)]|[School of Physics, University of Melbourne, Victoria 3010 (Australia)

    2009-01-07

    Time- and position-resolved synchrotron small angle X-ray scattering data were acquired from samples of two Australian coal seams: Bulli seam (Bulli 4, R{sub o} = 1.42%, Sydney Basin), which naturally contains CO{sub 2} and Baralaba seam (R{sub o} = 0.67%, Bowen Basin), a potential candidate for sequestering CO{sub 2}. This experimental approach has provided unique, pore-size-specific insights into the kinetics of CO{sub 2} sorption in the micro- and small mesopores (diameter 5 to 175 A) and the density of the sorbed CO{sub 2} at reservoir-like conditions of temperature and hydrostatic pressure. For both samples, at pressures above 5 bar, the density of CO{sub 2} confined in pores was found to be uniform, with no densification in near-wall regions. In the Bulli 4 sample, CO{sub 2} first flooded the slit pores between polyaromatic sheets. In the pore-size range analysed, the confined CO{sub 2} density was close to that of the free CO{sub 2}. The kinetics data are too noisy for reliable quantitative analysis, but qualitatively indicate faster kinetics in mineral-matter-rich regions. In the Baralaba sample, CO{sub 2} preferentially invaded the smallest micropores and the confined CO{sub 2} density was up to five times that of the free CO{sub 2}. Faster CO{sub 2} sorption kinetics was found to be correlated with higher mineral matter content but, the mineral-matter-rich regions had lower-density CO{sub 2} confined in their pores. Remarkably, the kinetics was pore-size dependent, being faster for smaller pores. These results suggest that injection into the permeable section of an interbedded coal-clastic sequence could provide a viable combination of reasonable injectivity and high sorption capacity. (author)

  16. 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 ele

  17. Effects of X-Ray Dose On Rhizosphere Studies Using X-Ray Computed Tomography.

    Directory of Open Access Journals (Sweden)

    Susan Zappala

    Full Text Available X-ray Computed Tomography (CT is a non-destructive imaging technique originally designed for diagnostic medicine, which was adopted for rhizosphere and soil science applications in the early 1980s. X-ray CT enables researchers to simultaneously visualise and quantify the heterogeneous soil matrix of mineral grains, organic matter, air-filled pores and water-filled pores. Additionally, X-ray CT allows visualisation of plant roots in situ without the need for traditional invasive methods such as root washing. However, one routinely unreported aspect of X-ray CT is the potential effect of X-ray dose on the soil-borne microorganisms and plants in rhizosphere investigations. Here we aimed to i highlight the need for more consistent reporting of X-ray CT parameters for dose to sample, ii to provide an overview of previously reported impacts of X-rays on soil microorganisms and plant roots and iii present new data investigating the response of plant roots and microbial communities to X-ray exposure. Fewer than 5% of the 126 publications included in the literature review contained sufficient information to calculate dose and only 2.4% of the publications explicitly state an estimate of dose received by each sample. We conducted a study involving rice roots growing in soil, observing no significant difference between the numbers of root tips, root volume and total root length in scanned versus unscanned samples. In parallel, a soil microbe experiment scanning samples over a total of 24 weeks observed no significant difference between the scanned and unscanned microbial biomass values. We conclude from the literature review and our own experiments that X-ray CT does not impact plant growth or soil microbial populations when employing a low level of dose (<30 Gy. However, the call for higher throughput X-ray CT means that doses that biological samples receive are likely to increase and thus should be closely monitored.

  18. Probing ballistic microdrop coalescence by stroboscopic small-angle X-ray scattering

    Science.gov (United States)

    Graceffa, R.; Burghammer, M.; Davies, R. J.; Riekel, C.

    2012-12-01

    The coalescence of ballistic microdrops has been explored by stroboscopic synchrotron radiation microbeam small-angle X-ray scattering (μSAXS). About 80 μm diameter microdrops generated by a drop-on-demand inkjet system travelled at ˜1.7 m/s through a ˜1 μm X-ray beam. Microdrops of cytochrome C and acetate buffer solutions were merged in order to study the pH driven conformational change. μSAXS patterns were accumulated on a pixel detector, which was activated for a few μsec during the transit time of each microdrop through the microbeam. Local probing of the merging microdrops reveals the internal protein solution flow.

  19. Mean glandular dose for different angles of the X-ray tube using different glandularity phantoms

    International Nuclear Information System (INIS)

    Digital breast tomosynthesis (DBT) is a three-dimensional radiographic technique that is beginning to be used as part of an imaging diagnostic program in some of Brazilian clinical practices. Studies are needed to evaluate the performance and to determine the radiation dose of patients that are undergoing this new procedure. The aim of this work is to present results of the mean glandular dose (DG) for different angles of the X-ray tube using a computed radiography (CR) mammography unit and different glandularity standard breast phantoms. DG values were derived from measurements of the incident air kerma (Ki) and tabulated conversion coefficients that are dependent on the half-value layer (HVL) of the X-ray spectrum. Irradiations were done in a 3000 Nova model Siemens MAMMOMAT mammography unit with the X-ray tube angle ranging from −30° to 30°. The protocol with 28 kV was used for Mo/Mo combination. The distance between focus and the 90×5–6 M model Radcal ionization chamber was 60.5 cm and the tube loading (PIt) used was 50 mA s. Exposures were done for DG determination using the semi-automatic exposure control mode and the 45 mm Computerized Imaging Reference Systems, Inc phantoms which approximately simulate a standard breast with glandularities of 0, 30, 50, 70 and 100%. DG values ranged from 1.3±0.1 to 7.6±0.7 mGy. The results are in according to the reference level of 3 mGy established by the International Basic Safety Standards (BSS115) to breast with 45 mm of thickness, 50% of glandularity and for the X-ray tube positioned in 0°. The results showed that DG increases with the glandularity and with the rotation of the X-ray tube. This work contributes to begin in Brazil the dosimetry in DBT equipments using different protocols and target/filter combinations. - Highlights: ► Glandularity phantoms and a computed radiography mammography unit were used. ► Results were calculated from the incident air kerma and conversion coefficients. ► They are in

  20. High-pressure structural transformations of PbCrO{sub 4} up to 51.2 GPa: An angle-dispersive synchrotron X-ray diffraction study

    Energy Technology Data Exchange (ETDEWEB)

    Errandonea, D., E-mail: daniel.errandonea@uv.es [Departamento de Física Aplicada-ICMUV, MALTA Consolider Team, Universidad de Valencia, Edificio de Investigación, C/Dr. Moliner 50, Burjassot, 46100 Valencia (Spain); Kumar, R.S. [High Pressure Science and Engineering Center, Department of Physics and Astronomy, University of Nevada Las Vegas, 4505 Maryland Parkway, Las Vegas, Nevada 89154-4002 (United States)

    2014-12-15

    Highlights: • PbCrO{sub 4} was studied under high pressure up to 51 GPa using synchrotron powder XRD. • The occurrence of three phase transitions is reported. • The crystal structures of the high-pressure phases are assigned. • Axial and bulk compressibilities are determined. - Abstract: We report on high-pressure X-ray diffraction measurements up to 51.2 GPa in PbCrO{sub 4} at room temperature. Three high-pressure phases with structures different than the ambient-pressure monazite-type (P2{sub 1}/n) are reported. One phase transition was found at 3.8 GPa to an isomorphic structure to monazite. A second transition occurs at 11.1 GPa. After this transition, the coexistence of tetragonal (I4{sub 1}/a) and monoclinic (P2{sub 1}) structures is detected up to 21.1 GPa. Beyond this pressure and up to 51.2 GPa, only the high-pressure monoclinic phase is observed. Upon decompression all structural changes are reversible. Finally, the axial compressibilities for the different phases have been determined as well as the equations of state.

  1. X-Ray Exam: Bone Age Study (For Parents)

    Science.gov (United States)

    ... Your Child All About Food Allergies X-Ray Exam: Bone Age Study KidsHealth > For Parents > X-Ray Exam: Bone Age Study Print A A A Text ... MORE ON THIS TOPIC Precocious Puberty X-Ray Exam: Wrist What Is a Growth Disorder? Turner Syndrome ...

  2. Laser-based X-ray and electron source for X-ray fluorescence studies

    CERN Document Server

    Brozas, F Valle; Roso, L; Conde, A Peralta

    2016-01-01

    In this work we present a modification to conventional X-rays fluorescence using electrons as excitation source, and compare it with the traditional X-ray excitation for the study of pigments. For this purpose we have constructed a laser-based source capable to produce X-rays as well as electrons. Because of the large penetration depth of X-rays, the collected fluorescence signal is a combination of several material layers of the artwork under study. However electrons are stopped in the first layers allowing therefore a more superficial analysis. We show that the combination of both excitation sources can provide extremely valuable information about the structure of the artwork.

  3. Hard X-Ray, Soft X-Ray, and EUV Studies of Solar Eruptions

    Science.gov (United States)

    Sterling, Alphonse C.; Wagner, William (Technical Monitor)

    2003-01-01

    Document study the hard X-ray (HXR), soft X-ray (SXR) ,EUV, and magnetic nature of solar eruptions, with the objective of elucidating the physics of the eruption process. In particular, it was examine the viability of two specific eruption mechanisms, detailed in our proposal. These mechanisms are the "breakout model", and the "tether cutting model". During the second year, it was a significant progress in the goals to Data Sets Utilized. In the publications during this second year of the grant period, the data was used from the E W Imaging Telescope (EIT) and the Michelson Doppler Imager (MDI) instruments on SOHO, and from the Soft X-ray Telescope (SXT), Hard X-ray Telescope (HXT), and the Bragg Crystal Spectrometer (BCS) on Yooh.

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

    International Nuclear Information System (INIS)

    A set of quantitative techniques is suggested for assessing SAXS data quality. These are applied in the form of a script, SAXStats, to a test set of 27 proteins, showing that these techniques are more sensitive than manual assessment of data quality. 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. 3-d chemical imaging using angle-scan nanotomography in a soft X-ray scanning transmission X-ray microscope

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

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

    1993-01-01

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

  7. Study of minimizing X-ray source region of calcium and phosphorous in hard tissue by X-ray microanalysis

    International Nuclear Information System (INIS)

    X-ray microprobe analysis (XMA) is the best method at present to analyze the quantitative concentration of calcium (Ca) or phosphorous (P) in hard tissues. However, the analytic area on intertubular dentin was not larger than the X-ray source region of Ca or P under the usual conditions of the XMA system. In this study, we considered reduction of the X-ray source region. XMA was conducted using a S-2500 CX scanning electron microscope (SEM: Hitachi, Tokyo, Japan) fitted with a Quantum delta IV energy-dispersive X-ray analytical system (EDX: Kevex, San Carlos, USA). We observed changes in X-ray source region with accelerated voltages (ACC. voltage) of SEM, and changes in analytic contents in a sample surface at various tilt angles. Consequently, the analytic area was able to be decreased on a sample surface at a tilt angle of 27.5 deg under a lower ACC. voltage of SEM. Actually, we analyzed Ca and P in the incisor rat dentin surface at the tilt angle 27.5 deg. Analytic portions were intertubular or peritubular dentin on the labial side in an incisor dentin. In this case, the SEM was operated at 7, 10 and 15 kV ACC. voltage with a 0.1 nA probe current. Then, XMAs were conducted for quantitative Ca and P in the intertubular and peritubular dentin on the lingual, proximal, distal, and labial sides in the incisor dentin. Though an ACC. voltage of 7 kV was able to obtain the most exact concentration in the results for intertubular or peritubular dentin, there was no significant difference against measurement values with 10 kV. The Ca content in the peritubular dentin on the labial side was higher than the measured value of peritubular dentin on the lingual side. (author)

  8. Angle-resolved x-ray circular and magnetic circular dichroisms: Definitions and applications

    OpenAIRE

    Tong, DSY; X Guo; Tobin, JG; Waddill, GD

    1996-01-01

    We introduce definitions of angle-resolved x-ray circular dichroism (ARXCD) and magnetic x-ray circular dichroism (ARMXCD). As defined, the much larger effect of circular dichroism (ARXCD) is separated from the smaller magnetic (ARMXCD) effect. In all materials, ARXCD is zero along mirror planes while nonzero elsewhere. ARMXCD is nonzero only in magnetic materials. The measurement and analysis of ARMXCD allow element specific surface magnetism and surface structure as well as their inter-rela...

  9. High energy x-ray phase contrast CT using glancing-angle grating interferometers

    Energy Technology Data Exchange (ETDEWEB)

    Sarapata, A., E-mail: adrian.sarapata@tum.de [Department of Physics and Astronomy, Johns Hopkins University, Baltimore, Maryland 21218 and Department of Physics and Institute of Medical Engineering, Technische Universität München, 85748 Garching (Germany); Stayman, J. W.; Siewerdsen, J. H. [Department of Biomedical Engineering, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Finkenthal, M.; Stutman, D. [Department of Physics and Astronomy, Johns Hopkins University, Baltimore, Maryland 21218 (United States); Pfeiffer, F. [Department of Physics and Institute of Medical Engineering, Technische Universität München, 85748 Garching (Germany)

    2014-02-15

    Purpose: The authors present initial progress toward a clinically compatible x-ray phase contrast CT system, using glancing-angle x-ray grating interferometry to provide high contrast soft tissue images at estimated by computer simulation dose levels comparable to conventional absorption based CT. Methods: DPC-CT scans of a joint phantom and of soft tissues were performed in order to answer several important questions from a clinical setup point of view. A comparison between high and low fringe visibility systems is presented. The standard phase stepping method was compared with sliding window interlaced scanning. Using estimated dose values obtained with a Monte-Carlo code the authors studied the dependence of the phase image contrast on exposure time and dose. Results: Using a glancing angle interferometer at high x-ray energy (∼45 keV mean value) in combination with a conventional x-ray tube the authors achieved fringe visibility values of nearly 50%, never reported before. High fringe visibility is shown to be an indispensable parameter for a potential clinical scanner. Sliding window interlaced scanning proved to have higher SNRs and CNRs in a region of interest and to also be a crucial part of a low dose CT system. DPC-CT images of a soft tissue phantom at exposures in the range typical for absorption based CT of musculoskeletal extremities were obtained. Assuming a human knee as the CT target, good soft tissue phase contrast could be obtained at an estimated absorbed dose level around 8 mGy, similar to conventional CT. Conclusions: DPC-CT with glancing-angle interferometers provides improved soft tissue contrast over absorption CT even at clinically compatible dose levels (estimated by a Monte-Carlo computer simulation). Further steps in image processing, data reconstruction, and spectral matching could make the technique fully clinically compatible. Nevertheless, due to its increased scan time and complexity the technique should be thought of not as

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

    International Nuclear Information System (INIS)

    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® 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 (β) 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: ► SAXS was used for morphological and crystalline studies of PHBV/OMMT nanocomposites. ► The crystalline structure was influenced by the presence of clay. ► The degree of clay dispersion in a polymer matrix was quantified. ► The morphology comprised exfoliated particles, nanoscale and microscale clusters. ► The results obtained by SAXS agreed well with TEM and WAXD results.

  11. 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.

  12. Microfibril angle variability in Masson Pine (Pinus massoniana Lamb.) using X-ray diffraction

    Institute of Scientific and Technical Information of China (English)

    Zhang Bo; Fei Ben-hua; Yu Yan; Zhao Rong-jun

    2007-01-01

    The microfibril angle of fiber walls is an ultra-microscopic feature affecting the performance of wood products. It is therefore essential to get more definitive information to improve selection and utilization. X-ray diffraction is a rapid method for measuring micro fibril angles. In this paper, the variability of microfibril angle in plantation-grown Masson pine was investigated by peak-fitting method. This method was compared with the traditional hand-drawn method, 40% peak height method and half peak height method. X-ray diffraction measurements indicated that the microfibril angle changed as a function of the position in the tree.The mean micro fibril angle decreased more gradually as the distance increased from the pith and reached the same level in mature wood. The microfibril angle also seemed to decrease clearly from the base upward. Differences of angle-intensity curves between heartwood and sapwood were also examined.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-10-15

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

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

    International Nuclear Information System (INIS)

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

  15. Spectroscopic studies of X-ray laser media

    International Nuclear Information System (INIS)

    velocity effects, τ0, the ratio of the spatial scalelength of the absorption coefficient to the Doppler decoupling length, R and the angle of the ray path to the normal to the planes. The net radiative bracket found to be related to the total optical depth, τ0tot, the R ratio and the optical depth at the emission point neglecting the velocity decoupling effects, τr. Results of an experiment carried out to generate wave-guides for x-ray lasers to minimise the transverse refraction losses are presented. Five beams of the VULCAN laser were used to illuminate 40 mm long Ge targets leading to well saturated Ge XRL outputs at 196A. Simulated x-ray laser output has been fitted to experimentally measured outputs to find the actual incident energy needed to allow for unmodelled energy losses in the absorption process. The input irradiances to the EHYBRID fluid and atomic physics code have been reduced by a factor F from the experimental irradiance until the code predictions and experimental results agree. After removing a previously utilised reduction of the monopole excitation rate in Ne-like ions, we found that a factor F = 0.7 gives simulated x-ray laser output energy for Ne-like Ge at 196 A in agreement with experiment for 75 ps irradiation. The uniformity of the line foci created with the five overlapping beams has been studied by simulating cross-slit camera images using EHYBRID code. The x-ray laser output was incident onto a short (∼ 4 mm) length of plasma irradiated to produce a density 'well' along the line focus length which acts a one-dimensional wave-guide. Analysing the XRL outputs from 40 mm long Ge targets with and without using the wave-guide showed that there was no amplification of the x-ray laser passing through the wave-guide. Some waveguiding without gain may have been achieved as the x-ray laser beam divergence was reduced after passing through the waveguiding plasma. Results from an experiment on travelling wave pumping of the Ne-like Ge x-ray lasers in

  16. 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.

    Science.gov (United States)

    Zhao, Nie; Yang, Chunming; Wang, Yuzhu; Zhao, Binyu; Bian, Fenggang; Li, Xiuhong; Wang, Jie

    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. PMID:26478320

  17. Design studies for ITER x-ray diagnostics

    International Nuclear Information System (INIS)

    Concepts for adapting conventional tokamak x-ray diagnostics to the harsh radiation environment of ITER include use of grazing-incidence (GI) x-ray mirrors or man-made Bragg multilayer (ML) elements to remove the x-ray beam from the neutron beam, or use of bundles of glass-capillary x-ray ''light pipes'' embedded in radiation shields to reduce the neutron/gamma-ray fluxes onto the detectors while maintaining usable x-ray throughput. The x-ray optical element with the broadest bandwidth and highest throughput, the GI mirror, can provide adequate lateral deflection (10 cm for a deflected-path length of 8 m) at x-ray energies up to 12, 22, or 30 keV for one, two, or three deflections, respectively. This element can be used with the broad band, high intensity x-ray imaging system (XIS), the pulseheight analysis (PHA) survey spectrometer, or the high resolution Johann x-ray crystal spectrometer (XCS), which is used for ion-temperature measurement. The ML mirrors can isolate the detector from the neutron beam with a single deflection for energies up to 50 keV, but have much narrower bandwidth and lower x-ray power throughput than do the GI mirrors; they are unsuitable for use with the XIS or PHA, but they could be used with the XCS; in particular, these deflectors could be used between ITER and the biological shield to avoid direct plasma neutron streaming through the biological shield. Graded-d ML mirrors have good reflectivity from 20 to 70 keV, but still at grazing angles (<3 mrad). The efficiency at 70 keV for double reflection (10 percent), as required for adequate separation of the x-ray and neutron beams, is high enough for PHA requirements, but not for the XIS. Further optimization may be possible

  18. A filter based analyzer for studies of X-ray Raman scattering

    CERN Document Server

    Seidler, G T

    2001-01-01

    Non-resonant X-ray Raman scattering (XRS) with hard X-rays holds the potential for measuring local structure and local electronic properties around low-Z atoms in environments where traditional soft X-ray techniques are inapplicable. However, the small cross-section for XRS requires that experiments must simultaneously achieve high detection efficiency, large collection solid angles, and good energy resolution. We report here that a simple X-ray analyzer consisting of an absorber and a point-focusing spatial filter can be used to study some X-ray Raman near-edge features. This apparatus has greater than 10% detection efficiency, has an energy resolution of 8 eV, and can be readily extended to collection angles of more than 1 sr. We present preliminary measurements of the XRS from the nitrogen 1 s shell in pyrolitic boron nitride.

  19. Application of X-ray absorption spectroscopy and anomalous small angle scattering to RNA polymerase

    International Nuclear Information System (INIS)

    X-ray absorption spectroscopy is ideally suited for the investigation of the electronic structure and the local environment (≤∝5 A) of specific atoms in biomolecules. While the edge region provides information about the valence state of the absorbing atom, the chemical identity of neighboring atoms, and the coordination geometry, the EXAFS region contains information about the number and average distance of neighboring atoms and their relative disorder. The development of sensitive detection methods has allowed studies using near-physiological concentrations (as low as ∝100 μM). With careful choice of model compounds, judicious use of fitting procedures, and consideration of the results of biochemical and other spectrOScopic results, this data has provided pivotal information about the structures of these active sites which store energy in their conformation changes or ligand exchanges. Although the application of anomalous small angle scattering to biomolecules has occurred more recently, it clearly provides a method of determining distances between active sites that are outside the range of X-ray absorption spectroscopy. The wavelength dependence of the X-ray scattering power varies rapidly near the edge of the absorbing atom in both amplitude and phase. This behavior selectively alters the contribution of the absorbing atom to the scattering pattern. The structure-function relationship of the intermediate states provide the key to understanding the mechanisms of these complex molecules. It is this precise structural information about the active sites that is not obtainable by other spectroscopic techniques. Combination of these techniques offers a unique approach to the determination of the organization of active sites in biomolecules, especially metalloenzymes. Application of these methods to the substrate and template binding sites of RNA polymerase which contain zinc atoms demonstrates the versatility of this approach. (orig.)

  20. Fabrication of large-area and low mass critical-angle x-ray transmission gratings

    Science.gov (United States)

    Heilmann, Ralf K.; Bruccoleri, Alex R.; Guan, Dong; Schattenburg, Mark L.

    2014-07-01

    Soft x-ray spectroscopy of celestial sources with high resolving power R = E/ΔE and large collecting area addresses important science listed in the Astro2010 Decadal Survey New Worlds New Horizons, such as the growth of the large scale structure of the universe and its interaction with active galactic nuclei, the kinematics of galactic outflows, as well as coronal emission from stars and other topics. Numerous studies have shown that a transmission grating spectrometer based on lightweight critical-angle transmission (CAT) gratings can deliver R = 3000-5000 and large collecting area with high efficiency and minimal resource requirements, providing spectroscopic figures of merit at least an order of magnitude better than grating spectrometers on Chandra and XMM-Newton, as well as future calorimeter-based missions. The recently developed CAT gratings combine the advantages of transmission gratings (low mass, relaxed figure and alignment tolerances) and blazed reflection gratings (high broad band diffraction efficiency, utilization of higher diffraction orders). Their working principle based on blazing through reflection off the smooth, ultra-high aspect ratio grating bar sidewalls has previously been demonstrated on small samples with x rays. For larger gratings (area greater than 1 inch square) we developed a fabrication process for grating membranes with a hierarchy of integrated low-obscuration supports. The fabrication involves a combination of advanced lithography and highly anisotropic dry and wet etching techniques. We report on the latest fabrication results of free-standing, large-area CAT gratings with polished sidewalls and preliminary x-ray tests.

  1. Dark field X-ray microscopy for studies of recrystallization

    DEFF Research Database (Denmark)

    Ahl, Sonja Rosenlund; Simons, Hugh; Jakobsen, Anders Clemen;

    2015-01-01

    We present the recently developed technique of Dark Field X-Ray Microscopy that utilizes the diffraction of hard X-rays from individual grains or subgrains at the (sub)micrometre- scale embedded within mm-sized samples. By magnifying the diffracted signal, 3D mapping of orientations and strains...... external influences. The capabilities of Dark Field X- Ray Microscopy are illustrated by examples from an ongoing study of recrystallization of 50% cold-rolled Al1050 specimens....

  2. Image reconstruction from limited angle projections collected by multi-source interior x-ray imaging systems

    OpenAIRE

    Liu, Baodong; Wang, Ge; Ritman, Erik L.; Cao, Guohua; Lu, Jianping; Zhou, Otto; Zeng, Li; Yu, Hengyong

    2011-01-01

    A multi-source x-ray interior imaging system with limited angle scanning is investigated to study the possibility of building an ultra-fast micro-CT for dynamic small animal imaging. And two methods are employed to perform interior reconstruction from a limited number of projections collected by the multi-source interior x-ray system. The first is total variation minimization with the steepest descent search (TVM-SD) and the second is total difference minimization with soft-threshold filterin...

  3. Watching nanoparticles form: an in situ (small-/wide-angle X-ray scattering/total scattering) study of the growth of yttria-stabilised zirconia in supercritical fluids.

    Science.gov (United States)

    Tyrsted, Christoffer; Pauw, Brian Richard; Jensen, Kirsten Marie Ørnsbjerg; Becker, Jacob; Christensen, Mogens; Iversen, Bo Brummerstedt

    2012-04-27

    Understanding nanoparticle-formation reactions requires multi-technique in situ characterisation, since no single characterisation technique provides adequate information. Here, the first combined small-angle X-ray scattering (SAXS)/wide-angle X-ray scattering (WAXS)/total-scattering study of nanoparticle formation is presented. We report on the formation and growth of yttria-stabilised zirconia (YSZ) under the extreme conditions of supercritical methanol for particles with Y(2)O(3) equivalent molar fractions of 0, 4, 8, 12 and 25 %. Simultaneous in situ SAXS and WAXS reveals a quick formation (seconds) of sub-nanometre amorphous material forming larger agglomerates with subsequent slow crystallisation (minutes) into nanocrystallites. The amount of yttria dopant is shown to strongly affect the crystallite size and unit-cell dimensions. At yttria-doping levels larger than 8 %, which is known to be the stoichiometry with maximum ionic conductivity, the strain on the crystal lattice is significantly increased. Time-resolved nanoparticle size distributions are calculated based on whole-powder-pattern modelling of the WAXS data, which reveals that concurrent with increasing average particle sizes, a broadening of the particle-size distributions occur. In situ total scattering provides structural insight into the sub-nanometre amorphous phase prior to crystallite growth, and the data reveal an atomic rearrangement from six-coordinated zirconium atoms in the initial amorphous clusters to eight-coordinated zirconia atoms in stable crystallites. Representative samples prepared ex situ and investigated by transmission electron microscopy confirm a transformation from an amorphous material to crystalline nanoparticles upon increased synthesis duration. PMID:22447391

  4. Density of hydrophobically confined deeply cooled water investigated by small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Kao-Hsiang, E-mail: codeliu@gmail.com [Department of Chemistry, National Taiwan University, Taipei 10617, Taiwan (China); Joint Institute for Neutron Science, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Zhang, Yang [Department of Nuclear, Plasma, and Radiological Engineering, University of Illinois at Urbana-Champaign, Urbana, Illinois 61801 (United States); Jeng, U-Ser [National Synchrotron Radiation Research Center, Hsinchu 30076, Taiwan (China); Mou, Chung-Yuan [Department of Chemistry, National Taiwan University, Taipei 10617, Taiwan (China)

    2015-09-07

    Water’s behavior near hydrophobic surfaces has attracted great attention due to chemical and geological applications. Here, we report small angle X-ray scattering (SAXS) studies of water confined in the hydrophobic nanoporous carbon material, CMK-1-14, from ambient to deeply cooled temperatures. By monitoring the scattering intensity of the first Bragg peak, which is directly related to the scattering length density contrast between the carbon matrix and the confined water, the average density of the hydrophobically confined water was determined from 300 K to 150 K at ambient pressure. Furthermore, differential scanning calorimetry and X-ray diffraction measurements showed that the majority of such hydrophobically confined water did not crystallize in the investigated temperature range. By exploiting the fast speed of SAXS measurements and the continuous temperature ramping, the average density profile and the deduced thermal expansion coefficient (α{sub p}) were obtained. We found that the well-known density maximum of water at 277 K downshifted to 260 K, and the density minimum which has been observed in hydrophilic confinement disappeared. In addition, the previously measured large density decreasing of 18% at low temperature was recalibrated to a more reasonable 10% instead. Consequently, the recalculated α{sub p} peak was found to be quite similar to that of the water confined in hydrophilic MCM-41-S-15 suggesting an intrinsic property of water, which does not sensitively depend on the confinement surface.

  5. Density of hydrophobically confined deeply cooled water investigated by small angle X-ray scattering.

    Science.gov (United States)

    Liu, Kao-Hsiang; Zhang, Yang; Jeng, U-Ser; Mou, Chung-Yuan

    2015-09-01

    Water's behavior near hydrophobic surfaces has attracted great attention due to chemical and geological applications. Here, we report small angle X-ray scattering (SAXS) studies of water confined in the hydrophobic nanoporous carbon material, CMK-1-14, from ambient to deeply cooled temperatures. By monitoring the scattering intensity of the first Bragg peak, which is directly related to the scattering length density contrast between the carbon matrix and the confined water, the average density of the hydrophobically confined water was determined from 300 K to 150 K at ambient pressure. Furthermore, differential scanning calorimetry and X-ray diffraction measurements showed that the majority of such hydrophobically confined water did not crystallize in the investigated temperature range. By exploiting the fast speed of SAXS measurements and the continuous temperature ramping, the average density profile and the deduced thermal expansion coefficient (αp) were obtained. We found that the well-known density maximum of water at 277 K downshifted to 260 K, and the density minimum which has been observed in hydrophilic confinement disappeared. In addition, the previously measured large density decreasing of 18% at low temperature was recalibrated to a more reasonable 10% instead. Consequently, the recalculated αp peak was found to be quite similar to that of the water confined in hydrophilic MCM-41-S-15 suggesting an intrinsic property of water, which does not sensitively depend on the confinement surface. PMID:26342380

  6. Density of hydrophobically confined deeply cooled water investigated by small angle X-ray scattering

    International Nuclear Information System (INIS)

    Water’s behavior near hydrophobic surfaces has attracted great attention due to chemical and geological applications. Here, we report small angle X-ray scattering (SAXS) studies of water confined in the hydrophobic nanoporous carbon material, CMK-1-14, from ambient to deeply cooled temperatures. By monitoring the scattering intensity of the first Bragg peak, which is directly related to the scattering length density contrast between the carbon matrix and the confined water, the average density of the hydrophobically confined water was determined from 300 K to 150 K at ambient pressure. Furthermore, differential scanning calorimetry and X-ray diffraction measurements showed that the majority of such hydrophobically confined water did not crystallize in the investigated temperature range. By exploiting the fast speed of SAXS measurements and the continuous temperature ramping, the average density profile and the deduced thermal expansion coefficient (αp) were obtained. We found that the well-known density maximum of water at 277 K downshifted to 260 K, and the density minimum which has been observed in hydrophilic confinement disappeared. In addition, the previously measured large density decreasing of 18% at low temperature was recalibrated to a more reasonable 10% instead. Consequently, the recalculated αp peak was found to be quite similar to that of the water confined in hydrophilic MCM-41-S-15 suggesting an intrinsic property of water, which does not sensitively depend on the confinement surface

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

    DEFF Research Database (Denmark)

    Tian, Xinsheng; Langkilde, Annette Eva; Thorolfsson, Matthias; Rasmussen, Hanne B; Vestergaard, Bente

    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 a...

  8. Reflection of parametric X-ray radiation at the right angle to the particle beam

    International Nuclear Information System (INIS)

    The angular distribution (AD) of the yield in the reflection of parametric X-ray radiation (PXR), generated by relativistic particles in a crystal at the right angle to the particle beam, is considered theoretically. It is shown that the AD should have five singular points. 23 refs., 2 figs

  9. Improved signal-to-noise ratio for non-perpendicular detection angles in x-ray fluorescence computed tomography (XFCT)

    Science.gov (United States)

    Sjölin, Martin; Danielsson, Mats

    2014-11-01

    The standard imaging setup in x-ray fluorescence computed tomography detects the fluorescence emission at a right angle with respect to the axis of the excitation beam. In this paper we have studied how the detection angle affects the signal-to-noise ratio (S/N), which is a major factor influencing the low-contrast sensitivity of the imaging system. This is done for an imaging setup using a collimated detector and a pencil beam of excitation x-rays. An ideal detection process is simulated for a generalized imaging case with gold/platinum tracers and experimental measurements are performed using a diagnostic x-ray tube. For monochromatic excitation, the results indicate that order-of-magnitude improvements of the S/N can be achieved by optimizing the detection angle. The maximal S/N, when exciting with an energy just above the K-edge, is achieved for large detection angles, i.e. with the detector close to the source. The improvements also transfer to polychromatic excitation sources and the experimental results show up to four-fold improvements of the S/N when changing the detection angle from 90° to 150°. Also, the changes of the S/N behavior when switching the fluorescent tracer is briefly demonstrated. These results suggest that the choice of detection angle should be taken seriously in the design of future XFCT imaging systems.

  10. 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.

  11. Crystallization and melting behavior of polymer blend observed by microbeam small-angle x-ray scattering

    International Nuclear Information System (INIS)

    The microbeam small angle x-ray scattering (SAXS) technique gives the novel information about micron-scale structural distribution (or inhomogeneity). By using microbeam SAXS, we have studied the crystallization and melting behavior of miscible polymer blend PCL (poly- ε caprolactone)/PVB (poly-vinyl butyral). In PCL/PVB, the very large spherulite with highly regular band structure is formed because of low frequency of nucleation. By irradiating an X-ray microbeam near the edge of the spherulite, we have measured the lamella formation at the growth front. It is found that PCL/PVB crystal has two populations of lamella bundle (longer and usual periodic structure) and the very long periodic structure grows before the appearance of the usual lamella period. We have also scanned the X-ray microbeam along the radial direction of the spherulite and have observed a periodic change of SAXS intensity, the period of which corresponds to the band period. (author)

  12. Influence of angle's ranges for recording an X-ray fluorescence hologram on reconstructed atomic images

    Institute of Scientific and Technical Information of China (English)

    XIE Hong-Lan; CHEN Jian-Wen; GAO Hong-Yi; ZHU Hua-Feng; LI Ru-Xin; XU Zhi-Zhan

    2004-01-01

    X-ray fluorescence holography (XFH) is a novel method for three-dimensional (3D) imaging of atomic structure. Theoretically, in an XFH experiment, one has to measure the fluorescence energy on a spherical surface to get well-resolved 3D images of atoms. But in practice, the experimental system arrangement does not allow the measurement of the fluorescent intensity oscillations in the full sphere. The holographic information losses because of the limited sampling range (less than 4π) will directly result in defective reconstructed atomic images. In this work, the atomic image of a Fe single crystal (001) was reconstructed by numerically simulating X-ray fluorescence holograms of the crystal at different recording angle's ranges and step lengths. Influences of the ranges of azimuth angles and polar angles and the step length of polar angles on the reconstructed atomic images were discussed.

  13. Microfocus wide-angle X-ray scattering of polymers crystallized in a fast scanning chip calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Drongelen, Martin van [Eindhoven University of Technology, 5600 MB Eindhoven (Netherlands); Meijer-Vissers, Tamara [Eindhoven University of Technology, 5600 MB Eindhoven (Netherlands); Dutch Polymer Institute (DPI), P.O. Box 902, 5600 AX Eindhoven (Netherlands); Cavallo, Dario, E-mail: d.cavallo1@tue.nl [Eindhoven University of Technology, 5600 MB Eindhoven (Netherlands); Portale, Giuseppe [ESRF, Dubble CRG, Netherlands Organization of Scientific Research (NWO), 38043 Grenoble (France); Poel, Geert Vanden [DSM Resolve, Urmonderbaan 22, 6167 RD Geleen (Netherlands); Androsch, René, E-mail: rene.androsch@iw.uni-halle.de [Martin-Luther-University Halle-Wittenberg, Center of Engineering Sciences, 06099 Halle/Saale (Germany)

    2013-07-10

    Graphical abstract: - Highlights: • Micro-focused synchrotron radiation was used for WAXS analysis of FSC samples. • FSC polymer crystallization experiments were completed by in situ X-ray structure analysis. • The supercooling-controlled polymorphism of iPP and PA 6 has been confirmed. - Abstract: Microfocus wide-angle X-ray scattering (WAXS) has been applied for analysis of the polymorphism of isotactic polypropylene and polyamide 6 prepared in a fast scanning chip calorimeter (FSC). Samples with a typical mass of few hundred nanograms, and lateral dimension and thickness of about 100 μm and 20 μm, respectively, were exposed to a defined thermal history in the FSC and subsequently analyzed regarding the X-ray structure at ambient temperature using an intense synchrotron microfocused X-ray beam. The relaxed melt of isotactic polypropylene was cooled at rates of 40 K s{sup −1} and 200 K s{sup −1} which allowed formation of α-crystals or mesophase, respectively. Polyamide 6 was isothermally crystallized at 95 °C and 180 °C which led to formation of γ-mesophase and α-crystals, respectively. This study demonstrated, for the first time, that FSC polymer crystallization experiments could be completed and expanded by subsequent in situ structure analysis by X-ray scattering.

  14. X-ray Studies of Flaring Plasma

    Indian Academy of Sciences (India)

    B. Sylwester; J. Sylwester; K. J. H. Phillips

    2008-03-01

    We present some methods of X-ray data analysis employed in our laboratory for deducing the physical parameters of flaring plasma. For example, we have used a flare well observed with Polish instrument RESIK aboard Russian CORONAS-F satellite. Based on a careful instrument calibration, the absolute fluxes in a number of individual spectral lines have been obtained. The analysis of these lines allows us to follow the evolution of important thermodynamic parameters characterizing the emitting plasma throughout this flare evolution.

  15. Amorphous silica studied by high energy x-ray diffraction

    DEFF Research Database (Denmark)

    Poulsen, H.F.; Neuefeind, J.; Neumann, H.B.;

    1995-01-01

    The use of hard X-rays (60-300 keV) for diffraction studies of disordered materials has several advantages: higher resolution in direct space, smaller correction terms, removal of truncation effects, the possibility for operating in extreme environments and for direct comparison between X-ray and...

  16. High-resolution X-ray diffraction studies of multilayers

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Hornstrup, Allan; Schnopper, H. W.

    1988-01-01

    High-resolution X-ray diffraction studies of the perfection of state-of-the-art multilayers are presented. Data were obtained using a triple-axis perfect-crystal X-ray diffractometer. Measurements reveal large-scale figure errors in the substrate. A high-resolution triple-axis set up is required...

  17. Planetary X-ray studies: past, present and future

    Science.gov (United States)

    Branduardi-Raymont, Graziella

    2016-07-01

    Our solar system is a fascinating physics laboratory and X-ray observations are now firmly established as a powerful diagnostic tool of the multiple processes taking place in it. The science that X-rays reveal encompasses solar, space plasma and planetary physics, and the response of bodies in the solar system to the impact of the Sun's activity. This talk will review what we know from past observations and what we expect to learn in the short, medium and long term. Observations with Chandra and XMM-Newton have demonstrated that the origin of Jupiter's bright soft X-ray aurorae lies in the Charge eXchange (CX) process, likely to involve the interaction with atmospheric neutrals of local magnetospheric ions, as well as those carried in the solar wind. At higher energies electron bremsstrahlung is thought to be the X-ray emitting mechanism, while the whole planetary disk acts as a mirror for the solar X-ray flux via Thomson and fluorescent scattering. This 'X-ray mirror' phenomenon is all that is observed from Saturn's disk, which otherwise lacks X-ray auroral features. The Earth's X-ray aurora is bright and variable and mostly due to electron bremsstrahlung and line emission from atmospheric species. Un-magnetised planets, Venus and Mars, do not show X-ray aurorae but display the interesting combination of mirroring the solar X-ray flux and producing X-rays by Solar Wind Charge eXchange (SWCX) in their exospheres. These processes respond to different solar stimulation (photons and solar wind plasma respectively) hence their relative contributions are seen to vary according to the Sun's output. Present and future of planetary X-ray studies are very bright. We are preparing for the arrival of the Juno mission at Jupiter this summer and for coordinated observations with Chandra and XMM-Newton on the approach and later during Juno's orbital phase. These will allow direct correlation of the local plasma conditions with the X-ray emissions and the establishment of the

  18. Brain tumor imaging using small-angle x-ray scattering tomography

    Science.gov (United States)

    Jensen, Torben H.; Bech, Martin; Bunk, Oliver; Thomsen, Maria; Menzel, Andreas; Bouchet, Audrey; Le Duc, Géraldine; Feidenhans'l, Robert; Pfeiffer, Franz

    2011-03-01

    We demonstrate high-resolution small-angle x-ray scattering computed tomography (SAXS-CT) of soft matter and soft tissue samples. Complete SAXS patterns over extended ranges of momentum transfer are reconstructed spatially resolved from volumes inside an extended sample. Several SAXS standard samples are used to quantitatively validate the method and demonstrate its performance. Further results on biomedical tissue samples (rat brains) are presented that demonstrate the advantages of the method compared to existing biomedical x-ray imaging approaches. Functional areas of the brains as well as tumor morphology are imaged. By providing insights into the structural organization at the nano-level, SAXS-CT complements and extends results obtainable with standard methods such as x-ray absorption tomography and histology.

  19. Investigation of irradiated biodegradable blends by FTIR and wide-angle X-ray diffraction

    International Nuclear Information System (INIS)

    In the present work, twin screw extruded films of PLLA and PCL biodegradable homopolymers and 50:50 (w:w) blend were irradiated with gamma rays from Co-60 and electron beam at doses in the range of 50 to 500 kGy in order to evaluate the effect of irradiations on homopolymers and blend. The FTIR results have shown that this technique was neither sensitive enough to observe the degradation promoted by ionizing radiation of studied homopolymers and blends and, nor on the miscibility of the blends. Wide-angle X-ray diffraction (WAXD) of PCL samples, non-irradiated and irradiated showed two strongest reflections at angles 2θ = 21.4 o and 2θ = 23.7 o that have been attributed in the literature to the (110) and (200) reflections, respectively. As for extruded non-irradiated and irradiated PLLA, it was observed broad diffusion peaks corresponding to an amorphous polymer. PLLA annealed samples showed reflections at angles 2θ =16.4 o and 2θ =18.7 o previously attributed in the literature to distorted 103 (α-form) helices. It was possible to observe slight alteration of the crystallite size of all irradiated samples of PCL in the dose range studied. (authors)

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

    International Nuclear Information System (INIS)

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

  1. A flexible setup for angle-resolved X-ray fluorescence spectrometry with laboratory sources

    Science.gov (United States)

    Spanier, M.; Herzog, C.; Grötzsch, D.; Kramer, F.; Mantouvalou, I.; Lubeck, J.; Weser, J.; Streeck, C.; Malzer, W.; Beckhoff, B.; Kanngießer, B.

    2016-03-01

    X-ray fluorescence (XRF) analysis is one of the standard tools for the analysis of stratified materials and is widely applied for the investigation of electronics and coatings. The composition and thickness of the layers can be determined quantitatively and non-destructively. Recent work showed that these capabilities can be extended towards retrieving stratigraphic information like concentration depth profiles using angle-resolved XRF (ARXRF). This paper introduces an experimental sample chamber which was developed as a multi-purpose tool enabling different measurement geometries suited for transmission measurements, conventional XRF, ARXRF, etc. The chamber was specifically designed for attaching all kinds of laboratory X-ray sources for the soft and hard X-ray ranges as well as various detection systems. In detail, a setup for ARXRF using an X-ray tube with a polycapillary X-ray lens as source is presented. For such a type of setup, both the spectral and lateral characterizations of the radiation field are crucial for quantitative ARXRF measurements. The characterization is validated with the help of a stratified validation sample.

  2. Multimodal particle size distribution or fractal surface of acrylic acid copolymer nanoparticles: A small-angle X-ray scattering study using direct Fourier and indirect maximum entropy methods

    OpenAIRE

    Mueller, J.J.; Hansen, S; Lukowski, G.; Gast, K.

    1995-01-01

    Acrylic acid copolymers are potential carriers for drug delivery. The surface, surface rugosity and the absolute dimension of the particles are parameters that determine the binding of drugs or detergents, diffusion phenomena at the surface and the distribution of the carrier within the human body. The particle-size distribution and surface rugosity of the particles have been investigated by small-angle X-ray scattering and dynamic light scattering. Direct Fourier transform as well as a new s...

  3. 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.

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

    International Nuclear Information System (INIS)

    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

  5. Micro scale distribution of nanoparticles studied with X-ray near-field scattering

    International Nuclear Information System (INIS)

    In the present study, we investigate the micron-scale inhomogeneous distribution of silica nanoparticles with X-ray near-field scattering. This technique allows us to measure structures of soft matters on a large size scale that is complementary to conventional ultra-small-angle X-ray scattering and/or X-ray imaging. We applied the technique to the observation of the anisotropic structural distribution of silica aggregates in uniaxially stretched rubber. The scattering images show anisotropic butterfly patterns that correspond to the inhomogeneous density distribution of silica aggregates. The spatial distribution of the inhomogeneity in the stretched rubber cab also be determined by this technique. (author)

  6. 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.

  7. Fabrication update on critical-angle transmission gratings for soft x-ray grating spectrometers

    Science.gov (United States)

    Heilmann, Ralf K.; Bruccoleri, Alex; Mukherjee, Pran; Yam, Jonathan; Schattenburg, Mark L.

    2011-09-01

    Diffraction grating-based, wavelength dispersive high-resolution soft x-ray spectroscopy of celestial sources promises to reveal crucial data for the study of the Warm-Hot Intergalactic Medium, the Interstellar Medium, warm absorption and outflows in Active Galactic Nuclei, coronal emission from stars, and other areas of interest to the astrophysics community. Our recently developed critical-angle transmission (CAT) gratings combine the advantages of the Chandra high and medium energy transmission gratings (low mass, high tolerance of misalignments and figure errors, polarization insensitivity) with those of blazed reflection gratings (high broad band diffraction efficiency, high resolution through use of higher diffraction orders) such as the ones on XMM-Newton. Extensive instrument and system configuration studies have shown that a CAT grating-based spectrometer is an outstanding instrument capable of delivering resolving power on the order of 5,000 and high effective area, even with a telescope point-spread function on the order of many arc-seconds. We have fabricated freestanding, ultra-high aspect-ratio CAT grating bars from silicon-on-insulator wafers using both wet and dry etch processes. The 200 nm-period grating bars are supported by an integrated Level 1 support mesh, and a coarser external Level 2 support mesh. The resulting grating membrane is mounted to a frame, resulting in a grating facet. Many such facets comprise a grating array that provides light-weight coverage of large-area telescope apertures. Here we present fabrication results on the integration of CAT gratings and the different high-throughput support mesh levels and on membrane-frame bonding. We also summarize recent x-ray data analysis of 3 and 6 micron deep wet-etched CAT grating prototypes.

  8. Critical-angle transmission grating spectrometer for high-resolution soft x-ray spectroscopy on the International X-ray Observatory

    Science.gov (United States)

    Heilmann, Ralf K.; Davis, John E.; Dewey, Daniel; Bautz, Mark W.; Foster, Rick; Bruccoleri, Alex; Mukherjee, Pran; Robinson, David; Huenemoerder, David P.; Marshall, Herman L.; Schattenburg, Mark L.; Schulz, Norbert S.; Guo, L. Jay; Kaplan, Alex F.; Schweikart, Russell B.

    2010-07-01

    High-resolution spectroscopy at energies below 1 keV covers the lines of C, N, O, Ne and Fe ions, and is central to studies of the Interstellar Medium, the Warm Hot Intergalactic Medium, warm absorption and outflows in Active Galactic Nuclei, coronal emission from stars, etc. The large collecting area, long focal length, and 5 arcsecond half power diameter telescope point-spread function of the International X-ray Observatory will present unprecedented opportunity for a grating spectrometer to address these areas at the forefront of astronomy and astrophysics. We present the current status of a transmission grating spectrometer based on recently developed high-efficiency critical-angle transmission (CAT) gratings that combine the traditional advantages of blazed reflection and transmission gratings. The optical design places light-weight grating arrays close to the telescope mirrors, which maximizes dispersion distance and thus spectral resolution and minimizes demands on mirror performance. It merges features from the Chandra High Energy Transmission Grating Spectrometer and the XMM-Newton Reflection Grating Spectrometer, and provides resolving power R = E/ΔE = 3000 - 5000 (full width half max) and effective area >1000 cm2 in the soft x-ray band. We discuss recent results on ray-tracing and optimization of the optical design, instrument configuration studies, and grating fabrication.

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

    DEFF Research Database (Denmark)

    Als-Nielsen, Jens Aage

    1986-01-01

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

  10. Small angles X-ray diffraction and Mössbauer characterization of annealed Tb/Fe multilayer

    Indian Academy of Sciences (India)

    O M Lemine

    2011-02-01

    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. After annealing at 873 K, a clear total mixing of the multilayers by interdiffusion has been evidenced. The results are compared with the effect of ion irradiation in the same system.

  11. Small-angle neutron and X-ray scattering reveal conformational changes in rhodopsin activation

    Science.gov (United States)

    Shrestha, Utsab R.; Bhowmik, Debsindhu; Perera, Suchitrhanga M. C. D.; Chawla, Udeep; Struts, Andrey V.; Graziono, Vito; Pingali, Sai Venkatesh; Heller, William T.; Qian, Shuo; Brown, Michael F.; Chu, Xiang-Qiang

    2015-03-01

    Understanding G-protein-coupled receptor (GPCR) activation plays a crucial role in the development of novel improved molecular drugs. During photo-activation, the retinal chromophore of the visual GPCR rhodopsin isomerizes from 11-cis to all-trans conformation, yielding an equilibrium between inactive Meta-I and active Meta-II states. The principal goals of this work are to address whether the activation of rhodopsin leads to a single state or a conformational ensemble, and how protein organizational structure changes with detergent environment in solution. We use both small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS) techniques to answer the above questions. For the first time we observe the change in protein conformational ensemble upon photo-activation by SANS with contrast variation, which enables the separate study of the protein structure within the detergent assembly. In addition, SAXS study of protein structure within detergent assembly suggests that the detergent molecules form a belt of monolayer (micelle) around protein with different geometrical shapes to keep the protein in folded state.

  12. Two methods for studying the X-ray variability

    Science.gov (United States)

    Yan, Shu-Ping; Ji, Li; Méndez, Mariano; Wang, Na; Liu, Siming; Li, Xiang-Dong

    2016-04-01

    The X-ray aperiodic variability and quasi-periodic oscillation (QPO) are the important tools to study the structure of the accretion flow of X-ray binaries. However, the origin of the complex X-ray variability from X-ray binaries remains yet unsolved. We proposed two methods for studying the X-ray variability. One is amplitude-ratio spectrum analysis method. The other is mapping analysis method. Based on the consideration that the aperiodic variability originates from all spectral components whereas the QPO originates from one spectral component, we divided the root-mean-square (rms) amplitude spectrum of the power density spectrum (PDS) broadband noise component by the amplitude spectrum of an accompanying QPO, and first identified a high-frequency (> 10 Hz) aperiodic variability from the accretion disk (Yan et al. 2013). We now present the evolution of the amplitude-ratio spectrum with the cycle phase of the heartbeat state of the microquasar GRS 1915+105. We produced the energy-frequency-power map to investigate the origin of the X-ray variability, and show that most aperiodic X-ray variability is produced in the corona, and the low-frequency aperiodic variability from the corona is significant in the hard phase of the cycle phase of the heartbeat state of GRS 1915+105 while the low-frequency aperiodic variability from the disk and the corona are both significant in the soft phase.

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

    DEFF Research Database (Denmark)

    Jesper, Nygaard; Munch, Henrik K.; Thulstrup, Peter W.; Christensen, Niels Johan; Hoeg-Jensen, Thomas; Jensen, Knud J.; Arleth, Lise

    2012-01-01

    Precise control of the oligomeric state of proteins is of central importance for biological function and for the properties of biopharmaceutical drugs. Here, the self-assembly of 2,2′-bipyridine conjugated monomeric insulin analogues, induced through coordination to divalent metal ions, was studi...

  14. Hybrid - block copolymer nanocomposites. characterization of nanostructure by small-angle X-ray scattering (SAXS)

    OpenAIRE

    A. Romo-Uribe

    2007-01-01

    The nanoscopic order of a series of block copolymer-inorganic nanocomposites was characterized using small-angle X-ray scattering (SAXS). The nanostructures were obtained via a diblock copolymer directed sol-gel synthesis. The copolymer consists of blocks of poly(isoprene) -PI- and blocks of poly(ethylene oxide) -PEO. The inorganic material consists of a crosslinked sol of 3-glycidoxypropyltrimethoxysilane and aluminum-tri-sec-butoxide in a 4:1 mole ratio, to generate an aluminosilicate ceram...

  15. Database for rapid protein classification based on small-angle X-ray scattering data

    International Nuclear Information System (INIS)

    A method was developed for rapid protein classification based on comparison of the experimental small-angle X-ray scattering data with scattering curves calculated for proteins with known structures. For this purpose, a database was compiled from about 1500 theoretical scattering curves for proteins with known structures. The potential of this method was illustrated by its application to analysis of the experimental scattering data from sperm whale myoglobin

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

    International Nuclear Information System (INIS)

    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 H2 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

  17. Upgrade of the small angle X-ray scattering beamlines at the Photon Factory

    International Nuclear Information System (INIS)

    BL-10C and BL-15A at the Photon Factory, which became operational in 1982, are some of the oldest small angle X-ray scattering beamlines in the world. Recently, both beamlines were upgraded for two-dimensional (2D) SAXS-WAXS experiments. A wide-area imaging plate (IP) detector and a fast-readout flat panel (FP) detector were installed at BL-10C and BL-15A, respectively. Preliminary experiments of both systems showed promising results.

  18. Spectroscopic Studies of X-Ray Binary Pulsars

    Indian Academy of Sciences (India)

    F. Nagase

    2002-03-01

    Several new features of X-ray binary pulsars are revealed from recent observations with ASCA, RXTE, BeppoSAX and other X-ray observatories. Among these, I will review in this paper some recent progress in spectroscopic studies of accreting X-ray pulsars in binary systems (XBPs). First, I will discuss soft excess features observed in the energy spectra of XBPs and propose that it is a common feature for various subclasses of XBPs. Next I will present some recent results of high resolution spectroscopy with ASCA and Chandra.

  19. Structure of wild type and mutant F508del CFTR: A small-angle X-ray scattering study of the protein-detergent complexes.

    Science.gov (United States)

    Pollock, Naomi L; Satriano, Letizia; Zegarra-Moran, Olga; Ford, Robert C; Moran, Oscar

    2016-04-01

    CFTR is an anionic channel expressed in epithelia whose mutations cause cystic fibrosis. Wild (WT) and mutated (F508del) types were over-expressed in yeast, solubilised in the detergent LPG-14 and purified. The detergent-CFTR complexes were studied by SAXS techniques using a solvent of variable density. The final result of the study is the numerical value of a set of parameters: molecular mass, volume and radius of gyration, average electron density and second moment of the electron density fluctuations inside the particles. It is also shown that in the complex the centres of gravity of CFTR and of the detergent are displaced relative to each other. The analysis of these parameters led to the determination of the size and shape of the volumes occupied by protein and by detergent in the complex. WT-CFTR to be an elongated molecule (maximum diameter ∼12.4nm) which spans a flat detergent micelle. The distance distribution function, P(r) confirms that the WT-CFTR is elongated and with an inhomogeneous electronic density. The F508del-CFTR molecule is also elongated (maximum diameter ∼13.2nm), but the associated detergent micelle hides a larger surface, plausibly related to an increased exposure of hydrophobic portions of the mutated protein. The corresponding P(r) is consistent with the presence of well defined domains, probably linked by flexible regions. These differences suggest that the full-length mutant F508del-CFTR has a detectably different conformation, in contrast to the minor differences observed for the isolated F508-containing domain. We interpret the data in terms of an incomplete post-translational assembly of the protein domains. PMID:26850167

  20. Simulation of photoelectric X-ray polarimetry and reconstruction of the photoelectron azimuthal angle

    International Nuclear Information System (INIS)

    Sensitive X-ray polarimetry in the keV energy range can be achieved by measuring the azimuthal angle distribution of emitted electrons after the photoelectric absorption of X-rays in a micropattern gas detector. However, the initial direction of the electron is not readily measurable due to the randomization of its motion during energy loss. By using the Geant4, Maxwell and Garfield packages, we simulated the detected electron tracks following photoelectric absorption, electron drift and diffusion in the gas, and proposed a technique capable of reconstructing the initial direction of the emitted photoelectron. The technique allows us to measure the angular modulation of flux predicted for a polarized X-ray beam. We calculated the modulation factors in 2-10 keV with a gas mixture of neon and CO2, and discussed how electron diffusion along the drift will dilute the track and suppress the modulation. These results are useful for the design of the X-ray polarimeter. (authors)

  1. Nucleation and crystal growth in a suspension of charged colloidal silica spheres with bi-modal size distribution studied by time-resolved ultra-small-angle X-ray scattering.

    Science.gov (United States)

    Hornfeck, Wolfgang; Menke, Dirk; Forthaus, Martin; Subatzus, Sebastian; Franke, Markus; Schöpe, Hans-Joachim; Palberg, Thomas; Perlich, Jan; Herlach, Dieter

    2014-12-01

    A suspension of charged colloidal silica spheres exhibiting a bi-modal size distribution of particles, thereby mimicking a binary mixture, was studied using time-resolved ultra-small-angle synchrotron X-ray scattering (USAXS). The sample, consisting of particles of diameters d(A) = (104.7 ± 9.0) nm and d(B) = (88.1 ± 7.8) nm (d(A)/d(B) ≈ 1.2), and with an estimated composition A(0.6(1))B(0.4(1)), was studied with respect to its phase behaviour in dependance of particle number density and interaction, of which the latter was modulated by varying amounts of added base (NaOH). Moreover, its short-range order in the fluid state and its eventual solidification into a long-range ordered colloidal crystal were observed in situ, allowing the measurement of the associated kinetics of nucleation and crystal growth. Key parameters of the nucleation kinetics such as crystallinity, crystallite number density, and nucleation rate density were extracted from the time-resolved scattering curves. By this means an estimate on the interfacial energy for the interface between the icosahedral short-range ordered fluid and a body-centered cubic colloidal crystal was obtained, comparable to previously determined values for single-component colloidal systems. PMID:25481168

  2. 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; Yennawar, Neela

    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...

  3. Synchrotron x-ray diffraction study of liquid surfaces

    DEFF Research Database (Denmark)

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

    1983-01-01

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

  4. High-resolution soft-X-ray beamline ADRESS at Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies

    OpenAIRE

    Strocov, V. N.; Schmitt, T; U. Flechsig; Schmidt, T.; Imhof, A; Q. Chen; J. Raabe; Betemps, R.; Zimoch, D.; Krempasky, J.; A. Piazzalunga; X Wang; Grioni, M.; Patthey, L.

    2009-01-01

    We describe the concepts and technical realization of the high-resolution soft-X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for Resonant Inelastic X-ray Scattering (RIXS) and Angle-Resolved Photoelectron Spectroscopy (ARPES). The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0-180 deg rotatable linear polarizations) but als...

  5. High-resolution soft X-ray beamline ADRESS at the Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies

    OpenAIRE

    Strocov, V. N.; Schmitt, T; U. Flechsig; Schmidt, T.; Imhof, A; Q. Chen; J. Raabe; Betemps, R.; Zimoch, D.; Krempasky, J.; X Wang; Grioni, M.; A. Piazzalunga; Patthey, L.

    2010-01-01

    The concepts and technical realisation of the high-resolution soft X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for resonant inelastic X-ray scattering (RIXS) and angle-resolved photoelectron spectroscopy (ARPES) are described. The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0–180° rotatable linear polarizations) but also...

  6. Wide angle crystal spectrometer for angularly and spectrally resolved x-ray scattering experiments

    OpenAIRE

    Garcia Saiz, E.; Khattak, F. Y.; G. Gregori; Bandyopadhyay, S; Clarke, R J; Fell, B.; Freeman, R R; Jeffries, J.; Jung, Daniel; Notley, M. M.; Weber, R. L.; Van Woerkom, L.; Riley, David

    2007-01-01

    A novel wide angle spectrometer has been implemented with a highly oriented pyrolytic graphite crystal coupled to an image plate. This spectrometer has allowed us to look at the energy resolved spectrum of scattered x rays from a dense plasma over a wide range of angles ( ~ 30°) in a single shot. Using this spectrometer we were able to observe the temporal evolution of the angular scatter cross section from a laser shocked foil. A spectrometer of this type may also be useful in investigations...

  7. X-ray microscopy study of bone mineralization

    International Nuclear Information System (INIS)

    Transmission spectro-microscopy around the calcium K-edge and fluorescence microscopy were performed respectively on the Transmission X-ray Microscope (TXM) and Scanning X-ray Microscope (SXM) end-stations of ID21 beamline at ESRF, to map the calcium distribution and the Ca/P ratio in bone samples. Preliminary results are presented. The motivation for these experiments is the study of the genetic determinism of bone mineralisation parameters in two different strains of mice

  8. Studies of subnanosecond x-ray switching and shuttering techniques

    International Nuclear Information System (INIS)

    This paper discusses experimental studies conducted of the changes in x-ray diffraction properties of crystals under intense subnanosecond laser heating. One beam of the PHOENIX laser system was used to create an intense source of x-ray line radiation. This radiation was in turn diffracted from a silicon crystal that was heated with the other beam of the laser. The diffracted radiation was temporally resolved with an x-ray streak camera. The diffracted lines are observed to broaden spectrally on a subnanosecond time scale. From the temporal structure of the diffrated radiation, information is derived on the nature of the laser heating process. Interruption of crystal diffraction on a subnanosecond time scale is potentially useful as mechanism for x-ray switching and shuttering. Considerations for the design and construction of such devices are discussed

  9. Investigation of gamma irradiated Pc/PLLA blend by wide-angle X-ray diffraction

    International Nuclear Information System (INIS)

    Biodegradable polymers are able to undergo deleterious changes in their properties due to an alteration in the chemical structure mediated at least partially by a biological system. It was observed in the literature that crosslinking of poly(ε-caprolactone), PCL, increases with the radiation dose induced by ionizing radiation. On the other hand, poly(lactic acid) predominantly degrades at ionizing radiation doses below 250 kGy and crosslinking preponderates at higher doses. It was also observed that Poly(L-lactic acid), PLLA crystallinity decreases with radiation dose up to 80 kGy. In the present work, twin screw extruded films of PLLA and PCL homopolymers and 50/50 (w/w) blend were irradiated with gamma rays from Co-60 at doses in the range of 25 to 500 kGy to investigate the effects of the ionizing radiation on their crystalline structure by wide-angle X- ray diffraction (WAXD). PCL samples, non irradiated and irradiated with 100 and 500 kGy, showed the two strongest reflections at Bragg angles 2θ =21.4 deg and 2θ =23.7 deg that have been attributed in the literature to the (110) and (200) reflections, respectively. For as extruded non irradiated and irradiated with 100 and 500 kGy doses PLLA it was observed broad diffusion peaks corresponding to amorphous polymer. PLLA annealed samples showed reflections at Bragg angles 2θ =16.4 deg and 2θ =18.7 deg previously attributed in the literature to distorted 103 (alpha-form) helices. It was possible to observe slight alteration on the crystallite size of all irradiated samples of PCL in the dose range studied. (author)

  10. An intensity correction for pole figure measurements by grazing incident and grazing exit angle X-ray diffraction

    International Nuclear Information System (INIS)

    In pole figure measurement by X-ray diffraction, the intensity must be corrected for geometric factors entering into the intensity. For the grazing (often, also called glancing) angle diffraction mode, the irradiated area changes with the grazing angle. A theoretical analysis of this effect was made and compared with measured data from a texture-free silver sample. An intensity correction factor is given as the ratio of the detector slit width and the width of the irradiated sample area as seen from the detector. As an application, the texture of thin copper film was studied

  11. An x-ray detector for time-resolved studies

    International Nuclear Information System (INIS)

    The development of ultrahigh-brightness x-ray sources makes time-resolved x-ray studies more and more feasible. Improvements in x-ray optics components are also critical for obtaining the appropriate beam for a particular type of experiment. Moreover, fast parallel detectors will be essential in order to exploit the combination of high intensity x-ray sources and novel optics for time-resolved experiments. A CCD detector with a time resolution of microseconds has been developed at the Advanced Photon Source (APS). This detector is fully programmable using CAMAC electronics and a Micro Vax computer. The techniques of time-resolved x-ray studies, which include scattering, microradiography, microtomography, stroboscopy, etc., can be applied to a range of phenomena (including rapid thermal annealing, surface ordering, crystallization, and the kinetics of phase transition) in order to understand these time-dependent microscopic processes. Some of these applications will be illustrated by recent results performed at synchrotrons. New powerful x-ray sources now under construction offer the opportunity to apply innovative approaches in time-resolved work

  12. Limited-angle tomography for analyzer-based phase-contrast x-ray imaging

    International Nuclear Information System (INIS)

    Multiple-image radiography (MIR) is an analyzer-based phase-contrast x-ray imaging method, which is emerging as a potential alternative to conventional radiography. MIR simultaneously generates three planar parametric images containing information about scattering, refraction and attenuation properties of the object. The MIR planar images are linear tomographic projections of the corresponding object properties, which allows reconstruction of volumetric images using computed tomography (CT) methods. However, when acquiring a full range of linear projections around the tissue of interest is not feasible or the scanning time is limited, limited-angle tomography techniques can be used to reconstruct these volumetric images near the central plane, which is the plane that contains the pivot point of the tomographic movement. In this work, we use computer simulations to explore the applicability of limited-angle tomography to MIR. We also investigate the accuracy of reconstructions as a function of number of tomographic angles for a fixed total radiation exposure. We use this function to find an optimal range of angles over which data should be acquired for limited-angle tomography MIR (LAT-MIR). Next, we apply the LAT-MIR technique to experimentally acquired MIR projections obtained in a cadaveric human thumb study. We compare the reconstructed slices near the central plane to the same slices reconstructed by CT-MIR using the full angular view around the object. Finally, we perform a task-based evaluation of LAT-MIR performance for different numbers of angular views, and use template matching to detect cartilage in the refraction image near the central plane. We use the signal-to-noise ratio of this test as the detectability metric to investigate an optimum range of tomographic angles for detecting soft tissues in LAT-MIR. Both results show that there is an optimum range of angular view for data acquisition where LAT-MIR yields the best performance, comparable to CT

  13. Limited-angle tomography for analyzer-based phase-contrast x-ray imaging

    Science.gov (United States)

    Majidi, Keivan; Wernick, Miles N.; Li, Jun; Muehleman, Carol; Brankov, Jovan G.

    2014-07-01

    Multiple-image radiography (MIR) is an analyzer-based phase-contrast x-ray imaging method, which is emerging as a potential alternative to conventional radiography. MIR simultaneously generates three planar parametric images containing information about scattering, refraction and attenuation properties of the object. The MIR planar images are linear tomographic projections of the corresponding object properties, which allows reconstruction of volumetric images using computed tomography (CT) methods. However, when acquiring a full range of linear projections around the tissue of interest is not feasible or the scanning time is limited, limited-angle tomography techniques can be used to reconstruct these volumetric images near the central plane, which is the plane that contains the pivot point of the tomographic movement. In this work, we use computer simulations to explore the applicability of limited-angle tomography to MIR. We also investigate the accuracy of reconstructions as a function of number of tomographic angles for a fixed total radiation exposure. We use this function to find an optimal range of angles over which data should be acquired for limited-angle tomography MIR (LAT-MIR). Next, we apply the LAT-MIR technique to experimentally acquired MIR projections obtained in a cadaveric human thumb study. We compare the reconstructed slices near the central plane to the same slices reconstructed by CT-MIR using the full angular view around the object. Finally, we perform a task-based evaluation of LAT-MIR performance for different numbers of angular views, and use template matching to detect cartilage in the refraction image near the central plane. We use the signal-to-noise ratio of this test as the detectability metric to investigate an optimum range of tomographic angles for detecting soft tissues in LAT-MIR. Both results show that there is an optimum range of angular view for data acquisition where LAT-MIR yields the best performance, comparable to CT

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

    International Nuclear Information System (INIS)

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

  15. Effects of x-ray does on rhizosphere studies using x-ray computed tomography

    OpenAIRE

    Susan Zappala; Jonathan R Helliwell; Tracy, Saoirse R.; Stefan Mairhofer; Sturrock, Craig J.; Tony Pridmore; Malcolm Bennett; Sacha J. Mooney

    2013-01-01

    X-ray Computed Tomography (CT) is a non-destructive imaging technique originally designed for diagnostic medicine, which was adopted for rhizosphere and soil science applications in the early 1980s. X-ray CT enables researchers to simultaneously visualise and quantify the heterogeneous soil matrix of mineral grains, organic matter, air-filled pores and water-filled pores. Additionally, X-ray CT allows visualisation of plant roots in situ without the need for traditional invasive methods such ...

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

    International Nuclear Information System (INIS)

    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 mm2, 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 106 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. Automated acquisition and analysis of small angle X-ray scattering data

    International Nuclear Information System (INIS)

    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.

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

    Science.gov (United States)

    Settens, Charles M.

    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, H 2 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 CD-SEM, 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, A.P.G. [Nuclear Instrumentation Laboratory (LIN/COPPE), P. O. Box 68509, 21945-970, Rio de Janeiro RJ (Brazil)], E-mail: delson@lin.ufrj.br; Braz, D. [Nuclear Instrumentation Laboratory (LIN/COPPE), P. O. Box 68509, 21945-970, Rio de Janeiro RJ (Brazil); Barroso, R.C. [Physics Institute (IF/UERJ), University of Rio de Janeiro State, 20550-900 Rio de Janeiro RJ (Brazil); Lopes, R.T. [Nuclear Instrumentation Laboratory (LIN/COPPE), P. O. Box 68509, 21945-970, Rio de Janeiro RJ (Brazil)

    2007-09-21

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

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

    Science.gov (United States)

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

    2007-09-01

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

  2. 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.

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

    International Nuclear Information System (INIS)

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

  4. Analysis of the Data from Compton X-ray Polarimeters which Measure the Azimuthal and Polar Scattering Angles

    CERN Document Server

    ,

    2011-01-01

    X-ray polarimetry has the potential to make key-contributions to our understanding of galactic compact objects like binary black hole systems and neutron stars, and extragalactic objects like active galactic nuclei, blazars, and neutron stars. Furthermore, several particle astrophysics topics can be addressed including uniquely sensitive tests of Lorentz invariance. In the energy range from 10-20 keV to several MeV, Compton polarimeters achieve the best performance. In this paper we evaluate the benefit that comes from using the azimuthal and polar angles of the Compton scattered photons in the analysis, rather than using the azimuthal scattering angles alone. We study the case of an ideal Compton polarimeter and show that a Maximum Likelihood analysis which uses the two scattering angles lowers the Minimum Detectable Polarization (MDP) by ~20% compared to a standard analysis based on the azimuthal scattering angles alone. The accuracies with which the polarization fraction and the polarization direction can ...

  5. The X-Ray Surveyor Mission: A Concept Study

    Science.gov (United States)

    Gaskin, Jessica A.; Weisskopf, Martin C.; Vikhlinin, Alexey; Tananbaum, Harvey D.; Bandler, Simon R.; Bautz, Marshall W.; Burrows, David N.; Falcone, Abraham D.; Harrison, Fiona A.; Heilmann, Ralf K.; Heinz, Sebastian; Hopkins, Randall C.; Kilbourne, Caroline A.; Kouveliotou, Chryssa; Kraft, Ralph P.; Kravtsov, Andrey V.; McEntaffer, Randall L.; Natarajan, Priyamvada; O'Dell, Stephen L.; Petre, Robert; Prieskorn, Zachary R.; Ptak, Andrew F.; Ramsey, Brian D.; Reid, Paul B.; Schnell, Andrew R.; Schwartz, Daniel A.; Townsley, Leisa K.

    2015-01-01

    NASA's Chandra X-ray Observatory continues to provide an unparalleled means for exploring the high-energy universe. With its half-arcsecond angular resolution, Chandra studies have deepened our understanding of galaxy clusters, active galactic nuclei, galaxies, supernova remnants, neutron stars, black holes, and solar system objects. As we look beyond Chandra, it is clear that comparable or even better angular resolution with greatly increased photon throughput is essential to address ever more demanding science questions-such as the formation and growth of black hole seeds at very high redshifts; the emergence of the first galaxy groups; and details of feedback over a large range of scales from galaxies to galaxy clusters. Recently, we initiated a concept study for such a mission, dubbed X-ray Surveyor. The X-ray Surveyor strawman payload is comprised of a high-resolution mirror assembly and an instrument set, which may include an X-ray microcalorimeter, a high-definition imager, and a dispersive grating spectrometer and its readout. The mirror assembly will consist of highly nested, thin, grazing-incidence mirrors, for which a number of technical approaches are currently under development-including adjustable X-ray optics, differential deposition, and new polishing techniques applied to a variety of substrates. This study benefits from previous studies of large missions carried out over the past two decades and, in most areas, points to mission requirements no more stringent than those of Chandra.

  6. The X-ray Surveyor Mission: a concept study

    Science.gov (United States)

    Gaskin, Jessica A.; Weisskopf, Martin C.; Vikhlinin, Alexey; Tananbaum, Harvey D.; Bandler, Simon R.; Bautz, Marshall W.; Burrows, David N.; Falcone, Abraham D.; Harrison, Fiona A.; Heilmann, Ralf K.; Heinz, Sebastian; Hopkins, Randall C.; Kilbourne, Caroline A.; Kouveliotou, Chryssa; Kraft, Ralph P.; Kravtsov, Andrey V.; McEntaffer, Randall L.; Natarajan, Priyamvada; O'Dell, Stephen L.; Petre, Robert; Prieskorn, Zachary R.; Ptak, Andrew F.; Ramsey, Brian D.; Reid, Paul B.; Schnell, Andrew R.; Schwartz, Daniel A.; Townsley, Leisa K.

    2015-08-01

    NASA's Chandra X-ray Observatory continues to provide an unparalleled means for exploring the high-energy universe. With its half-arcsecond angular resolution, Chandra studies have deepened our understanding of galaxy clusters, active galactic nuclei, galaxies, supernova remnants, neutron stars, black holes, and solar system objects. As we look beyond Chandra, it is clear that comparable or even better angular resolution with greatly increased photon throughput is essential to address ever more demanding science questions—such as the formation and growth of black hole seeds at very high redshifts; the emergence of the first galaxy groups; and details of feedback over a large range of scales from galaxies to galaxy clusters. Recently, we initiated a concept study for such a mission, dubbed X-ray Surveyor. The X-ray Surveyor strawman payload is comprised of a high-resolution mirror assembly and an instrument set, which may include an X-ray microcalorimeter, a high-definition imager, and a dispersive grating spectrometer and its readout. The mirror assembly will consist of highly nested, thin, grazing-incidence mirrors, for which a number of technical approaches are currently under development—including adjustable X-ray optics, differential deposition, and new polishing techniques applied to a variety of substrates. This study benefits from previous studies of large missions carried out over the past two decades and, in most areas, points to mission requirements no more stringent than those of Chandra.

  7. Estimation of liquids structural in narrow pores by small angle X ray radiography

    International Nuclear Information System (INIS)

    The method suggested for estimation of liquids structure in narrow pores is based on small angle X-ray radiography data. The investigation was carried out on porous carbon adsorbents with using a number of fluids. Additional small-angle scattering was observed during the filling of mesopores by organic fluids, which was not observed before. It was absent during the filling of micropores only. The additional radiography is a part of the diffraction pattern, which is an attribute of liquids and appears as one or several diffuse maxima in the range of wide angles. This diffraction pattern reflects an occurrence of the short-range order and shows similarity of the liquid structures in mesopores and in volume. The limiting value of pores inertia radius radiography is estimated, at which in liquids the short-range order is formed

  8. A Small Angle X-ray Scattering Method to Investigate the Crack Tip in Metals

    OpenAIRE

    Böhmert, Jürgen; Müller, Gudrun; Ouytsel, Krist'l van

    2010-01-01

    The work in this report, financed by the European Union through the Marie Curie Fellowship Association, was carried out at the FZ-Rossendorf. The subject of the research was to develop a method to investigate the damage, the high defect gradients at the tip of a ductile crack by means of Small Angle X-ray Scattering. The work explains the objectives and entails a brief introduction and background; it portrays and discusses the results which can be summarized as follows. Different damage param...

  9. A small-angle X-ray investigation of the satellite tobacco necrosis virus

    International Nuclear Information System (INIS)

    Small-angle X-ray data recorded from solutions of satellite tobacco necrosis (STN) virus in the concentration range 3.7-15.0 mg/cm3 are presented. The data were analysed using a least-squares computer program where the experimental, slit-smeared intensity function is used directly, without desmearing. The radius of gyration of the virus particles is 6.80 nm. From a scale factor obtained from the least-squares analysis, and the isopotential specific volume, which was determined to 0.683 cm3/g, the total molecular weight of the monomeric STN virus was determined to be 1.70 x 106. (orig.)

  10. 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.

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

    Directory of Open Access Journals (Sweden)

    Schneidman-Duhovny Dina

    2012-07-01

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

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

    International Nuclear Information System (INIS)

    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)

  13. Electron dynamics of copper oxide superconductors studied by soft X-ray, hard X-ray and neutron inelastic scattering

    International Nuclear Information System (INIS)

    We combine soft X-ray, hard X-ray, and neutron inelastic scattering measurements to study both spin and charge excitations in electron-doped copper oxide superconductors. Thanks to the recent development of beam sources and related experimental techniques, accessible energy range of the inelastic scattering measurements overlaps each other and it enables us to investigate spin and charge dynamics in the important but unexplored energy-momentum space of the cuprate superconductors. Our study demonstrates that complementary use of X-ray and neutron has become effective in inelastic scattering for studying electron dynamics of materials. (author)

  14. Large Area Transition Edge Sensor X-ray Microcalorimeters for Diffuse X-ray Background Studies

    Science.gov (United States)

    Morgan, K. M.; Busch, S. E.; Eckart, M. E.; Kilbourne, C. A.; McCammon, D.

    2014-08-01

    We are developing transition edge sensor (TES) mirocalorimeters with large area (0.72 mm) absorbers to study the keV diffuse X-ray background. The goal is to develop a 2 cm array of 256 pixels for a sounding rocket payload. We present a pixel design which includes a Mo/Au bilayer TES coupled to a large (850 x 850 x 0.2 m) gold absorber. Our simulations indicate that such a design can achieve energy resolution as good as 1.6 eV FWHM in our target bandpass of 0.05-1 keV. Additionally, thermal modelling shows that for typical gold layers, the position-dependent variation of the pulse shape over the large area of the absorber is not expected to significantly degrade this energy resolution. An array of devices will be fabricated in late 2013 to test this design.

  15. Cardiac motion correction based on partial angle reconstructed images in x-ray CT

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seungeon; Chang, Yongjin; Ra, Jong Beom, E-mail: jbra@kaist.ac.kr [Department of Electrical Engineering, KAIST, Daejeon 305-701 (Korea, Republic of)

    2015-05-15

    Purpose: Cardiac x-ray CT imaging is still challenging due to heart motion, which cannot be ignored even with the current rotation speed of the equipment. In response, many algorithms have been developed to compensate remaining motion artifacts by estimating the motion using projection data or reconstructed images. In these algorithms, accurate motion estimation is critical to the compensated image quality. In addition, since the scan range is directly related to the radiation dose, it is preferable to minimize the scan range in motion estimation. In this paper, the authors propose a novel motion estimation and compensation algorithm using a sinogram with a rotation angle of less than 360°. The algorithm estimates the motion of the whole heart area using two opposite 3D partial angle reconstructed (PAR) images and compensates the motion in the reconstruction process. Methods: A CT system scans the thoracic area including the heart over an angular range of 180° + α + β, where α and β denote the detector fan angle and an additional partial angle, respectively. The obtained cone-beam projection data are converted into cone-parallel geometry via row-wise fan-to-parallel rebinning. Two conjugate 3D PAR images, whose center projection angles are separated by 180°, are then reconstructed with an angular range of β, which is considerably smaller than a short scan range of 180° + α. Although these images include limited view angle artifacts that disturb accurate motion estimation, they have considerably better temporal resolution than a short scan image. Hence, after preprocessing these artifacts, the authors estimate a motion model during a half rotation for a whole field of view via nonrigid registration between the images. Finally, motion-compensated image reconstruction is performed at a target phase by incorporating the estimated motion model. The target phase is selected as that corresponding to a view angle that is orthogonal to the center view angles of

  16. Cardiac motion correction based on partial angle reconstructed images in x-ray CT

    International Nuclear Information System (INIS)

    Purpose: Cardiac x-ray CT imaging is still challenging due to heart motion, which cannot be ignored even with the current rotation speed of the equipment. In response, many algorithms have been developed to compensate remaining motion artifacts by estimating the motion using projection data or reconstructed images. In these algorithms, accurate motion estimation is critical to the compensated image quality. In addition, since the scan range is directly related to the radiation dose, it is preferable to minimize the scan range in motion estimation. In this paper, the authors propose a novel motion estimation and compensation algorithm using a sinogram with a rotation angle of less than 360°. The algorithm estimates the motion of the whole heart area using two opposite 3D partial angle reconstructed (PAR) images and compensates the motion in the reconstruction process. Methods: A CT system scans the thoracic area including the heart over an angular range of 180° + α + β, where α and β denote the detector fan angle and an additional partial angle, respectively. The obtained cone-beam projection data are converted into cone-parallel geometry via row-wise fan-to-parallel rebinning. Two conjugate 3D PAR images, whose center projection angles are separated by 180°, are then reconstructed with an angular range of β, which is considerably smaller than a short scan range of 180° + α. Although these images include limited view angle artifacts that disturb accurate motion estimation, they have considerably better temporal resolution than a short scan image. Hence, after preprocessing these artifacts, the authors estimate a motion model during a half rotation for a whole field of view via nonrigid registration between the images. Finally, motion-compensated image reconstruction is performed at a target phase by incorporating the estimated motion model. The target phase is selected as that corresponding to a view angle that is orthogonal to the center view angles of

  17. In situ X-ray studies of film cathodes for solid oxide fuel cells

    International Nuclear Information System (INIS)

    Highlights: •Synchrotron X-rays are used to study in operando the structural and chemical changes of LSM and LSCF film cathodes during half-cell operations. •A-site and B-site cations actively segregate or desegregate on the changes of temperature, pO2, and electrochemical potential. •Chemical lattice expansions show that oxygen-cathode interface is the primary source of rate-limiting processes. •The surface and subsurface of the LSM and LSCF films have different oxidation-states due to vacancy concentration changes. •Liquid-phase infiltration and coarsening processes of cathode materials into porous YSZ electrolyte backbone were monitored by USAXS. -- Abstract: Synchrotron-based X-ray techniques have been used to study in situ the structural and chemical changes of film cathodes during half-cell operations. The X-ray techniques used include X-ray reflectivity (XR), total-reflection X-ray fluorescence (TXRF), high-resolution diffraction (HRD), ultra-small angle X-ray scattering (USAXS). The epitaxial thin film model cathodes for XR, TXRF, and HRD measurements are made by pulse laser deposition and porous film cathodes for USAX measurements are made by screen printing technique. The experimental results reviewed here include A-site and B-site segregations, lattice expansion, oxidation-state changes during cell operations and liquid-phase infiltration and coarsening of cathode to electrolyte backbone

  18. X-ray tomography studies of prehistoric ceramic artifacts

    International Nuclear Information System (INIS)

    X-ray Computed Tomography (CT) is a powerful non-destructive technique that can yield interesting structural information not discernible through visual examination only. This paper presents the results of the CT scans of four objects belonging to the Romanian cultural heritage attributed to the Vinca, Cucuteni and Cruceni-Belegis cultures. The study was performed with an X-ray tomographic device developed at the Department for Applied Nuclear Physics from Horia Hulubei National Institute for Nuclear Physics and Engineering in Magurele, Romania. This apparatus was specially designed for archaeometric studies of low-Z artifacts: ceramic, wood, bone. The tomographic investigations revealed the internal configuration of the objects and provided information about the degree to which the previous manipulations affected the archaeological items. Based on the X-ray images resulting from the CT scans, hints about the techniques used in the manufacturing of the artifacts were obtained, as well as some indications useful for conservation/restoration purposes. (author)

  19. X-ray photoelectron study of Si+ ion implanted polymers

    International Nuclear Information System (INIS)

    X-ray photoelectron spectroscopy was used to characterize different polymer materials implanted with low energy Si+ ions (E=30 keV, D= 1.1017 cm-2). Two kinds of polymers were studied - ultra-high-molecular-weight poly-ethylene (UHMWPE), and poly-methyl-methacrylate (PMMA). The non-implanted polymer materials show the expected variety of chemical bonds: carbon-carbon, carbon being three- and fourfold coordinated, and carbon-oxygen in the case of PMMA samples. The X-ray photoelectron and Raman spectra show that Si+ ion implantation leads to the introduction of additional disorder in the polymer material. The X-ray photoelectron spectra of the implanted polymers show that, in addition to already mentioned bonds, silicon creates new bonds with the host elements - Si-C and Si-O, together with additional Si dangling bonds as revealed by the valence band study of the implanted polymer materials.

  20. X-ray photoelectron and X-ray Auger electron spectroscopy studies of heavy ion irradiated C60 films

    International Nuclear Information System (INIS)

    The influence of 200 MeV Au ion irradiation on the surface properties of polycrystalline fullerene films has been investigated. The X-ray photoelectron and X-ray Auger electron spectroscopies are employed to study the ion-induced modification of the fullerene, near the surface region. The shift of C 1s core level and decrease in intensity of shake-up satellite were used to investigate the structural changes (like sp2 to sp3 conversion) and reduction of π electrons, respectively, under heavy ion irradiation. Further, X-ray Auger electron spectroscopy was employed to investigate hybridization conversion qualitatively as a function of ion fluence

  1. [Wide-angle x-ray scattering comparison of the structure of crystalline cytochrome c and cytochrome c in solution].

    Science.gov (United States)

    Timchenko, A A; Denesiuk, A I; Fedorov, B A

    1981-01-01

    Large-angle X-ray diffuse scattering has been used for studying the conformational changes in cytochrome c during its transition from crystal into solution and during a change of the electron state of the heme. It has been found that the structure of cytochrome c in solution differs from its structure in crystal by a shift of the chain fragment in the region of 60-77 amino acid residues. The studies of the oxidized, reduced and cyanoforms of protein in solution have not revealed noticeable changes in the protein structure. PMID:6261840

  2. Soft X-ray Absorbers Enabling Study of the Diffuse X-ray Background Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Absorbers for soft x-rays need to be made thinner and with larger area, to collect more photons, and with minimal number of support stems. However, the structure is...

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

    Science.gov (United States)

    Carli, Larissa N; Bianchi, Otávio; Machado, Giovanna; Crespo, Janaina S; Mauler, Raquel S

    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® 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 (β) 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. PMID:25427508

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

    International Nuclear Information System (INIS)

    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 Cr23C6 in 9Cr-1 MoVNb steel

  5. Coherent X-ray diffraction studies of mesoscopic materials

    Energy Technology Data Exchange (ETDEWEB)

    Shabalin, Anatoly

    2015-12-15

    This thesis is devoted to three separate projects, which can be considered as independent. First, the dynamical scattering effects in the Coherent X-ray Diffractive Imaging (CXDI) method are discussed. Based on the simulation results, a straightforward method for correction for the refraction and absorption artifacts in the Bragg CXDI reconstruction is suggested. The second part summarizes the results of an Coherent X-ray Diffractive Imaging experiment with a single colloidal crystal grain. A remarkable result is that positions of individual particles in the crystal lattice have been resolved in three dimensions. The third project is devoted to X-ray diffraction experimental studies of structural evolution of colloidal crystalline films upon incremental heating. Based on the results of the analysis a model of structural evolution of a colloidal crystal upon heating on nanoscopic and mesoscopic length scales is suggested.

  6. Coherent X-ray diffraction studies of mesoscopic materials

    International Nuclear Information System (INIS)

    This thesis is devoted to three separate projects, which can be considered as independent. First, the dynamical scattering effects in the Coherent X-ray Diffractive Imaging (CXDI) method are discussed. Based on the simulation results, a straightforward method for correction for the refraction and absorption artifacts in the Bragg CXDI reconstruction is suggested. The second part summarizes the results of an Coherent X-ray Diffractive Imaging experiment with a single colloidal crystal grain. A remarkable result is that positions of individual particles in the crystal lattice have been resolved in three dimensions. The third project is devoted to X-ray diffraction experimental studies of structural evolution of colloidal crystalline films upon incremental heating. Based on the results of the analysis a model of structural evolution of a colloidal crystal upon heating on nanoscopic and mesoscopic length scales is suggested.

  7. X-ray diffraction study of surface-layer structure in parallel grazing rays

    International Nuclear Information System (INIS)

    An x-ray diffraction method is described for study of thin polycrystalline and amorphous films and surface layers in an extremely asymmetrical diffraction system in parallel grazing rays using a DRON-3.0 diffractometer. The minimum grazing angles correspond to diffraction under conditions of total external reflection and a layer depth of ∼ 2.5-8 nm

  8. Studies of atomic processes for x-ray lasers and x-ray sources

    International Nuclear Information System (INIS)

    A computer tool for displaying Grotrian diagram of atomic energy level structure is developed, which uses computed atomic data from the HULLAC code. This tool is intended for providing atomic data of complex multiply charged ions for modeling x-ray lasers and x-ray sources. Visualization of the atomic structure using the Grotrian tool appears to be useful for identifying dominant ionization/excitation processes and emission channels in the plasma. (author)

  9. Studies of atomic processes for x-ray lasers and x-ray sources

    International Nuclear Information System (INIS)

    An integrated system of computational atomic database for spectroscopic investigation of x-ray lasers and x-ray sources is developed. The system consists of atomic data codes, database, a collisional radiative code, and programs for visualizing spectrum. Gain of Ni-like La laser is analyzed using the model. Furthermore, EUV spectrum from Xe is investigated, to identify measured transition arrays in 10 nm to 16 nm for the EUV light source. (author)

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

    Science.gov (United States)

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

    2008-10-01

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

  11. Small-angle x-ray scattering measurements of hydrogen evolution from an epitaxial Nb film

    International Nuclear Information System (INIS)

    Small-angle x-ray scattering (SAXS) measurements have been performed to investigate particle morphology during in situ hydrogen evolution from a 1000-A epitaxial Nb film on (112-bar0) sapphire initially loaded to saturation with hydrogen. The SAXS intensity follows the plate or disk single-particle form factor (Q-2, where Q is the wave-vector transfer) during hydrogen evolution. A fit to this power-law behavior yields a plate thickness of ≅7 A. A second power-law behavior (Q-3) was observed after complete hydrogen evolution. This power law corresponds to the small-angle scattering response from edge dislocations and is consistent with the broadening of the lattice mosaic induced by hydride decomposition

  12. Nano structured materials studied by coherent X-ray diffraction

    International Nuclear Information System (INIS)

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  13. Nano structured materials studied by coherent X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Gulden, Johannes

    2013-03-15

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  14. [Prediction of Protein Conformational Mobility and Evaluation of Its Reliability Using Small-Angle X-ray Scattering].

    Science.gov (United States)

    Knyazev, S N; Kalyakin, V Y; Deryabin, I N; Fedorov, B A; Smirnov, A V; Stepanov, E O; Porozov, Yu B

    2015-01-01

    The "coarse-grained" model of protein conformational mobility is presented. We compared the trajectories of conformational motions predicted for five proteins using this model with the motion obtained by the method of the "nearest neighbor", based on small-angle X-ray scattering data. It is shown that for all studied proteins the sequence of conformations calculated on the basis of "coarse-grained" model and on the basis of the "nearest neighbor", coincides well, although there are exceptions. Some separate consideration should be given to each protein to discern the causes of these exceptions. PMID:26841499

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

    Science.gov (United States)

    Pabit, Suzette A.; Katz, Andrea M.; Tolokh, Igor S.; Drozdetski, Aleksander; Baker, Nathan; Onufriev, Alexey V.; Pollack, Lois

    2016-05-01

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

  16. 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

  17. Optical studies of massive X-ray binaries

    International Nuclear Information System (INIS)

    Photometric and spectroscopic studies of several optical counterparts of massive X-ray binaries are presented. Subjects of study were the binary systems:HD77581/4U0900-40 (Vela X-1), HD153919/4U1700-37, Wray 977/4U1223-62 and Sk160/4U0115-74 (=SMC X-1). (Auth.)

  18. X-ray study of weak interactions in two flavonoids

    Indian Academy of Sciences (India)

    Deepak Sharma; Vivek K Gupta; Goutam Brahmachari; Sadhan Mondal; Arindam Gangopadhyay

    2007-10-01

    X-ray diffraction studies were carried out on single crystals of two flavonoids, viz. 5-hydroxy-6,7,4′-trimethoxyflavone, C18H16O6, (I) and 5-hydroxy-3,7,4′-trimethoxyflavone, C18H16O6, (II). Crystal structures of both the flavonoids were solved by direct methods and refined by full-matrix least-squares procedures. In both the molecules, the benzopyran moiety is planar. The dihedral angle between the phenyl ring and the benzopyran portion is 5.50(4)° in (I) and 29.11(5)° in (II). In (I), the crystal packing is influenced by O–H…O hydrogen bonds, and weak C–H…O and $\\pi \\ldots \\pi$ interactions whereas in (II) the crystal structure is stabilized by the presence of four intermolecular short contacts of the type C–H…O. There is also one C–H$\\ldots \\pi$ hydrogen bond with H… centroid distance of < 2.7 Å. The molecules are further stabilized by – interactions.

  19. GLANCING INCIDENCE X-RAY STUDIES OF TITANIUM NITRIDE THIN FILMS USING A NEW MULTIPURPOSE LABORATORY SPECTROMETER

    OpenAIRE

    Buschert, R.C; Gibson, P.; Gissler, W.; Haupt, J.; Crabb, T.

    1989-01-01

    A multipurpose laboratory glancing angle X-ray spectrometer using a standard X-ray tube and a germanium solid state detector has been designed for vertical and horizontal diffraction scans, reflectivity and glancing angle fluorescence measurements. It has been used to study titanium nitride thin films grown under various conditions that vary the stoichiometry, strain, grain size, orientation and lattice parameter. In particular, films grown at liquid nitrogen substrate temperature show very h...

  20. Development of soft x-ray large solid angle camera onboard WF-MAXI

    Science.gov (United States)

    Kimura, Masashi; Tomida, Hiroshi; Ueno, Shiro; Kawai, Nobuyuki; Yatsu, Yoichi; Arimoto, Makoto; Mihara, Tatehiro; Serino, Motoko; Tsunemi, Hiroshi; Yoshida, Atsumasa; Sakamoto, Takanori; Kohmura, Takayoshi; Negoro, Hitoshi

    2014-07-01

    Wide-Field MAXI (WF-MAXI) planned to be installed in Japanese Experiment Module "Kibo" Exposed Facility of the international space station (ISS). WF-MAXI consists of two types of cameras, Soft X-ray Large Solid Angle Camera (SLC) and Hard X-ray Monitor (HXM). HXM is multi-channel arrays of CsI scintillators coupled with avalanche photodiodes (APDs) which covers the energy range of 20 - 200 keV. SLC is arrays of CCD, which is evolved version of MAXI/SSC. Instead of slit and collimator in SSC, SLC is equipped with coded mask allowing its field of view to 20% of all sky at any given time, and its location determination accuracy to few arcminutes. In older to achieve larger effective area, the number of CCD chip and the size of each chip will be larger than that of SSC. We are planning to use 59 x 31 mm2 CCD chip provided by Hamamatsu Photonics. Each camera will be quipped with 16 CCDs and total of 4 cameras will be installed in WF-MAXI. Since SLC utilize X-ray CCDs it must equip active cooling system for CCDs. Instead of using the peltier cooler, we use mechanical coolers that are also employed in Astro-H. In this way we can cool the CCDs down to -100C. ISS orbit around the earth in 90 minutes; therefore a point source moves 4 arcminutes per second. In order to achieve location determination accuracy, we need fast readout from CCD. The pulse heights are stacked into a single row along the vertical direction. Charge is transferred continuously, thus the spatial information along the vertical direction is lost and replaced with the precise arrival time information. Currently we are making experimental model of the camera body including the CCD and electronics for the CCDs. In this paper, we show the development status of SLC.

  1. Crystal defect studies using x-ray diffuse scattering

    International Nuclear Information System (INIS)

    Microscopic lattice defects such as point (single atom) defects, dislocation loops, and solute precipitates are characterized by local electronic density changes at the defect sites and by distortions of the lattice structure surrounding the defects. The effect of these interruptions of the crystal lattice on the scattering of x-rays is considered in this paper, and examples are presented of the use of the diffuse scattering to study the defects. X-ray studies of self-interstitials in electron irradiated aluminum and copper are discussed in terms of the identification of the interstitial configuration. Methods for detecting the onset of point defect aggregation into dislocation loops are considered and new techniques for the determination of separate size distributions for vacancy loops and interstitial loops are presented. Direct comparisons of dislocation loop measurements by x-rays with existing electron microscopy studies of dislocation loops indicate agreement for larger size loops, but x-ray measurements report higher concentrations in the smaller loop range. Methods for distinguishing between loops and three-dimensional precipitates are discussed and possibilities for detailed studies considered. A comparison of dislocation loop size distributions obtained from integral diffuse scattering measurements with those from TEM show a discrepancy in the smaller sizes similar to that described above

  2. Crystal defect studies using x-ray diffuse scattering

    Energy Technology Data Exchange (ETDEWEB)

    Larson, B.C.

    1980-01-01

    Microscopic lattice defects such as point (single atom) defects, dislocation loops, and solute precipitates are characterized by local electronic density changes at the defect sites and by distortions of the lattice structure surrounding the defects. The effect of these interruptions of the crystal lattice on the scattering of x-rays is considered in this paper, and examples are presented of the use of the diffuse scattering to study the defects. X-ray studies of self-interstitials in electron irradiated aluminum and copper are discussed in terms of the identification of the interstitial configuration. Methods for detecting the onset of point defect aggregation into dislocation loops are considered and new techniques for the determination of separate size distributions for vacancy loops and interstitial loops are presented. Direct comparisons of dislocation loop measurements by x-rays with existing electron microscopy studies of dislocation loops indicate agreement for larger size loops, but x-ray measurements report higher concentrations in the smaller loop range. Methods for distinguishing between loops and three-dimensional precipitates are discussed and possibilities for detailed studies considered. A comparison of dislocation loop size distributions obtained from integral diffuse scattering measurements with those from TEM show a discrepancy in the smaller sizes similar to that described above.

  3. Powder X-ray diffraction study af alkali alanates

    DEFF Research Database (Denmark)

    Cao, Thao; Mosegaard Arnbjerg, Lene; Jensen, Torben René

    Powder X-ray diffraction study of alkali alanates Thao Cao, Lene Arnbjerg, Torben R. Jensen. Center for Materials Crystallography (CMC), Center for Energy Materials (CEM), iNANO and Department of Chemistry, Aarhus University, DK-8000, Denmark. Abstract: To meet the energy demand in the future...

  4. Flash X-Ray Injector Study

    Energy Technology Data Exchange (ETDEWEB)

    Paul, A C

    2004-03-26

    The study described in this report1 models the FXR injector from the cathode to the exit of the injector. The calculations are compared to actual experimental measurements, table 1. In these measurements the anode voltage was varied by changing the Marks-Bank charging voltage. The anode-cathode spacing was varied by adjusting the location of the cathode in hopes of finding an island of minimum emittance (none found). The bucking coil current was set for zero field on the cathode. In these measurements, a pepper-pot mask was inserted into FXR at beam bug 135 and viewed downstream via a wiggle probe diagnostic at cell gap J21, figure 1. The observed expansion of the beamlets passing through the mask of known geometric layout and hole size allow a calculation of the phase space beam properties.

  5. Application of small angle X-ray scattering synchrotron technology for measuring ovine meat quality.

    Science.gov (United States)

    Hoban, J M; Hopkins, D L; Kirby, N; Collins, D; Dunshea, F R; Kerr, M G; Bailes, K; Cottrell, J J; Holman, B W B; Brown, W; Ponnampalam, E N

    2016-07-01

    A small angle X-ray scattering (SAXS) synchrotron was used to evaluate 100 ovine m. longissimus lumborum, representing lamb (n=50) and sheep (n=50). The diffraction of X-rays gives information on muscle myofibril structure and fat content. The linear relationships between SAXS measures with measures such as, shear force, intramuscular fat content (IMF) and collagen content/solubility, were investigated. A relationship was found between the d-spacing of the actin/myosin fibril spacing (SAX1 and SAX2) and the cross sectional area of the rhombohedral unit cell (Cell area) and shear force after 1 and 5day ageing. There was a positive relationship between IMF and a SAXS Fat area measure. There was a muscle site effect on SAX1, SAX2 and Cell area, with the cranial site having a larger distance between myofibrils. The potential of SAXS as a powerful research tool to determine not only the structural components of ovine tenderness, but also the fat content related to IMF is evident. PMID:26971308

  6. 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.

  7. 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.

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

    DEFF Research Database (Denmark)

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

    1984-01-01

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

  9. Ultra-high resolution small-angle x-ray diffractometry: measurements of very large periods in biological fibres

    International Nuclear Information System (INIS)

    The technique of small-angle x-ray scattering using a synchrotron source is described. Improved instrumentation is shown, using multiple-reflection crystal monoliths as high-quality collimators. A small-angle diffraction pattern from frog Sartorius muscle, using the improved apparatus, is shown. (U.K.)

  10. Three dimensional reconstruction of nanoislands from grazing-incidence small-angle X-ray scattering

    Science.gov (United States)

    Yefanov, O. M.; Vartanyants, I. A.

    2009-02-01

    The combination of grazing-incidence small-angle x-ray scattering (GISAXS) with tomographic methods and phase retrieval is proposed for the reconstruction of the three-dimensional (3D) electron density of nanometer sized objects. In this approach GISAXS data from a small object are collected successively at different azimuthal angular positions. This 3D intensity distribution in reciprocal space is used for the phase retrieval and reconstruction of the 3D electron density. The power of our approach is demonstrated in a series of calculations performed in the frame of kinematical and distorted-wave Born approximation (DWBA) theories for the case of GISAXS scattering on a 200 nm island in the form of truncated pyramid.

  11. 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.

  12. Structural characterization of surface-functionalized nanoparticles and nanocomposites by small angle x-ray scattering

    International Nuclear Information System (INIS)

    Full text: One of the driving forces in the development and chemical optimization of inorganic-organic nanocomposites is the substitution of traditional compounds, such as metals, ceramics or polymers, with superior physical properties. An example for the need of nanocomposites is the replacement of heavy weight materials, which cause a quite bad fuel economy in transportation industry, by novel light systems with similar or even better properties. Inorganic-organic nanocomposites often show excellent mechanical properties if the inorganic nanobuilding blocks such as nanoparticles are crosslinked with the organic matrix. This is achieved by surface-functionalization of the nanoparticles. Structural characterization of the resulting nanocomposites is performed by small angle x-ray scattering (SAXS) measurements: From the SAXS intensity, information on the size of nanoparticles and their aggregation behaviour is obtained. The effect of different surface-functionalization and different amounts of surface coverage on the aggregation behaviour of the nanoparticles within the nanocomposites are presented. (author)

  13. X-ray imaging in advanced studies of ophthalmic diseases

    International Nuclear Information System (INIS)

    Microscopic characterization of pathological tissues has one major intrinsic limitation, the small sampling areas with respect to the extension of the tissues. Mapping possible changes on vast tissues and correlating them with large ensembles of clinical cases is not a feasible procedure for studying most diseases, as for instance vision loss related diseases and, in particular, the cataract. Although intraocular lens implants are successful treatments, cataract still is a leading public-health issue that grows in importance as the population increases and life expectancy is extended worldwide. In this work we have exploited the radiation-tissue interaction properties of hard x-rays--very low absorption and scattering--to map distinct lesions on entire eye lenses. At the used synchrotron x-ray photon energy of 20 keV (wavelength λ=0.062 nm), scattering and refraction are angular resolved effects. It allows the employed x-ray image technique to efficiently characterize two types of lesions in eye lenses under cataractogenesis: distributions of tiny scattering centers and extended areas of fiber cell compaction. The data collection procedure is relatively fast; allowing dozens of samples to be totally imaged (scattering, refraction, and mass absorption images) in a single day of synchrotron beam time. More than 60 cases of canine cataract, not correlated to specific causes, were investigated in this first application of x-rays to image entire lenses. Cortical opacity cases, or partial opacity, could be related to the presence of calcificated tissues at the cortical areas, clearly visible in the images, whose elemental contents were verified by micro x-ray fluorescence as very rich in calcium. Calcificated tissues were also observed at nuclear areas in some cases of hypermature cataract. Total opacity cases without distinguishable amount of scattering centers consist in 70% of the analyzed cases, where remarkable fissure marks owing to extended areas of fiber cell

  14. 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)

    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)

  15. Portable high precision small/wide angle X-ray scattering diffractometer

    CERN Document Server

    Gaponov, Y A; Kochubey, D I; Tolochko, B P

    2001-01-01

    The portable high precision small/wide angle X-ray scattering diffractometer (modified Bonze-Hart optical scheme) was designed and developed for the investigation of structure rearrangement during liquid state-solid state transformations (with reaction time of 10 h or more) for the investigation of the process of solid state phase formation. The FEM detectors are used as monitor and detector. The double crystal Si sub 1 sub 1 sub 1 analyzer (with changeable relative angle of the second crystal) is used as analyzer. All controlling electronics are designed in CAMAC. The diffractometer is controlled by a Sun SPARCStation with SVIC/VCC modules under a Solaris 2.4 operating system, and allows one to obtain the SAXS curves with accuracies (on s-vector for photon energy 8 keV) of about delta s approx 0.002 nm sup - sup 1 , s sub m sub i sub n approx 0.005 nm sup - sup 1 (scattering centers with the size of about 200-500 nm may be observed) and s sub m sub a sub x approx 50 nm sup - sup 1 (scattering angle is about ...

  16. A large area, 2-D, high-pressure MWPC for wide angle X-ray diffraction

    International Nuclear Information System (INIS)

    Multi wire proportional counters (MWPCs) possess all the required features for recording X-ray diffraction patterns: large area, high detective quantum efficiency (DQE), low dead time and simultaneous spatial and spectral information. However, their suitability as wide-angle diffraction is compromised by an effect known as parallax broadening. This phenomenon is due to the low density of the gas in the detector, where photons incident at large angles following the same ray may interact at different points along it and therefore appear as different coordinates in the image. One way to reduce this effect is by increasing the density of the absorbing medium in order to ensure the photons interact in a thinner gas layer, this can be achieved if the pressure of the gas in the detector is increased. We present here a high-pressure (5 bar) detector which has the potential to bring the desirable features of a photon counting system to wide-angle diffraction experiments. The preliminary results are also presented. (orig.)

  17. Portable high precision small/wide angle X-ray scattering diffractometer

    International Nuclear Information System (INIS)

    The portable high precision small/wide angle X-ray scattering diffractometer (modified Bonze-Hart optical scheme) was designed and developed for the investigation of structure rearrangement during liquid state-solid state transformations (with reaction time of 10 h or more) for the investigation of the process of solid state phase formation. The FEM detectors are used as monitor and detector. The double crystal Si111 analyzer (with changeable relative angle of the second crystal) is used as analyzer. All controlling electronics are designed in CAMAC. The diffractometer is controlled by a Sun SPARCStation with SVIC/VCC modules under a Solaris 2.4 operating system, and allows one to obtain the SAXS curves with accuracies (on s-vector for photon energy 8 keV) of about δs∼0.002 nm-1, smin∼0.005 nm-1 (scattering centers with the size of about 200-500 nm may be observed) and smax∼50 nm-1 (scattering angle is about 80 deg.)

  18. X-ray and neutron diffraction studies of chalcocite oxidation

    International Nuclear Information System (INIS)

    Full text: The mineral chalcocite (Cu2S), which is often found in the enriched zone of sulphide deposits, is an important source of copper. The oxidation behaviour of chalcocite is of interest in terms of the mineral exploration technology and also for understanding the behaviour of the mineral under roasting conditions. Recently, the oxidation of chalcocite was the subject of a study by Dunn et al (1994) involving the use of thermal analysis, scanning electron microscopy, electron probe microanalysis, powder x-ray diffraction (XRD) and Fourier transform spectroscopy. The study indicated that the following transformations are likely to occur: at 430-490 deg C, partial conversion of Cu2S to Cu2O and CuSO4 via Cu1.96S and Cu1.80S; at 490-590 deg C, further conversion of Cu2S to Cu2O, CuO CuSO4 and CuSO4; and at 590-820 deg C, Cu2O, CuO CuSO4 and CuSO4 to CuO. In this study, the oxidation of chalcocite was analysed from a crystallographic perspective. Ambient x-ray diffraction and in-situ neutron diffraction were used to determine the phases present, at various temperatures, as oxidation progressed. Ambient x-ray experiments involved heating chalcocite powder in an air stream, to a target temperature, cooling it to room temperature in a nitrogen stream, and analysing by Bragg-Brentano x-ray powder diffractometry. In situ neutron experiments consisted of, powdered chalcocite being heated in an air stream to various target temperatures, and then held in a nitrogen stream at the given temperature while Medium Resolution Powder Diffractometry (EPD) was performed. Rietveld modelling of the x-ray and neutron data was used to confirm the phase identifications made by search/match analysis, and to then map the variations in phase levels with temperature as the oxidation progresses through various phase transformations. The talk will consider the results obtained from the study with particular reference to the identification of previously undetected phases, and the differences

  19. X-ray absorption studies of battery materials

    Energy Technology Data Exchange (ETDEWEB)

    McBreen, J.

    1996-10-01

    X-ray absorption spectroscopy (XAS) is ideal for {ital in}{ital situ} studies of battery materials because both the probe and signal are penetrating x rays. The advantage of XAS being element specific permits investigation of the environment of a constituent element in a composite material. This makes it very powerful for studying electrode additives and corrosion of individual components of complex metal hydride alloys. The near edge part of the spectrum (XANES) provides information on oxidation state and site symmetry of the excited atom. This is particularly useful in study of corrosion and oxidation changes in cathode materials during charge/discharge cycle. Extended fine structure (EXAFS) gives structural information. Thus the technique provides both chemical and structural information. Since XAS probes only short range order, it can be applied to study of amorphous electrode materials and electrolytes. This paper discusses advantages and limitations of the method, as well as some experimental aspects.

  20. X-Ray Study of Pressure-Collapsed Fullerite

    OpenAIRE

    Kosowsky, S. D.; Hsu, C.-H.; Chen, Nancy H.; Moshary, Fred; Pershan, Peter S.; Silvera, Isaac F.

    1993-01-01

    X-ray-diffraction studies are described for a new phase of carbon called collapsed fullerite (CF) that was produced by application of high pressure to fullerite (C\\(_{60}\\)). At \\(\\sim\\)20 GPa there is an irreversible transition to a phase that has neither the (111) Bragg peak of diamond nor any of the Bragg peaks associated with the fcc phase of C\\(_{60}\\). The spectrum of CF is flat and featureless in the range of study.

  1. X-ray apparatus

    International Nuclear Information System (INIS)

    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.)

  2. Studies on the development and applicability of modern industrial X-ray paper in dental radiology as a substitute for X-ray films

    International Nuclear Information System (INIS)

    The author investigated the applicability of advanced industrial X-ray paper (KODAK ''Industrex Instant'' 610) as a substitute for X-ray films in various fields of dental radiology. The studies covered intraoral and extraoral pictures of the teeth and shull, images of the hand skeleton produced by a dental X-ray device, and enlarged pantomograms, tomograms, and lateral and sagittal tele-X-ray images produced by special X-ray devices. In spite of the progress reported in the last few years in the field of X-ray papers, they cannot be recommended for clinical applications. (orig./MG)

  3. A beam expander facility for studying x-ray optics

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Hornstrup, Allan; Frederiksen, P.; Nilsson, C.; Grundsøe, Peter; Ørup, P.; Jacobsen, E.; Schnopper, H. W.; Lewis, R.; Hall, C.

    1992-01-01

    The detailed study of the performance of full scale x-ray optics often requires the illumination of large areas. This paper describes a beam expander facility at the Daresbury Synchrotron Radiation Facility. It combines monochromatization and beam expansion in one dimension. The beam expansion is...... obtained from an extremely asymmetric reflection in a large single crystal of Si. An expansion of a factor of 50 was obtained in one dimension. The expanded beam of ~85 mm is limited only by the crystal size. The facility is installed in a 12-m-long hutch. A specific application, in which a high throughput...... x-ray telescope will be studied, is described in detail. Review of Scientific Instruments is copyrighted by The American Institute of Physics....

  4. Future lunar mission Active X-ray Spectrometer development: Surface roughness and geometry studies

    Science.gov (United States)

    Naito, M.; Hasebe, N.; Kusano, H.; Nagaoka, H.; Kuwako, M.; Oyama, Y.; Shibamura, E.; Amano, Y.; Ohta, T.; Kim, K. J.; Lopes, J. A. M.

    2015-07-01

    The Active X-ray Spectrometer (AXS) is considered as one of the scientific payload candidates for a future Japanese mission, SELENE-2. The AXS consists of pyroelectric X-ray generators and a Silicon Drift Detector to conduct X-Ray Fluorescence spectroscopy (XRF) on the Moon to measure major elements: Mg, Al, Si, Ca, Ti, and Fe; minor elements: Na, K, P, S, Cr and Mn; and the trace element Ni depending on their concentration. Some factors such as roughness, grain size and porosity of sample, and the geometry of X-ray incidence, emission and energy will affect the XRF measurements precision. Basic studies on the XRF are required to develop the AXS. In this study, fused samples were used to make homogeneous samples free from the effect of grain size and porosity. Experimental and numerical studies on the XRF were conducted to evaluate the effects from incidence and emission angles and surface roughness. Angle geometry and surface roughness will be optimized for the design of the AXS on future missions from the results of the experiment and the numerical simulation.

  5. Future lunar mission Active X-ray Spectrometer development: Surface roughness and geometry studies

    International Nuclear Information System (INIS)

    The Active X-ray Spectrometer (AXS) is considered as one of the scientific payload candidates for a future Japanese mission, SELENE-2. The AXS consists of pyroelectric X-ray generators and a Silicon Drift Detector to conduct X-Ray Fluorescence spectroscopy (XRF) on the Moon to measure major elements: Mg, Al, Si, Ca, Ti, and Fe; minor elements: Na, K, P, S, Cr and Mn; and the trace element Ni depending on their concentration. Some factors such as roughness, grain size and porosity of sample, and the geometry of X-ray incidence, emission and energy will affect the XRF measurements precision. Basic studies on the XRF are required to develop the AXS. In this study, fused samples were used to make homogeneous samples free from the effect of grain size and porosity. Experimental and numerical studies on the XRF were conducted to evaluate the effects from incidence and emission angles and surface roughness. Angle geometry and surface roughness will be optimized for the design of the AXS on future missions from the results of the experiment and the numerical simulation

  6. Future lunar mission Active X-ray Spectrometer development: Surface roughness and geometry studies

    Energy Technology Data Exchange (ETDEWEB)

    Naito, M., E-mail: com-nm@akane.waseda.jp [School of Advanced Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo (Japan); Hasebe, N. [School of Advanced Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo (Japan); Research Institute for Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo (Japan); Kusano, H. [Research Institute for Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo (Japan); Nagaoka, H. [School of Advanced Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo (Japan); Research Institute for Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo (Japan); Kuwako, M.; Oyama, Y. [School of Advanced Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo (Japan); Shibamura, E.; Amano, Y. [Research Institute for Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku, Tokyo (Japan); Ohta, T. [School of Education and Integrated Arts and Science, Waseda University, 1-104 Totsuka, Shinjuku, Tokyo (Japan); Kim, K.J. [Korea Institute of Geoscience and Mineral Resources, Gwahang-no 124, Yuseong-gu, Daejeon 305-350 (Korea, Republic of); Lopes, J.A.M. [Department of Physics, University of Coimbra, Apartado 3020, 3001-401 Coimbra (Portugal); Instituto Superior de Engenharia de Coimbra, 3030-199 Coimbra (Portugal)

    2015-07-11

    The Active X-ray Spectrometer (AXS) is considered as one of the scientific payload candidates for a future Japanese mission, SELENE-2. The AXS consists of pyroelectric X-ray generators and a Silicon Drift Detector to conduct X-Ray Fluorescence spectroscopy (XRF) on the Moon to measure major elements: Mg, Al, Si, Ca, Ti, and Fe; minor elements: Na, K, P, S, Cr and Mn; and the trace element Ni depending on their concentration. Some factors such as roughness, grain size and porosity of sample, and the geometry of X-ray incidence, emission and energy will affect the XRF measurements precision. Basic studies on the XRF are required to develop the AXS. In this study, fused samples were used to make homogeneous samples free from the effect of grain size and porosity. Experimental and numerical studies on the XRF were conducted to evaluate the effects from incidence and emission angles and surface roughness. Angle geometry and surface roughness will be optimized for the design of the AXS on future missions from the results of the experiment and the numerical simulation.

  7. High-resolution soft-X-ray beamline ADRESS at Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies

    CERN Document Server

    Strocov, V N; Flechsig, U; Schmidt, T; Imhof, A; Chen, Q; Raabe, J; Betemps, R; Zimoch, D; Krempasky, J; Piazzalunga, A; Wang, X; Grioni, M; Patthey, L

    2009-01-01

    We describe the concepts and technical realization of the high-resolution soft-X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for Resonant Inelastic X-ray Scattering (RIXS) and Angle-Resolved Photoelectron Spectroscopy (ARPES). The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0-180 deg rotatable linear polarizations) but also the energy without changing the gap. The beamline optics is based on the well-established scheme of plane grating monochromator (PGM) operating in collimated light. The ultimate resolving power E/dE is above 33000 at 1 keV photon energy. The choice of blazed vs lamellar gratings and optimization of their profile parameters is described. Due to glancing angles on the mirrors as well as optimized groove densities and profiles of the gratings, high photon flux is achieved up to 1.0e13 photons/s/0.01%BW at 1 keV. Ellipsoida...

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

    Energy Technology Data Exchange (ETDEWEB)

    Tranquada,J.M.

    2008-09-01

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

  9. Resonant soft x-ray scattering studies of buried interfaces

    International Nuclear Information System (INIS)

    Resonant soft x-ray scattering (RSXS) is a unique experimental tool to access the electronic properties of buried interfaces in heterostructures that contain transition metal oxides. In this contribution, studies of SrTiO3/LaAlO3, SrTiO3/(La,Ca)MnO3 and NdGaO3/(La,Ca)MnO3 interfaces are presented. Specifically, RSXS was employed to examine the electronic reconstruction of Ti 3d and O 2p valence states at the interfaces of SrTiO3/LaAlO3 superlattices. Similarly, we used resonant soft x-ray reflectivity to investigate the electronic structure at the interfaces of SrTiO3/(La,Ca)MnO3 and NdGaO3/(La,Ca)MnO3 thin film systems.

  10. Resonance magnetic x-ray scattering study of erbium

    DEFF Research Database (Denmark)

    Sanyal, M.K.; Gibbs, D.; Bohr, J.;

    1994-01-01

    of this magnetic scattering and analyzed it using a simple model based on electric dipole and quadrupole transitions among atomic orbitals. The line shapes can be fitted to a magnetic structure combining both c-axis-modulated and basal-plane components. Below 18 K, we have observed unusual behavior......The magnetic phases of erbium have been studied by resonance x-ray-scattering techniques. When the incident x-ray energy is tuned near the L(III) absorption edge, large resonant enhancements of the magnetic scattering are observed above 18 K. We have measured the energy and polarization dependence...... of the magnetic scattering as a function of energy, whose origin is not understood....

  11. Thickness determination of molecularly thin lubricant films by angle-dependent X-ray photoelectron spectroscopy

    International Nuclear Information System (INIS)

    An angle-dependent X-ray photoelectron spectroscopy (XPS) method used to measure the thickness of molecularly thin lubricants was developed. The method was built based on an island model of patched overlayer on a flat substrate by using the photoemission signal solely from the lubricant film. Typical molecularly thin Zdol films on the CHx overcoat of unused commercial magnetic disks were measured to verify the metrology. The lubricant thickness determined by the metrology was equal to the recent result by thermostatic high vacuum atomic force microscopy. The measured deduction in the thickness of the molecularly thin lubricant films, successively irradiated by the monochromatic source operated at 14 kV/250 W, was as low as 1 A during the first irradiation hour. XPS spectra showed that no hydrocarbons, water or oxygen were adsorbed over the Zdol outer surfaces in the tested XPS conditions. The inelastic mean free path (IMFP) of C 1s in Zdol or in CHx was found to be independent of take off angle (TOA) when TOA o. The IMFP of C 1s in Zdol was ∼63.5 A and the lubricant island thickness was ∼35 A

  12. X-Ray Tomography Studies of Prehistoric Ceramic Artifacts

    Science.gov (United States)

    Pavel, Carmen; Constantin, Florin; Suciu, Cosmin Ioan; Bugoi, Roxana

    2014-02-01

    X-ray Computed Tomography (CT) is a powerful non-destructive technique that can yield interesting structural information not discernible through visual examination only. This paper presents the results of the CT scans of four objects belonging to the Romanian cultural heritage attributed to the Vinča, Cucuteni and Cruceni-Belegiš cultures. The study was performed with an X-ray tomographic device developed at the Department for Applied Nuclear Physics from Horia Hulubei National Institute for Nuclear Physics and Engineering in Măgurele, Romania. This apparatus was specially designed for archaeometric studies of low-Z artifacts: ceramic, wood, bone. The tomographic investigations revealed the internal configuration of the objects and provided information about the degree to which the previous manipulations affected the archaeological items. Based on the X-ray images resulting from the CT scans, hints about the techniques used in the manufacturing of the artifacts were obtained, as well as some indications useful for conservation/restoration purposes.

  13. Development of an x-ray beam line at the NSLS for studies in materials science using x-ray absorption spectroscopy: Annual progress report

    International Nuclear Information System (INIS)

    The research programs reported span virtually the entire range of condensed matter studies involving the fields of solid state physics, chemistry, electrochemistry, materials science and biochemistry. Results are discussed for various groups. Topics reported include work on amorphous chalcogenide semiconductors, particularly photostructural changes, kinetics of structural changes and rapid quenching, bond strengths, force constants and phonons. Also reported are temperature dependent EXAFS studies of bonding in high temperature alloys, amorphous systems, disordered alloys and studies of resolve electronic structure, EXAFS and XANES studies of permanent magnet systems based on Nd2Fe14B, glancing angle EXAFS study of Nb/Al and Nb/Si interfacial systems, x-ray absorption of krypton-implanted solids and high dose implants into silicon, and x-ray absorption and EXAFS studies of superconducting oxide compounds of Cu and related magnetic systems. Work is also reported on XAFS measurements on the icosahedral phase

  14. Simulation studies of atomic resolution X-ray holography

    Indian Academy of Sciences (India)

    Yogesh Kashyap; P S Sarkar; Amar Sinha; B K Godwal

    2004-02-01

    X-ray holography is a new method of structure determination based on measurement of interference of a known reference wave with an unknown object wave (containing information on atomic sites scattering the reference wave) so that phase information is preserved. Unlike X-ray diffraction, it does not demand for translational periodicity in the material. It is based on the idea similar to that of optical holography and has been tested on crystals, quasicrystals, thin films and doped semiconductors for their structure determination. In order to analyse potentials and limitations of this technique, we have carried out theoretical simulation studies on simple structures. In this paper we describe the basic algorithm of hologram generation and reconstruction of atomic positions from generated data. We illustrate this technique using Fe (bcc) single crystal as sample case to demonstrate its capabilities and limitations. Simulations were carried out on the Cu (fcc) structure and on complex structure such as the Al–Pd–Mn quasicrystal. Technical issues such as low signal to noise ratio, twin image problem etc have been discussed briefly to emphasize the need for high intensity X-ray source such as synchrotron for experiments and proper reconstruction algorithm. Finally the scope and potential of this technique have been discussed.

  15. X-ray graphical and thermodynamical study of mercury arsenates

    International Nuclear Information System (INIS)

    Purposes of the work are both determination of lattice parameters on the base of X-ray graphical data and experimental study of thermal conduction dependence of mercury arsenates Hg(AsO3)2 and Hg3(AsO4)2. In this work for the first time the parameters of elementary cell thermal conduction in the range 298.15-625 K were determined. Formation of equilibrium contents of mercury arsenates was confirmed by X-ray phase analysis conducted on DRON-2,0 unit under Cu K - radiation. Curves of thermal-differential analysis show, that Hg(AsO3)2 and Hg3(AsO4)2 melting incongruently, relatively at 725 and 790 grad C. Displaying of X-ray- grammars of examined compounds have been conducted by homology method. On the base the displaying parameter of lattice crystallization were determined. Further arsenates were exposed to calorimetric research for determination of its thermal conduction. It is shown, that Hg3(AsO4)2 thermal conduction has maximum at 448 K and then it value is go down at 473 K and then smoothly increasing. It was supposed, such behavior is related with second kind phase transformation

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

    Science.gov (United States)

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

    2014-12-01

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

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

    Science.gov (United States)

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

    2016-07-11

    In this paper we present a fast model system for monitoring the recrystallization of quench-cooled amorphous xylitol using Raman spectroscopy and wide-angle X-ray scattering. The use of these two methods enables comparison between surface and bulk crystallization. Non-ordered mesoporous silica micro-particles were added to the system in order to alter the rate of crystallization of the amorphous xylitol. Raman measurements showed that adding silica to the system increased the rate of surface crystallization, while X-ray measurements showed that the rate of bulk crystallization decreased. Using this model system it is possible to measure fast changes, which occur in minutes or within a few hours. Raman-spectroscopy and wide-angle X-ray scattering were found to be complementary techniques when assessing surface and bulk crystallization of amorphous xylitol. PMID:27163527

  18. X-ray microbeam bystander studies between stripes of dose

    International Nuclear Information System (INIS)

    Evidence is emerging that radiation exposure can change communication between cells of the same type, as well as between cells of different cell compartments within tissues. We are using a novel X-ray Microprobe Beamline at the Advanced Light Source (ALS) at LBNL to investigate bystander effects of low doses in well-characterized human mammary epithelial cells (HMEC) and human skin fibroblasts (HSF). The ALS facility is capable of producing a beam of 12.5 keV X-rays with a focussed spot size of 2 square micron and a wide range of doses and dose-rates. Unlike normal X-ray sources, this beam has a very small background of either low- or high-energy X-rays. In initial studies, cultures grown in microwell slide chambers have been irradiated with precise stripes of dose up to 100 micron wide. We are using fluorescence microscopy on a high-precision-controlled microscope stage to evaluate several classes of radiation-induced soluble signals, how these signals are communicated across cell compartments, and how radiation changes cell signaling both acutely and chronically. To evaluate the spatial dependence of intercellular communications, we varied the distance between dose stripes from 0-900 micrometers. We are investigating the radiation induction of p21Cip1 (CDKN1a), and phosphorylation of H2AX and p53 serine-15 as endpoints. Our preliminary results indicate that there is a dose- and cell-type-dependent expression of p53 serine-15P within 10 minutes after exposure to a 100 micron wide stripe of dose. Immunohistochemistry of p53-serine-15P-positive cells traversed by the beam illuminates the path of the X-ray microbeam, with epithelial cells responding more rapidly and with greater intensity than fibroblasts. The intensity of the immunofluorescence scales with the dose. The number of p53-serine-15P-positive cells in the unirradiated cell populations between the stripes has been counted as a measure of the bystander effect, and compared to appropriate controls. We will

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

    International Nuclear Information System (INIS)

    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)

  20. An angle-dependent estimation of CT x-ray spectrum from rotational transmission measurements

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Yuan, E-mail: yuan.lin@duke.edu; Samei, Ehsan [Carl E. Ravin Advanced Imaging Laboratories, Duke University Medical Center, Durham, North Carolina 27705 and Physics Department, Duke University, Durham, North Carolina 27708 (United States); Ramirez-Giraldo, Juan Carlos [Siemens Medical Solutions, Malvern, Pennsylvania 19355 (United States); Gauthier, Daniel J. [Physics Department, Duke University, Durham, North Carolina 27708 (United States); Stierstorfer, Karl [Siemens Healthcare, Forchheim 91301 (Germany)

    2014-06-15

    Purpose: Computed tomography (CT) performance as well as dose and image quality is directly affected by the x-ray spectrum. However, the current assessment approaches of the CT x-ray spectrum require costly measurement equipment and complicated operational procedures, and are often limited to the spectrum corresponding to the center of rotation. In order to address these limitations, the authors propose an angle-dependent estimation technique, where the incident spectra across a wide range of angular trajectories can be estimated accurately with only a single phantom and a single axial scan in the absence of the knowledge of the bowtie filter. Methods: The proposed technique uses a uniform cylindrical phantom, made of ultra-high-molecular-weight polyethylene and positioned in an off-centered geometry. The projection data acquired with an axial scan have a twofold purpose. First, they serve as a reflection of the transmission measurements across different angular trajectories. Second, they are used to reconstruct the cross sectional image of the phantom, which is then utilized to compute the intersection length of each transmission measurement. With each CT detector element recording a range of transmission measurements for a single angular trajectory, the spectrum is estimated for that trajectory. A data conditioning procedure is used to combine information from hundreds of collected transmission measurements to accelerate the estimation speed, to reduce noise, and to improve estimation stability. The proposed spectral estimation technique was validated experimentally using a clinical scanner (Somatom Definition Flash, Siemens Healthcare, Germany) with spectra provided by the manufacturer serving as the comparison standard. Results obtained with the proposed technique were compared against those obtained from a second conventional transmission measurement technique with two materials (i.e., Cu and Al). After validation, the proposed technique was applied to measure

  1. An angle-dependent estimation of CT x-ray spectrum from rotational transmission measurements

    International Nuclear Information System (INIS)

    Purpose: Computed tomography (CT) performance as well as dose and image quality is directly affected by the x-ray spectrum. However, the current assessment approaches of the CT x-ray spectrum require costly measurement equipment and complicated operational procedures, and are often limited to the spectrum corresponding to the center of rotation. In order to address these limitations, the authors propose an angle-dependent estimation technique, where the incident spectra across a wide range of angular trajectories can be estimated accurately with only a single phantom and a single axial scan in the absence of the knowledge of the bowtie filter. Methods: The proposed technique uses a uniform cylindrical phantom, made of ultra-high-molecular-weight polyethylene and positioned in an off-centered geometry. The projection data acquired with an axial scan have a twofold purpose. First, they serve as a reflection of the transmission measurements across different angular trajectories. Second, they are used to reconstruct the cross sectional image of the phantom, which is then utilized to compute the intersection length of each transmission measurement. With each CT detector element recording a range of transmission measurements for a single angular trajectory, the spectrum is estimated for that trajectory. A data conditioning procedure is used to combine information from hundreds of collected transmission measurements to accelerate the estimation speed, to reduce noise, and to improve estimation stability. The proposed spectral estimation technique was validated experimentally using a clinical scanner (Somatom Definition Flash, Siemens Healthcare, Germany) with spectra provided by the manufacturer serving as the comparison standard. Results obtained with the proposed technique were compared against those obtained from a second conventional transmission measurement technique with two materials (i.e., Cu and Al). After validation, the proposed technique was applied to measure

  2. Retrospective epidemiological study of the X-Ray exposure

    Energy Technology Data Exchange (ETDEWEB)

    Ivanov, E. V.; Kalnitsky, S. A.; Shubic, V. M.

    2004-07-01

    There are a large amount of epidemiological studies nowadays in the world which are devoted to the analysis of the medical effects and the radiation risk. But a few of them deal with the analysis of the medical diagnostic radiation influence on health. It is appropriate, for the large compared contingent of the patients and the possibility of comparing them in several decades after the exposure are necessary for the evaluation of the influence of small doses on health. Meanwhile the X-ray exposure of the population is one of the most important types of radiation influence among all the kinds and sources of radiation. It is characterized by high dose rate and the possibility of multiple influence on a weakened and diseased organism. In connection with that, the eleven of the indices of population health was analyzed for the first time in Russia. The population was influenced by different levels of X-ray exposure 10-50 years ago. The research was carried out in the two groups of the Tumen (Siberia) regions. These regions are more or less equal in the climatic; ecologic, social-economic and demographic conditions. Nevertheless, they are different even only in the value of accumulated doses of X-ray exposure of the population (mostly in 50-70s) more than three times. Disease and mortality cancer of population of the last ten years in the regions were analyzed. The regions were selected taking into account the absence of the influence of other possible negative environmental factors. The data are found as the result of the dosimetric and epidemiological studies, and the processing of the archive statistic information. These researches demonstrated that on the whole there is the considerable statistically proved rise of disease cancer in the regions with high level of long term accumulated doses of X-ray exposure of population. Inter-district differences in disease and mortality cancer run up to three times among people aged 60 and older. There are no statistically

  3. Retrospective epidemiological study of the X-Ray exposure

    International Nuclear Information System (INIS)

    There are a large amount of epidemiological studies nowadays in the world which are devoted to the analysis of the medical effects and the radiation risk. But a few of them deal with the analysis of the medical diagnostic radiation influence on health. It is appropriate, for the large compared contingent of the patients and the possibility of comparing them in several decades after the exposure are necessary for the evaluation of the influence of small doses on health. Meanwhile the X-ray exposure of the population is one of the most important types of radiation influence among all the kinds and sources of radiation. It is characterized by high dose rate and the possibility of multiple influence on a weakened and diseased organism. In connection with that, the eleven of the indices of population health was analyzed for the first time in Russia. The population was influenced by different levels of X-ray exposure 10-50 years ago. The research was carried out in the two groups of the Tumen (Siberia) regions. These regions are more or less equal in the climatic; ecologic, social-economic and demographic conditions. Nevertheless, they are different even only in the value of accumulated doses of X-ray exposure of the population (mostly in 50-70s) more than three times. Disease and mortality cancer of population of the last ten years in the regions were analyzed. The regions were selected taking into account the absence of the influence of other possible negative environmental factors. The data are found as the result of the dosimetric and epidemiological studies, and the processing of the archive statistic information. These researches demonstrated that on the whole there is the considerable statistically proved rise of disease cancer in the regions with high level of long term accumulated doses of X-ray exposure of population. Inter-district differences in disease and mortality cancer run up to three times among people aged 60 and older. There are no statistically

  4. Application of the X-ray diffractometer DRON to the study of long period structures

    International Nuclear Information System (INIS)

    It is shown that the stock-produced X-ray diffractometer DRON can be adapted for the study of long period structures up to ∼150 A. The experimental data on small-angle diffraction spectra, measured on it, from both lamellar and lateral structures of biological and lipid membranes are reported. The data show that lattice constants of these structures could be determined within the accuracy of 1 A. 15 refs.; 7 figs

  5. 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.

  6. Crystal Growth through Progressive Densification Identified by Synchrotron Small-Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Li, J.; Cookson, D.J.; Gerson, A.R. (U. South Australia); (Aust. Synch.)

    2008-08-21

    For the first time, evolution of the interfacial structure of aluminum hydroxide nuclei forming within concentrated caustic solutions has been examined in situ in real time. In both dilute and concentrated caustic aluminate solutions (NaOH = 1.0 and 3.0 M, respectively, [NaOH]/[Al] = 1.22), the measured synchrotron small-angle X-ray scattering data indicate distinctly different surface structures throughout the maturation process. In the dilute solution, the data are consistent with a thin layer of less dense, recently accreted material on the surface of large fully dense particles -- consistent with the familiar model process of species attachment to well-faceted surfaces. In contrast to this, the data for the concentrated solution are consistent with large diffuse particles growing with a mass fractal dimension of approximately 2.5 which densify to form rough surface fractal particles on maturation. This unusual densification crystallization mechanism may occur in analogous concentrated systems where the fractal structures may be entropically stablized.

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

    Science.gov (United States)

    Howell, Steven C.

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

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

    International Nuclear Information System (INIS)

    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.)

  9. Crystal Growth through Progressive Densification Identified by Synchrotron Small-Angle X-ray Scattering

    International Nuclear Information System (INIS)

    For the first time, evolution of the interfacial structure of aluminum hydroxide nuclei forming within concentrated caustic solutions has been examined in situ in real time. In both dilute and concentrated caustic aluminate solutions (NaOH = 1.0 and 3.0 M, respectively, (NaOH)/(Al) = 1.22), the measured synchrotron small-angle X-ray scattering data indicate distinctly different surface structures throughout the maturation process. In the dilute solution, the data are consistent with a thin layer of less dense, recently accreted material on the surface of large fully dense particles -- consistent with the familiar model process of species attachment to well-faceted surfaces. In contrast to this, the data for the concentrated solution are consistent with large diffuse particles growing with a mass fractal dimension of approximately 2.5 which densify to form rough surface fractal particles on maturation. This unusual densification crystallization mechanism may occur in analogous concentrated systems where the fractal structures may be entropically stablized.

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

    International Nuclear Information System (INIS)

    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.

  11. Counterion Distribution Around Protein-SNAs probed by Small-angle X-ray scattering

    Science.gov (United States)

    Krishnamoorthy, Kurinji; Bedzyk, Michael; Kewalramani, Sumit; Moreau, Liane; Mirkin, Chad

    Protein-DNA conjugates couple the advanced cell transfection capabilities of spherical DNA architecture and the biocompatible enzymatic activity of a protein core to potentially create therapeutic agents with dual functionality. An understanding of their stabilizing ionic environment is crucial to better understand and predict their properties. Here, we use Small-angle X-ray scattering techniques to decipher the structure of the counterion cloud surrounding these DNA coated nanoparticles. Through the use of anomalous scattering techniques we have mapped the local concentrations of Rb+ ions in the region around the Protein-DNA constructs. These results are further corroborated with simulations using a geometric model for the excess charge density as function of radial distance from the protein core. Further, we investigate the influence of solution ionic strength on the structure of the DNA corona and demonstrate a reduction in the extension of the DNA corona with increasing concentration of NaCl in solution for the case of both single and double stranded DNA shells. Our work reveals the distribution of counterions in the vicinity of Protein-DNA conjugates and decouples the effect of solution ionic strength on the thickness of the DNA layer.

  12. Small-angle x-ray scattering studies of calmodulin mutants with deletions in the linker region of the central helix indicate that the linker region retains a predominantly. alpha. -helical conformation

    Energy Technology Data Exchange (ETDEWEB)

    Kataoka, Mikio; Engelman, D.M. (Yale Univ., New Haven, CT (USA)); Head, J.F. (Boston Univ., MA (USA)); Persechini, A.; Kretsinger, R.H. (Univ. of Virginia, Charlottesville (USA))

    1991-02-05

    Two mutant forms of calmodulin were examined by small-angle X-ray scattering in solution and compared with the wild-type protein. Each mutant has deletions in the linker region of the central helix: one lacks residues Glu-83 and Glu-84 (Des2) and the other lacks residues Ser-81 through Glu-84 (Des4). The deletions change both the radii of gyration and the maximum dimensions of the molecules. In the presence of Ca{sup 2+}, the observed radii of gyration are 22.4 {angstrom} for wild-type bacterially expressed calmodulin, 19.5 {angstrom} for Des2 calmodulin, and 20.3 {angstrom} for Des4 calmodulin. A reduction in the radius of gyration by 1-2 {angstrom} on removal of calcium, previously observed in the native protein, was also found in the wild type and the Des4 mutant; however, no significant size change was observed in the Des2 mutant. The large calcium-dependent conformational change in calmodulin induced by the binding of melittin was observed in all the bacterially expressed proteins. Each protein appears to undergo a transition from a dumbbell shape to a more globular conformation on binding melittin in the presence of calcium, although quantitatively the changes in the wild-type and Des4 proteins greatly exceed those in Des2. Modeling shows that the structural properties of the deletion mutants are well described by modifications of an {alpha} helix in the central linker region of the molecule. Thus, the structure of the linker region is stable enough to maintain the average orientation and separation of the lobes yet flexible enough to permit the lobes to approach each other upon binding a peptide.

  13. Small-angle x-ray scattering studies of calmodulin mutants with deletions in the linker region of the central helix indicate that the linker region retains a predominantly α-helical conformation

    International Nuclear Information System (INIS)

    Two mutant forms of calmodulin were examined by small-angle X-ray scattering in solution and compared with the wild-type protein. Each mutant has deletions in the linker region of the central helix: one lacks residues Glu-83 and Glu-84 (Des2) and the other lacks residues Ser-81 through Glu-84 (Des4). The deletions change both the radii of gyration and the maximum dimensions of the molecules. In the presence of Ca2+, the observed radii of gyration are 22.4 angstrom for wild-type bacterially expressed calmodulin, 19.5 angstrom for Des2 calmodulin, and 20.3 angstrom for Des4 calmodulin. A reduction in the radius of gyration by 1-2 angstrom on removal of calcium, previously observed in the native protein, was also found in the wild type and the Des4 mutant; however, no significant size change was observed in the Des2 mutant. The large calcium-dependent conformational change in calmodulin induced by the binding of melittin was observed in all the bacterially expressed proteins. Each protein appears to undergo a transition from a dumbbell shape to a more globular conformation on binding melittin in the presence of calcium, although quantitatively the changes in the wild-type and Des4 proteins greatly exceed those in Des2. Modeling shows that the structural properties of the deletion mutants are well described by modifications of an α helix in the central linker region of the molecule. Thus, the structure of the linker region is stable enough to maintain the average orientation and separation of the lobes yet flexible enough to permit the lobes to approach each other upon binding a peptide

  14. Soft X-ray angle-resolved photoemission spectroscopy of heavily boron-doped superconducting diamond films

    Directory of Open Access Journals (Sweden)

    T. Yokoya, T. Nakamura, T. Matushita, T. Muro, H. Okazaki, M. Arita, K. Shimada, H. Namatame, M. Taniguchi, Y. Takano, M. Nagao, T. Takenouchi, H. Kawarada and T. Oguchi

    2006-01-01

    Full Text Available We have performed soft X-ray angle-resolved photoemission spectroscopy (SXARPES of microwave plasma-assisted chemical vapor deposition diamond films with different B concentrations in order to study the origin of the metallic behavior of superconducting diamond. SXARPES results clearly show valence band dispersions with a bandwidth of ~23 eV and with a top of the valence band at gamma point in the Brillouin zone, which are consistent with the calculated valence band dispersions of pure diamond. Boron concentration-dependent band dispersions near the Fermi level (EF exhibit a systematic shift of EF, indicating depopulation of electrons due to hole doping. These SXARPES results indicate that diamond bands retain for heavy boron doping and holes in the diamond band are responsible for the metallic states leading to superconductivity at low temperature. A high-resolution photoemission spectroscopy spectrum near EF of a heavily boron-doped diamond superconductor is also presented.

  15. Characterization of thin-film multilayers using magnetization curves and modeling of low-angle X-ray diffraction data

    Energy Technology Data Exchange (ETDEWEB)

    Lane, M. [Emory & Henry College, VA (United States); Chaiken, A.; Michel, R.P. [Lawrence Livermore National Lab., CA (United States)

    1994-12-01

    We have characterized thin-film multilayers grown by ion-beam sputtering using magnetization curves and modeling of low-angle x-ray diffraction data. In our films, we use ferromagnetic layer = Co, Fe, and NiFe and spacer layer = Si, Ge, FeSi{sub 2}, and CoSi{sub 2}. We have studied the effects of (1) deposition conditions; (2) thickness of layers; (3) different layer materials; and (4) annealing. We find higher magnetization in films grown at 1000V rather than 500V and in films with spacer layers of 50{angstrom} rather than 100{angstrom}. We find higher coercivity in films with cobalt grown on germanium rather than silicon, metal grown on gold underlayers rather than on glass substrates, and when using thinner spacer layers. Finally, modeling reveals that films grown with disilicide layers are more thermally stable than films grown with silicon spacer layers.

  16. A Grazing-Incidence Small-Angle X-Ray Scattering View of Vertically Aligned ZnO Nanowires

    Directory of Open Access Journals (Sweden)

    M. Lučić Lavčević

    2013-01-01

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

  17. Grazing-incidence small-angle X-ray scattering from alkaline phosphatase immobilized in atmospheric plasmapolymer coatings

    Science.gov (United States)

    Ortore, M. G.; Sinibaldi, R.; Heyse, P.; Paulussen, S.; Bernstorff, S.; Sels, B.; Mariani, P.; Rustichelli, F.; Spinozzi, F.

    2008-06-01

    Grazing-incidence small-angle X-ray scattering (GISAXS) has been used to study proteins embedded in thin polymer films obtained by a new cold, atmospheric-pressure plasma technique. In order to test the efficiency of the technology, four samples of alkaline phosphatase incorporated in organic polymer coatings in different plasma conditions have been investigated. Data have been analysed in the framework of the distorted-wave Born approximation (DWBA), by using a new method for the simultaneous fitting of the two-dimensional diffuse scattering from each sample. As a result, protein film concentration and aggregation state as well as a set of parameters describing the polymer coatings have been obtained.

  18. Simultaneous measurement of X-ray small angle scattering, absorption and reactivity: A continuous flow catalysis reactor

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Sungsik; Lee, Byeongdu; Seifert, Soenke [X-ray Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Vajda, Stefan [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Center for Nanoscale Materials, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Department of Chemical Engineering, Yale University, 9 Hillhouse Avenue, New Haven, CT 06520 (United States); Winans, Randall E., E-mail: rewinans@anl.gov [X-ray Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States)

    2011-09-01

    A fixed-bed, continuous flow catalysis reactor is described, in which GISAXS (grazing incidence small angle X-ray scattering)/GIXAS (grazing incidence X-ray absorption spectroscopy) and TPR (temperature-programmed reaction) can be measured simultaneously on samples with low metal coverage. The capabilities offered by this setup are illustrated in the example of the dehydrogenation of cyclohexene, where the size, oxidation state and reactivity of supported cobalt clusters were investigated under ambient pressure conditions. The GIXAS data reveal an evolution of the oxidation state of the catalytic particles with temperature. Simultaneously recorded GISAXS data show stable clusters, without any indication of sintering under employed reaction conditions.

  19. Critical-angle x-ray transmission grating spectrometer with extended bandpass and resolving power > 10,000

    OpenAIRE

    Heilmann, Ralf K.; Bruccoleri, Alexander R.; Kolodziejczak, Jeffery; Gaskin, Jessica A.; O'Dell, Stephen L.; Bhatia, Ritwik; Schattenburg, Mark L.

    2016-01-01

    Several high priority subjects in astrophysics can be addressed by a state-of-the-art soft x-ray grating spectrometer (XGS). An Explorer-scale, large-area (> 1,000 cm2), high resolving power (R > 3,000) XGS is highly feasible based on Critical-Angle Transmission (CAT) gratings, even for telescopes with angular resolution of 5-10 arcsec. Significantly higher performance can be provided by a CAT XGS on an X-ray-Surveyor-type mission. CAT gratings combine the advantages of blazed reflection grat...

  20. Flash X Ray: A Diagnostic Tool for Shaped Charge Studies

    Directory of Open Access Journals (Sweden)

    S. G. Tatake

    1992-10-01

    Full Text Available At present many antitank weapon systems are employing shaped charge warheads. It is, therefore, extremely important for a designer to avail of the methods capable of predicting performance of shaped charges, mainly to achieve maximum penetration. For this purpose, it is necessary to study the behaviour of the shaped charge during actual firing tests. These tests are difficult because of high speed of events that take place, production of intense light, smoke, debris, etc, and the large scale destruction caused. To overcome these difficulties, flash x-ray system during the jet studies on 30, 60 and 90 mm shaped charges and the evaluation of jet characteristics parameters.

  1. Studies of some alloys using x-ray fluorescence

    International Nuclear Information System (INIS)

    In this project an attempt has been made for the study of alloys commonly used using x-ray fluorescence ( XRF ) technique. The alloys selected for the study included gold jewellery, steels, brasses and coins. The XRF method proved to be simple, fast, non-destructive and reliable as compared to chemical methods. The results showed that most of the gold jewellery used in this country have carat value of 18 and 21. Also most coins used in different countries are alloys of Cu and Ni. A simple spark method was used for the determination of C in steels, since C is not possible to analyze by XRF. ( Author )

  2. X-ray-induced beam damage observed during x-ray photoelectron spectroscopy (XPS) studies of palladium electrode ink materials

    International Nuclear Information System (INIS)

    The surface compositional characteristics of two palladium metal electrode inks, air-dried on barium titanate (BaTiO3) dielectric ceramic substrates, have been studied using x-ray photoelectron spectroscopy (XPS). It is found that exposure of the inks to the x-ray beam during the time of analysis required for data acquisition causes surface damage. Changes in the C 1s and O 1s regions in particular, which reflect modifications to the organic, polymeric binder materials present in the inks, have been integrated as a function of x-ray exposure time, incident photon energy and beam power levels. Additional complexity in the C 1s spectral envelope that cannot be explained in terms of the expected contributing organic functionalities is observed. This is explained in terms of a difference in charging effects experienced by adventitious carbon species and those intimately associated with palladium metal centres. The degree of damage induced by the x-ray beam under specific operating conditions has been compared also with that caused by exposure of the surfaces to an electron beam. Indications of the time scales and operating parameters for conducting XPS experiments on the unmodified surface, prior to surface degradation, are given. (author)

  3. High-resolution soft X-ray beamline ADRESS at the Swiss Light Source for resonant inelastic X-ray scattering and angle-resolved photoelectron spectroscopies.

    Science.gov (United States)

    Strocov, V N; Schmitt, T; Flechsig, U; Schmidt, T; Imhof, A; Chen, Q; Raabe, J; Betemps, R; Zimoch, D; Krempasky, J; Wang, X; Grioni, M; Piazzalunga, A; Patthey, L

    2010-09-01

    The concepts and technical realisation of the high-resolution soft X-ray beamline ADRESS operating in the energy range from 300 to 1600 eV and intended for resonant inelastic X-ray scattering (RIXS) and angle-resolved photoelectron spectroscopy (ARPES) are described. The photon source is an undulator of novel fixed-gap design where longitudinal movement of permanent magnetic arrays controls not only the light polarization (including circular and 0-180 degrees rotatable linear polarizations) but also the energy without changing the gap. The beamline optics is based on the well established scheme of plane-grating monochromator operating in collimated light. The ultimate resolving power E/DeltaE is above 33000 at 1 keV photon energy. The choice of blazed versus lamellar gratings and optimization of their profile parameters is described. Owing to glancing angles on the mirrors as well as optimized groove densities and profiles of the gratings, the beamline is capable of delivering high photon flux up to 1 x 10(13) photons s(-1) (0.01% BW)(-1) at 1 keV. Ellipsoidal refocusing optics used for the RIXS endstation demagnifies the vertical spot size down to 4 microm, which allows slitless operation and thus maximal transmission of the high-resolution RIXS spectrometer delivering E/DeltaE > 11000 at 1 keV photon energy. Apart from the beamline optics, an overview of the control system is given, the diagnostics and software tools are described, and strategies used for the optical alignment are discussed. An introduction to the concepts and instrumental realisation of the ARPES and RIXS endstations is given. PMID:20724785

  4. The microfocus small-angle X-ray scattering at SSRF BL16B1

    CERN Document Server

    Hua, Wenqiang; Zhou, Ping; Li, Xiuhong; Bian, Fenggang; Wang, Jie

    2016-01-01

    Offering high-brilliance X-ray beams on micrometer length scales, the microfocus SAXS at SSRF BL16B1 was established with a KB mirror system for studying small sample volumes, or probing micro-scopic morphologies. The SAXS minimum q value was 0.1nm^-1 with a flux of 1.5 x 10^10photons/s. Two position-resolved scanning experimental methods was combined with microfocus SAXS that include STXM and CT. The experimental results of a standard sample was presented to illustrate the performance of the microfocus SAXS method. Because of the significant smearing effect in the horizontal direction, an effective and easy-to-use desmearing procedure for two-dimensional SAXS pattern based on the blind deconvolution was developed and the deblurring results demonstrated the good restoration effect for the defocus image.

  5. Size Determination of a Liposomal Drug by Small-Angle X-ray Scattering Using Continuous Contrast Variation.

    Science.gov (United States)

    Garcia-Diez, Raul; Gollwitzer, Christian; Krumrey, Michael; Varga, Zoltan

    2016-01-26

    The continuously growing complexity of nanodrugs urges for complementary characterization techniques which can elude the current limitations. In this paper, the applicability of continuous contrast variation in small-angle X-ray scattering (SAXS) for the accurate size determination of a complex nanocarrier is demonstrated on the example of PEGylated liposomal doxorubicin (Caelyx). The mean size and average electron density of Caelyx was determined by SAXS using a gradient of aqueous iodixanol (Optiprep), an iso-osmolar suspending medium. The study is focused on the isoscattering point position and the analysis of the Guinier region of the scattering curves recorded at different solvent densities. An average diameter of (69 ± 5) nm and electron density of (346.2 ± 1.2) nm(-3) were determined for the liposomal formulation of doxorubicin. The response of the liposomal nanocarrier to increasing solvent osmolality and the structure of the liposome-encapsulated doxorubicin after the osmotic shrinkage of the liposome are evaluated with sucrose contrast variation in SAXS and wide-angle X-ray scattering (WAXS). In the case of using sucrose as contrast agent, a clear osmolality threshold at 670 mOsm kg(-1) was observed, above which the liposomal drug carriers start to shrink, though preserving the intraliposomal doxorubicin structure. The average size obtained by this technique is smaller than the value measured by dynamic light scattering (DLS), though this difference is expected due to the hydrodynamic size of the PEG moieties attached to the liposomal surface, which are not probed with solvent contrast variation in SAXS. The advantages and drawbacks of the proposed technique are discussed in comparison to DLS, the most frequently used sizing method in nanomedicine. PMID:26673729

  6. X-ray crystal spectroscopy of JET - a design study

    International Nuclear Information System (INIS)

    This study describes the design and specification of a diagnostic system to measure the space- and time-resolved x-ray spectrum from JET discharges with high-resolution crystal spectrometers operating in the wavelength region 1 - 15A. The specification is given in terms of sensitivity, resolving power, detector, and data handling requirements, special attention being given to the problems encountered in interfacing the spectrometer arrays to the torus vacuum system and in their disposition to the machine. Shielding requirements during the active mode are evaluated and a staged diagnostic is proposed to accommodate D - T operation. (U.K.)

  7. Recent highlights in the X-ray study of blazars

    CERN Document Server

    Pian, E

    2002-01-01

    Blazars exhibit flux and spectral variations of largest amplitude at the highest frequencies. Therefore, monitoring their variability at X- and gamma-rays is the most effective tool to peer into the mighty powerhouse of these sources. High energy observations of the brightest blazars with the latest generation of satellites have allowed a detailed study of their behavior and have critically improved our understanding of the physics of blazar jets. I will review some of the recent results of blazar multiwavelength monitoring with emphasis on the X-ray campaigns accomplished with BeppoSAX and I will describe some of the future programs for blazar investigation from space, particularly with INTEGRAL.

  8. X-ray absorption study of cerium in the passive film on aluminum

    International Nuclear Information System (INIS)

    The corrosion-resistance of aluminum-based alloys and metal-matrix composites can be increased by treatment with cerium compounds. Immersion in a 1000 ppm solution of Ce Cl3 for periods of several days has been shown to increase the pitting potential and reduce the corrosion rate. Such treatment is being considered as an alternative to the use of chromate conversion coatings. The protective action of cerium is considered to be due to the formation of a film containing cerium oxide/hydroxide with cerium in the oxidation states 3 and 4. This occurs by precipitation of cerium compounds onto cathodic sites due to the increase of pH associated with oxygen reduction. Cerium compounds are considerably less soluble than aluminum compounds at high pH. It is proposed that the cerium oxide/hydroxide creates a barrier to the reduction of oxygen stifling cathodic reaction with a corresponding reduction in corrosion rate and open circuit potential. Glancing angle x-ray techniques are well-suited to studying the composition and structure of surface layers on materials. X-rays incident at very small angles (of the order of milliradians) below the critical angle do not penetrate beyond the surface layers of the material. With the extremely high brightness beams of x-rays provided by synchrotron sources the authors detect and characterize the chemical state of elements present in low concentrations in the surface of materials

  9. Study of caprine bones after moist and dry heat processes by X-ray diffraction

    International Nuclear Information System (INIS)

    Bone tissue is a biological material composed of hydroxyapatite (HAp) and collagen matrix. The bone X-ray diffraction (XRD) pattern presents characteristics of the hydroxyapatite crystallography planes. This paper presents the characterization by X-ray diffraction of caprine bone powder pattern and the comparison of this pattern with moist or dry heat cooked bone patterns. The parameters chosen to characterize the X-ray diffraction peaks were: angular position (2θ), full width at half maximumt (FWHM), and relative intensity (Irel). The X-ray diffraction patterns were obtained with a Shimadzu XRD-6000 diffractometer. The caprine bone XRD pattern revealed a significant correlation of several crystallographic parameters (lattice data) with hydroxyapatite. The profiles of the three bone types analyzed presented differences. The study showed as small angular displacement (decrease of the 2θ angle) of some peaks was observed after moist and dry heat cooking processes. The characterization of bone tissue aimed to contribute to future analysis in the field of archeology. (author)

  10. Study of caprine bones after moist and dry heat processes by X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Barbosa, Caroline M., E-mail: carolmattosb@yahoo.com.br [Instituto de Arqueologia Brasileira (IAB), Belford Roxo, RJ (Brazil); Azeredo, Soraia R.; Lopes, Ricardo T., E-mail: soraia@lin.ufrj.br [Coordenacao dos Programas de Pos-Graduacao em Engenharia (COPPE/LIN/UFRJ), Rio de Janeiro, RJ (Brazil). Laboratorio de Instrumentacao Nuclear; Souza, Sheila M.F.M de, E-mail: sferraz@ensp.fiocruz.br [Fundacao Oswaldo Cruz (ENSP/FIOCRUZ), Rio de Janeiro, RJ (Brazil). Escola Nacional de Saude Publica Sergio Arouca

    2013-07-01

    Bone tissue is a biological material composed of hydroxyapatite (HAp) and collagen matrix. The bone X-ray diffraction (XRD) pattern presents characteristics of the hydroxyapatite crystallography planes. This paper presents the characterization by X-ray diffraction of caprine bone powder pattern and the comparison of this pattern with moist or dry heat cooked bone patterns. The parameters chosen to characterize the X-ray diffraction peaks were: angular position (2θ), full width at half maximumt (FWHM), and relative intensity (I{sub rel}). The X-ray diffraction patterns were obtained with a Shimadzu XRD-6000 diffractometer. The caprine bone XRD pattern revealed a significant correlation of several crystallographic parameters (lattice data) with hydroxyapatite. The profiles of the three bone types analyzed presented differences. The study showed as small angular displacement (decrease of the 2θ angle) of some peaks was observed after moist and dry heat cooking processes. The characterization of bone tissue aimed to contribute to future analysis in the field of archeology. (author)

  11. An X-ray and optical study of the ultracompact X-ray binary A 1246-58

    NARCIS (Netherlands)

    in 't Zand, J. J. M.; Bassa, C. G.; Keek, L.; Verbunt, F.; Mendez, M.; Markwardt, C. B.; Jonker, P.G.

    2008-01-01

    Results are discussed of an X-ray and optical observation campaign of the low-mass X-ray binary A 1246-58 performed with instruments on Satellite per Astronomia X ("BeppoSAX"), the Rossi X-ray Timing Explorer (RXTE), the X-ray Multi-mirror Mission ("XMM-Newton"), the Swift mission, and the Very Larg

  12. An X-ray and optical study of the ultracompact X-ray binary A1246-58

    NARCIS (Netherlands)

    Zand, J. J. M. in 't

    2008-01-01

    Results are discussed of an X-ray and optical observation campaign of the low-mass X-ray binary A 1246-58 performed with instruments on Satellite per Astronomia X (’BeppoSAX’), the Rossi X-ray Timing Explorer (RXTE), the X-ray Multi-mirror Mission (’XMM-Newton’), the Swift mission, and the Very Larg

  13. Structural studies using X-ray absorption and scattering techniques

    International Nuclear Information System (INIS)

    The thesis presents extended X-ray absorption fine structure, EXAFS, and large angle X-ray scattering, LAXS, techniques; instrumentation, data collection and reduction, and applications. These techniques have been used to determine the structures of magnesium halides and organomagnesium halides in diethyl ether and tetrahydrofuran solution. The iodides were used for the LAXS measurements and Br K edge EXAFS data were collected for the corresponding bromides. Two different complexes are present in the diethyl ether solution of magnesium iodide; a polymeric chain-type structure where magnesium is tetrahedrally coordinated, as well as dimeric complex with octahedrally coordinated magnesium. Solvated MgI+ is the dominating species in tetrahydrofuran solution. The organomagnesium halides are present in diethyl ether solution as both solvated monomeric and dimeric complexes. Magnesium coordinates a halide ion, an alkyl or aryl group and four solvent molecules octahedrally in the monomeric complex. In the dimeric complex magnesium is octahedrally coordinated by two bridging halide ions, an alkyl or aryl group and three solvent molecules. The distribution of monomeric and dimeric complexes in various solutions are given by a dimerisation constant, Kdl. The results indicate that the Schlenk equilibrium is present in these solutions, however, in an extended form. In diethyl ether solution, where MgX2 does not dissociate, no MgX2 complex and thereby no Schlenk equilibrium has been observed. In tetrahydrofuran solution MgI2 has dissociated into mainly MgI+ and I-. This indicates that the concentration of MgI2 is low and that the Schlenk equilibrium should be expanded even further to include the dissociation equilibrium of the magnesium halide. In the thesis Fe K edge EXAFS data collected for the semireduced form of protein A of methane monooxygenase from Methylococcus capsulatus, are also presented. (139 refs.)

  14. Shielding of the child's head during x-ray studies

    International Nuclear Information System (INIS)

    Three devices for X-ray shielding of child's head are suggested; the first one is a protective attachment for shielding a child being in horizontal position on an X-ray table; the second one is a protective stand for shielding head and body at roentgenofraphy of upper extremities of a child sitting near the X-ray table; the third one is a prot ctive suspension for shielding the head of a child being in vertical position

  15. X-ray and synchrotron studies of porous silicon

    International Nuclear Information System (INIS)

    The results of comprehensive studies of layers of porous silicon of different conductivity types, grown by anodizing standard Si(111) substrates in an electrolyte based on fluoric acid and ethanol with the addition of 5% of iodine and kept in air for a long time, are discussed. Measurements are performed by scanning electron microscopy, high-resolution X-ray diffraction, and ultrasoft X-ray spectroscopy using synchrotron radiation. The structural parameters of the layers (thickness, strain, and porosity) and atomic and chemical composition of the porous-silicon surface are determined. It is found that an oxide layer 1.5–2.3-nm thick is formed on the surface of the silicon skeleton. The near-edge fine structure of the Si 2p absorption spectrum of this layer corresponds to the fine structure of the 2p spectrum of well coordinated SiO2. In this case, the fine structure in the Si 2p-edge absorption region of the silicon skeleton is identical to that of the 2p absorption spectrum of crystalline silicon

  16. Comparative assessment study of aboveground soft x-ray technology

    International Nuclear Information System (INIS)

    The soft x-ray regime accessible at the laboratory nominally extends from photon energies of 10 eV to 10 keV. The technology relies on capacitor-based, short-pulse energy storage devices to generate a high-energy-density plasma 1 cc in volume and lasting about 10 ns. The hot plasma is created either by conversion of short-pulse electrical energy into light ions that heat the plasma or into a magnetically-driven imploding plasma. Applications of these intense soft x-rays include evaluation of their interaction with materials, as an energy source for weapons effects, as a source for ICF experiments, and as a source for weapons physics experiments. Because of management's interest in encouraging the development of new applications to this technology, they did a year-long comparative assessment study that involved surveying scientists engaged in such research. The literature is filled with examples of benchmarking in the manufacturing and service industries; however, the authors found only one documented case where scientific research had been benchmarked. The experience in benchmarking an area of scientific research and some of the findings are described in this paper

  17. Comparative study of radiation dose between digital panoramic X-ray unit and general panoramic X-ray unit

    International Nuclear Information System (INIS)

    Objective: To compare the actual dose of patients who receive the same medical practice by either digital panoramic X-ray unit and general panoramic X-ray unit and give evidence for better selection of oral X-ray examination method. Methods: Round sheet lithium fluoride (LiF) thermoluminescent dosimeters (TLD) were used. The experiment was divided into natural background contrast group, general panoramic X-ray children group, general panoramic X-ray adults group, digital panoramic X-ray children group and digital panoramic X-ray adults group. The dosimeter of natural background radiation was placed at the office of the doctor, the dosimeters of general panoramic X-ray children group and general panoramic X-ray adults group were irradiated by different conditions according to the clinical application of panoramic X-ray to children and adults, the dosimeters of digital panoramic X-ray children group and digital panoramic X-ray adults group were irradiated by different conditions according to the clinical application of digital panoramic X-ray to children and adults. The thermoluminescent dosimeter was used to count and calculate the exposure doses in various groups. Results: The dose of children exposed in general panoramic X-ray unit was 1.28 times of that in digital panoramic X-ray unit, there was significant difference (t=6.904, P<0.01). The dose of adults exposed in general panoramic X-ray unit was 1.55 times of that in the digital panoramic X-ray unit, there also was significant difference (t=-11.514. P< 0.01). Conclusion: The digital panoramic X-ray unit can reduce the dose of patients, so the digital panoramic X-ray unit should be used as far as possible. (authors)

  18. A high-field pulsed magnet system for x-ray scattering studies in Voigt geometry

    CERN Document Server

    Islam, Zahirul; Ruff, Jacob P C; Das, Ritesh K; Trakhtenberg, Emil; Nojiri, Hiroyuki; Narumi, Yasuo; Canfield, Paul C

    2011-01-01

    We present a new pulsed-magnet system that enables x-ray single-crystal diffraction in addition to powder and spectroscopic studies in Voigt geometry. The apparatus consists of a large-bore solenoid, cooled by liquid nitrogen. A second independent closed-cycle cryostat is used for cooling samples near liquid helium temperatures. Pulsed magnetic fields up to ~30 T with a minimum of ~6 ms in total duration are generated by discharging a 40 kJ capacitor bank into the magnet coil. The unique characteristic of this instrument is the preservation of maximum scattering angle (~23.6 deg.) through the magnet bore by virtue of a novel double-funnel insert. This instrument would facilitate x-ray diffraction and spectroscopic studies that are impractical, if not impossible, to perform using conventional split-pair magnets and offers a practical solution for preserving optical access in future higher-field pulsed magnets.

  19. Glancing angle Talbot-Lau grating interferometers for phase contrast imaging at high x-ray energy

    Science.gov (United States)

    Stutman, D.; Finkenthal, M.

    2012-08-01

    A Talbot-Lau interferometer is demonstrated using micro-periodic gratings inclined at a glancing angle along the light propagation direction. Due to the increase in the effective thickness of the absorption gratings, the device enables differential phase contrast imaging at high x-ray energy, with improved fringe visibility (contrast). For instance, at 28° glancing angle, we obtain up to ˜35% overall interferometer contrast with a spectrum having ˜43 keV mean energy, suitable for medical applications. In addition, glancing angle interferometers could provide high contrast at energies above 100 keV, enabling industrial and security applications of phase contrast imaging.

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

    Directory of Open Access Journals (Sweden)

    Jörn Ostermann

    2012-12-01

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

  1. X-ray studies of nanoporous carbon powders produced from silicon carbide

    International Nuclear Information System (INIS)

    X-ray diffraction, small-angle X-ray scattering, and X-ray photoelectron spectroscopy were used to study the structure of nanoporous carbon powders produced directly by chlorination of polycrystalline α-SiC powders with various degrees of dispersion. Small-angle scattering data were used to derive the distribution function for scattering inhomogeneities with respect to inertia radii m(Rg). It is shown that the mean sizes and the fraction of large inhomogeneities increase with increasing size of grains in the starting powder. As follows from the diffraction patterns, the degree of 'graphitization' of nanocluster structure increases simultaneously, which is attributed to longer times required for carbonization of coarser grains. An analysis of photoelectron spectra for 1s electrons of carbon atoms shows that, for most of the C-C bonds (>65%), the hybridization of valence bonds is intermediate between those for graphite and diamond (spx, where 2 < x < 3), which is indicative of the bending of graphene-like layers in nanoclusters

  2. Synchrotron X-Ray Radiation and Deformation Studies

    DEFF Research Database (Denmark)

    Fæster Nielsen, Søren

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

  3. Basic study on electric optical devices for x-rays using piezoelectric single crystals

    International Nuclear Information System (INIS)

    Basic study about electric optical devices for x-rays was performed using the change of Bragg diffraction angles caused by the change of lattice spacing d of a piezoelectric single crystal on applying electric field. In this experiment, an α-quartz was chosen because of its abundant already-known physical properties in spite of low piezoelectricity. Both macroscopic deformation and the change of thickness of an α-quartz were measured when an electric field was applied. On the experiment, x-ray diffraction showed peak shift to the amount of 1.8 minutes, of which the value was one order of magnitude larger than that expected from the calculation of lattice spacing. This fact suggested that not only the change of lattice spacing, but also macroscopic deformation could contribute to the peak shift. Therefore, macroscopic deformation should be taken account of the development of electric optical devices. (Y. Kazumata)

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

    DEFF Research Database (Denmark)

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

    2013-01-01

    extract the structural information of the solute, the solvent response has to be treated. Methodologies capable of doing so include both theoretical modelling and experimental determination of the solvent response. In the work presented here, we have investigated how to obtain a reproducible solvent......In time-resolved laser pump, X-ray probe wide-angle X-ray scattering experiments on systems in solution the structural response of the system is accompanied by a solvent response. The solvent response is caused by reorganization of the bulk solvent following the laser pump event, and in order to...... response-the solvent term-experimentally when applying laser pump, X-ray probe time-resolved wide-angle X-ray scattering. The solvent term describes difference scattering arising from the structural response of the solvent to changes in the hydrodynamic parameters: pressure, temperature and density. We...

  5. Temporal Studies of Supergiant Fast X-ray Transients

    CERN Document Server

    Drave, S P; Clark, D J; McBride, V A; Hill, A B; Sguera, V; Scaringi, S; Bazzano, A; Townsend, L J

    2011-01-01

    SFXTs are a new class of HMXB unveiled by INTEGRAL. They are extreme systems characterised by very short outbursts (a few hours) and extreme X-ray luminosity dynamic ranges (~10^{4}). Ten confirmed systems are currently known and have shown parallels with both Sg-XRBs and Be-XRBs. Temporal studies across all timescales are key to understanding both the place of SFXTs within the HMXB hierarchy and the accretion mechanisms at work within the objects. Here we present the discovery of a new 51.47 \\pm 0.02 day orbital period in the SFXT XTE J1739$-$302 using INTEGRAL observations. We also present a higher time resolution study of the SFXTs SAX J1818.6-1703, IGR J16479-4514 and IGR J16465-4507 using RXTE that shows newly discovered flaring activity.

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

    CERN Document Server

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

    2002-01-01

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

  7. Quantitative Analysis of the Orientation of Mineral in Bone from Small-Angle X-Ray Scattering Patterns

    Science.gov (United States)

    Matsushima, Norio; Akiyama, Morio; Terayama, Yoshio

    1982-01-01

    The small-angle X-ray scattering data from a rabbit femur is quantitatively evaluated with respect to the mineral distribution in bone. The results show the existence of a needle-like mineral with a length of at least 300 A and a preferred orientation of the needle axes parallel to the long axis of the bone. The angular distribution of the needle axes gives a value of 30° for the mean inclination.

  8. Membrane surface modification and characterization by X-ray photoelectron spectroscopy, atomic force microscopy and contact angle measurements

    International Nuclear Information System (INIS)

    Surface modifying macromolecules (SMMs) were used to modify the top surface of polymeric membranes. SMMs are oligomeric fluoropolymers synthesized by polyurethane chemistry and tailored with fluorinated end groups. In this study, the surface of polyetherimide (PEI) flat-sheet membranes prepared by the phase inversion method was modified using 2 wt.% of SMM and 15 wt.% PEI concentration in the polymer casting solution. The effect of solvent evaporation time on membrane surface modification was investigated. X-ray photoelectron spectroscopy analysis shows enrichment of fluorine on the modified PEI membrane surfaces and their contact angles were higher than those of the unmodified PEI membrane. Both the surface fluorine content and contact angles of the SMM/PEI blended membrane increased when the solvent evaporation time was increased up to 5 min. The SMM modified and unmodified PEI membranes were characterized by means of tapping mode atomic force microscopy (TM-AFM). The mean pore size, nodule size, pore density, surface porosity and mean roughness of the modified membranes were determined and compared with those of the unmodified membrane

  9. Biological dosimetry of X-rays by micronuclei study

    International Nuclear Information System (INIS)

    Biological dosimetry consists of estimating absorbed doses for people exposed to radiation by mean biological methods. Several indicators used are based in hematological, biochemical an cytogenetics data, although nowadays without doubt, the cytogenetic method is considered to be the most reliable, in this case, the study of micronuclei in peripheral blood lymphocytes cytokinetic blocked can be related to absorbed dose through an experimental calibration curve. An experimental dose-response curve, using micronuclei assay for X-rays at 250 kVp, 43,79 rads/min and temperature 37 degree celsius has been produced. Experimental data is fitted to model Y=c+ α D+β D2 where. Y is the number micronuclei per cell and D the dose. the curve is compared with those produced elsewhere

  10. X-ray photoemission spectroscopy study of hexavalent uranium compounds

    International Nuclear Information System (INIS)

    The electronic structure of the outer occupied levels of a series of hexavalent uranium (predominately uranyl) compounds was studied using x-ray photoemission spectroscopy (XPS). The changes in the spectral features of the outer occupied levels with the variation of the uranium-oxygen bond lengths (1.7--2.1 A) are systematically investigated. Previously unexplained spectral structure has been found to result from ligand-field splitting of the occupied U 6p3/2 levels. The XPS results are compared with predictions of a relativistic molecular-cluster calculation and with the results of a simple point-charge crystal-field model. When the crystalline electric fields generated by both the primary and secondary ligands are taken into consideration, excellent quantitative agreement is obtained between the XPS data and the molecular-cluster results with no parameter adjustment

  11. X-ray photoemission study of MgB2

    International Nuclear Information System (INIS)

    A c-axis oriented thin film and a high-density sintered pellet of MgB2 have been studied by x-ray photoemission spectroscopy, and compared to measurements from MgO and MgF2 single crystals. The as-grown surface has a layer which is Mg-rich and oxidized, which is effectively removed by a nonaqueous etchant. The subsurface region of the pellet is Mg deficient. This nonideal near-surface region may explain varied scanning tunneling spectroscopy results. The MgB2 core level and Auger signals are similar to measurements from metallic Mg and transition-metal diborides, and the measured valence band is consistent with the calculated density of states

  12. X-ray microtomography study of a sandstone reservoir rock

    International Nuclear Information System (INIS)

    This paper presents the pore space characterization of a sandstone reservoir rock carried out with a microfocus X-ray computed tomography (μ-CT). The resulting spatial resolution of the image was 3.8 μm, which allowed a very good visualization and enabled a geometric quantification of grains and pores. A total of 956 μ-CT slices were taken to render a 3-D volume of the specimen. These CT slices were processed in order to characterize the geometrical microstructure of the sample: total porosity and pore size distribution. The possibility of having high-resolution 3-D μ-CT images reveals a promising scenario for studies and applications in porous media characterization. It is possible to simulate fluid invasion in these μ-CT structures and estimate their petrophysical properties

  13. Biological Dosimetry of X-rays by micronuclei study

    International Nuclear Information System (INIS)

    Biological dosimetry consists of estimating absorbed doses for people exposed to radiation by mean biological methods. Several indicators used are based in haematological, biochemical an cytogenetics data, although nowadays without doubt, the cytogenetic method is considered to be the most reliable, in this case, the study of micronuclei in peripheral blood lymphocytes citokinetics blocked can be related to absorbed dose through an experimental calibration curve. An experimental dose-response curve, using micronuclei assay for X-rays at 250 kVp, 43,79 rads/min and temperature 37 degree centigree has been produced. Experimental data is fitted to model Y=C+ αD+BD''2 where Y is the number of micronuclei per cell and D the dose. The curve is compared with those produced elsewhere. (Author) 24 refs

  14. Magnetoelastic effect in holmium studied by X-ray diffraction

    International Nuclear Information System (INIS)

    X-ray diffraction measurements have been performed on a single crystal sample of the rare earth metal holmium. The temperature and magnetic field dependence of the c-lattice parameter was studied in detail below the Neel temperature of 132K. Magnetic structural phase transitions were observed as a change in the c-lattice parameter. In addition, lattice modulations induced by the magnetic structure were investigated by observing satellite reflections. A model based on the exchange magnetostriction can explain these magnetostrictive behaviors. The magnetic structures which were used in the analysis were reproduced by the self-consistent mean field calculation. The model has explained the temperature and magnetic field dependence of the c-lattice parameter, as well as the behaviors of the wave number and the amplitude of the lattice modulation. (author)

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

    DEFF Research Database (Denmark)

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

    2014-01-01

    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...

  16. Study of osteoporosis using dual energy X-ray absorptiometry

    International Nuclear Information System (INIS)

    Dual energy X-ray absorptiometry (Hologic QDR-1000) was used to quantitatively analyze the diagnosis and prevention of osteoporosis. The peak bone mineral density (BMD) of the spine appeared in normal men in their twenties and in normal women in their thirties. There was acceleration of bone loss in the 50 to 60 year age bracket (premenopause and postmenopause) in normal women. On the contrary, the peak BMD of the femoral neck in normal men and women appeared in their twenties after which it decreased slightly with age. Comparison showed that the femoral neck BMD of normal women was lower than that of men throughout all ages. The fracture threshold, 0.756 g/cm2 for the spine, was obtained by scanning 73 females with spinal fractures, the mean BMDs for L2-L4 at the 90th percentile level were used as the fracture threshold. The fracture threshold of femoral neck fracture was the femoral proximal BMD of the 9th decile. Classification by the Public Welfare Silver Science Group's method and by the Singh index, except Grades I, II, and III, revealed a difference; as the severity of bone atrophy advanced, BMD tended to decrease. The percent reduction of MBD 10 years after premenopause was 21.0% in the spine and 13.2% in the femoral neck. Correlation between BMD and weight, weight/height ratio, BODY MASS INDEX was significant. No correlation between BMD and bone metabolism factors in the blood was found in 50 osteoporotic patients. The results of this study showed that dual energy X-ray absorptiometry (Hologic QDR-1000) can objectively diagnose and suggest measures for prevention of osteoporosis, and is clinically useful. (author)

  17. X-ray diffraction studies on single and mixed confectionery fats using synchrotron radiation

    International Nuclear Information System (INIS)

    Full text: Understanding and refining the molecular-scale processes involved in the manufacture of structured materials such as long-chain hydrocarbon compounds is important in many commercial areas such as the petrochemical, biochemical, food, pharmaceutical and soap industries. In such processes crystallisation is an important separation, purification and preparation technique. Despite this our knowledge of the crystallisation process itself is surprisingly limited. In order to improve the crystallisation of confectionery fats, the crystallisation of it's main component, cocoa butter fat, must be properly understood. Cocoa butter fat can exhibit up to 6 polymorphic forms of different crystallographic structures with melting points varying from 17.3 deg C to 36.3 deg C. During the production of chocolate it is essential to control the polymorphic form of fats present, in order to produce a final product with the correct physical and rheological properties. Both shear rate and temperature are thought to play a crucial role in this process. The most widely used method for studying polymorphism is X-ray diffraction. Typical X-ray diffraction patterns of fats exhibit two groups of diffraction lines corresponding to the long and short spacings. The long spacings correspond to the planes formed by the methyl end groups and are dependent on the chain length and the angle of tilt of the component fatty acids of the glyceride molecules. The short spacings refer to the cross sectional packing of the hydrocarbon chain and are independent of the chain length. The relationship between crystallisation rate, polymorphic form, shear and the fat composition has for the first time been quantified, which will enable more accurate control of the polymorhic form in chocolate production. This has been achieved by developing an improved in-situ cell for X-ray studies. The X-ray studies are necessary for the examination of on-line studies under well controlled conditions of temperature

  18. High resolution X-ray diffraction studies on unirradiated and irradiated strontium hexaferrite crystals

    Indian Academy of Sciences (India)

    Balwinder Kaur; Monita Bhat; F Licci; Ravi Kumar; K K Bamzai; P N Kotru

    2012-04-01

    High-resolution X-ray diffraction technique, employing a three-crystal monochromator–collimator combination is used to study the irradiation induced defects in flux grown Sr-hexaferrite crystals irradiated with 50 MeV Li3+ ion beams at room temperature with a fluence value of 1 × 1014 ions/cm2. The diffraction curves of the irradiated crystals suggest the possibility of creation of low angle grain boundaries and other point/clusters of defects causing amorphization in the irradiated crystals. The perfection of the irradiated and unirradiated (0001) cleaved surfaces of the crystals is studied using the bulk method of X-ray topography. The topographs supplement the findings suggestive of modifications in the crystalline quality of SrFe12O19 on irradiation with SHI of Li3+. Etching of the (0001) cleaved surfaces in H3PO4 at 120°C suggests that the dissolution characteristics of the surfaces get affected on irradiation with SHI of Li3+, besides supporting the findings of HRXRD and X-ray topography regarding modifications in the perfection of SrFe12O19 on irradiation.

  19. Determination of biological specimen optimal thickness for small-angle X-ray experiments by use polychromatic synchrotron radiation

    International Nuclear Information System (INIS)

    It is put forward the mode of evaluation of biological specimen optimal thickness for small-angle specimen thickness on various synchrotron radiation spectra are calculated. The curves allow to optimize an experiment by selecting either optimal specimen thickness for an available synchrotron radiation spectrum, or the disposition of the short-wave boundary for given specimen thickness (fibers, tissues and so on). The method gives the possibility apart from increasing both of the precision and reproducibility of X-ray experiments, either or both increase of the statistical precision upon given recording time of an X-ray pattern and decrease recording time upon retention of the same statistical precision. The 15-20 % deviation in the specimen thickness from that of optimal one is shown to lead to decrease in the scattering intensity less than 2 %. 15 refs.; 3 figs

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

    Directory of Open Access Journals (Sweden)

    Lauren Boldon

    2015-02-01

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

  1. Resonant X-ray scattering studies of concentrated aqueous solutions

    International Nuclear Information System (INIS)

    The microscopic structure of concentrated aqueous electrolyte solutions has been studied by resonant X-ray diffraction (RXD). This technique provides a method for the measurement of the structure around a specific atom or ion in solution. In that sense, RXD is the X-ray equivalent of neutron diffraction with isotopic substitution (NDIS). The use of RXD as an alternative to NDIS has been considered of interest for some time; it is potentially one of the best methods for overcoming the most important limitation of the neutron diffraction technique, i.e. the lack of suitable isotopes for every atomic species. Third generation synchrotron sources offer an unprecedented opportunity for the further development of RXD to study the microscopic structure of liquids and amorphous materials. One of the main aims of this thesis was to check whether it could be possible to obtain results of comparable accuracy to those of NDIS. In this work, the hydration structures of Br-, Rb+, Sr2+ and Y3+ in concentrated aqueous solutions have been studied by RXD. A detailed account of how the experiments were carried out and the data analysis procedure is given. The results are compared with those obtained for the same ion by other techniques and to those obtained for similar systems by NDIS. The reliability of these results and the observed trends in the measured structure when compared to other ions in the same series are discussed. A comparative study of the structure of the three cations is also presented in this thesis. This work illustrates one of the main advantages of RXD: the possibility of carrying out systematic structural studies on all elements with atomic number greater than 28 (Ni). Finally, a critical discussion on the actual stage of development of RXD is presented. The results shown offer evidence of the future prospects of the technique and justify further efforts to develop it to the level of reliability and ease of use that NDIS has reached after more than three decades

  2. X-ray exposure in utero and school performance: a population-based study of X-ray pelvimetry

    International Nuclear Information System (INIS)

    Aim: To investigate the association between exposure to ionising radiation from pelvimetric examinations in utero and school performance. Material and methods: This was a population-based cohort study comprising 46,066 children born in the county of Östergötland, Sweden, from 1980 through 1990. Through record linkage between Swedish registers, children exposed in utero to X-ray pelvimetry examination were compared to other children born in the same county during the study period, as well as to their unexposed siblings. Outcome variable was primary school grades, expressed in centiles and calculated through linear regression. Results: In the univariate analysis, children exposed to X-ray pelvimetry in utero had higher school grades compared to unexposed children (point estimate 3 centiles, 95% confidence interval [CI]: 1.5 to 4.6). When sex, mother's education and income, birth order, and birth position were included in the analysis; however, the difference was reduced and the association was no longer statistically significant (PE 1.4, 95% CI: –0.1 to 2.8). Comparing exposed children with their siblings showed no statistical difference in univariate analysis or in multivariate analysis. Conclusion: No suggestion was found of a negative effect on school performance from in utero exposure of diagnostic X-ray pelvimetry. -- Highlights: •Pelvimetric examinations expose fetus to low levels of radiation. •No detectable effect on childrens final primary school grades from pelvimetric examinations. •Pelvimetric examinations is a safe procedure for the fetus regarding shool performance

  3. Small-Angle X-ray Scattering Demonstrates Similar Nanostructure in Cortical Bone from Young Adult Animals of Different Species.

    Science.gov (United States)

    Kaspersen, Jørn Døvling; Turunen, Mikael Juhani; Mathavan, Neashan; Lages, Sebastian; Pedersen, Jan Skov; Olsson, Ulf; Isaksson, Hanna

    2016-07-01

    Despite the vast amount of studies focusing on bone nanostructure that have been performed for several decades, doubts regarding the detailed structure of the constituting hydroxyapatite crystal still exist. Different experimental techniques report somewhat different sizes and locations, possibly due to different requirements for the sample preparation. In this study, small- and wide-angle X-ray scattering is used to investigate the nanostructure of femur samples from young adult ovine, bovine, porcine, and murine cortical bone, including three different orthogonal directions relative to the long axis of the bone. The radially averaged scattering from all samples reveals a remarkable similarity in the entire q range, which indicates that the nanostructure is essentially the same in all species. Small differences in the data from different directions confirm that the crystals are elongated in the [001] direction and that this direction is parallel to the long axis of the bone. A model consisting of thin plates is successfully employed to describe the scattering and extract the plate thicknesses, which are found to be in the range of 20-40 Å for most samples but 40-60 Å for the cow samples. It is demonstrated that the mineral plates have a large degree of polydispersity in plate thickness. Additionally, and equally importantly, the scattering data and the model are critically evaluated in terms of model uncertainties and overall information content. PMID:26914607

  4. 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).

  5. X-ray and SEM studies on zirconia powders

    Directory of Open Access Journals (Sweden)

    L. Pająk

    2008-12-01

    Full Text Available Purpose: The microstructure characterization of commercially available zirconia powders was the purpose of this paper. Different methods of structure analysis were applied owing to the complex, multiphase structure of studied materials.Design/methodology/approach: The X-ray diffraction (XRD and scanning electron microscopy (SEM investigations were performed on three commercial zirconia ceramic materials: Amdry 204 NS (ZrO2  8 wt.% of Y2O3, Metco C8  YZ (ZrO2  8 wt.% of Y2O3 and Metco 202 (ZrO2  20 wt.% of Y2O3. The Rietveld method appeared to be very useful in the verification of the qualitative phase composition and in the determination of phase abundance. Hill and Howard procedure was applied for quantitative phase analysis. The parameters of the individual diffraction line profiles were determined by PRO-FIT Toraya procedure. The powder morphology was analyzed by SEM method.Findings: In the Amdry sample comparable contents of two phases: monoclinic (44.1 wt.% and cubic (55.9 wt.% was stated by XRD analysis. The presence of Y2O3 phase besides of monoclinic, tetragonal and cubic ZrO2 ones were stated for both Metco samples. The tetragonal phase (55.2 wt.% was found to be the main component of the Metco C8-YZ sample whereas the content of Y2O3 is the lowest (2.7 wt.%. On the other hand cubic phase (68.2 wt.% was the main component of the Metco 202 sample and the content of Y2O3 is again the lowest (4.5 wt.%. The SEM images of all the samples reveal the spherical shape of powder particles. The morphology of both Metco samples is quite similar. For Metco 202 sample the hierarchical type structure of powder particle is observed; the greater particles contain smaller ones. The shell of particles is composed of distinct patches. On the other hand the structure of spherical particles of Amdry sample is of branched, rather dense skeleton type. From X-ray diffraction data it can be concluded that the crystallite size of all involved phases

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

    International Nuclear Information System (INIS)

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

  7. Small angle X-ray scattering coupled with in situ electromechanical probing of nanoparticle-based resistive strain gauges.

    Science.gov (United States)

    Decorde, Nicolas; Sangeetha, Neralagatta M; Viallet, Benoit; Viau, Guillaume; Grisolia, Jérémie; Coati, Alessandro; Vlad, Alina; Garreau, Yves; Ressier, Laurence

    2014-12-21

    A comprehensive study on the electromechanical behavior of nanoparticle-based resistive strain gauges in action through normal and grazing incidence small angle X-ray scattering (SAXS/GISAXS) investigations is presented. The strain gauges were fabricated from arrays of colloidal gold nanoparticle (NP) wires assembled on flexible polyethylene terephthalate and polyimide substrates by convective self-assembly. Microstructural changes (mean interparticle distance variations) within these NP wires under uniaxial stretching estimated by SAXS/GISAXS are correlated to their macroscopic electrical resistance variations. SAXS measurements suggest a linear longitudinal extension and transversal contraction of the NP wires with applied strain (0 to ∼ 13%). The slope of this longitudinal variation is less than unity, implying a partial strain transfer from the substrate to the NP wires. The simultaneously measured electrical resistance of the strain gauges shows an exponential variation within the elastic domain of the substrate deformation, consistent with electron tunnelling through the interparticle gaps. A slower variation observed within the plastic domain suggests the formation of new electronic conduction pathways. Implications of transversal contraction of the NP wires on the directional sensitivities of strain gauges are evaluated by simulating electronic conduction in models mimicking a realistic NP arrangement. A loss of directionality of the NP-based strain gauges due to transversal current flow within the NP wires is deduced. PMID:25371292

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

    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)

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

    Energy Technology Data Exchange (ETDEWEB)

    Wells, Hannah C.; Sizeland, Katie H.; Kayed, Hanan R.; Haverkamp, Richard G., E-mail: r.haverkamp@massey.ac.nz [School of Engineering and Advanced Technology, Massey University, Private Bag 11222, Palmerston North 4442 (New Zealand); Kirby, Nigel; Hawley, Adrian; Mudie, Stephen T. [Australian Synchrotron, 800 Blackburn Road, Clayton, Victoria 3168 (Australia)

    2015-01-28

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

  11. The distribution of Sr2+ counterions around polyacrylate chains analyzed by anomalous small-angle X-ray scattering

    Science.gov (United States)

    Goerigk, G.; Schweins, R.; Huber, K.; Ballauff, M.

    2004-05-01

    The distribution of Sr counterions around negatively charged sodium polyacrylate chains (NaPA) in aqueous solution was studied by anomalous small-angle X-ray scattering. Different ratios of the concentrations of SrCl2/[NaPA] reveal dramatic changes in the scattering curves. At the lower ratio the scattering curves indicate a coil-like behavior, while at the higher ratio the scattering curves are contracted to smaller q-values, caused by the collapse of the NaPA coil. The form factor of the scattering contribution of the counterions was separated and analyzed. For the scattering curves of the collapsed chains, this analysis agrees with the model of a pearl necklace, consisting of collapsed sphere-like subdomains which are connected by stretched chain segments. An averaged radius of the pearls of 19 nm and a distance between neighbouring pearls close to 60 nm could be established for the collapsed state of the NaPA chains.

  12. Anomalous small-angle X-ray scattering of nanoporous two-phase atomistic models for amorphous silicon–germanium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Chehaidar, A., E-mail: Abdallah.Chehaidar@fss.rnu.tn

    2015-09-15

    The present work deals with a detailed analysis of the anomalous small-angle X-ray scattering in amorphous silicon–germanium alloy using the simulation technique. We envisage the nanoporous two-phase alloy model consisting in a mixture of Ge-rich and Ge-poor domains and voids at the nanoscale. By substituting Ge atoms for Si atoms in nanoporous amorphous silicon network, compositionally heterogeneous alloys are generated with various composition-contrasts between the two phases. After relaxing the as-generated structure, we compute its radial distribution function, and then we deduce by the Fourier transform technique its anomalous X-ray scattering pattern. Using a smoothing procedure, the computed X-ray scattering patterns are corrected for the termination errors due to the finite size of the model, allowing so a rigorous quantitative analysis of the anomalous small-angle scattering. Our simulation shows that, as expected, the anomalous small-angle X-ray scattering technique is a tool of choice for characterizing compositional heterogeneities coexisting with structural inhomogeneities in an amorphous alloy. Furthermore, the sizes of the compositional nanoheterogeneities, as measured by anomalous small-angle X-ray scattering technique, are X-ray energy independent. A quantitative analysis of the separated reduced anomalous small-angle X-ray scattering, as defined in this work, provided a good estimate of their size.

  13. An optical & X-ray study of the counterpart to the SMC X-ray binary pulsar system SXP327

    CERN Document Server

    Coe, M J; Corbet, R H D; Galache, J; McBride, V A; Townsend, L J; Udalski, A

    2008-01-01

    Optical and X-ray observations are presented here of a newly reported X-ray transient system in the Small Magellanic Cloud. The data reveal many previously unknown X-ray detections of this system and clear evidence for a 49.995d binary period. In addition, the optical photometry show recurring outburst features at the binary period which may well be indicative of the neutron star interacting with a circumstellar disk around a Be star.

  14. Study of the cosmic sources of hard x-rays

    International Nuclear Information System (INIS)

    An actively-shielded, high energy x-ray telescope was launched on-board OSO-8 on June 21, 1975. The primary objectives of this experiment are the measurements of the energy spectrum of discrete cosmic x-ray sources in the range 20 keV to 3 MeV and of the temporal variations in the intensity of each source detected with a time resolution of 0.3 msec. This detector provides the highest duty factor and the finest time resolution of any of its kind for observations over a period of up to 10 days. The background spectrum of this detector in orbit has been monitored continuously since shortly after launch. The minimum detectable source strength is estimated to be between 10-4 and 10-5 photons/cm2-sec keV, limited primarily by the effects of induced radioactivity. From July 16 through July 18, 1975 the x-ray binary, Cen X-3, was observed with the hard x-ray telescope. For this source, complete data coverage is needed before statistically significant results can be reported on the high energy x-ray spectrum and the energy dependence of the pulsed fraction. With the partial data coverage presently available, statistically significant results were obtained from observations of Cen A (July 27 through August 4, 1975) and Sco X-1 (September 6 through 9, 1975). Some of the hard x-ray sources which will be the observational objectives of this experiment during the period from October 1975 through June 1976 are Cyg X-1, Cyg X-2, Per X-1, Tau X-1, Vel X-1, Com X-1, Vir X-1, and 3C273

  15. Preliminary Studies on X-Ray-sensitive Liposome

    Institute of Scientific and Technical Information of China (English)

    MENG Fan-xu; XU Hua-ping; QI Yan-fei; XU Kun; SONG Xiu-ling; NIU Shu; LI Juan

    2012-01-01

    The synthesis of a new type of X-ray-sensitive compound “di-(1-hydroxylundecyl)diselenide” and its application in the preparation of a new type of liposome with X-ray sensitivity was reported.This new liposome was synthesized to encapsulate doxorubicin hydrochloride(Dox),with its physical and chemical properties,stability,and radiation sensitivity determined.Based on the pH-gradient method,liposomal Dox was prepared via ultrasonic emulsification and then purified on a Sephadex G50 mini-column.UV spectrophotometry and liquid chromatography were used to detect the encapsulation efficiency and radiation sensitivity of the Dox-loaded liposome.The results show that through changes in release rate,this liposome shows a relative radiosensitivity.In terms of radiation sensitivity,the drug leak rate of the X-ray-sensitive Dox-loaded liposome increased gradually and peaked at 65.4% under the X-ray radiation of a dose of 10 Gy or more than 10 Gy,which is significantly different from that of ordinary liposomes.Meanwhile,X-ray-sensitive Dox-loaded liposome has a good dispersion stability,with an average particle size of approximate 120 nm.The efficiency of this liposome encapsulating Dox was 75.84%,slightly lower than that of ordinary liposomes.The X-ray-sensitive Dox-loaded liposome exhibited suspension stability within 30 d of storage at 4 ℃,without visible precipitation.Di-(1-hydroxylundecyl)diselenide is safe and noncytotoxic and compared with those of synthetic phospholipids its synthesis is low cost and does not require complex conditions.

  16. X-ray diffraction study of synthetic tetraborates and hexaborates

    International Nuclear Information System (INIS)

    The results of the X-ray diffraction of the tetraborates (NH3CH2CH2NH3)(B4O5(OH)4), (NH4)(Co(NH3)5H2O)(B4O5(OH)4)2x5H2O and of the hexaborates Ni(H2O)4(B6O)(OH)6xH2O (triclinic and monoclinic modification). (NH4)2{Co(H2O)2(B6O7(OH)6)2}x2H2O, (Ni(H2O)6){Ni(B6O7(OH)3(OCH3)3)2}, Co(H2O)3(B6O7(OH)6)x1.5C2H5OH and Ni(H2O)3(B6O7(OH)6)xC2H5OH have been reviewed. The crystal solvates isostructural to the latter compound - nickel hexaborates containing propyl and allyl alcohols, acetone and methyl ethyl ketone have been studied

  17. Electron Paramagnetic Resonance studies of x-ray irradiated Nafion

    Science.gov (United States)

    Fragoso, Juan; Usher, Timothy

    2007-03-01

    Fuel cells promise a bright future as power sources for a variety of electronic equipment as well as more power demanding elements. Nafion (DuPont's trademark of a sulfonated tetrafluorethylene polymer modified from Teflon) is the heart of Proton Exchange Membrane Fuel Cells (PEMFCs) as well as Direct Methanol Fuel Cells (DMFCs). Fuel cells are used to power electronic equipment on spacecraft, satellites and unpiloted high altitude aircraft, where ionizing radiation can be a concern. Electron Paramagnetic Resonance (EPR) is a spectroscopic technique that is very sensitive to free radicals such as those produced by ionizing radiation therefore EPR can give us a window into the degradation of the Nafion membranes due to the ionizing radiation. Nafion samples were irradiated using a x-ray diffractometer with a copper target operating at 40kV and 55mA for at least 3hrs. X-Band EPR spectroscopy of the irradiated nafion reveals a peak at 3400G with a width of 10G, which decays over time, completely diminishing in a couple of weeks. Preliminary results from the polarization studies on the effects of ionizing radiation will also be presented.

  18. X-ray diffraction study of glucomannans and their acetates

    International Nuclear Information System (INIS)

    Crystalline polymorphs of four glucomannans with a different mannose/glucose ratio from 1.5 to 4.0 and their acetyl derivatives was studied by X-ray diffraction measurements. The glucomannans showed an amorphous or similar crystal structure (Mannan I or Mannan II polymorph) of β-1,4-d-mannan depending on their mannose content, indicating the occurrence of isomorphous replacement of mannose by glucose during glucomannan crystallization. When these glucomannans were annealed, however, Konjac glucomannan (mannose/glucose ratio = 1.6) showed a different powder pattern from both Mannans I and II. The fiber pattern of the annealed Konjac glucomannan indicated that it took an extended two-fold helical structure. Among the acetylated glucomannans, Higanbana glucomannan with a high mannose content (mannose/glucose = 4.0) showed a similar diffraction pattern to that of β-1,4-d-mannan triacetate, indicating that the isomorphous replacement also occurred in the acetyl derivative. However, glucomannan triacetate with a low mannose content (1.5 or 1.6) showed a different crystalline form from that of mannan triacetate. The fiber diffraction pattern of Konjac glucomannan acetate suggested that it took a three-fold helix

  19. Cytogenetic studies with laser or X-ray exposures

    International Nuclear Information System (INIS)

    Account is given of studies involving a total of 21 peripheral blood cultures given the following treatments: exposure to 20 0.13-joule pulses from an optic quantum generator (ruby), 9; exposure to 1000 R X-rays, 9; and unexposed controls, 3. Exposures were carried out on three cultures from each experimental series at each of three time intervals, namely 24 h, 48 h, and 72 h after initiation of cultures. On any day, 40 well-spread metaphases were examined. High quality metaphases were photographed and karyotyped in conformity to the Chicago Conference criteria. In the laser experiment, chromosome aberrations were observed in 65% of methaphases analyzed vs. 5.3% in controls. Anomalies encountered included aneuploidy, with hypoploid metaphases predominating, polyploidy (triploidy, tetraploidy, and partial endoreduplication), and structural alterations. The following structural chromosome rearrangements are found: acentric fragments, mostly pairs, occasionally single, including minute chromosomes; dicentric and tricentric chromosomes; interstitial deletions; and chromosome translocations. Most varied and abundant chromosome aberrations were seen in 72-h irradiated cultures. The data presented offer a new opportunity for assessing genetic lesions after laser exposure and may help to determine threshold doses. (author)

  20. A method for sizing sub-micron particles using small angle diffraction of soft x-rays

    International Nuclear Information System (INIS)

    The purpose of this work is to develop a method of sizing sub-micron particles using small-angle soft x-ray diffraction. Solid poly-styrene spheres of known sizes were used as scattering samples, with C-Kα (44.8/angstrom/) and V-Lα (24.3/angstrom/) radiation from a conventional x-ray source. Two devices were used to diffract the x-rays. One collimates the radiation using a series of pinholes immediately preceding the sample, and directs the unfocussed radiation onto film placed far from the sample. The other utilizes radiation from a single pinhole above the source onto the sample and a spherical multilayer mirror in series, so that the radiation passes twice through the sample and is focused onto film immediately above the pinhole assembly to increase the effective sample area. Using the latter device, two types of diffraction patterns were obtained: a sharp, relatively small pattern from spheres which form a hexagonal lattice structure, and a diffuse, larger pattern from an unordered, or random, array of spheres. Both patterns are presented in this work, along with the calculations, based upon light scattering from an unordered and an ordered array of particles, of the scattering patterns. 9 refs., 32 figs., 2 tabs

  1. Critical-angle x-ray transmission grating spectrometer with extended bandpass and resolving power > 10,000

    CERN Document Server

    Heilmann, Ralf K; Kolodziejczak, Jeffery; Gaskin, Jessica A; O'Dell, Stephen L; Bhatia, Ritwik; Schattenburg, Mark L

    2016-01-01

    Several high priority subjects in astrophysics can be addressed by a state-of-the-art soft x-ray grating spectrometer (XGS). An Explorer-scale, large-area (> 1,000 cm2), high resolving power (R > 3,000) XGS is highly feasible based on Critical-Angle Transmission (CAT) gratings, even for telescopes with angular resolution of 5-10 arcsec. Significantly higher performance can be provided by a CAT XGS on an X-ray-Surveyor-type mission. CAT gratings combine the advantages of blazed reflection gratings (high efficiency, use of higher diffraction orders) with those of transmission gratings (low mass, relaxed alignment and temperature requirements, transparent at high energies) with minimal mission resource demands. They are high-efficiency blazed transmission gratings that consist of freestanding, ultra-high aspect-ratio grating bars made from SOI wafers using anisotropic dry and wet etch techniques. Blazing is achieved through reflection off grating bar sidewalls. Silicon is well matched to the soft x-ray band, and...

  2. Observational studies of X-ray binary systems

    International Nuclear Information System (INIS)

    The subject of Chapter 1 is theoretical. The other chapters, Ch. 2 to 6, contain original observational data and efforts towards their interpretation. Of these, Ch. 3, 4 and 5 deal with massive X-ray binaries, Ch. 6 with low-mass systems and Ch. 2 with Cygnus X-3, which we have not yet been able to assign to any of these two classes. The X-ray observations described were made with the COS-B satellite. Work based on UV and optical observations is described in Ch. 5. The UV observations were made with the IUE satellite, the optical observations at several ground-based observatories. (Auth.)

  3. Application of X-ray CT to the study of microstructure and diffusivity in cementitious materials

    OpenAIRE

    Darma, Ivan Sandi

    2014-01-01

    At the beginning of its development, the X-ray CT technique originally was developed for medical analysis. However, along with the advances in technology, the ability of X-ray CT continues to increase. Therefore, the use of X-ray CT is no longer intended for medical application but has expanded to other fields such as civil engineering especially for material science. Related to construction materials, there are many experimental methods that can be used to study the microstructure of cementi...

  4. Experimental study on hard x-rays emitted from metre-scale negative discharges in air

    International Nuclear Information System (INIS)

    We investigate the development of metre long negative discharges and focus on their x-ray emissions. We describe appearance, timing and spatial distribution of the x-rays. They appear in bursts of nanosecond duration mostly in the cathode area. The spectrum can be characterized by an exponential function with 200 keV characteristic photon energy. With nanosecond-fast photography we took detailed images of the pre-breakdown phenomena during the time when x-rays were registered. We found bipolar discharge structures, also called ‘pilot systems’, in the vicinity of the cathode. As in our previous study of x-rays from positive discharges, we correlate the x-ray emission with encounters between positive and negative streamers. We suggest that a similar process is responsible for x-rays generated by lightning leaders. (paper)

  5. Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries.

    Science.gov (United States)

    Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

    2016-01-01

    We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

  6. X-ray source population study of the starburst galaxy M83 with XMM-Newton

    OpenAIRE

    Ducci, L.; Sasaki, M.; Haberl, F.; Pietsch, W.

    2013-01-01

    We present the results obtained from the analysis of three XMM-Newton observations of M83. The aims of the paper are studying the X-ray source populations in M83 and calculating the X-ray luminosity functions of X-ray binaries for different regions of the galaxy. We detected 189 sources in the XMM-Newton field of view in the energy range of 0.2-12 keV. We constrained their nature by means of spectral analysis, hardness ratios, studies of the X-ray variability, and cross-correlations with cata...

  7. X-ray Imaging and preliminary studies of the X-ray self-emission from an innovative plasma-trap based on the Bernstein waves heating mechanism

    Science.gov (United States)

    Caliri, C.; Romano, F. P.; Mascali, D.; Gammino, S.; Musumarra, A.; Castro, G.; Celona, L.; Neri, L.; Altana, C.

    2013-10-01

    Electron Cyclotron Resonance Ion Sources (ECRIS) are based on ECR heated plasmas emitting high fluxes of X-rays. Here we illustrate a pilot study of the X-ray emission from a compact plasma-trap in which an off-resonance microwave-plasma interaction has been attempted, highlighting a possible Bernstein-Waves based heating mechanism. EBWs-heating is obtained via the inner plasma EM-to-ES wave conversion and enables to reach densities much larger than the cut-off ones. At LNS-INFN, an innovative diagnostic technique based on the design of a Pinhole Camera (PHC) coupled to a CCD device for X-ray Imaging of the plasma (XRI) has been developed, in order to integrate X-ray traditional diagnostics (XRS). The complementary use of electrostatic probes measurements and X-ray diagnostics enabled us to gain knowledge about the high energy electrons density and temperature and about the spatial structure of the source. The combination of the experimental data with appropriate modeling of the plasma-source allowed to estimate the X-ray emission intensity in different energy domains (ranging from EUV up to Hard X-rays). The use of ECRIS as X-ray source for multidisciplinary applications, is now a concrete perspective due to the intense fluxes produced by the new plasma heating mechanism.

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

    Science.gov (United States)

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

    2010-10-01

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

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

    International Nuclear Information System (INIS)

    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.

  10. Pinhole X-ray Fluorescence Imaging of Gadolinium Nanoparticles: A Preliminary Monte Carlo Study

    Energy Technology Data Exchange (ETDEWEB)

    Jung, Seong Moon; Sung, Won Mo; Ye, Sung Joon [Seoul National University, Seoul (Korea, Republic of)

    2014-10-15

    X-ray fluorescence imaging is a modality for the element-specific imaging of a subject through analysis of characteristic x-rays produced by exploiting the interaction of high atomic number elements and incoming x-rays. Previous studies have utilized a polychromatic x-ray source to investigate the production of in vivo x-ray fluorescence images for the assessment of concentrations and locations of gold nanoparticles. However, previous efforts have so far been unable to detect low concentrations, such as 0.001% gold by weight, which is an expected concentration accumulated in tumors. We examined the feasibility of a monochromatic synchrotron x-rays implementation of pinhole x-ray fluorescence imaging by Monte Carlo simulations using MCNP5. In the current study, gadolinium (Gd) nanoparticles, which have been widely used as a contrast agent in magnetic resonance imaging and also as a dose enhancer in radiation therapy, were chosen for tumor targeting. Since a monochromatic x-ray source is used, the increased x-ray fluorescence signals allow the detection of low concentrations of Gd. Two different monochromatic x-ray beam energies, 50.5 keV near the Kedge energy (i.e., 50.207 keV) of Gd and 55 keV, were compared by their respective imaging results. Using Monte Carlo simulations the feasibility of imaging low concentrations of Gd nanoparticles (e.g., 0.001 wt%) with x-ray fluorescence using monochromatic synchrotron x-rays of two different energies was shown. In the case of imaging a single Gd column inserted in the center of a water phantom, the fluorescence signals from 0.05 wt% and 0.1 wt% Gd columns irradiated with a 50.5 keV photon beam were higher than those irradiated with 55 keV. Below 0.05 wt% region no significant differences were found.

  11. Pinhole X-ray Fluorescence Imaging of Gadolinium Nanoparticles: A Preliminary Monte Carlo Study

    International Nuclear Information System (INIS)

    X-ray fluorescence imaging is a modality for the element-specific imaging of a subject through analysis of characteristic x-rays produced by exploiting the interaction of high atomic number elements and incoming x-rays. Previous studies have utilized a polychromatic x-ray source to investigate the production of in vivo x-ray fluorescence images for the assessment of concentrations and locations of gold nanoparticles. However, previous efforts have so far been unable to detect low concentrations, such as 0.001% gold by weight, which is an expected concentration accumulated in tumors. We examined the feasibility of a monochromatic synchrotron x-rays implementation of pinhole x-ray fluorescence imaging by Monte Carlo simulations using MCNP5. In the current study, gadolinium (Gd) nanoparticles, which have been widely used as a contrast agent in magnetic resonance imaging and also as a dose enhancer in radiation therapy, were chosen for tumor targeting. Since a monochromatic x-ray source is used, the increased x-ray fluorescence signals allow the detection of low concentrations of Gd. Two different monochromatic x-ray beam energies, 50.5 keV near the Kedge energy (i.e., 50.207 keV) of Gd and 55 keV, were compared by their respective imaging results. Using Monte Carlo simulations the feasibility of imaging low concentrations of Gd nanoparticles (e.g., 0.001 wt%) with x-ray fluorescence using monochromatic synchrotron x-rays of two different energies was shown. In the case of imaging a single Gd column inserted in the center of a water phantom, the fluorescence signals from 0.05 wt% and 0.1 wt% Gd columns irradiated with a 50.5 keV photon beam were higher than those irradiated with 55 keV. Below 0.05 wt% region no significant differences were found

  12. Helical rearrangement of photoactivated rhodopsin in monomeric and dimeric forms probed by high-angle X-ray scattering

    OpenAIRE

    Imamoto, Yasushi; Kojima, Keiichi; Oka, Toshihiko; Maeda, Ryo; Shichida, Yoshinori

    2015-01-01

    Light-induced helical rearrangement of vertebrate visual rhodopsin was directly monitored by high-angle X-ray scattering (HAXS), ranging from Q (= 4π sin θ/λ) = 0.03 Å-1 to Q = 1.5 Å-1. HAXS of nanodiscs containing a single rhodopsin molecule was performed before and after photoactivation of rhodopsin. The intensity difference curve obtained by HAXS agreed with that calculated from the crystal structure of dark state rhodopsin and metarhodopsin II, indicating that the conformational change of...

  13. Synthesis of a nanorod ferrofluid and characterisation by magnetic-field-dependent small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Compared to conventional ferrofluids, which contain mostly spherical particles, a dispersion of highly anisometric particles such as rods or chains is expected to give rise to an enhancement or modification of well-known ferrofluid properties. This contribution reports on the synthesis of a ferrofluid containing stable chains of iron nanoparticles and on its microstructural characterisation by means of transmission electron microscopy and small-angle X-ray scattering (SAXS). The SAXS measurements develop a pronounced anisotropy of the scattering pattern as a function of an increasing external magnetic field. Evaluation of the radially averaged SAXS curves in terms of basic scattering functions is discussed

  14. Synthesis of a nanorod ferrofluid and characterisation by magnetic-field-dependent small-angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Doebrich, F. [Universitaet des Saarlandes, Technische Physik, Geb. D2 2, 66041 Saarbruecken (Germany)]. E-mail: f.doebrich@nano.uni-saarland.de; Michels, A. [Universitaet des Saarlandes, Technische Physik, Geb. D2 2, 66041 Saarbruecken (Germany); Birringer, R. [Universitaet des Saarlandes, Technische Physik, Geb. D2 2, 66041 Saarbruecken (Germany)

    2007-09-15

    Compared to conventional ferrofluids, which contain mostly spherical particles, a dispersion of highly anisometric particles such as rods or chains is expected to give rise to an enhancement or modification of well-known ferrofluid properties. This contribution reports on the synthesis of a ferrofluid containing stable chains of iron nanoparticles and on its microstructural characterisation by means of transmission electron microscopy and small-angle X-ray scattering (SAXS). The SAXS measurements develop a pronounced anisotropy of the scattering pattern as a function of an increasing external magnetic field. Evaluation of the radially averaged SAXS curves in terms of basic scattering functions is discussed.

  15. Small-angle X-ray scattering determination of the distribution of particle diameters in photochromic glasses

    International Nuclear Information System (INIS)

    The existing methods for determining particle size distributions from small angle X-ray scattering data are reviewed. The improved transform technique was used for calculating diameter distributions N(D) of lightsensitive silverhalide crystallites in photochromic glasses. From the evolution of N(D) during a certain heat treatment it can be concluded that two generations of crystallites of different size are precipitated. In glass I, the mean diameter D increases proportional to the time t of the treatment (reaction-limited growth) and in glass II D3 approximately t (diffusion-limited ripening) is obtained. (author)

  16. Analysis of biostructural changes, dynamics, and interactions - Small-angle X-ray scattering to the rescue.

    Science.gov (United States)

    Vestergaard, Bente

    2016-07-15

    Solution small angle X-ray scattering from biological macromolecules (BioSAXS) plays an increasingly important role in biostructural research. The analysis of complex protein mixtures, dynamic equilibriums, intrinsic disorder and evolving structural processes is facilitated by SAXS data, either in stand-alone applications, or with SAXS taking a prominent role in hybrid biostructural analysis. This is not the least due to the significant advances in both hardware and software that have taken place in particular at the large-scale facilities. Here, recent developments and the future potential of BioSAXS are reviewed, exemplified by numerous examples of elegant applications to challenging systems. PMID:26945933

  17. The geometry of radio-quiet AGN studied with X-ray polarimetry

    Science.gov (United States)

    Matt, Giorgio

    2016-07-01

    Our current X-ray view of AGN in the local Universe is based on spectroscopic, imaging and timing data. In this talk I will discuss the importance of adding the polarimetric view. The geometry of the matter around the black hole (from the X-ray emitting corona to more distant circumnuclear matter) can be probed by X-ray polarimetry. Observational perspectives in view of the X-ray polarimetric missions currently under study at NASA and ESA will be also discussed.

  18. The beginning of studies and use of X-rays in the Czech Lands

    International Nuclear Information System (INIS)

    Based on historical sources this paper to present the remarkably early response to Roentgen's discovery of X-rays in the Czech Lands, then part of the Austro-Hungarian Monarchy, and to call attention to some early radiological studies done here before the foundation of Czechoslovakia in 1918. The early X-ray experiments by physicists and engineers, the first attempts at X-ray diagnostics and therapy, and the early X-ray equipments of provincial hospitals and practitioners surgeries are reviewed. (J.K.) 6 refs

  19. X-ray diffraction study of directionally grown perylene crystallites

    DEFF Research Database (Denmark)

    Breiby, Dag W.; Lemke, H. T.; Hammershøj, P.;

    2008-01-01

    Using grazing incidence X-ray diffraction, perylene crystallites grown on thin highly oriented poly(tetrafluoroethylene) (PTFE) films on silicon substrates have been investigated. All the perylene crystallites are found to orient with the ab plane of the monoclinic unit cell parallel...

  20. Study of semiconductor detectors applied to diagnostic X-ray

    International Nuclear Information System (INIS)

    This work aims an evaluation of procedures for photons spectrum determination, produced by a X ray tube, normally used for medical diagnoses which operation voltage ranges from 20 to 150 kVp, to allow more precise characterization of the photon beam. The use of spectrum analysis will contribute to reduce the uncertainty in the ionization camera calibrations. For this purpose, two kind of detectors were selected, a Cadmium Zinc Telluride (CZT) and a planar HPGe detector. The X ray interaction with the detector's crystal produces, by electronic processes, a pulse high distribution as an output, which is no the true photon spectrum, due to the presence of K shell escape peaks, Compton scattering and to the fact that the detectors efficiency diminish rapidly with the increase of the photon energy. A detailed analysis of the contributing factors to distortions in the spectrum is necessary and was performed by Monte Carlo calculation with the MCNP 4B computer code. In order to determine the actual photon spectrum for a X ray tube a spectra stripping procedure is described for the HPGe detector. The detector's response curves, determined by the Monte Carlo calculation, were compared to the experimental ones, for isotropic point sources. For the methodology validation, stripped spectra were compared to the theoretical ones, for the same X ray tube's settings, for a qualitative evaluation. The air kerma rate calculated with the photon spectra were compared to the direct measurement using an ionization chamber, for a quantitative evaluation. (author)

  1. Oxygen precipitation studied by x-ray diffraction techniques

    Czech Academy of Sciences Publication Activity Database

    Meduňa, M.; Caha, O.; Růžička, J.; Bernatová, S.; Svoboda, Milan; Buršík, Jiří

    178 -179, - (2011), s. 325-330. ISSN 1012-0394 R&D Projects: GA ČR(CZ) GA202/09/1013 Institutional research plan: CEZ:AV0Z20410507 Keywords : Czochralski silicon * oxygen precipitates * x-ray Laue diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism

  2. X-ray fractography studies on austenitic stainless steels

    NARCIS (Netherlands)

    Rajanna, K.; Pathiraj, B.; Kolster, B.H.

    1996-01-01

    In this investigation, the fracture surfaces of SS 304 and SS 316 austenitic steels were analysed using the X-ray fractography technique. In both cases, a decrease in the austenite content was observed at the fracture surface as a result of deformation induced martensite, indicating a linear relatio

  3. X-RAY DIFFRACTION STUDY OF A PANCHAVAKTRA RAS

    Directory of Open Access Journals (Sweden)

    B. Srinivasulu*, P. Bhadra Dev, P.H.C. Murthy

    2012-06-01

    Full Text Available Analytical monitoring of Pharmaceutical products is necessary to ensure its safety and efficacy throughout all phases of the drug. A systematic approach should be adapted to the presentation and evaluation of stable information, which should include, as necessary, physical, chemical, biological and microbiological test characteristics. Indian System of Medicine (ISM frequently uses metal/mineral drugs. It is mandatory to standardize the preparatory procedures. For the Pharmaceutical standardization, three batches of the Panchavaktra ras were prepared and analytical study of final product carried out. Panchavaktra ras consist equal parts of Parada (Mercury, Gandhaka (Sulphur, Tankana (Borax Pippali (Piper longum L. and Marica (Piper nigrum L., and Mardhana (Grinding was done carefully with sufficient quantity of juice of Datura metel leaves for 24 hours and a final product was obtained in the form of Vati (tablet form. It is one of the formulations mentioned in Amavata (Rheumatoid Arthritis disease. The final products were subjected to Powder X-Ray Diffraction (XRD studies and values of XRD peaks of particular Panchavaktra ras were observed. This study revealed that high peaks of HgS (Metacinnabar, free S (Sulfur, Chabazite (Ca- exchanged, dehydrated Ca (structure- Rhombohedral in the final products. The structural and chemical characterization of the HgS (Metacinnabar found as cubic, free S (Sulphur as Orthorhombic in all the samples. The 50% strongest peaks of HgS were present at 2-Theta scale between 26-31, 43-44, 51-55, 70-72 degrees. This paper points out the importance of XRD, as a standard tool for further studies and research of Herbo-mineral formulations.

  4. A CMOS active pixel sensor system for laboratory- based x-ray diffraction studies of biological tissue.

    Science.gov (United States)

    Bohndiek, Sarah E; Cook, Emily J; Arvanitis, Costas D; Olivo, Alessandro; Royle, Gary J; Clark, Andy T; Prydderch, Mark L; Turchetta, Renato; Speller, Robert D

    2008-02-01

    X-ray diffraction studies give material-specific information about biological tissue. Ideally, a large area, low noise, wide dynamic range digital x-ray detector is required for laboratory-based x-ray diffraction studies. The goal of this work is to introduce a novel imaging technology, the CMOS active pixel sensor (APS) that has the potential to fulfil all these requirements, and demonstrate its feasibility for coherent scatter imaging. A prototype CMOS APS has been included in an x-ray diffraction demonstration system. An industrial x-ray source with appropriate beam filtration is used to perform angle dispersive x-ray diffraction (ADXRD). Optimization of the experimental set-up is detailed including collimator options and detector operating parameters. Scatter signatures are measured for 11 different materials, covering three medical applications: breast cancer diagnosis, kidney stone identification and bone mineral density calculations. Scatter signatures are also recorded for three mixed samples of known composition. Results are verified using two independent models for predicting the APS scatter signature: (1) a linear systems model of the APS and (2) a linear superposition integral combining known monochromatic scatter signatures with the input polychromatic spectrum used in this case. Cross validation of experimental, modelled and literature results proves that APS are able to record biologically relevant scatter signatures. Coherent scatter signatures are sensitive to multiple materials present in a sample and provide a means to quantify composition. In the future, production of a bespoke APS imager for x-ray diffraction studies could enable simultaneous collection of the transmitted beam and scattered radiation in a laboratory-based coherent scatter system, making clinical transfer of the technique attainable. PMID:18199908

  5. Small-angle X-ray scattering investigation of aging behavior of Al-Cu-Mg-Ag alloys using synchrotron radiation

    Institute of Scientific and Technical Information of China (English)

    2012-01-01

    The aging behavior of Al-Cu-Mg-Ag alloys with high Cu/Mg was studied by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) using synchrotron radiation. TEM study reveals that the major strengthening phases of the alloy after aging at 160?C for 10 h are Ω and less θ′. SAXS study shows that the scattering patterns are composed of several concentric circles at the beginning of aging process, which is replaced by the butterfly-wings scattering patterns with the increase of aging time...

  6. Non-destructive determination of moisture content and micro-fibril angle of wood using a poly-chromatic X-ray beam theoretical and experimental approach

    International Nuclear Information System (INIS)

    Non-destructive determination of moisture content and micro-fibril angle are important stakes for the sciences of the wood because these two parameters influence strongly the macroscopic behavior of the wood. For example, the shrinkage, the mechanical properties, the thermal and acoustic conductivity are dependent on the moisture content and their anisotropic character is largely governed by the micro-fibril angle. We used the light difference between X-ray mass attenuation coefficient for the water and for the wood in transmission. Regrettably, the results show that this difference between X-ray mass attenuation coefficient is insufficient to allow the precise measurement of the moisture content.In spite of this, the coherent scattering shows sensitive effects. So, by using a poly-energetic beam and a spectrometric system, we were able to discriminate between the crystalline constituent (cellulose) of the amorphous constituent (water) in a sample of wet wood, because for a given angle these phases scatter in different energy. Besides, the device created allowed us to study the crystalline phase of the wood. We were able to confront experimental profiles of diffraction with theoretical profiles of diffraction, obtained by means of a rigorous simulation, in the objective to estimate the average micro-fibril angle and its standard deviation. (author)

  7. Interest of the grazing X ray diffraction to study the evolution of materials under irradiation: behaviour of zirconia under irradiation

    International Nuclear Information System (INIS)

    This document was written to show that grazing X ray diffraction may be a powerful tool to study irradiation damages induced by ion beams in materials. Taking advantage of an asymmetric geometry and a curved detector, it is possible to analyse accurately diffraction diagrams at low angles by taking into account the specific effects induced by the grazing incidence. The interest of grazing incidence is to control the penetration depth of X rays. Such possibility allows to separate effects induced by damages (displacement cascades) and the implantation peak (elastic deformation of the lattice due to the insertion of projectile ions in the matrix). A Rietveld analysis on grazing X ray diagrams shows clearly that displacement cascades induce a phase transition on irradiated zirconia. (authors)

  8. Preflight performance studies of the PoGOLite hard X-ray polarimeter

    CERN Document Server

    Chauvin, M; Kawano, T; Kiss, M; Kole, M; Mikhalev, V; Moretti, E; Takahashi, H; Pearce, M

    2015-01-01

    Polarimetric studies of astrophysical sources can make important contributions to resolve the geometry of the emitting region and determine the photon emission mechanism. PoGOLite is a balloon-borne polarimeter operating in the hard X-ray band (25-240 keV), with a Pathfinder mission focussing on Crab observations. Within the polarimeter, the distribution of Compton scattering angles is used to determine the polarisation fraction and angle of incident photons. To assure an unbiased measurement of the polarisation during a balloon flight it is crucial to characterise the performance of the instrument before the launch. This paper presents the results of the PoGOLite calibration tests and simulations performed before the 2013 balloon flight. The tests performed confirm that the polarimeter does not have any intrinsic asymmetries and therefore does not induce bias into the measurements. Generally, good agreement is found between results from test data and simulations which allows the polarimeter performance to be...

  9. Accurate structure analyses of polymer crystals on the basis of wide-angle X-ray and neutron diffractions

    International Nuclear Information System (INIS)

    The crystal structure analysis of various polymer substances has been reviewed on the basis of wide-angle high-energy X-ray and neutron diffraction data. The progress in structural analytical techniques of polymer crystals have been reviewed at first. The structural models proposed so far were reinvestigated and new models have been proposed for various kinds of polymer crystals including polyethylene, poly(vinyl alcohol), poly(lactic acid) and its stereocomplex etc. The hydrogen atomic positions were also clarified by the quantitative analysis of wide-angle neutron diffraction data, from which the physical properties of polymer crystals have been evaluated theoretically. The bonded electron density distribution has been estimated for a polydiacetylene single crystal on the basis of the so-called X-N method or by the combination of structural information derived from X-ray and neutron diffraction data analysis. Some comments have been added about future developments in the field of structure-property relationship determination. (author)

  10. Formation of binary and ternary metal deposits on glass-ceramic carbon electrode surfaces: electron-probe X-ray microanalysis, total-reflection X-ray fluorescence analysis, X-ray photoelectron spectroscopy and scanning electron microscopy study

    International Nuclear Information System (INIS)

    The features of the formation of binary and ternary alloys during the electrochemical deposition and co-deposition of copper, cadmium and lead from aqueous solutions on disc glass-ceramic carbon electrode surfaces were studied by electron-probe X-ray microanalysis, total-reflection X-ray fluorescence analysis, X-ray photoelectron spectroscopy and scanning electron microscopy. The macroscopic properties of electrodeposits such as morphology, lateral distribution of the elements along the disc electrode surface and depth distribution of the elements in the electrodeposit bulk were established. The mechanisms of metal nucleation and growth of thin films of electrodeposits were discussed

  11. PLEIADES: a picosecond Compton scattering x-ray source for advanced backlighting and time-resolved material studies

    Energy Technology Data Exchange (ETDEWEB)

    Gibson, D J; Anderson, S G; Barty, C P; Betts, S M; Booth, R; Brown, W J; Crane, J K; Cross, R R; Fittinghoff, D N; Hartemann, F V; Kuba, J; Le Sage, G P; Tremaine, A M; Springer, P T; Rosenzweig, J B

    2003-10-20

    The PLEIADES (Picosecond Laser-Electron Inter-Action for the Dynamical Evaluation of Structures) facility has produced first light at 70 keV. This milestone offers a new opportunity to develop laser-driven, compact, tunable x-ray sources for critical applications such as diagnostics for the National Ignition Facility and time-resolved material studies. The electron beam was focused to 50 {micro}m rms, at 57 MeV, with 260 C of charge, a relative energy spread of 0.2%, and a normalized emittance of 5 mm mrad horizontally and 13 mm mrad vertically. The scattered 820-nm laser pulse had an energy of 180 mJ and a duration of 54 fs. Initial x-rays were captured with a cooled charge-coupled device using a Cesium Iodide scintillator; the peak photon energy was approximately 78 keV, with a total x-ray flux of 1.3 x 10{sup 6} photons/shot, and the observed angular distribution found to agree very well with three-dimensional codes. Simple K-edge radiography of a tantalum foil showed good agreement with the theoretical divergence-angle dependence of the x-ray energy. Optimization of the x-ray dose is currently underway, with the goal of reaching 10{sup 8} photons per shot and a peak brightness approaching 10{sup 20} photons/mm{sup 2}/mrad{sup 2}/s/0.1%bandwidth.

  12. (Synchrotron studies of x-ray reflectivity from surfaces)

    Energy Technology Data Exchange (ETDEWEB)

    Pershan, P.S.

    1992-03-03

    Following a long period of theoretical interest, but only limited measurements, there has recently been an increased number of attempts to expand the relative paucity of experimental information on the structure of liquid surfaces using techniques as diverse as ellipsometry, micro-force balances, non-linear optics, Auger and photoelectron spectroscopy, and x-ray scattering. Our group has played a leading role in the currently expanding application of scattering techniques to the general problem of characterizing the microscopic structure of liquid surfaces and we propose here that this work be extended specifically to liquid metals. In the following sections we will briefly describe the salient features of x-ray scattering that are relevant to the current project, the progress that we have made in the current grant period and the work that we propose to carry out in the forthcoming grant period.

  13. Preparation and X-ray Structural Study of Dibenziodolium Derivatives.

    Science.gov (United States)

    Postnikov, Pavel S; Guselnikova, Olga A; Yusubov, Mekhman S; Yoshimura, Akira; Nemykin, Victor N; Zhdankin, Viktor V

    2015-06-01

    New experimental procedures for the preparation of dibenziodolium salts by oxidative cyclization of 2-iodobiphenyl in the presence of appropriate strong acids are described. Particularly useful is a convenient one-pot synthesis of dibenziodolium hydrogen sulfate from 2-iodobiphenyl using Oxone as an inexpensive and environmentally safe oxidant. Dibenziodolium hydrogen sulfate, bis(triflyl)imidate, or triflate can be readily converted to various other dibenziodolium derivatives (chloride, bromide, thiocyanate, azide, cyanide, phenylsulfinate) by anion exchange. Structures of key products have been established by single-crystal X-ray diffraction analysis. Particularly interesting is the X-ray structure of dibenziodolium thiocyanate, which represents the first example of a structurally characterized hypervalent iodine compound with a relatively short iodine-sulfur secondary bond distance. PMID:25951091

  14. X-ray excited optical luminescence, photoluminescence, photostimulated luminescence and x-ray photoemission spectroscopy studies on BaFBr:Eu

    CERN Document Server

    Subramanian, N; Govinda-Rajan, K; Mohammad-Yousuf; Santanu-Bera; Narasimhan, S V

    1997-01-01

    The results of x-ray excited optical luminescence (XEOL), photoluminescence (PL), photostimulated luminescence (PSL) and x-ray photoemission spectroscopy (XPS) studies on the x-ray storage phosphor BaFBr:Eu are presented in this paper. Analyses of XEOL, PL and PSL spectra reveal features corresponding to the transitions from 4f sup 6 td sup 1 to 4f sup 7 configurations in different site symmetries of Eu sup 2 sup +. Increasing x-ray dose is seen to lead to a red shift in the maximum of the PL excitation spectrum for the 391 nm emission. The XEOL and XPS spectra do not show any signature of Eu sup 3 sup + in the samples studied by us, directly raising doubts about the model of Takahashi et al in which Eu sup 2 sup + is expected to ionize to Eu sup 3 sup + upon x-ray irradiation and remain stable until photostimulation. XEOL and PSL experiments with simultaneous x-ray irradiation and He - Ne laser excitation as well as those with sequential x-ray irradiation and laser stimulation bring out the competition betwe...

  15. Physiological and x-ray studies of potential antisickling agents.

    OpenAIRE

    Abraham, D. J.; Perutz, M F; Phillips, S E

    1983-01-01

    Several aromatic compounds have been found to inhibit the gelling of sickle cell hemoglobin. We have tried to correlate the antigelling activity of such compounds with the stereo-chemistry of their binding sites in the hemoglobin molecule. This approach led to the discovery that two known antilipoproteinemia drugs, clofibrate and gemfibrozil, have antigelling activity. X-ray analysis showed that three pairs of molecules of clofibric acid, the active metabolite of clofibrate, bound to the wall...

  16. X-Ray and Neutron Scattering Study of the Magnetic Structure of Neodymium Metal

    DEFF Research Database (Denmark)

    Lebech, Bente; Als-Nielsen, Jens Aage; McEwen, K. A.

    1979-01-01

    A combined x-ray and neutron diffraction study has shown that the so-called "triple-q⃗" structure is not the correct model of the magnetic structure of neodymium. The x-ray data showed only the Bragg reflections originating from the double-hcp lattice. Hence, all additional reflections observed b...

  17. Synthesis of Novel Amphiphilic Azobenzenes and X-ray Scattering Studies of Their Langmuir Monolayers

    DEFF Research Database (Denmark)

    Sørensen, Thomas Just; Kjær, Kristian; Breiby, Dag Werner;

    2008-01-01

    air-water interface, the amphiphilic azobenzenes form noncrystalline but stable Langmuir films that display an unusual reversible monolayer collapse close to 35 mN/m. The structures and phase transitions were studied by X-ray reflectivity (XR) and grazing-incidence X-ray diffraction, both utilizing...

  18. High energy x-ray reflectivity and scattering study from spectrum-x-gamma flight mirrors

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Budtz-Jørgensen, Carl; Frederiksen, P. Kk;

    1993-01-01

    Line radiation from Fe K-alpha(1), Cu K-alpha(1), and Ag K-alpha(1) is used to study the high energy X-ray reflectivity and scattering behavior of flight-quality X-ray mirrors having various Al substrates. When both the specular and the scattered radiation are integrated, near theoretical...

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

    NARCIS (Netherlands)

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

    2016-01-01

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

  20. X-ray fluorescence in Member States: Argentina. Synchrotron radiation total reflection X-ray fluorescence study of gums

    International Nuclear Information System (INIS)

    Full text: Over the years, the term gums has been used for a wide range of compounds including polysaccharides, terpenes, proteins, and synthetic polymers. In the 1990s, the term more specifically denotes a group of industrially useful polysaccharides or their derivatives that hydrate in hot or cold water to form viscous solutions, dispersions, or gels. Gums are used in industry because their aqueous solutions or dispersions have suspending and stabilizing properties. In addition, gums may produce gels or act as emulsifiers, adhesives, flocculants, binders, film formers, lubricants, or friction reducers, depending on the shape and chemical nature of the particular gum. They have increasingly been used in recent years by industry due to their controlled, reproducible and economical biosynthesis, and their biodegradability. Gums are classified as natural or modified. Natural gums include seaweed extracts, plant exudates, gums from seed or root, and gums obtained by microbial fermentation. Modified (semi-synthetic) gums include cellulose and starch derivatives and certain synthetic gums such as low methoxyl pectin, propylene glycol alginate, and carboxymethyl and hydroxypropyl guar gum. Selected polymers from the different groups were characterised in this work. Specifications of these polymers have to be controlled by European Community, Mercosur, etc. especially for toxic metals in food and pharmaceutical products. Synchrotron Radiation (SR) induced Total Reflection X-ray Fluorescence (SRTXRF) analysis expands the possibilities of conventional TXRF based on X-ray tube excitation. In this study the SRTXRF technique was successfully applied for the quantification of F, Na, Mg, S, K, Ca, V, Cr, Mn, Fe, Ni, Cu, Zn, As and Pb in high-viscosity gum aqueous solutions. The results were analysed from both toxic and alimentary point of view. (author)

  1. 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.

  2. Critical dimension small angle X-ray scattering measurements of FinFET and 3D memory structures

    Science.gov (United States)

    Settens, Charles; Bunday, Benjamin; Thiel, Brad; Kline, R. Joseph; Sunday, Daniel; Wang, Chengqing; Wu, Wen-li; Matyi, Richard

    2013-04-01

    We have demonstrated that transmission critical dimension small angle X-ray scattering (CD-SAXS) provides high accuracy and precision CD measurements on advanced 3D microelectronic architectures. The competitive advantage of CD-SAXS over current 3D metrology methods such as optical scatterometry is that CD-SAXS is able to decouple and fit cross-section parameters without any significant parameter cross-correlations. As the industry aggressively scales beyond the 22 nm node, CD-SAXS can be used to quantitatively measure nanoscale deviations in the average crosssections of FinFETs and high-aspect ratio (HAR) memory devices. Fitting the average cross-section of 18:1 isolated HAR contact holes with an effective trapezoid model yielded an average pitch of 796.9 +/- 0.4 nm, top diameter of 70.3 +/- 0.9 nm, height of 1088 +/- 4 nm, and sidewall angle below 0.1°. Simulations of dense 40:1 HAR contact holes and FinFET fin-gate crossbar structures have been analyzed using CD-SAXS to inquire the theoretical precision of the technique to measure important process parameters such as fin CD, height, and sidewall angle; BOX etch recess, thickness of hafnium oxide and titanium nitride layers; gate CD, height, and sidewall angle; and hafnium oxide and titanium nitride etch recess. The simulations of HAR and FinFET structures mimic the characteristics of experimental data collected at a synchrotron x-ray source. Using the CD-SAXS simulator, we estimate the measurement capabilities for smaller similar structures expected at future nodes to predict the applicability of this technique to fulfill important CD metrology needs.

  3. Larger scale structures in starch granules chartacterised via small-angle neutron and x-ray scattering

    International Nuclear Information System (INIS)

    Starch is the primary carbohydrate component in the human diet and the major storage polysaccharide in plants. Small angle scattering (SAS) techniques have an extensive track record in illuminating the semi-crystalline lamellar structure of the starch granule, however, 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. In this study, SAS data collected over an extended q range were gathered from dry and hydrated starch powders of various botanical origins. 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. SAXS measurements were obtained with the Bruker Nanostar, whilst SANS measurements taken at the QUOKKA instrument, ANSTO. Data were analysed with the 'unified' method, which fits SAS curves from hierarchical structures, with each level consisting of a Guinier and Porod component which can be refined during fitting. 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.

  4. 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.

  5. Emerging trends in X-ray spectroscopic studies of plasma produced by intense laser beams

    International Nuclear Information System (INIS)

    X-ray line emission from hot dense plasmas, produced by ultra-short high intensity laser systems, has been studied experimentally in recent years for applications in materials science as well as for back-lighter applications. By virtue of the CPA technology, several laser facilities delivering pulses with peak powers in excess of one petawatt (focused intensities > 1020 W-cm−2) have either been commissioned across the globe during the last few years or are presently under construction. On the other hand, hard x-ray sources on table top, generating ultra-short duration x-rays at a repetition rate up to 10 kHz, are routinely available for time resolved x-ray diffraction studies. In this paper, the recent experiments on x-ray spectroscopic studies of plasma produced by 45 fs, Ti:sapphire laser pulses (focused iintensity > 1018 W-cm−2) at RRCAT Indore will be presented

  6. Amplitude and phase changes on VLF/LF radio signals depending on solar zenith angle during occurrences of solar X-ray flares

    Science.gov (United States)

    Sulic, Desanka; Sreckovic, Vladimir; Mihajlov, A. A.

    2016-07-01

    The focus of this work is on the extraction of D-region electron density that is induced by the intensive X-ray flux under different solar zenith angle. The sensitivity of Very Low and Low Frequency (VLF and LF) propagation in the lower ionosphere makes it an ideal probe for remotely sensing the ambient state and localized perturbations of the ionosphere. The basis of this work is amplitude and phase data acquired by monitoring DHO/23.40 kHz and NSC/45.90 kHz radio signals during the period of ascending and maximum of the solar cycle 24. All the data were recorded at Belgrade station (44.85 ^{0} N, 20.38 ^{0} E) by AWESOME system. DHO-BEL and NSC-BEL are short paths with distances of 1300 and 953 km, respectively. These paths are in the same time zone. The diurnal amplitude and phase variations on VLF/LF radio signal against time vary in characteristic ways that are caused by solar zenith angles over path. Two amplitude minima are observed when sunrise and sunset terminators reach the middle of the propagation path. During daytime condition there are two amplitude minima (in morning and afternoon) developed under solar zenith angles χ ˜80 ^{0} over short path. In this study we considered amplitude and phase perturbations on VLF/LF radio signal induced by solar X-ray flares under solar zenith angles which are close with timings of amplitude minima during daytime under normal ionospheric condition. We expected and estimated differences in amplitude and phase perturbations on DHO/23.40 kHz and NSC/45.90 kHz radio signals induced by solar X-ray flares which occurrences are under solar zenith angles χ ≤ 80 ^{0}. The observations include solar flares with magnitudes in the range from C2 (I_{X} = 2 10^{-6} Wm^{-2} of X-ray flux in the band at 0.1 - 0.8 nm) to X2.1 (I_{X} = 2.1 10^{-4} Wm^{-2}) class. For example on 11 March 2015 occurred X2.1 class flare with maximum of intensity at 16:22 UT, when solar angle was χ = 81^{0} at Belgrade. One day before, under normal

  7. Atomic-Scale Studies of Oxides Supported Catalysts by X-ray and Imaging Methods

    Science.gov (United States)

    Feng, Zhenxing

    2011-12-01

    Oxide supported metal and metal oxide catalysts have been synthesized by molecular beam epitaxy (MBE) and atomic-layer deposition (ALD). To obtain a general idea of how a catalyst behaves chemically and structurally during reduction-oxidization (redox) reaction at atomic-scale, oxide single crystals with well-defined surfaces are used as supports to grow monolayer (ML) and sub-ML catalysts. Several model catalysis systems are investigated: Pt/SrTiO 3(001), WOX/alpha-Fe2O3(0001), VO X/alpha-TiO2(110) and mixed VOX/WOX/alpha-TiO 2(110). For purposes of comparison the catalysts include a noble metal (Pt), inert oxide (WOX) and active oxide (VOX). The oxide supports are categorized as a reducible substrate, alpha-Fe2 O3(0001), and non-reducible substrates, alpha-TiO 2(110) and SrTiO3(001). To obtain in situ information, a variety of X-ray and scanning imaging methods have been applied together to study the atomic-scale surface morphology, structure and cation dynamics during chemical reactions. These characterization techniques are: X-ray standing wave (XSW), grazing-incident small angle X-ray scattering (GISAXS), X-ray absorption fine structure (XAFS), X-ray reflectivity (XRR), X-ray fluorescence (XRF), X-ray photoelectron spectroscopy (XPS), atomic-force microscopy (AFM) and scanning electron microscopy (SEM). Our studies show that different combinations of catalysts and substrates give distinct structural and chemical state changes in redox reactions. For MBE deposited sub-monolayer (sub-ML) Pt on the 2 x 1 SrTiO 3(001) surface, AFM shows the formation of nanoparticles and XSW atomic imaging shows that these nanoparticles are composed of Pt face-centered-cubic nanocrystals with cube-on-cube epitaxy coherent to the substrate unit cell. Different Pt coverages lead to differences in the observed XSW image of the interfacial structure, which is explained by the Pt-Pt interaction becoming stronger than the Pt-substrate interaction as the coverage is increased from 0.2 to

  8. A statistical study of the relation between soft X-ray excess and accretion disk

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    To study the origin of the soft X-ray excess,we compile a sample of 94 unobscured,radio-quiet QSOs and Seyfert galaxies with available data from GALEX and ROSAT.We find that 50 sources show strong soft X-ray excess and the other 44 show weak/no soft X-ray excess.Systematic analyses of the data indicate that the difference in soft X-rays is mainly but not only resulting from different accretion rates(in units of Eddington rate).The statistical study of the sources with soft X-ray excess shows that the strength of soft X-ray excess weakly and positively correlates with the Eddington ratio and increases with the increase of the strength of UV radiations relative to the X-rays.Provided that the UV emissions are from the thin disk,the correlations imply that the origin of soft X-ray excess is associated with the thin disk,either by means of Comptonization of the disk photons or in some other ways.

  9. Time-resolved X-ray studies using third generation synchrotron radiation sources

    International Nuclear Information System (INIS)

    The third generation, high-brilliance, hard x-ray, synchrotron radiation (SR) sources currently under construction (ESRF at Grenoble, France; APS at Argonne, Illinois; and SPring-8 at Harima, Japan) will usher in a new era of x-ray experimentation for both physical and biological sciences. One of the most exciting areas of experimentation will be the extension of x-ray scattering and diffraction techniques to the study of transient or time-evolving systems. The high repetition rate, short-pulse duration, high brilliance, and variable spectral bandwidth of these sources make them ideal for x-ray time-resolved studies. The temporal properties (bunch length, interpulse period, etc.) of these new sources will be summarized. Finally, the scientific potential and the technological challenges of time-resolved x-ray scattering from these new sources will be described. 13 refs., 4 figs

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

    International Nuclear Information System (INIS)

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Eliezer, D.

    1994-06-01

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

  12. Quantum theory of X-ray radiation at Bragg angles at channeling

    International Nuclear Information System (INIS)

    In the framework of quantum electrodynamics the theory of the new type of X-ray radiation from the channeled electrons in vicinity of the Bragg angle—Diffracted Channeling Radiation (DCR) is developed beyond the dipole approximation. The DCR occurs due to transitions of the channeled electrons from one transverse energy level to another with the diffraction of the emitted photon. It is demonstrated that dipole approximation is valid for the first order of diffraction DCR and not valid for higher orders of diffraction. On the basis of obtained equations for the first time it is theoretically shown that the angular distribution of the DCR is a system of very narrow ring-shaped peaks around of the Bragg direction. The calculations were performed taking into account the band structure of the transverse motion energy. - Highlights: • For the first time we developed theory of the DCR beyond the dipole approximation. • The applicability of the dipole approximation is considered. • Analytically shown that DCR angular distribution represents system of double rings. • In planar case angular distribution is not symmetrical with respect to X- and Y-axis

  13. Magnetic dichroism in angle-resolved hard x-ray photoemission from buried layers

    Science.gov (United States)

    Kozina, Xeniya; Fecher, Gerhard H.; Stryganyuk, Gregory; Ouardi, Siham; Balke, Benjamin; Felser, Claudia; Schönhense, Gerd; Ikenaga, Eiji; Sugiyama, Takeharu; Kawamura, Naomi; Suzuki, Motohiro; Taira, Tomoyuki; Uemura, Tetsuya; Yamamoto, Masafumi; Sukegawa, Hiroaki; Wang, Wenhong; Inomata, Koichiro; Kobayashi, Keisuke

    2011-08-01

    This work reports the measurement of magnetic dichroism in angular-resolved photoemission from in-plane magnetized buried thin films. The high bulk sensitivity of hard x-ray photoelectron spectroscopy (HAXPES) in combination with circularly polarized radiation enables the investigation of the magnetic properties of buried layers. HAXPES experiments with an excitation energy of 8 keV were performed on exchange-biased magnetic layers covered by thin oxide films. Two types of structures were investigated with the IrMn exchange-biasing layer either above or below the ferromagnetic layer: one with a CoFe layer on top and another with a Co2FeAl layer buried beneath the IrMn layer. A pronounced magnetic dichroism is found in the Co and Fe 2p states of both materials. The localization of the magnetic moments at the Fe site conditioning the peculiar characteristics of the Co2FeAl Heusler compound, predicted to be a half-metallic ferromagnet, is revealed from the magnetic dichroism detected in the Fe 2p states.

  14. Calculations and surface quality measurements of high-asymmetry angle x-ray crystal monochromators for advanced x-ray imaging and metrological applications

    Science.gov (United States)

    Zápražný, Zdenko; Korytár, Dušan; Jergel, Matej; Šiffalovič, Peter; Dobročka, Edmund; Vagovič, Patrik; Ferrari, Claudio; Mikulík, Petr; Demydenko, Maksym; Mikloška, Marek

    2015-03-01

    We present the numerical optimization and the technological development progress of x-ray optics based on asymmetric germanium crystals. We show the results of several basic calculations of diffraction properties of germanium x-ray crystal monochromators and of an analyzer-based imaging method for various asymmetry factors using an x-ray energy range from 8 to 20 keV. The important parameter of highly asymmetric monochromators as image magnifiers or compressors is the crystal surface quality. We have applied several crystal surface finishing methods, including advanced nanomachining using single-point diamond turning (SPDT), conventional mechanical lapping, chemical polishing, and chemomechanical polishing, and we have evaluated these methods by means of atomic force microscopy, diffractometry, reciprocal space mapping, and others. Our goal is to exclude the chemical etching methods as the final processing technique because it causes surface undulations. The aim is to implement very precise deterministic methods with a control of surface roughness down to 0.1 nm. The smallest roughness (˜0.3 nm), best planarity, and absence of the subsurface damage were observed for the sample which was machined using an SPDT with a feed rate of 1 mm/min and was consequently polished using a fine polishing 15-min process with a solution containing SiO2 nanoparticles (20 nm).

  15. Novel detector design for reducing intercell x-ray cross-talk in the variable resolution x-ray CT scanner: A Monte Carlo study

    Energy Technology Data Exchange (ETDEWEB)

    Arabi, Hosein; Asl, Ali Reza Kamali; Ay, Mohammad Reza; Zaidi, Habib [Department of Radiation Medicine, Shahid Beheshti University, 1983963113 Tehran (Iran, Islamic Republic of); Research Centre for Science and Technology in Medicine, Tehran University of Medical Sciences, 1417613151 Tehran (Iran, Islamic Republic of); Department of Medical Physics and Biomedical Engineering, Tehran University of Medical Sciences, 1417613151 Tehran (Iran, Islamic Republic of); and Research Institute for Nuclear Medicine, Tehran University of Medical Sciences, 1417613151 Tehran (Iran, Islamic Republic of); Division of Nuclear Medicine, Geneva University Hospital, CH-1211 Geneva (Switzerland); Geneva Neuroscience Center, Geneva University, CH-1211 Geneva (Switzerland) and Department of Nuclear Medicine and Molecular Imaging, University Medical Center Groningen, University of Groningen, 9700 RB Groningen (Netherlands)

    2011-03-15

    Purpose: The variable resolution x-ray (VRX) CT scanner provides substantial improvement in the spatial resolution by matching the scanner's field of view (FOV) to the size of the object being imaged. Intercell x-ray cross-talk is one of the most important factors limiting the spatial resolution of the VRX detector. In this work, a new cell arrangement in the VRX detector is suggested to decrease the intercell x-ray cross-talk. The idea is to orient the detector cells toward the opening end of the detector. Methods: Monte Carlo simulations were used for performance assessment of the oriented cell detector design. Previously published design parameters and simulation results of x-ray cross-talk for the VRX detector were used for model validation using the GATE Monte Carlo package. In the first step, the intercell x-ray cross-talk of the actual VRX detector model was calculated as a function of the FOV. The obtained results indicated an optimum cell orientation angle of 28 deg. to minimize the x-ray cross-talk in the VRX detector. Thereafter, the intercell x-ray cross-talk in the oriented cell detector was modeled and quantified. Results: The intercell x-ray cross-talk in the actual detector model was considerably high, reaching up to 12% at FOVs from 24 to 38 cm. The x-ray cross-talk in the oriented cell detector was less than 5% for all possible FOVs, except 40 cm (maximum FOV). The oriented cell detector could provide considerable decrease in the intercell x-ray cross-talk for the VRX detector, thus leading to significant improvement in the spatial resolution and reduction in the spatial resolution nonuniformity across the detector length. Conclusions: The proposed oriented cell detector is the first dedicated detector design for the VRX CT scanners. Application of this concept to multislice and flat-panel VRX detectors would also result in higher spatial resolution.

  16. Design Case Studies of Anti-scattering X-ray Grid by MCNP Code Simulation

    International Nuclear Information System (INIS)

    The scattered photon cannot but be projected to the detector pixel where it is initially headed. Therefore, reducing the scattered photon in x-ray imaging system is essential to decrease unwanted radiation exposure to patient and increase the accuracy of diagnosis. In order to reduce scattered photons, an anti-scattering X-ray grid, which consists of shielding material and penetration materials, is equipped in X-ray imaging system. The design case study of anti-scattering X-ray grid was performed for the three designs of square, honeycomb and circle type by MCNP simulation. The optimization of thickness of shielding material was conducted on three cases of the length of a side of hexagon of honeycomb type anti-scattering X-ray grid. It was understood that the performance of grid was not depend on the grid type in this fundamental approach

  17. Some studies on low-frequency signal in relation to X-ray flares and climatic conditions

    Directory of Open Access Journals (Sweden)

    S. K. Sarkar

    Full Text Available The statistical behaviour of the sudden enhancement in signal strength (SES in relation to solar X-ray flares has been studied for the near east-west propagation of 40 kHz radio waves from Sanwa (36°11'N; 139°51'E in Japan to Calcutta (22°34'N; 88°24'E over a long distance path of 5100 km for a period of two years. The period has been divided into four phases - P1, P2, P3 and P4, according to the position of the overhead sun. The change in signal strength during X-ray flares is dependent on the solar zenith angle and climatic conditions. The statistical modal values of the time lag of the SES peak with respect to that solar X-ray flare is found to increase as solar zenith angle increases. The relative rates of increase and decrease of the signal strength (RRISS and RRDSS respectively have been evaluated for a number of SES which are related to large X-ray flares. Their characteristics have also been investigated. The modal values of the relaxation time have been found to be highly correlated with climatic conditions like temperature and humidity of the propagation path.

  18. Study of lead iodide crystals for X-Ray detection

    Czech Academy of Sciences Publication Activity Database

    Matuchová, Marie; Žďánský, Karel; Zavadil, Jiří

    2006-01-01

    Roč. 100, č. 8 (2006), s. 635. ISSN 0009-2770. [Sjezd chemických společností /58./. Ústí nad Labem, 04.09.2006-08.09.2006] R&D Projects: GA ČR(CZ) GA102/04/0959; GA ČR(CZ) GA102/03/0379 Institutional research plan: CEZ:AV0Z20670512 Keywords : zone melting * X-Ray diffraction * semiconductor technology Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 0.431, year: 2006

  19. X-ray studies of polymer/gold nanocomposites

    International Nuclear Information System (INIS)

    We demonstrate that x-ray reflection standing wave fluorescence spectroscopy is a highly sensitive technique for the determination of the distribution of metal nanoparticles inside polymer thin films. We investigate both the depth profile and the in-plane spatial correlation of gold nanoparticles in an asymmetric polystyrene-b-poly(2-vinylpyridine) block copolymer film. These copolymer films self-assemble into alternating, nanometer-sized domains that are, upon annealing, selectively decorated by thermally evaporated metal nanoparticles to form metal/polymer composites. copyright 1999 American Institute of Physics

  20. High-pressure powder x-ray diffraction study of EuVO{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Garg, Alka B. [High Pressure and Synchrotron Radiation Physics Division, Bhabha Atomic Research Centre, Mumbai 400085, Maharashtra (India); Errandonea, D., E-mail: daniel.errandonea@uv.es [Departamento de Física Aplicada—ICMUV, MALTA Consolider Team, Universidad de Valencia, Edificio de Investigación, C/Dr. Moliner 50, Burjassot, 46100 Valencia (Spain)

    2015-03-15

    The high-pressure structural behavior of europium orthovanadate has been studied using in-situ, synchrotron based, high-pressure x-ray powder diffraction technique. Angle-dispersive x-ray diffraction measurements were carried out at room temperature up to 34.7 GPa using a diamond-anvil cell, extending the pressure range reported in previous experiments. We confirmed the occurrence of zircon–scheelite phase transition at 6.8 GPa and the coexistence of low- and high-pressure phases up to 10.1 GPa. In addition, clear evidence of a scheelite–fregusonite transition is found at 23.4 GPa. The fergusonite structure remains stable up to 34.7 GPa, the highest pressure reached in the present measurements. A partial decomposition of EuVO{sub 4} was also observed from 8.1 to 12.8 GPa; however, this fact did not preclude the identification of the different crystal structures of EuVO{sub 4}. The crystal structures of the different phases have been Rietveld refined and their equations of state (EOS) have been determined. The results are compared with the previous experimental data and theoretical calculations. - Graphical abstract: The high-pressure structural sequence of EuVO{sub 4}. - Highlights: • EuVO{sub 4} is studied under pressure up to 35 GPa using synchrotron XRD. • The zircón–scheelite–fergusonite structural sequence is observed. • Crystal structures are refined and equations of state determined.

  1. The soft x-ray instrument for materials studies at the linac coherent light source x-ray free-electron laser

    OpenAIRE

    Schlotter, W. F.; Turner, J. J.; Fernández-Perea, M.; Kelez, N.; Lee, S.; Coffee, R.; Hays, G.; Beye, M; Gerken, N.; Sorgenfrei, F.; Hau-Riege, S.; Juha, L.; Rowen, M; Chalupsky, J.; Hajkova, V

    2012-01-01

    The soft x-ray materials science instrument is the second operational beamline at the linac coherent light source x-ray free electron laser. The instrument operates with a photon energy range of 480-2000 eV and features a grating monochromator as well as bendable refocusing mirrors. A broad range of experimental stations may be installed to study diverse scientific topics such as: ultrafast chemistry, surface science, highly correlated electron systems, matter under extreme conditions, and la...

  2. 6 MV x-ray dose in the build up region: empirical model and the incident angle effect

    International Nuclear Information System (INIS)

    A simple and fast empirical model has been developed which accurately predicts central axis surface and build up dose for a 6MV radiotherapy x-ray beam. The model is based on fits to experimental data and accounts for open fields, block trays and wedges at normal incidence and at angle. The model separates the beam into components produced by primary photon interactions which have only interacted in the phantom at normal and oblique incidence and head scattered photons/ electrons generated in the treatment head. The model quantifies these components for open unwedged fields and then the effect on each component by introducing beam modifying devices / accessories or changing the angle of incidence is determined. Dose results at oblique incidence for Monte Carlo (electron contamination free) and experimental (electron contamination present) are sufficiently close to imply that the increase in build up dose with beam angle is mainly due to changes in photon interactions within the phantom and only a slight increase with angle is due to changes in the electron contamination. Electron contamination/ head scatter component was found to be measurable by three methods. These being TLD extrapolation in air, ionisation chamber measurements in air and Monte Carlo pure photon methods. These methods produced comparable electron contamination/head scatter dose results at all field sizes. 19 refs., 10 figs

  3. Study of archaeological ceramics by total-reflection X-ray fluorescence spectrometry: Semi-quantitative approach

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Ruiz, R. [Universidad Autonoma de Madrid, Facultad de Ciencias, Servicio Interdepartamental de Investigacion, Modulo C-9, Laboratorio de TXRF, Crta. Colmenar, Km 15, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Garcia-Heras, M. [Instituto de Historia-CSIC, C/Serrano, 13. E-28001, Madrid (Spain); CENIM-CSIC, Avda. Gregorio del Amo, 8. E-28040, Madrid (Spain)

    2007-10-15

    Total-reflection X-ray fluorescence spectrometry has been compared with Instrumental Neutron Activation Analysis in order to test its potential application to the study of archaeological ceramics in the archaeometric field. Two direct solid non-chemical sample preparation procedures have been checked: solid sedimentation and solid chemical homogenization. For sedimentation procedure, total-reflection X-ray fluorescence allows the analysis of the elemental composition with respect to the size fraction but not the average evaluation of the composition. For solid chemical homogenization procedure, total-reflection X-ray fluorescence provides precise (from 0.8% to 27% of coefficient of variation) and accurate results (from 91% to 110% of recovery) for 15 elements (Cr, Hf, Ni, Rb, Al, Ba, Ca, K, Mn, Ti, V, Cu, Ga, Y and Fe) with an easy sample preparation process of the solid clay and without previous chemical treatment. The influence of the particle sizes has been checked by total-reflection X-ray fluorescence sample angle scans and anomalous behaviors have been found for three additional detected elements: As, Sr and Zn, which can be attributed to interference effects of the mineral grain sizes of their associated chemical phases in the total-reflection X-ray fluorescence interference region. The solid chemical homogenization procedure produces data useful for archaeological interpretation, which is briefly illustrated by a case-study. Finally, the decantation procedure data can be also useful for size chemical speciation and, consequently, for alternative environmental total-reflection X-ray fluorescence applications.

  4. Study of archaeological ceramics by total-reflection X-ray fluorescence spectrometry: Semi-quantitative approach

    International Nuclear Information System (INIS)

    Total-reflection X-ray fluorescence spectrometry has been compared with Instrumental Neutron Activation Analysis in order to test its potential application to the study of archaeological ceramics in the archaeometric field. Two direct solid non-chemical sample preparation procedures have been checked: solid sedimentation and solid chemical homogenization. For sedimentation procedure, total-reflection X-ray fluorescence allows the analysis of the elemental composition with respect to the size fraction but not the average evaluation of the composition. For solid chemical homogenization procedure, total-reflection X-ray fluorescence provides precise (from 0.8% to 27% of coefficient of variation) and accurate results (from 91% to 110% of recovery) for 15 elements (Cr, Hf, Ni, Rb, Al, Ba, Ca, K, Mn, Ti, V, Cu, Ga, Y and Fe) with an easy sample preparation process of the solid clay and without previous chemical treatment. The influence of the particle sizes has been checked by total-reflection X-ray fluorescence sample angle scans and anomalous behaviors have been found for three additional detected elements: As, Sr and Zn, which can be attributed to interference effects of the mineral grain sizes of their associated chemical phases in the total-reflection X-ray fluorescence interference region. The solid chemical homogenization procedure produces data useful for archaeological interpretation, which is briefly illustrated by a case-study. Finally, the decantation procedure data can be also useful for size chemical speciation and, consequently, for alternative environmental total-reflection X-ray fluorescence applications

  5. High-pressure powder x-ray diffraction study of EuVO4

    Science.gov (United States)

    Garg, Alka B.; Errandonea, D.

    2015-03-01

    The high-pressure structural behavior of europium orthovanadate has been studied using in-situ, synchrotron based, high-pressure x-ray powder diffraction technique. Angle-dispersive x-ray diffraction measurements were carried out at room temperature up to 34.7 GPa using a diamond-anvil cell, extending the pressure range reported in previous experiments. We confirmed the occurrence of zircon-scheelite phase transition at 6.8 GPa and the coexistence of low- and high-pressure phases up to 10.1 GPa. In addition, clear evidence of a scheelite-fregusonite transition is found at 23.4 GPa. The fergusonite structure remains stable up to 34.7 GPa, the highest pressure reached in the present measurements. A partial decomposition of EuVO4 was also observed from 8.1 to 12.8 GPa; however, this fact did not preclude the identification of the different crystal structures of EuVO4. The crystal structures of the different phases have been Rietveld refined and their equations of state (EOS) have been determined. The results are compared with the previous experimental data and theoretical calculations.

  6. Structure and kinetics of chemically cross-linked protein gels from small-angle X-ray scattering

    CERN Document Server

    Kaieda, Shuji; Halle, Bertil

    2014-01-01

    Glutaraldehyde (GA) reacts with amino groups in proteins, forming intermolecular cross-links that, at sufficiently high protein concentration, can transform a protein solution into a gel. Although GA has been used as a cross-linking reagent for decades, neither the cross-linking chemistry nor the microstructure of the resulting protein gel have been clearly established. Here we use small-angle X-ray scattering (SAXS) to characterise the microstructure and structural kinetics of gels formed by cross-linking of pancreatic trypsin inhibitor, myoglobin or intestinal fatty acid-binding protein. By comparing the scattering from gels and dilute solutions, we extract the structure factor and the pair correlation function of the gel. The protein gels are spatially heterogeneous, with dense clusters linked by sparse networks. Within the clusters, adjacent protein molecules are almost in contact, but the protein concentration in the cluster is much lower than in a crystal. At the $\\sim$ 1 nm SAXS resolution, the native ...

  7. Measurement of latent tracks in amorphous SiO{sub 2} using small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Kluth, P. [Department of Electronic Materials Engineering, Australian National University, Canberra ACT 0200 (Australia)], E-mail: patrick.kluth@anu.edu.au; Schnohr, C.S.; Sprouster, D.J. [Department of Electronic Materials Engineering, Australian National University, Canberra ACT 0200 (Australia); Byrne, A.P. [Department of Nuclear Physics, Faculty of Physics, Australian National University, Canberra ACT 0200 (Australia); Cookson, D.J. [Australian Synchrotron Research Program, Building 434, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Ridgway, M.C. [Department of Electronic Materials Engineering, Australian National University, Canberra ACT 0200 (Australia)

    2008-06-15

    In this paper we present preliminary yet promising results on the measurement of latent ion tracks in amorphous, 2 {mu}m thick SiO{sub 2} layers using small angle X-ray scattering (SAXS). The tracks were generated by ion irradiation with 89 MeV Au ions to fluences between 3 x 10{sup 10} and 3 x 10{sup 12} ions/cm{sup 2}. Transmission SAXS measurements show distinct scattering from the irradiated SiO{sub 2} as compared to the unirradiated material. Analysis of the SAXS spectra using a cylindrical model suggests a core-shell like density distribution in the ion tracks with a lower density core and a higher density shell as compared to unirradiated material. The total track radius of {approx}48 A is in very good agreement with previous experiments and calculations based on an inelastic thermal spike model.

  8. Measurement of latent tracks in amorphous SiO2 using small angle X-ray scattering

    International Nuclear Information System (INIS)

    In this paper we present preliminary yet promising results on the measurement of latent ion tracks in amorphous, 2 μm thick SiO2 layers using small angle X-ray scattering (SAXS). The tracks were generated by ion irradiation with 89 MeV Au ions to fluences between 3 x 1010 and 3 x 1012 ions/cm2. Transmission SAXS measurements show distinct scattering from the irradiated SiO2 as compared to the unirradiated material. Analysis of the SAXS spectra using a cylindrical model suggests a core-shell like density distribution in the ion tracks with a lower density core and a higher density shell as compared to unirradiated material. The total track radius of ∼48 A is in very good agreement with previous experiments and calculations based on an inelastic thermal spike model

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

    International Nuclear Information System (INIS)

    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

  10. Characterization of the nanopore structures of PAN-based carbon fiber precursors by small angle X-ray scattering

    International Nuclear Information System (INIS)

    The nanopore structures m precursors are crucial to the performance of PAN-based carbon fibers. Four carbon-fiber precursors are prepared. They are bath-fed filaments (A), water-washing filaments (B), hot-stretching filaments (C) and drying-densification filaments (D). Synchrotron radiation small angle X-ray scattering is used to probe and compare the nanopore structures of the four fibers. The nanopore size, discrete volume distribution, nanopore orientation degree along the fiber axis and the porosity are obtained. The results demonstrate that the nanopores are mainly formed in the water-washing stage. During the processes of the subsequent production technologies, the slenderness ratio of nanopores and their orientation degree along the fiber axis increase further and simultaneously, the porosity decreases. These results are helpful for improving the performance of the final carbon fibers. (authors)

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

    International Nuclear Information System (INIS)

    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 × 106 photons/s at a beam size of 1.2 × 1.2 mm2 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−1 down to 0.009 Å−1 in SAXS configuration and of 0.26 Å−1 up to 5.7 Å−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−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

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

    Science.gov (United States)

    Bruetzel, Linda K.; Fischer, Stefan; Salditt, Annalena; Sedlak, Steffen M.; Nickel, Bert; Lipfert, Jan

    2016-02-01

    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 × 106 photons/s at a beam size of 1.2 × 1.2 mm2 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-1 down to 0.009 Å-1 in SAXS configuration and of 0.26 Å-1 up to 5.7 Å-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-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.

  13. 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.

  14. Development of a high-resolution soft x-ray (30--1500 eV) beamline at the Advanced Light Source and its use for the study of angle-resolved photoemission extended fine structure

    International Nuclear Information System (INIS)

    ALS Bending magnet beamline 9.3.2 is for high resolution spectroscopy, with circularly polarized light. Fixed included-angle SGM uses three gratings for 30--1500 eV photons; circular polarization is produced by an aperture for selecting the beam above or below the horizontal plane. Photocurrent from upper and lower jaws of entrance slit sets a piezoelectric drive feedback loop on the vertically deflecting mirror for stable beam. End station has a movable platform. With photomeission data from Stanford, structure of c(2x2)P/Fe(100) was determined using angle-resolved photoemission extended fine structure (ARPEFS). Multiple-scattering spherical-wave (MSSW) calculations indicate that P atoms adsorb in fourfold hollow sites 1.02A above the first Fe layer. Self-consistent-field Xα scattered wave calculation confirm that the Fe1-Fe2 space is contracted for S/Fe but not for P/Fe; comparison is made to atomic N and O on Fe(100). Final-state effects on ARPEFS curves used literature data from the S 1s and 2p core levels of c(2x2)S/Ni(001); a generalized Ramsauer-Townsend splitting is present in the 1s but not 2p data. An approximate method for analyzing ARPEFS data from a non-s initial state using only the higher-ell partial wave was tested successfully. ARPEFS data from clean surfaces were collected normal to Ni(111) (3p core levels) and 5 degree off-normal from Cu(111)(3s, 3p). Fourier transforms (FT) resemble adsorbate systems, showing backscattering signals from atoms up to 4 layers below emitters. 3p FTs show scattering from 6 nearest neighbors in the same crystal layer as the emitters. MSSW calulation indicate that Cu 3p photoemission is mostly d-wave. FTs also indicate double-scattering and single-scattering from laterally distant atoms; calculations indicate that the signal is dominated by photoemission from the first 2 crystal layers

  15. Purification, crystallization and preliminary X-ray study of the fungal laccase from Cerrena maxima

    International Nuclear Information System (INIS)

    The crystallization and preliminary X-ray structure at 1.9 Å resolution of the fungal laccase from C. maxima are presented. Laccases are members of the blue multi-copper oxidase family that oxidize substrate molecules by accepting electrons at a mononuclear copper centre and transferring them to a trinuclear centre. Dioxygen binds to the trinuclear centre and, following the transfer of four electrons, is reduced to two molecules of water. Crystals of the laccase from Cerrena maxima have been obtained and X-ray data were collected to 1.9 Å resolution using synchrotron radiation. A preliminary analysis shows that the enzyme has the typical laccase structure and several carbohydrate sites have been identified. The carbohydrate chains appear to be involved in stabilization of the intermolecular contacts in the crystal structure, thus promoting the formation of well ordered crystals of the enzyme. Here, the results of an X-ray crystallographic study on the laccase from the fungus Cerrena maxima are reported. Crystals that diffract well to a resolution of at least 1.9 Å (R factor = 18.953%; Rfree = 23.835; r.m.s.d. bond lengths, 0.06 Å; r.m.s.d. bond angles, 1.07°) have been obtained despite the presence of glycan moieties. The overall spatial organization of C. maxima laccase and the structure of its copper-containing active centre have been determined by the molecular-replacement method using the laccase from Trametes versicolor (Piontek et al., 2002 ▶) as a structural template. In addition, four glycan-binding sites were identified and the 1.9 Å X-ray data were used to determine the previously unknown primary structure of this protein. The identity (calculated from sequence alignment) between the C. maxima laccase and the T. versicolor laccase is about 87%. Tyr196 and Tyr372 show significant extra density at the ortho positions and this has been interpreted in terms of NO2 substituents

  16. LIGHT SOURCE: A simulation study of Tsinghua Thomson scattering X-ray source

    Science.gov (United States)

    Tang, Chuan-Xiang; Li, Ren-Kai; Huang, Wen-Hui; Chen, Huai-Bi; Du, Ying-Chao; Du, Qiang; Du, Tai-Bin; He, Xiao-Zhong; Hua, Jian-Fei; Lin, Yu-Zhen; Qian, Hou-Jun; Shi, Jia-Ru; Xiang, Dao; Yan, Li-Xin; Yu, Pei-Cheng

    2009-06-01

    Thomson scattering X-ray sources are compact and affordable facilities that produce short duration, high brightness X-ray pulses enabling new experimental capacities in ultra-fast science studies, and also medical and industrial applications. Such a facility has been built at the Accelerator Laboratory of Tsinghua University, and upgrade is in progress. In this paper, we present a proposed layout of the upgrade with design parameters by simulation, aiming at high X-ray pulses flux and brightness, and also enabling advanced dynamics studies and applications of the electron beam. Design and construction status of main subsystems are also presented.

  17. Resonant Soft X-ray Spectroscopic Studies of Light Actinides and Copper Systems

    OpenAIRE

    Modin, Anders

    2009-01-01

    Light actinides and copper systems were studied using resonant soft X-ray spectroscopy. An instrumental and experimental setup for soft X-ray spectroscopy meeting the requirements of a closed source for radioactivity was developed and described in detail. The setup was used for studies of single-crystal PuO2 oxidation. The existence of higher oxidation state than Pu(IV) in some surface areas of the single crystal were found from O 1s X-ray absorption measurements. Furthermore, from comparison...

  18. Soft X-ray emission studies of biomaterials

    International Nuclear Information System (INIS)

    Soft X-ray fluorescence measurements are used to characterize three groups of biomaterials: Vitamin B12 and derivatives, antioxidants (aspirin and paracetamol), and human teeth. We show that the chemical bonding in Vitamin B12 is characterized by the strong Co-C bond and the relatively weak Co-N bond. The Co-C bond in cyanocobalamin is found to be stronger than that of methylcobalamin leading to their different biological activity. The chemical bonding of paracetamol and aspirin is characterized by the formation of oxygen lone-pair π-orbitals, which can neutralize free radicals and therefore be related to antioxidant activity of these compounds. Carbon Kα emission spectra of a caries lesion suggest that the CaCO3 like phase exists in sound enamel and that a selective loss of carbonate occurs during the early stages of a caries attack

  19. X-ray photoemission spectroscopy study of zirconium hydride

    International Nuclear Information System (INIS)

    X-ray photoemission spectroscopy (XPS) measurements are reported for ZrH/sub 1.65/ and Zr metal. The valence-band measurements are compared with available band-theory density-of-states calculations for the metal and hydride. The hydride spectrum differs significantly from the metal spectrum. Most important, a strong peak associated with hydrogen s electrons appears approximately 7 eV below the Fermi level. XPS measurements of Zr 4p core levels show a binding-energy shift of 1 eV between Zr metal and ZrH/sub 1.65/. It is argued that this shift results from charge readjustment in the vicinity of the Zr site. With the addition of hydrogen, net charge must be transferred from the Zr site to the hydrogen site. A charge-density analysis based on simplified cluster calculations is presented

  20. Numerical study of X-ray FELS including quantum fluctuation

    Science.gov (United States)

    Reiche, S.; Saldin, E. L.; Schneidmiller, E. A.; Yurkov, M. V.

    1997-06-01

    One of the fundamental limitations towards achieving very short wavelength in a self amplified spontaneous emission free electron laser (SASE FEL) is connected with the energy diffusion in the electron beam due to quantum fluctuations of undulator radiation. Parameters of the LCLS and TESLA X-ray FEL projects are very close to this limit and there exists necessity in upgrading FEL simulation codes for optimization of SASE FEL for operation at a shortest possible wavelength. In this report we describe a one-dimensional FEL simulation code taking into account the effects of incoherent undulator radiation. Using similarity techniques we have calculated universal functions describing degradation of the FEL process due to quantum fluctuations of undulator radiation.

  1. Soft X-ray emission studies of biomaterials

    Energy Technology Data Exchange (ETDEWEB)

    Kurmaev, E.Z. E-mail: kurmaev@ifmlrs.uran.ru; Werner, J.P.; Moewes, A.; Chiuzbaian, S.; Bach, M.; Ching, W.-Y.; Motozaki, W.; Otsuka, T.; Matsuya, S.; Endo, K.; Neumann, M

    2004-07-01

    Soft X-ray fluorescence measurements are used to characterize three groups of biomaterials: Vitamin B{sub 12} and derivatives, antioxidants (aspirin and paracetamol), and human teeth. We show that the chemical bonding in Vitamin B{sub 12} is characterized by the strong Co-C bond and the relatively weak Co-N bond. The Co-C bond in cyanocobalamin is found to be stronger than that of methylcobalamin leading to their different biological activity. The chemical bonding of paracetamol and aspirin is characterized by the formation of oxygen lone-pair {pi}-orbitals, which can neutralize free radicals and therefore be related to antioxidant activity of these compounds. Carbon K{alpha} emission spectra of a caries lesion suggest that the CaCO{sub 3} like phase exists in sound enamel and that a selective loss of carbonate occurs during the early stages of a caries attack.

  2. Studies of soft x-ray emission during solar flares

    International Nuclear Information System (INIS)

    Solar flare soft x-ray emission from 0.5 A to 8.5 A was observed during 1967-68 by Bragg crystal (LiF and EDDT) spectrometers aboard the OSO-4 satellite and also by NRL broad-band ionization detectors aboard the OGO-4 satellite. In this work, instrumental parameters for the LiF crystal spectrometer based on experimental values have been determined and used in the data analysis. The total continuum emission in the 0.5 to 3 A and the 1 to 8 A broad band segments has been determined from OGO-4 data for 21 flares. In doing this, a simple and approximate method of converting the total emission based on the gray body approximation (in which the OGO-4 data are reported) to one based on the thermal continuum spectrum has been developed. (author)

  3. Environmental studies in Khartoum area using x-ray fluorescence

    International Nuclear Information System (INIS)

    In the present work an attempt has been made for the analysis of some soil, plant, sediments and fish samples of relevance to environmental pollution in Khartoum area. These samples have been collected from different places in residential areas, so as to cover industrial areas, agricultural and residential areas, as well as Tuti Island as control area. Special attention has been dedicated to the analysis of lead concentrations resulting from automobile-emissions in soils and to other toxic metals such as Cr in some industries. The samples were analysed by x-ray fluorescence (XRF) technique. The results obtained using XRF measurements and computer software called QXAS for data analysis. The concentrations of lead and some heavy metals such as Cr in soils from certain locations were alarming and may create pollution problems in the near future. The results obtained from different countries. The results are generally lower than the international limits. (Author)

  4. Comprehensive Study of the X-Ray Flares from Gamma-ray Bursts Observed by Swift

    Science.gov (United States)

    Yi, Shuang-Xi; Xi, Shao-Qiang; Yu, Hai; Wang, F. Y.; Mu, Hui-Jun; Lü, Lian-Zhong; Liang, En-Wei

    2016-06-01

    X-ray flares are generally supposed to be produced by later activities of the central engine, and may share a similar physical origin with the prompt emission of gamma-ray bursts (GRBs). In this paper, we have analyzed all significant X-ray flares from the GRBs observed by Swift from 2005 April to 2015 March. The catalog contains 468 bright X-ray flares, including 200 flares with redshifts. We obtain the fitting results of X-ray flares, such as start time, peak time, duration, peak flux, fluence, peak luminosity, and mean luminosity. The peak luminosity decreases with peak time, following a power-law behavior {L}{{p}}\\propto {T}{peak,z}-1.27. The flare duration increases with peak time. The 0.3–10 keV isotropic energy of the distribution of X-ray flares is a log-normal peaked at {10}51.2 erg. We also study the frequency distributions of flare parameters, including energies, durations, peak fluxes, rise times, decay times, and waiting times. Power-law distributions of energies, durations, peak fluxes, and waiting times are found in GRB X-ray flares and solar flares. These distributions could be well explained by a fractal-diffusive, self-organized criticality model. Some theoretical models based on magnetic reconnection have been proposed to explain X-ray flares. Our result shows that the relativistic jets of GRBs may be dominated by Poynting flux.

  5. Pinpointing the base of the AGN jets through general relativistic X-ray reverberation studies

    CERN Document Server

    Emmanoulopoulos, D

    2014-01-01

    Many theoretical models of Active Galactic Nuclei (AGN) predict that the X-ray corona, lying above the black hole, constitutes the base of the X-ray jet. Thus, by studying the exact geometry of the close black hole environment, we can pinpoint the launching site of the jet. Detection of negative X-ray reverberation time delays (i.e. soft band X-ray variations lagging behind the corresponding hard band X-ray variations) can yield significant information about the geometrical properties of the AGN, such as the location of the X-ray source, as well as the physical properties of the the black hole, such as its mass and spin. In the frame-work of the lamp-post geometry, I present the first systematic X-ray time-lag modelling results of an ensemble of 12 AGN, using a fully general relativistic (GR) ray tracing approach for the estimation of the systems' response functions. By combing these state-of-the art GR response models with statistically innovative fitting routines, I derive the geometrical layout of the clos...

  6. X-ray diffraction and mechanical properties studies on Kevlar-49 fibres

    International Nuclear Information System (INIS)

    The thesis deals with the effect of annealing in the temperature range 150-500 degrees celsius, and long-term ageing (1-150 days) at 150 degrees celsius, on the structure and mechanical properties of Kevlar-49 fibres. Wide-angle x-ray diffraction techniques were used to characterize quantitatively the structure in terms of crystallinity, crystallite size and orientation. The mechanical properties were characterized in terms of initial Young's modulus, tensile strength, and elongation at break. Thermogravimetric analysis was performed to determine the loss in weight after annealing. Differential Thermal Analysis (DTA) scan was performed to determine the 'peak melting point' of the untreated Kevlar-49 fibres. The surface topography, fracture behaviour and microfibrillar character of Kevlar-49 were studied in a scanning electron microscope. 52 refs., 30 figs., 6 tabs. (A.M.H.)

  7. X-RAY VARIABILITY STUDY OF POLAR SCATTERED SEYFERT1 GALAXIES

    Directory of Open Access Journals (Sweden)

    Tobias Beuchert

    2014-08-01

    Full Text Available We study 12 Seyfert 1 galaxies with a high level of optical polarization. Optical light emerging from the innermost regions is predominantly scattered in a polar region above the central engine directly in our line of sight. These sources show characteristics of Seyfert 2 galaxies, e.g. polarized broad lines. The polarization signatures suggest a viewing angle of 45°, classifying them as intermediate Seyfert 1/2 types. The unified model predicts this line of sight to pass through the outer layer of the torus resulting in significant soft X-ray variability due to a strongly varying column density. The aim is to find evidence for this geometrical assumption in the spectral variability of all available historical observations of these sources by XMM-Newton and Swift.

  8. X-ray diffraction studies of NbTe2 single crystal

    Indian Academy of Sciences (India)

    Neha Bhatt; Rajiv Vaidya; S G Patel; A R Jani

    2004-02-01

    NbTe2 is a member of transition metal dichalcogenide (TMDC) group. Single crystals of niobium ditelluride (NbTe2) have been grown by a chemical vapour transport technique using iodine as transporting agent. The composition of the grown crystals was confirmed on the basis of energy dispersive analysis by X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and X-ray density have been carried out for the grown crystals. The particle size for a number of reflections has been calculated using Scherrer’s formula.

  9. Study of dielectric liquids at room temperature for high energy x ray Tomography

    International Nuclear Information System (INIS)

    The detection of X rays by means of a dielectric liquid detector system, at room temperature, is discussed. The physico-chemical properties of a dielectric liquid, the construction of a cleaning device and of two electrode configurations, and the utilization of different amplifier models are studied. The results allowed the analysis and characterization of the behavior of the dielectric liquid under X ray irradiation. Data obtained is confirmed by computerized simulation. The choice of Tetramethyl-germanium for the X ray tomography, applied in nondestructive analysis, is explained. The investigation of the system parameters allowed the setting of the basis of a prototype project for a multi-detector

  10. Experimental study of neutron induced background noise on gated x-ray framing cameras

    International Nuclear Information System (INIS)

    A temporally gated x-ray framing camera based on a proximity focus microchannel plate is one of the most important diagnostic tools of inertial confinement fusion experiments. However, fusion neutrons produced in imploded capsules interact with structures surrounding the camera and produce background to x-ray signals. To understand the mechanisms of this neutron induced background, we tested several gated x-ray cameras in the presence of 14 MeV neutrons produced at the Omega laser facility. Differences between background levels observed with photographic film readout and charge-coupled-device readout have been studied.

  11. X-ray scattering and absorption studies of MnAs/GaAs heterostructures

    Science.gov (United States)

    Huang, S.; Ming, Z. H.; Soo, Y. L.; Kao, Y. H.; Tanaka, M.; Munekata, H.

    1996-02-01

    Ferromagnetic MnAs thin films grown on GaAs (001) substrates by molecular-beam epitaxy have been studied by the methods of grazing incidence x-ray scattering, x-ray diffraction, and extended x-ray-absorption fine structure. Microstructures in two films prepared with different first-layer growth conditions (template effects) are compared in terms of the interfacial roughness in the layer structure, lattice constants, epilayer thickness, local environment surrounding the Mn atoms, coordination number, and local disorder. Our results indicate that the template effects can cause significant differences in the local structures and crystallinity of the MnAs epitaxial layers.

  12. Soft X-Ray Spectroscopic Study of Fullerene Based Transition-Metal Compounds and Related Systems

    OpenAIRE

    Qian, Limin

    2001-01-01

    This thesis addresses the electronic and geometric structures of fullerene based transition-metal compounds and other related systems. The formation of TixC60, VxC60 and NbxC60 compounds has been examined by X-ray photoelectron, soft X-ray absorption and emission and spectroscopy techniques, including resonant inelastic X-ray scattering (RIXS). The symmetry and character of the chemical bond of transition metal-fulleride has been determined. A related study of single-walled carbon nanotubes i...

  13. X-ray interferometers

    International Nuclear Information System (INIS)

    An improved type of amplitude-division x-ray interferometer is described. The wavelength at which the interferometer can operate is variable, allowing the instrument to be used to measure x-ray wavelength, and the angle of inclination is variable for sample investigation. (U.K.)

  14. Magnetism in heterogeneous thin film systems: Resonant X-ray scattering studies

    CERN Document Server

    Kortright, J B; Bader, S D; Hellwig, O; Marguiles, D T; Fullerton, E E

    2003-01-01

    Magnetic and chemical heterogeneity are common in a broad range of magnetic thin film systems. Emerging resonant soft X-ray scattering techniques are well suited to resolve such heterogeneity at relevant length scales. Resonant X-ray magneto-optical Kerr effect measurements laterally average over heterogeneity but can provide depth resolution in different ways, as illustrated in measurements resolving reversible and irreversible changes in different layers of exchange-spring heterostructures. Resonant small-angle scattering measures in-plane heterogeneity and can resolve magnetic and chemical scattering sources in different ways, as illustrated in measurements of granular alloy recording media.

  15. Synchrotron X-Ray Study on Structures of Ni80Fe20/Cu Superlattices

    Institute of Scientific and Technical Information of China (English)

    XU Ming; LUO Guang-Ming; CHAI Chun-Lin; YANG Tao; MAI Zhen-Hong; LAI Wu-Yan; WU Zhong-Hua; WANG De-Wu

    2001-01-01

    We have shown that, in contrast to the results in the literature, the Bragg peak intensity of Ni80Fe20/Cu superlattices is enhanced at the incident x-ray energy slightly higher than the absorption edge of the heavier element (Cu). The atomic density at Ni80Fe20/Cu interface was analysed by the diffraction anomalous fine structure technology with the incident angle of x-ray fixed at the first Bragg peak. Our results demonstrate the epitaxy growth of Ni80Fe20/Cu superlattices. Upon annealing, the epitaxity of Ni80Fe20/Cu multilayers becomes poor but the local crystallinity in each layer is improved.

  16. Development of autocorrelator for hard X-ray free electron laser. Study on alignment procedure

    International Nuclear Information System (INIS)

    X-ray free electron laser (XFEL) sources, which produce unprecedented brilliant, transversely coherent, and ultra-short x-ray pulses, are the powerful tools for exploring new possibilities in ultrafast science with hard x rays. A split-delay optics called autocorrelator provides two replica pulses with time delay precisely controlled, which is essential to realize XFEL pump and XFEL probe experiments. In order to overlap two XFEL pulses sufficiently, precise tuning of crystal angles is required. We investigated influences of each angular error to pointing displacement of XFEL beams and the tolerated error calculated by ray trace method was ±0.07 μrad at Japan's XFEL facility, SACLA. We also present some alignment methods to parallelize the two beams after autocorrelator precisely. (author)

  17. Structural study on sodium choride by X-ray powder diffraction method

    International Nuclear Information System (INIS)

    The procedure for the crystal structure analysis by means of the X-ray powder diffraction method has been shown using the sodium chloride as a sample. The twelve X-ray diffraction intensity peaks for sodium chloride powder were collected rotating 2 THETA sub(hkl). Bragg angle of X-ray diffractometer from 20 to 160 degrees, in which Cu Ksub(α) radition filtered by nickel had been used. For assigning indices of each reflecting plane, the relationship between lattice parameter and interplanar spacing has been used. This result has shown that sodium chloride is face-centered cubic, space group F 4/m 3-2/m with until cell dimension a = 5.36 A and z = 4. The experimental and theoretical integrated intensities of the reflecting planes are in good agreement with each other. (author)

  18. Study on the influences of X Ray Scattering on radioscopic inspection

    International Nuclear Information System (INIS)

    This study issued from European project 'Verdict' (Virtual Evaluation and Robust Detection for engine Components non destructive Testing), aimed at developing and evaluating X Ray Non Destructive Method simulation. An qualitative appreciation and quantification for X Ray scattering for modelling (SINDBAD software) was identified. The effect of such radiation on radiogram results in a disturbing blur for interpretation of indications. The method and the results described are innovative in the analysis of X Ray scattering because for aeronautic field, the configurations used with this energy range are breakthrough. The approach followed consists in an experimental and practical method for evaluating scattered radiation on final image issued from the inspection. Experimental tests results confirmed that the influence of scattering radiation are linked to density variation, geometry of parts in the axis of direct radiation and spatial area. This study performed in industrial configurations contributed to improve X Ray scattering understanding. (authors)

  19. Electromigration in integrated circuit interconnects studied by X-ray microscopy

    CERN Document Server

    Schneider, G; Anderson, E; Bates, W; Salmassi, F; Nachimuthu, P; Pearson, A; Richardson, D; Hambach, D; Hoffmann, N; Hasse, W; Hoffmann, K

    2003-01-01

    To study mass transport phenomena in advanced microelectronic devices with X-rays requires penetration of dielectric and Si layers up to 30 mu m thick. X-ray imaging at 1.8 keV photon energy provides a high amplitude contrast between Cu or Al interconnects and dielectric layers and can penetrate through the required thickness. To perform X-ray microscopy at 1.8 keV, a new Ru/Si multilayer was designed for the transmission X-ray microscope XM-1 installed at the Advanced Light Source in Berkeley. The mass flow in a passivated Cu interconnect was studied at current densities up to 10 sup 7 A/cm sup 2. In addition, we demonstrated the high material contrast from different elements in integrated circuits with a resolution of about 40 nm.

  20. A preliminary study of synchrotron light sources for x-ray lithography

    International Nuclear Information System (INIS)

    A preliminary study of synchrotron light sources has been made, primarily oriented toward x-ray lithography. X-ray lithography is being pursued vigorously in several countries, with a goal of manufacturing high-density computer chips (0.25 μm feature sizes), and may attain commercial success in the next decade. Many other applications of soft x-rays appear worthy of investigation as well. The study group visited synchrotron radiation facilities and had discussions with members of the synchrotron radiation community, particularly Canadians. It concluded that accelerator technology for a conventional synchrotron light source appropriate for x-ray lithography is well established and is consistent with skills and experience at Chalk River Nuclear Laboratories. Compact superconducting systems are being developed also. Their technical requirements overlap with capabilities at Chalk River. (32 refs)

  1. Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

    Energy Technology Data Exchange (ETDEWEB)

    Van de Voorde, Lien, E-mail: lien.vandevoorde@ugent.be [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vekemans, Bart [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Verhaeven, Eddy [Antwerp University, Faculty of Design Sciences, Mutsaardstraat 31, B-2000 Antwerpen (Belgium); Tack, Pieter; De Wolf, Robin; Garrevoet, Jan [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vandenabeele, Peter [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium)

    2015-08-01

    A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg–Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position. - Highlights: • New X-ray fluorescence and X-ray diffraction instrument for non-destructive analysis • Commercially available, mobile system • One of the lightest and most compact of its kind • Characterization, data acquisition and analysis are performed. • Results of measurements on pigment model samples and cultural heritage materials.

  2. Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

    International Nuclear Information System (INIS)

    A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg–Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position. - Highlights: • New X-ray fluorescence and X-ray diffraction instrument for non-destructive analysis • Commercially available, mobile system • One of the lightest and most compact of its kind • Characterization, data acquisition and analysis are performed. • Results of measurements on pigment model samples and cultural heritage materials

  3. Polarization dependent interface properties of ferroelectric Schottky barriers studied by soft X-ray absorption spectroscopy

    OpenAIRE

    Kohlstedt, H.; Petraru, A.; Denlinger, M. Meier J.; Guo, J.; Wanli, Y.; A. Scholl; Freelon, B.; Schneller, T.; Waser, R.; Yu, P; Ramesh, R.; Learmonth, T.; Glans, P.-A.; Smith, K. E.

    2008-01-01

    We applied soft X-ray absorption spectroscopy to study the Ti L-edge in ferroelectric capacitors using a modified total electron yield method. The inner photo currents and the X-ray absorption spectra were polarization state dependent. The results are explained on the basis of photo electric effects and the inner potential in the ferroelectric capacitors as a result of back-to-back Schottky barriers superimposed by the potential due to the depolarization field. In general, the presented metho...

  4. Recent Developments in the Application of X-ray Microanalysis to the Study of Food Systems

    OpenAIRE

    Brooker, B E

    1991-01-01

    Low temperature scanning electron microscopy in conjunction with X-ray microanalysis can be used to study not only the internal structure of intact bulk food systems but also the distribution of their constitutive chemical elements. However, the considerable practical problems that are usually encountered when performing X-ray analysis on frozen samples include: a) the controlled deposition of a good quality carbon film to prevent charging, b) producing digital elemental distribution maps of ...

  5. X-rays detection system to obtain digital imagines for the study of artworks

    International Nuclear Information System (INIS)

    X-ray radiography plays an important role in the study of artworks. It particularly provides information on the origin, authenticity, painting technique, material conditions and its conservation history. This article describes a system based on semiconductor microstrip detector for obtaining X-ray images using the k-edge logarithmic substraction technique. The system has been characterized and the first images of its application for pigment detection are shown. (Author)

  6. Effects of Thermal Roughness on X-ray Studies of Liquid Surfaces

    OpenAIRE

    Pershan, Peter S.

    2000-01-01

    The effects of thermal roughness on X-ray studies of liquid surfaces will be discussed. In contrast to solid surfaces, for which the surface height–height correlation function remains finite at large distances, for liquid surfaces thermal fluctuations induce a logarithmic dependence for distances smaller than a gravitationally induced cutoff that is of the order of mm. As a result of this there is no true specular X-ray reflectivity liquid surfaces. Theory and measurements explaining this phe...

  7. X-Ray Photoemission Study of the Oxidation of Hafnium

    International Nuclear Information System (INIS)

    About 20 angstrom of hafnium were deposited on silicon substrates using the electron beam evaporation technique. Two types of samples were investigated. In one type, the substrate was kept at the ambient temperature. After the deposition, the substrate temperature was increased to 100, 200, and 300 degree C. In the other type, the substrate temperature was held fixed at some value during the deposition. For this type, the substrate temperatures used were 100, 200, 300, 400, 500, 550, and 600 degree C. The samples were characterized in situ by the technique of X-ray photoelectron spectroscopy. No trace of elemental hafnium is observed in the deposited overlayer. Also, there is no evidence of any chemical reactivity between the overlayer and the silicon substrate over the temperature range used. The hafnium overlayer shows a mixture of the dioxide and the suboxide. The ratio of the suboxide to dioxide is observed to be more in the first type of samples. The spectral data indicate that hafnium has a strong affinity for oxygen. The overlayer gets completely oxidized to form HfO2 at substrate temperature around 300 degree C for the first type of samples and at substrate temperature greater than 550 degree C for the second type

  8. High Time Resolution Studies of Binary X-Ray Pulsars

    Science.gov (United States)

    Cominsky, Lynn R.

    1996-05-01

    The work for this project was substantially more than anticipated, and involved recreating an analysis system for all the HEAO A-1 scanning data which had been converted to the ELE format. As a result of this work, a complete software analysis package was first created at Sonoma State University using Fortran, that can extract the data for any given X-ray source, and produce light curves from the scanning data. A second complete software analysis package was also created, this time in IDL, which can also display all the data in a timely manner, allowing data screening without the generation of hardcopy plots. The creation of the software systems was not the original goal of the project; rather this was a necessary result when the NRL computers became inoperable due to old age and could not be used to support the project, as originally planned. There were 6 sources originally proposed for analysis: SMC X-1, A0538-66, LMC X-1, LMC X-3, (these 3 sources are all located in the Large Magellanic Cloud region), 4UO115+63 and 4U1626-67. Results on these sources are summarized.

  9. X-Ray Photoemission Study of the Oxidation of Hafnium

    Directory of Open Access Journals (Sweden)

    A. R. Chourasia

    2009-01-01

    Full Text Available About 20 Å of hafnium were deposited on silicon substrates using the electron beam evaporation technique. Two types of samples were investigated. In one type, the substrate was kept at the ambient temperature. After the deposition, the substrate temperature was increased to 100, 200, and 300∘C. In the other type, the substrate temperature was held fixed at some value during the deposition. For this type, the substrate temperatures used were 100, 200, 300, 400, 500, 550, and 600∘C. The samples were characterized in situ by the technique of X-ray photoelectron spectroscopy. No trace of elemental hafnium is observed in the deposited overlayer. Also, there is no evidence of any chemical reactivity between the overlayer and the silicon substrate over the temperature range used. The hafnium overlayer shows a mixture of the dioxide and the suboxide. The ratio of the suboxide to dioxide is observed to be more in the first type of samples. The spectral data indicate that hafnium has a strong affinity for oxygen. The overlayer gets completely oxidized to form HfO2 at substrate temperature around 300∘C for the first type of samples and at substrate temperature greater than 550∘C for the second type.

  10. Microbial biofilm study by synchrotron X-ray microscopy

    Science.gov (United States)

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

    2015-11-01

    Microbial biofilm has already being used to remove metals and other pollutants from wastewater. In this sense, our proposal was to isolate and cultivate bacteria consortia from mangrove's sediment resistant to Zn (II) and Cu (II) at 50 mg L-1 and to observe, through synchrotron X-ray fluorescence microscopy (microXRF), whether the biofilm sequestered the metal. The biofilm area analyzed was 1 mm2 and a 2D map was generated (pixel size 20×20 μm2, counting time 5 s/point). The biofilm formation and retention followed the sequence Zn>Cu. Bacterial consortium zinc resistant formed dense biofilm and retained 63.83% of zinc, while the bacterial consortium copper resistant retained 3.21% of copper, with lower biofilm formation. Dehydrogenase activity of Zn resistant bacterial consortium was not negatively affect by 50 mg ml-1 zinc input, whereas copper resistant bacterial consortium showed a significant decrease on dehydrogenase activity (50 mg mL-1 of Cu input). In conclusion, biofilm may protect bacterial cells, acting as barrier against metal toxicity. The bacterial consortia Zn resistant, composed by Nitratireductor spp. and Pseudomonas spp formed dense biofilm and sequestered metal from water, decreasing the metal bioavailability. These bacterial consortia can be used in bioreactors and in bioremediation programs.

  11. Neutron and x-ray diffraction studies in cement

    International Nuclear Information System (INIS)

    Full text: Phase quantification of cement is difficult due to the complexity of phases, and cement composition is complicated by the polymorphic modifications of these phases. Only three of the seven polymorphs of the main component of cement, tricalcium silicate, have their structures fully determined, although more polymorphs are likely to be present There has been an increase in the use of Rietveld refinement for the analysis of cement in recent years, and an advantage of the method is the ability to define the tricalcium silicate form. It is usual to include a polymorph of tricalcium silicate in each of the three crystal systems encountered when beginning a refinement, and then exclude those not found. Care must be taken not to allow one crystal system to alter itself to compensate for another. Using synchrotron x-ray diffraction data, refinement of some atomic positions in a tricalcium silicate form resulted in a 24.5% improvement in the fits of the phase. An investigation using neutron data also showed significant improvement in the rb values for two polymorph of tricalcium silicate in a clinker sample, and also showed slight deviation in the phase quantification results obtained

  12. Small angle X-ray scattering studies to access the influence of bovine serum albumin (BSA) and carbonic anhydrase (Boca) on the size and interaction among Aerosol-O T reversed micelles as a function of the micellar hydration degree

    International Nuclear Information System (INIS)

    Full text: Reversed micelles (RMs) of AOT (sodium bis-2-ethylhexyl sulfosuccinate) has constitute an efficient system to investigate membrane interaction and physical chemical behavior of short biologically active peptides, proteins and enzymes in water controlled environment and apolar medium. Information may be obtained from protein-membrane interaction, including solubilization, binding location, conformational changes, activity size droplet-dependent, and changes in the properties of RM environment, useful in studies in biocatalysis and bioseparation systems [1]. In this work, changes in the structural features and interactive forces among AOT RMs in hexane were monitored in several stages of micellar hydration W (= [buffer]/[0.1M AOT]), and in the presence of BSA (66.5 kDa) and BCA (30 Kda), by SAXS. The interactive forces between the RMs with proteins were analyzed within the framework of repulsion and attractive interaction potentials through the pairing stick hardsphere (PSHS) model [2]. In this way, the spherical core radius to the system of pure AOT RMs at W = 4, 10, 20 and 30 were respectively 15, 22, 33 and 43 A (20% of polydispersity), evaluated from the particle form factor P(q) modeling [1]. The PSHS analysis from SAXS curves of AOT RMs with BSA and BCA at smaller droplets size of 4 and 10, showed, respectively, an interplay between attractive and repulsive interactions between the micelles (attractive component in S(q) was predominant) with the preservation of the discrete RM radius in the presence of protein. On the other hand, for protein confined in the bigger RM droplet size with W=30, the attractive inter micellar forces were of minor importance for BSA and the appearing of a predominant repulsive hard sphere component in SAXS curves accompanied by a decreasing of the micellar radius to 36 A were detected. For BCA, however, at higher W (30), a phase separation was observed probably associated to the formation of unstable large BCA aggregates

  13. Calibrated time-resolved transmission grating spectrometer for the study of ultrafast x-ray sources.

    Science.gov (United States)

    Pelletier, J F; Chaker, M; Kieffer, J C

    1996-01-01

    A transmission grating spectrometer has been coupled to a high-temporal-resolution soft x-ray streak camera for the study of picosecond laser-plasma x-ray sources. A procedure to deconvolve the overlapping contributions of diffraction orders and to calibrate the instrument has been established in order to obtain absolute time-resolved x-ray emission spectra in the 0.1-1.2 keV spectral region. The deconvolution and calibration techniques are presented along with measurements establishing the temporal resolution of this diagnostic at ~2 ps. Examples of calibrated spectra of laser-plasma x-ray sources created by 400 fs laser pulses at intensities of 1018 W/cm2 are also shown. PMID:21307534

  14. High-resolution x-ray studies of an AXAF high-energy transmission grating

    DEFF Research Database (Denmark)

    Abdali, S.; Christensen, Finn Erland; Schnopper, H. W.;

    1993-01-01

    A triple axis X-ray diffractometer, designed and built at the Danish Space Research Institute, was used to make a high resolution study of the performance of a 2000 angstroms period, high energy X-ray transmission grating developed at MIT for one of the grating spectrometers on the Advanced X......-ray Astrophysics Facility. Data was obtained at CuK(alpha )1 (8.048 keV) and, using single reflection asymmetric Si(044) crystals for both the monochromator and analyzer, an angular resolution of 1.5 arcsec FWHM was achieved. The efficiency of the grating in all orders up to the 15th was measured using a 12 k......W rotating anode X-ray generator. These data provided the basis for a modelling of the grating structure....

  15. Molecular orientation in soft matter thin films studied by resonant soft X-ray reflectivity

    Energy Technology Data Exchange (ETDEWEB)

    Mezger, Markus; Jerome, Blandine; Kortright, Jeffrey B.; Valvidares, Manuel; Gullikson, Eric; Giglia, Angelo; Mahne, Nicola; Nannarone, Stefano

    2011-01-12

    We present a technique to study depth profiles of molecular orientation in soft matter thin films with nanometer resolution. The method is based on dichroism in resonant soft X-ray reflectivity using linear s- and p-polarization. It combines the chemical sensitivity of Near-Edge X-ray Absorption Fine Structure spectroscopy to specific molecular bonds and their orientation relative to the polarization of the incident beam with the precise depth profiling capability of X-ray reflectivity. We demonstrate these capabilities on side chain liquid crystalline polymer thin films with soft X-ray reflectivity data at the carbon K edge. Optical constants of the anisotropic refractive index ellipsoid were obtained from a quantitative analysis using the Berreman formalism. For films up to 50 nm thickness we find that the degree of orientation of the long axis exhibits no depth variation and isindependent of the film thickness.

  16. The characterization of oil-soluble calcium carbonate dispersions using Small-Angle X-ray Scattering (SAXS) and Small-Angle Neutron Scattering (SANS)

    International Nuclear Information System (INIS)

    Calcium carbonate dispersions stabilized by an adsorbed surfactant layer are used to regulate the acidity of lubricating oils for internal combustion engines. Three typical commercial samples have been examined using a combination of X-ray and neutron scattering techniques. The solid active material was extracted from the samples and redispersed in heptane and mixtures of toluene and toluene-d8 and n-octane and n-octane-d18. The results were in broad agreement with the core/shell model. The core radius was obtained from SAXS data. The total particle radius (∝20-50A) and hence the shell thickness were obtained by model fitting to the deuterated-solvent and 65% deuterated solvent SANS data with the core radius from the X-ray data. In determining the best fit, the core density, amount of solvent in the shell and polydispersity were also adjusted to give fits with a shell-to-core-volume ratio and a volume fraction that agreed with the expected values. The SANS data were weaker than expected assuming a simple monodisperse core/shell model with a calcite core. This is consistent with the observed polydispersity and in addition implies diffuse boundaries. Although WAXS (wide-angle X-ray scattering) confirmed that the cores were non-crystalline the best model fits were obtained with a core scattering density not much less than that calculated for calcite. The absolute intensities suggested that some solvent was incorporated into the shells of all the samples and one sample showed a preference for uptake of octane as compared to toluene. (orig./GSCH)

  17. The X-Ray Zurich Environmental Study (X-ZENS). II. X-ray Observations of the Diffuse Intragroup Medium in Galaxy Groups

    CERN Document Server

    Miniati, Francesco; Silverman, John D; Carollo, Marcella; Cibinel, Anna; Lilly, Simon J; Schawinski, Kevin

    2014-01-01

    We present the results of a pilot XMM-$Newton$ and $Chandra$ program aimed at studying the diffuse intragroup medium (DIM) of optically-selected nearby groups from the Zurinch ENvironmental Study (ZENS) catalog. The groups are in a narrow mass range about $10^{13}M_\\odot$, a mass scale at which the interplay between the DIM and the group member galaxies is still largely unprobed. X-ray emission from the DIM is detected in the energy band 0.5--2 keV with flux $\\le 10^{-14}$ erg cm$^{-1}$ s$^{-1}$, which is one order of magnitude fainter than for typical ROSAT groups (RASS). For many groups we set upper limits to the X-ray luminosity, indicating that the detections are likely probing the upper envelope of the X-ray emitting groups. We find evidence for our optically selected groups to be under-luminous with respect to predictions from X-ray scaling relations. X-ray mass determinations are in best agreement with those based on the member galaxies bulge luminosity, followed by their total optical luminosity and v...

  18. Phase Sensitive X-Ray Diffraction Imaging Study of Protein Crystals

    Science.gov (United States)

    Hu, Z. W.

    2003-01-01

    The study of defects and growth of protein crystals is of importance in providing a fundamental understanding of this important category of systems and the rationale for crystallization of better ordered crystals for structural determination and drug design. Yet, as a result of the extremely weak scattering power of x-rays in protein and other biological macromolecular crystals, the extinction lengths for those crystals are extremely large and, roughly speaking, of the order of millimeters on average compared to the scale of micrometers for most small molecular crystals. This has significant implication for x-ray diffraction and imaging study of protein crystals, and presents an interesting challenge to currently available x-ray analytical techniques. We proposed that coherence-based phase sensitive x-ray diffraction imaging could provide a way to augment defect contrast in x-ray diffraction images of weakly diffracting biological macromolecular crystals. I shall examine the principles and ideas behind this approach and compare it to other available x-ray topography and diffraction methods. I shall then present some recent experimental results in two model protein systems-cubic apofemtin and tetragonal lysozyme crystals to demonstrate the capability of the coherence-based imaging method in mapping point defects, dislocations, and the degree of perfection of biological macromolecular crystals with extreme sensitivity. While further work is under way, it is intended to show that the observed new features have yielded important information on protein crystal perfection and nucleation and growth mechanism otherwise unobtainable.

  19. 3D contrast-enhanced MR portography and direct X-ray portography: a correlation study

    International Nuclear Information System (INIS)

    Objective: To evaluate the accuracy of 3D contrast-enhanced MR portography (3D CEMRP) by correlating with direct X-ray portography. Methods: Twenty-six patients underwent 3D CEMRP study. The findings of 3D CEMRP including the patency of the portal vein and its intrahepatic left and right branches, as well as collaterals were evaluated and compared with those from direct x-ray portography. Causes of disagreement between the two methods were analyzed. Results: The main portal vein appearance was accordant with 3D CEMRP and direct x-ray portography in all cases. For intrahepatic portal veins, the results agreed in 21 patients but disagreed in 5. In one patient with a huge tumor in right liver, the right posterior portal vein was classified as occluded at 3D CEMRP, but displaced and diffusely narrowed at direct x-ray portography. The findings of left intrahepatic portal vein were discordant in three patients with hepatocelluar carcinoma in the left lobe. 3D CE MRP demonstrated complete occlusion of the left portal veins, whereas direct x-ray portography showed proximal narrowing and distal occlusion. In another patient with hepatocelluar carcinoma, a small non-occlusive thrombus involving the sagittal segment of the left portal vein was seen on MRP but not on direct x-ray portography. With demonstration of portosystemic collaterals, 3D CEMRP showed results similar to those of X-ray portography, except one recanalized para-umbilical vein was excluded from the limited scan coverage. Conclusion: 3D CE MRP correlated well with direct x-ray portography in most cases. Compared with direct portography, 3D CEMRP had limitation in distinguishing narrowing of an intrahepatic portal vein from occlusion. But it showed advantage in demonstrating small thrombus within portal vein. (authors)

  20. Solar flares with similar soft but different hard X-ray emissions: case and statistical studies

    Science.gov (United States)

    Sharykin, Ivan N.; Struminsky, Alexei B.; Zimovets, Ivan V.; Gan, Wei-Qun

    2016-01-01

    From the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI) catalog we select events which have approximately the same GOES class (high C - low M or 500-1200 counts s-1 within the RHESSI 6-12 keV energy band), but with different maximal energies of detected hard X-rays. The selected events are subdivided into two groups: (1) flares with X-ray emissions observed by RHESSI up to only 50 keV and (2) flares with hard X-ray emission observed also above 50 keV. The main task is to understand observational peculiarities of these two flare groups. We use RHESSI X-ray data to obtain spectral and spatial information in order to find differences between selected groups. Spectra and images are analyzed in detail for six events (case study). For a larger number of samples (85 and 28 flares in the low-energy and high-energy groups respectively) we only make some generalizations. In spectral analysis we use the thick-target model for hard X-ray emission and one temperature assumption for thermal soft X-ray emission. RHESSI X-ray images are used for determination of flare region sizes. Although thermal and spatial properties of these two groups of flares are not easily distinguishable, power law indices of hard X-rays show significant differences. Events from the high-energy group generally have a harder spectrum. Therefore, the efficiency of chromospheric evaporation is not sensitive to the hardness of nonthermal electron spectra but rather depends on the total energy flux of nonthermal electrons.