WorldWideScience

Sample records for angle x-ray studies

  1. Glancing angle x-ray studies of oxide films

    International Nuclear Information System (INIS)

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

    1989-01-01

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

  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)

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

    2011-01-01

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

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

    International Nuclear Information System (INIS)

    Zipper, P.; Durchschlag, H.

    1980-01-01

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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  6. 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.

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

    Science.gov (United States)

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

    2017-11-01

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

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

    International Nuclear Information System (INIS)

    Ogawa, Hiroki; Kanaya, Toshiji

    2011-01-01

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

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

    Science.gov (United States)

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

    2017-11-01

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

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

    Science.gov (United States)

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

    1987-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    Science.gov (United States)

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

    2005-09-01

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

  13. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Jensen, K F

    1983-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    Science.gov (United States)

    Reconditi, Massimo

    2006-10-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-10-15

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

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

    International Nuclear Information System (INIS)

    Pinto, Nivia G. Villela; Barroso, Regina C.; Mota, Carla L.S.; Almeida, Andre P.; Azeredo, Soraia R.; Braz, Delson

    2009-01-01

    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. 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)

  20. 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...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-04-01

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

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

    DEFF Research Database (Denmark)

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

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Pople, John A

    2001-03-29

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-01

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

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

    Science.gov (United States)

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

    2010-10-01

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

  6. 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..

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

    Science.gov (United States)

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

    2015-09-21

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-01-01

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

  9. X-ray diffraction study with small- and wide-angle simultaneous measurement of polymorphic crystallization of triacylglycerols

    Energy Technology Data Exchange (ETDEWEB)

    Ueno, Satoru [Hiroshima Univ., Faculty of Applied Biological Science, Higashi-Hiroshima, Hiroshima (Japan)

    2002-01-01

    Polymorphism of triacylglycerols (TAGs) is an important phenomenon which influences the physical chemical properties of fats employed in foods, pharmaceuticals, cosmetics etc. In particular, precise analysis of kinetic properties of polymorphic crystallization is closely related to technical control of fat crystallization in confectionery and food industry. In the melt-mediated crystallization, which is one of the typical methods of crystallizing the more stable form for industrial use, the more stable form is induced by rapidly melting the less stable forms. Recently, X-ray diffraction spectroscopy using a synchrotron radiation source has been used in study of dynamic processes of polymorphic transformations of many TAGs. This approach has allowed us to gain a better understanding of the kinetics of processes occurring during the polymorphic crystallization and transformations of TAGs at the molecular level. In the present study, polymorphic crystallization of TAG has been examined with the time-resolved X-ray diffraction method with small- and wide-angle simultaneous measurement using synchrotron radiation. The main result is as follows: the melt mediation gave rise to the formation of a liquid crystalline structure having long spacing values of 5.1 nm and 4.6 nm in SOS (sn-1,3-distearoyl-2-oleoyl glycerol). Consequently, the use of the time-resolved X-ray diffraction method with small- and wide-angle simultaneous measurement using synchrotron radiation unveiled quite newer aspects of the polymorphic crystallization of the triacylglycerols from neat liquid, which were not detectable in conventional XRD techniques. (author)

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

    CERN Document Server

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

    2002-01-01

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

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

    International Nuclear Information System (INIS)

    Ohnuma, Masato; Suzuki, Jun-ichi

    2006-01-01

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

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

    Science.gov (United States)

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

    2010-02-23

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

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

    DEFF Research Database (Denmark)

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

    2001-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  15. Time-Resolving Study of Stress-Induced Transformations of Isotactic Polypropylene through Wide Angle X-ray Scattering Measurements

    Directory of Open Access Journals (Sweden)

    Finizia Auriemma

    2018-02-01

    Full Text Available The development of a highly oriented fiber morphology by effect of tensile deformation of stereodefective isotactic polypropylene (iPP samples, starting from the unoriented γ form, is studied by following the transformation in real time during stretching through wide angle X-ray scattering (WAXS measurements. In the stretching process, after yielding, the initial γ form transforms into the mesomorphic form of iPP through mechanical melting and re-crystallization. The analysis of the scattering invariant measured in the WAXS region highlights that the size of the mesomorphic domains included in the well oriented fiber morphology obtained at high deformations increases through a process which involves the coalescence of the small fragments formed by effect of tensile stress during lamellar destruction with the domain of higher dimensions.

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

    Science.gov (United States)

    Pillon, Monica C; Guarné, Alba

    2017-11-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  18. Glancing angle synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Cernik, R.J.

    1996-01-01

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

  19. 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.

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

    International Nuclear Information System (INIS)

    Vollet, D.

    1983-01-01

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

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

    Science.gov (United States)

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

    2014-12-01

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

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

    Science.gov (United States)

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

    2014-04-01

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

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

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

    International Nuclear Information System (INIS)

    Itri, R.

    1986-01-01

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

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

    Science.gov (United States)

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

    2017-05-01

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

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

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

    DEFF Research Database (Denmark)

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

    2003-01-01

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

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

    CSIR Research Space (South Africa)

    Bandyopadhyay, J

    2012-04-01

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

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

    Science.gov (United States)

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

    2017-05-01

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

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

    DEFF Research Database (Denmark)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

    Babilas, Rafał; Hawełek, Łukasz; Burian, Andrzej

    2014-01-01

    The local atomic structure of the Fe 80 B 20 , Fe 70 Nb 10 B 20 and Fe 62 Nb 8 B 30 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 Fe 3 B, Fe 23 B 6 and bcc Fe structures are also discussed. - Graphical abstract: Pair distribution functions (a) and best-fit model and experimental radial distribution functions for Fe 80 B 20 (b), Fe 70 Nb 10 B 20 (c) and Fe 62 Nb 8 B 30 (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

  12. Combined angle-resolved X-ray photoelectron spectroscopy, density functional theory and kinetic study of nitridation of gallium arsenide

    Science.gov (United States)

    Mehdi, H.; Monier, G.; Hoggan, P. E.; Bideux, L.; Robert-Goumet, C.; Dubrovskii, V. G.

    2018-01-01

    The high density of interface and surface states that cause the strong Fermi pinning observed on GaAs surfaces can be reduced by depositing GaN ultra-thin films on GaAs. To further improve this passivation, it is necessary to investigate the nitridation phenomena by identifying the distinct steps occurring during the process and to understand and quantify the growth kinetics of GaAs nitridation under different conditions. Nitridation of the cleaned GaAs substrate was performed using N2 plasma source. Two approaches have been combined. Firstly, an AR-XPS (Angle Resolved X-ray Photoelectron Spectroscopy) study is carried out to determine the chemical environments of the Ga, As and N atoms and the composition depth profile of the GaN thin film which allow us to summarize the nitridation process in three steps. Moreover, the temperature and time treatment have been investigated and show a significant impact on the formation of the GaN layer. The second approach is a refined growth kinetic model which better describes the GaN growth as a function of the nitridation time. This model clarifies the exchange mechanism of arsenic with nitrogen atoms at the GaN/GaAs interface and the phenomenon of quasi-saturation of the process observed experimentally.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-10-01

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

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

    Science.gov (United States)

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

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

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

    Science.gov (United States)

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

    2014-07-24

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

  16. Large Solid Angle Spectrometer for Inelastic X-ray Scattering

    International Nuclear Information System (INIS)

    Gelebart, F.; Morand, M.; Dermigny, Q.; Giura, P.; Shukla, A.; Rueff, J.-P.

    2007-01-01

    We have designed a large solid angle spectrometer mostly devoted to inelastic x-ray scattering (IXS) studies of materials under extreme conditions (high pressure / temperature) in the hard x-ray range. The new IXS spectrometer is designed to optimize the photon throughput while preserving an excellent resolving power of ∼10000 in the considered energy range. The spectrometer consists of an array of up to 4 spherically bent 0.5 m radius analyzer crystals and a solid-state detector positioned on the Rowland circle. The four analyzers can cover a solid angle more than one order of magnitude larger than conventional spectrometers. The spectrometer is to be installed on the GALAXIES beamline at SOLEIL in the near future

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    International Nuclear Information System (INIS)

    Mayolo, C.M.G. de.

    1991-01-01

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

  19. 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.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Science.gov (United States)

    de la Venta, J; Bouzas, V; Pucci, A; Laguna-Marco, M A; Haskel, D; te Velthuis, S G E; Hoffmann, A; Lal, J; Bleuel, M; Ruggeri, G; de Julián Fernández, C; García, M A

    2009-11-01

    X-ray magnetic circular dichroism (XMCD) and Small Angle Neutron Scattering (SANS) measurements were performed on thiol capped Au nanoparticles (NPs) embedded into polyethylene. An XMCD signal of 0.8 x 10(-4) was found at the Au L3 edge of thiol capped Au NPs embedded in a polyethylene matrix for which Superconducting Quantum Interference Device (SQUID) magnetometry yielded a saturation magnetization, M(S), of 0.06 emu/g(Au). SANS measurements showed that the 3.2 nm average-diameter nanoparticles are 28% polydispersed, but no detectable SANS magnetic signal was found with the resolution and sensitivity accessible with the neutron experiment. A comparison with previous experiments carried out on Au NPs and multilayers, yield to different values between XMCD signals and magnetization measured by SQUID magnetometer. We discuss the origin of those differences.

  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. 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.

  4. 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.

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

    Indian Academy of Sciences (India)

    2015-11-27

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

  6. Static X-ray diffraction study of cerium: The standard approach and the magic-angle approach

    International Nuclear Information System (INIS)

    Chesnut, Gary N.; Streetman, Becky D.; Schiferl, David; Anderson, William W.; Nicol, Malcolm; Meng Yue

    2004-01-01

    Cerium, a member of the rare earth metals, has been studied up to 300 kilobars in a diamond-anvil cell using energy- and angular-dispersive x-ray diffraction with a synchrotron source. The purpose of this experiment was to examine the electronic and structural behavior of cerium and to examine the effects of deviatoric stress due to non-hydrostatic conditions within the sample environment. Using the standard sample orientation and data from various orientations, the effects of deviatoric stress are shown

  7. Low angle X-ray scattering

    International Nuclear Information System (INIS)

    Torrianni, I.L.

    1983-01-01

    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.) [pt

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

    Directory of Open Access Journals (Sweden)

    Takatsugu Endo

    2017-01-01

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

  9. 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

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

    Directory of Open Access Journals (Sweden)

    Emanuela Di Cola

    2016-03-01

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

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

    Science.gov (United States)

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

    2016-03-28

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

  12. Raman and Wide Angle X-Ray Studies on Polystyrene-Block Polyisoprene-Block Polystyrene - Graphene Nanocomposites

    Science.gov (United States)

    Chipara, Dorina; Guerrero, Oscar M.; Gonzalez, Alejandra; Yust, Brian; Elamin, Ibrahim; Hinthorne, James; Chipara, Mircea

    2015-03-01

    Nanocomposites have been obtained by loading a block copolymer Polystyrene-Block Polyisoprene-Block Polystyrene (PS-bPI-bPS), containing 17% styrene (purchased from Sigma Aldrich) with various amounts of graphene nano platelets (HD Plas Grade 4), purchased from Cheap Tubes Inc., through the solution path: PS-bPI-bPS was dissolved within cyclohexane, then nanofiller was added and the mixture was sonicated for 1 h. The high power sonication (500 mW) improved the dispersion of the filler within the polymeric matrix. The homogenized solution was poured on glass slides covered by aluminum foil and left to evaporate the solvent. A final thermal treatment of the as obtained nanocomposites at 75 °C, has been performed overnight, in an oven. Nanocomposites containing various weight fraction of fillers ranging between 0% and 40% have been obtained. The as obtained films have been investigated by Wide Angle X-Ray Scattering, using a Bruker Discovery 8 spectrometer, FTIR (Bruker Tensor 27), UV-Vis, and Raman spectroscopy, (using a Bruker Senterra, confocal Raman microscope operating at 785 nm). The dependence of these spectra originating from the polymeric matrix and from the filler on the loading with graphene is discussed.

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

    Czech Academy of Sciences Publication Activity Database

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2018-04-11

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

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

    Science.gov (United States)

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

    2017-10-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1986-05-15

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

  17. C60-propylamine adduct monolayers at the gas/water interface: A Brewster angle microscopy and x-ray scattering study

    International Nuclear Information System (INIS)

    Fukuto, M.; Penanen, K.; Heilmann, R.K.; Pershan, P.S.; Vaknin, D.

    1997-01-01

    Brewster angle microscopy (BAM), x-ray specular reflectivity and grazing-incidence x-ray diffraction (GID) studies of C 60 -propylamine adduct monolayers at the gas/water interface as a function of molecular area are reported. At large molecular areas (A>∼150 Angstrom 2 /molecule), BAM images reveal macroscopic heterogeneity in the film, consisting of the coexistence between regions covered with uniform solidlike monolayer and bare water surface. After compression to a limiting molecular area of 150 Angstrom 2 /molecule, the film is observed to be homogeneous, with the uniform monolayer covering the entire available surface. Both the x-ray reflectivity results and the GID patterns are consistent with the formation of a uniform monolayer at A∼150 Angstrom 2 /molecule, while the little dependence that the GID patterns have on the molecular area for A>∼150 Angstrom 2 /molecule is consistent with the heterogeneity in the film. Upon further compression to higher densities (A 2 /molecule), the x-ray reflectivity results suggest the formation of a partial layer either at the molecule/gas interface or at the molecule/water interface. In this high density regime, the shift in the observed GID pattern with molecular area is much smaller than would be expected if the film were to remain a homogeneous monolayer, also consistent with the formation of an inhomogeneous partial layer. The analysis of the broad GID pattern observed from a uniform monolayer in terms of a model 2D radial distribution function, implies a short range positional correlation, extending to only a few molecular distances. The average nearest neighbor distance (d∼13 Angstrom), extracted from the GID analysis, is consistent with the limiting molecular area (A∼150 Angstrom 2 /molecule) assuming local hexagonal packing. (Abstract Truncated)

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

    Directory of Open Access Journals (Sweden)

    Emmanuel Kentzinger

    2016-03-01

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

  19. Small angle x-ray scattering and its applications

    International Nuclear Information System (INIS)

    Buckely, C.E.

    2002-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Markus Beckers

    2017-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-02-15

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

  3. 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...... 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...

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    International Nuclear Information System (INIS)

    Thomson, T.

    2005-01-01

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

  6. Low angle X-ray scattering in biological tissues

    Energy Technology Data Exchange (ETDEWEB)

    Lemos, Carla; Braz, Delson; Pinto, Nivia G.V.; Lima, Joao C.; Castro, Carlos R.F.; Filgueiras, R.A.; Mendonca, Leonardo; Lopes, Ricardo T. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE). Lab. de Instrumentacao Nuclear]. E-mail: delson@lin.ufrj.br; Barroso, Regina C. [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Inst. de Fisica]. E-mail: cely@uerj.br

    2007-07-01

    Low-angle x-ray scatter (LAXS) for tissue characterization is based on the differences which result from the interference of photons coherently scattered from molecules of each sample. Biological samples (bone, blood and blood components) have been studied in recent years in our laboratory using powder diffractometer. The scattering information was obtained using a Shimadzu DRX 6000 diffractometer at the Nuclear Instrumentation Laboratory, Rio de Janeiro, Brazil. Unpolarized monoenergetic K{alpha} radiation from Cu provided 8.04 keV photons. The measurements were made in reflection mode ({theta}-2{theta} geometry), with the sample stationary on a goniometer which rotates the sample and detector about an axis lying in the plane of the top of the sample holder. LAXS profiles from whole blood, plasma and formed elements were measured to investigate the nature of scattering from such lyophilized samples. The statistical analysis shows that the variation found for the characterization parameters is significant for whole blood considering the age. Gender was positively associated with the variation of the second peak position for the profiles obtained for formed elements. The correlation of the measured relative coherent intensity with the mineral content in the bone samples was investigated. These results suggest that the measurement of bone mineral content within trabecular bone can be performed by using quantitative coherent scattering information. (author)

  7. Determining the orientation angle of directional leads for deep brain stimulation using computed tomography and digital x-ray imaging: A phantom study.

    Science.gov (United States)

    Sitz, Alexander; Hoevels, Mauritius; Hellerbach, Alexandra; Gierich, Andreas; Luyken, Klaus; Dembek, Till A; Klehr, Martin; Wirths, Jochen; Visser-Vandewalle, Veerle; Treuer, Harald

    2017-09-01

    Orientating the angle of directional leads for deep brain stimulation (DBS) in an axial plane introduces a new degree of freedom that is indicated by embedded anisotropic directional markers. Our aim was to develop algorithms to determine lead orientation angles from computed tomography (CT) and stereotactic x-ray imaging using standard clinical protocols, and subsequently assess the accuracy of both methods. In CT the anisotropic marker artifact was taken as a signature of the lead orientation angle and analyzed using discrete Fourier transform of circular intensity profiles. The orientation angle was determined from phase angles at a frequency 2/360° and corrected for aberrations at oblique leads. In x-ray imaging, frontal and lateral images were registered to stereotactic space and sub-images containing directional markers were extracted. These images were compared with projection images of an identically located virtual marker at different orientation angles. A similarity index was calculated and used to determine the lead orientation angle. Both methods were tested using epoxy phantoms containing directional leads (Cartesia™, Boston Scientific, Marlborough, USA) with known orientation. Anthropomorphic phantoms were used to compare both methods for DBS cases. Mean deviation between CT and x-ray was 1.5° ± 3.6° (range: -2.3° to 7.9°) for epoxy phantoms and 3.6° ± 7.1° (range: -5.6° to 14.6°) for anthropomorphic phantoms. After correction for imperfections in the epoxy phantoms, the mean deviation from ground truth was 0.0° ± 5.0° (range: -12° to 14°) for x-ray. For CT the results depended on the polar angle of the lead in the scanner. Mean deviation was -0.3° ± 1.9° (range: -4.6° to 6.6°) or 1.6° ± 8.9° (range: -23° to 34°) for polar angles ≤ 40° or > 40°. The results show that both imaging modalities can be used to determine lead orientation angles with high accuracy. CT is superior to x-ray imaging, but oblique leads (polar

  8. Depth profiling study of in situ CdCl{sub 2} treated CdTe/CdS heterostructure with glancing angle incidence X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Vamsi Krishna, K.; Dutta, V

    2004-03-01

    CdTe thin films have been deposited using spray pyrolysis technique without and with in situ CdCl{sub 2} treatment. Scanning electron microscopy studies show enhanced grain growth in the presence of CdCl{sub 2}. Glancing angle incidence X-ray diffraction is used for the micro structural study of polycrystalline CdS/CdTe heterostructure at different depths by changing the incident angle. Spraying of CdCl{sub 2} on CdS prior to CdTe deposition promotes S diffusion throughout CdTe film and also Te diffusion into CdS. Whereas spraying of CdCl{sub 2} in between CdTe deposition prevents S diffusion partially and Te diffusion completely. There is an associated change in the microstress of the CdTe film at different layers. The films without CdCl{sub 2} treatment show compressive microstress varying from -98 to -158 MPa with increasing incident angle. CdCl{sub 2} spray during CdTe deposition shows compressive microstress, which varies from -98 MPa at the interface to -19 MPa near the surface and CdCl{sub 2} spray prior to CdTe deposition leads to a mildly tensile stress, from +40 to +20 MPa, which is very close to the standard shear stress of {approx}10 MPa for CdTe.

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

    Indian Academy of Sciences (India)

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

  10. Surface oxidation of a Melinex 800 PET polymer material modified by an atmospheric dielectric barrier discharge studied using X-ray photoelectron spectroscopy and contact angle measurement

    International Nuclear Information System (INIS)

    Cui Naiyi; Upadhyay, Deepesh J.; Anderson, Colin A.; Meenan, Brian J.; Brown, Norman M.D.

    2007-01-01

    Surface properties of a Melinex 800 PET polymer material modified by an atmospheric-pressure air dielectric barrier discharge (DBD) have been studied using X-ray photoelectron microscopy (XPS) and contact angle measurement. The results show that the material surface treated by the DBD was modified significantly in chemical composition, with the highly oxidised carbon species increasing as the surface processing proceeds. The surface hydrophilicity was dramatically improved after the treatment, with the surface contact angle reduced from 81.8 o for the as-supplied sample to lower than 50 deg. after treatment. Post-treatment recovery effect is found after the treated samples were stored in air for a long period of time, with the ultimate contact angles, as measured, being stabilised in the range 58-69 deg. after the storage, varying with the DBD-treatment power density. A great amount of the C-O type bonding formed during the DBD treatment was found to be converted into the C=O type during post-treatment storage. A possible mechanism for this bond conversion has been suggested

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

    International Nuclear Information System (INIS)

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

    1989-01-01

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

  12. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-03-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-04-16

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

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

    DEFF Research Database (Denmark)

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

    2012-01-01

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

  16. 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.

  17. 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.

  18. Low-angle X-ray scattering from spices

    International Nuclear Information System (INIS)

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

    2002-01-01

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

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

    International Nuclear Information System (INIS)

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

    1978-01-01

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

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

    Science.gov (United States)

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

    2015-03-01

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

  1. Microstructural parameters in 8 MeV Electron irradiated Bombyx mori silk fibers by wide-angle X-ray scattering studies (WAXS)

    International Nuclear Information System (INIS)

    Halabhavi, Sangappa

    2009-01-01

    The present work looks into the microstructural modification in Bombyx mori silk fibers, induced by electron irradiation. The irradiation process was performed in air at room temperature by use of 8 MeV electron accelerators at different doses: 0, 25, 50, 75 and 100 kGy respectively. Irradiation of polymer can be used to crosslink or degrade the desired component or to fixate the polymer morphology. The changes in microstructural parameters in these natural polymer fibers have been studied using wide angle X-ray scattering (WAXS) method. The crystal imperfection parameters such as crystallite size , lattice strain (g in %) and enthalpy (a * ) have been determined by line profile analysis (LPA) using Fourier method of Warren. Exponential, Lognormal and Reinhold functions for the column length distributions have been used for the determination of these parameters. The goodness of the fit and the consistency of these results suggest that the exponential distribution gives much better results, even though lognormal distribution has been widely used to estimate the similar stacking faults in metal oxide compounds. (author)

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

    DEFF Research Database (Denmark)

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

    2000-01-01

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

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

    Science.gov (United States)

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

    2016-03-01

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

  4. Wide-Angle X-ray Scattering Study on Shear-Induced Crystallization of Propylene-1-Butylene Random Copolymer: Experiment and Diffraction Pattern Simulation

    Energy Technology Data Exchange (ETDEWEB)

    Y Mao; C Burger; F Zuo; B Hsiao; A Mehta; C Mitchell; A Tsou

    2011-12-31

    Shear-induced crystallization of a propylene-1-butylene random copolymer with low butylene content (5.7 mol %) was studied using time-resolved wide-angle X-ray scattering (WAXS) techniques. Polymorphism, preferred crystal orientation, crystallization kinetics, and disorder effect were investigated based on WAXS 2D whole pattern analysis. It was found that at 100 C, the crystallite of P-B copolymer was a mixture of 80% {gamma}-form and 20% {alpha}-form of isotactic polypropylene (iPP) crystals. The application of a step shear (shear rate = 100 s{sup -1}, shear duration =3s) induced {gamma}-form crystals with c-axis oriented perpendicular to the shear direction. In contrast, the c-axis of {alpha}-form crystals was normally in parallel to the shear direction. Both crystallization kinetics and crystallinity were greatly enhanced by shear. The disorder effect was found to play an important role in the crystallization behavior of P-B copolymer. In the early stage crystallization, the chosen copolymer contained a large amount of structure defects, where crystals became more ordered upon annealing. The degree of crystal orientation was also found to decrease during crystallization due to the relaxation after shear.

  5. A portable extruder for in situ wide angle x-ray scattering study on multi-dimensional flow field induced crystallization of polymer

    Science.gov (United States)

    Chang, Jiarui; Wang, Zhen; Tang, Xiaoliang; Tian, Fucheng; Ye, Ke; Li, Liangbin

    2018-02-01

    We have designed and constructed a portable extruder with a rotatable mandrel, which can be employed to study the multi-dimensional flow field (MDFF) induced crystallization of polymer combined with in situ wide angle x-ray scattering (WAXS). With the piston driving the melt sample to flow along the channel, a direct axial shear field is achieved. At the same time, the central mandrel keeps rotating under a stable speed, providing the sample with an additional circumferential shear field. By presetting different proportions of the two shear fields, namely, axial and circumferential, various flow states of the sample can be obtained, which makes it capable of investigating the effects of MDFF on polymer crystallization. We have performed an in situ WAXS experiment of MDFF induced crystallization of isotactic polypropylene based on the portable extruder at the beam line BL16B in Shanghai Synchrotron Radiation Facility. The rheological and structural information is collected simultaneously, which manifests the viability of the portable extruder on regulating MDFF and can provide guidance for polymer processing.

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

    Indian Academy of Sciences (India)

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

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

    Indian Academy of Sciences (India)

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

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

    Indian Academy of Sciences (India)

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

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

    African Journals Online (AJOL)

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

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

    Indian Academy of Sciences (India)

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

  11. Radiobiological studies using gamma and x rays.

    Energy Technology Data Exchange (ETDEWEB)

    Potter, Charles Augustus; Longley, Susan W.; Scott, Bobby R.; Lin, Yong; Wilder, Julie; Hutt, Julie A.; Padilla, Mabel T.; Gott, Katherine M.

    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.

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

    DEFF Research Database (Denmark)

    Yennawar, Hemant; Møller, Magda; Gillilan, Richard

    2011-01-01

    The X-ray crystal structure of sheep liver sorbitol dehydrogenase (slSDH) has been determined using the crystal structure of human sorbitol dehydrogenase (hSDH) as a molecular-replacement model. slSDH crystallized in space group I222 with one monomer in the asymmetric unit. A conserved tetramer...... the substrate-binding pocket together with the acetate designed by nature to fit large polyol substrates. The substrate-binding pocket is seen to be in close proximity to the tetramer interface, which explains the need for the structural integrity of the tetramer for enzyme activity. Small-angle X-ray...

  13. X-ray small angle scattering of polymer solutions

    International Nuclear Information System (INIS)

    Koyama, Ryuzo

    1975-01-01

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

  14. Reflection of X-rays from a rough surface at extremely small grazing angles.

    Science.gov (United States)

    Wen, Mingwu; Kozhevnikov, Igor V; Wang, Zhanshan

    2015-09-21

    Peculiarities of X-ray diffraction from a rough surface at an extremely small grazing angle of an incident beam are theoretically studied. The interrelation of four diffraction channels (coherent reflectance, coherent transmittance, diffuse scattering in vacuum, and scattering into the matter depth) is analyzed for different limiting cases (large and small correlation length of roughness and large and extremely small grazing angle of incident radiation). Both the Debye-Waller and the Nevot-Croce factors are demonstrated to describe improperly the features of X-ray diffraction at extremely small grazing angles. More appropriate simple analytic expressions for the specular reflectivity and total integrated scattering in vacuum are obtained instead. Transformation of one limiting diffraction regime into another one with variation in the correlation length of roughness is discussed.

  15. Microstructural Parameters in 8 MeV Electron-Irradiated BOMBYX MORI Silk Fibers by Wide-ANGLE X-Ray Scattering Studies (waxs)

    Science.gov (United States)

    Sangappa, Asha, S.; Sanjeev, Ganesh; Subramanya, G.; Parameswara, P.; Somashekar, R.

    2010-01-01

    The present work looks into the microstructural modification in electron irradiated Bombyx mori P31 silk fibers. The irradiation process was performed in air at room temperature using 8 MeV electron accelerator at different doses: 0, 25, 50 and 100 kGy. Irradiation of polymer is used to cross-link or degrade the desired component or to fix the polymer morphology. The changes in microstructural parameters in these natural polymer fibers have been computed using wide angle X-ray scattering (WAXS) data and employing line profile analysis (LPA) using Fourier transform technique of Warren. Exponential, Lognormal and Reinhold functions for the column length distributions have been used for the determination of crystal size, lattice strain and enthalpy parameters.

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

    DEFF Research Database (Denmark)

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

    2002-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-12-21

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

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

    Science.gov (United States)

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

    2011-12-16

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

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

    Science.gov (United States)

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

    2011-01-01

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

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

    Science.gov (United States)

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

    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 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 (X-ray CT means that doses that biological samples receive are likely to increase and thus should be closely monitored. PMID:23840640

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

    Directory of Open Access Journals (Sweden)

    Matthias Schwartzkopf

    2016-12-01

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

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    Science.gov (United States)

    Long, Gabrielle; Levine, Lyle

    1997-03-01

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

  4. Picosecond x-ray streak camera studies

    International Nuclear Information System (INIS)

    Kasyanov, Yu.S.; Malyutin, A.A.; Richardson, M.C.; Chevokin, V.K.

    1975-01-01

    Some initial results of direct measurement of picosecond x-ray emission from laser-produced plasmas are presented. A PIM-UMI 93 image converter tube, incorporating an x-ray sensitive photocathode, linear deflection, and three stages of image amplification was used to analyse the x-ray radiation emanating from plasmas produced from solid Ti targets by single high-intensity picosecond laser pulses. From such plasmas, the x-ray emission typically persisted for times of 60psec. However, it is shown that this detection system should be capable of resolving x-ray phenomena of much shorter duration. (author)

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

    Science.gov (United States)

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

    2015-07-07

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-07-01

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

  8. X-Ray Studies of Phase Transitions on Surfaces

    DEFF Research Database (Denmark)

    Als-Nielsen, Jens Aage

    1984-01-01

    The density variation across the surface from vapor to liquid in liquid crystal materials has been measured in the isotropic, nematic and smectic A phases by specular reflection of X rays with grazing angles from θc to θB (total reflection angle and Bragg angle for smectic A layering, respectively......) using synchroton X-rays in HASYLAB, Hamburg. Crystalline surface structures may be deduced from X-ray diffraction, utilizing the evanescent beam occuring for grazing angles less than θc to obtain surface sensitivity. Results from the reconstruction of Au(110) surface are reviewed....

  9. Graphical method for analyzing wide-angle x-ray diffraction

    Science.gov (United States)

    Chen, XiaoHui; Xue, Tao; Liu, DongBing; Yang, QingGuo; Luo, BinQiang; Li, Mu; Li, XiaoYa; Li, Jun

    2018-01-01

    Wide-angle X-ray diffraction on large-scale laser facility is a well-established experimental method, which is used to study the shock response of single crystal materials by recording X-rays diffracted from numerous lattice planes. We present a three-dimensional graphical method for extracting physical understanding from the raw diffraction data in shocked experiments. This method advances beyond the previous iterative process by turning abstract diffraction theories in shock physics into mathematic issues, providing three-dimensional visualization and quick extraction of data characteristics. The capability and versatility of the method are exhibited by identifying lattice planes for single crystal samples with different orientations and quantitatively measuring the lattice compression and rotation under dynamic loading.

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

    DEFF Research Database (Denmark)

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

    2014-01-01

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

  11. Resonant inelastic x-ray scattering studies of elementary excitations

    NARCIS (Netherlands)

    Ament, Lucas Johannes Peter (Luuk)

    2010-01-01

    Resonant Inelastic X-ray Scattering (RIXS) is an X-ray in, X-ray out technique that enables one to study the dispersion of excitations in solids. In this thesis, we investigated how various elementary excitations of transition metal oxides show up in RIXS spectra.

  12. Gas multidetector for neutron and X-ray diffraction studies

    International Nuclear Information System (INIS)

    Allemand, R.

    1975-01-01

    In the context of nuclear imagery research the LETI is studying neutron, X-ray and γ-ray localisation detectors, the fields of application being neutron diffraction, X-ray diffraction and nuclear medicine. This report deals only with gas localisation methods, describing the physical results obtained in neutron and X-ray diffraction [fr

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

    International Nuclear Information System (INIS)

    Oliveira, B.B.; Nogueira, M.S.

    2014-01-01

    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 (D G ) for different angles of the X-ray tube using a computed radiography (CR) mammography unit and different glandularity standard breast phantoms. D G values were derived from measurements of the incident air kerma (K i ) 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 (P It ) used was 50 mA s. Exposures were done for D G 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%. D G 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 D G 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.

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

    International Nuclear Information System (INIS)

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

    1981-01-01

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

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

    Science.gov (United States)

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

    2018-02-01

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

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

    Science.gov (United States)

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

    2011-12-01

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

  17. X-ray Studies of Flaring Plasma

    Indian Academy of Sciences (India)

    2016-01-27

    Jan 27, 2016 ... Sun; flares; X-rays; spectroscopic plasma diagnostic. Abstract. 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 ...

  18. 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

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

    International Nuclear Information System (INIS)

    Sano, Tsuneyoshi; Egawa, Kaoru; Nonaka, Naoko; Takiguchi, Reiji

    1999-01-01

    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)

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

    Science.gov (United States)

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

    2015-01-01

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

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

    Science.gov (United States)

    Fiori, F.; Spinozzi, F.

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

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

    DEFF Research Database (Denmark)

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

    2010-01-01

    Background: Genome sequencing projects have expanded the gap between the amount of known protein sequences and structures. The limitations of current high resolution structure determination methods make it unlikely that this gap will disappear in the near future. Small angle X-ray scattering (SAXS......) is an established low resolution method for routinely determining the structure of proteins in solution. The purpose of this study is to develop a method for the efficient calculation of accurate SAXS curves from coarse-grained protein models. Such a method can for example be used to construct a likelihood function...

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

    International Nuclear Information System (INIS)

    Schmidt, P.W.

    1988-01-01

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

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

  5. A double area detector system for simultaneous small and wide-angle X-ray scattering

    CERN Document Server

    Pokric, B; Ryan, A J; Fairclough, P; Dobson, B R; Derbyshire, G E; Helsby, W; Long, G; Moon, K

    2002-01-01

    A novel area detector has been designed for material science SR studies, capable of simultaneously collecting the diffraction data in two angular regimes. The detector for collecting wide-angle X-ray scattering (WAXS) data consists of four taper-coupled CCDs arranged as a 2x2 mosaic with a central aperture about 40 mm in diameter, so permitting the inclusion of a distant on-axis CCD detector for small-angle X-ray scattering (SAXS). The distance of the SAXS detector from the sample can be varied over the range 0.27 m to about 2 m. The overall aperture of WAXS detector is approximately 200x200 mm sup 2 allowing the measurement of the diffraction patterns from 5 deg. to 45 deg. with an average angular resolution of 0.05 deg. The parallax error for large angles is substantially reduced as the individual WAXS CCDs are tilted towards the specimen location. Both WAXS and SAXS diffraction data are simultaneously collected at 30 MB/s data rate, which is equivalent to 6 complete frames per second. Each pixel value is d...

  6. Structural Studies on Plasmodium falciparum Erythrocyte Membrane Protein 1 (PfEMP1) Malaria Antigens Using Small Angle X-Ray Scattering (SAXS)

    DEFF Research Database (Denmark)

    Christoffersen, Stig

    Infection with the pathogenic Plasmodium falciparum parasite causes the potentially deadly Malaria disease which leads to over 1 million fatalities each year according to the WHO (World Health Organization). Individuals subjected to multiple infections gradually become immune to the disease...... purposes. Macromolecular crystallography is typically the biophysical method of choice for obtaining detailed structural information but it unfortunately requires the formation of X-ray scattering protein crystals. The protein crystallization step remains a major bottleneck for X-ray protein...... crystallography. While conducting the SAXS experiments on PfEMP1 protein solutions, I alongside performed crystallization experiments using these solutions and found that the purified proteins showed very poor aptitude towards crystals formation. On the other hand, the SAXS method proved itself as a valuable tool...

  7. 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.

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

    International Nuclear Information System (INIS)

    Inoue, Katsuaki; Doutch, James; Terrill, Nick

    2013-01-01

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

  9. 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.

  10. Studying Microquasars with X-Ray Polarimetry

    Directory of Open Access Journals (Sweden)

    Giorgio Matt

    2018-03-01

    Full Text Available Microquasars are Galactic black hole systems in which matter is transferred from a donor star and accretes onto a black hole of, typically, 10–20 solar masses. The presence of an accretion disk and a relativistic jet made them a scaled down analogue of quasars—thence their name. Microquasars feature prominently in the scientific goals of X-ray polarimeters, because a number of open questions, which are discussed in this paper, can potentially be answered: the geometry of the hot corona believed to be responsible for the hard X-ray emission; the role of the jet; the spin of the black hole.

  11. Biplanar variable angle x-ray examining apparatus

    International Nuclear Information System (INIS)

    Grady, J.K.

    1986-01-01

    This invention relates to radiological equipment, particularly to apparatus for supporting and maneuvering a plurality of radiological examination sets to permit simultaneous or sequential exposure through different planes of an organ. The apparatus comprises: a first radiological examining set including a radiation source, receptor, and support for holding the source and receptor along an axis; and a second examining set with the source and receptor aligned to intersect the first axis at a common isocenter. The first support means is rotatable independently of the second support means about a rotational axis intersecting the common isocenter. The support means for one radiological examining set comprises two arms respectively carrying the radiation source and the radiation receptor of the one set and means reciprocally supporting the respective arms for movement independently of each other parallel to the rotational axis, whereby a series of substantially simultaneous radiological examinations can be made on both radiation axes through the subject at variable angles between the axes

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

    International Nuclear Information System (INIS)

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

    1985-01-01

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

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

    International Nuclear Information System (INIS)

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

    1997-01-01

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

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

    Science.gov (United States)

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

    2018-03-01

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

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

    Science.gov (United States)

    Hopkins, Jesse B; Thorne, Robert E

    2016-06-01

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

  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. Resonance magnetic x-ray scattering study of erbium

    DEFF Research Database (Denmark)

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

    1994-01-01

    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...

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

    Directory of Open Access Journals (Sweden)

    Krit Koyvanich

    2013-01-01

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

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

    NARCIS (Netherlands)

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

    2007-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1986-08-01

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

  1. 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.

  2. Grazing Incidence angle X-ray Diffraction of implanted stainless steel: comparison between simulated data and experimental data

    International Nuclear Information System (INIS)

    Dudognon, J.; Vayer, M.; Pineau, A.; Erre, R.

    2006-01-01

    Austenitic stainless steel was implanted with specific elements using specific conditions. The goal of this studies was to compare the predicted structural modifications within the implanted layer with the experimental ones observed by Grazing Incidence angle X-ray Diffraction (GIXD).During ion implantation implanted austenite steel layer undergoes modifications such as austenite lattice expansion, ferrite apparition and structure destruction. The X-ray diffraction austenite peak shape was predicted using the concentration depth profile of implanted element, the information depth profile of diffracted intensity and a linear relationship between implanted element concentration and lattice parameter. Experimental and predicted austenite X-ray diffraction peaks are in good accordance as long as the implanted layer contents mainly austenite. Whatever the nature of implanted element, ferrite appears above a given threshold of incoming energy amount. Moreover, the structure of the implanted layer is destroyed above a given amount of incoming energy

  3. Modeling the X-ray Process, and X-ray Flaw Size Parameter for POD Studies

    Science.gov (United States)

    Koshti, Ajay M.

    2014-01-01

    Nondestructive evaluation (NDE) method reliability can be determined by a statistical flaw detection study called probability of detection (POD) study. In many instances, the NDE flaw detectability is given as a flaw size such as crack length. The flaw is either a crack or behaving like a crack in terms of affecting the structural integrity of the material. An alternate approach is to use a more complex flaw size parameter. The X-ray flaw size parameter, given here, takes into account many setup and geometric factors. The flaw size parameter relates to X-ray image contrast and is intended to have a monotonic correlation with the POD. Some factors such as set-up parameters, including X-ray energy, exposure, detector sensitivity, and material type that are not accounted for in the flaw size parameter may be accounted for in the technique calibration and controlled to meet certain quality requirements. The proposed flaw size parameter and the computer application described here give an alternate approach to conduct the POD studies. Results of the POD study can be applied to reliably detect small flaws through better assessment of effect of interaction between various geometric parameters on the flaw detectability. Moreover, a contrast simulation algorithm for a simple part-source-detector geometry using calibration data is also provided for the POD estimation.

  4. Study on TV X-ray system characteristics

    International Nuclear Information System (INIS)

    Semenov, A.P.; Volkov, A.V.

    1978-01-01

    The results are presented of comparative investigations into the main characteristics of TV X-ray systems (TXS) and X-ray radiography when X-raying of the 1Kh18N9T steel. The following characteristics are considered: the threshold contrast sensitivity, the sensitivity to revealing standard defects, and the dose rate of X-radiation at the input of the X-ray converter. Practical recommendations are given on the use of TXS in flaw detection of various materials. It is remarked to use introscopes for testing of thick welded products articles, and X-ray vidicon systems for study of low-contrast images (in testing of welds made by point welding, and of thin-wall products)

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

    NARCIS (Netherlands)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, P.W.

    1980-09-01

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

  7. Determination of precise X-ray diffraction angles by fast Fourier transform

    International Nuclear Information System (INIS)

    Tokita, S.; Kojima, T.

    1987-01-01

    A new analytical method is presented for the separation of two or more closely overlapping X-ray diffraction lines using the narrowly distributed Gaussian function and one-dimensional fast Fourier transform pair. To test the method, the diffraction lines associated with characteristic Kα 1 and Kα 2 rays are measured by an X-ray diffractometer using a Brazilian quartz powder as a standard sample. It is found that the observed diffraction lines can be completely separated into Kα 1 and Kα 2 lines and that the accuracy of those diffraction angles is better than 2x10 -4 . (orig.)

  8. 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.

  9. Reliability analysis of Cobb angle measurements of congenital scoliosis using X-ray and 3D-CT images.

    Science.gov (United States)

    Tauchi, Ryoji; Tsuji, Taichi; Cahill, Patrick J; Flynn, John M; Flynn, John M; Glotzbecker, Michael; El-Hawary, Ron; Heflin, John A; Imagama, Shiro; Joshi, Ajeya P; Nohara, Ayato; Ramirez, Norman; Roye, David P; Saito, Toshiki; Sawyer, Jeffrey R; Smith, John T; Kawakami, Noriaki

    2016-01-01

    Therapeutic decisions for congenital scoliosis rely on Cobb angle measurements on consecutive radiographs. There have been no studies documenting the variability of measuring the Cobb angle using 3D-CT images in children with congenital scoliosis. The purpose of this study was to compare the reliability and measurement errors using X-ray images and those utilizing 3D-CT images. The X-ray and 3D-CT images of 20 patients diagnosed with congenital scoliosis were used to assess the reliability of the digital 3D-CT images for the measurement of the Cobb angle. Thirteen observers performed the measurements, and each image was analyzed by each observer twice with a minimum interval of 1 week between measurements. The analysis of intraobserver variation was expressed as the mean absolute difference (MAD) and standard deviation (SD) between measurements and the intraclass correlation coefficient (IaCC) of the measurements. In addition, the interobserver variation was expressed as the MAD and interclass correlation coefficient (IeCC). The average MAD and SD was 4.5° and 3.2° by the X-ray method and 3.7° and 2.6° by the 3D-CT method. The intraobserver and interobserver intraclass ICCs were excellent in both methods (X-ray: IaCC 0.835-0.994 IeCC 0.847, 3D-CT: IaCC 0.819-0.996 IeCC 0.893). There was no significant MAD difference between X-ray and 3D-CT images in measuring each type of congenital scoliosis by each observer. Results of Cobb angle measurements in patients with congenital scoliosis using X-ray images in the frontal plane could be reproduced with almost the same measurement variance (3°-4° measurement error) using 3D-CT images. This suggests that X-ray images are clinically useful for assessing any type of congenital scoliosis about measuring the Cobb angle alone. However, since 3D-CT can provide more detailed images of the anterior and posterior components of malformed vertebrae, the volume of information that can be obtained by evaluating them has

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

    Science.gov (United States)

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

    2012-06-01

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

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

    DEFF Research Database (Denmark)

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

    2014-01-01

    This study examines the nanoscale structures in a radiochromic dosimeter that was based on leuco-malachite-green dye and the surfactant sodium dodecyl sulfate (SDS) suspended in a gelatin matrix. Small-angle X-ray scattering was used to investigate the structures of a range of compositions...... of the dosimeter. When omitting gelatin, ellipsoidal micelles of SDS were formed with a core radius near 15 Å, an eccentricity of 1.6, and a head-group shell thickness near 7 Å. Gelatin significantly changed the micelles to a cylindrical shape with around three times lower core radius and four times larger shell...... thickness, which shows that the gelatin is present in the shell and the outer part of the core. Insight into the detailed structure might help to improve the dosimeter performance and increase the dose response to clinically relevant dose levels....

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

    DEFF Research Database (Denmark)

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

    2014-01-01

    Owing to the demand for low sample consumption and automated sample changing capabilities at synchrotron small-angle X-ray (solution) scattering (SAXS) beamlines, X-ray microfluidics is receiving continuously increasing attention. Here, a remote-controlled microfluidic device is presented...... for simultaneous SAXS and ultraviolet absorption measurements during protein dialysis, integrated directly on a SAXS beamline. Microfluidic dialysis can be used for monitoring structural changes in response to buffer exchange or, as demonstrated, protein concentration. By collecting X-ray data during...... the concentration procedure, the risk of inducing protein aggregation due to excessive concentration and storage is eliminated, resulting in reduced sample consumption and improved data quality. The proof of concept demonstrates the effect of halted or continuous flow in the microfluidic device. No sample...

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

    International Nuclear Information System (INIS)

    Barrea, Raul; Mainardi, R.T.

    1987-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Spanier, M., E-mail: mspanier@physik.tu-berlin.de; Herzog, C.; Grötzsch, D.; Kramer, F.; Mantouvalou, I.; Malzer, W.; Kanngießer, B. [Institute for Optics and Atomic Physics, Technische Universität Berlin, Hardenbergstraße 36, 10623 Berlin (Germany); Lubeck, J.; Weser, J.; Streeck, C.; Beckhoff, B. [Physikalisch-Technische Bundesanstalt, Abbestraße 2-12, 10587 Berlin (Germany)

    2016-03-15

    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.

  15. X-ray Diffraction Study of Arsenopyrite at High Pressure

    Energy Technology Data Exchange (ETDEWEB)

    D Fan; M Ma; W Zhou; S Wei; Z Chen; H Xie

    2011-12-31

    The high-pressure X-ray diffraction study of a natural arsenopyrite was investigated up to 28.2 GPa using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at National Synchrotron Light Source, Brookhaven National Laboratory. The 16:3:1 methanol-ethanol-water mixture was used as a pressure-transmitting medium. Pressures were measured using the ruby-fluorescence method. No phase change has been observed up to 28.2 GPa. The isothermal equation of state (EOS) was determined. The values of K{sub 0}, and K'{sub 0} refined with a third-order Birch-Murnaghan EOS are K{sub 0} = 123(9) GPa, and K'{sub 0} = 5.2(8). Furthermore, we confirm that the linear compressibilities ({beta}) along a, b and c directions of arsenopyrite is elastically isotropic ({beta}{sub a} = 6.82 x 10{sup -4}, {beta}{sub b} = 6.17 x 10{sup -4} and {beta}{sub c} = 6.57 x 10{sup -4} GPa{sup -1}).

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  17. 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...

  18. Soft-x-ray spectroscopy study of nanoscale materials

    International Nuclear Information System (INIS)

    Guo, J.-H.

    2005-01-01

    The ability to control the particle size and morphology of nanoparticles is of crucial importance nowadays both from a fundamental and industrial point of view considering the tremendous amount of high-tech applications. Controlling the crystallographic structure and the arrangement of atoms along the surface of nanostructured material will determine most of its physical properties. In general, electronic structure ultimately determines the properties of matter. Soft X-ray spectroscopy has some basic features that are important to consider. X-ray is originating from an electronic transition between a localized core state and a valence state. As a core state is involved, elemental selectivity is obtained because the core levels of different elements are well separated in energy, meaning that the involvement of the inner level makes this probe localized to one specific atomic site around which the electronic structure is reflected as a partial density-of-states contribution. The participation of valence electrons gives the method chemical state sensitivity and further, the dipole nature of the transitions gives particular symmetry information. The new generation synchrotron radiation sources producing intensive tunable monochromatized soft X-ray beams have opened up new possibilities for soft X-ray spectroscopy. The introduction of selectively excited soft X-ray emission has opened a new field of study by disclosing many new possibilities of soft X-ray resonant inelastic scattering. In this paper, some recent findings regarding soft X-ray absorption and emission studies of various nanostructured systems are presented

  19. Thermal Stability of Au/NbOx/Nb and Au/Nb2O5/W Model Catalysts Studied by Angle-resolved X-ray Photoelectron Spectroscopy

    Czech Academy of Sciences Publication Activity Database

    Lykhach, Yaroslava; Plšek, Jan; Spirovová, Ilona; Bastl, Zdeněk

    2003-01-01

    Roč. 68, č. 10 (2003), s. 1791-1804 ISSN 0010-0765 R&D Projects: GA ČR GA104/02/0664 Institutional research plan: CEZ:AV0Z4040901 Keywords : model metal catalysts * angle resolved photoemission * depth profiles Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.041, year: 2003

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-07-01

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

  2. Application of X-ray and neutron small angle scattering techniques to study the hierarchical structure of plant cell walls: a review.

    Science.gov (United States)

    Martínez-Sanz, Marta; Gidley, Michael J; Gilbert, Elliot P

    2015-07-10

    Plant cell walls present an extremely complex structure of hierarchically assembled cellulose microfibrils embedded in a multi-component matrix. The biosynthesis process determines the mechanism of cellulose crystallisation and assembly, as well as the interaction of cellulose with other cell wall components. Thus, a knowledge of cellulose microfibril and bundle architecture, and the structural role of matrix components, is crucial for understanding cell wall functional and technological roles. Small angle scattering techniques, combined with complementary methods, provide an efficient approach to characterise plant cell walls, covering a broad and relevant size range while minimising experimental artefacts derived from sample treatment. Given the system complexity, approaches such as component extraction and the use of plant cell wall analogues are typically employed to enable the interpretation of experimental results. This review summarises the current research status on the characterisation of the hierarchical structure of plant cell walls using small angle scattering techniques. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

  3. Energy dispersive X-Ray fluorescence spectrometric study of ...

    African Journals Online (AJOL)

    Energy dispersive X-Ray fluorescence spectrometric study of compositional differences in trace elements in dried Moringa oleifera leaves grown in two different agro-ecological locations in Ebonyi State, Nigeria.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-01

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

  5. 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....

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

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Hornstrup, Allan; Frederiksen, P.

    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...... x-ray telescope will be studied, is described in detail. Review of Scientific Instruments is copyrighted by The American Institute of Physics....

  7. X-ray scattering studies of surfaces and interfaces

    International Nuclear Information System (INIS)

    Sanyal, M.K.

    1998-01-01

    Here we shall briefly review the basics and some applications of x-ray specular reflectivity and diffuse scattering techniques. These x-ray scattering techniques are uniquely suited to study of the structure of surfaces and interfaces at atomic resolutions as they are nondestructive and can probe even interfaces which are buried. The study of structure of surfaces and interfaces is not only required in understanding physics in reduced dimensions but is also essential in developing technologically important materials

  8. 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.

  9. X-ray microscopy and spectromicroscopy - tools for environmental studies

    International Nuclear Information System (INIS)

    Thieme, J.

    2002-01-01

    Full text: X-ray microscopy achieves a much higher resolution than light microscopy. This is due to the much shorter wavelength of X-rays compared to visible light. The smallest structures that can be seen in an X-ray microscope at present are about 20 nm in size. X-ray microscopy is also capable of imaging specimens directly in aqueous media. By choosing the wavelength of the X-radiation appropriately, it is possible to perform spectromicroscopy studies. Comprising, it is a tool very well suited to study colloidal structures in the environment. X-ray microscopy can be performed with two types of instruments. An X-ray microscope quickly takes high-resolution images of objects to be studied, whereas a scanning X-ray microscope is an analytical instrument for spectromicroscopy. Here, an object can be imaged using energies above and below the absorption edge of an element. Dividing both images gives rise to a map of the distribution of this element in the sample. Using near-edge resonances it is possible to conduct NEXAFS studies. As the X-ray energy is raised to match the absorption edge resonances are found, that reflect the chemical bonding state of the element. Therefore, it is possible with X-ray microscopy to combine high spatial resolution with high spectral resolution for studies of colloidal structures. The Institute of X-ray physics builds up an X-ray microscopy beamline at the electron storage ring BESSY II with both, an X-ray microscope and a scanning X-ray microscope. The status of this beamline will be presented in this talk. Colloidal structures play an important role in the environment. Due to their surface activity they are involved in various processes. Substances can be bound and immobilized or transported, colloids can attach to microorganisms building up microhabitats, and organic substances as humics can flocculate due the interaction with metals. A great variety of colloidal structures from the environment have been studied using X-ray

  10. Note: Grazing incidence small and wide angle x-ray scattering combined with imaging ellipsometry

    Energy Technology Data Exchange (ETDEWEB)

    Koerstgens, V.; Meier, R.; Ruderer, M. A.; Guo, S.; Chiang, H.-Y.; Mueller-Buschbaum, P. [Technische Universitaet Muenchen, Physik-Department, Lehrstuhl fuer Funktionelle Materialien, James-Franck-Str. 1, 85748 Garching (Germany); Perlich, J.; Roth, S. V.; Gehrke, R. [HASYLAB, DESY, Notkestr. 85, 22607, Hamburg (Germany)

    2012-07-15

    The combination of grazing incidence small angle x-ray scattering (GISAXS) and grazing incidence wide angle x-ray scattering (GIWAXS) with optical imaging ellipsometry is presented as an upgrade of the available measurement techniques at the wiggler beamline BW4 of the Hamburger Synchrotronstrahlungslabor. The instrument is introduced with the description of the alignment procedure to assure the measurement of imaging ellipsometry and GISAXS/GIWAXS on the same sample spot. To demonstrate the possibilities of the new instrument examples of morphological investigation on films made of poly(3-hexylthiophene) and [6,6]-phenyl-C{sub 61} butyric acid methyl ester as well as textured poly(9,9-dioctylfluorene-alt-benzo-thia-diazole) are shown.

  11. Applicability study of x-ray computed tomography technique

    International Nuclear Information System (INIS)

    Tanai, Kenji

    2003-03-01

    Several experiments on the study of high level radioactive waste disposal indirectly measured various physical quantity in the closed test vessel by various sensor. This measurement technique on closed-system cause limit of understanding of mechanisms. Therefore, new observation technique by nondestructive technique such a X-ray computed tomography is necessary for HLW disposal study. In this work, the objective of this study are as follows; (1) to clarify the relationship between dry density of bentonite and CT number, (2) to observed infiltration behaviour of liquid in bentonite specimen using X-ray CT (3) to observed gas migration behaviour in bentonite specimen using X-ray CT. The major conclusions obtained in this study are as follows; (1) CT number of X-ray increases linearly with degree of saturation and density of bentonite specimen. (2) Infiltration behaviour of liquid in bentonite specimen can be observed by X-ray CT. (3) Gas permeability of bentonite with a dry density of 1.6 Mg/m3 is approximately 6 x 10 -20 m 2 . And, this result was almost the same with the other experimental results. But, significant difference of breakthrough phenomena was observed between this test and other experiments results. In visualization study of gas migration through bentonite, gas migration behavior through bentonite was not observed by X-ray CT. (author)

  12. Concerns about a variance approach to X-ray diffractometric estimation of microfibril angle in wood

    Science.gov (United States)

    Steve P. Verrill; David E. Kretschmann; Victoria L. Herian; Michael C. Wiemann; Harry A. Alden

    2011-01-01

    In this article, we raise three technical concerns about Evans’ 1999 Appita Journal “variance approach” to estimating microfibril angle (MFA). The first concern is associated with the approximation of the variance of an X-ray intensity half-profile by a function of the MFA and the natural variability of the MFA. The second concern is associated with the approximation...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-12-01

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

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

    International Nuclear Information System (INIS)

    Buckley, C.E.

    1999-01-01

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

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

    International Nuclear Information System (INIS)

    Wang Shuo; Ji Jianfeng; Han Dong; Feng Hua

    2013-01-01

    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 CO 2 , 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)

  16. Studying Dust Scattering Halos with Galactic X-ray Binaries

    Science.gov (United States)

    Beeler, Doreen; Corrales, Lia; Heinz, Sebastian

    2018-01-01

    Dust is an important part of the interstellar medium (ISM) and contributes to the formation of stars and planets. Since the advent of modern X-ray telescopes, Galactic X-ray point sources have permitted a closer look at all phases of the ISM. Interstellar metals from oxygen to iron — in both gas and dust form — are responsible for absorption and scattering of X-ray light. Dust scatters the light in a forward direction and creates a diffuse halo image surrounding many bright Galactic X-ray binaries. We use all the bright X-ray point sources available in the Chandra HETG archive to study dust scattering halos from the local ISM. We have described a data analysis pipeline using a combination of the data reduction software CIAO and Python. We compare our results from Chandra HETG and ACIS-I observations of a well studied dust scattering halo around GX 13+1, in order to characterize any systematic errors associated with the HETG data set. We describe how our data products will be used to measure ISM scaling relations for X-ray extinction, dust abundance, and dust-to-metal ratios.

  17. Identifications studies of Lauha Bhasma by X-ray diffraction and X-ray fluorescence.

    Science.gov (United States)

    Bhargava, S C; Reddy, K R C; Sastry, G V S

    2012-01-01

    Procedures for preparation of Lauha Bhasma are described in ancient texts of Ayurveda. These procedures also begin with different source material for iron such as Teekshna Lauha and Kanta Lauha etc. In the present study, we have selected different source materials viz. magnetite iron ore for Kanta Lauha and pure (Armco grade) iron turnings for Teekshna Lauha. The standard procedures of preparation of Lauha Bhasma are carried out in identical conditions for these two raw materials. The final product from the Puta are characterized by using X-ray diffraction and X-ray fluorescence spectroscopy to understanding the crystallographic form or forms of iron oxides and their composition at the end of each Puta. The iron content at the end of repeated Putas (18 for Kanta Lauha and 20 for Teekshna Lauha) have shown a decrease in case of Teekshna Lauha since the starting material is pure iron while it showed only marginal decreases in the case of Kanta Lauha because the Fe(3)O(4) of magnetite is undergoing oxidation to Fe(2)O(3). The trace elements remain within the Bhasma in the form of various oxides of Si, Al, Ca, etc.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    International Nuclear Information System (INIS)

    Ohnuma, Masato

    2017-01-01

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

  20. Prospects of x-ray microscopy and x-ray microtomography for interface studies

    International Nuclear Information System (INIS)

    Erre, D.; Thomas, X.; Mouze, D.; Patat, J.M.; Trebbia, P.; Cazaux, J.

    1992-01-01

    Microfocal x-ray projection microscopy allows the non-destructive investigation of thick specimens with a lateral resolution in the micrometre range. The minimum detectable thickness lies below 100 nm for strongly absorbing materials. For further investigation, x-ray microtomography leads to three-dimensional reconstruction of the specimen. Some applications of x-ray microscopy are connected with the localization and imaging of solid/solid interfaces deeply buried in a matrix. In the future, solid/liquid interfaces and their motion will be of interest. The performance of x-ray microscopy is discussed and x-ray projection images obtained with a simple modified scanning electron microscope are shown. (author)

  1. Energy response calibration of photon-counting detectors using x-ray fluorescence: a feasibility study.

    Science.gov (United States)

    Cho, H-M; Ding, H; Ziemer, B P; Molloi, S

    2014-12-07

    Accurate energy calibration is critical for the application of energy-resolved photon-counting detectors in spectral imaging. The aim of this study is to investigate the feasibility of energy response calibration and characterization of a photon-counting detector using x-ray fluorescence. A comprehensive Monte Carlo simulation study was performed using Geant4 Application for Tomographic Emission (GATE) to investigate the optimal technique for x-ray fluorescence calibration. Simulations were conducted using a 100 kVp tungsten-anode spectra with 2.7 mm Al filter for a single pixel cadmium telluride (CdTe) detector with 3 × 3 mm(2) in detection area. The angular dependence of x-ray fluorescence and scatter background was investigated by varying the detection angle from 20° to 170° with respect to the beam direction. The effects of the detector material, shape, and size on the recorded x-ray fluorescence were investigated. The fluorescent material size effect was considered with and without the container for the fluorescent material. In order to provide validation for the simulation result, the angular dependence of x-ray fluorescence from five fluorescent materials was experimentally measured using a spectrometer. Finally, eleven of the fluorescent materials were used for energy calibration of a CZT-based photon-counting detector. The optimal detection angle was determined to be approximately at 120° with respect to the beam direction, which showed the highest fluorescence to scatter ratio (FSR) with a weak dependence on the fluorescent material size. The feasibility of x-ray fluorescence for energy calibration of photon-counting detectors in the diagnostic x-ray energy range was verified by successfully calibrating the energy response of a CZT-based photon-counting detector. The results of this study can be used as a guideline to implement the x-ray fluorescence calibration method for photon-counting detectors in a typical imaging laboratory.

  2. JMFA2—a graphically interactive Java program that fits microfibril angle X-ray diffraction data

    Science.gov (United States)

    Steve P. Verrill; David E. Kretschmann; Victoria L. Herian

    2006-01-01

    X-ray diffraction techniques have the potential to decrease the time required to determine microfibril angles dramatically. In this paper, we discuss the latest version of a curve-fitting toll that permits us to reduce the time required to evaluate MFA X-ray diffraction patterns. Further, because this tool reflects the underlying physics more accurately than existing...

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

    DEFF Research Database (Denmark)

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

    2012-01-01

    . This protein drug system was designed to form non-native homo-oligomers through selective coordination of two divalent metal ions, Fe(II) and Zn(II), respectively. The insulin type chosen for this study is a variant designed for a reduced tendency toward native dimer formation at physiological concentrations......Precise control of the oligomeric state of proteins is of central importance for biological function and for the properties of biopharmaceutical drugs. Here, the self-assembly of 2,2′-bipyridine conjugated monomeric insulin analogues, induced through coordination to divalent metal ions, was studied...

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

    CERN Document Server

    Paul, Amitesh

    2017-01-01

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

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

    Science.gov (United States)

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

    2017-06-30

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

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

    Science.gov (United States)

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

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

  7. Structural Studies on Plasmodium falciparum Erythrocyte Membrane Protein 1 (PfEMP1) Malaria Antigens Using Small Angle X-Ray Scattering (SAXS)

    DEFF Research Database (Denmark)

    Christoffersen, Stig

    against placental malaria, VAR2CSA was studied extensively. By the use of SAXS on multiple truncated VAR2CSA constructs it was possible to combine the acquired information and present a structural model for the DBL and CIDR domain arrangement in VAR2CSA. This work was published in Journal of Biological...... symptoms and vaccine research is focused on trying to mimic or advance this immune acquisition. Immunity is primarily caused by acquisition of antibodies directed against a family of Plasmodium protein antigens called PfEMP1s located on the surface of infected erythrocytes. The PfEMP1 proteins are adhesive...... knowledge for these proteins is required. During the time course of this PhD thesis I have studied a number of PfEMP1 proteins using the SAXS technique. This biophysical technique has gained widespread attention during the past decade due to scientific and computational developments. SAXS is X...

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  9. Small-angle X-ray scattering (SAXS) studies on porous materials with fractal structure; Badanie metoda malokatowego rozpraszania promieni rentgenowskich (SAXS) materialow porowatych o strukturze fraktalnej

    Energy Technology Data Exchange (ETDEWEB)

    Pajak, L.; Bierska, B.; Lagiewka, E. [Instytut Fizyki i Chemii Metali, Uniwersytet Slaski, Katowice (Poland)

    1998-12-31

    The structure of most porous materials is quite complex. The porosity of materials (total volume fraction of material occupied by pores) can vary in a very broad range, from much less than 1% up to more than 99 % , in the case of aerogels. In the last two decades the characterization of the structure of porous materials has made a milestone progress owing to the use of fractal geometry. At present it is generally accepted that the fractal models of pore structure describe the real morphology better than the classical models which assume the existence of macro-, meso- and micropores of simple geometry. The SAXS method is specially useful in the studies of porous materials in the length scale 10-1000 A. It gives information which is difficult to obtain or even not available by use of other methods. The SAXS studies were performed on silica aerogels and copper foils electrodeposited in galvanostatic conditions. The fractal concept was applied in the interpretation of SAXS results. (author) 17 refs, 8 figs, 1 tab

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

    International Nuclear Information System (INIS)

    Hendricks, R.W.

    1979-12-01

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

  11. 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.

  12. Sodium dodecyl sulfate (SDS) effect on the thermal stability of oxy-HbGp: dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) studies.

    Science.gov (United States)

    Carvalho, José Wilson P; Alves, Fernanda Rosa; Batista, Tatiana; Carvalho, Francisco Adriano O; Santiago, Patrícia S; Tabak, Marcel

    2013-11-01

    Glossoscolex paulistus (HbGp) hemoglobin is an oligomeric protein, presenting a quaternary structure constituted by 144 globin and 36 non-globin chains (named linkers) with a total molecular mass of 3.6 MDa. SDS effects on the oxy-HbGp thermal stability were studied, by DLS and SAXS, at pH 5.0, 7.0 and 9.0. DLS and SAXS data show that the SDS-oxy-HbGp interactions induce a significant decrease of the protein thermal stability, with the formation of larger aggregates, at pH 5.0. At pH 7.0, oxy-HbGp undergoes complete oligomeric dissociation, with increase of temperature, in the presence of SDS. Besides, oxy-HbGp 3.0mg/mL, pH 7.0, in the presence of SDS, has the oligomeric dissociation process reduced as compared to 0.5mg/mL of protein. At pH 9.0, oxy-HbGp starts to dissociate at 20 °C, and the protein is totally dissociated at 50 °C. The thermal dissociation kinetic data show that oxy-HbGp oligomeric dissociation at pH 7.0, in the presence of SDS, is strongly dependent on the protein concentration. At 0.5mg/mL of protein, the oligomeric dissociation is complete and fast at 40 and 42 °C, with kinetic constants of (2.1 ± 0.2) × 10(-4) and (5.5 ± 0.4) × 10(-4) s(-1), respectively, at 0.6 mmol/L SDS. However, at 3.0mg/mL, the oligomeric dissociation process starts at 46 °C, and only partial dissociation, accompanied by aggregates formation is observed. Moreover, our data show, for the first time, that, for 3.0mg/mL of protein, the oligomeric dissociation, denaturation and aggregation phenomena occur simultaneously, in the presence of SDS. Our present results on the surfactant-HbGp interactions and the protein thermal unfolding process correspond to a step forward in the understanding of SDS effects. Copyright © 2013 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    Data.gov (United States)

    National Aeronautics and Space Administration — Fabricate and demonstrate performance of new large-area soft x-ray absorbers, using techniques that allow integration with either magnetic penetration thermometers...

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

    Science.gov (United States)

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

    2008-03-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2014-10-10

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

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

    Science.gov (United States)

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

    2017-11-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Fuoss, Paul, E-mail: fuoss@anl.gov; Chang, Kee-Chul; You, Hoydoo, E-mail: hyou@anl.gov

    2013-10-15

    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, pO{sub 2}, 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.

  1. Coherent X-ray diffraction studies of mesoscopic materials

    International Nuclear Information System (INIS)

    Shabalin, Anatoly

    2015-12-01

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

    Xia Qingzhong; Fan Zhijian; Chen Bo

    2007-12-01

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

  5. 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.

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

    International Nuclear Information System (INIS)

    Bergmann, A.

    2000-08-01

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

  7. 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

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

    International Nuclear Information System (INIS)

    Gulden, Johannes

    2013-03-01

    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

  9. Raman spectroscopy and X-ray diffraction studies on celestite

    International Nuclear Information System (INIS)

    Chen Yenhua; Yu Shucheng; Huang, Eugene; Lee, P.-L.

    2010-01-01

    High-pressure Raman spectroscopy and X-ray diffraction studies of celestite (SrSO 4 ) were carried out in a diamond anvil cell at room temperature. Variation in the Raman vibrational frequency and change of lattice parameters with pressure indicate that a transformation occurs in celestite. This transformation caused an adjustment in the Sr-O polyhedra that affected the stretching-force constant of SO 4 . Moreover, compressibilities along the crystallographic axes decreased in the order a to c to b. From the compression data, the bulk modulus of the celestite was 87 GPa. Both X-ray and Raman data show that the transition in celestite is reversible.

  10. X-ray study of bow shocks in runaway stars

    Science.gov (United States)

    De Becker, M.; del Valle, M. V.; Romero, G. E.; Peri, C. S.; Benaglia, P.

    2017-11-01

    Massive runaway stars produce bow shocks through the interaction of their winds with the interstellar medium, with the prospect for particle acceleration by the shocks. These objects are consequently candidates for non-thermal emission. Our aim is to investigate the X-ray emission from these sources. We observed with XMM-Newton a sample of five bow shock runaways, which constitutes a significant improvement of the sample of bow shock runaways studied in X-rays so far. A careful analysis of the data did not reveal any X-ray emission related to the bow shocks. However, X-ray emission from the stars is detected, in agreement with the expected thermal emission from stellar winds. On the basis of background measurements we derive conservative upper limits between 0.3 and 10 keV on the bow shocks emission. Using a simple radiation model, these limits together with radio upper limits allow us to constrain some of the main physical quantities involved in the non-thermal emission processes, such as the magnetic field strength and the amount of incident infrared photons. The reasons likely responsible for the non-detection of non-thermal radiation are discussed. Finally, using energy budget arguments, we investigate the detectability of inverse Compton X-rays in a more extended sample of catalogued runaway star bow shocks. From our analysis we conclude that a clear identification of non-thermal X-rays from massive runaway bow shocks requires one order of magnitude (or higher) sensitivity improvement with respect to present observatories.

  11. PREPARATION, SPECTROSCOPIC STUDIES AND X-RAY ...

    African Journals Online (AJOL)

    Molar conductance measurements in dmf indicate 1:3 electrolytes in all cases. Magnetic moment values are close proximity of the Van Vleck values. IR studies suggest the coordination of the ligand is through the azomethine, the phenolic oxygen atom and the carbonyl oxygen of the hydrazonic moiety. The nitrate ion is also ...

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

    International Nuclear Information System (INIS)

    Kim, Seungeon; Chang, Yongjin; Ra, Jong Beom

    2015-01-01

    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

  13. High resolution X-ray diffraction studies on unirradiated

    Indian Academy of Sciences (India)

    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 ...

  14. 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.

  15. The complementary nature of x-ray photoelectron spectroscopy and angle-resolved x-ray diffraction part II: Analysis of oxides on dental alloys

    Science.gov (United States)

    Kerber, S. J.; Barr, T. L.; Mann, G. P.; Brantley, W. A.; Papazoglou, E.; Mitchell, J. C.

    1998-06-01

    X-ray photoelectron spectroscopy (XPS) and angle-resolved x-ray diffraction (ARXRD) were used to analyze the oxide layer on three palladium-gallium-based dental casting alloys. The oxide layers were approximately 10 Μm thick. The use of the techniques helped to determine which mechanism was responsible for oxide formation—either (a) oxide layer growth via diffusion of oxygen through the scale to the metal, causing the scale to grow at the metal-oxide interface, or (b) an oxide layer formed by metal ions diffusing through the scale to the surface and reacting with oxygen, causing the scale to grow at the oxide-air interface. The oxide growth mechanisms were correlated to previous layer adhesion results determined with biaxial flexure testing.

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

    International Nuclear Information System (INIS)

    Krebs, A.

    1996-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1992-09-15

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

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

    Science.gov (United States)

    Ma, Shufen; Liu, Haiguang

    2016-04-01

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

  19. X-ray and neutron scattering studies of complex confined fluids

    International Nuclear Information System (INIS)

    Sinha, S. K.

    1999-01-01

    We review recent X-ray and neutron scattering studies of the structure and dynamics of confined complex fluids. This includes the study of polymer conformations and binary fluid phase transitions in porous media using Small Angle Neutron scattering, and the use of synchrotrons radiation to study ordering and fluctuation phenomena at solid/liquid and liquid/air interfaces. Ordering of liquids near a solid surface or in confinement will be discussed, and the study, via specular and off-specular X-ray reflectivity, of capillary wave fluctuations on liquid polymer films. Finally, we shall discuss the use of high-brilliance beams from X-ray synchrotrons to study via photon correlation spectroscopy the slow dynamics of soft condensed matter systems

  20. X-ray and neutron scattering studies of complex confined fluids.

    Energy Technology Data Exchange (ETDEWEB)

    Sinha, S. K.

    1999-08-04

    We review recent X-ray and neutron scattering studies of the structure and dynamics of confined complex fluids. This includes the study of polymer conformations and binary fluid phase transitions in porous media using Small Angle Neutron scattering, and the use of synchrotrons radiation to study ordering and fluctuation phenomena at solid/liquid and liquid/air interfaces. Ordering of liquids near a solid surface or in confinement will be discussed, and the study, via specular and off-specular X-ray reflectivity, of capillary wave fluctuations on liquid polymer films. Finally, we shall discuss the use of high-brilliance beams from X-ray synchrotrons to study via photon correlation spectroscopy the slow dynamics of soft condensed matter systems.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-24

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    DEFF Research Database (Denmark)

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

    1984-01-01

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

  5. 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

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

    International Nuclear Information System (INIS)

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

    1975-01-01

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

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

    DEFF Research Database (Denmark)

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

    2013-01-01

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

  8. Nonlocal heat transport and improved target design for x-ray heating studies at x-ray free electron lasers

    Science.gov (United States)

    Hoidn, Oliver; Seidler, Gerald T.

    2018-01-01

    The extremely high-power densities and short durations of single pulses of x-ray free electron lasers (XFELs) have opened new opportunities in atomic physics, where complex excitation-relaxation chains allow for high ionization states in atomic and molecular systems, and in dense plasma physics, where XFEL heating of solid-density targets can create unique dense states of matter having temperatures on the order of the Fermi energy. We focus here on the latter phenomena, with special emphasis on the problem of optimum target design to achieve high x-ray heating into the warm dense matter (WDM) state. We report fully three-dimensional simulations of the incident x-ray pulse and the resulting multielectron relaxation cascade to model the spatial energy density deposition in multicomponent targets, with particular focus on the effects of nonlocal heat transport due to the motion of high energy photoelectrons and Auger electrons. We find that nanoscale high-Z /low-Z multicomponent targets can give much improved energy density deposition in lower-Z materials, with enhancements reaching a factor of 100. This has three important benefits. First, it greatly enlarges the thermodynamic parameter space in XFEL x-ray heating studies of lower-Z materials. Second, it allows the use of higher probe photon energies, enabling higher-information content x-ray diffraction (XRD) measurements such as in two-color XFEL operations. Third, while this is merely one step toward optimization of x-ray heating target design, the demonstration of the importance of nonlocal heat transport establishes important common ground between XFEL-based x-ray heating studies and more traditional laser plasma methods.

  9. X-ray apparatus

    International Nuclear Information System (INIS)

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

    1976-01-01

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

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

    International Nuclear Information System (INIS)

    Agamalyan, M.M.

    1989-01-01

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

  11. Design of a novel transmission-grating spectrometer for soft X-ray emission studies

    Energy Technology Data Exchange (ETDEWEB)

    Hatsui, Takaki [Institute for Molecular Science, Myodaiji, Okazaki 444-8585 (Japan) and Graduate School for Advanced Studies, Myodaiji, Okazaki 444-8585 (Japan)]. E-mail: hatsui@ims.ac.jp; Setoyama, Hiroyuki [Institute for Molecular Science, Myodaiji, Okazaki 444-8585 (Japan); Shigemasa, Eiji [Institute for Molecular Science, Myodaiji, Okazaki 444-8585 (Japan); Graduate School for Advanced Studies, Myodaiji, Okazaki 444-8585 (Japan); Kosugi, Nobuhiro [Institute for Molecular Science, Myodaiji, Okazaki 444-8585 (Japan); Graduate School for Advanced Studies, Myodaiji, Okazaki 444-8585 (Japan)

    2005-06-15

    The design of a transmission-grating spectrometer for high-resolution soft X-ray emission studies has been proposed. It is different from conventional types of soft X-ray emission spectrometers; that is, the spectrometer has a Wolter type I mirror, a free-standing transmission grating, and a back-illuminated CCD. A high collection angle up to 1.5 x 10{sup -3} sr is achieved by utilizing the Wolter mirror as a prefocusing system. The CCD is mounted at 1400 mm downstream of the grating on a Rowland torus mount. Diffracted X-rays are detected by the CCD in the normal incidence geometry, resulting in high detection efficiency. The energy resolution is limited by the figure errors of the optical elements and the spatial resolution of the detector. The ray-tracing results confirm that the aberrations do not practically degrade the energy resolution.

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

    KAUST Repository

    Spannuth, Melissa

    2011-02-01

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

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

    Science.gov (United States)

    Rambo, Robert P; Tainer, John A

    2010-03-01

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

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

    Science.gov (United States)

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

    2016-03-01

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

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

    International Nuclear Information System (INIS)

    Schelten, J.

    1978-01-01

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

  16. The oblique view for spondylolysis in the growing period. X-ray projection angle to spondylolytic lumbar vertebra based on CT scanning

    Energy Technology Data Exchange (ETDEWEB)

    Kobayashi, Yoshimitsu; Minato, Izumi; Nagano, Junji; Inoue, Yoshiya; Takahashi, Yuji; Saito, Hidehiko [Seirei Hamamatsu General Hospital, Shizuoka (Japan)

    1996-02-01

    In this study, CT images of 239 vertebrae from 227 patients with spondylolysis in the growing period were obtained to analyze x-ray oblique separation images based on the relationship between x-ray incidence angle and CT. The age of the subjects ranged from 5 to 23 years (average 14.8 years), of which 224 patients were 18 years or lower. The CT images obtained were classified into four according to our classification, i.e., Type Ia, 112 vertebrae; Type Ib, 175; Type II, 66; Type III, 67. All patients underwent plain x-ray from 4 directions including 45deg. The angle of separation line and posterior margin of the vertebral body was obtained and the average angle of all slices was determined as separation angle. As a result, depiction level of separation line was better in 30deg oblique images than 45deg oblique images in Ia, Ib, and III groups. It is thus desirable to take the relationship between incidence angle of x-ray, separation angle, and CT classification into consideration. (S.Y.).

  17. The oblique view for spondylolysis in the growing period. X-ray projection angle to spondylolytic lumbar vertebra based on CT scanning

    International Nuclear Information System (INIS)

    Kobayashi, Yoshimitsu; Minato, Izumi; Nagano, Junji; Inoue, Yoshiya; Takahashi, Yuji; Saito, Hidehiko

    1996-01-01

    In this study, CT images of 239 vertebrae from 227 patients with spondylolysis in the growing period were obtained to analyze x-ray oblique separation images based on the relationship between x-ray incidence angle and CT. The age of the subjects ranged from 5 to 23 years (average 14.8 years), of which 224 patients were 18 years or lower. The CT images obtained were classified into four according to our classification, i.e., Type Ia, 112 vertebrae; Type Ib, 175; Type II, 66; Type III, 67. All patients underwent plain x-ray from 4 directions including 45deg. The angle of separation line and posterior margin of the vertebral body was obtained and the average angle of all slices was determined as separation angle. As a result, depiction level of separation line was better in 30deg oblique images than 45deg oblique images in Ia, Ib, and III groups. It is thus desirable to take the relationship between incidence angle of x-ray, separation angle, and CT classification into consideration. (S.Y.)

  18. X-ray induced dimerization of cinnamic acid: Time-resolved inelastic X-ray scattering study.

    Science.gov (United States)

    Inkinen, Juho; Niskanen, Johannes; Talka, Tuomas; Sahle, Christoph J; Müller, Harald; Khriachtchev, Leonid; Hashemi, Javad; Akbari, Ali; Hakala, Mikko; Huotari, Simo

    2015-11-16

    A classic example of solid-state topochemical reactions is the ultraviolet-light induced photodimerization of α-trans-cinnamic acid (CA). Here, we report the first observation of an X-ray-induced dimerization of CA and monitor it in situ using nonresonant inelastic X-ray scattering spectroscopy (NRIXS). The time-evolution of the carbon core-electron excitation spectra shows the effects of two X-ray induced reactions: dimerization on a short time-scale and disintegration on a long time-scale. We used spectrum simulations of CA and its dimerization product, α-truxillic acid (TA), to gain insight into the dimerization effects. From the time-resolved spectra, we extracted component spectra and time-dependent weights corresponding to CA and TA. The results suggest that the X-ray induced dimerization proceeds homogeneously in contrast to the dimerization induced by ultraviolet light. We also utilized the ability of NRIXS for direct tomography with chemical-bond contrast to image the spatial progress of the reactions in the sample crystal. Our work paves the way for other time-resolved studies on chemical reactions using inelastic X-ray scattering.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-01-01

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

  20. 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.

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

    Science.gov (United States)

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

    2018-01-01

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

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

    Science.gov (United States)

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

    2017-12-01

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

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

    Science.gov (United States)

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

    2017-04-01

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

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

    Science.gov (United States)

    Lambard, Jacques; Lesieur, Pierre; Zemb, Thomas

    1992-06-01

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

  5. Momentum-resolved electronic structure at a buried interface from soft X-ray standing-wave angle-resolved photoemission

    NARCIS (Netherlands)

    Gray, A.X.; Minar, J.; Plucinski, L.; Huijben, Mark; Bostwick, A.; Rotenberg, E.; Yang, S.-H.; Braun, J.; Winkelmann, A.; Conti, G.; Eiteneer, D.; Rattanachata, A.; Greer, A.A.; Ciston, J.; Ophus, C.; Rijnders, Augustinus J.H.M.; Blank, David H.A.; Doennig, D.; Pentcheva, R.; Kortright, J.B.; Schneider, C.M.; Ebert, H.; Fadley, C.S.

    2013-01-01

    Angle-resolved photoemission spectroscopy (ARPES) is a powerful technique for the study of electronic structure, but it lacks a direct ability to study buried interfaces between two materials. We address this limitation by combining ARPES with soft X-ray standing-wave (SW) excitation (SWARPES), in

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

    International Nuclear Information System (INIS)

    Tranquada, J.M.

    2008-01-01

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

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

    International Nuclear Information System (INIS)

    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.

    2015-01-01

    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

  8. Feasibility study for PTV measurement using x-ray holography

    International Nuclear Information System (INIS)

    Uemura, Tomomasa; Yamamoto, Yasufumi; Murata, Shigeru; Nishio, Shigeru; Iguchi, Manabu; Uesugi, Kentaro

    2005-01-01

    Some X-ray imaging techniques are examined for a feasibility study for micro-PIV in this study. There are three X-ray imaging method, the absorption contrast method, the refraction contrast method, and the phase contrast method. The first one is a common method but its spatial resolution is rather poor. The 2nd method corresponds to the Schlieren method that utilizes refraction of parallel light. The characteristics of the method, edge enhancement, can be effective in extracting tracer images. The third method is a kind of holography methods, and this method can record fine tracer particles. Among the three methods, the second and the third method are seemed to be applicable to PIV imaging, and those methods need a parallel X-ray. The SPring-8, the synchrotron radiation facility in Harima, is utilized. There are some methods to realize phase contrast image, most of them requires ultra-high precision in optical alignment. In the present study, though a coherent source is indispensable, the simplest and robust holography method, the inline holography, is used to take phase contrast pictures. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-01

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

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

    Science.gov (United States)

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

    2010-10-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  12. Analysis of low-angle x-ray scattering peaks from lyophilized biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Desouky, Omar S. [Radiation Physics Department, National Center for Radiation Research and Technology, A.E.A., Cairo (Egypt)]. E-mail: omardesouky@yahoo.com; Elshemey, Wael M. [Biophysics Department, Faculty of Science, Cairo University (Egypt); Selim, Nabila S.; Ashour, Ahmed H. [Radiation Physics Department, National Center for Radiation Research and Technology, A.E.A., Cairo (Egypt)

    2001-08-01

    Low-angle x-ray scattering (LAXS) from lyophilized blood and its constituents is characterized by the presence of two peaks in the forward direction of scattering. These peaks are found to be sensitive to the variations in the molecular structure of a given sample. The present work aims to explore the nature of LAXS from a variety of lyophilized biological samples. It also aims to investigate the possibility that a certain biological macromolecule is responsible of the production of LAXS peaks. This is carried out through measurements of LAXS from complex biological samples and their basic constituents. Among the measured samples are haemoglobin (Hb), globin, haem, packed red blood cells, bovine albumin, egg albumin, milk, casein, glutamine, alanine, fat, muscle and DNA. A table containing some characteristic parameters of the LAXS profiles of these samples is also presented. Analysis of measured profiles shows that all lyophilized samples produce at least one relatively broad peak at a scattering angle around 10.35 deg. The full width at half maximum (FWHM) of this peak varies considerably among the measured samples. Except for milk and casein, one additional peak at a scattering angle around 4.65 deg. is observed only in the LAXS profiles of proteins or protein-rich samples. This fact strongly suggests protein to be the biological macromolecule from which this characteristic peak originates. The same idea is further strengthened through discussion of some previous observations. (author)

  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)

    Sayers, D.E.

    1987-01-01

    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 Nd 2 Fe 14 B, 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. Small-Angle X-ray and Neutron Scattering Study on Microphase Separation Induced by Non-Solvent in a Semi-Dilute Solution of an Ultra-High-Molecular-Weight Block Copolymer

    International Nuclear Information System (INIS)

    Okamoto, Shigeru

    2009-01-01

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

  15. Spectroscopic Studies of X-Ray Binary Pulsars

    Indian Academy of Sciences (India)

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

    X-ray spectra of black hole binaries and active galactic nuclei show a non- thermal power law spectra extended over wide energy range toward hard X-rays to γ-rays. In contrast to these X-ray sources, XBPs fundamentally show a power law spectra with photon indices 1–2 with high-energy turnover at relatively low energies.

  16. In Situ Local Contact Angle Measurement in a CO2-Brine-Sand System Using Microfocused X-ray CT.

    Science.gov (United States)

    Lv, Pengfei; Liu, Yu; Wang, Zhe; Liu, Shuyang; Jiang, Lanlan; Chen, Junlin; Song, Yongchen

    2017-04-11

    The wettability of porous media is of major interest in a broad range of natural and engineering applications. The wettability of a fluid on a solid surface is usually evaluated by the contact angle between them. While in situ local contact angle measurements are complicated by the topology of porous media, which can make it difficult to use traditional methods, recent advances in microfocused X-ray computed tomography (micro-CT) and image processing techniques have made it possible to measure contact angles on the scale of the pore sizes in such media. However, the effects of ionic strength, CO 2 phase, and flow pattern (drainage or imbibition) on pore-scale contact angle distribution are still not clear and have not been reported in detail in previous studies. In this study, we employed a micro-CT scanner for in situ investigation of local contact angles in a CO 2 -brine-sand system under various conditions. The effects of ionic strength, CO 2 phase, and flow pattern on the local contact-angle distribution were examined in detail. The results showed that the local contact angles vary over a wide range as a result of the interaction of surface contaminants, roughness, pore topology, and capillarity. The wettability of a porous surface could thus slowly weaken with increasing ionic strength, and the average contact angle could significantly increase when gaseous CO 2 (gCO 2 ) turns into supercritical CO 2 (scCO 2 ). Contact angle hysteresis also occurred between drainage and imbibition procedures, and the hysteresis was more significant under gCO 2 condition.

  17. Cosmic x ray physics

    Science.gov (United States)

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

    1991-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-01

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

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

    Science.gov (United States)

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

    2017-02-16

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

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

    Science.gov (United States)

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

    2016-07-11

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

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

    International Nuclear Information System (INIS)

    Bolze, J.

    2011-01-01

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

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

    International Nuclear Information System (INIS)

    Gordelij, V.I.; Lushchikov, V.I.; Syrykh, A.G.; Cherezon, V.G.

    1991-01-01

    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

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

    Directory of Open Access Journals (Sweden)

    Dritan Siliqi

    2018-02-01

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

  4. 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

    2014-12-14

    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 Sr(2+)) 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.

  5. 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.; Jonker, P.G.; Keek, L.; Verbunt, F.W.M.; Méndez, M.; Markwardt, C.B.

    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

  6. Oxides neutron and synchrotron X-ray diffraction studies

    CERN Document Server

    Sosnowska, I M

    1999-01-01

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

  7. Diagnosis of secondary caries in esthetic restorations: influence of the incidence vertical angle of the X-ray beam.

    Science.gov (United States)

    Moreira, Patrícia Lima; Messora, Michel Reis; Pereira, Stela Márcia; Almeida, Solange Maria de; Cruz, Adriana Dibo da

    2011-01-01

    The aim of this study was to evaluate the accuracy on the diagnosis of secondary caries-like lesions simulated on esthetic restorations of different materials, changing the incidence vertical angle (IVA) of the x-ray beam. Twenty human teeth received MOD inlay preparations. In the experimental group (n=10), a round cavity was made in the floor of the proximal box to simulate the caries-like lesion. All teeth were restored with 3 composite resins (Charisma, Filtek-Z250 and TPH-Spectrum) at 3 moments. Two radiographic images were acquired with 0º and 10º IVA. Ten observers evaluated the images using a 5-point confidence scale. Intra- and interobserver reliability was analyzed with the Interclass Correlation Coefficient and the diagnostic accuracy was evaluated using the area under the ROC curve (A(z)), Friedman test and Wilcoxon test (α=0.05). Higher accuracy values were obtained with 10º IVA (A(z)=0.66, Filtek-Z250>A(z)=0.56, TPH-Spectrum) compared to 0º (A(z)=0.55, Charisma>A(z)=0.37, TPH-Spectrum), though without statistically significant difference (p>0.05). The detection of secondary caries-like lesions simulated on esthetic restorations of different materials suffered no negative influence by changing the IVA of the x-ray beam.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-07-21

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

  9. A compact high vacuum heating chamber for in-situ x-ray scattering studies.

    Science.gov (United States)

    Bertram, F; Deiter, C; Pflaum, K; Seeck, O H

    2012-08-01

    A very compact multi purpose high vacuum heating chamber for x-ray scattering techniques was developed. The compact design allows the chamber to be installed on high precision diffractometers which usually cannot support heavy and/or large equipment. The chamber is covered by a Be dome allowing full access to the hemisphere above the sample which is required for in-plane grazing incident x-ray diffraction and out-off plane wide angle x-ray diffraction.

  10. A compact high vacuum heating chamber for in-situ x-ray scattering studies

    Energy Technology Data Exchange (ETDEWEB)

    Bertram, F.; Deiter, C.; Pflaum, K.; Seeck, O. H. [Hamburger Synchrotronstrahlungslabor am Deutschen Elektronen-Synchrotron, Notkestr. 85, 22607 Hamburg (Germany)

    2012-08-15

    A very compact multi purpose high vacuum heating chamber for x-ray scattering techniques was developed. The compact design allows the chamber to be installed on high precision diffractometers which usually cannot support heavy and/or large equipment. The chamber is covered by a Be dome allowing full access to the hemisphere above the sample which is required for in-plane grazing incident x-ray diffraction and out-off plane wide angle x-ray diffraction.

  11. X-MIME: An imaging x-ray spectrometer for detailed study of Jupiter's icy moons and the planet's x-ray aurora.

    Science.gov (United States)

    Elsner, R. F.; Ramsey, B. D.; Waite, J. H.; Rehak, P.; Johnson, R. E.; Cooper, J. F.; Swartz, D. A.

    2004-11-01

    Remote observations with the Chandra X-ray Observatory and the XMM-Newton Observatory have shown that the Jovian system is a source of x-rays with a rich and complicated structure. The planet's polar auroral zones and its disk are powerful sources of x-ray emission. Chandra observations revealed x-ray emission from the Io Plasma Torus and from the Galilean moons Io, Europa, and possibly Ganymede. The emission from the moons is due to bombardment of their surfaces by highly energetic magnetospheric protons, oxygen and sulfur ions. These ions excite atoms in their surfaces leading to fluorescent x-ray emission lines. Although the x-ray emission from the Galilean moons is faint when observed from Earth orbit, an imaging x-ray spectrometer in orbit around these moons, operating at 200 eV and above with 150 eV energy resolution, would provide a detailed mapping of the elemental composition in their surfaces. Here we describe the physical processes leading to x-ray emission from the surfaces of Jupiter's moons and the instrumental properties required to map the elemental composition of their surfaces. We describe the characteristics of X-MIME, an imaging x-ray spectrometer undergoing a feasibility study for the JIMO mission, with the ultimate goal of providing unprecedented x-ray studies of the elemental composition of the surfaces of Jupiter's icy moons and Io, as well as of Jupiter's auroral x-ray emission.

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

    NARCIS (Netherlands)

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

    2004-01-01

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

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

    DEFF Research Database (Denmark)

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

    2017-01-01

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

  14. Studies of dark energy with X-ray observatories.

    Science.gov (United States)

    Vikhlinin, Alexey

    2010-04-20

    I review the contribution of Chandra X-ray Observatory to studies of dark energy. There are two broad classes of observable effects of dark energy: evolution of the expansion rate of the Universe, and slow down in the rate of growth of cosmic structures. Chandra has detected and measured both of these effects through observations of galaxy clusters. A combination of the Chandra results with other cosmological datasets leads to 5% constraints on the dark energy equation-of-state parameter, and limits possible deviations of gravity on large scales from general relativity.

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

    International Nuclear Information System (INIS)

    Bateman, J.E.; Hobby, M.G.; Peacock, N.J.

    1980-02-01

    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.)

  16. 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...... for mobile applications, new materials with high gravimetric and volumetric storage capacity of hydrogen have to be developed. Alkali alanates are promising for hydrogen storage materials. Sodium alanate stores hydrogen reversibly at moderate conditions when catalysed with, e.g. titanium, whereas potassium...

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

    International Nuclear Information System (INIS)

    Lin, Yuan; Samei, Ehsan; Ramirez-Giraldo, Juan Carlos; Gauthier, Daniel J.; Stierstorfer, Karl

    2014-01-01

    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

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

    Science.gov (United States)

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

    2016-09-01

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-09-15

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

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

    International Nuclear Information System (INIS)

    Ericson, Agneta.

    1989-01-01

    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, K dl . The results indicate that the Schlenk equilibrium is present in these solutions, however, in an extended form. In diethyl ether solution, where MgX 2 does not dissociate, no MgX 2 complex and thereby no Schlenk equilibrium has been observed. In tetrahydrofuran solution MgI 2 has dissociated into mainly MgI + and I - . This indicates that the concentration of MgI 2 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.)

  2. 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)

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

    International Nuclear Information System (INIS)

    Barbosa, Caroline M.; Azeredo, Soraia R.; Lopes, Ricardo T.; Souza, Sheila M.F.M de

    2013-01-01

    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 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)

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

    Science.gov (United States)

    Balogh, Joakim; Pedersen, Jan Skov

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

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

    Science.gov (United States)

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

    2012-11-01

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

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

    Science.gov (United States)

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

    2000-04-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-03-29

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

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

    Science.gov (United States)

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

    2017-04-01

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

  10. 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.

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

    International Nuclear Information System (INIS)

    Li Qingshan; Duan Tao; Wang Xiaoyun; Zhao Li; Dong Jian; Wei Lei

    2010-01-01

    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)

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

    Czech Academy of Sciences Publication Activity Database

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

    2017-01-01

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

  13. Study of x-ray CCD image sensor and application

    Science.gov (United States)

    Wang, Shuyun; Li, Tianze

    2008-12-01

    In this paper, we expounded the composing, specialty, parameter, its working process, key techniques and methods for charge coupled devices (CCD) twice value treatment. Disposal process for CCD video signal quantification was expatiated; X-ray image intensifier's constitutes, function of constitutes, coupling technique of X-ray image intensifier and CCD were analyzed. We analyzed two effective methods to reduce the harm to human beings when X-ray was used in the medical image. One was to reduce X-ray's radiation and adopt to intensify the image penetrated by X-ray to gain the same effect. The other was to use the image sensor to transfer the images to the safe area for observation. On this base, a new method was presented that CCD image sensor and X-ray image intensifier were combined organically. A practical medical X-ray photo electricity system was designed which can be used in the records and time of the human's penetrating images. The system was mainly made up with the medical X-ray, X-ray image intensifier, CCD vidicon with high resolution, image processor, display and so on. Its characteristics are: change the invisible X-ray into the visible light image; output the vivid images; short image recording time etc. At the same time we analyzed the main aspects which affect the system's resolution. Medical photo electricity system using X-ray image sensor can reduce the X-ray harm to human sharply when it is used in the medical diagnoses. At last we analyzed and looked forward the system's application in medical engineering and the related fields.

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

    Science.gov (United States)

    Shtykova, E. V.; Bogacheva, E. N.; Dadinova, L. A.; Jeffries, C. M.; Fedorova, N. V.; Golovko, A. O.; Baratova, L. A.; Batishchev, O. V.

    2017-11-01

    A complex structural analysis of nuclear export protein NS2 (NEP) of influenza virus A has been performed using bioinformatics predictive methods and small-angle X-ray scattering data. The behavior of NEP molecules in a solution (their aggregation, oligomerization, and dissociation, depending on the buffer composition) has been investigated. It was shown that stable associates are formed even in a conventional aqueous salt solution at physiological pH value. For the first time we have managed to get NEP dimers in solution, to analyze their structure, and to compare the models obtained using the method of the molecular tectonics with the spatial protein structure predicted by us using the bioinformatics methods. The results of the study provide a new insight into the structural features of nuclear export protein NS2 (NEP) of the influenza virus A, which is very important for viral infection development.

  16. Evolution of the characteristics of Parametric X-ray Radiation from textured polycrystals under different observation angles

    Science.gov (United States)

    Alekseev, V. I.; Eliseyev, A. N.; Irribarra, E.; Kishin, I. A.; Klyuev, A. S.; Kubankin, A. S.; Nazhmudinov, R. M.; Zhukova, P. N.

    2018-02-01

    The Parametric X-Ray radiation (PXR) spectra and yield dependencies on the orientation angle are measured during the interaction of 7 MeV electrons with a tungsten textured polycrystalline foil for different observation angles. The effects of PXR spectral density increase and PXR yield orientation dependence broadening in the backward direction is shown experimentally for the first time. The experimental results are compared with PXR kinematical theories for both mosaic crystals and polycrystals.

  17. A quality measurement study of a diagnostic x-ray

    International Nuclear Information System (INIS)

    Nishitani, Motohiro; Fujimoto, Nobuhisa; Yamada, Katsuhiko

    1982-01-01

    It is important to check periodically the quality and quantity of the X-rays emitted, in order to obtain the best possible performance from your diagnostic X-ray apparatus. The best way of checking the exact quality of the X-ray is to measure the spectrum of the X-ray, but it is not an easy task to carry out. The second way is to plot the attenuation curve of the X-rays. We have developed a method to plot the attenuation curve by a single exposure, utilizing J.r. Greening's empirical formula. The output of the three cavity ionization chambers, one with 7 mmAl filter, another with a 3 mmAl and the third without any filter, exposed to the same X-ray, were put into a microcomputer. The programming was arranged to display the attenuation curve of the X-rays, effective energy of the X-rays, the 1st HVL and the 2nd HVL on the CRT. The attenuation curves of the X-rays, emitted at a tube voltage at between 60 and 140 kV obtained by this method, agreed with the experimental results with an error of +-4 %. The effective energy obtained by this method agreed with the experimental data with an error of +-1 %. (author)

  18. X-ray diffraction studies of NbTe 2 single crystal

    Indian Academy of Sciences (India)

    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 ...

  19. Use of wide-angle X-ray diffraction to measure shape and size of dispersed colloidal particles.

    Science.gov (United States)

    Qazi, S Junaid S; Rennie, Adrian R; Cockcroft, Jeremy K; Vickers, Martin

    2009-10-01

    Laboratory X-ray diffraction is used to investigate the size and shape of dispersed plate-like and spherical colloidal particles. Analysis of the wide-angle diffraction data provides information about the size and shape of crystals from the width of the Bragg peaks according to the Debye-Scherrer formula. The measurements, data analysis, and evaluation are discussed. It is shown that X-ray diffraction with conventional laboratory equipment on dispersed particles is feasible as a tool to determine both particle size and shape. Data for two samples--gold colloids and nickel (II) hydroxide particles are presented. The advantages and limitations of the method are discussed. X-ray diffraction measurements that are made in combination with dynamic light scattering can be used to estimate the thickness of stabilizing layers of polymers.

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

    Science.gov (United States)

    Chen, Sen; Luo, Sheng Nian

    2018-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Sen; Luo, Sheng-Nian (Jiaotong); (Peac)

    2018-02-16

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

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

  3. Spectroscopic Studies of X-Ray Binary Pulsars

    Indian Academy of Sciences (India)

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

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

  4. High-k Gate Dielectric Films Studied by Extremely Asymmetric X-ray Diffraction and X-ray Photoelectron Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ito, Yuki [Graduate School of Engineering, Nagoya University, Nagoya, 464-8603 (Japan); Akimoto, Koichi [Graduate School of Engineering, Nagoya University, Nagoya, 464-8603 (Japan); Yoshida, Hironori [Graduate School of Engineering, Nagoya University, Nagoya, 464-8603 (Japan); Emoto, Takashi [Toyota National College of Technology, Toyota, Aichi 471-8525 (Japan); Kobayashi, Daisuke [Institute of Space and Astronautical Science, Sagamihara, Kanagawa 229-8510 (Japan); Hirose, Kazuyuki [Institute of Space and Astronautical Science, Sagamihara, Kanagawa 229-8510 (Japan)

    2007-10-15

    We studied HfAlO{sub x}(N)/SiO{sub 2}/Si films which were fabricated by the layer-by-layer deposition and annealing (LL-D and A) method with different annealing conditions. In this time, in-situ annealing was performed at various temperatures in an NH{sub 3} ambient. In addition, post-deposition annealing (PDA) was performed for some samples. For each sample, the interfacial lattice strain was evaluated using extremely asymmetric X-ray diffraction and the local dielectric constant near the Al atoms was measured by X-ray photoelectron spectroscopy (XPS). Observation of the strain field was done by measuring the X-ray rocking curve of the Si 113 reflection of the Si (001) substrate under grazing incidence conditions. It was found that in the case of the samples without PDA, for higher in-situ annealing temperatures compressive strain is introduced and the local dielectric constant becomes lower. For the samples with PDA, the differences of the lattice strain and the local dielectric constant are small for different in-situ annealing temperatures.

  5. Synchrotron X-Ray Radiation and Deformation Studies

    DEFF Research Database (Denmark)

    Fæster Nielsen, Søren

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

  6. Final Report - X-ray Studies of Highly Correlated Systems

    Energy Technology Data Exchange (ETDEWEB)

    Burns, Clement [Western Michigan Univ., Kalamazoo MI (United States)

    2017-11-27

    The overall goal of the research was to improve the capabilities of x-ray synchrotron instrumentation to enable cutting-edge research in condensed matter physics. The main goal of the current grant cycle was to find a method to measure the polarization of the scattered x-ray in resonant inelastic x-ray scattering. To do this, we developed a polarization analysis apparatus using a thin, toroidally bent single crystal, which could be set to reflect one or the other of the two polarization components in the scattered x-ray beam. Resonant x-ray scattering measurements were also carried out on interfaces and the charge density wave in high temperature superconducting materials.

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

    Science.gov (United States)

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

    2000-01-01

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

  8. Low-energy x-ray irradiation for electrophysiological studies

    Energy Technology Data Exchange (ETDEWEB)

    Schauer, D.A.; Zeman, G.H.; Pellmar, T.C.

    1989-01-01

    High-dose-rate acute whole-body exposures have been the main focus of radiobiology research conducted at the Armed Forces Radiobiology Research Institute (AFRRI) for many years. Extensive quantitative studies have been conducted analyzing behavioral effects, radiation-induced syndromes, and combined injury phenomena. Tolliver and Pellmar initiated a study to evaluate radiation damage to brain neurophysiology. A 50-kVp molybdenum target/filter x-ray tube was installed inside a lead-shielded Faraday cage. High-dose rates of up to 1.54 Gy/min (17.4-keV weighted average photons) were used to conduct local in vitro irradiations of the hippocampal region of guinea pig brains. Electrophysiological recordings of subtle changes in neuronal activity indicate this system is suitable for this application.

  9. Study of brain atrophy using X-ray computed tomography

    International Nuclear Information System (INIS)

    Kawabata, Masayoshi

    1987-01-01

    Cerebrospinal fluid space-cranial cavity ratio (CCR) of 811 subjects with no brain damage were investigated using X-ray computed tomography. Brain volume of healthy adults aged 20 - 59 years was almost constant and decreased gradually after 60 years. CCR of men aged 20 - 49 years kept constant value and increased with aging after 50 years. CCR of women aged 20 - 59 years kept equal value and CCR increased with aging after 60 years. Brain atrophy with aging was investigated in this study also. In retrospective study, CCR of patients in any age diagnosed brain atrophy in daily CT reports were beyond the normal range of CCR of healthy subjects aged 20 - 49 years. In 48 patients with Parkinson's disease, almost of CCR of them were included within normal range of CCR in age-matched control. (author)

  10. Feasibility study on X-ray source with pinhole imaging method

    International Nuclear Information System (INIS)

    Qiu Rui; Li Junli

    2007-01-01

    In order to verify the feasibility of study on X-ray source with pinhole imaging method, and optimize the design of X-ray pinhole imaging system, an X-ray pinhole imaging equipment was set up. The change of image due to the change of the position and intensity of X-ray source was estimated with mathematical method and validated with experiment. The results show that the change of the spot position and gray of the spot is linearly related with the change of the position and intensity of X-ray source, so it is feasible to study X-ray source with pinhole imaging method in this application. The results provide some references for the design of X-ray pinhole imaging system. (authors)

  11. Physical methods for studying minerals and solid materials: X-ray, electron and neutron diffraction; scanning and transmission electron microscopy; X-ray, electron and ion spectrometry

    International Nuclear Information System (INIS)

    Eberhart, J.-P.

    1976-01-01

    The following topics are discussed: theoretical aspects of radiation-matter interactions; production and measurement of radiations (X rays, electrons, neutrons); applications of radiation interactions to the study of crystalline materials. The following techniques are presented: X-ray and neutron diffraction, electron microscopy, electron diffraction, X-ray fluorescence analysis, electron probe microanalysis, surface analysis by electron emission spectrometry (ESCA and Auger electrons), scanning electron microscopy, secondary ion emission analysis [fr

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

    Science.gov (United States)

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

    2017-12-01

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

  13. Counter tube window and X-ray fluorescence analyzer study

    Science.gov (United States)

    Hertel, R.; Holm, M.

    1973-01-01

    A study was performed to determine the best design tube window and X-ray fluorescence analyzer for quantitative analysis of Venusian dust and condensates. The principal objective of the project was to develop the best counter tube window geometry for the sensing element of the instrument. This included formulation of a mathematical model of the window and optimization of its parameters. The proposed detector and instrument has several important features. The instrument will perform a near real-time analysis of dust in the Venusian atmosphere, and is capable of measuring dust layers less than 1 micron thick. In addition, wide dynamic measurement range will be provided to compensate for extreme variations in count rates. An integral pulse-height analyzer and memory accumulate data and read out spectra for detail computer analysis on the ground.

  14. Biological Dosimetry of X-rays by micronuclei study

    International Nuclear Information System (INIS)

    Gomez, E.; Silva, A.; Navlet, J.

    1991-01-01

    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

  15. Biological dosimetry of X-rays by micronuclei study

    International Nuclear Information System (INIS)

    Gomez, E.; Silva, A.; Navlet, J.

    1991-01-01

    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 D 2 where. Y is the number micronuclei per cell and D the dose. the curve is compared with those produced elsewhere

  16. X-ray diffraction study of choline chloride's β form

    International Nuclear Information System (INIS)

    Petrouleas, V.; Lemmon, R.M.; Christensen, A.

    1978-01-01

    The organic salt choline chloride exists in two crystalline polymorphs. One (the α form) is extraordinarily sensitive to ionizing radiation, the other (the β form) is not. The present report describes an x-ray diffraction study of the β form. The structure has been found to be highly disordered face centered cubic. A reasonable least-square refinement of the intensity data has been achieved in the centrosymmetric space group Fm3 or Fm3m by use of a molecular model with restrained bond lengths. The results show that in the β form the electronic density due to the choline cation is closely spaced around the N, so that hydrogen bonding to the chloride is unlikely. Comparison with infrared and NMR data indicates that the disordering is dynamic and can be ascribed to rotations of the choline ion around crystallographic symmetry axes. Possible connections of these results with the radiation stability of the β form are discussed

  17. 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.

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

    Science.gov (United States)

    Frost, Anja; Renners, Eike; Hötter, Michael; Ostermann, Jörn

    2013-01-01

    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. PMID:23344378

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

    Energy Technology Data Exchange (ETDEWEB)

    Someya, Misao (Showa Univ., Tokyo (Japan). School of Medicine)

    1992-04-01

    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/cm[sup 2] 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).

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

    Science.gov (United States)

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

    2017-06-01

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

  1. X-ray Spectromicroscopy Studies of Nanoparticles in the Environment

    Science.gov (United States)

    Sedlmair, J.; Gleber, S.-C.; Schirz, A.; Zanker, H.; Thieme, J.

    2009-04-01

    Motivation: In recent time, carbon nanotubes (CNTs) have drawn a lot of attention due to their unique properties and due to that possible application, for instance in pharmacology, material sciences or as semiconductors. CNTs are tubes with diameters in the nanometer scale, but with lengths up to several millimeters. Their walls consist of carbon atoms, each bound to three other carbon atoms (sp2-hybridization), which results in a hexagonal honeycomb-like structure. They can also be functionalized, e.g. with carboxyl- or hydroxyl groups. Although the production and modification of CNTs in sizable quantities have been improved continuously, the characterization of these nano-particles still needs to be advanced. Additionally, the ecological aspect comes into account. Since most of these new materials consist of particles too small to be biodegraded, it is important to analyze the impact of CNTs on the environment (and biomolecular matter in general). Here we present the result of a study of pristine and functionalized carbon nanotubes (CNTs) using the x-ray scanning transmission microscope (STXM) at the storage ring BESSY II in Berlin for a NEXAFS (near edge x-ray absorption spectroscopy) analysis with spatial resolution. Experiment and results: We characterized three types of multi-walled CNTs (3-15 walls, outer diameter of 13-16 nm and length distribution 1-10 nm) by x-ray spectromicroscopy. To be more specific, we have investigated different CNT-samples with energies around the C1s K-shell edge (~284 eV) dry and in aqueous environment at ambient conditions. Using the STXM, the spatial information from the x-ray image with a pixel size of 50 nm can be combined with NEXAFS-spectra[5] of each pixel of the image area. The differences between the species are observable both in the microscopic images and the spectral data. The evaluation[1][2] of the NEXAFS-spectra yields information about the chemical bindings in the sample. Discussion The difference between the

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

    Science.gov (United States)

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

    2012-04-01

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

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

    Science.gov (United States)

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

    2017-04-01

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

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

    International Nuclear Information System (INIS)

    Zinke, M.

    1979-01-01

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

  5. A = Rb, K: Single crystal X-ray diffraction studies

    Indian Academy of Sciences (India)

    Unknown

    X-ray diffraction on structural phase transition. 475. Figure 2. Powder X-ray diffraction pattern of KLHS at 298 and 100 K. 3. Structure determination and refinement. 3.1 Structure of RLHS at 293 K. A crystal of size 0⋅7 × 0⋅3 × 0⋅4 mm was mounted on a BRUKER AXS SMART APEX. CCD9 diffractometer with a crystal to ...

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

    Energy Technology Data Exchange (ETDEWEB)

    MacMillan, S.C.; Roberts, K.J.; Wells, M.; Polgreen, M.; Smith, I. [Heriot-Watt University, Edinburgh, (United Kingdom). Department of Mechanical and Chemical Engineering, Centre for Molecular and Interface Engineering

    1999-12-01

    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

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

    International Nuclear Information System (INIS)

    MacMillan, S.C.; Roberts, K.J.; Wells, M.; Polgreen, M.; Smith, I.

    1999-01-01

    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

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

    International Nuclear Information System (INIS)

    Nordenskjöld, A.C.; Palme, M.; Kaijser, M.

    2015-01-01

    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

  9. Studies on low-voltage x-ray radiography for graphite materials

    International Nuclear Information System (INIS)

    Muraoka, Susumu; Itami, Hiroharu

    1978-09-01

    Low-voltage radiography has been studied to provide optimum technique for graphite less than 50 mm thick. First we determined the exposure conditions under which the most appropriate photographic density can be obtained. By parametric studies, an exposure chart was prepared. Then we studied how the environment of photographing affected the film density. Thirdly, by use of graphite materials with artificial flaws, Image Quality Indicator (I.Q.I.) sensitivity was determined. Detectability of a crack depended on an incidence angle of X-rays onto a crack. Finally, we photographed graphites having natural flaws and gained a useful information. (author)

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

    Science.gov (United States)

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

    2016-07-01

    A number of high priority subjects in astrophysics can be addressed by a state-of-the-art soft x-ray grating spectrometer, such as the role of Active Galactic Nuclei in galaxy and star formation, characterization of the Warm-Hot Intergalactic Medium and the missing baryon problem, characterization of halos around the Milky Way and nearby galaxies, as well as stellar coronae and surrounding winds and disks. An Explorer-scale, largearea (> 1,000 cm2), high resolving power (R =λ/Δλ > 3,000) soft x-ray grating spectrometer is highly feasible based on Critical-Angle Transmission (CAT) grating technology, even for telescopes with angular resolution of 5-10 arcsec. Still, significantly higher performance can be provided by a CAT grating spectrometer 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 conventional transmission gratings (lowmass, relaxed alignment tolerances and temperature requirements, transparent at higher energies) with minimalmission resource requirements. They are high-efficiency blazed transmission gratings that consist of freestanding, ultra-high aspect-ratio grating bars fabricated from silicon-on-insulator (SOI) wafers using advanced anisotropic dry and wet etch techniques. Blazing is achieved through grazing-incidence reflection off the smooth grating bar sidewalls. The reflection properties of silicon are well matched to the soft x-ray band, and existing silicon CAT gratings can exceed 30% absolute diffraction efficiency, with clear paths for further improvement. Nevertheless, CAT gratings with sidewalls made of higher atomic number elements allow extension of the CAT grating principle to higher energies and larger dispersion angles, thus enabling higher resolving power at shorter wavelengths. We show x-ray data from CAT gratings coated with a thin layer of platinum using atomic layer deposition, and demonstrate efficient

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

    International Nuclear Information System (INIS)

    Nagler, S.E.

    1991-01-01

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

  12. Theoretical Study on Angular Dependence of X-ray Natural Circular Dichroism

    Science.gov (United States)

    Katsumoto, Hiroshi; Fujii, Hitoshi; Oguchi, Tamio

    Natural circular dichroism (NCD) can be detected as a difference in the photo-absorption between right- and left-circularly polarized lights in a non-centrosymmetric crystal. It originates in an interference term of electric dipole (E1) and magnetic dipole (M1) transitions in optical ranges, while in that of E1 and electric quadruple (E2) transition in x-ray ranges. In the latter case, the electronic transitions occur from particular inner core states to empty conduction bands depending on the x-ray energy and polarization, being called selection rules. To cause such an interference, the final states should be parity violated because of the selection rules for the E1 and E2 transitions. In this study, we calculate x-ray NCD (XNCD) spectra by using density-functional-theory electronic structure calculation method and Fermi's golden rule for LiIO3 (space group P63) and TeO2 (P212121). The dependence of the incident angle in the XNCD spectra is calculated and discussed in detail by comparing with its analytic expression.

  13. X-ray photoemission spectroscopy (XPS) and extended x-ray absorption fine structure (EXAFS) studies of silicate based glasses

    International Nuclear Information System (INIS)

    Karim, D.; Lam, D.J.

    1979-01-01

    The application of the x-ray photoemission spectroscopy (XPS) technique to study the electronic structure and bonding of heavy metal oxides in alkali- and alkali-earth-silicate glasses had been demonstrated. The bonding characteristics of the iron oxide and uranium oxide in sodium silicate glasses were deduced from the changes in the oxygen 1s levels and the heavy metal core levels. It is reasonable to expect that the effect of leaching on the heavy metal ions can be monitored using the appropriate core levels of these ions. To study the effect of leaching on the glass forming network, the valence band structure of the bridging and nonbridging oxygens in sodium silicate glasses were investigated. The measurement of extended x-ray absorption fine-structure (EXAFS) is a relatively new analytical technique for obtaining short range (<5 A) structural information around atoms of a selected species in both solid and fluid systems. Experiments have recently begun to establish the feasibility of using EXAFS to study the bonding of actinides in silicate glasses. Because of the ability of EXAFS to yield specific structural data even in complex multicomponent systems, it could prove to be an invaluable tool in understanding glass structure

  14. Energetic electron pitch angle distribution parameters at 6.6 Re, as deduced from GOES X-ray observations

    Science.gov (United States)

    Garcia, H. A.

    1996-05-01

    X-ray sensors that measure the Sun's radiant output in two soft X-ray channels, 1-8 and 0.5-4 Å, are carried on all GOES geostationary equatorial weather satellites. A comparison of X-ray measurements from two co-operational GOES reveals a systematic difference signal that shows periodic diurnal and seasonal variations. These effects are seen during geomagnetically quiet times as well as disturbed times and are most noticeable when solar activity is low to moderate. The GOES orbit lies just above the main outer electron belt of the van Allen radiation belts but it falls inside the region containing >2MeV trapped electrons; thus the local particle environment includes electrons of sufficient energy to cause significant Bremsstrahlung on the walls of the ion chamber as well as direct deposition of energy through the entrance aperture. These background effects occur despite passive shielding of the ion chambers and in-orbit electronic suppression of the spurious particle contribution. However, because of the regularity of the difference signal it is possible to exploit this X-ray contaminant to infer certain properties of the energetic electron pitch angle distribution in anisotropy and in local time, on the assumption that these energetic electrons are responsible for the spurious X-ray detector response. The basic attributes of the observed diurnal and seasonal effects can be re-created in a model that incorporates a tilted dipole magnetosphere and local-time-dependent, generic pitch angle distributions. It is possible to infer the anisotropy index, n, for dayside sin n(α) distributions and the anisotropy index, m, for nightside sin m(2α) butterfly distributions as well as the local times where these distributions convert from normal loss-cone to butterfly in the afternoon and return to normal loss-cone in the morning. Examples of the diurnal and seasonal variations in the observed X-ray difference signal are shown, and these waveforms are re-created by a model

  15. Bismuth X-ray absorber studies for TES microcalorimeters

    Energy Technology Data Exchange (ETDEWEB)

    Sadleir, J.E. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States) and University of Illinois Physics Department, Urbana, IL 61801 (United States)]. E-mail: sadleir@milkyway.gsfc.nasa.gov; Bandler, S.R. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Brekosky, R.P. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Chervenak, J. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Figueroa-Feliciano, E. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Finkbeiner, F. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Iyomoto, N. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Kelley, R.L. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Kilbourne, C.A. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); King, J.M. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Porter, F.S. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Robinson, I.K. [University of Illinois Physics Department, Urbana, IL 61801 (United States); Saab, T. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Talley, D.J. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States)

    2006-04-15

    Bismuth's large atomic number and low carrier density makes it an attractive X-ray absorber material for microcalorimeters. Bismuth's long Fermi wavelength and long mean free paths have motivated much interest in the fabrication of high quality bismuth films to study quantum size effects. Despite such incentives, fabrication of high quality bismuth films has proven difficult, and measured properties of such films are highly variable in the literature. Implementing a bismuth deposition process for TES (superconducting Transition Edge Sensor) device fabrication presents additional challenges particularly at interfaces due to the inherent granularity and surface roughness of its films, its low melting point, and its tendency to diffuse and form undesired intermetallic phases. We report observations of Bi-Cu and Bi-Au diffusion in our devices correlating with large shifts in T{sub c} (superconducting transition temperature). Using SEM and in situ R vs T annealing experiments we have been able to study these diffusion processes and identify their activation temperatures.

  16. Hard X-ray studies on the Castor tokamak

    International Nuclear Information System (INIS)

    Mlynar, J.

    1990-04-01

    The electron runaway processes in tokamaks are discussed with regard to hard X radiation measurements. The origin and confinement of runaway electrons, their bremsstrahlung spectra and the influence of lower hybrid current drive on the distribution of high-energy electrons are analyzed for the case of the Castor tokamak. The hard X-ray spectrometer designed for the Castor tokamak is also described and preliminary qualitative results of hard X-ray measurements are presented. The first series of integral measurements made it possible to map the azimuthal dependence of the hard X radiation

  17. Observational studies of X-ray binary systems

    International Nuclear Information System (INIS)

    Klis, M. van der.

    1983-01-01

    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.)

  18. 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...... inside the selected grain is performed with an angular resolution of 0:005o and a spatial resolution of 200 nm. Furthermore, the speed of the measurements at high- intensity synchrotron facilities allows for fast non-destructive in situ determination of structural changes induced by annealing or other...

  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 to the subst......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. Atomic structure of large angle grain boundaries determined by quantitative X-ray diffraction techniques

    International Nuclear Information System (INIS)

    Fitzsimmons, M.R.; Sass, S.L.

    1988-01-01

    Quantitative X-ray diffraction techniques have been used to determine the atomic structure of the Σ = 5 and 13 [001] twist boundaries in Au with a resolution of 0.09 Angstrom or better. The reciprocal lattices of these boundaries were mapped out using synchrotron radiation. The atomic structures were obtained by testing model structures against the intensity observations with a chi square analysis. The boundary structure were modeled using polyhedra, including octahedra, special configurations of tetrahedra and Archimedian anti-prisms, interwoven together by the boundary symmetry. The results of this work point to the possibility of obtaining general rules for grain boundary structure based on X-ray diffraction observations that give the atomic positions with high resolution

  1. Titanium Dioxide Nanoparticles: Synthesis, X-Ray Line Analysis and Chemical Composition Study

    OpenAIRE

    Chenari,Hossein Mahmoudi; Seibel,Christoph; Hauschild,Dirk; Reinert,Friedrich; Abdollahian,Hossein

    2016-01-01

    TiO$_{2}$ nanoparticleshave been synthesized by the sol-gel method using titanium alkoxide and isopropanolas a precursor. The structural properties and chemical composition of the TiO$_{2}$ nanoparticles were studied usingX-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy.The X-ray powder diffraction pattern confirms that the particles are mainly composed of the anatase phase with the preferential orientation along [101] direction.The physical parameters suc...

  2. 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.

  3. X-ray photoelectron spectroscopy (XPS) studies of rhenium catalyst

    International Nuclear Information System (INIS)

    Mohd Ambar Yarmo; Che Seman Mahmood

    2000-01-01

    Rhenium oxide on alumina (Re 2 O 7 /Al 2 O 3 ) is a very active catalyst system for olefin metathesis reaction. The catalyst can be prepared by wet impregnation of ammonium perrhenate (NH 4 ReO 4 ) solution onto alumina (γ-AI 2 O 3 ) support followed by drying and calcination in air. In this study, rhenium catalysts at different treatment conditions namely active, non-active and during propylene metathesis reaction were investigated using X-ray photoelectron spectroscopy (XPS) technique. Analysis of O 1s , photoelectron peak shows that some chemical interaction between rhenium oxides and the support have been established through Re-O-Al linkage. Analysis of Re 4f7/2 photoelectron peak by using a systematic deconvolution procedure, shows that the metal was in a mixed and varied oxidation states from Re(IV) to Re(VII) depending on their treatment condition. The presence of the metal-carbene complex, the reaction intermediate, could possibly be observed by analysing the C 1s , photoelectron peak. However, a much higher vacuum (i.e. 10 -10 - 10 -11 torr) is needed in the spectroscopy system in order to have the improved detection sensitivity. (Author)

  4. Cytogenetic studies with laser or X-ray exposures

    International Nuclear Information System (INIS)

    Bozduganov, A.; Genkov, P.

    1975-01-01

    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)

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

    Science.gov (United States)

    2016-12-01

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

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

    Science.gov (United States)

    2016-12-01

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

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

    CERN Document Server

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

    2013-01-01

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

  8. 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.

  9. The beginning of studies and use of X-rays in the Czech Lands

    International Nuclear Information System (INIS)

    Tesinska, E.; Hlava, A.; Zackova, H.

    1995-01-01

    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

  10. Experimental study on hard X-ray generation of relativistic electron beams in azimuthal magnetic field

    CERN Document Server

    Fan Ya Jun; Qiu Aici

    2002-01-01

    Experimental study on hard X-ray generation was carried out on Flash 2 accelerator, with the method of relativistic electron beams transported in a low pressure gas via azimuthal magnetic field and interacted with Ta target. At 47 cm transporting distance, the measured areal integral of hard X-ray dose rate was 2.1 x 10 sup 1 sup 0 Gy centre dot cm sup 2 /s, total areal integral of hard X-ray dose was 1843 Gy centre dot cm sup 2 , and X-ray convert rate was 108 Gy centre dot cm sup 2 /kJ

  11. Study of complex waveguide structure using soft X-ray reflectivity technique

    Science.gov (United States)

    Singh, Amol; Modi, Mohammed H.; Dhawan, R.; Jonnard, P.; Le Guen, K.; André, J.-M.

    2017-05-01

    Grazing incidence x-ray reflectivity (GIXRR) technique is commonly used for structural investigation of layered structures. In case of complex x-ray waveguide structure it is difficult to obtain structural parameters using GIXRR technique owing to narrowly spaced Kiessig fringes. We used GIXRR and soft x-ray reflectivity (SXR) technique to study the x-ray waveguide structure composed of 4 layers Al/ZrC/Al/W on a Si substrate. Structural parameters of the stacks, density, thickness and roughness of the layers, are determined through fitting of SXR data. Advantages of SXR over GIXRR for such layered structure are shown.

  12. 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).

  13. 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

  14. Study of semiconductor detectors applied to diagnostic X-ray

    International Nuclear Information System (INIS)

    Salgado, Cesar Marques

    2003-08-01

    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)

  15. X-ray scattering studies of lanthanides magnetism

    DEFF Research Database (Denmark)

    McMorrow, D.; Bohr, Jakob; Gibbs, D.

    1999-01-01

    Interest in the applications of X-ray synchrotron radiation has grown rapidly during the last decade. At the present time, intense, ultra-bright synchrotron radiation is available on a routine basis from third-generation sources located in Europe (ESRF), North America (APS) and Japan (Spring8). T...

  16. Experiment of optical axis angle of electro-optic crystal by conoscopic interference and x-ray diffraction method

    Science.gov (United States)

    Li, Dong; Liu, Yong; Liu, Xu; Jiang, Hongzhen; Zheng, Fanglan

    2017-10-01

    Owing to the advantages of low loss, high spatial uniformity and high damage threshold, plasma electrode pockels cell (PEPC) is the key element of multi-pass amplifying technology in large laser facilities. Properties of PEPC is directly affected by the optical axis angle of the electro-optic crystal. Therefore, high precision measurement of the optical axis angle is indispensable. X-ray diffraction analysis method is a traditional way to determine the direction of optical axis of crystal, which is presented. By using conoscopic interference technique, a measurement system for optical axis angle of electro-optic crystal is introduced. The principle of conoscopic interference method is described in detail, and a series of techniques are implied in this measurement system to improve the accuracy. The optical axis angle two different electro-optic crystal is measured by X-ray diffraction analysis method and our conoscopic interference measurement system, respectively. The absolute error is less than 0.01mrad, while the relative error is nearly 2%.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  20. A CMOS active pixel sensor system for laboratory- based x-ray diffraction studies of biological tissue

    International Nuclear Information System (INIS)

    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

    2008-01-01

    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

  1. Time-resolved structural studies at synchrotrons and X-ray free electron lasers: opportunities and challenges

    Science.gov (United States)

    Neutze, Richard; Moffat, Keith

    2012-01-01

    X-ray free electron lasers (XFELs) are potentially revolutionary X-ray sources because of their very short pulse duration, extreme peak brilliance and high spatial coherence, features that distinguish them from today’s synchrotron sources. We review recent time-resolved Laue diffraction and time-resolved wide angle X-ray scattering (WAXS) studies at synchrotron sources, and initial static studies at XFELs. XFELs have the potential to transform the field of time-resolved structural biology, yet many challenges arise in devising and adapting hardware, experimental design and data analysis strategies to exploit their unusual properties. Despite these challenges, we are confident that XFEL sources are poised to shed new light on ultrafast protein reaction dynamics. PMID:23021004

  2. X-ray diffraction and X-ray K absorption near edge studies of copper (II) complexes with amino acids

    Science.gov (United States)

    Sharma, P. K.; Mishra, Ashutosh; Malviya, Varsha; Kame, Rashmi; Malviya, P. K.

    2017-05-01

    Synthesis of copper (II) complexes [CuL1L2X].nH2O, where n=1, 2,3 (X=Cl,Br,NO3) (L1is 2,2’-bipyridine and L2 is L-tyrosine) by the chemical root method. The XRD data for the samples have been recorded. EXAFS spectra have also been recorded at the K-edge of Cu using the dispersive beam line BL-8 at 2.5 Gev Indus-2 Synchrotron radiation source at RRCAT, Indore, India. XRD and EXAFS data have been analysed using the computer software. X-ray diffraction studies of all complexes indicate their crystalline nature. Lattice parameter, bond length, particle size have been determined from XRD data.

  3. X-ray studies of pure and doped vanadium sesquioxide

    Energy Technology Data Exchange (ETDEWEB)

    Chen, S.

    1982-01-01

    The crystal structure of V/sub 2/O/sub 3/ was studied first with substitution by Cr/sub 2/O/sub 3/ from 0 to 5% Cr, then as a function of temperature, with 0.325% and 0.350% Cr content, from 23/sup 0/ to 550/sup 0/C; finally, the distribution of valence electron density in metallic V/sub 2/O/sub 3/ and insulating 1.0% Cr-V/sub 2/O/sub 3/ was mapped, using x-ray diffraction data from single crystals. Doping V/sub 2/O/sub 3/ with up to 1.25% Cr produces changes in structure consistent with a slight weakening of the bonding metal-metal interactions in the basal plane, leading to an increase in the metal-metal distances coupled with changes which maintain constant metal-oxygen distances. A discontinuity appears at about 1.25% Cr as the first-order transition from metal to insulating behavior occurs with increasing Cr content. No change in crystal symmetry accompanies this transformation. It appears that the metal-metal interactions are retained even in the insulating phase of Cr-doped V/sub 2/O/sub 3/. The distribution of valence electron density in metallic V/sub 2/O/sub 3/ and insulating 1.0% Cr-V/sub 2/O/sub 3/ are similar. Both show significant bonding interaction between near-neighboring metal atoms.

  4. Microbial biofilm study by synchrotron X-ray microscopy

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  5. 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)

    Simeone, D.; Gosset, D.; Bechade, J.L.

    2001-01-01

    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)

  6. 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...

  7. A new large solid angle multi-element silicon drift detector system for low energy X-ray fluorescence spectroscopy

    Science.gov (United States)

    Bufon, J.; Schillani, S.; Altissimo, M.; Bellutti, P.; Bertuccio, G.; Billè, F.; Borghes, R.; Borghi, G.; Cautero, G.; Cirrincione, D.; Fabiani, S.; Ficorella, F.; Gandola, M.; Gianoncelli, A.; Giuressi, D.; Kourousias, G.; Mele, F.; Menk, R. H.; Picciotto, A.; Rachevski, A.; Rashevskaya, I.; Sammartini, M.; Stolfa, A.; Zampa, G.; Zampa, N.; Zorzi, N.; Vacchi, A.

    2018-03-01

    Low-energy X-ray fluorescence (LEXRF) is an essential tool for bio-related research of organic samples, whose composition is dominated by light elements. Working at energies below 2 keV and being able to detect fluorescence photons of lightweight elements such as carbon (277 eV) is still a challenge, since it requires in-vacuum operations to avoid in-air photon absorption. Moreover, the detectors must have a thin entrance window and collect photons at an angle of incidence near 90 degrees to minimize the absorption by the protective coating. Considering the low fluorescence yield of light elements, it is important to cover a substantial part of the solid angle detecting ideally all emitted X-ray fluorescence (XRF) photons. Furthermore, the energy resolution of the detection system should be close to the Fano limit in order to discriminate elements whose XRF emission lines are often very close within the energy spectra. To ensure all these features, a system consisting of four monolithic multi-element silicon drift detectors was developed. The use of four separate detector units allows optimizing the incidence angle on all the sensor elements. The multi-element approach in turn provides a lower leakage current on each anode, which, in combination with ultra-low noise preamplifiers, is necessary to achieve an energy resolution close to the Fano limit. The potential of the new detection system and its applicability for typical LEXRF applications has been proved on the Elettra TwinMic beamline.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-01

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

  10. Soft X-ray angle-resolved photoemission with micro-positioning techniques for metallic V2O3

    Science.gov (United States)

    Fujiwara, Hidenori; Kiss, Takayuki; Wakabayashi, Yuki K.; Nishitani, Yoshito; Mori, Takeo; Nakata, Yuki; Kitayama, Satoshi; Fukushima, Kazuaki; Ikeda, Shinji; Fuchimoto, Hiroto; Minowa, Yosuke; Mo, Sung-Kwan; Denlinger, Jonathan D.; Allen, James W.; Metcalf, Patricia; Imai, Masaki; Yoshimura, Kazuyoshi; Suga, Shigemasa; Muro, Takayuki; Sekiyama, Akira

    2015-01-01

    Soft X-ray angle-resolved photoemission has been performed for metallic V2O3. By combining a microfocus beam (40 µm × 65 µm) and micro-positioning techniques with a long-working-distance microscope, it has been possible to observe band dispersions from tiny cleavage surfaces with a typical size of several tens of µm. The photoemission spectra show a clear position dependence, reflecting the morphology of the cleaved sample surface. By selecting high-quality flat regions on the sample surface, it has been possible to perform band mapping using both photon-energy and polar-angle dependences, opening the door to three-dimensional angle-resolved photoemission spectroscopy for typical three-dimensional correlated materials where large cleavage planes are rarely obtained. PMID:25931096

  11. High Pressure X-ray Diffraction Studies on Barium.

    Science.gov (United States)

    Barnett, J D; Bennion, R B; Hall, H T

    1963-08-09

    Simultaneous x-ray diffraction and electrical resistance measurements on barium establish, with certainty, that Bridgman's 78-kb resistance transition is identical with his 59-kb volumetransition. During this transition, the bodycentered cubic structure changes to hexagonalclose packed. Lattice parameters for the latter structure at 62 kb (volume scale) are: a = 3.90 A, c = 6.15 A, and c/a = 1.58. Compression (AV/Vo) at 62 kb is 0.359 + 0.005 compared to 0.345 previously reported by Bridgman. Below the transition, at 49 kb, compression is 0.300 +/- 0.005 compared to Bridgman's 0.288. Bridgman's 17-kb volume transition was not detected by x-ray diffraction.

  12. X-ray photoelectron spectroscopic study of PuSb

    International Nuclear Information System (INIS)

    Baptist, R.; Chayrouse, J.; Courteix, D.; Heintz, L.; Damien, D.; Wojakowski, A.

    1983-01-01

    After presenting photoemission results for two uranium monopnictides, uranium nitride and antimonide, we present and analyse the X-ray photoemission spectroscopy results for PuSb. The increase of the 5f electron localization along the uranium monopnictides series is also observed when going from USb to PuSb. In this last case, the localization is due to an increase of the 5f intra-atomic Coulomb interaction in plutonium atoms compared to that in the uranium atoms [fr

  13. Opportunities and challenges for time-resolved studies of protein structural dynamics at X-ray free-electron lasers.

    Science.gov (United States)

    Neutze, Richard

    2014-07-17

    X-ray free-electron lasers (XFELs) are revolutionary X-ray sources. Their time structure, providing X-ray pulses of a few tens of femtoseconds in duration; and their extreme peak brilliance, delivering approximately 10(12) X-ray photons per pulse and facilitating sub-micrometre focusing, distinguish XFEL sources from synchrotron radiation. In this opinion piece, I argue that these properties of XFEL radiation will facilitate new discoveries in life science. I reason that time-resolved serial femtosecond crystallography and time-resolved wide angle X-ray scattering are promising areas of scientific investigation that will be advanced by XFEL capabilities, allowing new scientific questions to be addressed that are not accessible using established methods at storage ring facilities. These questions include visualizing ultrafast protein structural dynamics on the femtosecond to picosecond time-scale, as well as time-resolved diffraction studies of non-cyclic reactions. I argue that these emerging opportunities will stimulate a renaissance of interest in time-resolved structural biochemistry.

  14. 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

  15. X-ray diffraction studies of NbTe2 single crystal

    Indian Academy of Sciences (India)

    Unknown

    X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and ... The layered structure compound, NbTe2, is one of the typical materials which lead to charge .... financial assistance to carry out this work. References. Brown B E 1966 Acta ...

  16. A high resolution X-ray crystal spectrometer to study electron and ...

    Indian Academy of Sciences (India)

    We have studied fast ion–atom and electron–atom collision processes using a reconditioned high resolution X-ray spectrometer. The X-rays, generated by the collisions, are dispersed by a curved ADP crystal (Johansson geometry) and detected by a gas proportional counter. A self-written LabVIEW based program has ...

  17. Study of X-ray transients with Scanning Sky Monitor (SSM) onboard ...

    Indian Academy of Sciences (India)

    SSM scans the sky for X-ray transient sources in this energy range of interest. If an X-ray transient source is detected in outburst by SSM, the information will be provided to the astronomical community for follow-up observations to do a detailed study of the source in various other bands. SSM instrument, since its power-ON ...

  18. Enrichment study of hot intra-cluster gas through X-ray spectroscopy

    NARCIS (Netherlands)

    Plaa, J. de

    2007-01-01

    Enrichment study of hot intra-cluster gas through X-ray spectroscopy Clouds of hot X-ray emitting gas associated with clusters of galaxies are the biggest aggregates of baryons that we know, except for the cosmic web. A typical cloud contains the nuclear-fusion products of billions of supernovae.

  19. Corrosion and degradation studies utilizing X-ray photoelectron spectroscopy

    Science.gov (United States)

    Hixson, Holly Gwyndolen

    1997-08-01

    This dissertation involves studies of corrosion behavior at the surface of various metal samples, as well as the degradation of wool fibers obtained from the Star-Spangled Banner. Molybdenum metal and iron-zinc alloys were examined under corrosive conditions, and the degradation of the wool fibers was studied. The behavior of a polished molybdenum metal surface upon exposure to both aerated and deaerated water and 1.0 M NaCl solution was studied by X-ray Photoelectron Spectroscopy (XPS). Exposure to deaerated water and NaCl failed to produce oxidation of the metal surfaces, but exposing the polished metal surface to aerated water produced significant oxidation. Metal surfaces cleaned by argon-ion etching were found to be inert to oxidation by aerated water. The etching process also appears to passivate the metal surface. The behavior of molybdenum metal in 0.5 M Hsb2SOsb4 treated at various potentials has been studied using core and valence band XPS. The study indicates that Mosp{IV} and Mosp{VI} (including possibly Mosp{V} in some cases) were formed as the potential of the system was increased within the active range of molybdenum. The corrosive behavior of iron-zinc alloys that have been electroplated on plain steel in both aerated and deaerated quadruply-distilled water has been studied using XPS. Several different iron-zinc alloys were electroplated for comparative purposes: an iron-rich alloy, a zinc-rich alloy, and an alloy of similar iron and zinc composition. Treatment in aerated water produces oxidation for the iron-rich and similar composition alloys, but the oxide is reduced for the zinc-rich alloy. Degradation of the fibers in the original Star-Spangled Banner has been monitored using XPS and Scanning Electron Microscopy (SEM). Comparison of white and red wool fibers and linen fibers from the flag with new, mechanically-abraded, and chemically-treated white, red, and linen fibers, respectively, was performed in an attempt to determine the fibers' levels

  20. Study of X-ray transients with Scanning Sky Monitor (SSM) onboard AstroSat

    Science.gov (United States)

    Ramadevi, M. C.; Ravishankar, B. T.; Sarwade, Abhilash R.; Vaishali, S.; Iyer, Nirmal Kumar; Nandi, Anuj; Girish, V.; Agarwal, Vivek Kumar; Baby, Blessy Elizabeth; Hasan, Mohammed; Seetha, S.; Bhattacharya, Dipankar

    2018-02-01

    Scanning Sky Monitor (SSM) onboard AstroSat is an X-ray sky monitor in the energy range 2.5-10 keV. SSM scans the sky for X-ray transient sources in this energy range of interest. If an X-ray transient source is detected in outburst by SSM, the information will be provided to the astronomical community for follow-up observations to do a detailed study of the source in various other bands. SSM instrument, since its power-ON in orbit, has observed a number of X-ray sources. This paper discusses observations of few X-ray transients by SSM. The flux reported by SSM for few sources during its Performance Verification phase (PV phase) is studied and the results are discussed.

  1. Grazing angle X-ray fluorescence from periodic structures on silicon and silica surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Nowak, S.H., E-mail: nowak@ifg-adlershof.de [Physics Department, University of Fribourg, CH-1700 Fribourg (Switzerland); Banaś, D. [Institute of Physics, Jan Kochanowski University, 25-406 Kielce (Poland); Błchucki, W.; Cao, W.; Dousse, J.-Cl. [Physics Department, University of Fribourg, CH-1700 Fribourg (Switzerland); Hönicke, P. [Physikalisch-Technische Bundesanstalt (PTB), D-10587 Berlin (Germany); Hoszowska, J. [Physics Department, University of Fribourg, CH-1700 Fribourg (Switzerland); Jabłoński, Ł. [Institute of Physics, Jan Kochanowski University, 25-406 Kielce (Poland); Kayser, Y. [Physics Department, University of Fribourg, CH-1700 Fribourg (Switzerland); Kubala-Kukuś, A.; Pajek, M. [Institute of Physics, Jan Kochanowski University, 25-406 Kielce (Poland); Reinhardt, F. [Physikalisch-Technische Bundesanstalt (PTB), D-10587 Berlin (Germany); Savu, A.V. [Microsystems Laboratory (LMIS1), Ecole Polytechnique Fédérale de Lausanne, CH-1015 Lausanne (Switzerland); Szlachetko, J. [Institute of Physics, Jan Kochanowski University, 25-406 Kielce (Poland); Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland)

    2014-08-01

    Various 3-dimensional nano-scaled periodic structures with different configurations and periods deposited on the surface of silicon and silica substrates were investigated by means of the grazing incidence and grazing emission X-ray fluorescence techniques. Apart from the characteristics which are typical for particle- and layer-like samples, the measured angular intensity profiles show additional periodicity-related features. The latter could be explained by a novel theoretical approach based on simple geometrical optics (GO) considerations. The new GO-based calculations were found to yield results in good agreement with experiment, also in cases where other theoretical approaches are not valid, e.g., periodic particle distributions with an increased surface coverage.

  2. Grazing angle X-ray fluorescence from periodic structures on silicon and silica surfaces

    International Nuclear Information System (INIS)

    Nowak, S.H.; Banaś, D.; Błchucki, W.; Cao, W.; Dousse, J.-Cl.; Hönicke, P.; Hoszowska, J.; Jabłoński, Ł.; Kayser, Y.; Kubala-Kukuś, A.; Pajek, M.; Reinhardt, F.; Savu, A.V.; Szlachetko, J.

    2014-01-01

    Various 3-dimensional nano-scaled periodic structures with different configurations and periods deposited on the surface of silicon and silica substrates were investigated by means of the grazing incidence and grazing emission X-ray fluorescence techniques. Apart from the characteristics which are typical for particle- and layer-like samples, the measured angular intensity profiles show additional periodicity-related features. The latter could be explained by a novel theoretical approach based on simple geometrical optics (GO) considerations. The new GO-based calculations were found to yield results in good agreement with experiment, also in cases where other theoretical approaches are not valid, e.g., periodic particle distributions with an increased surface coverage

  3. Development of a portable system of grazing exit X-Ray fluorescence applied to environmental and biological studies

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Ramon S.; Oliveira, Davi F.; Anjos, Marcelino J. [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Instituto de Fisica; Assis, Joaquim T., E-mail: ramonziosp@yahoo.com.br, E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br, E-mail: joaquim.iprj@gmail.com [Universidade do Estado do Rio de Janeiro (UERJ), Nova Friburgo, RJ (Brazil). Instituto Politécnico

    2017-07-01

    In this study was developed a portable system of grazing exit X-ray fluorescence (geometric 90° - 0°) that will be applied in environmental studies (aerosol samples) and biological studies. GE-XRF portable system is formed by a mini X-ray tube of low power (anode of Au, maximum voltage and current of 50 kV and 200 μA, respectively) and a SiPIN detector (model XR-100CR of the Amptek). The reflectors used as sample support (sampler carrier) were quartz discs with 25.4 mm diameter and 3.0 mm thickness. The grazing exit angle was experimentally determined by measuring a cooper solution (10 μg.g{sup -1}). The system of GE-XRF proved to be quite stable and reproducible. It was calculated the sensibility curve of the system using multielement solutions. The accuracy of the system was checked using multielement reference solution as standard reference material. The relative errors between measured and certified values are in the range of 4 to 19%. The first results showed a background was drastically reduced at grazing exit angles, enabling trace elemental analysis. This paper shows that it is possible to produce a portable system of grazing exit X-ray fluorescence compact, efficient, low-cost and easy-to-handle instrumentation using a low-power X-ray tube and a SiPIN compact detector. (author)

  4. Stress measurements by multi-reflection grazing-incidence X-ray diffraction method (MGIXD) using different radiation wavelengths and different incident angles

    International Nuclear Information System (INIS)

    Marciszko, Marianna; Baczmański, Andrzej; Braham, Chedly; Wróbel, Mirosław; Wroński, Sebastian; Cios, Grzegorz

    2017-01-01

    The presented study introduces the development of the multi-reflection grazing-incidence X-ray diffraction method (MGIXD) for residual stress determination. The proposed new methodology is aimed at obtaining more reliable experimental data and increasing the depth of non-destructive stress determination below the sample surface. To verify proposed method measurements were performed on a classical X-ray diffractometer (Cu Kα radiation) and using synchrotron radiation (three different wavelengths: λ = 1.2527 Å, λ = 1.5419 Å and λ = 1.7512 Å). The Al2017 alloy subjected to three different surface treatments was investigated in this study. The obtained results showed that the proposed development of MGIXD method, in which not only different incident angles but also different wavelengths of X-ray are used, can be successfully applied for residual stress determination, especially when stress gradients are present in the sample.

  5. A Study of the Resolution of Dental Intraoral X-Ray Machines

    International Nuclear Information System (INIS)

    Kim, Seon Ju; Chung, Hyon De

    1990-01-01

    The purpose of this study was to assess the resolution and focal spot size of dental X-ray machines. Fifty dental X-ray machines were selected for measuring resolution and focal spot size. These machines were used in general dental clinics. The time on installation of the X-ray machine varies from 1 years to 10 years. The resolution of these machines was measured with the test pattern. The focal spot size of these machines was measured with the star test pattern. The following results were obtained: 1. The resolution of dental intraoral X-ray machines was not significantly changed in ten years. 2. The focal spot size of dental intraoral X-ray machines was not significantly increased in ten years. The statistical analysis between the mean focal spot size and nominal focal spot size was significant at the 0.05 level about the more than 3 years used machines.

  6. X-ray and neutron diffraction studies of superionic conductors: protonic compounds

    International Nuclear Information System (INIS)

    Tranqui, D.; Anne, M.

    1982-01-01

    Rapid reviews of X-ray and neutron diffraction theories and instrumentations are presented. It is shown that X-ray diffraction is a very powerful tool to determine three dimensional crystal structures. However localization of light atoms by X-ray is somewhat uncertain in compounds containing heavy atoms. In neutron diffraction the irregular but limited variation of scattering lengths of all elements within the periodic table render it possible to localize almost all atoms, especially hydrogen atoms in solids. Some recent and successful studies of protonic compounds and other by X-ray and neutron diffraction are cited. These examples demonstrate that the combined X-ray and neutron techniques should be used to obtain not only geometrical features of rigid framework in superionic conductor materials but also in an indirect way the dynamic properties of mobile ions. (author)

  7. Preparing monodisperse macromolecular samples for successful biological small-angle X-ray and neutron-scattering experiments.

    Science.gov (United States)

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

    2016-11-01

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

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

    International Nuclear Information System (INIS)

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

    1978-01-01

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

  9. Accurate structure analyses of polymer crystals on the basis of wide-angle X-ray and neutron diffractions

    International Nuclear Information System (INIS)

    Tashiro, Kohji; Hanesaka, Makoto; Yamamoto, Hiroko; Wasanasuk, Kaewkan; Jayaratri, Paramita; Yoshizawa, Yoshinori; Tanaka, Ichiro; Niimura, Nobuo; Kusaka, Katsuhiro; Hosoya, Takaaki; Ohhara, Takashi; Kurihara, Kazuo; Kuroki, Ryota; Tamada, Taro; Fujiwara, Satoru; Katsube, Katsuyoshi; Morikawa, Keisuke; Komiya, Yukiatsu; Kitano, Toshiaki; Nishu, Takashi; Ozeki, Tomoji

    2014-01-01

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

    International Nuclear Information System (INIS)

    Eliezer, D.

    1994-06-01

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

  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. 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

  13. Surface X-ray studies of catalytic clean technologies.

    Science.gov (United States)

    Lee, Adam F; Prabhakaran, Vinod; Wilson, Karen

    2010-06-14

    The rational design of new heterogeneous catalysts for clean chemical technologies can be accelerated by molecular level insight into surface chemical processes. In situ methodologies, able to provide time-resolved and/or pressure dependent information on the evolution of reacting adsorbed layers over catalytically relevant surfaces, are therefore of especial interest. Here we discuss recent applications of surface X-ray techniques to surface-catalysed oxidations, (de)hydrogenations, C-C coupling, dehalogenation and associated catalyst restructuring, and explore how these may help to shape future sustainable chemistry.

  14. Study of moire fringes using synchrotron X-rays

    International Nuclear Information System (INIS)

    Yoshimura, Jun-ichi

    1992-01-01

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

  15. X-ray diffraction applied to powder studies

    International Nuclear Information System (INIS)

    Assaf, Josiane

    1982-01-01

    the thesis starts with general definitions of x-ray: their nature, sources and production mechanism. it describesdifferent methods such as Debye-scherrer, absorption coefficient method, diffractometer method...The use of pattern-fitting techniques for the characterization of the microstructure is discussed through applications to nanocrystalline materials. Remarkable results achieved in the solution of crystal structures are presented, as well as the impact in solid-state chemistry of powder crystallography, particularly for elucidating the crystal chemistry of families of compounds for which only powders are available

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

    Science.gov (United States)

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

    2016-01-01

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

  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

    1994-08-01

    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. Pinhole X-ray fluorescence imaging of gadolinium and gold nanoparticles using polychromatic X-rays: a Monte Carlo study.

    Science.gov (United States)

    Jung, Seongmoon; Sung, Wonmo; Ye, Sung-Joon

    2017-01-01

    This work aims to develop a Monte Carlo (MC) model for pinhole K-shell X-ray fluorescence (XRF) imaging of metal nanoparticles using polychromatic X-rays. The MC model consisted of two-dimensional (2D) position-sensitive detectors and fan-beam X-rays used to stimulate the emission of XRF photons from gadolinium (Gd) or gold (Au) nanoparticles. Four cylindrical columns containing different concentrations of nanoparticles ranging from 0.01% to 0.09% by weight (wt%) were placed in a 5 cm diameter cylindrical water phantom. The images of the columns had detectable contrast-to-noise ratios (CNRs) of 5.7 and 4.3 for 0.01 wt% Gd and for 0.03 wt% Au, respectively. Higher concentrations of nanoparticles yielded higher CNR. For 1×10 11 incident particles, the radiation dose to the phantom was 19.9 mGy for 110 kVp X-rays (Gd imaging) and 26.1 mGy for 140 kVp X-rays (Au imaging). The MC model of a pinhole XRF can acquire direct 2D slice images of the object without image reconstruction. The MC model demonstrated that the pinhole XRF imaging system could be a potential bioimaging modality for nanomedicine.

  19. Critical-angle transmission grating technology development for high resolving power soft x-ray spectrometers on Arcus and Lynx

    Science.gov (United States)

    Heilmann, Ralf K.; Bruccoleri, Alexander R.; Song, Jungki; Kolodziejczak, Jeffery; Gaskin, Jessica A.; O'Dell, Stephen L.; Cheimetz, Peter; Hertz, Edward; Smith, Randall K.; Burwitz, Vadim; Hartner, Gisela; La Caria, Marlis-Madeleine; Schattenburg, Mark L.

    2017-08-01

    Soft x-ray spectroscopy with high resolving power (R = λ/Δλ) and large effective area (A) addresses numerous unanswered science questions about the physical laws that lead to the structure of our universe. In the soft x-ray band R > 1000 can currently only be achieved with diffraction grating-based spectroscopy. Criticalangle transmission (CAT) gratings combine the advantages of blazed reflection gratings (high efficiency, use of higher diffraction orders) with those of conventional transmission gratings (relaxed alignment tolerances and temperature requirements, transparent at higher energies, low mass), resulting in minimal mission resource requirements, while greatly improving figures of merit. Diffraction efficiency > 33% and R > 10, 000 have been demonstrated for CAT gratings. Last year the technology has been certified at Technology Readiness Level 4 based on a probe class mission concept. The Explorer-scale (A > 450 cm2 , R > 2500) grating spectroscopy Arcus mission can be built with today's CAT grating technology and has been selected in the current Explorer round for a Phase A concept study. Its figure of merit for the detection of weak absorption lines will be an order of magnitude larger than current instruments on Chandra and XMM-Newton. Further CAT grating technology development and improvements in the angular resolution of x-ray optics can provide another order of magnitude improvement in performance, as is envisioned for the X-ray Surveyor/Lynx mission concept currently under development for input into the 2020 Decadal Survey. For Arcus we have tested CAT gratings in a spectrometer setup in combination with silicon pore optics (SPO) and obtained resolving power results that exceed Arcus requirements before and after environmental testing of the gratings. We have recently fabricated the largest (32 mm x 32 mm) CAT gratings to date, and plan to increase grating size further. We mounted two of these large gratings to frames and aligned them in the

  20. 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.

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

    Science.gov (United States)

    Doutch, James; Gilbert, Elliot P

    2013-01-02

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

  2. 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.

  3. Study of uniaxial nematic lyomesophases by x-ray diffraction and auxiliary techniques

    International Nuclear Information System (INIS)

    Bittencourt, D.R.S.

    1986-01-01

    The uniaxial lyotropic nematic liquid crystals made of amphiphile/water/decanol/salt have been studied. The amphiphiles sodium decyl sulphate and sodium dodecil sulphate have been used. Characterization of samples conditioned in plane and cylindrical cells has been made by orthoscopic polarized optical microscopy (OM) and X.ray diffraction (XD) by observation of orientation under surface and magnetic field effects. It was possible to determine the director orientation of uniaxial discotic (N D ) and cylindrical (N C ) samples under surface and magnetic effects by both OM and XD techniques in independent ways. The homologous amphiphilies sodium octil, decil and dodecil sulfate, in powder form, have been studied by Debye-Scherrer technique. Observed reflexions have been indexed and crystallographic parameters determined. Good agreement between calculated and measured densities has been obtained. A crysostat for temperature variation in the interval- 10 0 /60 0 has been constructed, XD diagrams has been obtained for sodium decil sulfate samples allowing determination of phase transitions of two systems. Scattering curves at room temperatures have been obtained in a small-angle X-ray diffractometer. Analysis of profiles allowed determination of short range positional order and correlation ranges. Interference function between scattering objects have been obtained using structural models for the micelles of the uniaxial nematic phases. (author) [pt

  4. 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.

  5. Study of Cavitation Shedding Dynamics on a NACA0015 Hydrofoil Using X-Ray Densitometry

    Science.gov (United States)

    Ganesh, Harish; Wu, Juliana; Ceccio, Steven

    2016-11-01

    Cavitation dynamics on the NACA0015 hydrofoil at several attack angles are found to be spectrally rich, being multi-modal with abrupt changes in Strouhal number with change in cavitation number. Present study focusses on identifying the physical mechanisms responsible for the change in cavitation dynamics on a NACA0015 hydrofoil in a re-circulating water tunnel using time resolved X-ray densitometry. Time-resolved void fraction flow fields obtained using X-ray densitometry, synchronized with acoustic noise measurements using a hydrophone, are used to identify different flow features and mechanisms that are responsible for the change in the observed spectral behavior. It is shown that under higher cavitation numbers, the shedding mechanism is predominantly re-entrant liquid flow based, but as the cavitation number drops many different processes are at play. At lower cavitation numbers, the shed cavity cloud collapse arrests cavity growth and this results in altered cycle dynamics and hence the Strouhal number. In addition, propagation bubbly shock waves are also found to be a dominant mechanism of shedding for certain conditions. The multi-modal nature of the acoustic pressure signature is explained by presence of different flow features, which could be concurrent or alternating. Office of Naval Research.

  6. Bone X-Ray (Radiography)

    Medline Plus

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

  7. An x-ray diffraction study of interface roughness and diffusion in Ag/Pd superlattices

    NARCIS (Netherlands)

    Temst, K.; van Bael, M.J.; van Haesendonck, Ch.; Bruynseraede, Y.; de Groot, D.G.; Koeman, N.J.; Griessen, R.P.

    1999-01-01

    The influence of thermal annealing on the surface and interface roughness of epitaxial Ag/Pd superlattices has been quantitatively characterized by high-angle X-ray diffraction and atomic force microscopy. Although Ag and Pd form a continuous series of solid solutions, it is shown that thermal

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

    DEFF Research Database (Denmark)

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

    2016-01-01

    This article introduces a simple microfluidic device that can be combined with synchrotron small-angle X-ray scattering (SAXS) for monitoring dynamic structural transitions. The microfluidic device is a thiol-ene-based system equipped with 125 µm-thick polystyrene windows, which are suitable for X....... The combination of microfluidics with X-ray techniques can be used for investigating protein unfolding, for monitoring the formation of nanoparticles in real time, and for other biomedical and pharmaceutical investigations....

  9. X-ray absorption and emission studies of diamond nanoparticles

    International Nuclear Information System (INIS)

    Van Buuren, T.; Willey, T.; Raty, J.Y.; Galli, G.; Terminello, L.J.; Bostedt, C.

    2004-01-01

    Full text: A new family of carbon nanopaticles produced in detonations, are found to have a core of diamond with a coating fullerene- like carbon. X-ray diffraction and TEM show that the nanodiamond powder is crystalline and approximately 4 nm in diameter. These nano-sized diamonds do not display the characteristic property of other group IV nanoparticles: a strong widening of the energy gap between the conduction and valence bands owing to quantum-confinement effects. For nano-sized diamond with a size distribution of 4 nm, there is no shift of the band energies relative to bulk diamond. Although the C1s core exciton feature clearly observed in the K-edge absorption edge of bulk diamond is shifted and broadening due to increased overlap of the excited electron with the core holein the small particle. Also the depth of the second gap in the nanodiamond spectra is shallower than that of bulk diamond. A feature at lower energy in the X-ray absorption spectra that is not present in the bulk samples is consistent with a fullerene like surface reconstruction. By exposing the diamond nanoparticles to an Argon /Oxygen plasma then annealing in a UHV environment we have obtained a hydrogen free surface. The nanodiamonds processed in this manner show an increase fullerene type contribution in the carbon x-ray absorption pre-edge. High spatial resolution EELS measurements of the empty states of a single nanodiamond particle acquired with a ld emission TEM also show the core of the particle is bulk diamond like where as the surface has a fullerene like structure. Standard density-functional calculations on clusters in which the diamond surface bonds are terminated with hydrogen atoms, show that the bandgap begins to increase above the bulk value only for clusters smaller than 1 nm. Surface hydrogen atoms are found to be about as close as they do in molecular hydrogen and can escape as H 2 , forcing the respective carbon atoms to rearrange. A series of such rearrangements can

  10. Purification, crystallization and preliminary X-ray study of the fungal laccase from Cerrena maxima

    International Nuclear Information System (INIS)

    Lyashenko, Andrey V.; Zhukhlistova, Nadegda E.; Gabdoulkhakov, Azat G.; Zhukova, Yuliya N.; Voelter, Wolfang; Zaitsev, Viatcheslav N.; Bento, Isabel; Stepanova, Elena V.; Kachalova, Galina S.; Koroleva, Ol’ga V.; Cherkashyn, Evgeniy A.; Tishkov, Vladimir I.; Lamzin, Victor S.; Schirwitz, Katja; Morgunova, Ekaterina Yu.; Betzel, Christian; Lindley, Peter F.; Mikhailov, Al’bert M.

    2006-01-01

    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%; R free = 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 NO 2 substituents

  11. Purification, crystallization and preliminary X-ray study of the fungal laccase from Cerrena maxima

    Energy Technology Data Exchange (ETDEWEB)

    Lyashenko, Andrey V.; Zhukhlistova, Nadegda E.; Gabdoulkhakov, Azat G.; Zhukova, Yuliya N. [A. V. Shubnikov Institute of Crystallography, RAS, Leninskiy Prospect 59, 119333 Moscow (Russian Federation); Voelter, Wolfang [Institute of Biochemistry, University of Tuebingen, Physiologisch-Chemisches Institut, Hoppe-Seyler-Strasse 4, 72076 Tuebingen (Germany); Zaitsev, Viatcheslav N. [University of St Andrews, Centre for Biomolecular Sciences, North Haugh, St Andrews, KY16 9ST,Scotland (United Kingdom); Bento, Isabel [Instituto de Tecnologia Química e Biológica (ITQB), Universidade Nova de Lisboa, Apartado 127, Av. Republica, 2781-901 Oeiras (Portugal); Stepanova, Elena V. [A. N. Bakh Institute of Biochemistry, RAS, Leninskiy Prospect 33, 119071 Moscow (Russian Federation); Kachalova, Galina S. [Institute of Theoretical and Experimental Biophysics of RAS, Institutskaya Street 3, 142290 Puschino, Moscow Region (Russian Federation); Koroleva, Ol’ga V. [A. N. Bakh Institute of Biochemistry, RAS, Leninskiy Prospect 33, 119071 Moscow (Russian Federation); Cherkashyn, Evgeniy A.; Tishkov, Vladimir I. [Department of Chemical Enzymology, M. V. Lomonosov Moscow State University, 119992 Moscow (Russian Federation); Lamzin, Victor S.; Schirwitz, Katja [European Molecular Biology Laboratory, c/o DESY, Notkestrasse 85, 22603 Hamburg (Germany); Morgunova, Ekaterina Yu. [A. V. Shubnikov Institute of Crystallography, RAS, Leninskiy Prospect 59, 119333 Moscow (Russian Federation); Betzel, Christian [University of Hamburg, Institute fur Biochemie und Lebensmittelchemie, Department of Biochemistry and Molecular Biology, c/o DESY, Building 22a, Notkestrasse 85, 22603 Hamburg (Germany); Lindley, Peter F. [Instituto de Tecnologia Química e Biológica (ITQB), Universidade Nova de Lisboa, Apartado 127, Av. Republica, 2781-901 Oeiras (Portugal); Mikhailov, Al’bert M., E-mail: amm@ns.crys.ras.ru [A. V. Shubnikov Institute of Crystallography, RAS, Leninskiy Prospect 59, 119333 Moscow (Russian Federation)

    2006-10-01

    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%; R{sub free} = 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 NO{sub 2} substituents.

  12. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-11-15

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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

  16. 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.

  17. Environmental studies in Khartoum area using x-ray fluorescence

    International Nuclear Information System (INIS)

    Abdel Elmagid, Suliman Alamin

    1996-06-01

    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)

  18. Studies of soft x-ray emission during solar flares

    International Nuclear Information System (INIS)

    Anandaram, M.N.

    1973-01-01

    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)

  19. Liquid structure of trihexyltetradecylphosphonium chloride at ambient temperature: an X-ray scattering and simulation study.

    Science.gov (United States)

    Gontrani, Lorenzo; Russina, Olga; Celso, Fabrizio Lo; Caminiti, Ruggero; Annat, Gary; Triolo, Alessandro

    2009-07-09

    We report on an experimental and simulation study done on a representative room temperature ionic liquid, namely tetradecyltrihexylphosphonium chloride, at ambient conditions. The study was conducted using small and wide angle X-ray scattering and molecular dynamics simulations. Both approaches converge in indicating that this material is characterized by the existence of strong P-Cl interactions (with characteristic distances between 3.5 and 5.0 A) and by the occurrence of nanoscale segregation, despite the symmetric nature of the cation and similarly to other room temperature ionic liquids. A good agreement is found between the structure factor and pair correlation functions obtained from MD simulations and the corresponding experimental observables, thus strongly validating the interaction potential used in the simulations.

  20. Study of the polarization dependence of the photoelectric effect in the soft X-ray band - A focal plane photoelectric stellar X-ray polarimeter for the Spectrum-X-Gamma mission

    International Nuclear Information System (INIS)

    Heckler, A.; Blaer, A.; Kaaret, P.; Novick, R.

    1989-01-01

    An experimental study of the polarization dependence of the photoelectric effect in cesium iodide in the soft X-ray band was started (Heckler et al., 1989). At a grazing angle of 10 degrees and a photon energy of 2.6 keV, it is found that the photoelectric yield from a thin layer of evaporated cesium iodide varies by 12.4 percent as the polarization vector of the incident X-ray beam is rotated about the line-of-sight. The rotation angle corresponding to the maximum photoyield is displaced by 16 degrees from the normal to the photocathode. This modulation and phase shift are in good agreement with the results recently reported by Fraser, et al. (1989) It is shown that a focal plane stellar X-ray polarimeter based on this photoelectric effect will be substantially more efficient than convential X-ray polarimeters such as those based on either Bragg reflection or scattering from low atomic number targets. 7 refs

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

    Directory of Open Access Journals (Sweden)

    Bing Wang

    2018-04-01

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

  2. A structural study of ceramic oxides by X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Akhtar, M.J.

    1995-01-01

    A detailed structural study of ceramic oxides is presented by employing X-ray Absorption Spectroscopy (XAS). In the present work X-ray Absorption Near Edge Structure (XANES) is used for the investigation of valence state of metal cations; whereas, Extended X-ray Absorption Fine Structure EXAFS) is employed for the determination for bond lengths, coordination numbers and nature of the elements present in the near neighbour shells surrounding the absorbing atom. These results show that local environment of dopant and host cations are different; and this variation in local structure depends on the nature and concentration of the dopant ions. (author)

  3. Study of dielectric liquids at room temperature for high energy x ray Tomography

    International Nuclear Information System (INIS)

    Lepert, S.

    1989-09-01

    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 [fr

  4. Magnetism in heterogeneous thin film systems: Resonant X-ray scattering studies

    International Nuclear Information System (INIS)

    Kortright, J.B.; Jiang, J.S.; Bader, S.D.; Hellwig, O.; Marguiles, D.T.; Fullerton, E.E.

    2002-01-01

    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

  5. A new type of crystal spectrometer for cosmic X-ray studies

    International Nuclear Information System (INIS)

    Berthelsdorf, R.F.; Mitchell, R.J.; Culhane, J.L.

    1976-01-01

    A crystal spectrometer using a crystal panel curved in two dimensions and a position sensitive proportional counter is described. The instrument uses conical focussing to minimize detector size, and the crystal panel is bent to simultaneously present a range of Bragg angles to incoming X-rays, resulting in a one-to-one correspondence between the energy of a reflected X-ray and its point of incidence on the proportional counter. The advantages of such an instrument are high sensitivity, mechanical simplicity, and the capability of measuring spectra of rapidly varying sources. (Auth.)

  6. Computation of mass-density images from x-ray refraction-angle images

    International Nuclear Information System (INIS)

    Wernick, Miles N; Yang Yongyi; Mondal, Indrasis; Chapman, Dean; Hasnah, Moumen; Parham, Christopher; Pisano, Etta; Zhong Zhong

    2006-01-01

    In this paper, we investigate the possibility of computing quantitatively accurate images of mass density variations in soft tissue. This is a challenging task, because density variations in soft tissue, such as the breast, can be very subtle. Beginning from an image of refraction angle created by either diffraction-enhanced imaging (DEI) or multiple-image radiography (MIR), we estimate the mass-density image using a constrained least squares (CLS) method. The CLS algorithm yields accurate density estimates while effectively suppressing noise. Our method improves on an analytical method proposed by Hasnah et al (2005 Med. Phys. 32 549-52), which can produce significant artefacts when even a modest level of noise is present. We present a quantitative evaluation study to determine the accuracy with which mass density can be determined in the presence of noise. Based on computer simulations, we find that the mass-density estimation error can be as low as a few per cent for typical density variations found in the breast. Example images computed from less-noisy real data are also shown to illustrate the feasibility of the technique. We anticipate that density imaging may have application in assessment of water content of cartilage resulting from osteoarthritis, in evaluation of bone density, and in mammographic interpretation

  7. An interpretation of two X-ray studies of vanadium sesquioxide (V 2O 3)

    Science.gov (United States)

    Lovesey, S. W.; Sivia, D. S.; Knight, K. S.

    2002-06-01

    Recent studies of V 2O 3 include experiments performed with X-rays, and exploit atomic resonances of V ions. In one case, the K-edge resonance has been used to enhance Bragg intensities, and in a second experiment the absorption signal has been monitored at L 2 and L 3 edges. Data collected on magnetically ordered V 2O 3 is successfully interpreted on the basis of an atomic model, and the established chemical and magnetic structures. The extensive diffraction data gathered in azimuthal-angle scans at charge-forbidden reflections is found to infer the V ion wave function, which in turn permits estimates to be made of atomic quantities not measured by diffraction, and including the absorption signal.

  8. 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.

  9. X-ray diffraction and mechanical properties studies on Kevlar-49 fibres

    International Nuclear Information System (INIS)

    Abdo, S. M.

    1988-01-01

    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.)

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

    International Nuclear Information System (INIS)

    Zhao Jiyong; Jiang Jianhua; Tian Yulian

    1992-01-01

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

  11. [X-ray endoscopic semiotics and diagnostic algorithm of radiation studies of preneoplastic gastric mucosa changes].

    Science.gov (United States)

    Akberov, R F; Gorshkov, A N

    1997-01-01

    The X-ray endoscopic semiotics of precancerous gastric mucosal changes (epithelial dysplasia, intestinal epithelial rearrangement) was examined by the results of 1574 gastric examination. A diagnostic algorithm was developed for radiation studies in the diagnosis of the above pathology.

  12. Studies in K-shell X-ray energy shift for a 2p spectator vacancy

    Energy Technology Data Exchange (ETDEWEB)

    Bhattacharya, J.; Talukdar, B.; Laha, U.

    1989-10-01

    We examine a simple model for calculating X-ray energy shifts due to outer atomic vacancies and present some case studies. We find that this model is a good supplement for the traditional approach to the problem. (orig.).

  13. Coordination chemistry and X-ray studies with novel sterically constrained diphosphonite ligands

    NARCIS (Netherlands)

    van der Vlugt, JI; Sablong, R; Mills, AM; Kooijman, H; Spek, AL; Meetsma, A; Vogt, D

    2003-01-01

    The coordination of two novel, sterically constrained diphosphonite ligands towards different palladium, platinum and rhodium precursors has been studied. Complexes of this hitherto unexplored class of diphosphonites, based on rigid xanthene backbones, have been characterized by X-ray

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1979-01-01

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

  15. Characterization of the α-SN/CDTE(110) interface by angle-resolved X-ray photoemission

    International Nuclear Information System (INIS)

    Lin, T.S.; Partin, W.J.; Chung, Y.W.

    1987-01-01

    Stoichiometric and atomically clean CdTe(110) surfaces have been prepared by suitable chemical etching, followed by argon sputtering, and sample annealing in ultra-high vacuum. Cubic (α) -tin was grown on CdTe(110) by tin evaporation from a tungsten filament at a substrate temperature of 30 0 C. Angle-resolved X-ray photoelectron spectroscopy (ARXPS) was used to determine the α-Sn growth mechanism and the composition profile of this semiconductor heterostructure nondestructively. From their analyses, the authors conclude that α-Sn grows on CdTe(110) at 30 0 C by a layer by layer mechanism and forms an abrupt junction with CdTe(110)

  16. Depth profile characterization of electrodeposited multi-thin-film structures by low angle of incidence X-ray diffractometry

    International Nuclear Information System (INIS)

    Nauer, M.; Ernst, K.; Kautek, W.; Neumann-Spallart, M.

    2005-01-01

    Typical structures of heterojunction photovoltaic cells were prepared by sequential electrodeposition of II-VI semiconductor thin films on a transparent conductor, SnO 2 on glass. The structures comprised a wide bandgap window, ZnSe or ZnTe, a medium bandgap light absorber, CdTe, and an ohmic back contact. It is demonstrated that low incidence angle X-ray diffraction (LIXD) can be successfully used as a process monitoring tool, featuring non-destructive depth profiling and phase characterization of such thin film structures. LIXD results are compared to Secondary Ion Mass Spectroscopy (SIMS) and Scanning Electron Microscopy (SEM) data. Both, SIMS and SEM, corroborate the LIXD results as to layer sequence and presence/absence of intermixing

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

    Science.gov (United States)

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

    2015-12-09

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

  18. 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)

    Van de Voorde, Lien; Vekemans, Bart; Verhaeven, Eddy; Tack, Pieter; De Wolf, Robin; Garrevoet, Jan; Vandenabeele, Peter; Vincze, Laszlo

    2015-01-01

    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

  19. 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.

  20. 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.

  1. Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

    Science.gov (United States)

    Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

    2009-09-01

    Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.

  2. Study of magnetic metal periodic structures by X-Ray and electron microscopy methods

    Science.gov (United States)

    Prutskov, G. V.; Chesnokov, Yu. M.; Vasilliev, A. L.; Likhachev, I. A.; Pashaev, E. M.; Subbotin, I. A.

    2017-11-01

    Complex studies of magnetic periodic metallic systems based on Dy/Gd layers have been carried out by X-ray diffraction, resonance X-ray reflectometry, transmission electronic microscopy, and energydispersve microanalysis. The application of these methods and joint analysis of their results provide an effective approach to study of the structure and determination of the parameters of individual layers and interfaces and their structural quality with a high degree of reliability.

  3. High-resolution x-ray scatter and reflectivity study of sputtered IR surfaces

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Abdali, S.; Hornstrup, Allan

    1993-01-01

    In recent years there has been an increased interest in the possible use of Ir as the reflecting surface in X-ray telescope programs. An X-ray study of such surfaces produced by sputtering of Ir on highly polished Zerodur flats is presented here. The study was performed using Fe K(alpha) 1 (6...... result shows that an Ir coating can be produced with nominal bulk density....

  4. Resonant X-ray Raman scattering on molecules: A benchmark study on HCl

    International Nuclear Information System (INIS)

    Carniato, Stephane; Taieb, Richard; Journel, Loic; Guillemin, Renaud; Stolte, Wayne C.; Lindle, Dennis W.; Gel'mukhanov, Faris; Simon, Marc

    2010-01-01

    Resonant X-ray Raman scattering is a powerful tool to study molecular dynamics and subtle chemical effects like the molecular field beyond vibrational and lifetime limitations. Using this technique in the tender X-ray region, gas phase HCl is studied as a benchmark molecule for other compounds like freons, which play an important role in physical-chemical properties of the ozone layer of atmosphere.

  5. Resonant X-ray Raman scattering on molecules: A benchmark study on HCl

    Energy Technology Data Exchange (ETDEWEB)

    Carniato, Stephane [UPMC Univ Paris 06, UMR 7614, Laboratoire de Chimie Physique Matiere et Rayonnement, F-75005 Paris (France); CNRS, UMR 7614, Laboratoire de Chimie Physique Matiere et Rayonnement, F-75005 Paris (France); Taieb, Richard, E-mail: richard.taieb@upmc.f [UPMC Univ Paris 06, UMR 7614, Laboratoire de Chimie Physique Matiere et Rayonnement, F-75005 Paris (France); CNRS, UMR 7614, Laboratoire de Chimie Physique Matiere et Rayonnement, F-75005 Paris (France); Journel, Loic; Guillemin, Renaud [UPMC Univ Paris 06, UMR 7614, Laboratoire de Chimie Physique Matiere et Rayonnement, F-75005 Paris (France); CNRS, UMR 7614, Laboratoire de Chimie Physique Matiere et Rayonnement, F-75005 Paris (France); Stolte, Wayne C.; Lindle, Dennis W. [Department of Chemistry, University of Nevada, Las Vegas, NV 89154-4003 (United States); Gel' mukhanov, Faris [Theoretical Chemistry, Roslagstullsbacken 15, Royal Institute of Technology, S-106 91 Stockholm (Sweden); Simon, Marc [UPMC Univ Paris 06, UMR 7614, Laboratoire de Chimie Physique Matiere et Rayonnement, F-75005 Paris (France); CNRS, UMR 7614, Laboratoire de Chimie Physique Matiere et Rayonnement, F-75005 Paris (France)

    2010-08-15

    Resonant X-ray Raman scattering is a powerful tool to study molecular dynamics and subtle chemical effects like the molecular field beyond vibrational and lifetime limitations. Using this technique in the tender X-ray region, gas phase HCl is studied as a benchmark molecule for other compounds like freons, which play an important role in physical-chemical properties of the ozone layer of atmosphere.

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

    International Nuclear Information System (INIS)

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

    1980-01-01

    An attempt is made to obtain complete data on the form, sizes, weight and hydration of the T7 bacteriophage cultivated on E.coli cells and the peculiarities of phage DNA structure using the method of small-angle scattering

  7. [Study on spectrum analysis of X-ray based on rotational mass effect in special relativity].

    Science.gov (United States)

    Yu, Zhi-Qiang; Xie, Quan; Xiao, Qing-Quan

    2010-04-01

    Based on special relativity, the formation mechanism of characteristic X-ray has been studied, and the influence of rotational mass effect on X-ray spectrum has been given. A calculation formula of the X-ray wavelength based upon special relativity was derived. Error analysis was carried out systematically for the calculation values of characteristic wavelength, and the rules of relative error were obtained. It is shown that the values of the calculation are very close to the experimental values, and the effect of rotational mass effect on the characteristic wavelength becomes more evident as the atomic number increases. The result of the study has some reference meaning for the spectrum analysis of characteristic X-ray in application.

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

    International Nuclear Information System (INIS)

    Wakabayashi, Katsuzo

    1991-01-01

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

  9. X-ray magnification studies in biology and some other applications. Chapter 6

    International Nuclear Information System (INIS)

    Van Emden, H.F.; Ely, R.V.

    1980-01-01

    The facilities of X-ray mirofocal equipment of particular value in biological research are outlined. The applications of X-ray magnification techniques in various entomological studies is described particularly for observing plant pests. The value of these techniques in miscellaneous botanical studies is also described, e.g. in seed quality analysis, the monitoring of the early stages of reproductive development in seeds, the distribution of crystals in plant tissues and the X-ray absorption of cell constituents. Reference is also made to the use of transmission target techniques which permit higher direct X-ray magnifications of small selected specimen areas, e.g. penetration of paints and resins into timber. Further miscellaneous research applications of X-ray magnification techniques are described, e.g. in geological studies of fossils and sedimentary rocks, in archaeological studies of metal objects, excavated human bones etc. and in Fine Art studying the technique of past artists and detecting art forgeries. Finally it is pointed out that another important application of microfocal X-rays could be in the study of radiation damage in living animals or plants. (U.K.)

  10. The principles of 'reglamentation' of dosage loads during X-ray studies of patients

    International Nuclear Information System (INIS)

    Barkhudarov, R.M.; Stavitsky, R. von; Lerbedev, A.L.

    2008-01-01

    Full text: Irradiation during medical X-ray studies is one of the leading factors contributing to the total radiation dosage of people. According to the modern national and international norms, radiation dosages during X-ray diagnostics and treatment are not regulated, but fall under the main principles of ICRP - justification and optimization. The realization of these principles in practice is hindered by the lack of a well-tested and verified model and, therefore, the application of these principles in the Russian health system remains only a recommendation, although attempts have been made at defining allowed levels of irradiation of patients during radionuclide diagnostics by weighing the risks and gains. By using this principle, the values of the control levels of irradiation dosages during X-ray diagnostics are proposed for different groups of patients, depending on the type of studies. The values of these levels should serve as the upper limits for the area of optimization of the dosage loads. The categories of patients are considered: Category A - persons, which undergo X-ray studies in relation to a cancer or suspicion of cancer as a diagnosis is verified, as well as in urgent conditions, X-ray surgery and tuberculosis; Category B - persons, which undergo X-ray studies for diagnosis verification or to help determine the treatment strategy for a non-cancer related ailment; Category C - persons, which undergo preventive X-ray treatment or are part of a research study. For Category A, we suggest a control level for the annual effective dose of 150 mSv which practically excludes deterministic effects and results in a possible theoretical number of additional cancerous disorders of less than 7-10% of cases diagnosed and cured through timely X-ray testing. For patients in Category B a somewhat elevated risk - in comparison to the rest of the population - could be justified because of the usefulness and value of the X-ray diagnostic information. About 70% of the

  11. X-Ray Photoemission Study of the Oxidation of Hafnium

    International Nuclear Information System (INIS)

    Chourasia, R.; Hickman, J.L.; Miller, R.L.; Nixon, G.A.; Seabolt, M.A.

    2011-01-01

    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 HfO 2 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

  12. 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.

  13. Soft x-ray emission studies of several aluminum alloys

    International Nuclear Information System (INIS)

    Tsang, K.L.; Zhang, C.H.; Callcott, T.A.; Arakawa, E.T.; Ederer, D.L.; Biancaniello, F.; Curelaru, I.

    1986-01-01

    During the first few months of operation of our soft x-ray spectrometer at the NSLS, we have measured the L emission spectrum for three classes of aluminum alloys: dilute aluminum-magnesium alloys to extend the Al-Mg system to the impurity limit; a 50-50 alloy of aluminum-lithium to characterize the band structure of bulk samples of this potential battery electrolite; and the icosahedral and normal Al-Mn alloys to see if the two phases had measurably different density of states which have been predicted. All spectra shown are produced when core holes generated by energetic electrons or photons are filled by radiative transitions from conduction band states. Dipole selection rules govern the transitions. Thus, K spectra provide a measure of the p-symmetic partial density of states (DOS) near the atom. Similarly, L spectra produced by transitions to p-core holes map the s and d symmetric DOS in the vicinity of the atom with the core hole

  14. Soft x-ray emission studies of several aluminum alloys

    Energy Technology Data Exchange (ETDEWEB)

    Tsang, K.L.; Zhang, C.H.; Callcott, T.A.; Arakawa, E.T.; Ederer, D.L.; Biancaniello, F.; Curelaru, I.

    1986-09-23

    During the first few months of operation of our soft x-ray spectrometer at the NSLS, we have measured the L emission spectrum for three classes of aluminum alloys: dilute aluminum-magnesium alloys to extend the Al-Mg system to the impurity limit; a 50-50 alloy of aluminum-lithium to characterize the band structure of bulk samples of this potential battery electrolite; and the icosahedral and normal Al-Mn alloys to see if the two phases had measurably different density of states which have been predicted. All spectra shown are produced when core holes generated by energetic electrons or photons are filled by radiative transitions from conduction band states. Dipole selection rules govern the transitions. Thus, K spectra provide a measure of the p-symmetic partial density of states (DOS) near the atom. Similarly, L spectra produced by transitions to p-core holes map the s and d symmetric DOS in the vicinity of the atom with the core hole.

  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. High-energy X-ray diffraction studies of disordered materials

    International Nuclear Information System (INIS)

    Kohara, Shinji; Suzuya, Kentaro

    2003-01-01

    With the arrival of the latest generation of synchrotron sources and the introduction of advanced insertion devices (wigglers and undulators), the high-energy (E≥50 keV) X-ray diffraction technique has become feasible, leading to new approaches in the quantitative study of the structure of disordered materials. High-energy X-ray diffraction has several advantages: higher resolution in real space due to a wide range of scattering vector Q, smaller correction terms (especially the absorption correction), reduction of truncation errors, the feasibility of running under extreme environments, including high-temperatures and high-pressures, and the ability to make direct comparisons between X-ray and neutron diffraction data. Recently, high-energy X-ray diffraction data have been combined with neutron diffraction data from a pulsed source to provide more detailed and reliable structural information than that hitherto available

  17. Fast X-ray microdiffraction techniques for studying irreversible transformations in materials.

    Science.gov (United States)

    Kelly, Stephen T; Trenkle, Jonathan C; Koerner, Lucas J; Barron, Sara C; Walker, Nöel; Pouliquen, Philippe O; Tate, Mark W; Gruner, Sol M; Dufresne, Eric M; Weihs, Timothy P; Hufnagel, Todd C

    2011-05-01

    A pair of techniques have been developed for performing time-resolved X-ray microdiffraction on irreversible phase transformations. In one technique capillary optics are used to focus a high-flux broad-spectrum X-ray beam to a 60 µm spot size and a fast pixel array detector is used to achieve temporal resolution of 55 µs. In the second technique the X-rays are focused with Kirkpatrick-Baez mirrors to achieve a spatial resolution better than 10 µm and a fast shutter is used to provide temporal resolution better than 20 µs while recording the diffraction pattern on a (relatively slow) X-ray CCD camera. Example data from experiments are presented where these techniques are used to study self-propagating high-temperature synthesis reactions in metal laminate foils.

  18. Feasibility study of total reflection X-ray fluorescence analysis using a liquid metal jet X-ray tube

    Energy Technology Data Exchange (ETDEWEB)

    Maderitsch, A.; Smolek, S. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria); Wobrauschek, P., E-mail: wobi@ati.ac.at [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria); Streli, C. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria); Takman, P. [Excillum AB, Finlandsgatan 14, 164 74 Kista (Sweden)

    2014-09-01

    Total reflection X-ray spectroscopy (TXRF) is a powerful analytical technique for qualitative and quantitative analysis of trace and ultratrace elements in a sample with lower limits of detection (LLDs) of pg/g to ng/g in concentration and absolute high fg levels are attainable. Several X-ray sources, from low power (few W), 18 kW rotating anodes to synchrotron radiation, are in use for the excitation and lead accordingly to their photon flux delivered on the sample the detection limits specified. Not only the power, but also the brilliance and focal shape are of importance for TXRF. A microfocus of 50–100 μm spot size or the line focus of diffraction tubes is best suited. Excillum developed a new approach in the design of a source: the liquid metal jet anode. In this paper the results achieved with this source are described. A versatile TXRF spectrometer with vacuum chamber designed at Atominstitut was used for the experiments. A multilayer monochromator selecting the intensive Ga-Kα radiation was taken and the beam was collimated by 50 μm slits. Excellent results regarding geometric beam stability, high fluorescence intensities and low background were achieved leading to detection limits in the high fg range for Ni. A 100 mm{sup 2} silicon drift detector (SDD) collimated to 80 mm{sup 2} was used to collect the fluorescence radiation. The results from measurements on single element samples are presented. - Highlights: • Using a new X-ray source for TXRF • Liquid metal jet X-ray source from Excillum • Offers improvements for lab based TXRF spectrometers • Can also be important for related techniques.

  19. Study of properties of chemically modified samples of halloysite mineral with X-ray fluorescence and X-ray powder diffraction methods

    International Nuclear Information System (INIS)

    Banaś, D.; Kubala-Kukuś, A.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.; Czech, K.; Garnuszek, M.; Słomkiewicz, P.; Szczepanik, B.

    2013-01-01

    Elemental and chemical composition of raw and activated samples of halloysite mineral using wavelength dispersive X-ray fluorescence (WDXRF), total reflection X-ray fluorescence (TXRF) and X-ray powder diffraction (XRPD) methods were determined. As the result, it has been shown that application of the complementary X-ray spectrometry techniques allows very precise observation of changes in composition of halloysite mineral samples caused by its chemical modifications. Sample preparation procedure and usability of the research methods applied are described in details. Procedure of activation of raw halloysite mineral samples by etching them in sulfuric acid of various concentrations has been described and discussed. The ability of the samples to adsorb lead from intentionally contaminated water was tested and confirmed. - Author-Highlights: • We measured elemental and chemical composition of raw and activated halloysite mineral samples. • We showed that X-ray techniques allow precise study of changes in the sample composition. • We describe procedure of activation of the samples by etching them in sulfuric acid. • We tested ability of halloysite mineral to absorb lead from contaminated water

  20. In vitro enzymatic studies on the nature and repair of x-ray induced lesions in DNA

    International Nuclear Information System (INIS)

    Wallace, S.S.

    1979-01-01

    Areas studied include: purification and properties of enzyme probes for x-ray induced DNA lesions using E. Coli x-ray endonuclease and S. cerevisiae endonuclease E; use of enzymes probes; and use of physical, chemical and enzymatic probes to quantify x-ray-induced lesions in viruses and cells

  1. A study of the reactivity of elemental Cr/Se/Te thin multilayers using X-ray reflectometry, in situ X-ray diffraction and X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Behrens, Malte; Tomforde, Jan; May, Enno; Kiebach, Ragnar; Bensch, Wolfgang; Haeussler, Dietrich; Jaeger, Wolfgang

    2006-01-01

    The reactivity of [Cr/Se/Te] multilayers under annealing was investigated using X-ray reflectometry, in situ X-ray diffraction, X-ray absorption fine structure (XAFS) measurements and transmission electron microscopy. For all samples, interdiffusion was complete at temperatures between 100 and 300 deg. C, depending on the repeating tri-layer thickness. A crystalline phase nucleated approximately 20 deg. C above the temperature where interdiffusion was finished. The first crystalline phase in a binary Cr/Te sample was layered CrTe 3 nucleating at 230 deg. C. In ternary samples (Se:Te=0.6-1.2), the low-temperature nucleation of such a layered CrQ 3 (Q=Se, Te) phase is suppressed and instead the phase Cr 2 Q 3 nucleates first. Interestingly, this phase decomposes around 500 deg. C into layered CrQ 3 . In contrast, binary Cr/Se samples form stable amorphous alloys after interdiffusion and Cr 3 Se 4 nucleates around 500 deg. C as the only crystalline phase. Evaluation of the XAFS data of annealed samples yield Se-Cr distances of 2.568(1) and 2.552(1) A for Cr 2 Q 3 and CrQ 3 , respectively. In the latter sample, higher coordination shells around Se are seen accounting for the Se-Te contacts in the structure. - Graphical abstract: The first step of the reaction of elemental Cr/Te/Se-multilayers is the interdiffusion of the elements as evidenced by the decay of the modulation peaks in the low-angle region of the X-ray diffraction patterns. The subsequent growth of Bragg peaks at higher scattering angles indicates crystallization of chromium chalcogenide Cr 2 Te 3- x Se x

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

    Indian Academy of Sciences (India)

    WINTEC

    CgI…CgJ represents the distance between the ring centroids; CgI…P, the perpendicu- lar distance of the centroid of one ring from the plane of the other. α is the dihedral angle between the planes of rings I and J; β is the angle between normal to the cen- troid of ring I and the line joining ring centroids; Δ is the displacement ...

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

    International Nuclear Information System (INIS)

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

    2001-01-01

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

  4. Development of an x-ray beam line at the NSLS for studies in materials science using x-ray absorption spectroscopy. Progress report

    International Nuclear Information System (INIS)

    Sayers, D.E.

    1985-01-01

    This has been an exciting year for our PRT, highlighted by the running of the NSLS x-ray ring in an operational mode beginning in May of this year. Our line X-11A was the first to obtain an experimental spectrum and the first to publish a paper with results from the x-ray ring. These early successes have allowed us to run in an operational mode during the entire time that the x-raying ring itself has been operational. In addition to a number of exciting initial scientific results described, the initial results, particularly in the four crystal mode, have verified our original optical design and demonstrated an improved resolution using the four crystals. This will have a significant impact on near edge (XANES) studies

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

    Science.gov (United States)

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

    2013-01-01

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

  6. Radiation effects and metalloproteins studied by x-ray photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Wurzbach, J.A.

    1975-07-01

    X-ray photoelectron spectroscopy (XPS) is used to study the bonding structure at the iron site of cytochrome c and the bonding of rare earth ions to the phosphate oxygens of ATP. Radiation effects are studied on several amino acid and simple peptide model systems. The emission spectrum of the x-ray source is calculated from literature references. The distributions of photon energy as a function of photon frequency and as a function of take-off angle are obtained. From these distributions, the radiation dose absorbed by an organic sample is found to be 10 6 rads/sec. The C 1s and N 1s spectra of amino acids and peptides are studied to characterize an internal reference standard for protein XPS spectra. Samples of native cytochrome c prepared from solutions of pH 1.5, 3, 7, and 11 are studied. Control samples include porphyrin cytochrome c (PCC), the metal free analogue of the native protein, and microperoxidase (MP), a mixture of heme peptides derived from the peptic digestion of cytochrome c. These samples show two S 2p peaks. The first peak has a binding energy (BE) of 163 eV, which corresponds to the S containing amino acids; the second peak is shifted to 167 eV. This large shift may be the result of Fe-S binding, or oxidation, or both. Low spin ferricytochrome c and ferri-MP were found to have Fe 3p BE's that are unusually low (51 eV) compared to other ferric compounds (54 to 58 eV) and even Fe metal (53 eV). X-ray crystal structures of these compounds show that low spin heme Fe lies in the porphyrin plane; while, high spin heme Fe is displaced above the plane. The N 1s and P 2p spectra of ATP show no change except slight broadening when Nd 3+ is substituted for Na + . Thus, there is no inconsistency with proposals that rare earth ions might be useful as substitutes for alkali metal ions and alkaline earth ions in proteins

  7. Radiation effects and metalloproteins studied by x-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Wurzbach, J.A.

    1975-07-01

    X-ray photoelectron spectroscopy (XPS) is used to study the bonding structure at the iron site of cytochrome c and the bonding of rare earth ions to the phosphate oxygens of ATP. Radiation effects are studied on several amino acid and simple peptide model systems. The emission spectrum of the x-ray source is calculated from literature references. The distributions of photon energy as a function of photon frequency and as a function of take-off angle are obtained. From these distributions, the radiation dose absorbed by an organic sample is found to be 10/sup 6/ rads/sec. The C 1s and N 1s spectra of amino acids and peptides are studied to characterize an internal reference standard for protein XPS spectra. Samples of native cytochrome c prepared from solutions of pH 1.5, 3, 7, and 11 are studied. Control samples include porphyrin cytochrome c (PCC), the metal free analogue of the native protein, and microperoxidase (MP), a mixture of heme peptides derived from the peptic digestion of cytochrome c. These samples show two S 2p peaks. The first peak has a binding energy (BE) of 163 eV, which corresponds to the S containing amino acids; the second peak is shifted to 167 eV. This large shift may be the result of Fe-S binding, or oxidation, or both. Low spin ferricytochrome c and ferri-MP were found to have Fe 3p BE's that are unusually low (51 eV) compared to other ferric compounds (54 to 58 eV) and even Fe metal (53 eV). X-ray crystal structures of these compounds show that low spin heme Fe lies in the porphyrin plane; while, high spin heme Fe is displaced above the plane. The N 1s and P 2p spectra of ATP show no change except slight broadening when Nd/sup 3 +/ is substituted for Na/sup +/. Thus, there is no inconsistency with proposals that rare earth ions might be useful as substitutes for alkali metal ions and alkaline earth ions in proteins.

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

    International Nuclear Information System (INIS)

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

    1997-01-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  10. Neutron, x-ray scattering and TEM studies of Ni-Ti multilayers

    International Nuclear Information System (INIS)

    Keem, J.E.; Wood, J.; Grupido, N.; Hart, K.; Nutt, S.; Reichel, D.G.; Yelon, W.B.

    1988-01-01

    The authors present an analysis of Ni-Ti multilayer neutron reflectors and supermirrors undertaken to identify the causes of the lower than expected observed scattering power and critical angle enhancement of Ni-Ti supermirrors. Results of these investigations focus attention on cusp formation in the Ni-Ti bilayers as probable cause for the reduced neutron scattering power. Grazing angle x-ray and neutron scattering, wide angle neutron diffraction and analytical cross sectional TEM have been used. The multilayers were produced by magnetron sputtering and ion-beam deposition on float glass substrates and silicon wafers

  11. Orientation of mineral crystals by collagen fibers during in vivo bone engineering: An X-ray diffraction imaging study

    International Nuclear Information System (INIS)

    Cedola, A.; Mastrogiacomo, M.; Lagomarsino, S.; Cancedda, R.; Giannini, C.; Guagliardi, A.; Ladisa, M.; Burghammer, M.; Rustichelli, F.; Komlev, V.

    2007-01-01

    The mechanism of mineralized bone matrix deposition was investigated taking advantage of a tissue engineering approach in which bone tissue is formed when porous ceramic scaffold is loaded with bone marrow stromal cells and implanted in vivo. The aim of our study is to point out the interaction between the newly formed mineral crystals and the scaffold imposing the three-dimensional desired architecture to the growing bone. High spatial resolution Small Angle X-ray Scattering measurements obtained using synchrotron radiation and X-ray waveguide as optical element allowed a local structural study at the bone-scaffold interface. Using an original methodology for data analysis, we obtained a two-dimensional microscopic map of the mineralization degree, the collagen presence and the mineral orientation degree around the scaffold pore

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

    Science.gov (United States)

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

    2017-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-01

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

  14. 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)

    Sayers, D.E.

    1986-01-01

    Although only in operation since May, 1985, the X-11 participation research team (PRT) at the NSLS has already demonstrated that it is one of the leading centers of x-ray absorption spectroscopy (XAS). During this time, results have been obtained and programs initiated in a number of areas, for example: interfaces, including deposited metal-metal and metal-semiconductor systems, multilayers and ion implanted layers; electrochemical systems, including Pt electrode fuel cells, Ni oxide battery electrodes, conducting polymers, passivation and corrosion; catalysts, including highly-dispersed supported metal catalysts and zeolite systems; quasi-crystals, heavy fermion systems, uranium and neptunium compounds, rare gas clusters, disordered metals and semiconductors, ferroelectric transition; and, biological systems and related models, including synthetic porphyrins and a number of metalloproteins. In concert with these scientific results have been a number of developments involving the technique itself. These include implementation of unique optical systems on both the A and B lines for optical performance over their designed energy ranges, advances in experimental capability, particular in glancing angle studies, optimization of ion chambers for surface studies, the improvement of electron yield detectors, and improved software for data acquisition and analysis. This report emphasizes some of the research highlights and significant developments of our PRT which occurred during the past year. A detailed bibliography of papers and talks resulting from work done at our beamline and the progress reports for our PRT which were in the 1985 NSLS Annual Report are appended

  15. A comprehensive long term study of the radio and X-ray Variability of NGC 4051 Paper II

    OpenAIRE

    Jones, Sadie; McHardy, Ian; Maccarone, Thomas J.

    2016-01-01

    The origin of the low luminosity radio emission in radio-quiet AGN, is unknown. The detection of a positive correlation between the radio and X-ray emission would imply a jet-like origin, similar to that seen in `hard state' X-ray binary systems. In our previous work, we found no believable radio variability in the well known X-ray bright Seyfert 1 galaxy NGC 4051, despite large amplitude X-ray variability. In this study we have carefully re-analysed radio and X-ray observations using the sam...

  16. Feasibility study of total reflection X-ray fluorescence analysis using a liquid metal jet X-ray tube

    Science.gov (United States)

    Maderitsch, A.; Smolek, S.; Wobrauschek, P.; Streli, C.; Takman, P.

    2014-09-01

    Total reflection X-ray spectroscopy (TXRF) is a powerful analytical technique for qualitative and quantitative analysis of trace and ultratrace elements in a sample with lower limits of detection (LLDs) of pg/g to ng/g in concentration and absolute high fg levels are attainable. Several X-ray sources, from low power (few W), 18 kW rotating anodes to synchrotron radiation, are in use for the excitation and lead accordingly to their photon flux delivered on the sample the detection limits specified. Not only the power, but also the brilliance and focal shape are of importance for TXRF. A microfocus of 50-100 μm spot size or the line focus of diffraction tubes is best suited. Excillum developed a new approach in the design of a source: the liquid metal jet anode. In this paper the results achieved with this source are described. A versatile TXRF spectrometer with vacuum chamber designed at Atominstitut was used for the experiments. A multilayer monochromator selecting the intensive Ga-Kα radiation was taken and the beam was collimated by 50 μm slits. Excellent results regarding geometric beam stability, high fluorescence intensities and low background were achieved leading to detection limits in the high fg range for Ni. A 100 mm2 silicon drift detector (SDD) collimated to 80 mm2 was used to collect the fluorescence radiation. The results from measurements on single element samples are presented.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-11-14

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

  18. Application of the X-ray fluorescence analysis and X-ray diffraction in geochemical studies of the Pleistocene tills from Holy Cross Mountains

    Science.gov (United States)

    Kubala-Kukuś, A.; Ludwikowska-Kȩdzia, M.; Banaś, D.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.

    2013-12-01

    X-ray fluorescence analysis methods (wavelength dispersive X-ray fluorescence analysis (WDXRF) and total reflection X-ray fluorescence (TXRF)) and X-ray powder diffraction (XRPD) have been applied in complementary geochemical studies of the Pleistocene till samples. The XRPD technique gave information about the mineral composition of the analyzed samples while the WDXRF and TXRF studies allowed the fast elemental analysis. The till samples were collected from different regions of Holy Cross Mountains (located in central Poland) which are still not unambiguously described in the context of the geochemical studies of the Quaternary sediments. The analysis was concentrated on the geochemical composition of the till samples both for materials occurring on the surface (characterized by continuous weathering processes) and for samples taken from core borehole. The overriding purpose of these studies is determination of the local lithotype of the tills and its lithologic and petrographic diagnostic properties, including the chemical composition of clay and minerals found in the clay. In the presented work the experimental sets up, sample preparation procedure and measurements programme will be discussed in details. Finally, the elemental and mineral compositions will be presented for studied different groups of the samples.

  19. Dental x-rays and the risk of thyroid cancer: A case-control study

    International Nuclear Information System (INIS)

    Memon, Anjum; Godward, Sara; Williams, Dillwyn; Siddique, Iqbal; Al-Saleh, Khalid

    2010-01-01

    The thyroid gland is highly susceptible to radiation carcinogenesis and exposure to high-dose ionising radiation is the only established cause of thyroid cancer. Dental radiography, a common source of low-dose diagnostic radiation exposure in the general population, is often overlooked as a radiation hazard to the gland and may be associated with the risk of thyroid cancer. An increased risk of thyroid cancer has been reported in dentists, dental assistants, and x-ray workers; and exposure to dental x-rays has been associated with an increased risk of meningiomas and salivary tumours. Methods. To examine whether exposure to dental x-rays was associated with the risk of thyroid cancer, we conducted a population-based case-control interview study among 313 patients with thyroid cancer and a similar number of individually matched (year of birth ± three years, gender, nationality, district of residence) control subjects in Kuwait. Results. Conditional logistic regression analysis, adjusted for other upper-body x-rays, showed that exposure to dental x-rays was significantly associated with an increased risk of thyroid cancer (odds ratio = 2.1, 95% confidence interval: 1.4, 3.1) (p=0.001) with a dose-response pattern (p for trend <0.0001). The association did not vary appreciably by age, gender, nationality, level of education, or parity. Discussion. These findings, based on self-report by cases/controls, provide some support to the hypothesis that exposure to dental x-rays, particularly multiple exposures, may be associated with an increased risk of thyroid cancer; and warrant further study in settings where historical dental x-ray records may be available.

  20. Ultrashort X-ray pulse science

    Energy Technology Data Exchange (ETDEWEB)

    Chin, Alan Hap [Univ. of California, Berkeley, CA (US). Dept. of Physics; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    1998-05-01

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90° Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ~ 300 fs, 30 keV (0.4 Å) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been demonstrated as a