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Sample records for solutions small-angle x-ray

  1. Small-angle X-ray scattering of solutions

    International Nuclear Information System (INIS)

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

    1982-01-01

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

  2. 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

  3. 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)

  4. 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

  5. X-ray small angle scattering of polymer solutions

    International Nuclear Information System (INIS)

    Koyama, Ryuzo

    1975-01-01

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

  6. 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 ...

  7. 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.

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

  9. 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)

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

    CERN Document Server

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

    2002-01-01

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

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

    Science.gov (United States)

    Banuelos, Jose; Urquidi, Jacob

    2008-10-01

    The ability of proteins to change their conformation in response to changes in their environment has consequences in biological processes like metabolism, chemical regulation in cells, and is believed to play a role in the onset of several neurodegenerative diseases. Factors such as a change in temperature, pressure, and the introduction of ions into the aqueous environment of a protein can give rise to the folding/unfolding of a protein. As a protein unfolds, the ratio of nonpolar to polar groups exposed to water changes, affecting a protein's thermodynamic properties. Using small angle x-ray scattering (SAXS), we are currently studying the intermediate protein conformations that arise during the folding/unfolding process as a function of temperature for five globular proteins. Trends in the observed intermediate structures of these globular proteins, along with correlations with data on protein thermodynamics may help elucidate shared characteristics between all proteins in the folding/unfolding process. Experimental design considerations will be discussed and preliminary results for some of these systems will be presented.

  12. 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.)

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  14. 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.

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

    Science.gov (United States)

    Li, Mu; Zhang, Mingxin; Wang, Weiyu; Cheng, Stephen Z. D.; Yin, Panchao

    2018-05-01

    Nano-scaled polyoxometalates (POMs) clusters with sizes ranging from 1 to 10 nm attract tremendous attention and have been extensively studied due to POMs' fascinating structural characteristics and prospects for wide-ranging applications. As a unique class of nanoparticles with well-defined structural topologies and monodispersed masses, the structures and properties of POMs in both bulk state and solutions have been explored with several well-developed protocols. Small-angle X-ray scattering (SAXS) technique, as a powerful tool for studying polymers and nanoparticles, has been recently extended to the investigating of solution behaviors of POMs. In this mini-review, the general principle and typical experimental procedures of SAXS are illustrated first. The applications of SAXS in characterizing POMs' morphology, counterion distribution around POMs, and short-range interactions among POMs in solutions are highlighted. [Figure not available: see fulltext.

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

    International Nuclear Information System (INIS)

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

    1981-01-01

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

  17. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-31

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

  19. 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

  20. Small Angle X-Ray Scattering Detector

    Energy Technology Data Exchange (ETDEWEB)

    Hessler, Jan P.

    2004-06-15

    A detector for time-resolved small-angle x-ray scattering includes a nearly constant diameter, evacuated linear tube having an end plate detector with a first fluorescent screen and concentric rings of first fiber optic bundles for low angle scattering detection and an annular detector having a second fluorescent screen and second fiber optic bundles concentrically disposed about the tube for higher angle scattering detection. With the scattering source, i.e., the specimen under investigation, located outside of the evacuated tube on the tube's longitudinal axis, scattered x-rays are detected by the fiber optic bundles, to each of which is coupled a respective photodetector, to provide a measurement resolution, i.e., dq/q, where q is the momentum transferred from an incident x-ray to an x-ray scattering specimen, of 2% over two (2) orders of magnitude in reciprocal space, i.e., qmax/qmin approx=lO0.

  1. Study on the conformal variations of bovine and human serum albumin in solution using small angle X-ray scattering

    International Nuclear Information System (INIS)

    Olivieri, Johnny Rizzieri.

    1992-01-01

    It is reported a Small Angle X-Ray Scattering (SAXS) study of BSA (Bovine Serum Albumin) and HSA (Human Serum Albumin) on pH between 2.5 and 7.0. The measured scattering intensities, normalized in relation to incident beam, exposition time and scattering due to solvent and capillary, and corrected due to concentration and beam shape effects, have shown a strong dependence of the protein shape with pH for both albumins. It was found that the radius of gyration varies between 26.7 and 35 A, and the analyses of the distance distribution function. P(r), indicated that these proteins undergoes conformational changes with pH. Different theoretical shapes have been proposed and analysed comparing the computed P(r) function generated from the models with the experimental P(r). A large variety of shapes were found in both proteins, indicating that BSA and HSA are very flexibility macromolecules. (author). 60 refs., 49 figs., 7 tabs

  2. Solution small-angle x-ray scattering as a screening and predictive tool in the fabrication of asymmetric block copolymer membranes

    KAUST Repository

    Dorin, Rachel Mika; Marques, Debora S.; Sai, Hiroaki; Vainio, Ulla; Phillip, William A.; Peinemann, Klaus; Nunes, Suzana Pereira; Wiesner, Ulrich B.

    2012-01-01

    Small-angle X-ray scattering (SAXS) analysis of the diblock copolymer poly(styrene-b-(4-vinyl)pyridine) in a ternary solvent system of 1,4-dioxane, tetrahydrofuran, and N,N-dimethylformamide, and the triblock terpolymer poly(isoprene-b-styrene-b-(4-vinyl)-pyridine) in a binary solvent system of 1,4-dioxane and tetrahydrofuran, reveals a concentration-dependent onset of ordered structure formation. Asymmetric membranes fabricated from casting solutions with polymer concentrations at or slightly below this ordering concentration possess selective layers with the desired nanostructure. In addition to rapidly screening possible polymer solution concentrations, solution SAXS analysis also predicts hexagonal and square pore lattices of the final membrane surface structure. These results suggest solution SAXS as a powerful tool for screening casting solution concentrations and predicting surface structure in the fabrication of asymmetric ultrafiltration membranes from self-assembled block copolymers. (Figure presented) © 2012 American Chemical Society.

  3. Solution small-angle x-ray scattering as a screening and predictive tool in the fabrication of asymmetric block copolymer membranes

    KAUST Repository

    Dorin, Rachel Mika

    2012-05-15

    Small-angle X-ray scattering (SAXS) analysis of the diblock copolymer poly(styrene-b-(4-vinyl)pyridine) in a ternary solvent system of 1,4-dioxane, tetrahydrofuran, and N,N-dimethylformamide, and the triblock terpolymer poly(isoprene-b-styrene-b-(4-vinyl)-pyridine) in a binary solvent system of 1,4-dioxane and tetrahydrofuran, reveals a concentration-dependent onset of ordered structure formation. Asymmetric membranes fabricated from casting solutions with polymer concentrations at or slightly below this ordering concentration possess selective layers with the desired nanostructure. In addition to rapidly screening possible polymer solution concentrations, solution SAXS analysis also predicts hexagonal and square pore lattices of the final membrane surface structure. These results suggest solution SAXS as a powerful tool for screening casting solution concentrations and predicting surface structure in the fabrication of asymmetric ultrafiltration membranes from self-assembled block copolymers. (Figure presented) © 2012 American Chemical Society.

  4. 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 ...

  5. Investigation of the topological shape of bovine serum albumin in solution by small-angle x-ray scattering at Beijing synchrotron radiation facility

    International Nuclear Information System (INIS)

    Dong Shuqiang; Chen Ximeng; Li Liqin; Liu Peng; Dong Yuhui

    2008-01-01

    This paper reports that at a newly constructed small-angle x-ray scattering station of Beijing Synchrotron Radiation Facility, the topological shape of ligand-free bovine serum albumin in solution has been investigated. An appropriate scattering curve is obtained and the calculated value of the gyration radius is 31.2ű0.25A (1Å=0.1 nm) which is coincident with other ones' results. It finds that the low-resolution structure models obtained by making use of ab initio reconstruction methods are fitting the crystal structure of human serum albumin very well. All of these results perform the potential of the beamline to apply to structural biology studies. The characteristics, the defects, and the improving measures of the station in future are also discussed. (condensed matter: structure, thermal and mechanical properties)

  6. 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...

  7. 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

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

    Science.gov (United States)

    Fukasawa, Toshiko; Sato, Takaaki

    2011-02-28

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

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

    International Nuclear Information System (INIS)

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

    1981-02-01

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

  10. 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.

  11. Small-angle X-ray Solution Scattering Study of the Multi-aminoacyl-tRNA Synthetase Complex Reveals an Elongated and Multi-armed particle*

    Science.gov (United States)

    Dias, José; Renault, Louis; Pérez, Javier; Mirande, Marc

    2013-01-01

    In animal cells, nine aminoacyl-tRNA synthetases are associated with the three auxiliary proteins p18, p38, and p43 to form a stable and conserved large multi-aminoacyl-tRNA synthetase complex (MARS), whose molecular mass has been proposed to be between 1.0 and 1.5 MDa. The complex acts as a molecular hub for coordinating protein synthesis and diverse regulatory signal pathways. Electron microscopy studies defined its low resolution molecular envelope as an overall rather compact, asymmetric triangular shape. Here, we have analyzed the composition and homogeneity of the native mammalian MARS isolated from rabbit liver and characterized its overall internal structure, size, and shape at low resolution by hydrodynamic methods and small-angle x-ray scattering in solution. Our data reveal that the MARS exhibits a much more elongated and multi-armed shape than expected from previous reports. The hydrodynamic and structural features of the MARS are large compared with other supramolecular assemblies involved in translation, including ribosome. The large dimensions and non-compact structural organization of MARS favor a large protein surface accessibility for all its components. This may be essential to allow structural rearrangements between the catalytic and cis-acting tRNA binding domains of the synthetases required for binding the bulky tRNA substrates. This non-compact architecture may also contribute to the spatiotemporal controlled release of some of its components, which participate in non-canonical functions after dissociation from the complex. PMID:23836901

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

    Science.gov (United States)

    Dahani, Mohamed; Barret, Laurie-Anne; Raynal, Simon; Jungas, Colette; Pernot, Pétra; Polidori, Ange; Bonneté, Françoise

    2015-01-01

    The structural and interactive properties of two novel hemifluorinated surfactants, F2H9-β-M and F4H5-β-M, the syntheses of which were based on the structure and hydrophobicity of the well known dodecyl-β-maltoside (DD-β-M), are described. The shape of their micellar assemblies was characterized by small-angle X-ray scattering and their intermicellar inter­actions in crystallizing conditions were measured by dynamic light scattering. Such information is essential for surfactant phase-diagram determination and membrane-protein crystallization. PMID:26144228

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

    DEFF Research Database (Denmark)

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  15. The new NCPSS BL19U2 beamline at the SSRF for small-angle X-ray scattering from biological macromolecules in solution.

    Science.gov (United States)

    Li, Na; Li, Xiuhong; Wang, Yuzhu; Liu, Guangfeng; Zhou, Ping; Wu, Hongjin; Hong, Chunxia; Bian, Fenggang; Zhang, Rongguang

    2016-10-01

    The beamline BL19U2 is located in the Shanghai Synchrotron Radiation Facility (SSRF) and is its first beamline dedicated to biological material small-angle X-ray scattering (BioSAXS). The electrons come from an undulator which can provide high brilliance for the BL19U2 end stations. A double flat silicon crystal (111) monochromator is used in BL19U2, with a tunable monochromatic photon energy ranging from 7 to 15 keV. To meet the rapidly growing demands of crystallographers, biochemists and structural biologists, the BioSAXS beamline allows manual and automatic sample loading/unloading. A Pilatus 1M detector (Dectris) is employed for data collection, characterized by a high dynamic range and a short readout time. The highly automated data processing pipeline SASFLOW was integrated into BL19U2, with help from the BioSAXS group of the European Molecular Biology Laboratory (EMBL, Hamburg), which provides a user-friendly interface for data processing. The BL19U2 beamline was officially opened to users in March 2015. To date, feedback from users has been positive and the number of experimental proposals at BL19U2 is increasing. A description of the new BioSAXS beamline and the setup characteristics is given, together with examples of data obtained.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-05-01

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

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

    International Nuclear Information System (INIS)

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

    1980-01-01

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

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

    International Nuclear Information System (INIS)

    Rinnerthaler, S.

    1998-06-01

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

  19. 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)

  20. 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)

  1. Low-Resolution Structure of the Full-Length Barley (Hordeum vulgare) SGT1 Protein in Solution, Obtained Using Small-Angle X-Ray Scattering

    Science.gov (United States)

    Taube, Michał; Pieńkowska, Joanna R.; Jarmołowski, Artur; Kozak, Maciej

    2014-01-01

    SGT1 is an evolutionarily conserved eukaryotic protein involved in many important cellular processes. In plants, SGT1 is involved in resistance to disease. In a low ionic strength environment, the SGT1 protein tends to form dimers. The protein consists of three structurally independent domains (the tetratricopeptide repeats domain (TPR), the CHORD- and SGT1-containing domain (CS), and the SGT1-specific domain (SGS)), and two less conserved variable regions (VR1 and VR2). In the present study, we provide the low-resolution structure of the barley (Hordeum vulgare) SGT1 protein in solution and its dimer/monomer equilibrium using small-angle scattering of synchrotron radiation, ab-initio modeling and circular dichroism spectroscopy. The multivariate curve resolution least-square method (MCR-ALS) was applied to separate the scattering data of the monomeric and dimeric species from a complex mixture. The models of the barley SGT1 dimer and monomer were formulated using rigid body modeling with ab-initio structure prediction. Both oligomeric forms of barley SGT1 have elongated shapes with unfolded inter-domain regions. Circular dichroism spectroscopy confirmed that the barley SGT1 protein had a modular architecture, with an α-helical TPR domain, a β-sheet sandwich CS domain, and a disordered SGS domain separated by VR1 and VR2 regions. Using molecular docking and ab-initio protein structure prediction, a model of dimerization of the TPR domains was proposed. PMID:24714665

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

    International Nuclear Information System (INIS)

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

    1985-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Schneidman-Duhovny Dina

    2012-07-01

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

  4. 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

  5. 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)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

  7. 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.

  8. 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

  9. 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.

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    CERN Document Server

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

    2003-01-01

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

  12. 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.

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

    Indian Academy of Sciences (India)

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

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

    NARCIS (Netherlands)

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

    2012-01-01

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

  15. 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.

  16. 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...

  17. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  20. Small-angle X-ray scattering 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.

  1. 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.

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

    International Nuclear Information System (INIS)

    Singh, P.; White, J.

    1999-01-01

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

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

    International Nuclear Information System (INIS)

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

    1976-01-01

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

  4. 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)

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

    CERN Document Server

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

    2002-01-01

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

  6. 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.

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

    Directory of Open Access Journals (Sweden)

    Michal Jan Gajda

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

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

    Science.gov (United States)

    Dahal, Eshan; Choi, Mina; Alam, Nadia; Bhirde, Ashwinkumar A.; Beaucage, Serge L.; Badano, Aldo

    2017-08-01

    Amyloid fibrils are highly structured protein aggregates associated with a wide range of diseases including Alzheimer’s and Parkinson’s. We report a structural investigation of an amyloid fibril model prepared from a commonly used plasma protein (bovine serum albumin (BSA)) using small-angle x-ray scattering (SAXS) technique. As a reference, the size estimates from SAXS are compared to dynamic light scattering (DLS) data and the presence of amyloid-like fibrils is confirmed using Congo red absorbance assay. Our SAXS results consistently show the structural transformation of BSA from spheroid to rod-like elongated structures during the fibril formation process. We observe the elongation of fibrils over two months with fibril length growing from 35.9  ±  3.0 nm to 51.5  ±  2.1 nm. Structurally metastable fibrils with distinct SAXS profiles have been identified. As proof of concept, we demonstrate the use of such distinct SAXS profiles to detect fibrils in the mixture solutions of two species by estimating their volume fractions. This easily detectable and well-characterized amyloid fibril model from BSA can be readily used as a control or standard reference to further investigate SAXS applications in the detection of structurally diverse amyloid fibrils associated with protein aggregation diseases.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-01

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

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

    Science.gov (United States)

    Schaff, Florian; Bech, Martin; Zaslansky, Paul; Jud, Christoph; Liebi, Marianne; Guizar-Sicairos, Manuel; Pfeiffer, Franz

    2015-11-19

    When used in combination with raster scanning, small-angle X-ray scattering (SAXS) has proven to be a valuable imaging technique of the nanoscale, for example of bone, teeth and brain matter. Although two-dimensional projection imaging has been used to characterize various materials successfully, its three-dimensional extension, SAXS computed tomography, poses substantial challenges, which have yet to be overcome. Previous work using SAXS computed tomography was unable to preserve oriented SAXS signals during reconstruction. Here we present a solution to this problem and obtain a complete SAXS computed tomography, which preserves oriented scattering information. By introducing virtual tomography axes, we take advantage of the two-dimensional SAXS information recorded on an area detector and use it to reconstruct the full three-dimensional scattering distribution in reciprocal space for each voxel of the three-dimensional object in real space. The presented method could be of interest for a combined six-dimensional real and reciprocal space characterization of mesoscopic materials with hierarchically structured features with length scales ranging from a few nanometres to a few millimetres--for example, biomaterials such as bone or teeth, or functional materials such as fuel-cell or battery components.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Changizi V

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-12-15

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

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

    International Nuclear Information System (INIS)

    Hoyt, J.

    1982-07-01

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

  16. 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.

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

    Science.gov (United States)

    Renner, Max; Paesen, Guido C; Grison, Claire M; Granier, Sébastien; Grimes, Jonathan M; Leyrat, Cédric

    2017-11-01

    The phosphoprotein (P) is the main and essential cofactor of the RNA polymerase (L) of non-segmented, negative-strand RNA viruses. P positions the viral polymerase onto its nucleoprotein-RNA template and acts as a chaperone of the nucleoprotein (N), thereby preventing nonspecific encapsidation of cellular RNAs. The phosphoprotein of human metapneumovirus (HMPV) forms homotetramers composed of a stable oligomerization domain (P core ) flanked by large intrinsically disordered regions (IDRs). Here we combined x-ray crystallography of P core with small angle x-ray scattering (SAXS)-based ensemble modeling of the full-length P protein and several of its fragments to provide a structural description of P that captures its dynamic character, and highlights the presence of varyingly stable structural elements within the IDRs. We discuss the implications of the structural properties of HMPV P for the assembly and functioning of the viral transcription/replication machinery.

  18. 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.

  19. 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

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

    International Nuclear Information System (INIS)

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

    1983-01-01

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

  1. 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

  2. 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.

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

    Science.gov (United States)

    König, Nico; Paulus, Michael; Julius, Karin; Schulze, Julian; Voetz, Matthias; Tolan, Metin

    2017-12-01

    In the present work two subclasses of the human antibody Immunoglobulin G (IgG) have been investigated by Small-Angle X-ray Scattering under high hydrostatic pressures up to 5kbar. It is shown that IgG adopts a symmetric T-shape in solution which differs significantly from available crystal structures. Moreover, high-pressure experiments verify the high stability of the IgG molecule. It is not unfolded by hydrostatic pressures of up to 5kbar but a slight increase of the radius of gyration was observed at elevated pressures. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. 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.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

    The early caries lesion in bovine tooth enamel was studied by two different X-ray diffraction systems at the SPring-8 third generation synchrotron radiation facility. Both allowed us simultaneous measurement of the small and large angle regions. The beam size was 6μm at BL40XU and 50μm at BL45XU. The small-angle scattering from voids in the hydroxyapatite crystallites and the wide-angle diffraction from the hydroxyapatite crystals were observed simultaneously. At BL40XU an X-ray image intensifier was used for the small-angle and a CMOS flatpanel detector for the large-angle region. At BL45XU, a large-area CCD detector was used to cover both regions. A linear microbeam scan at BL40XU showed a detailed distribution of voids and crystals and made it possible to examine the structural details in the lesion. The two-dimensional scan at BL45XU showed distribution of voids and crystals in a wider region in the enamel. The simultaneous small- and wide-angle measurement with a microbeam is a powerful tool to elucidate the mechanisms of demineralization and remineralization in the early caries lesion.

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

    Science.gov (United States)

    Paudel, Durga; Atta-Fynn, Raymond; Drabold, David A.; Elliott, Stephen R.; Biswas, Parthapratim

    2018-05-01

    We present a computational study of small-angle x-ray scattering (SAXS) in amorphous silicon (a -Si) with particular emphasis on the morphology and microstructure of voids. The relationship between the scattering intensity in SAXS and the three-dimensional structure of nanoscale inhomogeneities or voids is addressed by generating large high-quality a -Si networks with 0.1%-0.3% volume concentration of voids, as observed in experiments using SAXS and positron annihilation spectroscopy. A systematic study of the variation of the scattering intensity in the small-angle scattering region with the size, shape, number density, and the spatial distribution of the voids in the networks is presented. Our results suggest that the scattering intensity in the small-angle region is particularly sensitive to the size and the total volume fraction of the voids, but the effect of the geometry or shape of the voids is less pronounced in the intensity profiles. A comparison of the average size of the voids obtained from the simulated values of the intensity, using the Guinier approximation and Kratky plots, with that of the same from the spatial distribution of the atoms in the vicinity of void surfaces is presented.

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

    International Nuclear Information System (INIS)

    Choi, Sung Min

    2009-01-01

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

  8. Small angle neutron scattering by polymer solutions

    International Nuclear Information System (INIS)

    Farnoux, B.; Jannink, G.

    1980-08-01

    Small angle neutron scattering is an experimental technique introduced since about 10 years for the observation of the polymer conformation in all the concentration range from dilute solution to the melt. After a brief recall of the elementary relations between scattering amplitude, index of refraction and scattered intensity, two concepts related to this last quantity (the contrast and the pair correlation function) are discussed in details

  9. 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.

  10. 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.

  11. 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.

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  13. 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.

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

    KAUST Repository

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

    2011-01-01

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

  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. 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.

  17. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-03-01

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

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

    International Nuclear Information System (INIS)

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

    1985-01-01

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

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

    International Nuclear Information System (INIS)

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

    1981-07-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  2. 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

  3. 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)

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Athanasios Ch Mitropoulos

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

  6. 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.

  7. 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.

  8. 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.

  9. 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

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  11. 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.

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

    DEFF Research Database (Denmark)

    Stribeck, Norbert; Schneider, Konrad; Zeinolebadi, Ahmad

    2014-01-01

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

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

    Science.gov (United States)

    Jeffries, Cy M.; Graewert, Melissa A.; Blanchet, Clément E.; Langley, David B.; Whitten, Andrew E.; Svergun, Dmitri I

    2017-01-01

    Small-angle X-ray and neutron scattering (SAXS and SANS) are techniques used to extract structural parameters and determine the overall structures and shapes of biological macromolecules, complexes and assemblies in solution. The scattering intensities measured from a sample contain contributions from all atoms within the illuminated sample volume including the solvent and buffer components as well as the macromolecules of interest. In order to obtain structural information, it is essential to prepare an exactly matched solvent blank so that background scattering contributions can be accurately subtracted from the sample scattering to obtain the net scattering from the macromolecules in the sample. In addition, sample heterogeneity caused by contaminants, aggregates, mismatched solvents, radiation damage or other factors can severely influence and complicate data analysis so it is essential that the samples are pure and monodisperse for the duration of the experiment. This Protocol outlines the basic physics of SAXS and SANS and reveals how the underlying conceptual principles of the techniques ultimately ‘translate’ into practical laboratory guidance for the production of samples of sufficiently high quality for scattering experiments. The procedure describes how to prepare and characterize protein and nucleic acid samples for both SAXS and SANS using gel electrophoresis, size exclusion chromatography and light scattering. Also included are procedures specific to X-rays (in-line size exclusion chromatography SAXS) and neutrons, specifically preparing samples for contrast matching/variation experiments and deuterium labeling of proteins. PMID:27711050

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

    Directory of Open Access Journals (Sweden)

    Dritan Siliqi

    2018-02-01

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

  15. 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.

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

    International Nuclear Information System (INIS)

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

    1989-01-01

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

  17. 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

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

    Science.gov (United States)

    Baker, Matthew A B; Tuckwell, Andrew J; Berengut, Jonathan F; Bath, Jonathan; Benn, Florence; Duff, Anthony P; Whitten, Andrew E; Dunn, Katherine E; Hynson, Robert M; Turberfield, Andrew J; Lee, Lawrence K

    2018-06-04

    The rational design of complementary DNA sequences can be used to create nanostructures that self-assemble with nanometer precision. DNA nanostructures have been imaged by atomic force microscopy and electron microscopy. Small-angle X-ray scattering (SAXS) provides complementary structural information on the ensemble-averaged state of DNA nanostructures in solution. Here we demonstrate that SAXS can distinguish between different single-layer DNA origami tiles that look identical when immobilized on a mica surface and imaged with atomic force microscopy. We use SAXS to quantify the magnitude of global twist of DNA origami tiles with different crossover periodicities: these measurements highlight the extreme structural sensitivity of single-layer origami to the location of strand crossovers. We also use SAXS to quantify the distance between pairs of gold nanoparticles tethered to specific locations on a DNA origami tile and use this method to measure the overall dimensions and geometry of the DNA nanostructure in solution. Finally, we use indirect Fourier methods, which have long been used for the interpretation of SAXS data from biomolecules, to measure the distance between DNA helix pairs in a DNA origami nanotube. Together, these results provide important methodological advances in the use of SAXS to analyze DNA nanostructures in solution and insights into the structures of single-layer DNA origami.

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

    DEFF Research Database (Denmark)

    Yennawar, Hemant; Møller, Magda; Gillilan, Richard

    2011-01-01

    The X-ray crystal structure of sheep liver sorbitol dehydrogenase (slSDH) has been determined using the crystal structure of human sorbitol dehydrogenase (hSDH) as a molecular-replacement model. slSDH crystallized in space group I222 with one monomer in the asymmetric unit. A conserved tetramer...

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

    OpenAIRE

    Grudinin , Sergei; Garkavenko , Maria; Kazennov , Andrei

    2017-01-01

    International audience; A new method called Pepsi-SAXS is presented that calculates small-angle X-ray scattering profiles from atomistic models. The method is based on the multipole expansion scheme and is significantly faster compared with other tested methods. In particular, using the Nyquist–Shannon–Kotelnikov sampling theorem, the multipole expansion order is adapted to the size of the model and the resolution of the experimental data. It is argued that by using the adaptive expansion ord...

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

    CSIR Research Space (South Africa)

    Jonah, EO

    2012-10-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Sen; Luo, Sheng-Nian

    2018-02-16

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

  3. 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.

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

    Science.gov (United States)

    Jonas, A. M.; Legras, R.; Ferain, E.

    1998-03-01

    Nanoporous track-etched membranes with narrow pore size distributions and average pore size diameters tunable from 100 to 1000 Åare produced by the chemical etching of latent tracks in polymer films after irradiation by a beam of accelerated heavy ions. Nanoporous membranes are used for highly demanding filtration purposes, or as templates to obtain metallic or polymeric nanowires (L. Piraux et al., Nucl. Instr. Meth. Phys. Res. 1997, B131, 357). Such applications call for developments in nanopore size characterization techniques. In this respect, we report on the characterization by small-angle X-ray scattering (SAXS) of nanopore size distribution (nPSD) in polycarbonate track-etched membranes. The obtention of nPSD requires inverting an ill-conditioned inhomogeneous equation. We present different numerical routes to overcome the amplification of experimental errors in the resulting solutions, including a regularization technique allowing to obtain the nPSD without a priori knowledge of its shape. The effect of deviations from cylindrical pore shape on the resulting distributions are analyzed. Finally, SAXS results are compared to results obtained by electron microscopy and conductometry.

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

    International Nuclear Information System (INIS)

    Hayashi, Hisao; Hamada, Fumiyuki; Nakajima, Akio

    1975-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-07-27

    This contribution presents the main design features of the upgraded beamline ID02 (TRUSAXS). The beamline combines different small-angle X-ray scattering techniques in one unique instrument. The key component of this instrument is an evacuated (5×10{sup −3} mbar) stainless steel detector tube of length 34 m and diameter 2 m. Three different detectors (Rayonix MX170, Pilatus 300 K and FReLoN 4M) are housed inside a motorized wagon which travels along a rail system with very low parasitic lateral movements (± 0.3 mm). This system allows automatically changing the sample-to-detector distance from about 1 m to 31 m and selecting the desired detector. In addition, a wide angle detector (Rayonix LX170) is installed just above the entrance cone of the tube for optional wide-angle X-ray scattering measurements. The beamstop system enables monitoring of the X-ray beam intensity in addition to blocking the primary beam, and automated insertion of selected masks behind the primary beamstop. The focusing optics and collimation system permit to cover a scattering vector (q) range of 0.002 nm{sup −1} ≤ q ≤ 50 nm{sup −1} with one unique setting using 0.1 nm X-ray wavelength for moderate flux (5×10{sup 12} photons/sec). However, for higher flux (6x10{sup 13} photons/sec) or higher resolution (minimum q < 0.001 nm{sup −1}), focusing and collimation, respectively need to be varied. For a sample-to-detector distance of 31 m and 0.1 nm wavelength, two dimensional ultra small-angle X-ray scattering patterns can be recorded down to q≈0.001 nm{sup −1} with far superior quality as compared to one dimensional profiles obtained with a Bonse-Hart instrument.

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

    Energy Technology Data Exchange (ETDEWEB)

    Rol' bin, Yu A; Svergun, D I; Feigin, L A; Gashpar, Sh; Ronto, D [AN SSSR, Moscow. Inst. Kristallografii

    1980-01-01

    An attempt is made to obtain complete data on the form, sizes, weight and hydration of the T7 bacteriophage cultivated on E.coli cells and the peculiarities of phage DNA structure using the method of small-angle scattering.

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

    Science.gov (United States)

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

    2009-05-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    DEFF Research Database (Denmark)

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

    2018-01-01

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

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

    Science.gov (United States)

    Thompson, M.; Kluth, P.; Doerner, R. P.; Kirby, N.; Riley, D.; Corr, C. S.

    2016-02-01

    Grazing incidence small angle x-ray scattering was performed on tungsten samples exposed to helium plasma in the MAGPIE and Pisces-A linear plasma devices to measure the size distributions of resulting helium nano-bubbles. Nano-bubbles were fitted assuming spheroidal particles and an exponential diameter distribution. These particles had mean diameters between 0.36 and 0.62 nm. Pisces-A exposed samples showed more complex patterns, which may suggest the formation of faceted nano-bubbles or nano-scale surface structures.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-15

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

  14. 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.

  15. 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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

    The Src-homology 2 (SH2) domain of Csk-family protein tyrosine kinases acts as a conformational switch to regulate their catalytic activity, which in turn promotes the inhibition of their proto-oncogenic targets, the Src-family kinases. Here, the expression, purification, small-angle X-ray scattering and preliminary diffraction analysis of the SH2 domain of the Csk-homologous kinase is reported. The C-terminal Src kinase (Csk) and Csk-homologous kinase (CHK) are endogenous inhibitors of the proto-oncogenic Src family of protein tyrosine kinases (SFKs). Phosphotyrosyl peptide binding to their Src-homology 2 (SH2) domains activates Csk and CHK, enhancing their ability to suppress SFK signalling; however, the detailed mechanistic basis of this activation event is unclear. The CHK SH2 was expressed in Escherichia coli and the purified protein was characterized as monomeric by synchrotron small-angle X-ray scattering in-line with size-exclusion chromatography. The CHK SH2 crystallized in 0.2 M sodium bromide, 0.1 M bis-Tris propane pH 6.5 and 20% polyethylene glycol 3350 and the best crystals diffracted to ∼1.6 Å resolution. The crystals belonged to space group P2, with unit-cell parameters a = 25.8, b = 34.6, c = 63.2 Å, β = 99.4°

  17. 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.)

  18. 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.

  19. 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.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Science.gov (United States)

    Allen, Andrew; Zhang, Fan; Levine, Lyle; Ilavsky, Jan

    2013-03-01

    Ultra-small-angle X-ray scattering (USAXS) can probe microstructures over the nanometer-to-micrometer scale range. Through use of a small instrument entrance slit, X-ray photon correlation spectroscopy (XPCS) exploits the partial coherence of an X-ray synchrotron undulator beam to provide unprecedented sensitivity to the dynamics of microstructural change. In USAXS/XPCS studies, the dynamics of local structures in a scale range of 100 nm to 1000 nm can be related to an overall hierarchical microstructure extending from 1 nm to more than 1000 nm. Using a point-detection scintillator mode, the equilibrium dynamics at ambient temperature of small particles (which move more slowly than nanoparticles) in aqueous suspension have been quantified directly for the first time. Using a USAXS-XPCS scanning mode for non-equilibrium dynamics incipient processes within dental composites have been elucidated, prior to effects becoming detectable using any other technique. Use of the Advanced Photon Source, an Office of Science User Facility operated for the United States Department of Energy (U.S. DOE) Office of Science by Argonne National Laboratory, was supported by the U.S. DOE under Contract No. DE-AC02-06CH11357.

  2. 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).

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

    Science.gov (United States)

    Shang, Chao; Rice, James A.; Eberl, Dennis D.; Lin, Jar-Shyong

    2003-01-01

    It has been suggested that interstratified illite-smectite (I-S) minerals are composed of aggregates of fundamental particles. Many attempts have been made to measure the thickness of such fundamental particles, but each of the methods used suffers from its own limitations and uncertainties. Small-angle X-ray scattering (SAXS) can be used to measure the thickness of particles that scatter X-rays coherently. We used SAXS to study suspensions of Na-rectorite and other illites with varying proportions of smectite. The scattering intensity (I) was recorded as a function of the scattering vector, q = (4 /) sin(/2), where  is the X-ray wavelength and  is the scattering angle. The experimental data were treated with a direct Fourier transform to obtain the pair distance distribution function (PDDF) that was then used to determine the thickness of illite particles. The Guinier and Porod extrapolations were used to obtain the scattering intensity beyond the experimental q, and the effects of such extrapolations on the PDDF were examined. The thickness of independent rectorite particles (used as a reference mineral) is 18.3 Å. The SAXS results are compared with those obtained by X-ray diffraction peak broadening methods. It was found that the power-law exponent (α) obtained by fitting the data in the region of q = 0.1-0.6 nm-1 to the power law (I = I0q-α) is a linear function of illite particle thickness. Therefore, illite particle thickness could be predicted by the linear relationship as long as the thickness is within the limit where α <4.0.

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

    International Nuclear Information System (INIS)

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

    1979-01-01

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

  5. 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.

  6. 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

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

    Science.gov (United States)

    Herzog, Gerd; Benecke, Gunthard; Buffet, Adeline; Heidmann, Berit; Perlich, Jan; Risch, Johannes F H; Santoro, Gonzalo; Schwartzkopf, Matthias; Yu, Shun; Wurth, Wilfried; Roth, Stephan V

    2013-09-10

    We investigated the spray deposition and subsequent self-assembly during drying of a polystyrene nanoparticle dispersion with in situ grazing incidence small-angle X-ray scattering at high time resolution. During the fast deposition of the dispersion and the subsequent evaporation of the solvent, different transient stages of nanoparticle assembly can be identified. In the first stage, the solvent starts to evaporate without ordering of the nanoparticles. During the second stage, large-scale structures imposed by the breakup of the liquid film are observable. In this stage, the solvent evaporates further and nanoparticle ordering starts. In the late third drying stage, the nanoparticles self-assemble into the final layer structure.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-11-01

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

  10. 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)

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

    Science.gov (United States)

    Nepal, Prakash; Saldin, D. K.

    2018-05-01

    Time-resolved small-angle x-ray scattering/wide-angle x-ray scattering (SAXS/WAXS) is capable of recovering difference structures directly from difference SAXS/WAXS curves. It does so by means of the theory described here because the structural changes in pump-probe detection in a typical time-resolved experiment are generally small enough to be confined to a single residue or group in close proximity which is identified by a method akin to the difference Fourier method of time-resolved crystallography. If it is assumed, as is usual with time-resolved structures, that the moved atoms lie within the residue, the 100-fold reduction in the search space (assuming a typical protein has about 100 residues) allows the exaction of the structure by a simulated annealing algorithm with a huge reduction in computing time and leads to a greater resolution by varying the positions of atoms only within that residue. This reduction in the number of potential moved atoms allows us to identify the actual motions of the individual atoms. In the case of a crystal, time-resolved calculations are normally performed using the difference Fourier method, which is, of course, not directly applicable to SAXS/WAXS. The method developed in this paper may be thought of as a substitute for that method which allows SAXS/WAXS (and hence disordered molecules) to also be used for time-resolved structural work.

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

    Science.gov (United States)

    Dev, Arun Singh; Kumar, Dileep; Potdar, Satish; Pandit, Pallavi; Roth, Stephan V.; Gupta, Ajay

    2018-04-01

    The present work describes the design and performance of a vacuum compatible portable mini chamber for temperature dependent GISAXS and GIWAXS studies of thin films and multilayer structures. The water cooled body of the chamber allows sample annealing up to 900 K using ultra high vacuum compatible (UHV) pyrolytic boron nitride heater, thus making it possible to study the temperature dependent evolution of structure and morphology of two-dimensional nanostructured materials. Due to its light weight and small size, the chamber is portable and can be accommodated at synchrotron facilities worldwide. A systematic illustration of the versatility of the chamber has been demonstrated at beamline P03, PETRA-III, DESY, Hamburg, Germany. Temperature dependent grazing incidence small angle x-ray scattering (GISAXS) and grazing incidence wide angle x-ray scattering (GIWAXS) measurements were performed on oblique angle deposited Co/Ag multilayer structure, which jointly revealed that the surface diffusion in Co columns in Co/Ag multilayer enhances by increasing temperature from RT to ˜573 K. This results in a morphology change from columnar tilted structure to densely packed morphological isotropic multilayer.

  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. Small angle X-ray scattering study of calreticulin reveals conformational plasticity

    DEFF Research Database (Denmark)

    Toft, Katrine Nørgaard; Larsen, Nanna; Jørgensen, Flemming Steen

    2008-01-01

    . The data from the calreticulin monomer reveal the shape of calreticulin in solution: The previously structurally un-described C-terminal is seen as a globular domain, and the P-domain beta-hairpin extends from the N-domain in a spiral like conformation. In the calreticulin solution dimer, the N-, C-, and P......-domains are easily identified, and the P-domain is in an extended conformation connecting to the second calreticulin molecule. The SAXS solution data enables the construction of a medium-resolution model of calreticulin. In the light of the unresolved chaperone mechanism of calreticulin and calnexin, we discuss...

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

    Science.gov (United States)

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

    2011-03-01

    The C-terminal Src kinase (Csk) and Csk-homologous kinase (CHK) are endogenous inhibitors of the proto-oncogenic Src family of protein tyrosine kinases (SFKs). Phosphotyrosyl peptide binding to their Src-homology 2 (SH2) domains activates Csk and CHK, enhancing their ability to suppress SFK signalling; however, the detailed mechanistic basis of this activation event is unclear. The CHK SH2 was expressed in Escherichia coli and the purified protein was characterized as monomeric by synchrotron small-angle X-ray scattering in-line with size-exclusion chromatography. The CHK SH2 crystallized in 0.2 M sodium bromide, 0.1 M bis-Tris propane pH 6.5 and 20% polyethylene glycol 3350 and the best crystals diffracted to ∼1.6 Å resolution. The crystals belonged to space group P2, with unit-cell parameters a=25.8, b=34.6, c=63.2 Å, β=99.4°.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-01

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

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

    International Nuclear Information System (INIS)

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

    1992-09-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

    PEGylated liposomes composed of a benzamidine derivative (TRX), hydrogenated soybean phosphatidylcholine (HSPC), and N-(monomethoxy-polyethyleneglycolcarbamyl) distearoyl phosphatidylethanolamine (PEG-PE) were examined in terms of how the addition of TRX affects their structures with small angle x-ray scattering (SAXS) as well as transmission electron microscopy (TEM). TEM images showed the presence of unilamella vesicles for both with and without TRX, though a small amount of multilamella vesicles were observed in absence of TRX. We analyzed SAXS profiles at contained TRX composition combined with contrast variation technique by adding PEG solution and unilamella vesicle model could be reproduced. Subsequently, we analyzed SAXS profiles at no TRX composition. The mixture model of unilamella and multilamella vesicle was reconstructed and we estimated about 10 % multilamella vesicles from a fitting parameter.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-10-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1998-12-01

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-01-28

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

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

    International Nuclear Information System (INIS)

    Quiroz, Soledad; Sukuru, Sai Chetan K.; Hausinger, Robert P.; Kuhn, Leslie A.; Heller, William T

    2008-01-01

    Conformational changes of Klebsiella aerogenes urease apoprotein (UreABC) 3 induced upon binding of the UreD and UreF accessory proteins were examined by a combination of flexibility analysis, mutagenesis, and small-angle X-ray scattering (SAXS). ProFlex analysis of urease provided evidence that the major domain of UreB can move in a hinge-like motion to account for prior chemical cross-linking results. Rigidification of the UreB hinge region, accomplished through a G11P mutation, reduced the extent of urease activation, in part by decreasing the nickel content of the mutant enzyme, and by sequestering a portion of the urease apoprotein in a novel activation complex that includes all of the accessory proteins. SAXS analyses of urease, (UreABC-UreD) 3 , and (UreABC-UreDF) 3 confirm that UreD and UreF bind near UreB at the periphery of the (UreAC) 3 structure. This study supports an activation model in which a domain-shifted UreB conformation in (UreABC-UreDF) 3 allows CO 2 and nickel ions to gain access to the nascent active site

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    CERN Document Server

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

    2001-01-01

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

  7. 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.

  8. 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)

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

    Directory of Open Access Journals (Sweden)

    Lauren Boldon

    2015-02-01

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

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

    Science.gov (United States)

    Kameya, Yuki; Lee, Kyeong O.

    2013-10-01

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

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

    International Nuclear Information System (INIS)

    Kameya, Yuki; Lee, Kyeong O.

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-10-01

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

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

    International Nuclear Information System (INIS)

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

    1997-01-01

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

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

    Science.gov (United States)

    Toolan, Daniel T W; Adlington, Kevin; Isakova, Anna; Kalamiotis, Alexis; Mokarian-Tabari, Parvaneh; Dimitrakis, Georgios; Dodds, Christopher; Arnold, Thomas; Terrill, Nick J; Bras, Wim; Hermida Merino, Daniel; Topham, Paul D; Irvine, Derek J; Howse, Jonathan R

    2017-08-09

    Microwave annealing has emerged as an alternative to traditional thermal annealing approaches for optimising block copolymer self-assembly. A novel sample environment enabling small angle X-ray scattering to be performed in situ during microwave annealing is demonstrated, which has enabled, for the first time, the direct study of the effects of microwave annealing upon the self-assembly behavior of a model, commercial triblock copolymer system [polystyrene-block-poly(ethylene-co-butylene)-block-polystyrene]. Results show that the block copolymer is a poor microwave absorber, resulting in no change in the block copolymer morphology upon application of microwave energy. The block copolymer species may only indirectly interact with the microwave energy when a small molecule microwave-interactive species [diethylene glycol dibenzoate (DEGDB)] is incorporated directly into the polymer matrix. Then significant morphological development is observed at DEGDB loadings ≥6 wt%. Through spatial localisation of the microwave-interactive species, we demonstrate targeted annealing of specific regions of a multi-component system, opening routes for the development of "smart" manufacturing methodologies.

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

    Science.gov (United States)

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

    2010-07-14

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

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

    Science.gov (United States)

    Boldon, Lauren; Laliberte, Fallon; Liu, Li

    2015-01-01

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

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

    DEFF Research Database (Denmark)

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

    2011-01-01

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

  18. 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...

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

    DEFF Research Database (Denmark)

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

    2009-01-01

    A small-angle X-ray scattering (SAXS) set-up has recently been developed at beamline I711 at the MAX II storage ring in Lund (Sweden). An overview of the required modifications is presented here together with a number of application examples. The accessible q range in a SAXS experiment is 0.009-0...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-10-15

    UDP-galactopyranose mutase (UGM) is a flavoenzyme that catalyzes the conversion of UDP-galactopyranose to UDP-galactofuranose, which is a central reaction in galactofuranose biosynthesis. Galactofuranose has never been found in humans but is an essential building block of the cell wall and extracellular matrix of many bacteria, fungi, and protozoa. The importance of UGM for the viability of many pathogens and its absence in humans make UGM a potential drug target. Here we report the first crystal structures and small-angle x-ray scattering data for UGM from the fungus Aspergillus fumigatus, the causative agent of aspergillosis. The structures reveal that Aspergillus UGM has several extra secondary and tertiary structural elements that are not found in bacterial UGMs yet are important for substrate recognition and oligomerization. Small-angle x-ray scattering data show that Aspergillus UGM forms a tetramer in solution, which is unprecedented for UGMs. The binding of UDP or the substrate induces profound conformational changes in the enzyme. Two loops on opposite sides of the active site move toward each other by over 10 {angstrom} to cover the substrate and create a closed active site. The degree of substrate-induced conformational change exceeds that of bacterial UGMs and is a direct consequence of the unique quaternary structure of Aspergillus UGM. Galactopyranose binds at the re face of the FAD isoalloxazine with the anomeric carbon atom poised for nucleophilic attack by the FAD N5 atom. The structural data provide new insight into substrate recognition and the catalytic mechanism and thus will aid inhibitor design.

  1. Extensive small-angle X-ray scattering studies of blood coagulation factor VIIa reveal interdomain flexibility

    DEFF Research Database (Denmark)

    Mosbæk, Charlotte Rode; Nolan, David; Persson, Egon

    2010-01-01

    Blood coagulation factor VIIa (FVIIa) is used in the treatment of replacement therapy resistant hemophilia patients, and FVIIa is normally activated upon complex formation with tissue factor (TF), potentially in context with structural rearrangements. The solution behavior of uncomplexed FVIIa...... is important for understanding the mechanism of activation and for the stability and activity of the pharmaceutical product. However, crystal structures of FVIIa in complex with TF and of truncated free FVIIa reveal different overall conformations while previous small-angle scattering studies suggest FVIIa...... causing resistance to activation, thereby emphasizing the connection between the distribution of different conformations of FVII and the mechanism of activation....

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

    KAUST Repository

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

    2014-01-01

    The paper shows how a table top superbright microfocus laboratory X-ray source and an innovative restoring-data algorithm, used in combination, allow to analyze the super molecular structure of soft matter by means of Small Angle X-ray Scattering ex-situ experiments. The proposed theoretical approach is aimed to restore diffraction features from SAXS profiles collected from low scattering biomaterials or soft tissues, and therefore to deal with extremely noisy diffraction SAXS profiles/maps. As biological test cases we inspected: i) residues of exosomes' drops from healthy epithelial colon cell line and colorectal cancer cells; ii) collagen/human elastin artificial scaffolds developed for vascular tissue engineering applications; iii) apoferritin protein in solution. Our results show how this combination can provide morphological/structural nanoscale information to characterize new artificial biomaterials and/or to get insight into the transition between healthy and pathological tissues during the progression of a disease, or to morphologically characterize nanoscale proteins, based on SAXS data collected in a room-sized laboratory.

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

    KAUST Repository

    Sibillano, T.

    2014-11-10

    The paper shows how a table top superbright microfocus laboratory X-ray source and an innovative restoring-data algorithm, used in combination, allow to analyze the super molecular structure of soft matter by means of Small Angle X-ray Scattering ex-situ experiments. The proposed theoretical approach is aimed to restore diffraction features from SAXS profiles collected from low scattering biomaterials or soft tissues, and therefore to deal with extremely noisy diffraction SAXS profiles/maps. As biological test cases we inspected: i) residues of exosomes\\' drops from healthy epithelial colon cell line and colorectal cancer cells; ii) collagen/human elastin artificial scaffolds developed for vascular tissue engineering applications; iii) apoferritin protein in solution. Our results show how this combination can provide morphological/structural nanoscale information to characterize new artificial biomaterials and/or to get insight into the transition between healthy and pathological tissues during the progression of a disease, or to morphologically characterize nanoscale proteins, based on SAXS data collected in a room-sized laboratory.

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

    Science.gov (United States)

    Sibillano, T.; de Caro, L.; Altamura, D.; Siliqi, D.; Ramella, M.; Boccafoschi, F.; Ciasca, G.; Campi, G.; Tirinato, L.; di Fabrizio, E.; Giannini, C.

    2014-11-01

    The paper shows how a table top superbright microfocus laboratory X-ray source and an innovative restoring-data algorithm, used in combination, allow to analyze the super molecular structure of soft matter by means of Small Angle X-ray Scattering ex-situ experiments. The proposed theoretical approach is aimed to restore diffraction features from SAXS profiles collected from low scattering biomaterials or soft tissues, and therefore to deal with extremely noisy diffraction SAXS profiles/maps. As biological test cases we inspected: i) residues of exosomes' drops from healthy epithelial colon cell line and colorectal cancer cells; ii) collagen/human elastin artificial scaffolds developed for vascular tissue engineering applications; iii) apoferritin protein in solution. Our results show how this combination can provide morphological/structural nanoscale information to characterize new artificial biomaterials and/or to get insight into the transition between healthy and pathological tissues during the progression of a disease, or to morphologically characterize nanoscale proteins, based on SAXS data collected in a room-sized laboratory.

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

    Science.gov (United States)

    Grudinin, Sergei; Garkavenko, Maria; Kazennov, Andrei

    2017-05-01

    A new method called Pepsi-SAXS is presented that calculates small-angle X-ray scattering profiles from atomistic models. The method is based on the multipole expansion scheme and is significantly faster compared with other tested methods. In particular, using the Nyquist-Shannon-Kotelnikov sampling theorem, the multipole expansion order is adapted to the size of the model and the resolution of the experimental data. It is argued that by using the adaptive expansion order, this method has the same quadratic dependence on the number of atoms in the model as the Debye-based approach, but with a much smaller prefactor in the computational complexity. The method has been systematically validated on a large set of over 50 models collected from the BioIsis and SASBDB databases. Using a laptop, it was demonstrated that Pepsi-SAXS is about seven, 29 and 36 times faster compared with CRYSOL, FoXS and the three-dimensional Zernike method in SAStbx, respectively, when tested on data from the BioIsis database, and is about five, 21 and 25 times faster compared with CRYSOL, FoXS and SAStbx, respectively, when tested on data from SASBDB. On average, Pepsi-SAXS demonstrates comparable accuracy in terms of χ 2 to CRYSOL and FoXS when tested on BioIsis and SASBDB profiles. Together with a small allowed variation of adjustable parameters, this demonstrates the effectiveness of the method. Pepsi-SAXS is available at http://team.inria.fr/nano-d/software/pepsi-saxs.

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  7. Structure of human low-density lipoprotein subfractions, determined by X-ray small-angle scattering.

    Science.gov (United States)

    Baumstark, M W; Kreutz, W; Berg, A; Frey, I; Keul, J

    1990-01-19

    The structure of low-density lipoprotein (LDL) particles from three different density ranges (LDL-1: d = 1.006-1.031 g/ml; LDL-3: d = 1.034-1.037 g/ml; LDL-6: d = 1.044-1.063 g/ml) was determined by X-ray small-angle scattering. By using a theoretical particle model, which accounted for the polydispersity of the samples, we were able to obtain fits of the scattering intensity that were inside the noise interval of the measured intensity. The assumption of deviations from radial symmetry is not supported by our data. This implies a spread-out conformation of the apolipoprotein B (apoB) molecule, which appears to be localized in the outer surface shell. A globular structure is not consistent with our data. Furthermore, different models exist concerning the structure of the cholesterol ester core below the phase transition temperature. The electron density data suggest an arrangement in which the steroid moieties are localized at average radii of 3.2 and 6.4 nm. Model calculations show that packing problems can only be avoided if approximately half of the acyl chains of each shell are pointing towards the center of the particle, the other half towards the surface. This arrangement of the acyl chains has never been proposed before. The LDL particles of different density classes differ mainly with respect to the size of the core but also with respect to the width of the surface shells. Model calculations show that the size of different LDL particles can be accurately predicted from the compositional data.

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-02-15

    We demonstrate the use of a molybdenum-anode-based in-house small-angle X-ray scattering (SAXS) setup to study biological macromolecules in solution. Our system consists of a microfocus X-ray tube delivering a highly collimated flux of 2.5 × 10{sup 6} photons/s at a beam size of 1.2 × 1.2 mm{sup 2} at the collimation path exit and a maximum beam divergence of 0.16 mrad. The resulting observable scattering vectors q are in the range of 0.38 Å{sup −1} down to 0.009 Å{sup −1} in SAXS configuration and of 0.26 Å{sup −1} up to 5.7 Å{sup −1} in wide-angle X-ray scattering (WAXS) mode. To determine the capabilities of the instrument, we collected SAXS data on weakly scattering biological macromolecules including proteins and a nucleic acid sample with molecular weights varying from ∼12 to 69 kDa and concentrations of 1.5–24 mg/ml. The measured scattering data display a high signal-to-noise ratio up to q-values of ∼0.2 Å{sup −1} allowing for an accurate structural characterization of the samples. Moreover, the in-house source data are of sufficient quality to perform ab initio 3D structure reconstructions that are in excellent agreement with the available crystallographic structures. In addition, measurements for the detergent decyl-maltoside show that the setup can be used to determine the size, shape, and interactions (as characterized by the second virial coefficient) of detergent micelles. This demonstrates that the use of a Mo-anode based in-house source is sufficient to determine basic geometric parameters and 3D shapes of biomolecules and presents a viable alternative to valuable beam time at third generation synchrotron sources.

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

    International Nuclear Information System (INIS)

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

    1980-01-01

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

  11. Structure development during isothermal crystallisation of high-density polyethylene: Synchrotron small-angle X-ray scattering study

    International Nuclear Information System (INIS)

    Ślusarczyk, Czesław

    2013-01-01

    Isothermal melt crystallisation in high-density polyethylene (HDPE) was studied using the time-resolved SAXS method with synchrotron radiation over a wide range of crystallisation temperatures. The SAXS profile was analysed by an interface distribution function, g 1 (r), which is a superposition of three contributions associated with the size distributions of crystalline (L C ) and amorphous (L A ) layers and a distribution of long period (LP). The morphological parameters extracted from the g 1 (r) functions show that the lamellar thickness increases with time, obeying a logarithmic time dependence. The time evolution of L C observed for the sample crystallised at 122 °C leads to the conclusion that crystallisation proceeds according to the mechanism of thickening growth. For samples crystallised at lower temperatures (116 °C and 118 °C), the lamellar thickening mechanism has been observed. The rate of lamellar thickening in these cases is much lower than that at 122 °C. At 40 °C, thickening of the crystalline layer does not occur. The interface distribution functions were deconvoluted, and the relative standard deviation σ C /L C obtained in this way is an additional parameter that is varied during crystallisation and can be used for analysis of this process. Time-dependent changes in the σ C /L C at large supercooling (T C =40 °C) indicates that L C presents a broad distribution in which the relative standard deviation increases with time. At lower supercooling (T C =122 °C), L C shows a much sharper distribution. In this case, the relative standard deviation decreases with time. - Highlights: • Isothermal melt crystallisation of high-density polyethylene (HDPE) was studied by time-resolved synchrotron small-angle X-ray scattering (SAXS) over a wide-range of supercoolings. • The SAXS profile was analysed by an interface distribution, g 1 (r), function. • At large supercooling (40 °C) the thickening of the crystalline layer does not occur. At

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

    Czech Academy of Sciences Publication Activity Database

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    KAUST Repository

    Ogorzalek, Tadeusz L.

    2018-01-04

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

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

    KAUST Repository

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

    2018-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-07-01

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

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

    Science.gov (United States)

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

    2017-10-01

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

  19. Estimation of degree of polymerization of poly-acrylonitrile-grafted carbon nanotubes using Guinier plot of small angle x-ray scattering.

    Science.gov (United States)

    Cho, Hyunjung; Jin, Kyeong Sik; Lee, Jaegeun; Lee, Kun-Hong

    2018-07-06

    Small angle x-ray scattering (SAXS) was used to estimate the degree of polymerization of polymer-grafted carbon nanotubes (CNTs) synthesized using a 'grafting from' method. This analysis characterizes the grafted polymer chains without cleaving them from CNTs, and provides reliable data that can complement conventional methods such as thermogravimetric analysis or transmittance electron microscopy. Acrylonitrile was polymerized from the surface of the CNTs by using redox initiation to produce poly-acrylonitrile-grafted CNTs (PAN-CNTs). Polymerization time and the initiation rate were varied to control the degree of polymerization. Radius of gyration (R g ) of PAN-CNTs was determined using the Guinier plot obtained from SAXS solution analysis. The results showed consistent values according to the polymerization condition, up to a maximum R g  = 125.70 Å whereas that of pristine CNTs was 99.23 Å. The dispersibility of PAN-CNTs in N,N-dimethylformamide was tested using ultraviolet-visible-near infrared spectroscopy and was confirmed to increase as the degree of polymerization increased. This analysis will be helpful to estimate the degree of polymerization of any polymer-grafted CNTs synthesized using the 'grafting from' method and to fabricate polymer/CNT composite materials.

  20. Constrained Maximum Likelihood Estimation of Relative Abundances of Protein Conformation in a Heterogeneous Mixture from Small Angle X-Ray Scattering Intensity Measurements

    Science.gov (United States)

    Onuk, A. Emre; Akcakaya, Murat; Bardhan, Jaydeep P.; Erdogmus, Deniz; Brooks, Dana H.; Makowski, Lee

    2015-01-01

    In this paper, we describe a model for maximum likelihood estimation (MLE) of the relative abundances of different conformations of a protein in a heterogeneous mixture from small angle X-ray scattering (SAXS) intensities. To consider cases where the solution includes intermediate or unknown conformations, we develop a subset selection method based on k-means clustering and the Cramér-Rao bound on the mixture coefficient estimation error to find a sparse basis set that represents the space spanned by the measured SAXS intensities of the known conformations of a protein. Then, using the selected basis set and the assumptions on the model for the intensity measurements, we show that the MLE model can be expressed as a constrained convex optimization problem. Employing the adenylate kinase (ADK) protein and its known conformations as an example, and using Monte Carlo simulations, we demonstrate the performance of the proposed estimation scheme. Here, although we use 45 crystallographically determined experimental structures and we could generate many more using, for instance, molecular dynamics calculations, the clustering technique indicates that the data cannot support the determination of relative abundances for more than 5 conformations. The estimation of this maximum number of conformations is intrinsic to the methodology we have used here. PMID:26924916

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-03-01

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

  2. 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.

  3. 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

  4. Microstructure investigation on micropore formation in microporous silica materials prepared via a catalytic sol-gel process by small angle X-ray scattering.

    Science.gov (United States)

    Shimizu, Wataru; Hokka, Junsuke; Sato, Takaaki; Usami, Hisanao; Murakami, Yasushi

    2011-08-04

    The so-called sol-gel technique has been shown to be a template-free, efficient way to create functional porous silica materials having uniform micropores. This appears to be closely linked with a postulation that the formation of weakly branched polymer-like aggregates in a precursor solution is a key to the uniform micropore generation. However, how such a polymer-like structure can precisely be controlled, and further, how the generated low-fractal dimension solution structure is imprinted on the solid silica materials still remain elusive. Here we present fabrication of microporous silica from tetramethyl orthosilicate (TMOS) using a recently developed catalytic sol-gel process based on a nonionic hydroxyacetone (HA) catalyst. Small angle X-ray scattering (SAXS), nitrogen adsorption porosimetry, and transmission electron microscope (TEM) allowed us to observe the whole structural evolution, ranging from polymer-like aggregates in the precursor solution to agglomeration with heat treatment and microporous morphology of silica powders after drying and hydrolysis. Using the HA catalyst with short chain monohydric alcohols (methanol or ethanol) in the precursor solution, polymer-like aggregates having microscopic correlation length (or mesh-size) micropores with diameters 2 nm) in the solid product due to apertures between the particle-like aggregates. The data demonstrate that the extremely fine porous silica architecture comes essentially from a gaussian polymer-like nature of the silica aggregates in the precursor having the microscopic mesh-size and their successful imprint on the solid product. The result offers a general but significantly efficient route to creating precisely designed fine porous silica materials under mild condition that serve as low refractive index and efficient thermal insulation materials in their practical applications.

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

    International Nuclear Information System (INIS)

    Heller, William T; Tjioe, Elina

    2007-01-01

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

  6. 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.

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

    Science.gov (United States)

    Bras, Wim; Koizumi, Satoshi; Terrill, Nicholas J

    2014-11-01

    Small- and wide-angle X-ray scattering (SAXS, WAXS) are standard tools in materials research. The simultaneous measurement of SAXS and WAXS data in time-resolved studies has gained popularity due to the complementary information obtained. Furthermore, the combination of these data with non X-ray based techniques, via either simultaneous or independent measurements, has advanced understanding of the driving forces that lead to the structures and morphologies of materials, which in turn give rise to their properties. The simultaneous measurement of different data regimes and types, using either X-rays or neutrons, and the desire to control parameters that initiate and control structural changes have led to greater demands on sample environments. Examples of developments in technique combinations and sample environment design are discussed, together with a brief speculation about promising future developments.

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Hennig, Janosch; Wang, Iren; Sonntag, Miriam [Institute of Structural Biology, Helmholtz Zentrum Muenchen (Germany); Gabel, Frank [Extremophiles and Large Molecular Assemblies Group (ELMA), Institut de Biologie Structurale (IBS) CEA-CNRS-UJF (France); Sattler, Michael, E-mail: sattler@helmholtz-muenchen.de [Institute of Structural Biology, Helmholtz Zentrum Muenchen (Germany)

    2013-05-15

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

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

    DEFF Research Database (Denmark)

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

    2016-01-01

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

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

    Science.gov (United States)

    Cinar, Süleyman; Al-Ayoubi, Samy; Sternemann, Christian; Peters, Judith; Winter, Roland; Czeslik, Claus

    2018-01-31

    Calmodulin (CaM) is a Ca 2+ sensor and mediates Ca 2+ signaling through binding of numerous target ligands. The binding of ligands by Ca 2+ -saturated CaM (holo-CaM) is governed by attractive hydrophobic and electrostatic interactions that are weakened under high pressure in aqueous solutions. Moreover, the potential formation of void volumes upon ligand binding creates a further source of pressure sensitivity. Hence, high pressure is a suitable thermodynamic variable to probe protein-ligand interactions. In this study, we compare the binding of two different ligands to holo-CaM as a function of pressure by using X-ray and neutron scattering techniques. The two ligands are the farnesylated hypervariable region (HVR) of the K-Ras4B protein, which is a natural binding partner of holo-CaM, and the antagonist trifluoperazine (TFP), which is known to inhibit holo-CaM activity. From small-angle X-ray scattering experiments performed up to 3000 bar, we observe a pressure-induced partial unfolding of the free holo-CaM in the absence of ligands, where the two lobes of the dumbbell-shaped protein are slightly swelled. In contrast, upon binding TFP, holo-CaM forms a closed globular conformation, which is pressure stable at least up to 3000 bar. The HVR of K-Ras4B shows a different binding behavior, and the data suggest the dissociation of the holo-CaM/HVR complex under high pressure, probably due to a less dense protein contact of the HVR as compared to TFP. The elastic incoherent neutron scattering experiments corroborate these findings. Below 2000 bar, pressure induces enhanced atomic fluctuations in both holo-CaM/ligand complexes, but those of the holo-CaM/HVR complex seem to be larger. Thus, the inhibition of holo-CaM by TFP is supported by a low-volume ligand binding, albeit this is not associated with a rigidification of the complex structure on the sub-ns Å-scale.

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

    International Nuclear Information System (INIS)

    Stubblefield, F.W.

    1985-11-01

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

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

    International Nuclear Information System (INIS)

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

    1977-01-01

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

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

    International Nuclear Information System (INIS)

    Pons, Charles-Henri

    1980-01-01

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

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

    Science.gov (United States)

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

    2014-10-01

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

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

    Science.gov (United States)

    Schmiele, Martin; Schindler, Torben; Unruh, Tobias; Busch, Sebastian; Morhenn, Humphrey; Westermann, Martin; Steiniger, Frank; Radulescu, Aurel; Lindner, Peter; Schweins, Ralf; Boesecke, Peter

    2013-06-01

    Dispersions of crystalline nanoparticles with at least one sufficiently large unit cell dimension can give rise to Bragg reflections in the small-angle scattering range. If the nanocrystals possess only a small number of unit cells along these particular crystallographic directions, the corresponding Bragg reflections will be broadened. In a previous study of phospholipid stabilized dispersions of β-tripalmitin platelets [Unruh, J. Appl. Crystallogr.JACGAR0021-889810.1107/S0021889807044378 40, 1008 (2007)], the x-ray powder pattern simulation analysis (XPPSA) was developed. The XPPSA method facilitates the interpretation of the rather complicated small-angle x-ray scattering (SAXS) curves of such dispersions of nanocrystals. The XPPSA method yields the distribution function of the platelet thicknesses and facilitates a structural characterization of the phospholipid stabilizer layer at the solid-liquid interface between the nanocrystals and the dispersion medium from the shape of the broadened 001 Bragg reflection. In this contribution an improved and extended version of the XPPSA method is presented. The SAXS and small-angle neutron scattering patterns of dilute phospholipid stabilized tripalmitin dispersions can be reproduced on the basis of a consistent simulation model for the particles and their phospholipid stabilizer layer on an absolute scale. The results indicate a surprisingly flat arrangement of the phospholipid molecules in the stabilizer layer with a total thickness of only 12 Å. The stabilizer layer can be modeled by an inner shell for the fatty acid chains and an outer shell including the head groups and additional water. The experiments support a dense packing of the phospholipid molecules on the nanocrystal surfaces rather than isolated phospholipid domains.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    International Nuclear Information System (INIS)

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

    1981-01-01

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

  20. Wavelet-based feature extraction applied to small-angle x-ray scattering patterns from breast tissue: a tool for differentiating between tissue types

    International Nuclear Information System (INIS)

    Falzon, G; Pearson, S; Murison, R; Hall, C; Siu, K; Evans, A; Rogers, K; Lewis, R

    2006-01-01

    This paper reports on the application of wavelet decomposition to small-angle x-ray scattering (SAXS) patterns from human breast tissue produced by a synchrotron source. The pixel intensities of SAXS patterns of normal, benign and malignant tissue types were transformed into wavelet coefficients. Statistical analysis found significant differences between the wavelet coefficients describing the patterns produced by different tissue types. These differences were then correlated with position in the image and have been linked to the supra-molecular structural changes that occur in breast tissue in the presence of disease. Specifically, results indicate that there are significant differences between healthy and diseased tissues in the wavelet coefficients that describe the peaks produced by the axial d-spacing of collagen. These differences suggest that a useful classification tool could be based upon the spectral information within the axial peaks

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

    International Nuclear Information System (INIS)

    Ueki, Tatzuo; Inoko, Yoji; Izumi, Yoshinobu; Tagawa, Hiroyuki; Muroga, Yoshio

    1985-01-01

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

  2. Core–Shell Structure and Aggregation Number of Micelles Composed of Amphiphilic Block Copolymers and Amphiphilic Heterografted Polymer Brushes Determined by Small-Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Szymusiak, Magdalena; Kalkowski, Joseph; Luo, Hanying; Donovan, Alexander J.; Zhang, Pin; Liu, Chang; Shang, Weifeng; Irving, Thomas; Herrera-Alonso, Margarita; Liu, Ying (JHU); (IIT); (UIC)

    2017-08-31

    A large group of functional nanomaterials employed in biomedical applications, including targeted drug delivery, relies on amphiphilic polymers to encapsulate therapeutic payloads via self-assembly processes. Knowledge of the micelle structures will provide critical insights into design of polymeric drug delivery systems. Core–shell micelles composed of linear diblock copolymers poly(ethylene glycol)-b-poly(caprolactone) (PEG-b-PCL), poly(ethylene oxide)-b-poly(lactic acid) (PEG-b-PLA), as well as a heterografted brush consisting of a poly(glycidyl methacrylate) backbone with PEG and PLA branches (PGMA-g-PEG/PLA) were characterized by dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS) measurements to gain structural information regarding the particle morphology, core–shell size, and aggregation number. The structural information at this quasi-equilibrium state can also be used as a reference when studying the kinetics of polymer micellization.

  3. Core–Shell Structure and Aggregation Number of Micelles Composed of Amphiphilic Block Copolymers and Amphiphilic Heterografted Polymer Brushes Determined by Small-Angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Szymusiak, Magdalena [Department; Kalkowski, Joseph [Department; Luo, Hanying [Department; Donovan, Alexander J. [Department; Zhang, Pin [Department; Liu, Chang [Department; Shang, Weifeng [Department; Irving, Thomas [Department; Herrera-Alonso, Margarita [Department; Liu, Ying [Department; Department

    2017-08-16

    A large group of functional nanomaterials employed in biomedical applications, including targeted drug delivery, relies on amphiphilic polymers to encapsulate therapeutic payloads via self-assembly processes. Knowledge of the micelle structures will provide critical insights into design of polymeric drug delivery systems. Core–shell micelles composed of linear diblock copolymers poly(ethylene glycol)-b-poly(caprolactone) (PEG-b-PCL), poly(ethylene oxide)-b-poly(lactic acid) (PEG-b-PLA), as well as a heterografted brush consisting of a poly(glycidyl methacrylate) backbone with PEG and PLA branches (PGMA-g-PEG/PLA) were characterized by dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS) measurements to gain structural information regarding the particle morphology, core–shell size, and aggregation number. The structural information at this quasi-equilibrium state can also be used as a reference when studying the kinetics of polymer micellization.

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

    Energy Technology Data Exchange (ETDEWEB)

    Ueki, Tatzuo; Inoko, Yoji; Hiragi, Yuzuru; Kataoka, Mikio; Amemiya, Yoshiyuki; Izumi, Yoshinobu; Tagawa, Hiroyuki; Muroga, Yoshio

    1985-11-01

    A rapid mixing system of the stopped-flow type, used with small-angle X-ray scattering equipment using synchrotron radiation, is described. The process of aggregation of bovine serum albumin was traced with a time interval of 50s, initiated upon cleavage of its disulfide bonds by reduction with dithiothreitol. The results indicate that a 218-fold molar excess of dithiothreitol over the number of moles of disulfide bonds in bovine serum albumin is sufficient to initiate the reaction immediately after mixing, which reaches equilibrium in about 15 min. On the other hand, half this amount is not sufficient to initiate the reaction, so that the reaction is delayed by about 150s. Such a single-shot time-resolved experiment showed that experiments with a time interval of 100 ms are possible with repeated multi-shot runs. 26 refs.; 8 figs.

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

    DEFF Research Database (Denmark)

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

    2012-01-01

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

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

    DEFF Research Database (Denmark)

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

    2009-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Xueming [Beijing Univ. of Chemical Technology (China); Duan, Yonghao [Beijing Univ. of Chemical Technology (China); He, Lilin [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Singh, Seema [Sandia National Lab. (SNL-CA), Livermore, CA (United States); Joint BioEnergy Inst. (JBEI), Emeryville, CA (United States); Simmons, Blake [Joint BioEnergy Inst. (JBEI), Emeryville, CA (United States); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Cheng, Gang [Beijing Univ. of Chemical Technology (China); Joint BioEnergy Inst. (JBEI), Emeryville, CA (United States); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    2017-02-08

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

  8. Note: Comparison of grazing incidence small angle x-ray scattering of a titania sponge structure at the beamlines BW4 (DORIS III) and P03 (PETRA III)

    International Nuclear Information System (INIS)

    Rawolle, M.; Körstgens, V.; Ruderer, M. A.; Metwalli, E.; Guo, S.; Müller-Buschbaum, P.; Herzog, G.; Benecke, G.; Schwartzkopf, M.; Buffet, A.; Perlich, J.; Roth, S. V.

    2012-01-01

    Grazing incidence small angle x-ray scattering (GISAXS) is a powerful technique for morphology investigation of nanostructured thin films. GISAXS measurements at the newly installed P03 beamline at the storage ring PETRA III in Hamburg, Germany, are compared to the GISAXS data from the beamline BW4 at the storage ring DORIS III, which had been used extensively for GISAXS investigations in the past. As an example, a titania thin film sponge structure is investigated. Compared to BW4, at beamline P03 the resolution of larger structures is slightly improved and a higher incident flux leads to a factor of 750 in scattered intensity. Therefore, the acquisition time in GISAXS geometry is reduced significantly at beamline P03.

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

    International Nuclear Information System (INIS)

    Yin Chuanyuan; Gu Qingchao

    1997-01-01

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

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

    Science.gov (United States)

    Liebi, Marianne; Georgiadis, Marios; Kohlbrecher, Joachim; Holler, Mirko; Raabe, Jörg; Usov, Ivan; Menzel, Andreas; Schneider, Philipp; Bunk, Oliver; Guizar-Sicairos, Manuel

    2018-01-01

    Small-angle X-ray scattering tensor tomography, which allows reconstruction of the local three-dimensional reciprocal-space map within a three-dimensional sample as introduced by Liebi et al. [Nature (2015), 527, 349-352], is described in more detail with regard to the mathematical framework and the optimization algorithm. For the case of trabecular bone samples from vertebrae it is shown that the model of the three-dimensional reciprocal-space map using spherical harmonics can adequately describe the measured data. The method enables the determination of nanostructure orientation and degree of orientation as demonstrated previously in a single momentum transfer q range. This article presents a reconstruction of the complete reciprocal-space map for the case of bone over extended ranges of q. In addition, it is shown that uniform angular sampling and advanced regularization strategies help to reduce the amount of data required.

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

    Energy Technology Data Exchange (ETDEWEB)

    Viani, Alberto, E-mail: viani@itam.cas.cz [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Sotiriadis, Konstantinos [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic); Len, Adél [Wigner Research Centre for Physics HAS, Konkoly-Thege 29-33, 1121 Budapest (Hungary); Šašek, Petr; Ševčík, Radek [Institute of Theoretical and Applied Mechanics AS CR, Centre of Excellence Telč, Batelovská 485, CZ-58856 Telč (Czech Republic)

    2016-06-15

    Full characterization of fired-clay bricks is crucial for the improvement of process variables in manufacturing and, in case of old bricks, for restoration/replacement purposes. To this aim, five bricks produced in a plant in Czech Republic in the past have been investigated with a combination of analytical techniques in order to derive information on the firing process. An additional old brick from another brickyard was also used to study the influence of different raw materials on sample microstructure. The potential of X-ray diffraction with the Rietveld method and small angle neutron scattering technique has been exploited to describe the phase transformations taking place during firing and characterize the brick microstructure. Unit-cell parameter of spinel and amount of hematite are proposed as indicators of the maximum firing temperature, although for the latter, limited to bricks produced from the same raw material. The fractal quality of the surface area of pores obtained from small angle neutron scattering is also suggested as a method to distinguish between bricks produced from different raw clays. - Highlights: • Rietveld method helps in describing microstructure and physical properties of bricks. • XRPD derived cell parameter of spinel is proposed as an indicator of firing temperature. • SANS effectively describes brick micro and nanostructure, including closed porosity. • Fractal quality of pore surface is proposed as ‘fingerprint’ of brick manufacturing.

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

    International Nuclear Information System (INIS)

    Yamamoto, Katsuhiro; Sakurai, Shinichi

    2006-01-01

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

  13. 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.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  15. 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.

  16. A small angle X-ray scattering method to investigate the crack tip in metals. Final report of the Marie Curie individual fellowship project

    International Nuclear Information System (INIS)

    Ouytsel, K. van; Boehmert, J.; Mueller, G.

    2003-08-01

    Structural materials, such as ferritic and austenitic steels or aluminium alloys used in the nuclear and aircraft industry, are subjected to external operational loads in different environments. Adopting a damage tolerant design principle, understanding the growth of preexisting or newly formed cracks under these conditions is of prime relevance to prevent extensive crack propagation and failure of the component. Within this framework, the characterization of early stages of the damage processes, as nucleation, growth and coalescence of micro-voids and the evolution of the spatial dislocation distribution (dislocation patterning) is a particularly challenging aspect. It was the objective of the work performed to investigate the damage structure near a crack tip by means of small angle X-ray scattering (SAXS). Pre-cracked fracture mechanics standard specimens from different aluminium alloys and steels were loaded up to different amounts of crack growth. From the crack tip range samples of 100 to 200 μm thickness were prepared and a small region around the crack tip was scanned using a microfocused Synchrotron beam. The SAXS experiments were performed at different Synchrotron sources and equipments with different beam cross section, scan step width and X-ray energy. Additionally, the investigation was completed by other methods like X-ray diffraction, X-ray imaging diffraction technique (MAXIM), transmission electron microscopy, scanning electron microscopy, and positron annihilation spectroscopy. The SAXS intensity pattern shows location-related effects. Potential SAXS parameters to characterize the damage are the integral intensity, a fractal dimension parameter and a value determined from the ratio of the intensity vertical and horizontal to the direction of crack growth. Above all, the last parameter is suitable to depict the damage zone around the crack tip. It is robust and applicable even for a material which exhibits an anisotropic SAXS pattern in the

  17. Abstract ID: 176 Geant4 implementation of inter-atomic interference effect in small-angle coherent X-ray scattering for materials of medical interest.

    Science.gov (United States)

    Paternò, Gianfranco; Cardarelli, Paolo; Contillo, Adriano; Gambaccini, Mauro; Taibi, Angelo

    2018-01-01

    Advanced applications of digital mammography such as dual-energy and tomosynthesis require multiple exposures and thus deliver higher dose compared to standard mammograms. A straightforward manner to reduce patient dose without affecting image quality would be removal of the anti-scatter grid, provided that the involved reconstruction algorithms are able to take the scatter figure into account [1]. Monte Carlo simulations are very well suited for the calculation of X-ray scatter distribution and can be used to integrate such information within the reconstruction software. Geant4 is an open source C++ particle tracking code widely used in several physical fields, including medical physics [2,3]. However, the coherent scattering cross section used by the standard Geant4 code does not take into account the influence of molecular interference. According to the independent atomic scattering approximation (the so-called free-atom model), coherent radiation is indistinguishable from primary radiation because its angular distribution is peaked in the forward direction. Since interference effects occur between x-rays scattered by neighbouring atoms in matter, it was shown experimentally that the scatter distribution is affected by the molecular structure of the target, even in amorphous materials. The most important consequence is that the coherent scatter distribution is not peaked in the forward direction, and the position of the maximum is strongly material-dependent [4]. In this contribution, we present the implementation of a method to take into account inter-atomic interference in small-angle coherent scattering in Geant4, including a dedicated data set of suitable molecular form factor values for several materials of clinical interest. Furthermore, we present scatter images of simple geometric phantoms in which the Rayleigh contribution is rigorously evaluated. Copyright © 2017.

  18. Structural analysis of the yeast exosome Rrp6p–Rrp47p complex by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Dedic, Emil; Seweryn, Paulina; Jonstrup, Anette Thyssen; Flygaard, Rasmus Koch; Fedosova, Natalya U.; Hoffmann, Søren Vrønning; Boesen, Thomas; Brodersen, Ditlev Egeskov

    2014-01-01

    Highlights: • We show that S. cerevisiae Rrp6p and Rrp47p stabilise each other in vitro. • We determine molecular envelopes of the Rrp6p–Rrp47p complex by SAXS. • Rrp47p binds at the top of the Rrp6p exonuclease domain. • Rrp47p modulates the activity of Rrp6p on a variety of RNA substrates. • Rrp47p does not affect RNA affinity by Rrp6p. - Abstract: The RNase D-type 3′–5′ exonuclease Rrp6p from Saccharomyces cerevisiae is a nuclear-specific cofactor of the RNA exosome and associates in vivo with Rrp47p (Lrp1p). Here, we show using biochemistry and small-angle X-ray scattering (SAXS) that Rrp6p and Rrp47p associate into a stable, heterodimeric complex with an elongated shape consistent with binding of Rrp47p to the nuclease domain and opposite of the HRDC domain of Rrp6p. Rrp47p reduces the exonucleolytic activity of Rrp6p on both single-stranded and structured RNA substrates without significantly altering the affinity towards RNA or the ability of Rrp6p to degrade RNA secondary structure

  19. Unravelling the shape and structural assembly of the photosynthetic GAPDH-CP12-PRK complex from Arabidopsis thaliana by small-angle X-ray scattering analysis.

    Science.gov (United States)

    Del Giudice, Alessandra; Pavel, Nicolae Viorel; Galantini, Luciano; Falini, Giuseppe; Trost, Paolo; Fermani, Simona; Sparla, Francesca

    2015-12-01

    Oxygenic photosynthetic organisms produce sugars through the Calvin-Benson cycle, a metabolism that is tightly linked to the light reactions of photosynthesis and is regulated by different mechanisms, including the formation of protein complexes. Two enzymes of the cycle, glyceraldehyde-3-phosphate dehydrogenase (GAPDH) and phosphoribulokinase (PRK), form a supramolecular complex with the regulatory protein CP12 with the formula (GAPDH-CP122-PRK)2, in which both enzyme activities are transiently inhibited during the night. Small-angle X-ray scattering analysis performed on both the GAPDH-CP12-PRK complex and its components, GAPDH-CP12 and PRK, from Arabidopsis thaliana showed that (i) PRK has an elongated, bent and screwed shape, (ii) the oxidized N-terminal region of CP12 that is not embedded in the GAPDH-CP12 complex prefers a compact conformation and (iii) the interaction of PRK with the N-terminal region of CP12 favours the approach of two GAPDH tetramers. The interaction between the GAPDH tetramers may contribute to the overall stabilization of the GAPDH-CP12-PRK complex, the structure of which is presented here for the first time.

  20. Characterization of oxidized tannins: comparison of depolymerization methods, asymmetric flow field-flow fractionation and small-angle X-ray scattering.

    Science.gov (United States)

    Vernhet, Aude; Dubascoux, Stéphane; Cabane, Bernard; Fulcrand, Hélène; Dubreucq, Eric; Poncet-Legrand, Céline

    2011-09-01

    Condensed tannins are a major class of plant polyphenols. They play an important part in the colour and taste of foods and beverages. Due to their chemical reactivity, tannins are not stable once extracted from plants. A number of chemical reactions can take place, leading to structural changes of the native structures to give so-called derived tannins and pigments. This paper compares results obtained on native and oxidized tannins with different techniques: depolymerization followed by high-performance liquid chromatography analysis, small-angle X-ray scattering (SAXS) and asymmetric flow field-flow fractionation (AF4). Upon oxidation, new macromolecules were formed. Thioglycolysis experiments showed no evidence of molecular weight increase, but thioglycolysis yields drastically decreased. When oxidation was performed at high concentration (e.g., 10 g L(-1)), the weight average degree of polymerization determined from SAXS increased, whereas it remained stable when oxidation was done at low concentration (0.1 g L(-1)), indicating that the reaction was intramolecular, yet the conformations were different. Differences in terms of solubility were observed; ethanol being a better solvent than water. We also separated soluble and non-water-soluble species of a much oxidized fraction. Thioglycolysis showed no big differences between the two fractions, whereas SAXS and AF4 showed that insoluble macromolecules have a weight average molecular weight ten times higher than the soluble ones.

  1. Structural analysis of the yeast exosome Rrp6p–Rrp47p complex by small-angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Dedic, Emil; Seweryn, Paulina; Jonstrup, Anette Thyssen; Flygaard, Rasmus Koch [Centre for mRNP Biogenesis and Metabolism, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Department of Molecular Biology and Genetics, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Fedosova, Natalya U. [Department of Biomedicine, Ole Worms Allé 6, Aarhus University, DK-8000 Aarhus C (Denmark); Hoffmann, Søren Vrønning [Institute for Storage Ring Facilities (ISA), Department of Physics and Astronomy, Ny Munkegade 120, Aarhus University, DK-8000 Aarhus C (Denmark); Boesen, Thomas [Centre for Membrane Pumps in Cells and Disease – PUMPKIN, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Department of Molecular Biology and Genetics, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Brodersen, Ditlev Egeskov, E-mail: deb@mb.au.dk [Centre for mRNP Biogenesis and Metabolism, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark); Department of Molecular Biology and Genetics, Gustav Wieds Vej 10c, Aarhus University, DK-8000 Aarhus C (Denmark)

    2014-07-18

    Highlights: • We show that S. cerevisiae Rrp6p and Rrp47p stabilise each other in vitro. • We determine molecular envelopes of the Rrp6p–Rrp47p complex by SAXS. • Rrp47p binds at the top of the Rrp6p exonuclease domain. • Rrp47p modulates the activity of Rrp6p on a variety of RNA substrates. • Rrp47p does not affect RNA affinity by Rrp6p. - Abstract: The RNase D-type 3′–5′ exonuclease Rrp6p from Saccharomyces cerevisiae is a nuclear-specific cofactor of the RNA exosome and associates in vivo with Rrp47p (Lrp1p). Here, we show using biochemistry and small-angle X-ray scattering (SAXS) that Rrp6p and Rrp47p associate into a stable, heterodimeric complex with an elongated shape consistent with binding of Rrp47p to the nuclease domain and opposite of the HRDC domain of Rrp6p. Rrp47p reduces the exonucleolytic activity of Rrp6p on both single-stranded and structured RNA substrates without significantly altering the affinity towards RNA or the ability of Rrp6p to degrade RNA secondary structure.

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

    Science.gov (United States)

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

    2014-07-23

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

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  4. Structure of a mouse immunoglobulin G that lacks the entire C sub H 1 domain: Protein sequencing and small-angle X-ray scattering studies

    Energy Technology Data Exchange (ETDEWEB)

    Igarashi, Takako; Tanaka, Toshiyuki; Nakanishi, Mamoru; Arata, Yoji (Univ. of Tokyo (Japan)); Sato, Mamoru; Katsube, Yukiteru (Osaka Univ. (Japan)); Takio, Koji (Institute of Physical and Chemical Research, Saitama (Japan))

    1990-06-19

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

  5. In situ ultra-small-angle X-ray scattering study under uniaxial stretching of colloidal crystals prepared by silica nanoparticles bearing hydrogen-bonding polymer grafts

    Directory of Open Access Journals (Sweden)

    Ryohei Ishige

    2016-05-01

    Full Text Available A molded film of single-component polymer-grafted nanoparticles (SPNP, consisting of a spherical silica core and densely grafted polymer chains bearing hydrogen-bonding side groups capable of physical crosslinking, was investigated by in situ ultra-small-angle X-ray scattering (USAXS measurement during a uniaxial stretching process. Static USAXS revealed that the molded SPNP formed a highly oriented twinned face-centered cubic (f.c.c. lattice structure with the [11−1] plane aligned nearly parallel to the film surface in the initial state. Structural analysis of in situ USAXS using a model of uniaxial deformation induced by rearrangement of the nanoparticles revealed that the f.c.c. lattice was distorted in the stretching direction in proportion to the macroscopic strain until the strain reached 35%, and subsequently changed into other f.c.c. lattices with different orientations. The lattice distortion and structural transition behavior corresponded well to the elastic and plastic deformation regimes, respectively, observed in the stress–strain curve. The attractive interaction of the hydrogen bond is considered to form only at the top surface of the shell and then plays an effective role in cross-linking between nanoparticles. The rearrangement mechanism of the nanoparticles is well accounted for by a strong repulsive interaction between the densely grafted polymer shells of neighboring particles.

  6. Investigation of the collagen-mineral-relation in bone with special respect to bone diseases with collagen defects by small-angle X-ray scattering

    International Nuclear Information System (INIS)

    Schreiber, S. A.

    1996-06-01

    Small-angle X-ray scattering (SAXS) was used to study the structure of the collagen/mineral composite of bone in the nanometer range. The most important results were: - In horse radius, the angular distribution of mineral crystals as measured by SAXS agreed well with previous measurements of collagen orientation using circularly polarized light microscopy. This shows that the crystals are parallel to the collagen fibrils. - The effect of sodium fluoride, which stimulates bone formation, and bisphosphonates, which reduce bone resorption, were analyzed. A slight increase in the average thickness of the mineral crystals as well as changes in the structure of the mineral/collagen composite were found in the case of fluoride treated animals. No differences were found between alendronate treated animals and controls. The changes with NaF correlate with bone weakening found in an earlier study with the same animals. - In cortical bone from 9 patients with Osteogenesis Imperfecta (brittle bone disease) the mean thickness of the mineral crystals was found approximately constant around 2.4 nm, while in control bones it constantly increased with age up to about 3.5 nm. In addition, the parallel alignment of the mineral crystals was less in OI-bone than in normal controls. Hence, despite the great variability of this genetic collagen defect, smaller and less well aligned mineral crystals seem to characterize the collagen/mineral composite in OI-bone. (author)

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

    Directory of Open Access Journals (Sweden)

    Ludovic F. Dumée

    2016-09-01

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

  8. 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.

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

    Directory of Open Access Journals (Sweden)

    Hourston Douglas J.

    2001-01-01

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

  10. Location of cholesterol in liposomes by using small-angle X-ray scattering (SAXS) data and the generalized indirect Fourier transformation (GIFT) method.

    Science.gov (United States)

    Aburai, Kenichi; Ogura, Taku; Hyodo, Ryo; Sakai, Hideki; Abe, Masahiko; Glatter, Otto

    2013-01-01

    We investigated the location of cholesterol (Chol) in liposomes and its interaction with phospholipids using small-angle x-ray scattering (SAXS) data and applying the generalized indirect Fourier transformation (GIFT) method. The GIFT method has been applied to lamellar liquid crystal systems and it gives quantitative data on bilayer thickness, electron density profile, and membrane flexibility (Caillé parameter). When the GIFT method is applied to the SAXS data of dipalmitoylphosphatidylcholine (DPPC) alone (Chol [-]) or a DPPC/Chol = 7/3 mixed system (Chol [+], molar ratio), change in the bilayer thickness was insignificant in both systems. However, the electron density for the Chol (+) system was higher than that for the Chol (-) system at the location of hydrophilic groups of phospholipids, and whereas Caillé parameter value increased with temperature for the Chol (-) system, no significant change with temperature was observed in the Caillé parameter for the Chol (+) system. These results indicated that Chol is located in the vicinity of the hydrophilic group of the phospholipids and constricts the packing of the acyl chain of phospholipids in the bilayer.

  11. Comprehension of direct extraction of hydrophilic antioxidants using vegetable oils by polar paradox theory and small angle X-ray scattering analysis.

    Science.gov (United States)

    Li, Ying; Fabiano-Tixier, Anne Sylvie; Ruiz, Karine; Rossignol Castera, Anne; Bauduin, Pierre; Diat, Olivier; Chemat, Farid

    2015-04-15

    Since the polar paradox theory rationalised the fact that polar antioxidants are more effective in nonpolar media, extractions of phenolic compounds in vegetable oils were inspired and achieved in this study for obtaining oils enriched in phenolic compounds. Moreover, the influence of surfactants on the extractability of phenolic compounds was experimentally studied first, followed by the small angle X-ray scattering analysis for the oil structural observation before and after extraction so as to better understand the dissolving mechanism underpinning the extraction. The results showed a significant difference on the extraction yield of phenolic compounds among oils, which was mainly dependent on their composition instead of the unsaturation of fatty acids. Appropriate surfactant additions could significantly improve extraction yield for refined sunflower oils, which 1% w/w addition of glyceryl oleate was determined as the optimal. Besides, 5% w/w addition of lecithin performed the best in oil enrichments compared with mono- and di-glycerides. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

    DEFF Research Database (Denmark)

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

    2009-01-01

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

  13. Small angle neutron scattering (SANS) study of gastric mucin solutions

    Science.gov (United States)

    Hong, Z.; Bansil, R.; Waigh, T.; Turner, B.; Bhaskar, K. R.; Afdhal, N.; Lal, J.

    2002-03-01

    We report the first results from a SANS study of purified porcine gastric mucin solutions in D2O. The ability of this glycoprotein to protect the stomach epithelium from acid damage, may be due to a pH dependent conformational transition which leads to gelation at low pH Cao et. al. (Biophysical. J. 76, 1250, 1999). SANS measurements were made over the concentration range of 1 -15 mg/ml at pH 7, 4 and 2. The data indicate that at pH 7 the excluded volume exponent is 1.7, characteristic of swollen chains whereas at pH 2 this exponent increases to 2, indicating theta or poor solvent conditions, consistent with the hydrophobic interactions increasing at lower pH. From a Guinier analysis of the 1mg/ml data at low q's (0.003- 0.007 Å-1) we estimate the cross section radius of the effective cylinder to be 23nm and its length as 96nm in an unbuffered sample, i.e. close to pH 7. In the intermediate q-range (0.01 -0.1Å-1) at pH 7 a fit to the Debye chain gives radius of gyration Rg of 16nm. Mucin is best modelled as an elongated micelle with a cylindrical or worm-like chain to represent the protein core and the sugar chains forming the corona. Results of such calculations will be presented.

  14. Segment-segment interactions of poly(N-isopropylacrylamide) in aqueous methanol solutions by using small-angle scattering

    CERN Document Server

    Shimizu, S; Furusaka, M

    2002-01-01

    Small-angle neutron and X-ray scattering from semidilute solutions of poly(N-isopropylacrylamide) in D sub 2 O, methanol and methanol-water mixtures has been measured in the poor solvent regime. The binary and the ternary cluster integrals of polymer segments were determined from the concentration dependence of the correlation length at several temperatures just below the lower critical solution temperature. Then, contributions of segment-segment interactions to the entropy and the enthalpy have been calculated from the temperature dependence of interaction parameters and it has been found that both values are positive in the D sub 2 O and the methanol-water systems at a small content of methanol, while both values are negative in the other system. (orig.)

  15. Segment-segment interactions of poly(N-isopropylacrylamide) in aqueous methanol solutions by using small-angle scattering

    International Nuclear Information System (INIS)

    Shimizu, S.; Kurita, K.; Furusaka, M.

    2002-01-01

    Small-angle neutron and X-ray scattering from semidilute solutions of poly(N-isopropylacrylamide) in D 2 O, methanol and methanol-water mixtures has been measured in the poor solvent regime. The binary and the ternary cluster integrals of polymer segments were determined from the concentration dependence of the correlation length at several temperatures just below the lower critical solution temperature. Then, contributions of segment-segment interactions to the entropy and the enthalpy have been calculated from the temperature dependence of interaction parameters and it has been found that both values are positive in the D 2 O and the methanol-water systems at a small content of methanol, while both values are negative in the other system. (orig.)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-05-02

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

  17. Structure and optical function of amorphous photonic nanostructures from avian feather barbs: a comparative small angle X-ray scattering (SAXS) analysis of 230 bird species.

    Science.gov (United States)

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

    2012-10-07

    Non-iridescent structural colours of feathers are a diverse and an important part of the phenotype of many birds. These colours are generally produced by three-dimensional, amorphous (or quasi-ordered) spongy β-keratin and air nanostructures found in the medullary cells of feather barbs. Two main classes of three-dimensional barb nanostructures are known, characterized by a tortuous network of air channels or a close packing of spheroidal air cavities. Using synchrotron small angle X-ray scattering (SAXS) and optical spectrophotometry, we characterized the nanostructure and optical function of 297 distinctly coloured feathers from 230 species belonging to 163 genera in 51 avian families. The SAXS data provided quantitative diagnoses of the channel- and sphere-type nanostructures, and confirmed the presence of a predominant, isotropic length scale of variation in refractive index that produces strong reinforcement of a narrow band of scattered wavelengths. The SAXS structural data identified a new class of rudimentary or weakly nanostructured feathers responsible for slate-grey, and blue-grey structural colours. SAXS structural data provided good predictions of the single-scattering peak of the optical reflectance of the feathers. The SAXS structural measurements of channel- and sphere-type nanostructures are also similar to experimental scattering data from synthetic soft matter systems that self-assemble by phase separation. These results further support the hypothesis that colour-producing protein and air nanostructures in feather barbs are probably self-assembled by arrested phase separation of polymerizing β-keratin from the cytoplasm of medullary cells. Such avian amorphous photonic nanostructures with isotropic optical properties may provide biomimetic inspiration for photonic technology.

  18. 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.

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

    KAUST Repository

    Yu, Hsiu-Yu

    2014-09-15

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

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

    International Nuclear Information System (INIS)

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

    1988-01-01

    Whole casein occurs in milk as a spherical colloidal complex of protein and salts called the casein micelle, with approximate average radii of 650 A as determined by electron microscopy. Removal of Ca2+ is thought to result in dissociation into smaller noncolloidal protein complexes called submicelles. Hydrodynamic and light scattering studies on whole casein submicelles suggest that they are predominantly spherical particles with a hydrophobic core. To investigate whether the integrity of a hydrophobically stabilized submicellar structure is preserved in the electrostatically stabilized colloidal micellar structure, small-angle X-ray scattering (SAXS) experiments were undertaken on whole casein from bovine milk under submicellar and micellar conditions. All SAXS results showed multiple Gaussian character and could be analyzed best by nonlinear regression in place of the customary Guinier plot. Analysis of the SAXS data for submicellar casein showed two Gaussian components which could be interpreted in terms of a particle with two concentric regions of different electron density, designated as a compact core and a loose shell, respectively. The submicelle was found to have an average molecular weight of 285,000 +/- 14,600 and a mass fraction of higher electron density core, k, of 0.212 +/- 0.028. The radius of gyration of the core, RC, was 37.98 +/- 0.01 A with an electron density difference, delta rho C, of 0.0148 +/- 0.0014 e-/A3, while the loose region had values of RL = 88.2 +/- 0.8 A with delta rho L = 0.0091 +/- 0.0003 e-/A3. Calculated distance distribution functions and normalized scattering curves also were consistent with an overall spherical particle with a concentric spherical inner core of higher electron density. (Abstract Truncated)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-02-06

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

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

    Science.gov (United States)

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

    2014-12-07

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

  3. A Solution to Hammer's X-ray Reconstruction Problem

    DEFF Research Database (Denmark)

    Gardner, Richard J.; Kiderlen, Markus

    2007-01-01

    We propose algorithms for reconstructing a planar convex body K from possibly noisy measurements of either its parallel X-rays taken in a fixed finite set of directions or its point X-rays taken at a fixed finite set of points, in known situations that guarantee a unique solution when the data is...... to K in the Hausdorff metric as k tends to infinity. This solves, for the first time in the strongest sense, Hammer’s X-ray problem published in 1963....

  4. Evaluation of solution stability for two-component polydisperse systems by small-angle scattering

    Science.gov (United States)

    Kryukova, A. E.; Konarev, P. V.; Volkov, V. V.

    2017-12-01

    The article is devoted to the modelling of small-angle scattering data using the program MIXTURE designed for the study of polydisperse multicomponent mixtures. In this work we present the results of solution stability studies for theoretical small-angle scattering data sets from two-component models. It was demonstrated that the addition of the noise to the data influences the stability range of the restored structural parameters. The recommendations for the optimal minimization schemes that permit to restore the volume size distributions for polydisperse systems are suggested.

  5. Edible oil structures at low and intermediate concentrations. II. Ultra-small angle X-ray scattering of in situ tristearin solids in triolein

    Science.gov (United States)

    Peyronel, Fernanda; Ilavsky, Jan; Mazzanti, Gianfranco; Marangoni, Alejandro G.; Pink, David A.

    2013-12-01

    Ultra-small angle X-ray scattering has been used for the first time to elucidate, in situ, the aggregation structure of a model edible oil system. The three-dimensional nano- to micro-structure of tristearin solid particles in triolein solvent was investigated using 5, 10, 15, and 20% solids. Three different sample preparation procedures were investigated: two slow cooling rates of 0.5°/min, case 1 (22 days of storage at room temperature) and case 2 (no storage), and one fast cooling of 30°/min, case 3 (no storage). The length scale investigated, by using the Bonse-Hart camera at beamline ID-15D at the Advanced Photon Source, Argonne National Laboratory, covered the range from 300 Å to 10 μm. The unified fit and the Guinier-Porod models in the Irena software were used to fit the data. The former was used to fit 3 structural levels. Level 1 structures showed that the primary scatterers were essentially 2-dimensional objects for the three cases. The scatterers possessed lateral dimensions between 1000 and 4300 Å. This is consistent with the sizes of crystalline nanoplatelets present which were observed using cryo-TEM. Level 2 structures were aggregates possessing radii of gyration, Rg2 between 1800 Å and 12000 Å and fractal dimensions of either D2=1 for case 3 or 1.8≤D2≤2.1 for case 1 and case 2. D2 = 1 is consistent with unaggregated 1-dimensional objects. 1.8 ≤ D2 ≤ 2.1 is consistent with these 1-dimensional objects (below) forming structures characteristic of diffusion or reaction limited cluster-cluster aggregation. Level 3 structures showed that the spatial distribution of the level 2 structures was uniform, on the average, for case 1, with fractal dimension D3≈3 while for case 2 and case 3 the fractal dimension was D3≈2.2, which suggested that the large-scale distribution had not come to equilibrium. The Guinier-Porod model showed that the structures giving rise to the aggregates with a fractal dimension given by D2 in the unified fit level 2

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

    Science.gov (United States)

    Akinlalu, Ademola V.

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

  7. 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.

  8. An X-ray absorption spectroelectrochemical cell for radioactive solutions

    International Nuclear Information System (INIS)

    Rettig, D.; Herrmann, S.; Mitschke, F.; Vonau, W.; Brendler, V.; Geipel, G.; Reich, T.; Bernhard, G.

    2002-01-01

    A spectroelectrochemical cell was designed and constructed for measurement of X-ray absorption spectra under electrochemical control of the redox potential of actinide-containing solutions. A first inactive test demonstrated the feasibility of an Ag anode as a non-gassing auxiliary electrode in chloride solutions. (orig.)

  9. Synchrotron X-ray induced solution precipitation of nanoparticles

    CERN Document Server

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

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, D.

    2007-07-01

    Homogeneous nucleation rates of the n-alcohols and the n-alkanes have been determined by combining information from two sets of supersonic Laval nozzle expansion experiments under identical conditions. The nucleation rates J=N/{delta}t{sub Jmax} for the n-alcohols are in the range of 1.10{sup 17}Small Angle X-ray Scattering experiments are conducted to determine the particle number density for both substance classes. Particle number densities in the range of 1.10{sup 12}

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

    International Nuclear Information System (INIS)

    Ghosh, D.

    2007-01-01

    Homogeneous nucleation rates of the n-alcohols and the n-alkanes have been determined by combining information from two sets of supersonic Laval nozzle expansion experiments under identical conditions. The nucleation rates J=N/Δt Jmax for the n-alcohols are in the range of 1.10 17 -3 s -1 17 for the temperatures 207≤T/K≤249, the nucleation rates for the n-alkanes lie in the range of 5.10 15 -3 s -1 18 for the temperatures 143 ≤T/K≤215. For the first time it is shown that the nucleation rate is not only a function of the supersaturation and temperature but clearly also sensitive to the expansion rate during supersonic nozzle expansion. A good agreement between the experimental results and those available in literature is found by applying Hale's scaling formalism [Hale, B., Phys. Rev. A 33, 4256 (1986); Hale, B., Metall. Trans. A 23, 1863 (1992)]. The scaling parameters from this work are also in good agreement with those shown by Rusyniak et al. [Rusyniak, M., M. S. El-Shall, J. Phys. Chem. B 105, 11873 (2001)] and Brus et al. [Brus, D., V. Zdimal F. Stratmann, J. Chem Phys. 124, 164306 (2006)]. In the first experiment static pressure measurements were conducted for the n-alkanes to determine the condensible partial pressure, temperature, supersaturation, characteristic time, and the expansion rate corresponding to the maximum nucleation rate. Characteristic times in the range of 13≤Δt Jmax /μs≤34 were found. In the second set of experiments, the first flow rate resolved Small Angle X-ray Scattering experiments are conducted to determine the particle number density for both substance classes. Particle number densities in the range of 1.10 12 -3 12 and 1.10 11 -3 12 for the n-alcohols and n-alkanes are found, respectively. Additionally, by analyzing the radially averaged scattering spectrum, information on the mean radius and the width of the size distribution of the aerosols is obtained. Mean radii for the n-alcohols in the range of 4< left angle r

  12. Edible oil structures at low and intermediate concentrations. II. Ultra-small angle X-ray scattering of in situ tristearin solids in triolein

    Energy Technology Data Exchange (ETDEWEB)

    Peyronel, Fernanda; Marangoni, Alejandro G. [Food Science Department, University of Guelph, Guelph, Ontario N1G 2W1 (Canada); Ilavsky, Jan [Advanced Photon Source, Argonne National Laboratory, 9700S Cass Ave., Bldg. 434D, Argonne, Illinois 60439 (United States); Mazzanti, Gianfranco [Department of Process Engineering and Applied Science, Dalhousie University, Halifax, Nova Scotia B3H 4R2 (Canada); Pink, David A. [Food Science Department, University of Guelph, Guelph, Ontario N1G 2W1 (Canada); Physics Department, St. Francis Xavier University, Antigonish, Nova Scotia B2G 2W5 (Canada)

    2013-12-21

    Ultra-small angle X-ray scattering has been used for the first time to elucidate, in situ, the aggregation structure of a model edible oil system. The three-dimensional nano- to micro-structure of tristearin solid particles in triolein solvent was investigated using 5, 10, 15, and 20% solids. Three different sample preparation procedures were investigated: two slow cooling rates of 0.5°/min, case 1 (22 days of storage at room temperature) and case 2 (no storage), and one fast cooling of 30°/min, case 3 (no storage). The length scale investigated, by using the Bonse-Hart camera at beamline ID-15D at the Advanced Photon Source, Argonne National Laboratory, covered the range from 300 Å to 10 μm. The unified fit and the Guinier-Porod models in the Irena software were used to fit the data. The former was used to fit 3 structural levels. Level 1 structures showed that the primary scatterers were essentially 2-dimensional objects for the three cases. The scatterers possessed lateral dimensions between 1000 and 4300 Å. This is consistent with the sizes of crystalline nanoplatelets present which were observed using cryo-TEM. Level 2 structures were aggregates possessing radii of gyration, R{sub g2} between 1800 Å and 12000 Å and fractal dimensions of either D{sub 2}=1 for case 3 or 1.8≤D{sub 2}≤2.1 for case 1 and case 2. D{sub 2} = 1 is consistent with unaggregated 1-dimensional objects. 1.8 ≤ D{sub 2} ≤ 2.1 is consistent with these 1-dimensional objects (below) forming structures characteristic of diffusion or reaction limited cluster-cluster aggregation. Level 3 structures showed that the spatial distribution of the level 2 structures was uniform, on the average, for case 1, with fractal dimension D{sub 3}≈3 while for case 2 and case 3 the fractal dimension was D{sub 3}≈2.2, which suggested that the large-scale distribution had not come to equilibrium. The Guinier-Porod model showed that the structures giving rise to the aggregates

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

    CSIR Research Space (South Africa)

    Bandyopadhyay, J

    2011-05-01

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

  14. Structure of polyacrylic acid and polymethacrylic acid solutions : a small angle neutron scattering study

    OpenAIRE

    Moussaid , A.; Schosseler , F.; Munch , J.; Candau , S.

    1993-01-01

    The intensity scattered from polyacrylic acid and polymethacrylic acid solutions has been measured by small angle neutron scattering experiemnts. The influence of polymer concentration, ionization degree, temperature and salt content has been investigated. Results are in qualitative agreement with a model which predicts the existence of microphases in the unstable region of the phase diagram. Quantitative comparison with the theory is performed by fitting the theoretical structure factor to t...

  15. Structure of fullerene aggregates in pyridine/water solutions by small-angle neutron scattering

    International Nuclear Information System (INIS)

    Aksenov, V.L.; Belushkin, A.V.; Avdeev, M.V.; Rosta, L.; Mihailovic, D.; Mrzel, A.; Serdyuk, I.N.; Timchenko, A.A.

    2001-01-01

    Results of small-angle neutron scattering experiments on fullerenes (C 60 ) in pyridine/water solutions are reported. They confirm conclusions of the previous studies, in particular, dynamic light scattering experiments. Aggregates with characteristic radius of about 20 nm are formed in the solutions. The contrast variation using different combinations of protonated/deuterated components (water and pyridine) of the solutions points to the small pyridine content inside the aggregates. This fact testifies that the aggregates consist of a massive fullerene core covered by a thin pyridine shell

  16. 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...

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

    DEFF Research Database (Denmark)

    Khan, Jamal; Hawley, Adrian; Rades, Thomas

    2016-01-01

    In situ lipolysis and synchrotron small-angle X-ray scattering (SAXS) were used to directly detect and elucidate the solid-state form of precipitated fenofibrate from the digestion of a model lipid-based formulation (LBF). This method was developed in light of recent findings that indicate variab...... on drugs, and experimental conditions, which are anticipated to produce altered solid-state forms upon the precipitation of drug (i.e., polymorphs, amorphous forms, and salts). © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci....

  18. Structure of polyacrylic acid and polymethacrylic acid solutions: a small angle neutron scattering study

    Energy Technology Data Exchange (ETDEWEB)

    Moussaid, A. (Lab. d' Ultrasons et de Dynamique des Fluides Complexes, Univ. Louis Pasteur, 67 - Strasbourg (France)); Schosseler, F. (Lab. d' Ultrasons et de Dynamique des Fluides Complexes, Univ. Louis Pasteur, 67 - Strasbourg (France)); Munch, J.P. (Lab. d' Ultrasons et de Dynamique des Fluides Complexes, Univ. Louis Pasteur, 67 - Strasbourg (France)); Candau, S.J. (Lab. d' Ultrasons et de Dynamique des Fluides Complexes, Univ. Louis Pasteur, 67 - Strasbourg (France))

    1993-04-01

    The intensity scattered from polyacrylic acid and polymethacrylic acid solutions has been measured by small angle neutron scattering experiments. The influence of polymer concentration, ionization degree, temperature and salt content has been investigated. Results are in qualitative agreement with a model which predicts the existence of microphases in the unstable region of the phase diagram. Quantitative comparison with the theory is performed by fitting the theoretical structure factor to the experimental data. For a narrow range of ionization degrees nearly quantitative agreement with the theory is found for the polyacrylic acid system. (orig.).

  19. Structure of polyacrylic acid and polymethacrylic acid solutions : a small angle neutron scattering study

    Science.gov (United States)

    Moussaid, A.; Schosseler, F.; Munch, J. P.; Candau, S. J.

    1993-04-01

    The intensity scattered from polyacrylic acid and polymethacrylic acid solutions has been measured by small angle neutron scattering experiemnts. The influence of polymer concentration, ionization degree, temperature and salt content has been investigated. Results are in qualitative agreement with a model which predicts the existence of microphases in the unstable region of the phase diagram. Quantitative comparison with the theory is performed by fitting the theoretical structure factor to the experimental data. For a narrow range of ionizaiton degrees nearly quantitative agreement with the theory is found for the polyacrylic acide system.

  20. ATSAS 2.8: a comprehensive data analysis suite for small-angle scattering from macromolecular solutions.

    Science.gov (United States)

    Franke, D; Petoukhov, M V; Konarev, P V; Panjkovich, A; Tuukkanen, A; Mertens, H D T; Kikhney, A G; Hajizadeh, N R; Franklin, J M; Jeffries, C M; Svergun, D I

    2017-08-01

    ATSAS is a comprehensive software suite for the analysis of small-angle scattering data from dilute solutions of biological macromolecules or nanoparticles. It contains applications for primary data processing and assessment, ab initio bead modelling, and model validation, as well as methods for the analysis of flexibility and mixtures. In addition, approaches are supported that utilize information from X-ray crystallography, nuclear magnetic resonance spectroscopy or atomistic homology modelling to construct hybrid models based on the scattering data. This article summarizes the progress made during the 2.5-2.8 ATSAS release series and highlights the latest developments. These include AMBIMETER , an assessment of the reconstruction ambiguity of experimental data; DATCLASS , a multiclass shape classification based on experimental data; SASRES , for estimating the resolution of ab initio model reconstructions; CHROMIXS , a convenient interface to analyse in-line size exclusion chromatography data; SHANUM , to evaluate the useful angular range in measured data; SREFLEX , to refine available high-resolution models using normal mode analysis; SUPALM for a rapid superposition of low- and high-resolution models; and SASPy , the ATSAS plugin for interactive modelling in PyMOL . All these features and other improvements are included in the ATSAS release 2.8, freely available for academic users from https://www.embl-hamburg.de/biosaxs/software.html.

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-04-01

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

  3. Neutron and X-ray small angle scattering (S.A.S.) study of the amorphous alloy Tbsub(.25)Cusub(.75)

    International Nuclear Information System (INIS)

    Boucher, B.

    1980-07-01

    The magnetic properties of amorphous alloys REsub(x) Msub(x-1) (R.E.=heavy rare earths, M=Cu, Ag, Au) have been widely studied. They are of the speromagnetic type for x>=0.33 and are mictomagnetic for x -12 cm). Also the atomic volume of Terbium (approximately 33 A 3 ) is almost three times that of Copper (11.8 A 3 ) and Cu is less absorbant than Ag or Au. Tb alloys exhibit high magnetic ordering temperatures and important moments in contrast to the majority of other alloys of the same family. One inconvenience with Terbium, however, is the large (X-ray) fluorescence (lambda Cu). In order to confirm some interpretations of S.A.S., we were obliged to determine some physical parameters such as the density and porosity and to examine the sample with microscope. These results are also given here

  4. 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

    hydrated binary membranes composed of dimyristoylphosphatidylcholine (DMPC) and N-palmitoyl-ceramide (C16:0-ceramide, up to a mole fraction X-cer = 0.35) were resolved in further detail by high-sensitivity differential scanning calorimetry (DSC) and x-ray diffraction. Both methods reveal very strong...... 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...... no longer be resolved. The main transition enthalpy Delta H remains practically unaltered while its width increases significantly, and the upper phase boundary temperature of the mixture shifts to similar to 63 degrees C at X-cer = 0.30. Upon cooling, profound phase separation is evident, and for all...

  5. Time Resolved X-Ray Scattering of molecules in Solution

    DEFF Research Database (Denmark)

    Brandt van Driel, Tim

    The dissertation describes the use of Time-Resolved X-ray Diffuse Scattering (TR-XDS) to study photo-induced structural changes in molecules in solution. The application of the technique is exemplified with experiments on two bimetallic molecules. The main focus is on the data-flow and process......)42+ obtained at European Synchrotron Radiation Facility (ESRF) are presented to exemplify TR-XDS at synchrotrons. Similarly, measurements on Ir2(dimen)42+ are used to show the XFEL data-flow and how it deviates from the prior. A method to identify and account for systematic fluctuations...

  6. X-Ray Characterization of Non-Equilibrium Solid Solutions

    Energy Technology Data Exchange (ETDEWEB)

    Brown, A; Rosdahl, Oe

    1975-07-01

    The Rudman approach to composition line broadening in X-ray diffraction patterns, originally designed for the study of diffusion in alloys, is seen to provide a basis for characterizing inhomogeneous solid solutions. Limitations, imposed on this treatment when the cell dimensions of the primary components differ by less than 0.1 A, are attributable to experimental effects such as instrument broadening. These limitations can be overcome by a rigorous numerical treatment of the measured data. Thus, separate elimination of the Kalpha{sub 2} radiation component followed by iterative deconvolution are advocated for the recovery of the intrinsic broadening. This course of action is made possible chiefly through the availability of large, fast memory computers and primary data recorded in the form of a step scan on punched paper tape. The characteristics of inhomogeneous solid solutions made available by the above treatment are the identity of closely similar, solid solution phases, the frequency distribution curve for a chosen component, and the degree of homogeneity of the X-ray sample

  7. X-Ray Characterization of Non-Equilibrium Solid Solutions

    International Nuclear Information System (INIS)

    Brown, A.; Rosdahl, Oe.

    1975-01-01

    The Rudman approach to composition line broadening in X-ray diffraction patterns, originally designed for the study of diffusion in alloys, is seen to provide a basis for characterizing inhomogeneous solid solutions. Limitations, imposed on this treatment when the cell dimensions of the primary components differ by less than 0.1 A, are attributable to experimental effects such as instrument broadening. These limitations can be overcome by a rigorous numerical treatment of the measured data. Thus, separate elimination of the Kα 2 radiation component followed by iterative deconvolution are advocated for the recovery of the intrinsic broadening. This course of action is made possible chiefly through the availability of large, fast memory computers and primary data recorded in the form of a step scan on punched paper tape. The characteristics of inhomogeneous solid solutions made available by the above treatment are the identity of closely similar, solid solution phases, the frequency distribution curve for a chosen component, and the degree of homogeneity of the X-ray sample

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

    Science.gov (United States)

    Hong, Xinguo; Hao, Quan

    2009-01-01

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

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

    International Nuclear Information System (INIS)

    Hong Xinguo; Hao Quan

    2009-01-01

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

  10. Small-angle neutron scattering study of D2O-alcohol solutions

    International Nuclear Information System (INIS)

    D'Arrigo, G.

    1990-01-01

    Small-angle neutron scattering (SANS) measurements have been carried out on heavy water solutions of ethanol, isopropyl alcohol, n-propyl alcohol, t-butyl alcohol and butoxyethanol between 5 and 37 0 C at the concentrations where ultrasonic attenuation exhibits peak values. The wavevector dependence and the absolute intensity of the scattered intensities were analysed according to a microscopic model of the solutions in terms of aggregated complexes. The results indicate that at 25 0 C there exist either alcohol 'micelle-like' structures or alcohol-heavy water complexes which increase on going from the lower to higher alcohol solutions. As temperature increases from 25 to 37 0 C a higher aggregation is observed in butyl alcohol and butoxyethanol solutions. This behaviour is attributed to the demixing tendency of these systems at high temperatures. On going from 25 to 5 0 C the aggregation increases again. This trend is associated with the anomalous behaviour of the specific heat and ultrasonic attenuation of these systems. The occurrence of a low-temperature phase transition suggested by these anomalies is supported by our results. (author)

  11. Small angle neutron scattering study of the gemini nonionic surfactant in heavy water solutions

    International Nuclear Information System (INIS)

    Rajewska, A

    2012-01-01

    The nonionic gemini surfactant α α'-[2,4,7,9-tetramethyl-5-decyne-4,7diyl]bis[ω hydroxyl-polyoxyethylene] (S-10) was investigated in heavy water solutions only for concentrations: 2.3%, 2.5%,3%, 3.4%, 4% and 5% at temperature 25 C with small angle neutron scattering (SANS) method. All of surfactants solutions were prepared using D 2 O (99.9% deuterated, Prikladnaia Chimia, St. Petersburg, Russia) as a solvent. The nonionic gemini surfactant S-10 was obtained from Air Products and Chemicals, Inc., and used without further purification. All SANS measurements were performed on V-4 SANS spectrometer at BENSC, Berlin (Germany). Neutrons were used in wavelength range of 0.02 - 4 nm - 1. For the measurements quartz cells of were used during experiment. Up to 14 such cells were placed in a holder. Results from experiment was calculated and evaluated with PCG 2.0 program from Graz University (Austria). In the investigated solutions two axis ellipsoidal micelles was observed.

  12. Influence of multiple well defined conformations on small-angle scattering of proteins in solution.

    Science.gov (United States)

    Heller, William T

    2005-01-01

    A common structural motif for many proteins comprises rigid domains connected by a flexible hinge or linker. The flexibility afforded by these domains is important for proper function and such proteins may be able to adopt more than one conformation in solution under equilibrium conditions. Small-angle scattering of proteins in solution samples all conformations that exist in the sampled volume during the time of the measurement, providing an ensemble-averaged intensity. In this paper, the influence of sampling an ensemble of well defined protein structures on the small-angle solution scattering intensity profile is examined through common analysis methods. Two tests were performed using simulated data: one with the extended and collapsed states of the bilobal calcium-binding protein calmodulin and the second with the catalytic subunit of protein kinase A, which has two globular domains connected by a glycine hinge. In addition to analyzing the simulated data for the radii of gyration Rg, distance distribution function P(r) and particle volume, shape restoration was applied to the simulated data. Rg and P(r) of the ensemble profiles could be easily mistaken for a single intermediate state. The particle volumes and models of the ensemble intensity profiles show that some indication of multiple conformations exists in the case of calmodulin, which manifests an enlarged volume and shapes that are clear superpositions of the conformations used. The effect on the structural parameters and models is much more subtle in the case of the catalytic subunit of protein kinase A. Examples of how noise influences the data and analyses are also presented. These examples demonstrate the loss of the indications of multiple conformations in cases where even broad distributions of structures exist. While the tests using calmodulin show that the ensemble states remain discernible from the other ensembles tested or a single partially collapsed state, the tests performed using the

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  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. Soft X-ray Absorption Spectroscopy of Liquids and Solutions.

    Science.gov (United States)

    Smith, Jacob W; Saykally, Richard J

    2017-12-13

    X-ray absorption spectroscopy (XAS) is an electronic absorption technique for which the initial state is a deeply buried core level. The photon energies corresponding to such transitions are governed primarily by the binding energies of the initial state. Because the binding energies of core electrons vary significantly among atomic species, this makes XAS an element-selective spectroscopy. Proper interpretation of XA spectra can provide detailed information on the local chemical and geometric environment of the target atom. The introduction of liquid microjet and flow cell technologies into XAS experiments has enabled the general study of liquid samples. Liquids studied to date include water, alcohols, and solutions with relevance to biology and energy technology. This Review summarizes the experimental techniques employed in XAS studies of liquid samples and computational methods used for interpretation of the resulting spectra and summarizes salient experiments and results obtained in the XAS investigations of liquids.

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

    Science.gov (United States)

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

    2017-01-01

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

  17. Effective interactions in lysozyme aqueous solutions: a small-angle neutron scattering and computer simulation study.

    Science.gov (United States)

    Abramo, M C; Caccamo, C; Costa, D; Pellicane, G; Ruberto, R; Wanderlingh, U

    2012-01-21

    We report protein-protein structure factors of aqueous lysozyme solutions at different pH and ionic strengths, as determined by small-angle neutron scattering experiments. The observed upturn of the structure factor at small wavevectors, as the pH increases, marks a crossover between two different regimes, one dominated by repulsive forces, and another one where attractive interactions become prominent, with the ensuing development of enhanced density fluctuations. In order to rationalize such experimental outcome from a microscopic viewpoint, we have carried out extensive simulations of different coarse-grained models. We have first studied a model in which macromolecules are described as soft spheres interacting through an attractive r(-6) potential, plus embedded pH-dependent discrete charges; we show that the uprise undergone by the structure factor is qualitatively predicted. We have then studied a Derjaguin-Landau-Verwey-Overbeek (DLVO) model, in which only central interactions are advocated; we demonstrate that this model leads to a protein-rich/protein-poor coexistence curve that agrees quite well with the experimental counterpart; experimental correlations are instead reproduced only at low pH and ionic strengths. We have finally investigated a third, "mixed" model in which the central attractive term of the DLVO potential is imported within the distributed-charge approach; it turns out that the different balance of interactions, with a much shorter-range attractive contribution, leads in this latter case to an improved agreement with the experimental crossover. We discuss the relationship between experimental correlations, phase coexistence, and features of effective interactions, as well as possible paths toward a quantitative prediction of structural properties of real lysozyme solutions. © 2012 American Institute of Physics

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

    DEFF Research Database (Denmark)

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

    2011-01-01

    )-b-poly(ethylene oxide) (PEP-PEO) in a 70% ethanol solution are investigated. The polymers have identical PEP blocks of 5.0 kDa and varying PEO blocks of 2.8-49 kDa. The SLS contrasts of PEP and PEO are similar, providing a homogeneous contrast, making SLS ideal for determining the overall micelle morphology. The SAXS...... contrasts of the two components are very different, allowing for resolution of the internal micelle structure. A core-shell model with a PEP core and PEO corona is fitted simultaneously to the SAXS and SLS data using the different contrasts of the two blocks for each technique. With increasing PEO molecular...

  19. Fluorescence x-ray analyzer for plating-bath solution

    International Nuclear Information System (INIS)

    Komatsu, Shigemi; Hato, Yoshio; Tono, Miki; Ishijima, Hiroshi

    1984-01-01

    This analyzer was developed for the analysis of plating solution composition and the measurement of plating thickness at the same time in the noble and base metal plating applied to electronic components. The analyzer operates on the principle of fluorescence X-ray measurement which features the capability of high accuracy, non-destructive and multi-element simultaneous analysis. In this paper, the principle of measurement, the configuration of a model SFA 875 analyzer and also the main specifications and measurement examples are described. As the measurement examples, it is described in detail that the model SFA 875 achieved the expansion of the range of application and the improvement of accuracy and the accuracy of simply repeated measurement by combining a digital filter with the linear method of least squares. The digital filter method is that for eliminating noise in data, smoothing spectra and subtracting background. The linear method of least squares is the method for separating the spectra with overlapping peaks into individual peaks. The combination of them allows the analyzer to perform various analyses even by using the spectra obtained with proportional counters. The analysis of the elements whose atomic numbers are close to each other is also possible. The accuracy of measurement of plating thickness is about 0.2 to 2.0 μm, and that of solution composition is about 0.4 to 0.7 g/l. (Wakatsuki, Y.)

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

    Science.gov (United States)

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

    2018-03-01

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

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

    Science.gov (United States)

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

    2015-05-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  3. Ultrafast X-ray absorption study of longitudinal-transverse phonon coupling in electrolyte aqueous solution

    DEFF Research Database (Denmark)

    Jiao, Yishuo; Adams, Bernhard W.; Dohn, Asmus Ougaard

    2017-01-01

    Ultrafast X-ray absorption spectroscopy is applied to study the conversion of longitudinal to transverse phonons in aqueous solution. Permanganate solutes serve as X-ray probe molecules that permit the measurement of the conversion of 13.5 GHz, longitudinal phonons to 27 GHz, transverse phonons...

  4. In situ X-ray scattering studies of protein solution droplets drying on micro- and nanopatterned superhydrophobic PMMA surfaces.

    Science.gov (United States)

    Accardo, Angelo; Gentile, Francesco; Mecarini, Federico; De Angelis, Francesco; Burghammer, Manfred; Di Fabrizio, Enzo; Riekel, Christian

    2010-09-21

    Superhydrophobic poly(methyl methacrylate) surfaces with contact angles of ∼170° and high optical and X-ray transparencies have been fabricated through the use of optical lithography and plasma etching. The surfaces contain either a microscale pattern of micropillars or a random nanofibrillar pattern. Nanoscale asperities on top of the micropillars closely resemble Nelumbo nucifera lotus leaves. The evolution of the contact angle of water and lysozyme solution droplets during evaporation was studied on the micro- and nanopatterned surfaces, showing in particular contact-line pinning for the protein solution droplet on the nanopatterned surface. The microstructural evolution of lysozyme solution droplets was studied on both types of surfaces in situ under nearly contact-free conditions by synchrotron radiation microbeam wide-angle and small-angle X-ray scattering revealing the increasing protein concentration and the onset of precipitation. The solid residuals show hollow sphere morphologies. Rastermicrodiffraction of the detached residuals suggests about a 1/3 volume fraction of ≥17 nm lysozyme nanocrystalline domains and about a 2/3 short-range-order volume fraction. About 5-fold larger nanocrystalline domains were observed at the attachment points of the sphere to the substrates, which is attributed to particle growth in a shear flow. Such surfaces represent nearly contact-free sample supports for studies of inorganic and organic solution droplets, which find applications in biochips.

  5. Buffer-induced swelling and vesicle budding in binary lipid mixtures of dioleoylphosphatidylcholine:dioleoylphosphatidylethanolamine and dioleoylphosphatidylcholine:lysophosphatidylcholine using small-angle X-ray scattering and ³¹P static NMR.

    Science.gov (United States)

    Barriga, Hanna M G; Bazin, Richard; Templer, Richard H; Law, Robert V; Ces, Oscar

    2015-03-17

    A large variety of data exists on lipid phase behavior; however, it is mostly in nonbuffered systems over nonbiological temperature ranges. We present biophysical data on lipid mixtures of dioleoylphosphatidylcholine (DOPC), dioleoylphosphatidylethanolamine (DOPE), and lysophosphatidylcholine (LysoPC) examining their behaviors in excess water and buffer systems over the temperature range 4-34 °C. These mixtures are commonly used to investigate the effects of spontaneous curvature on integral membrane proteins. Using small-angle X-ray scattering (SAXS) and (31)P NMR, we observed lamellar and vesicle phases, with the buffer causing an increase in the layer spacing. Increasing amounts of DOPE in a DOPC bilayer decreased the layer spacing of the mesophase, while the opposite trend was observed for increasing amounts of LysoPC. (31)P static NMR was used to analyze the DOPC:LysoPC samples to investigate the vesicle sizes present, with evidence of vesicle budding observed at LysoPC concentrations above 30 mol %. NMR line shapes were fitted using an adapted program accounting for the distortion of the lipids within the magnetic field. The distortion of the vesicle, because of magnetic susceptibility, varied with LysoPC content, and a discontinuity was found in both the water and buffer samples. Generally, the distortion increased with LysoPC content; however, at a ratio of DOPC:LysoPC 60:40, the sample showed a level of distortion of the vesicle similar to that of pure DOPC. This implies an increased flexibility in the membrane at this point. Commonly, the assumption is that for increasing LysoPC concentration there is a reduction in membrane tension, implying that estimations of membrane tension based on spontaneous curvature assumptions may not be accurate.

  6. The crystal structure and small-angle X-ray analysis of CsdL/TcdA reveal a new tRNA binding motif in the MoeB/E1 superfamily.

    Directory of Open Access Journals (Sweden)

    Miguel López-Estepa

    Full Text Available Cyclic N6-threonylcarbamoyladenosine ('cyclic t6A', ct(6A is a non-thiolated hypermodification found in transfer RNAs (tRNAs in bacteria, protists, fungi and plants. In bacteria and yeast cells ct(6A has been shown to enhance translation fidelity and efficiency of ANN codons by improving the faithful discrimination of aminoacylated tRNAs by the ribosome. To further the understanding of ct(6A biology we have determined the high-resolution crystal structures of CsdL/TcdA in complex with AMP and ATP, an E1-like activating enzyme from Escherichia coli, which catalyzes the ATP-dependent dehydration of t6A to form ct(6A. CsdL/TcdA is a dimer whose structural integrity and dimer interface depend critically on strongly bound K+ and Na+ cations. By using biochemical assays and small-angle X-ray scattering we show that CsdL/TcdA can associate with tRNA with a 1:1 stoichiometry and with the proper position and orientation for the cyclization of t6A. Furthermore, we show by nuclear magnetic resonance that CsdL/TcdA engages in transient interactions with CsdA and CsdE, which, in the latter case, involve catalytically important residues. These short-lived interactions may underpin the precise channeling of sulfur atoms from cysteine to CsdL/TcdA as previously characterized. In summary, the combination of structural, biophysical and biochemical methods applied to CsdL/TcdA has afforded a more thorough understanding of how the structure of this E1-like enzyme has been fine tuned to accomplish ct(6A synthesis on tRNAs while providing support for the notion that CsdA and CsdE are able to functionally interact with CsdL/TcdA.

  7. Small angle neutron scattering study on short and long chain phosphatidylcholine mixture in trehalose solution

    Energy Technology Data Exchange (ETDEWEB)

    Takahashi, Hiroshi [Department of Physics, Gunma University, Maebashi, Gunma (Japan)

    2001-03-01

    Trehalose protects cells and proteins against various stresses due to low temperatures or dryness. In order to clarify the molecular mechanism of cryoprotective function of trehalose, we have studied the interaction between trehalose and phosphatidylcholine (PC) which is a main lipid component of cell membranes. In this study, the structural change of a binary PC mixture by the presence of trehalose was investigated by means of small angle neutron scattering. The PC binary mixture studied contains dihexanoyl-PC (diC{sub 6}PC) and dihexadecy-PC (DHPC). The former has short hydrocarbon chains and the latter has long hydrocarbon chains. The scattering profiles from the DHPC/diC{sub 6}PC mixture were changed, depending on trehalose concentrations. This change can be interpreted as suggesting that the presence of trehalose reduces the interfacial area between water and PCs. (author)

  8. Automatic protein structure solution from weak X-ray data

    Science.gov (United States)

    Skubák, Pavol; Pannu, Navraj S.

    2013-11-01

    Determining new protein structures from X-ray diffraction data at low resolution or with a weak anomalous signal is a difficult and often an impossible task. Here we propose a multivariate algorithm that simultaneously combines the structure determination steps. In tests on over 140 real data sets from the protein data bank, we show that this combined approach can automatically build models where current algorithms fail, including an anisotropically diffracting 3.88 Å RNA polymerase II data set. The method seamlessly automates the process, is ideal for non-specialists and provides a mathematical framework for successfully combining various sources of information in image processing.

  9. X-ray structure of the pestivirus NS3 helicase and its conformation in solution.

    Science.gov (United States)

    Tortorici, M Alejandra; Duquerroy, Stéphane; Kwok, Jane; Vonrhein, Clemens; Perez, Javier; Lamp, Benjamin; Bricogne, Gerard; Rümenapf, Till; Vachette, Patrice; Rey, Félix A

    2015-04-01

    Pestiviruses form a genus in the Flaviviridae family of small enveloped viruses with a positive-sense single-stranded RNA genome. Viral replication in this family requires the activity of a superfamily 2 RNA helicase contained in the C-terminal domain of nonstructural protein 3 (NS3). NS3 features two conserved RecA-like domains (D1 and D2) with ATPase activity, plus a third domain (D3) that is important for unwinding nucleic acid duplexes. We report here the X-ray structure of the pestivirus NS3 helicase domain (pNS3h) at a 2.5-Å resolution. The structure deviates significantly from that of NS3 of other genera in the Flaviviridae family in D3, as it contains two important insertions that result in a narrower nucleic acid binding groove. We also show that mutations in pNS3h that rescue viruses from which the core protein is deleted map to D3, suggesting that this domain may be involved in interactions that facilitate particle assembly. Finally, structural comparisons of the enzyme in different crystalline environments, together with the findings of small-angle X-ray-scattering studies in solution, show that D2 is mobile with respect to the rest of the enzyme, oscillating between closed and open conformations. Binding of a nonhydrolyzable ATP analog locks pNS3h in a conformation that is more compact than the closest apo-form in our crystals. Together, our results provide new insight and bring up new questions about pNS3h function during pestivirus replication. Although pestivirus infections impose an important toll on the livestock industry worldwide, little information is available about the nonstructural proteins essential for viral replication, such as the NS3 helicase. We provide here a comparative structural and functional analysis of pNS3h with respect to its orthologs in other viruses of the same family, the flaviviruses and hepatitis C virus. Our studies reveal differences in the nucleic acid binding groove that could have implications for understanding the

  10. On the attenuation of x-rays and gamma-rays in dilute solutions

    DEFF Research Database (Denmark)

    Gerward, Leif

    1996-01-01

    The theory of X-ray and gamma-ray attenuation in solutions is developed. The rule of mixture for the calculation of mass and linear attenuation coefficients is elaborated in the general case as well as in the limit of extreme dilution. The validity of the latter approximation is illustrated...... by the attenuation of 17.443 keV X-rays in aqueous solutions of NaCl. Copyright (C) 1996 Elsevier Science Ltd...

  11. Structure and dynamics of nonaqueous electrolyte solutions by small angle neutron scattering, brownian dynamics and primitive model theories

    International Nuclear Information System (INIS)

    Kunz, W.; Turq, P.

    1990-01-01

    The study of electrolyte solutions by small angle neutron scattering (static) of quasi-elastic neutron scattering (dynamics) gives new perspectives to the primitive model of electrolytes, for both static and dynamic properties of those systems. Whereas all properties can be interpreted by brownian dynamics, integral equations cannot be used at the present time to get transport coefficients in all cases. As regards the choice of the potentials at the McMillan Mayer level, specific Gurney terms for solvation are not needed for tetraalkylammonium salts. (orig.)

  12. Reliable structural interpretation of small-angle scattering data from bio-molecules in solution--the importance of quality control and a standard reporting framework.

    Science.gov (United States)

    Jacques, David A; Guss, Jules Mitchell; Trewhella, Jill

    2012-05-17

    Small-angle scattering is becoming an increasingly popular tool for the study of bio-molecular structures in solution. The large number of publications with 3D-structural models generated from small-angle solution scattering data has led to a growing consensus for the need to establish a standard reporting framework for their publication. The International Union of Crystallography recently established a set of guidelines for the necessary information required for the publication of such structural models. Here we describe the rationale for these guidelines and the importance of standardising the way in which small-angle scattering data from bio-molecules and associated structural interpretations are reported.

  13. Supercrystallization of KCl from solution irradiated by soft X-rays

    Science.gov (United States)

    Janavičius, A. J.; Rinkūnas, R.; Purlys, R.

    2016-10-01

    The X-rays influence on KCl crystallization in a saturated water solution has been investigated for the aim of comparing it with previously considered NaCl crystallization. The rate of crystallization has been measured in the drying drop in the solution activated by the irradiation. We have measured the influence of the irradiation time of the solution on the rates of KCl crystallization as well as the beginning of the crystallization processes on drying drops. For a longer irradiation time of the solution early crystallization in the drops occurs. A saturated water solution of KCl was irradiated with the diffractometer DRON-3M (Russian device) and this had a great influence on the two-step processes of crystallization. The ionization of the solution by soft X-rays can produce ions, metastable radicals in water, excited crystals' seeds and vacancies in growing crystals by Auger's effect. The X-rays generate a very fast crystallization in the drying drop.

  14. Determination of plutonium in nitric acid solutions using energy dispersive L X-ray fluorescence with a low power X-ray generator

    Energy Technology Data Exchange (ETDEWEB)

    Py, J. [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France); Groetz, J.-E., E-mail: jegroetz@univ-fcomte.fr [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Hubinois, J.-C.; Cardona, D. [Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France)

    2015-04-21

    This work presents the development of an in-line energy dispersive L X-ray fluorescence spectrometer set-up, with a low power X-ray generator and a secondary target, for the determination of plutonium concentration in nitric acid solutions. The intensity of the L X-rays from the internal conversion and gamma rays emitted by the daughter nuclei from plutonium is minimized and corrected, in order to eliminate the interferences with the L X-ray fluorescence spectrum. The matrix effects are then corrected by the Compton peak method. A calibration plot for plutonium solutions within the range 0.1–20 g L{sup −1} is given.

  15. Exploring the structure of biological macromolecules in solution using Quokka, the small angle neutron scattering instrument, at ANSTO

    International Nuclear Information System (INIS)

    Wood, Kathleen; Jeffries, Cy M.; Knott, Robert B.; Sokolova, Anna; Jacques, David A.; Duff, Anthony P.

    2015-01-01

    Small angle neutron scattering (SANS) is widely used to extract structural parameters, shape and other types of information from a vast array of materials. The technique is applied to biological macromolecules and their complexes in solution to reveal information often not accessible by other techniques. SANS measurements on biomolecules present some particular challenges however, one of which is suitable instrumentation. This review details SANS experiments performed on two well-characterised globular proteins (lysozyme and glucose isomerase) using Quokka, the recently commissioned SANS instrument at the Australian Nuclear Science and Technology Organisation (ANSTO). The instrument configuration as well as data collection and reduction strategies for biological investigations are discussed and act as a general reference for structural biologists who use the instrument. Both model independent analysis of the two proteins and ab initio modelling illustrate that Quokka-SANS data can be used to successfully model the overall shapes of proteins in solution, providing a benchmark for users

  16. Anomalous and resonance small-angle scattering

    International Nuclear Information System (INIS)

    Epperson, J.E.; Thiyagarajan, P.

    1988-01-01

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

  17. Studies in small angle scattering techniques

    International Nuclear Information System (INIS)

    Moellenbach, K.

    1980-03-01

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

  18. Solution spectroelectrochemical cell for in situ X-ray absorption fine structure

    International Nuclear Information System (INIS)

    Antonio, M.R.; Soderholm, L.

    1995-01-01

    A purpose-built spectroelectrochemical cell for in situ fluorescence XAFS (X-ray Absorption Fine Structure) measurements of bulk solution species during constant-potential electrolysis is described. The cell performance was demonstrated by the collection of europium L 3 -edge XANES (X-ray Absorption Near Edge Structure) throughout the course of electrolysis of an aqueous solution of EuCl 3 ·6H 2 O in 1 M H 2 SO 4 . The europium L 3 -edge resonances reported here for the Eu III and Eu II ions demonstrate that their 2p 3/2 → 5d electronic transition probabilities are not the same

  19. Summary of existing information on gamma-ray and X-ray attenuation coefficients of solutions

    DEFF Research Database (Denmark)

    Singh, K.; Gerward, Leif

    2002-01-01

    Accurate values of X-ray and gamma-ray attenuation coefficients of different chemicals are required in spectrometry as well as in many other scientific, engineering and medical disciplines involving photon radiation. The current state of knowledge of experimental and theoretical gamma-ray and X-r......-ray attenuation coefficients in aqueous solutions of salts is presented and exemplified by recent work. The results presented provide a basis for studying X-ray and gamma-ray photon interactions with ions in solution (hydrated ions) rather than ion compounds in solid form....

  20. The X-ray electronic spectra of TiC-NbC solid solution

    International Nuclear Information System (INIS)

    Cherkashenko, V.M.; Ezhov, A.V.; Nazarova, S.Z.; Kurmaev, Eh.Z.; Nojmann, M.

    2001-01-01

    X-ray photoelectronic spectra of inner levels and valency lands in TiC-NbC solid solutions were studied. Results of combining TiL α -, NbL β2.15 -, CK α - X-ray emission spectra and photoelectronic spectra of valency bands in one energy scale in reference to the Fermi level were analyzed. It is shown that a change in crystal lattice parameters, as well as charge redistribution between titanium and niobium atoms, produce a strong effect on electronic structure formation in the mixed carbides mentioned [ru

  1. The scattering problem in X-ray adsorptiometry using an MWPC; and its solution

    International Nuclear Information System (INIS)

    Bateman, J.E.

    1978-03-01

    It is shown that a large aperture imaging X-ray absorptiometric system (in this case a xenon filled MWPC) suffers very badly from scattering in the water bath and soft tissue components of the imaged system in the bone mass measuring case. Applications of a fine focused collimator provides a satisfactory solution to the problem. (author)

  2. Small angle spectrometers: Summary

    International Nuclear Information System (INIS)

    Courant, E.; Foley, K.J.; Schlein, P.E.

    1986-01-01

    Aspects of experiments at small angles at the Superconducting Super Collider are considered. Topics summarized include a small angle spectrometer, a high contingency spectrometer, dipole and toroid spectrometers, and magnet choices

  3. On the attenuation of X-rays and gamma-rays for aqueous solutions of salts

    CERN Document Server

    Teli, M T

    1998-01-01

    Disparities in the linear attenuation coefficients of X-rays and gamma rays for aqueous solutions of soluble salts arising from the nonequality of volume of the solution with the sum of volumes of its components are analysed and the mixture rule is reformulated. The disparities are illustrated for NaCl solution for concentrations c=0 to 1 gm/cm sup 3 which indicates that the mixture rule of Teli et al. works well within generally acceptable limits.

  4. Counterion Association and Structural Conformation Change of Charged PAMAM Dendrimer in Aqueous Solutions Revealed by Small Angle Neutron Scattering

    International Nuclear Information System (INIS)

    Chen, Wei-Ren

    2009-01-01

    Our previous study of the structure change of poly(amidoamine) starburst dendrimers (PAMAM) dendrimer of generation 5 (G5) have demonstrated that although the overall molecular size is practically unaffected by increasing DCl concentration, a configurational transformation, from a diffusive density profile to a more uniform density distribution, is clearly observed. In the current paper, the focus is placed on understanding the effect of counterion identity on the inter-molecular structure and the conformational properties by studying the effect due to DBr using small angle neutron scattering (SANS) and integral equation theory. While the overall molecular size is found to be essentially unaffected by the change in the pD of solutions, it is surprising that the intra-molecular configurational transformation is not observed when DBr is used. The overall effective charge of a dendrimer is nearly the same for 1, the effect of counterion identity becomes significant, the effective charge carried by a charged G5 PAPAM protonated by DBr becomes smaller than that of solutions with DCl. As a consequence, a counterion identity dependence of counterion association is revealed: Under the same level of molecular protonation, the specific counterion association, which is defined as the ratio of bound chloride anions to positively charged amines per molecule, is larger for the G5 PAMAM dendrimer charged by DBr than the one by DCl.

  5. Conformational effect on small angle neutron scattering behavior of interacting polyelectrolyte solutions: a perspective of integral equation theory.

    Science.gov (United States)

    Shew, Chwen-Yang; Do, Changwoo; Hong, Kunlun; Liu, Yun; Porcar, Lionel; Smith, Gregory S; Chen, Wei-Ren

    2012-07-14

    We present small angle neutron scattering (SANS) measurements of deuterium oxide (D(2)O) solutions of linear and star sodium poly(styrene sulfonate) (NaPSS) as a function of polyelectrolyte concentration. Emphasis is on understanding the dependence of their SANS coherent scattering cross section I(Q) on the molecular architecture of single polyelectrolyte. The key finding is that for a given concentration, star polyelectrolytes exhibit more pronounced characteristic peaks in I(Q), and the position of the first peak occurs at a smaller Q compared to their linear counterparts. Based on a model of integral equation theory, we first compare the SANS experimental I(Q) of salt-free polyelectrolyte solutions with that predicted theoretically. Having seen their satisfactory qualitative agreement, the dependence of counterion association behavior on polyelectrolyte geometry and concentration is further explored. Our predictions reveal that the ionic environment of polyelectrolyte exhibits a strong dependence on polyelectrolyte geometry at lower polyelectrolyte concentration. However, when both linear and star polyelectrolytes exceed their overlap concentrations, the spatial distribution of counterion is found to be essentially insensitive to polyelectrolyte geometry due to the steric effect.

  6. A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions

    International Nuclear Information System (INIS)

    Brown, Matthew A.; Redondo, Amaia Beloqui; Duyckaerts, Nicolas; Mächler, Jean-Pierre; Jordan, Inga; Wörner, Hans Jakob; Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Birrer, Mario; Honegger, Juri; Wetter, Reto; Bokhoven, Jeroen A. van

    2013-01-01

    A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented

  7. A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions.

    Science.gov (United States)

    Brown, Matthew A; Redondo, Amaia Beloqui; Jordan, Inga; Duyckaerts, Nicolas; Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Müächler, Jean-Pierre; Birrer, Mario; Honegger, Juri; Wetter, Reto; Wörner, Hans Jakob; van Bokhoven, Jeroen A

    2013-07-01

    A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.

  8. A new endstation at the Swiss Light Source for ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy measurements of liquid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Brown, Matthew A.; Redondo, Amaia Beloqui; Duyckaerts, Nicolas; Mächler, Jean-Pierre [Institute for Chemical and Bioengineering, ETH Zürich, CH-8093 Zürich (Switzerland); Jordan, Inga; Wörner, Hans Jakob [Laboratory of Physical Chemistry, ETH Zürich, CH-8093 Zürich (Switzerland); Lee, Ming-Tao; Ammann, Markus; Nolting, Frithjof; Kleibert, Armin; Huthwelker, Thomas; Birrer, Mario; Honegger, Juri; Wetter, Reto [Paul Scherrer Institute, CH-5232 Villigen PSI (Switzerland); Bokhoven, Jeroen A. van [Institute for Chemical and Bioengineering, ETH Zürich, CH-8093 Zürich (Switzerland); Paul Scherrer Institute, CH-5232 Villigen PSI (Switzerland)

    2013-07-15

    A new liquid microjet endstation designed for ultraviolet (UPS) and X-ray (XPS) photoelectron, and partial electron yield X-ray absorption (XAS) spectroscopies at the Swiss Light Source is presented. The new endstation, which is based on a Scienta HiPP-2 R4000 electron spectrometer, is the first liquid microjet endstation capable of operating in vacuum and in ambient pressures up to the equilibrium vapor pressure of liquid water at room temperature. In addition, the Scienta HiPP-2 R4000 energy analyzer of this new endstation allows for XPS measurements up to 7000 eV electron kinetic energy that will enable electronic structure measurements of bulk solutions and buried interfaces from liquid microjet samples. The endstation is designed to operate at the soft X-ray SIM beamline and at the tender X-ray Phoenix beamline. The endstation can also be operated using a Scienta 5 K ultraviolet helium lamp for dedicated UPS measurements at the vapor-liquid interface using either He I or He II α lines. The design concept, first results from UPS, soft X-ray XPS, and partial electron yield XAS measurements, and an outlook to the potential of this endstation are presented.

  9. Reliable structural interpretation of small-angle scattering data from bio-molecules in solution - the importance of quality control and a standard reporting framework

    Directory of Open Access Journals (Sweden)

    Jacques David A

    2012-05-01

    Full Text Available Abstract Small-angle scattering is becoming an increasingly popular tool for the study of bio-molecular structures in solution. The large number of publications with 3D-structural models generated from small-angle solution scattering data has led to a growing consensus for the need to establish a standard reporting framework for their publication. The International Union of Crystallography recently established a set of guidelines for the necessary information required for the publication of such structural models. Here we describe the rationale for these guidelines and the importance of standardising the way in which small-angle scattering data from bio-molecules and associated structural interpretations are reported.

  10. Quantitative determination of uranium in organic solution by X-ray fluorescence

    International Nuclear Information System (INIS)

    Leyt, D.V. de; Colangelo, C.H.

    1987-01-01

    An X-ray fluorescent method for the determination of uranium in tributilphosphate-kerosene-nitriacid solution has been developed. Chemical properties of the matrix elements were studied in order to select a convenient procedure to determine samples and standards on the same way. The method avoids the destruction of the organic material and has proved to be very useful for the fast control of uranium concentration. (Author) [es

  11. Chemical analysis of zinc electroplating solutions by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Jung, Sung-Mo; Cho, Young-Mo; Na, Han-Gil

    2007-01-01

    A quantitative analysis method used to analyze chlorine, iron and zinc in electroplating solutions, using X-ray spectrometry in atmospheric He mode, is proposed. The present research concerns the replacement of the conventional analyses of electroplating solutions with rapid and reproducible quantification using X-ray fluorescence spectrometer. An in-depth investigation conducted in the present study identifies the species present in the real electroplating solutions. XRD patterns and semi-quantitative results for the electroplating solutions show synthetic standards based on the compositional range of solutions by analyzing the electroplating solutions obtained in real processes. 28 calibration standard solutions are prepared by diluting liquid standard solutions certified by titration and ICP-OES analyses used to construct the XRF calibration curves for Cl, Fe and Zn. The suggested method showed satisfactory precision and accuracy in the analysis of electroplating solutions. The present study provides evidences that the proposed XRF spectrometry could be an alternative analytical method to replace the conventional techniques by comparing the uncertainties estimated for each method. (author)

  12. In-situ x-ray absorption study of copper films in ground water solutions

    International Nuclear Information System (INIS)

    Kvashnina, K.O.; Butorin, S.M.; Modin, A.; Soroka, I.; Marcellini, M.; Nordgren, J.; Guo, J.-H.; Werme, L.

    2007-01-01

    This study illustrates how the damage from copper corrosion can be reduced by modifying the chemistry of the copper surface environment. The surface modification of oxidized copper films induced by chemical reaction with Cl - and HCO 3 - in aqueous solutions was monitored by in situ X-ray absorption spectroscopy. The results show that corrosion of copper can be significantly reduced by adding even a small amount of sodium bicarbonate. The studied copper films corroded quickly in chloride solutions, whereas the same solution containing 1.1 mM HCO 3 - prevented or slowed down the corrosion processes

  13. Performance of a micro-strip gas chamber in solution X-ray scattering

    CERN Document Server

    Toyokawa, H; Inoko, Y; Nagayoshi, T; Nishi, Y; Nishikawa, Y; Ochi, A; Suzuki, M; Tanimori, T

    2001-01-01

    The performance of a Micro-Strip Gas Chamber in solution X-ray scattering was studied at the RIKEN structural biology beamline I of the SPring-8 facility. The practical dynamic range was confirmed to be approx 1,000,000 : 1 by measuring S sup - sup 4 decay from a polystyrene latex solution. Steep troughs of scattering profile from an apoferritin solution were clearly obtained without smearing. An unfolding process of a pH jump of cytochrome c was measured. A time resolution of 500 mu s was achieved.

  14. Thorium determination by X-ray Fluorescence Spectrometry in simulated thorex process solutions

    International Nuclear Information System (INIS)

    Yamaura, M.; Matsuda, H.T.

    1989-01-01

    The X-ray fluorescence method for thorium determination in aqueous and organic (TBP-n-dodecane) solutions is described. The thin film-technique for sample preparation and a suitable internal standard have been used. Some parameters as analytical line, internal standard, filter paper, paper geometry, sample volume and measurement conditions were studied. Uranium, fission products, corrosion products and thorex reagent components were studied as interfering elements in the thorium analysis, as well as the matrix effect by using the thorex process simulated solutions the method to thorium determination in irradiated thorium solutions was applied. (M.J.C.) [pt

  15. X-ray Raman spectroscopy of lithium-ion battery electrolyte solutions in a flow cell.

    Science.gov (United States)

    Ketenoglu, Didem; Spiekermann, Georg; Harder, Manuel; Oz, Erdinc; Koz, Cevriye; Yagci, Mehmet C; Yilmaz, Eda; Yin, Zhong; Sahle, Christoph J; Detlefs, Blanka; Yavaş, Hasan

    2018-03-01

    The effects of varying LiPF 6 salt concentration and the presence of lithium bis(oxalate)borate additive on the electronic structure of commonly used lithium-ion battery electrolyte solvents (ethylene carbonate-dimethyl carbonate and propylene carbonate) have been investigated. X-ray Raman scattering spectroscopy (a non-resonant inelastic X-ray scattering method) was utilized together with a closed-circle flow cell. Carbon and oxygen K-edges provide characteristic information on the electronic structure of the electrolyte solutions, which are sensitive to local chemistry. Higher Li + ion concentration in the solvent manifests itself as a blue-shift of both the π* feature in the carbon edge and the carbonyl π* feature in the oxygen edge. While these oxygen K-edge results agree with previous soft X-ray absorption studies on LiBF 4 salt concentration in propylene carbonate, carbon K-edge spectra reveal a shift in energy, which can be explained with differing ionic conductivities of the electrolyte solutions.

  16. 2017 publication guidelines for structural modelling of small-angle scattering data from biomolecules in solution: an update.

    Science.gov (United States)

    Trewhella, Jill; Duff, Anthony P; Durand, Dominique; Gabel, Frank; Guss, J Mitchell; Hendrickson, Wayne A; Hura, Greg L; Jacques, David A; Kirby, Nigel M; Kwan, Ann H; Pérez, Javier; Pollack, Lois; Ryan, Timothy M; Sali, Andrej; Schneidman-Duhovny, Dina; Schwede, Torsten; Svergun, Dmitri I; Sugiyama, Masaaki; Tainer, John A; Vachette, Patrice; Westbrook, John; Whitten, Andrew E

    2017-09-01

    In 2012, preliminary guidelines were published addressing sample quality, data acquisition and reduction, presentation of scattering data and validation, and modelling for biomolecular small-angle scattering (SAS) experiments. Biomolecular SAS has since continued to grow and authors have increasingly adopted the preliminary guidelines. In parallel, integrative/hybrid determination of biomolecular structures is a rapidly growing field that is expanding the scope of structural biology. For SAS to contribute maximally to this field, it is essential to ensure open access to the information required for evaluation of the quality of SAS samples and data, as well as the validity of SAS-based structural models. To this end, the preliminary guidelines for data presentation in a publication are reviewed and updated, and the deposition of data and associated models in a public archive is recommended. These guidelines and recommendations have been prepared in consultation with the members of the International Union of Crystallography (IUCr) Small-Angle Scattering and Journals Commissions, the Worldwide Protein Data Bank (wwPDB) Small-Angle Scattering Validation Task Force and additional experts in the field.

  17. A note on the assay of special nuclear materials in solution by x-ray fluorescence

    International Nuclear Information System (INIS)

    Canada, T.R.; Hsue, S.T.

    1982-01-01

    Presents a formulation that allows empirical results of the ''internal standard'' approach to be understood in a quantifiable manner, and suggests an alternative measurement procedure that removes many of the technique's undesirable features while maintaining those that add to instrumental accuracy. Assumes that the reader is familiar with x-ray fluorescence (XRF) technology. Promises a more detailed presentation, including proof-of-principle experimental results, in the future. Points out that practical applications of this approach may be achieved with both K- and L-x-ray fluorescence. Concludes that the formulation and alternative measurement procedure suggested indicates that the ''internal standard'' approach may be improved by making measurements at one or more additional x-ray energies of the element to be assayed. Effects of solution acidity variations and the relative concentrations of plutonium and uranium may be avoided. Because of the inherent stability of ratio techniques, little or no modification to this formulation is anticipated for cylindrical near-field geometries

  18. Small-angle X-ray titration study on the complex formation between 5-S RNA and the L18 protein of the Escherichia coli 50-S ribosome particle

    International Nuclear Information System (INIS)

    Oesterberg, R.; Garrett, A.

    1977-01-01

    The 5-S RNA (A) and the L 18 protein (B) from Escherichia coli ribosomes form one single AB complex in the concentration ranges supposed to prevail in vivo; at concentrations of L 18 higher than 40 mM there is some indication for a minor species, most probably an AB 2 species. This is indicated from the X-ray scattering titration data of the 5-S RNA/L 18 system recorded at 21 0 C in ribosomal reconstitution buffer. As a result of the 1 : 1 complex formation, there is a relatively small but defined increase in the radius of gyration from 3.61 to 3.85 nm. This result as well as the experimental scattering curve can be explained by models where it is assumed that the elongated L 18 model is quite far from the electron density centre and where protein L 18 interacts with one or both of the minor arms of the supposed Y-shaped 5-S RNA molecule. (orig.) [de

  19. BioSAXS Sample Changer: a robotic sample changer for rapid and reliable high-throughput X-ray solution scattering experiments.

    Science.gov (United States)

    Round, Adam; Felisaz, Franck; Fodinger, Lukas; Gobbo, Alexandre; Huet, Julien; Villard, Cyril; Blanchet, Clement E; Pernot, Petra; McSweeney, Sean; Roessle, Manfred; Svergun, Dmitri I; Cipriani, Florent

    2015-01-01

    Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC.

  20. X-ray Studies of Regenerated Cellulose Fibers Wet Spun from Cotton Linter Pulp in NaOH/Thiourea Aqueous Solutions

    Energy Technology Data Exchange (ETDEWEB)

    Chen,X.; Burger, C.; Fang, D.; Ruan, D.; Zhang, L.; Hsiao, B.; Chu, B.

    2006-01-01

    Regenerated cellulose fibers were fabricated by dissolution of cotton linter pulp in NaOH (9.5 wt%) and thiourea (4.5 wt%) aqueous solution followed by wet-spinning and multi-roller drawing. The multi-roller drawing process involved three stages: coagulation (I), coagulation (II) and post-treatment (III). The crystalline structure and morphology of regenerated cellulose fiber was investigated by synchrotron wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) techniques. Results indicated that only the cellulose II crystal structure was found in regenerated cellulose fibers, proving that the cellulose crystals were completely transformed from cellulose I to II structure during spinning from NaOH/thiourea aqueous solution. The crystallinity, orientation and crystal size at each stage were determined from the WAXD analysis. Drawing of cellulose fibers in the coagulation (II) bath (H{sub 2}SO{sub 4}/H{sub 2}O) was found to generate higher orientation and crystallinity than drawing in the post-treatment (III). Although the post-treatment process also increased crystal orientation, it led to a decrease in crystallinity with notable reduction in the anisotropic fraction. Compared with commercial rayon fibers fabricated by the viscose process, the regenerated cellulose fibers exhibited higher crystallinity but lower crystal orientation. SAXS results revealed a clear scattering maximum along the meridian direction in all regenerated cellulose fibers, indicating the formation of lamellar structure during spinning.

  1. BioSAXS Sample Changer: a robotic sample changer for rapid and reliable high-throughput X-ray solution scattering experiments

    Energy Technology Data Exchange (ETDEWEB)

    Round, Adam, E-mail: around@embl.fr; Felisaz, Franck [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Fodinger, Lukas; Gobbo, Alexandre [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Huet, Julien [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Villard, Cyril [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Blanchet, Clement E., E-mail: around@embl.fr [EMBL c/o DESY, Notkestrasse 85, 22603 Hamburg (Germany); Pernot, Petra; McSweeney, Sean [ESRF, 6 Rue Jules Horowitz, 38000 Grenoble (France); Roessle, Manfred; Svergun, Dmitri I. [EMBL c/o DESY, Notkestrasse 85, 22603 Hamburg (Germany); Cipriani, Florent, E-mail: around@embl.fr [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France)

    2015-01-01

    A robotic sample changer for solution X-ray scattering experiments optimized for speed and to use the minimum amount of material has been developed. This system is now in routine use at three high-brilliance European synchrotron sites, each capable of several hundred measurements per day. Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC.

  2. Limiting cases of the small-angle scattering approximation solutions for the propagation of laser beams in anisotropic scattering media

    Science.gov (United States)

    Box, M. A.; Deepak, A.

    1981-01-01

    The propagation of photons in a medium with strongly anisotropic scattering is a problem with a considerable history. Like the propagation of electrons in metal foils, it may be solved in the small-angle scattering approximation by the use of Fourier-transform techniques. In certain limiting cases, one may even obtain analytic expressions. This paper presents some of these results in a model-independent form and also illustrates them by the use of four different phase-function models. Sample calculations are provided for comparison purposes

  3. 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...

  4. Preparation of uranium standard solutions for x-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Wong, C.M.; Cate, J.L.; Pickles, W.L.

    1978-03-01

    A method has been developed for gravimetrically preparing uranium nitrate standards with an estimated mean error of 0.1% (1 sigma) and a maximum error of 0.2% (1 sigma) for the total uranium weight. Two source materials, depleted uranium dioxide powder and NBS Standard Reference Material 960 uranium metal, were used to prepare stock solutions. The NBS metal proved to be superior because of the small but inherent uncertainty in the stoichiometry of the uranium oxide. These solutions were used to prepare standards in a freeze-dried configuration suitable for x-ray fluorescence analysis. Both gravimetric and freeze-drying techniques are presented. Volumetric preparation was found to be unsatisfactory for 0.1% precision for the sample size of interest. One of the primary considerations in preparing uranium standards for x-ray fluorescence analysis is the development of a technique for dispensing a 50-μl aliquot of a standard solution with a precision of 0.1% and an accuracy of 0.1%. The method developed corrects for variation in aliquoting and for evaporation loss during weighing. Two sets, each containing 50 standards have been produced. One set has been retained by LLL and one set retained by the Savannah River project

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-12-01

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

  6. Modeling small angle scattering data using FISH

    International Nuclear Information System (INIS)

    Elliott, T.; Buckely, C.E.

    2002-01-01

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

  7. THE TRANSIENT ACCRETING X-RAY PULSAR XTE J1946+274: STABILITY OF X-RAY PROPERTIES AT LOW FLUX AND UPDATED ORBITAL SOLUTION

    Energy Technology Data Exchange (ETDEWEB)

    Marcu-Cheatham, Diana M.; Pottschmidt, Katja [CRESST and Department of Physics, University of Maryland Baltimore County, 1000 Hilltop Circle, Baltimore, MD 21250 (United States); Kühnel, Matthias; Müller, Sebastian; Falkner, Sebastian; Kreykenbohm, Ingo [Dr. Karl Remeis-Observatory and ECAP, University Erlangen-Nuremberg, Sternwartstr. 7, Bamberg (Germany); Caballero, Isabel [Laboratoire AIM, CEA/IRFU, CNRS/INSU, Université Paris Diderot, CEA DSM/IRFU/SAp, F-91191 Gif-sur-Yvette (France); Finger, Mark H. [Universities Space Research Association, National Space Science and Technology Center, 320 Sparkman Drive, Huntsville, AL 35805 (United States); Jenke, Peter J. [University of Alabama in Huntsville, 301 Sparkman Drive, Huntsville, AL 35899 (United States); Wilson-Hodge, Colleen A. [Astrophysics Office, ZP 12, NASA Marshall Space Flight Center, Huntsville, AL 35812 (United States); Fürst, Felix [Cahill Center for Astronomy and Astrophysics, California Institute of Technology, Pasadena, CA 91125 (United States); Grinberg, Victoria [Massachusetts Institute of Technology, Kavli Institute for Astrophysics, Cambridge, MA 02139 (United States); Hemphill, Paul B.; Rothschild, Richard E. [University of California, San Diego, Center for Astrophysics and Space Sciences, 9500 Gilman Drive, La Jolla, CA 92093-0424 (United States); Klochkov, Dmitry [Institut für Astronomie und Astrophysik, Universität Tübingen (IAAT), Sand 1, Tübingen (Germany); Terada, Yukikatsu [Graduate School of Science and Engineering, Saitama University, 255 Simo-Ohkubo, Sakura-ku, Saitama City, Saitama 338-8570 (Japan); and others

    2015-12-10

    We present a timing and spectral analysis of the X-ray pulsar XTE J1946+274 observed with Suzaku during an outburst decline in 2010 October and compare with previous results. XTE J1946+274 is a transient X-ray binary consisting of a Be-type star and a neutron star with a 15.75 s pulse period in a 172 days orbit with 2–3 outbursts per orbit during phases of activity. We improve the orbital solution using data from multiple instruments. The X-ray spectrum can be described by an absorbed Fermi–Dirac cut-off power-law model along with a narrow Fe Kα line at 6.4 keV and a weak Cyclotron Resonance Scattering Feature (CRSF) at ∼35 keV. The Suzaku data are consistent with the previously observed continuum flux versus iron line flux correlation expected from fluorescence emission along the line of sight. However, the observed iron line flux is slightly higher, indicating the possibility of a higher iron abundance or the presence of non-uniform material. We argue that the source most likely has only been observed in the subcritical (non-radiation dominated) state since its pulse profile is stable over all observed luminosities and the energy of the CRSF is approximately the same at the highest (∼5 × 10{sup 37} erg s{sup −1}) and lowest (∼5 × 10{sup 36} erg s{sup −1}) observed 3–60 keV luminosities.

  8. Simulated x-ray scattering of protein solutions using explicit-solvent models

    International Nuclear Information System (INIS)

    Park, Sanghyun; Bardhan, Jaydeep P.; Makowski, Lee; Roux, Benoit

    2009-01-01

    X-ray solution scattering shows new promise for the study of protein structures, complementing crystallography and nuclear magnetic resonance. In order to realize the full potential of solution scattering, it is necessary to not only improve experimental techniques but also develop accurate and efficient computational schemes to relate atomistic models to measurements. Previous computational methods, based on continuum models of water, have been unable to calculate scattering patterns accurately, especially in the wide-angle regime which contains most of the information on the secondary, tertiary, and quaternary structures. Here we present a novel formulation based on the atomistic description of water, in which scattering patterns are calculated from atomic coordinates of protein and water. Without any empirical adjustments, this method produces scattering patterns of unprecedented accuracy in the length scale between 5 and 100 A, as we demonstrate by comparing simulated and observed scattering patterns for myoglobin and lysozyme.

  9. A novel solution to the gated x-ray detector gain droop problem

    International Nuclear Information System (INIS)

    Oertel, J. A.; Archuleta, T. N.

    2014-01-01

    Microchannel plate (MCP), microstrip transmission line based, gated x-ray detectors used at the premier ICF laser facilities have a drop in gain as a function of mircostrip length that can be greater than 50% over 40 mm. These losses are due to ohmic losses in a microstrip coating that is less than the optimum electrical skin depth. The electrical skin depth for a copper transmission line at 3 GHz is 1.2 μm while the standard microstrip coating thickness is roughly half a single skin depth. Simply increasing the copper coating thickness would begin filling the MCP pores and limit the number of secondary electrons created in the MCP. The current coating thickness represents a compromise between gain and ohmic loss. We suggest a novel solution to the loss problem by overcoating the copper transmission line with five electrical skin depths (∼6 μm) of Beryllium. Beryllium is reasonably transparent to x-rays above 800 eV and would improve the carrier current on the transmission line. The net result should be an optically flat photocathode response with almost no measurable loss in voltage along the transmission line

  10. Accounting for thermodynamic non-ideality in the Guinier region of small-angle scattering data of proteins.

    Science.gov (United States)

    Scott, David J

    2016-12-01

    Hydrodynamic studies of the solution properties of proteins and other biological macromolecules are often hard to interpret when the sample is present at a reasonably concentrated solution. The reason for this is that solutions exhibit deviations from ideal behaviour which is manifested as thermodynamic non-ideality. The range of concentrations at which this behaviour typically is exhibited is as low as 1-2 mg/ml, well within the range of concentrations used for their analysis by techniques such as small-angle scattering. Here we discuss thermodynamic non-ideality used previously used in the context of light scattering and sedimentation equilibrium analytical ultracentrifugation and apply it to the Guinier region of small-angle scattering data. The results show that there is a complementarity between the radially averaged structure factor derived from small-angle X-ray scattering/small-angle neutron scattering studies and the second virial coefficient derived from sedimentation equilibrium analytical ultracentrifugation experiments.

  11. Small angle X-ray scattering-based elucidation of the self-association mechanism of human insulin analogue lys(B29)(N(e)¿-carboxyheptadecanoyl) des(B30)

    DEFF Research Database (Denmark)

    Jensen, Malene Hillerup; Wahlund, Per-Olof; Toft, Katrine Nørgaard

    2013-01-01

    of biophysical and structural methods (field flow fractionation, dynamic and multiangle light scattering, circular dichroism, size exclusion chromatography, and crystallography), we propose a mechanism for the self-association expected to occur upon subcutaneous injection of this insulin analogue. SAXS data...... provide evidence of the in solution structure of the self-associated oligomer, which is a long straight rod composed of "tense" state insulin hexamers (T(6)-hexamers) as the smallest repeating unit. The smallest oligomer building block in the process is a T(6)T(6)-dihexamer. This tense dihexamer is formed...... by the allosteric change of the initial equilibrium between a proposed "relaxed" state R(6)-hexamer and an R(3)T(3)T(3)R(3)-dihexamer. The allosteric change from relaxed to tense is triggered by removal of phenol, mimicking subcutaneous injection. The data hence provide the first unequivocal evidence...

  12. Thorium determination by x-ray fluorescence spectrometry in simulated thorex process solutions

    International Nuclear Information System (INIS)

    Yamaura, M.; Matsuda, H.T.

    1991-11-01

    The X-ray fluorescence method for thorium determination in aqueous and organic (TBP/n-dodecane) solutions is described. The thin film technique for sample preparation and a suitable internal standard had been used. The best conditions for Thorium determination had been established studying some parameters as analytical line, internal standard, filter paper, paper geometry, sample volume and measurement conditions. With the established conditions, thorium was concentration range of to 200 g Th/L and in organic solutions (2-63g Th/L) with 1,5% of precision. The accuracy of the proposed method was 3% in aqueous and organic phases. The detection limit was 1,2μg thorium for aqueous solutions and 1,4μg for organic solutions. Uranium, fission products, corrosion products and Thorex reagent components were studied as interfering elements in the thorium analysis. The matrix effect was also studied using the Thorex process simulated solutions. Finally, the method was applied to thorium determination in irradiated thorium solutions with satisfactory results. (author)

  13. Redox-Phen solution: A water equivalent dosimeter for UVA, UVB and X-rays radiation

    Science.gov (United States)

    Marini, A.; Ciribolla, C.; Lazzeri, L.; d'Errico, F.

    2018-06-01

    Polysulphone films are the only type of UV passive dosimeters that are widely adopted for research and personal monitoring. Even though many studies concentrated on the development and characterization of these films, they still present some shortcomings. The more important limitations of them are that they can measure only UVB radiations and that they change color at 330 nm, requiring special equipment to read them. To overcome these limitations we developed an aqueous dosimeter that is sensitive to UVA, UVB and X-rays named Redox-Phen solution. This dosimeter is inexpensive and water equivalent, being made of more than 99 wt% of water. It changes color in the visible region upon irradiation, thus it can be measured via simple optical method, and an evaluation of the exposition can be made also by naked eyes.

  14. K-edge x-ray fluorescence analysis for actinide and heavy elements solution concentration measurements

    International Nuclear Information System (INIS)

    Camp, D.C.

    1984-07-01

    Advantages of using Co-57 as an exciter for K XRFA include: a compact design that requires no x-ray tubes; the exciter-detector assembly locates remote from support electronics; on-line, at-line, or off-line configurations for monitor/measurements; systems that can be run by semi-skilled technicians, once programmed; and operated via remote terminals with results sent to control rooms; heavy element concentrations that are measurable thru industrial pipes; independent of minor changes in solution matrix or source half life with concentration results reported in near-real-time; a dynamic range of measurable concentrations that is greater than 10 4 ; measurement times that are reasonable even at 1 gram/liter; and for nuclear safeguards, it provides the <0.5% accuracy required by DOE for the accountability of U, Pu, or both, once the system is calibrated

  15. Double crystal X-ray analysis of phosphorus precipitation in supersaturated Si-P solid solutions

    International Nuclear Information System (INIS)

    Servidori, M.; Zini, Q.; Dal Monte, C.

    1983-01-01

    The physical nature of the electrically inactive phosphorus in silicon is investigated by double crystal X-ray diffraction measurements. This analysis is performed on laser annealed supersaturated samples, doped by ion implantation up to 5 x 10 21 cm -3 . After isothermal heat treatments, these solid solutions show marked reductions in the electrically active phosphorus concentration. In particular, 850 0 C heatings give rise to a carrier concentration which corresponds to the phosphorus solubility in equilibrium with the inactive dopant. This dopant is characterized by means of lattice strain measurements: they are found consistent with the presence of perfectly coherent cubic SiP precipitates. This result is in agreement with the one obtained in preceeding works by electrical measurements and transmission electron microscopy observations and contradicts the hypothesis that the excess dopant atoms are, at least in part, charged point defects (E-centres). (author)

  16. Quaternary structure of human, Drosophila melanogaster and Caenorhabditis elegans MFE-2 in solution from synchrotron small-angle X-ray scattering.

    Science.gov (United States)

    Mehtälä, Maija L; Haataja, Tatu J K; Blanchet, Clément E; Hiltunen, J Kalervo; Svergun, Dmitri I; Glumoff, Tuomo

    2013-02-14

    Multifunctional enzyme type 2 (MFE-2) forms part of the fatty acid β-oxidation pathway in peroxisomes. MFE-2s from various species reveal proteins with structurally homologous functional domains assembled in different compilations. Crystal structures of all domain types are known. SAXS data from human, fruit fly and Caenorhabditiselegans MFE-2s and their constituent domains were collected, and both ab initio and rigid body models constructed. Location of the putative substrate binding helper domain SCP-2L (sterol carrier protein 2-like), which is not part of MFE-2 protein in every species and not seen as part of any previous MFE-2 structures, was determined. The obtained models of human and C. elegans MFE-2 lend a direct structural support to the idea of the biological role of SCP-2L. Copyright © 2013 Federation of European Biochemical Societies. Published by Elsevier B.V. All rights reserved.

  17. Astrophysical parameters and orbital solution of the peculiar X-ray transient IGR J00370+6122

    Science.gov (United States)

    González-Galán, A.; Negueruela, I.; Castro, N.; Simón-Díaz, S.; Lorenzo, J.; Vilardell, F.

    2014-06-01

    Context. BD + 60° 73 is the optical counterpart of the X-ray source IGR J00370+6122, a probable accretion-powered X-ray pulsar. The X-ray light curve of this binary system shows clear periodicity at 15.7 d, which has been interpreted as repeated outbursts around the periastron of an eccentric orbit. Aims: We aim to characterise the binary system IGR J00370+6122 by deriving its orbital and physical parameters. Methods: We obtained high-resolution spectra of BD + 60° 73 at different epochs. We used the fastwind code to generate a stellar atmosphere model to fit the observed spectrum and obtain physical magnitudes. The synthetic spectrum was used as a template for cross-correlation with the observed spectra to measure radial velocities. The radial velocity curve provided an orbital solution for the system. We also analysed the RXTE/ASM and Swift/BAT light curves to confirm the stability of the periodicity. Results: BD + 60° 73 is a BN0.7 Ib low-luminosity supergiant located at a distance ~3.1 kpc, in the Cas OB4 association. We derive Teff = 24 000 K and log gc = 3.0, and chemical abundances consistent with a moderately high level of evolution. The spectroscopic and evolutionary masses are consistent at the 1-σ level with a mass M∗ ≈ 15 M⊙. The recurrence time of the X-ray flares is the orbital period of the system. The neutron star is in a high-eccentricity (e = 0.56 ± 0.07) orbit, and the X-ray emission is strongly peaked around orbital phase φ = 0.2, though the observations are consistent with some level of X-ray activity happening at all orbital phases. Conclusions: The X-ray behaviour of IGR J00370+6122 is reminiscent of "intermediate" supergiant X-ray transients, though its peak luminosity is rather low. The orbit is somewhat wider than those of classical persistent supergiant X-ray binaries, which when combined with the low luminosity of the mass donor, explains the low X-ray luminosity. IGR J00370+6122 will very likely evolve towards a persistent

  18. Small angle neutron scattering

    International Nuclear Information System (INIS)

    Bernardini, G.; Cherubini, G.; Fioravanti, A.; Olivi, A.

    1976-09-01

    A method for the analysis of the data derived from neutron small angle scattering measurements has been accomplished in the case of homogeneous particles, starting from the basic theory without making any assumption on the form of particle size distribution function. The experimental scattering curves are interpreted with the aid the computer by means of a proper routine. The parameters obtained are compared with the corresponding ones derived from observations at the transmission electron microscope

  19. X-ray L/sub III/-edge densitometer for assay of mixed S.N.M. solutions

    International Nuclear Information System (INIS)

    Russo, P.A.; Canada, T.R.; Langner, D.G.; Tape, J.W.; Hsue, S.T.; Cowder, L.R.; Mosley, W.C.; Reynolds, L.; Thompson, M.C.

    1979-01-01

    Simultaneous nondestructive analysis of uranium and plutonium in coprocessed solutions is accomplished using L/sub III/-edge densitometry in at-line instrumentation. The densitometer measures the transmission through solutions of a continuous x-ray spectrum, and gives accuracies of approximately one-half percent and three percent for uranium and plutonium concentrations respectively

  20. 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,

  1. Study on the management of the Boohung X-Dol 90 developer and fixing solution for automatic X-ray film processor

    International Nuclear Information System (INIS)

    Hyan, Yong Sil; Kim, Heung Tae; Kwon, Dal Gwan; Choi, Myung Joon; Cheung, Hwan

    1986-01-01

    Recently, Demands of Automatic X-ray film Processors are increasing more and more at University Hospitals and general Hospitals and Private clinics, but various troubles because of incorrect control were found out. Authors have researched to find out the function and Activity of Automatic X-ray film processor for 2 weeks Kodak RPX-OMAT Processor and Sakura GX3000 Processor and Doosan parka 2000 Processor and results obtained were as follows: 1. Automatic X-ray film processor have an advantage to conduct the rapid treatment of X-ray film processing but incorrect handling of developing and fixing agents were brought about a great change in Contrast and Optical density of X-ray film pictures. 2. About 300 X-ray film could be finished by same developing and fixing solution without exchanging any other solutions in each Automatic X-ray film processor

  2. Structure solution from powder neutron and x-ray diffraction data: getting the best of both worlds

    International Nuclear Information System (INIS)

    Hunter, B.A.

    2000-01-01

    Full text: Powder diffraction methods have traditionally been used in three main areas: phase identification and quantification, lattice parameter determination and structure refinement. Until recently structure solution has been the almost exclusive domain of single crystal diffraction methods, predominantly using x-rays. The increasing use of synchrotron and neutron sources, and the unrelenting advances in computing hardware and software means that powder methods are challenging single crystal methods as a practical method for structure solution, especially when single crystal method can not be applied. It is known that structural refinements from a known starting structure using combined X-ray and neutron data sets are capable of providing highly accurate structures. Likewise, using combined x-ray and neutron powder diffraction data in the structure solution process should also be a powerful technique, although to date no one is pursuing this methodology. This paper present examples of solutions to the problem. Namely we are using high resolution powder X-ray and neutron methods to solve the structures of molecular materials and minerals, then refining the structures using both sets of data. In this way we exploit the advantages of both methods while minimising the disadvantages. We present our solution for a small amino acid structure, a metalorganic and a mineral structure

  3. X-ray imager using solution processed organic transistor arrays and bulk heterojunction photodiodes on thin, flexible plastic substrate

    NARCIS (Netherlands)

    Gelinck, G.H.; Kumar, A.; Moet, D.; Steen, J.L. van der; Shafique, U.; Malinowski, P.E.; Myny, K.; Rand, B.P.; Simon, M.; Rütten, W.; Douglas, A.; Jorritsma, J.; Heremans, P.L.; Andriessen, H.A.J.M.

    2013-01-01

    We describe the fabrication and characterization of large-area active-matrix X-ray/photodetector array of high quality using organic photodiodes and organic transistors. All layers with the exception of the electrodes are solution processed. Because it is processed on a very thin plastic substrate

  4. Study of the solid solution formation in mixed oxides by X-ray diffraction

    International Nuclear Information System (INIS)

    Riella, H.G.

    1984-01-01

    A method to determine the plutonium distribution in mixed oxides - UO 2 /PuO 2 is described. The distribution function and the medium size of crystallite are obtained from the X-ray diffraction profile. Through the deconvolution by Fourier analysis, the X-ray diffraction profile is obtained without the influence of the difractrometer. Some experimental results for different samples of UO 2 -PuO 2 discussed. (Author) [pt

  5. X-ray absorption studies of graphite intercalates and metal-ammonia solutions

    International Nuclear Information System (INIS)

    Robertson, A.S.

    1979-09-01

    X-ray absorption spectroscopy (XAS) was used to study the arsenic fluorocomplexes, including the AsF 5 and AsF 6 - intercalates of graphite, and rubidium metal-ammonia solutions. The As-F distances obtained for AsF 3 and AsF 5 gas are both in excellent agreement with electron diffraction data (within 0.004 A). A superior measurement which is significantly shorter than the accepted value of the bond distance in an undistorted AsF 6 - octahedra is reported. Both the XAES and EXAFS data presented support the hypothesis that the AsF 5 oxidizes graphite upon intercalation to produce AsF 6 - and AsF 3 intercalant species. Changes in the Rb K-edge features which are consistent with the known properties of Rb-NH 3 are correlated with conductivity and delocalization of the solvated electrons. In the XAES region, intensity and position changes of absorption transitions are explained. In the EXAFS region, the Rb-N bond distance and the relative number of nitrogen atoms in the first shell are measured. XAS has been shown to provide unique information about the nature of the metal-ammonia phase separation, phase transition, and density fluctuations

  6. Closed-form solution for the Wigner phase-space distribution function for diffuse reflection and small-angle scattering in a random medium.

    Science.gov (United States)

    Yura, H T; Thrane, L; Andersen, P E

    2000-12-01

    Within the paraxial approximation, a closed-form solution for the Wigner phase-space distribution function is derived for diffuse reflection and small-angle scattering in a random medium. This solution is based on the extended Huygens-Fresnel principle for the optical field, which is widely used in studies of wave propagation through random media. The results are general in that they apply to both an arbitrary small-angle volume scattering function, and arbitrary (real) ABCD optical systems. Furthermore, they are valid in both the single- and multiple-scattering regimes. Some general features of the Wigner phase-space distribution function are discussed, and analytic results are obtained for various types of scattering functions in the asymptotic limit s > 1, where s is the optical depth. In particular, explicit results are presented for optical coherence tomography (OCT) systems. On this basis, a novel way of creating OCT images based on measurements of the momentum width of the Wigner phase-space distribution is suggested, and the advantage over conventional OCT images is discussed. Because all previous published studies regarding the Wigner function are carried out in the transmission geometry, it is important to note that the extended Huygens-Fresnel principle and the ABCD matrix formalism may be used successfully to describe this geometry (within the paraxial approximation). Therefore for completeness we present in an appendix the general closed-form solution for the Wigner phase-space distribution function in ABCD paraxial optical systems for direct propagation through random media, and in a second appendix absorption effects are included.

  7. Small Angle Neutron Scattering Studies of the Counterion Effects on the Molecular Conformation and Structure of Charged G4 PAMAM Dendrimers in Aqueous Solutions

    International Nuclear Information System (INIS)

    Chen, Wei-Ren

    2007-01-01

    The structural properties of generation 4 (G4) poly(amidoamine) starburst dendrimers (PAMAM) with an ethylenediamine ne (EDA) central core in D O 2 solutions have been studied by small angle neutron scattering. Upon the addition of DCl , SANS patterns show a pronounced inter-particle 2 correlation peaks due to the strong repulsion introduced by the protonation of the amino groups of the dendrimers. By solving the Ornstein-Zernike integral equation (OZ) with hypernetted chain closure (HNC), the dendrimer-dendrimer er structure factor S(Q) is determined and used to fit the experimental data. Quantitative information such as the effective charge per dendrimer and its conformational change at different conditions can be obtained. The results obtained show clear evidence that significant counterion association occurs, strongly mediating the inter-dendrimer interaction. The influence of interplay between counterions and molecular protonation of dendrimers has strong effect on the dendrimer conformation and effective interaction.

  8. Characterization of Nanoparticles and Colloids in Aquatic Systems 1. Small Angle Neutron Scattering Investigations of Suwannee River Fulvic Acid Aggregates in Aqueous Solutions

    International Nuclear Information System (INIS)

    Diallo, Mamadou S.; Glinka, Charles J.; Goddard, William A.; Johnson, James H.

    2005-01-01

    Fulvic acids (FA) and humic acids (HA) constitute 30-50% of dissolved organic matter in natural aquatic systems. In aqueous solutions, a commonly accepted view is that FA and HA exist as soluble macroligands at low concentration and as supramolecular aggregates at higher concentration. The size, shape and structure of these aggregates are still the subject of ongoing debate in the environmental chemistry literature. In this article, we use small angle neutron scattering (SANS) to assess the effects of solute concentration, solution pH and background electrolyte (NaCl) concentration on the structures of Suwannee River FA (SRFA) aggregates in D 2 O. The qualitative features of the SANS curves and data analysis are not consistent with the view point that SRFA forms micelle-like aggregates as its concentration in aqueous solution increases. We find that SRFA forms fractal aggregates in D 2 0 with size greater than 242 nm. The SRFA aggregates undergo a significant degree of restructuring in compactness as solution pH, solute concentration and NaCl concentration increase

  9. Electronic structure and optical properties of CdS{sub x}Se{sub 1−x} solid solution nanostructures from X-ray absorption near edge structure, X-ray excited optical luminescence, and density functional theory investigations

    Energy Technology Data Exchange (ETDEWEB)

    Murphy, M. W. [DESY (Deutsches Elektronen-Synchrotron), FS-PEX, Notkestrasse 85, 22607 Hamburg (Germany); Yiu, Y. M., E-mail: yyiu@uwo.ca; Sham, T. K. [Department of Chemistry, University of Western Ontario, London, ON N6A5B7 (Canada); Ward, M. J. [Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY 14853 (United States); Liu, L. [Institute of Functional Nano and Soft Materials (FUNSOM) and Soochow University-Western University Center for Synchrotron Radiation Research, Soochow University, Suzhou, Jiangsu, 215123 (China); Hu, Y. [Canadian Light Source, University of Saskatchewan, Saskatoon, SK S7N2V3 (Canada); Zapien, J. A. [Center Of Super-Diamond and Advanced Films (COSDAF) and Department of Physics and Materials Science, City University of Hong Kong, Hong Kong SAR (China); Liu, Yingkai [Institute of Physics and Electronic Information, Yunnan Normal University, Kunming, Yunnan, 650500 (China)

    2014-11-21

    The electronic structure and optical properties of a series of iso-electronic and iso-structural CdS{sub x}Se{sub 1−x} solid solution nanostructures have been investigated using X-ray absorption near edge structure, extended X-ray absorption fine structure, and X-ray excited optical luminescence at various absorption edges of Cd, S, and Se. It is found that the system exhibits compositions, with variable local structure in-between that of CdS and CdSe accompanied by tunable optical band gap between that of CdS and CdSe. Theoretical calculation using density functional theory has been carried out to elucidate the observations. It is also found that luminescence induced by X-ray excitation shows new optical channels not observed previously with laser excitation. The implications of these observations are discussed.

  10. X-ray diffraction

    International Nuclear Information System (INIS)

    Vries, J.L. de.

    1976-01-01

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

  11. Calibration of X-ray densitometers for the determination of uranium and plutonium concentrations in reprocessing input and product solutions

    International Nuclear Information System (INIS)

    Ottmar, H.; Eberle, H.; Michel-Piper, I.; Kuhn, E.; Johnson, E.

    1985-11-01

    In June 1985 a calibration exercise has been carried out, which included the calibration of the KfK K-Edge Densitometer for uranium assay in the uranium product solutions from reprocessing, and the calibration of the Hybrid K-Edge/K-XRF Instrument for the determination of total uranium and plutonium in reprocessing input solutions. The calibration measuremnts performed with the two X-ray densitometers are described and analyzed, and calibration constants are evaluated from the obtained results. (orig.)

  12. In-Situ Synchrotron X-ray Study of the Phase and Texture Evolution of Ceria and Superconductor Films Deposited by Chemical Solution Method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; He, Dong

    2012-01-01

    In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry/differential ther......In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry...

  13. On the microstructure of organic solutions of mono-carboxylic acids: Combined study by infrared spectroscopy, small-angle neutron scattering and molecular dynamics simulations

    Energy Technology Data Exchange (ETDEWEB)

    Eremin, Roman A., E-mail: era@jinr.ru [Joint Institute for Nuclear Research, Dubna 141980 (Russian Federation); Kholmurodov, Kholmirzo T. [Joint Institute for Nuclear Research, Dubna 141980 (Russian Federation); International University “Dubna”, Dubna 141980 (Russian Federation); Petrenko, Viktor I. [Joint Institute for Nuclear Research, Dubna 141980 (Russian Federation); Taras Shevchenko National University of Kyiv, Kyiv 03022 (Ukraine); Rosta, László [Wigner Research Centre for Physics, Hungarian Academy of Sciences, Budapest H-1525 (Hungary); Grigoryeva, Natalia A. [Faculty of Physics, Saint-Petersburg State University, 198504 Saint-Petersburg (Russian Federation); Avdeev, Mikhail V. [Joint Institute for Nuclear Research, Dubna 141980 (Russian Federation)

    2015-11-05

    Highlights: • The model of the scattering particle for a reliable SANS analysis is proposed. • The structural parameters of saturated mono-carboxylic acids in solutions are obtained. • The differences in nematic transitions correlate to solvation peculiarities. - Abstract: The data of infrared spectroscopy (IR), molecular dynamics (MD) simulations and small-angle neutron scattering (SANS) have been combined to conclude about the nanoscale structural organization of organic non-polar solutions of saturated mono-carboxylic acids with different alkyl chain lengths for diluted solutions of saturated myristic (C14) and stearic (C18) acids in benzene and decalin. In particular, the degree of dimerization was found from the IR spectra. The structural anisotropy of the acids and their dimers was used in the treatment of the data of MD simulations to describe the solute–solvent interface in a cylindrical approximation and show its rather strong influence on SANS. The corresponding scattering length density profiles were used to fit the experimental SANS data comprising the information about the acid molecule isomerization. The SANS data from concentrated solutions showed a partial self-assembling of the acids within the nematic transition is different for two solvents due to lyophobic peculiarities.

  14. Structural and phase transition changes of sodium dodecyl sulfate micellar solution in alcohols probed by small-angle neutron scattering (SANS)

    Energy Technology Data Exchange (ETDEWEB)

    Putra, Edy Giri Rachman [Neutron Scattering Laboratory, National Nuclear Energy Agency of Indonesia (BATAN), Gedung 40 BATAN, Kawasan Puspiptek Serpong, Tangerang 15314 (Indonesia); Patriati, Arum [Neutron Scattering Laboratory, National Nuclear Energy Agency of Indonesia (BATAN), Gedung 40 BATAN, Kawasan Puspiptek Serpong, Tangerang 15314 (Indonesia); Department of Chemistry, Faculty of Mathematics and Natural Sciences, University of Gadjah Mada, Bulaksumur, Yogyakarta 55281, Indonesia giri@batan.go.id (Indonesia)

    2015-04-16

    Small-angle neutron scattering (SANS) measurements on 0.3M sodium dodecyl sulfate (SDS) micellar solutions have been performed in the presence of n-alcohols, from ethanol to decanol at different alcohol concentrations, 2–10 wt%. The ellipsoid micellar structure which occurred in the 0.3M SDS in aqueous solution with the size range of 30–50 Å has different behavior at various hydrocarbon chain length and concentration of alcohols. At low concentration and short chain-length of alcohols, such as ethanol, propanol, and butanol, the size of micelles reduced and had a spherical-like structure. The opposite effect occurred as medium to long chain alcohols, such as hexanol, octanol and decanol was added into the 0.3M SDS micellar solutions. The micelles structure changed to be more elongated in major axis and then crossed the critical phase transition from micellar solution into liquid crystal phase as lamellar structure emerged by further addition of alcohols. The inter-lamellar distances were also depending on the hydrocarbon chain length and concentration of alcohols. In the meantime, the persistent micellar structures occurred in addition of medium chain of n-alcohol, pentanol at all concentrations.

  15. Structural and phase transition changes of sodium dodecyl sulfate micellar solution in alcohols probed by small-angle neutron scattering (SANS)

    International Nuclear Information System (INIS)

    Putra, Edy Giri Rachman; Patriati, Arum

    2015-01-01

    Small-angle neutron scattering (SANS) measurements on 0.3M sodium dodecyl sulfate (SDS) micellar solutions have been performed in the presence of n-alcohols, from ethanol to decanol at different alcohol concentrations, 2–10 wt%. The ellipsoid micellar structure which occurred in the 0.3M SDS in aqueous solution with the size range of 30–50 Å has different behavior at various hydrocarbon chain length and concentration of alcohols. At low concentration and short chain-length of alcohols, such as ethanol, propanol, and butanol, the size of micelles reduced and had a spherical-like structure. The opposite effect occurred as medium to long chain alcohols, such as hexanol, octanol and decanol was added into the 0.3M SDS micellar solutions. The micelles structure changed to be more elongated in major axis and then crossed the critical phase transition from micellar solution into liquid crystal phase as lamellar structure emerged by further addition of alcohols. The inter-lamellar distances were also depending on the hydrocarbon chain length and concentration of alcohols. In the meantime, the persistent micellar structures occurred in addition of medium chain of n-alcohol, pentanol at all concentrations

  16. Small angle neutron scattering

    Directory of Open Access Journals (Sweden)

    Cousin Fabrice

    2015-01-01

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

  17. Observation of glassy state relaxation during annealing of frozen sugar solutions by X-ray computed tomography.

    Science.gov (United States)

    Nakagawa, Kyuya; Tamiya, Shinri; Do, Gabsoo; Kono, Shinji; Ochiai, Takaaki

    2018-06-01

    Glassy phase formation in a frozen product determines various properties of the freeze-dried products. When an aqueous solution is subjected to freezing, a glassy phase forms as a consequence of freeze-concentration. During post-freezing annealing, the relaxation of the glassy phase and the ripening of ice crystals (i.e. Ostwald ripening) spontaneously occur, where the kinetics are controlled by the annealing and glass transition temperatures. This study was motivated to observe the progress of glassy state relaxation separate from ice coarsening during annealing. X-ray computed tomography (CT) was used to observe a frozen and post-freezing annealed solutions by using monochromatized X-ray from the synchrotron radiation. CT images were successfully obtained, and the frozen matrix were analyzed based on the gray level values that were equivalent to the linear X-ray attenuation coefficients of the observed matters. The CT images obtained from rapidly frozen sucrose and dextrin solutions with different concentrations gave clear linear relationships between the linear X-ray attenuation coefficients values and the solute concentrations. It was confirmed that the glassy state relaxation progressed as increasing annealing time, and this trend was larger in the order of the glass transition temperature of the maximally freeze-concentrated phase. The sucrose-water system required nearly 20 h of annealing time at -5 °C for the completion of the glassy phase relaxation, whereas dextrin-water systems required much longer periods because of their higher glass transition temperatures. The trends of ice coarsening, however, did not perfectly correspond to the trends of the relaxation, suggesting that the glassy phase relaxation and Ostwald ripening would jointly control the ice crystal growth/ripening kinetics, and the dominant mechanism differed by the annealing stage. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Determination of zinc in ammoniacal ore leaching solutions by X-ray fluorescence spectrometry using a radioactive source

    International Nuclear Information System (INIS)

    Cornejo, N.; Afailal, A.; Garcia, F.; Palacios, M.

    1994-01-01

    A method was developed for the fast determination of zinc in leaching solutions by radioisotope energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The measured intensities were used to develop regression models for estimating the zinc concentration. The primary radiation was provided by the 244 Cm radioisotope. Several experimental parameters including the saturation thickness and detection limit were determined. The advantages of the utilization of conditioning agents with elements of low atomic number such as nitric acid were established. (orig.)

  19. Interparticle interactions and structure in nonideal solutions of human serum albumin studied by small-angle neutron scattering and Monte Carlo simulation

    DEFF Research Database (Denmark)

    Sjöberg, B.; Mortensen, K.

    1994-01-01

    of human serum albumin (HSA) up to a concentration of 0.26 g/cm(3) in 1.08 M NaCl. In order to obtain a model for the interactions we have combined the SANS data with results obtained by Monte Carlo simulations where we calculate the structure factor S(Q) and the pair correlation function g......Moderately or highly concentrated nonideal solutions of macromolecules are very important systems e.g. in biology and in many technical processes. In this work we have used the small-angle neutron scattering technique (SANS) to study the interactions and interparticle structure in solutions......(r). The advantage of using the Monte Carlo method is that completely general models for the particle shape and the interactions can be considered. It is found that the SANS data can be explained by a model where the shape of the HSA molecule is approximated by an ellipsoid of revolution with semiaxes a = 6.8 nm...

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  1. Probing the influence of X-rays on aqueous copper solutions using time-resolved in situ combined video/X-ray absorption near-edge/ultraviolet-visible spectroscopy

    NARCIS (Netherlands)

    Mesu, J. Gerbrand; Beale, Andrew M.; de Groot, Frank M. F.; Weckhuysen, Bert M.

    2006-01-01

    Time-resolved in situ video monitoring and ultraviolet-visible spectroscopy in combination with X-ray absorption near-edge spectroscopy (XANES) have been used for the first time in a combined manner to study the effect of synchrotron radiation on a series of homogeneous aqueous copper solutions in a

  2. Trace elemental analysis of leaching solutions of hijiki seaweeds by a portable total reflection X-ray fluorescence spectrometer

    International Nuclear Information System (INIS)

    Liu, Ying; Imashuku, Susumu; Kawai, Jun

    2014-01-01

    A portable total reflection X-ray fluorescence spectrometer (TXRF) was used to analyze leaching solutions of hijiki seaweeds. S, Cl, K, Ca, Ti, Fe, Ni, As and Br were detected in the solutions. Arsenic quantification results were compared to those from ICP-AES. The TXRF quantification results of arsenic were not significantly different from those of ICP-AES, as two-way analysis of variance (ANOVA) method was applied to the significance test. This kind of small and high sensitive TXRF spectrometer can be used in food quality and environmental pollution investigation. (author)

  3. Soft X-ray absorption spectra of aqueous salt solutions with highly charged cations in liquid microjets

    Energy Technology Data Exchange (ETDEWEB)

    Schwartz, Craig P.; Uejio, Janel S.; Duffin, Andrew M.; Drisdell, Walter S.; Smith, Jared D.; Saykally, Richard J.

    2010-03-11

    X-ray absorption spectra of 1M aqueous solutions of indium (III) chloride, yttrium (III) bromide, lanthanum (III) chloride, tin (IV) chloride and chromium (III) chloride have been measured at the oxygen K-edge. Relatively minor changes are observed in the spectra compared to that of pure water. SnCl{sub 4} and CrCl{sub 3} exhibit a new onset feature which is attributed to formation of hydroxide or other complex molecules in the solution. At higher energy, only relatively minor, but salt-specific changes in the spectra occur. The small magnitude of the observed spectral changes is ascribed to offsetting perturbations by the cations and anions.

  4. X-ray absorption spectroscopic study of trivalent and tetravalent actinides in solution at varying pH values

    Energy Technology Data Exchange (ETDEWEB)

    Brendebach, B.; Banik, N.L.; Marquardt, C.M.; Rothe, J.; Denecke, M.A.; Geckeis, H. [Forschungszentrum Karlsruhe (Germany). Inst. fuer Nukleare Entsorgung

    2009-07-01

    We perform X-ray absorption spectroscopy (XAS) investigations to monitor the stabilization of redox sensitive trivalent and tetravalent actinide ions in solution at acidic conditions in a pH range from 0 to 3 after treatment with holding reductants, hydroxylamine hydrochloride (NH{sub 2}OHHCl) and Rongalite (sodium hydroxymethanesulfinate, CH{sub 3}NaO{sub 3}S). X-ray absorption near edge structure (XANES) measurements clearly demonstrate the stability of the actinide species for several hours under the given experimental conditions. Hence, structural parameters can be accurately derived by extended X-ray absorption fine structure (EXAFS) investigations. The coordination structure of oxygen atoms belonging to water ligands surrounding the actinide ions does not change with increasing pH value (approximately 11 O atoms at 2.42 A in the case of U(IV) at pH 1, 9 0 atoms at 2.52 A for Np(III) at pH 1.5, and 10 O atoms at 2.49 A for Pu(III) up to pH 3), indicating that hydrolysis reactions are suppressed under the given chemical conditions. (orig.)

  5. A new cell for temperature-dependent X-ray absorption spectroscopy of liquid solutions: application to PbBr2 solutions in diethylene glycol.

    Science.gov (United States)

    Lützenkirchen-Hecht, D; Oldag, T; Keil, P; Keller, H L; Frahm, R

    2005-03-01

    An in situ cell has been constructed for temperature-dependent X-ray absorption experiments (EXAFS and XANES) of lead bromine (PbBr2) solutions in diethylene glycol in the temperature range from room temperature up to about 433 K. The solution is kept in a thermostated container made of carbon-reinforced teflon between two thin chemically inert quartz glass windows with a high transmission for hard X-rays. The construction of the cell ensures that these X-ray windows are thermalized so that any possible precipitation of solid products from the solution is inhibited. The cell consists mainly of two hermetically sealed teflon containers for the thermostating fluid (silicon oil) that were fitted together in such a way that a small and variable volume (approximately 2-4 cm3) for the liquid under investigation was achieved. A small thermocouple in a glass enclosure was placed in the solution to maintain temperature control and feedback to the thermostat. The cell design and its performance for temperature-dependent in situ investigations with X-rays are reported. Some preliminary results obtained for PbBr2 solutions in diethylene glycol are given.

  6. Simulation of small-angle scattering patterns using a CPU-efficient algorithm

    Science.gov (United States)

    Anitas, E. M.

    2017-12-01

    Small-angle scattering (of neutrons, x-ray or light; SAS) is a well-established experimental technique for structural analysis of disordered systems at nano and micro scales. For complex systems, such as super-molecular assemblies or protein molecules, analytic solutions of SAS intensity are generally not available. Thus, a frequent approach to simulate the corresponding patterns is to use a CPU-efficient version of the Debye formula. For this purpose, in this paper we implement the well-known DALAI algorithm in Mathematica software. We present calculations for a series of 2D Sierpinski gaskets and respectively of pentaflakes, obtained from chaos game representation.

  7. Structure in defocused beams of x-ray mirrors: causes and possible solutions

    Science.gov (United States)

    Sutter, John P.; Alcock, Simon G.; Rust, Fiona; Wang, Hongchang; Sawhney, Kawal

    2014-09-01

    Grazing incidence mirrors are now a standard optic for focusing X-ray beams. Both bimorph and mechanically bendable mirrors are widely used at Diamond Light Source because they permit a wide choice of focal lengths. They can also be deliberately set out of focus to enlarge the X-ray beam, and indeed many beamline teams now wish to generate uniform beam spots of variable size. However, progress has been slowed by the appearance of fine structure in these defocused beams. Measurements showing the relationship between the medium-frequency polishing error and this structure over a variety of beam sizes will be presented. A theoretical model for the simulations of defocused beams from general mirrors will then be developed. Not only the figure error and its first derivative the slope error, but also the second derivative, the curvature error, must be considered. In conclusion, possible ways to reduce the defocused beam structure by varying the actuators' configuration and settings will be discussed.

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

  9. Study of an X-ray fluorescence thin film method for the determination of uranium in low activity solutions

    International Nuclear Information System (INIS)

    Diaz-Guerra, J. P.

    1980-01-01

    The application of the X-ray fluorescence thin film technique to the uranium determination in nitric solutions for a concentration range from 1 g/l to 100 g/l and activity levels under 5 mCi/ml is studied. The most suited excitation and measurement conditions are also studied and the uranium matrix effect correction, which is performed through the double dilution, α U U interaction coefficient calculation and internal standard methods, is discussed. The specimen preparation is satisfactorily accomplished by using P.V.C. filters fixed on aluminium supports. (Author) 18 refs

  10. Induced alignment of a solution-cast discotic hexabenzocoronene derivative for electronic devices investigated by surface X-ray diffraction

    DEFF Research Database (Denmark)

    Bunk, Oliver; Nielsen, Martin Meedom; Sølling, Theis Ivan

    2003-01-01

    A surface X-ray diffraction study is presented showing that highly ordered and uniaxially aligned hexa(3,7-dimethyl-octanyl)hexa-peri-hexabenzocoronene (HBC-C8,2) films can be fabricated by crystallization from solution onto friction-transferred poly(tetrafluoroethylene) (PTFE) layers. Three...... crystalline HBC-C8,2 majority phases result. In all three phases, the HBC-C8,2 molecules self-organize into columns which are uniaxially aligned along the direction defined by the PTFE macromolecules of the substrate. The three phases are quite similar, the major difference being their orientation...

  11. Calculation of X-ray scattering curves and electron distance distribution functions of biological macromolecules in solution using the PROTEIN DATA BANK

    International Nuclear Information System (INIS)

    Mueller, J.J.; Friedrichowicz, E.; Nothnagel, A.; Wunderlich, T.; Ziehlsdorf, E.; Damaschun, G.

    1983-01-01

    The wide angle X-ray scattering curve, the electron distance distribution function and the solvent excluded volume of a macromolecule in solution are calculated from the atomic coordinates contained in the PROTEIN DATA BANK. The structures and the projections of the excluded volumes are depicted using molecule graphic routines. The described computer programs are used to determine the three-dimensional structure of macromolecules in solution from wide angle X-ray scattering data. (author)

  12. Small-angle scattering in materials science

    International Nuclear Information System (INIS)

    Paris, O.; Fratzl, P.

    1999-01-01

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

  13. Using acoustic levitation in synchrotron based laser pump hard x-ray probe experiments

    Science.gov (United States)

    Hu, Bin; Lerch, Jason; Suthar, Kamlesh; Dichiara, Anthony

    Acoustic levitation provides a platform to trap and hold a small amount of material by using standing pressure waves without a container. The technique has a potential to be used for laser pump x-ray probe experiments; x-ray scattering and laser distortion from the container can be avoided, sample consumption can be minimized, and unwanted chemistry that may occur at the container interface can be avoided. The method has been used at synchrotron sources for studying protein and pharmaceutical solutions using x-ray diffraction (XRD) and small angle x-ray scattering (SAXS). However, pump-probe experiments require homogeneously excited samples, smaller than the absorption depth of the material that must be held stably at the intersection of both the laser and x-ray beams. We discuss 1) the role of oscillations in acoustic levitation and the optimal acoustic trapping conditions for x-ray/laser experiments, 2) opportunities to automate acoustic levitation for fast sample loading and manipulation, and 3) our experimental results using SAXS to monitor laser induced thermal expansion in gold nanoparticles solution. We also performed Finite Element Analysis to optimize the trapping performance and stability of droplets ranging from 0.4 mm to 2 mm. Our early x-ray/laser demonstrated the potential of the technique for time-resolved X-ray science.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  15. Small-angle neutron scattering in materials science

    International Nuclear Information System (INIS)

    Fratzl, P.

    1999-01-01

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

  16. High-temperature x-ray diffraction study of HfTiO4-HfO2 solid solutions

    International Nuclear Information System (INIS)

    Carpenter, D.A.

    1975-01-01

    High-temperature x-ray diffraction techniques were used to determine the axial thermal expansion curves of HfTiO 4 -HfO 2 solid solutions as a function of composition. Data show increasing anisotropy with increasing HfO 2 content. An orthorhombic-to-monoclinic phase transformation was detected near room temperature for compositions near the high HfO 2 end of the orthorhombic phase field and for compositions within the two-phase region (HfTiO 4 solid solution plus HfO 2 solid solution). An orthorhombic-to-cubic phase transformation is indicated by data from oxygen-deficient materials at greater than 1873 0 K. (U.S.)

  17. Red mercuric iodide crystals obtained by isothermal solution evaporation: Characterization for mammographic X-ray imaging detectors

    Energy Technology Data Exchange (ETDEWEB)

    Caldeira, A.M.F.; Ugucioni, J.C.; Mulato, M.

    2014-02-11

    Millimeter-sized mercury iodide crystals were obtained by the isothermal evaporation technique using dimethylformamide (DMF), diethyl-ether/DMF mixture and THF. Different concentrations (18 mM and 400 mM) and solution temperature (25–80 °C) were used to obtain varied evaporation rates (0.1×10{sup −4}–5000×10{sup −4} ml/h). Different crystal sizes and shapes were obtained by changing solvents, mixture and initial solution volume. According to X-ray diffraction the samples are monocrystalline. The top surface was investigated by SEM. Optical band-gaps above 2 eV were obtained from photoacoustic spectroscopy. Photoluminescence spectra indicated band-to-band electronic transitions, and the presence of sub-band gap states. Excitons, structural defects and the presence of impurities are discussed and correlated to the electrical measurements. Crystals obtained using pure DMF as solvent showed better general properties, including under the exposure to mammographic X-ray energy range that led to sensibility of about 25 μC/Rcm{sup 2}.

  18. Synthesis of a colloid solution of silica-coated gold nanoparticles for X-ray imaging applications

    Science.gov (United States)

    Kobayashi, Yoshio; Nagasu, Ryoko; Shibuya, Kyosuke; Nakagawa, Tomohiko; Kubota, Yohsuke; Gonda, Kohsuke; Ohuchi, Noriaki

    2014-08-01

    This work proposes a method for fabricating silica-coated gold (Au) nanoparticles, surface modified with poly(ethylene glycol) (PEG) (Au/SiO2/PEG), with a particle size of 54.8 nm. X-ray imaging of a mouse is performed with the colloid solution. A colloid solution of 17.9 nm Au nanoparticles was prepared by reducing Au ions (III) with sodium citrate in water at 80 °C. The method used for silica-coating the Au nanoparticles was composed of surface-modification of the Au nanoparticles with (3-aminopropyl)-trimethoxysilane (APMS) and a sol-gel process. The sol-gel process was performed in the presence of the surface-modified Au nanoparticles using tetraethylorthosilicate, APMS, water, and sodium hydroxide, in which the formation of silica shells and the introduction of amino groups to the silica-coated particles took place simultaneously (Au/SiO2-NH2). Surface modification of the Au/SiO2-NH2 particles with PEG, or PEGylation of the particle surface, was performed by adding PEG with a functional group that reacted with an amino group in the Au/SiO2-NH2 particle colloid solution. A computed tomography (CT) value of the aqueous colloid solution of Au/SiO2/PEG particles with an actual Au concentration of 0.112 M was as high as 922 ± 12 Hounsfield units, which was higher than that of a commercial X-ray contrast agent with the same iodine concentration. Injecting the aqueous colloid solution of Au/SiO2/PEG particles into a mouse increased the light contrast of tissues. A CT value of the heart rose immediately after the injection, and this rise was confirmed for up to 6 h.

  19. Skull x-ray

    Science.gov (United States)

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

  20. Neck x-ray

    Science.gov (United States)

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  2. X-ray CT-Derived Soil Characteristics Explain Varying Air, Water, and Solute Transport Properties across a Loamy Field

    DEFF Research Database (Denmark)

    Paradelo Pérez, Marcos; Katuwal, Sheela; Møldrup, Per

    2016-01-01

    -derived parameters by using a best subsets regression analysis. The regression coefficients improved using CTmatrix, limiting macroporosity, and genus density, while the best model for t0.05 used CTmatrix only. The scanning resolution and the time for soil structure development after mechanical activities could......The characterization of soil pore space geometry is important for explaining fluxes of air, water, and solutes through soil and understanding soil hydrogeochemical functions. X-ray computed tomography (CT) can be applied for this characterization, and in this study CT-derived parameters were used...... to explain water, air, and solute transport through soil. Forty-five soil columns (20 by 20 cm) were collected from an agricultural field in Estrup, Denmark, and subsequently scanned using a medical CT scanner. Nonreactive tracer leaching experiments were performed in the laboratory along with measurements...

  3. A study on the structure of thorium salt solutions

    International Nuclear Information System (INIS)

    Magini, M.; Cabrini, A.; Di Bartolomeo, A.

    1975-01-01

    The structure of highly hydrolyzed thorium salt solutions has been investigated by large and small angle X-ray scattering techniques. The diffraction data obtained with large angle measurements show the presence in solution of microcrystalline particles with the thorium oxide structure. Particles larger than those were discovered by small angle measurements. A possible shape of these colloidal particles has been discussed

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

    Science.gov (United States)

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

    2010-05-01

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

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

    CERN Document Server

    Benediktovitch, Andrei; Ulyanenkov, Alexander

    2013-01-01

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

  6. Structure of Profiled Crystals Based on Solid Solutions of Bi2Te3 and Their X-Ray Diagnostics

    Science.gov (United States)

    Voronin, A. I.; Bublik, V. T.; Tabachkova, N. Yu.; Belov, Yu. M.

    2011-05-01

    In this work, we used x-ray structural diagnostic data to reveal the formation of structural regularities in profiled polycrystalline ingots based on Bi and Sb chalcogenide solid solutions. In Bi2Te3 lattice crystals, the solid phase grows such that the cleavage surfaces are perpendicular to the crystallization front. The crystallization singularity determines the nature of the growth texture. Because texture is an important factor determining the anisotropy of properties, which in turn determines the suitability of an ingot for production of modules and the possibility of figure of merit improvement, its diagnostics is an important issue for technology testing. Examples of texture analysis using the method of straight pole figure (SPF) construction for profiled crystals are provided. The structure of the surface layers in the profiled ingots was studied after electroerosion cutting. In addition, the method of estimation of the disturbed layer depth based on the nature of texture changes was used.

  7. X-ray imaging with toroidal mirror

    International Nuclear Information System (INIS)

    Aoki, Sadao; Sakayanagi, Yoshimi

    1978-01-01

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

  8. Exact and approximate solutions for the one-dimensional transfer of polarized radiation, and applications to X-ray pulsars

    International Nuclear Information System (INIS)

    Meszaros, P.; Nagel, W.; Ventura, J.

    1979-11-01

    Theoretical studies of the radiation from hot, strongly magnetized plasmas, as encountered in pulsars, require a knowledge of solutions to the transfer equations for polarized radiation. We present here an analytic solution of the radiative transfer equations for one-dimensional propagation across a homogeneous slab of finite depth, as well as for a semi-infinite atmosphere. Absorption, scattering and mode-exchange between the two polarizations is included, the role of this latter being crucial. A physical discussion of the solutions for certain limiting cases, and an interpretation in terms of probabilistic (quantum escape approach) arguments, fully corrobrates these solutions, and provides a better intuitive feel for the behaviour of the radiated spectra. Whereas our analytic solutions are valid for any birefringent medium (not necessarily magnetic), our numerical examples and the qualitative discussion presented refer to the particular problem of the radiation from X-ray pulsars. Large scale qualitative changes from the nonmagnetic spectra aae found, which affect both the continum and the spectral lines. (orig.) 891 WL/orig. 892 RDG

  9. X-ray diffraction phase analysis of crystalline copper corrosion products after treatment in different chloride solutions

    International Nuclear Information System (INIS)

    Chmielova, M.; Seidlerova, J.; Weiss, Z.

    2003-01-01

    The corrosion products Cu 2 (OH) 3 Cl, Cu 2 O, and CuCl 2 were identified on the surface of copper plates after their four days treating in three different sodium chloride, sodium/magnesium, and sodium/calcium chloride solutions using X-ray diffraction powder analysis. However, the quantitative proportions of individual corrosion products differ and depend on the type of chloride solution used. Treating of copper plates only in the sodium chloride solution produced the mixture of corrosion products where Cu 2 O is prevailing over the Cu 2 (OH) 3 Cl and CuCl 2 was not identified. The sample developed after treating of the cooper surface in the sodium/magnesium chloride solution contains Cu 2 (OH) 3 Cl and CuCl 2 prevailing over the Cu 2 O, while the sample developed after treatment of copper in sodium/calcium chloride solution contains Cu 2 (OH) 3 Cl prevailing over CuCl 2 and Cu 2 O was not identified

  10. Fitness function and nonunique solutions in x-ray reflectivity curve fitting: crosserror between surface roughness and mass density

    International Nuclear Information System (INIS)

    Tiilikainen, J; Bosund, V; Mattila, M; Hakkarainen, T; Sormunen, J; Lipsanen, H

    2007-01-01

    Nonunique solutions of the x-ray reflectivity (XRR) curve fitting problem were studied by modelling layer structures with neural networks and designing a fitness function to handle the nonidealities of measurements. Modelled atomic-layer-deposited aluminium oxide film structures were used in the simulations to calculate XRR curves based on Parratt's formalism. This approach reduced the dimensionality of the parameter space and allowed the use of fitness landscapes in the study of nonunique solutions. Fitness landscapes, where the height in a map represents the fitness value as a function of the process parameters, revealed tracks where the local fitness optima lie. The tracks were projected on the physical parameter space thus allowing the construction of the crosserror equation between weakly determined parameters, i.e. between the mass density and the surface roughness of a layer. The equation gives the minimum error for the other parameters which is a consequence of the nonuniqueness of the solution if noise is present. Furthermore, the existence of a possible unique solution in a certain parameter range was found to be dependent on the layer thickness and the signal-to-noise ratio

  11. X-ray diffraction study on the structure of concentrated aqueous solutions involving alanine molecules with different optical activities

    International Nuclear Information System (INIS)

    Kameda, Yasuo; Okuyama, Aya; Amo, Yuko; Usuki, Takeshi; Kohara, Shinji

    2007-01-01

    X-ray diffraction measurements on aqueous 2.5 mol% DL-, L-, and D-alanine solutions in D 2 O were carried out at 26±2degC in order to obtain information concerning the difference in the hydrogen-bonded structure between aqueous solutions involving amino acid molecules with different optical activities. The difference function, Δi inter (Q), between intermolecular interference term observed for DL- and L-alanine and between DL- and D-alanine solutions both exhibited a first peak at Q=1.6 A -1 , followed by oscillatory features extending to higher-Q region, implying that there is a difference in the intermolecular structure is present between these solutions. The difference distribution function, Δg inter (r), obtained from the Fourier transform of the Δi inter (Q) between DL- and L-, and between DL- and D-alanine solutions showed an obvious negative peak at r=2.8 A, which was attributed to the nearest neighbor hydrogen-bonded O...O interaction. The least squares fitting analysis of the observed Δi inter (Q) showed that the intermolecular O...O distance and the difference in the coordination number between DL- and L-, and between DL- and D-alanine solutions are 2.76(2) A and -0.18(1), and 2.81(3) A and -0.18(1), respectively. It was concluded that the intermolecular hydrogen-bonded network in aqueous L- and D-alanine solutions is stronger than that in the DL-alanine solution. (author)

  12. Simultaneous use of solution NMR and X-ray data in REFMAC5 for joint refinement/detection of structural differences

    Energy Technology Data Exchange (ETDEWEB)

    Rinaldelli, Mauro; Ravera, Enrico; Calderone, Vito; Parigi, Giacomo [University of Florence, Via L. Sacconi 6, 50019 Sesto Fiorentino (Finland) (Italy); University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino (Finland) (Italy); Murshudov, Garib N., E-mail: garib@mrc-lmb.cam.ac.uk [MRC Laboratory of Molecular Biology, Francis Crick Avenue, Cambridge Biomedical Campus, Cambridge CB2 0QH (United Kingdom); Luchinat, Claudio, E-mail: garib@mrc-lmb.cam.ac.uk [University of Florence, Via L. Sacconi 6, 50019 Sesto Fiorentino (Finland) (Italy); University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino (Finland) (Italy)

    2014-04-01

    Paramagnetic NMR data (pseudocontact shifts and self-orientation residual dipolar couplings) and diamagnetic residual dipolar couplings can now be used in the program REFMAC5 from CCP4 as structural restraints together with X-ray crystallographic data. These NMR restraints can reveal differences between solid state and solution conformations of molecules or, in their absence, can be used together with X-ray crystallographic data for structural refinement. The program REFMAC5 from CCP4 was modified to allow the simultaneous use of X-ray crystallographic data and paramagnetic NMR data (pseudocontact shifts and self-orientation residual dipolar couplings) and/or diamagnetic residual dipolar couplings. Incorporation of these long-range NMR restraints in REFMAC5 can reveal differences between solid-state and solution conformations of molecules or, in their absence, can be used together with X-ray crystallographic data for structural refinement. Since NMR and X-ray data are complementary, when a single structure is consistent with both sets of data and still maintains reasonably ‘ideal’ geometries, the reliability of the derived atomic model is expected to increase. The program was tested on five different proteins: the catalytic domain of matrix metalloproteinase 1, GB3, ubiquitin, free calmodulin and calmodulin complexed with a peptide. In some cases the joint refinement produced a single model consistent with both sets of observations, while in other cases it indicated, outside the experimental uncertainty, the presence of different protein conformations in solution and in the solid state.

  13. Simultaneous use of solution NMR and X-ray data in REFMAC5 for joint refinement/detection of structural differences

    International Nuclear Information System (INIS)

    Rinaldelli, Mauro; Ravera, Enrico; Calderone, Vito; Parigi, Giacomo; Murshudov, Garib N.; Luchinat, Claudio

    2014-01-01

    Paramagnetic NMR data (pseudocontact shifts and self-orientation residual dipolar couplings) and diamagnetic residual dipolar couplings can now be used in the program REFMAC5 from CCP4 as structural restraints together with X-ray crystallographic data. These NMR restraints can reveal differences between solid state and solution conformations of molecules or, in their absence, can be used together with X-ray crystallographic data for structural refinement. The program REFMAC5 from CCP4 was modified to allow the simultaneous use of X-ray crystallographic data and paramagnetic NMR data (pseudocontact shifts and self-orientation residual dipolar couplings) and/or diamagnetic residual dipolar couplings. Incorporation of these long-range NMR restraints in REFMAC5 can reveal differences between solid-state and solution conformations of molecules or, in their absence, can be used together with X-ray crystallographic data for structural refinement. Since NMR and X-ray data are complementary, when a single structure is consistent with both sets of data and still maintains reasonably ‘ideal’ geometries, the reliability of the derived atomic model is expected to increase. The program was tested on five different proteins: the catalytic domain of matrix metalloproteinase 1, GB3, ubiquitin, free calmodulin and calmodulin complexed with a peptide. In some cases the joint refinement produced a single model consistent with both sets of observations, while in other cases it indicated, outside the experimental uncertainty, the presence of different protein conformations in solution and in the solid state

  14. Inverse planning for x-ray rotation therapy: a general solution of the inverse problem

    International Nuclear Information System (INIS)

    Oelfke, U.; Bortfeld, T.

    1999-01-01

    Rotation therapy with photons is currently under investigation for the delivery of intensity modulated radiotherapy (IMRT). An analytical approach for inverse treatment planning of this radiotherapy technique is described. The inverse problem for the delivery of arbitrary 2D dose profiles is first formulated and then solved analytically. In contrast to previously applied strategies for solving the inverse problem, it is shown that the most general solution for the fluence profiles consists of two independent solutions of different parity. A first analytical expression for both fluence profiles is derived. The mathematical derivation includes two different strategies, an elementary expansion of fluence and dose into polynomials and a more practical approach in terms of Fourier transforms. The obtained results are discussed in the context of previous work on this problem. (author)

  15. SoftWAXS: a computational tool for modeling wide-angle X-ray solution scattering from biomolecules.

    Science.gov (United States)

    Bardhan, Jaydeep; Park, Sanghyun; Makowski, Lee

    2009-10-01

    This paper describes a computational approach to estimating wide-angle X-ray solution scattering (WAXS) from proteins, which has been implemented in a computer program called SoftWAXS. The accuracy and efficiency of SoftWAXS are analyzed for analytically solvable model problems as well as for proteins. Key features of the approach include a numerical procedure for performing the required spherical averaging and explicit representation of the solute-solvent boundary and the surface of the hydration layer. These features allow the Fourier transform of the excluded volume and hydration layer to be computed directly and with high accuracy. This approach will allow future investigation of different treatments of the electron density in the hydration shell. Numerical results illustrate the differences between this approach to modeling the excluded volume and a widely used model that treats the excluded-volume function as a sum of Gaussians representing the individual atomic excluded volumes. Comparison of the results obtained here with those from explicit-solvent molecular dynamics clarifies shortcomings inherent to the representation of solvent as a time-averaged electron-density profile. In addition, an assessment is made of how the calculated scattering patterns depend on input parameters such as the solute-atom radii, the width of the hydration shell and the hydration-layer contrast. These results suggest that obtaining predictive calculations of high-resolution WAXS patterns may require sophisticated treatments of solvent.

  16. DMSO-Water Clustering in Solution Observed in Soft X-ray Spectra.

    Science.gov (United States)

    Engel, Nicholas; Atak, Kaan; Lange, Kathrin M; Gotz, Malte; Soldatov, Mikhail; Golnak, Ronny; Suljoti, Edlira; Rubensson, Jan-Erik; Aziz, Emad F

    2012-12-20

    The significant deviation from the ideality of dimethyl sulfoxide (DMSO)/water mixtures can be addressed based on the change of the local molecular orbitals of each solvent upon mixing. Oxygen K-edge absorption and emission spectra of DMSO/water solutions were measured using the liquid microjet technique. The spectra demonstrate that the hydrogen bond network in liquid water is already influenced at small DMSO concentrations, and at the molar fraction xDMSO = 0.43 we find strong evidence of DMSO-water clustering reflected by the influence on the occupied molecular orbitals.

  17. Real-time x-ray response of biocompatible solution gate AlGaN/GaN high electron mobility transistor devices

    International Nuclear Information System (INIS)

    Hofstetter, Markus; Funk, Maren; Paretzke, Herwig G.; Thalhammer, Stefan; Howgate, John; Sharp, Ian D.; Stutzmann, Martin

    2010-01-01

    We present the real-time x-ray irradiation response of charge and pH sensitive solution gate AlGaN/GaN high electron mobility transistors. The devices show stable and reproducible behavior under and following x-ray radiation, including a linear integrated response with dose into the μGy range. Titration measurements of devices in solution reveal that the linear pH response and sensitivity are not only retained under x-ray irradiation, but an irradiation response could also be measured. Since the devices are biocompatible, and can be simultaneously operated in aggressive fluids and under hard radiation, they are well-suited for both medical radiation dosimetry and biosensing applications.

  18. Microrheology of polymeric solutions using x-ray photon correlation spectroscopy

    International Nuclear Information System (INIS)

    Papagiannopoulos, A; Waigh, T A; Fluerasu, A; Fernyhough, C; Madsen, A

    2005-01-01

    We demonstrate the technique of XPCS microrheology on opaque polymeric solutions (1-20% w/w) using colloidal silica probes. The short time decay of the intensity correlation function provides the mean square displacement (MSD) of the colloidal probes. The MSDs of the probes are subsequently transformed using the generalized Stokes-Einstein equation, allowing the linear viscoelastic spectra of a biopolymer (gellan) and a synthetic polyelectrolyte (polystyrene sulfonate, PSS) to be calculated over two decades of frequency. MSDs can be measured that are two orders of magnitude smaller than those possible with video particle tracking microrheology, with a sensitivity of ∼10 nm s -1 for displacements of ∼nms. The XPCS data for water, glycerol and PSS combs are in agreement with video particle tracking microrheology experiments performed at lower polymer concentrations. (letter to the editor)

  19. X-Ray

    Science.gov (United States)

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

  20. Abdominal x-ray

    Science.gov (United States)

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

  1. Chest X-Ray

    Medline Plus

    Full Text Available ... talk with you about chest radiography also known as chest x-rays. Chest x-rays are the ... treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray ...

  2. Anomalous small-angle scattering as a way to solve the Babinet principle problem

    International Nuclear Information System (INIS)

    Boiko, M. E.; Sharkov, M. D.; Boiko, A. M.; Bobyl, A. V.

    2013-01-01

    X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions

  3. Anomalous small-angle scattering as a way to solve the Babinet principle problem

    Energy Technology Data Exchange (ETDEWEB)

    Boiko, M. E., E-mail: m.e.boiko@mail.ioffe.ru; Sharkov, M. D.; Boiko, A. M.; Bobyl, A. V. [Russian Academy of Sciences, Ioffe Physicotechnical Institute (Russian Federation)

    2013-12-15

    X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

  4. Anomalous small-angle scattering as a way to solve the Babinet principle problem

    Science.gov (United States)

    Boiko, M. E.; Sharkov, M. D.; Boiko, A. M.; Bobyl, A. V.

    2013-12-01

    X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

  5. X-ray astronomy

    International Nuclear Information System (INIS)

    Giacconi, R.; Gursky, H.

    1974-01-01

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

  6. Conformation and arrangement of polyelectrolytes in semi-diluted solution. A study by small angle neutrons scattering; Conformation et arrangement des polyelectrolytes en solution semi-diluee. Etude par diffusion des neutrons aux petits angles

    Energy Technology Data Exchange (ETDEWEB)

    Spiteri, M N

    1997-03-25

    Polyelectrolytes have particular physical and chemical properties and can thus be used for instance for petroleum production. Some of their microscopic properties have been studied in this work. With the particular zero average contrast technique, the small angle neutron scattering allows to directly know the form factors in semi-diluted solutions of polyelectrolytes where the chains are mixed. Another measure leads to the crystal structure. The electrostatic screen effects when salt is added in aqueous solutions of completely charged PSSNa solutions (f=1) (sodium polystyrene sulfonate) are studied. It seems that the chains take a vermiform conformation. Their persistence length varies as I{sup -1/3} (I is the ionic force). The hydrophobicity effects in partially charged PSSNa solutions (f<1) are given too. They lead to a progressive collapse of the chains when their charge rates decrease. The screen and condensation effects when the charge rate f of the PSSNa (f>f(Manning)) varies in a polar solvent (DMSO) are studied. The vermiform chains have the same persistence length (for each f) which varies as I{sup -1/4}. Lastly, the f variation effects in the case of a weakly charged hydrophilic poly-ion (f

  7. Small-angle neutron scattering studies of sodium butyl benzene

    Indian Academy of Sciences (India)

    Na-NBBS), in aqueous solutions is investigated by small-angle neutron scattering (SANS). Nearly ellipsoidal aggregates of Na-NBBS at concentrations well above its minimum hydrotrope concentration were detected by SANS. The hydrotrope ...

  8. Small angle scattering and polymers

    International Nuclear Information System (INIS)

    Cotton, J.P.

    1996-01-01

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

  9. Crystalline self-assembly of organic molecules with metal ions at the air-aqueous solution interface. A grazing incidence X-ray scattering study

    DEFF Research Database (Denmark)

    Weissbuch, I.; Buller, R.; Kjær, K.

    2002-01-01

    The advent of intense X-rays from synchrotron sources made possible to probe, at the molecular level, the structural aspects of self-assemblies generated at interfaces. Here we present the two-dimensional (2-D) packing arrangements of two-, three- and multi-component organo-metallic self......-assemblies formed via interfacial reaction at the air-aqueous solution interface, as determined by grazing incidence X-ray diffraction (GIRD) and X-ray specular reflectivity techniques. GIXD yields structural information on the crystalline part of the Langmuir film, including the ions and counterions lateral order...... of metal ions bound to the polar head groups of amphipilic molecules; use of bolaamphiphiles to generate oriented thin films with metal ions arranged in periodic layers; delineation of differences in the lateral organization of metal ions at interfaces as induced by racemates and enantiomerically pure...

  10. The structure of normal ionic micelles by interpretation of small-angle neutron scattering data from selectively labeled (2H, 19F) surfactant solutions

    International Nuclear Information System (INIS)

    Berr, S.S.

    1986-12-01

    We have determined the structure of micelles formed in water by several classes of ionic surfactants under a variety of experimental conditions using small-angle neutron scattering (SANS) techniques. Contrast between the micelles and the solvent was achieved through either selective deuteration or fluorination of the surfactant, or through the use of D 2 O. Interpretation of SANS data was facilitated by the use of Hayter, Penfold, and Hansen's rescaled Mean Spherical Approximation theory to calculate the scattering due to interparticle interactions. We have devised a number of micelle models, both spherical and ellipsoidal, to account for the scattering due to single micelles. It was found that changing the solvent from H 2 O to D 2 O results in the formation of larger micelles due to changes in the solvent-surfactant hydrocarbon interactions. This solvent isotope effect increased as the length of the alkyl chain increased. The fractional micellar charge did not change with respect to isotopic composition of solvent. We found that alkyltrimethylammonium bromide surfactants form drier micelles than do the sodium alkyl sulfate surfactants of equal chain length. Also, all micelles studied were found to be dry near the critical micelle concentration (cmc) and to become increasingly wetter as the concentration increased. The increase in aggregation number with respect to the square root of surfactant concentration was found to be linear for all systems studied. 80 figs

  11. Determination of the structure of the organized phase of the block copolymer PEO-PPO-PEO in aqueous solutions under flow by small-angle neutron scattering

    International Nuclear Information System (INIS)

    Perreur, Christelle; Habas, Jean-Pierre; Francois, Jeanne; Peyrelasse, Jean; Lapp, Alain

    2002-01-01

    The organization of Tetronic 908 registered (T908), a star copolymer of poly(ethylene oxide) (PEO) and poly(propylene oxide) (PPO) blocks, has been examined. Above critical conditions of temperature and concentration, the micelles formed by the aggregation of PPO units self-organize into particular structures. While small-angle neutron scattering (SANS) characterizations performed with static conditions demonstrate the organization of the medium, the experimental results do not allow us to make a distinction between simple cubic and body-centered-cubic structures. However, SANS measurements realized under shear produce characteristic diffraction diagrams. In this paper, an accurate methodology is proposed to identify, without ambiguity, the exact nature of the organized phase. Applied to our system, indexing of the diffraction pattern spots reveals that the organization of T908 is of bcc type oriented with the [111] direction parallel to the direction of flow, but the crystals can present any orientation about this direction. The lattice size has been estimated and compared to previous published results

  12. Acemetacin cocrystals and salts: structure solution from powder X-ray data and form selection of the piperazine salt

    Directory of Open Access Journals (Sweden)

    Palash Sanphui

    2014-03-01

    Full Text Available Acemetacin (ACM is a non-steroidal anti-inflammatory drug (NSAID, which causes reduced gastric damage compared with indomethacin. However, acemetacin has a tendency to form a less soluble hydrate in the aqueous medium. We noted difficulties in the preparation of cocrystals and salts of acemetacin by mechanochemical methods, because this drug tends to form a hydrate during any kind of solution-based processing. With the objective to discover a solid form of acemetacin that is stable in the aqueous medium, binary adducts were prepared by the melt method to avoid hydration. The coformers/salt formers reported are pyridine carboxamides [nicotinamide (NAM, isonicotinamide (INA, and picolinamide (PAM], caprolactam (CPR, p-aminobenzoic acid (PABA, and piperazine (PPZ. The structures of an ACM–INA cocrystal and a binary adduct ACM–PABA were solved using single-crystal X-ray diffraction. Other ACM cocrystals, ACM–PAM and ACM–CPR, and the piperazine salt ACM–PPZ were solved from high-resolution powder X-ray diffraction data. The ACM–INA cocrystal is sustained by the acid...pyridine heterosynthon and N—H...O catemer hydrogen bonds involving the amide group. The acid...amide heterosynthon is present in the ACM–PAM cocrystal, while ACM–CPR contains carboxamide dimers of caprolactam along with acid–carbonyl (ACM hydrogen bonds. The cocrystals ACM–INA, ACM–PAM and ACM–CPR are three-dimensional isostructural. The carboxyl...carboxyl synthon in ACM–PABA posed difficulty in assigning the position of the H atom, which may indicate proton disorder. In terms of stability, the salts were found to be relatively stable in pH 7 buffer medium over 24 h, but the cocrystals dissociated to give ACM hydrate during the same time period. The ACM–PPZ salt and ACM–nicotinamide cocrystal dissolve five times faster than the stable hydrate form, whereas the ACM–PABA adduct has 2.5 times faster dissolution rate. The pharmaceutically acceptable

  13. Acemetacin cocrystals and salts: structure solution from powder X-ray data and form selection of the piperazine salt.

    Science.gov (United States)

    Sanphui, Palash; Bolla, Geetha; Nangia, Ashwini; Chernyshev, Vladimir

    2014-03-01

    Acemetacin (ACM) is a non-steroidal anti-inflammatory drug (NSAID), which causes reduced gastric damage compared with indomethacin. However, acemetacin has a tendency to form a less soluble hydrate in the aqueous medium. We noted difficulties in the preparation of cocrystals and salts of acemetacin by mechanochemical methods, because this drug tends to form a hydrate during any kind of solution-based processing. With the objective to discover a solid form of acemetacin that is stable in the aqueous medium, binary adducts were prepared by the melt method to avoid hydration. The coformers/salt formers reported are pyridine carboxamides [nicotinamide (NAM), isonicotinamide (INA), and picolinamide (PAM)], caprolactam (CPR), p-aminobenzoic acid (PABA), and piperazine (PPZ). The structures of an ACM-INA cocrystal and a binary adduct ACM-PABA were solved using single-crystal X-ray diffraction. Other ACM cocrystals, ACM-PAM and ACM-CPR, and the piperazine salt ACM-PPZ were solved from high-resolution powder X-ray diffraction data. The ACM-INA cocrystal is sustained by the acid⋯pyridine heterosynthon and N-H⋯O catemer hydrogen bonds involving the amide group. The acid⋯amide heterosynthon is present in the ACM-PAM cocrystal, while ACM-CPR contains carboxamide dimers of caprolactam along with acid-carbonyl (ACM) hydrogen bonds. The cocrystals ACM-INA, ACM-PAM and ACM-CPR are three-dimensional isostructural. The carboxyl⋯carboxyl synthon in ACM-PABA posed difficulty in assigning the position of the H atom, which may indicate proton disorder. In terms of stability, the salts were found to be relatively stable in pH 7 buffer medium over 24 h, but the cocrystals dissociated to give ACM hydrate during the same time period. The ACM-PPZ salt and ACM-nicotinamide cocrystal dissolve five times faster than the stable hydrate form, whereas the ACM-PABA adduct has 2.5 times faster dissolution rate. The pharmaceutically acceptable piperazine salt of acemetacin exhibits superior

  14. X-ray fluorescence determination of Sn, Sb, Pb in lead-based bearing alloys using a solution technique

    Science.gov (United States)

    Tian, Lunfu; Wang, Lili; Gao, Wei; Weng, Xiaodong; Liu, Jianhui; Zou, Deshuang; Dai, Yichun; Huang, Shuke

    2018-03-01

    For the quantitative analysis of the principal elements in lead-antimony-tin alloys, directly X-ray fluorescence (XRF) method using solid metal disks introduces considerable errors due to the microstructure inhomogeneity. To solve this problem, an aqueous solution XRF method is proposed for determining major amounts of Sb, Sn, Pb in lead-based bearing alloys. The alloy samples were dissolved by a mixture of nitric acid and tartaric acid to eliminated the effects of microstructure of these alloys on the XRF analysis. Rh Compton scattering was used as internal standard for Sb and Sn, and Bi was added as internal standard for Pb, to correct for matrix effects, instrumental and operational variations. High-purity lead, antimony and tin were used to prepare synthetic standards. Using these standards, calibration curves were constructed for the three elements after optimizing the spectrometer parameters. The method has been successfully applied to the analysis of lead-based bearing alloys and is more rapid than classical titration methods normally used. The determination results are consistent with certified values or those obtained by titrations.

  15. X-ray study of CuGa sub x In sub 1-x Se sub 2 solid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Suri, D.K.; Nagpal, K.C. (National Physical Lab., New Delhi (India). Materials Characterization Div.); Chadha, G.K. (Delhi Univ. (India). Dept. of Physics and Astrophysics)

    1989-12-01

    The semiconducting compound CuGa{sub x}In{sub 1-x}Se{sub 2} crystallizes in the chalcopyrite structure (space group Ianti 42d, Z=4). The X-ray powder data for x=1, 0.75, 0.6, 0.5, 0.4, 0.25 and 0.0 have been collected and it is found that the lattice parameters a and c and their ratio c/a vary linearly with x. Thus the composition of any chalcopyrite in the pseudo-binary system CuGaSe{sub 2} and CuInSe{sub 2} can be obtained from the accurate lattice parameters. The crystallite size determined from the (112) plane is minimum for x=0.50 ({proportional to}1000 A) and away from x=0.50 it increases. A value of u=0.240 (5) has been established for fixing, the Se-atom positions in the CuGa{sub 0.5}In{sub 0.5}Se{sub 2} solid solution. The JCPDS Diffraction File No. for CuInSe{sub 2} is 40-1487 and for CuGa{sub 0.5}In{sub 0.5}Se{sub 2} is 40-1488. (orig.).

  16. In situ surface X-ray diffraction study of ultrathin epitaxial Co films on Au(111) in alkaline solution

    International Nuclear Information System (INIS)

    Reikowski, Finn; Maroun, Fouad; Di, Nan; Allongue, Philippe; Ruge, Martin; Stettner, Jochim; Magnussen, Olaf M.

    2016-01-01

    The oxidation behavior of ultrathin electrodeposited Co films on Au(111) in alkaline electrolyte was studied using in situ surface X-ray scattering techniques employing synchrotron radiation and complementary optical reflectivity and electrochemical measurements. The films are formed at pH 4 and consist of (001)-oriented hcp Co crystallites that are several nm high, a few ten nm in diameter, and remain largely unchanged after electrolyte exchange to pH 12 solution. In the pre-oxidation peak only minor changes were observed in the diffraction studies, excluding the formation of Co(OH)_2 layers. In the potential regime of Co hydroxide formation a rapid reduction of the amount of Co is observed, while the characteristic height of the islands decreases only slightly. On longer times scales, growth of 3D crystals of Co(OH)_2 occurs as well as irreversible Co dissolution into the electrolyte is found. On the basis of the structural observations oxidation of the Co film is proposed to proceed via fast formation of an ultrathin passivating layer, followed by nucleation and growth of 3D hydroxide crystals at the grain boundaries in the Co deposit.

  17. Quantitative Characterization of Configurational Space Sampled by HIV-1 Nucleocapsid Using Solution NMR, X-ray Scattering and Protein Engineering.

    Science.gov (United States)

    Deshmukh, Lalit; Schwieters, Charles D; Grishaev, Alexander; Clore, G Marius

    2016-06-03

    Nucleic-acid-related events in the HIV-1 replication cycle are mediated by nucleocapsid, a small protein comprising two zinc knuckles connected by a short flexible linker and flanked by disordered termini. Combining experimental NMR residual dipolar couplings, solution X-ray scattering and protein engineering with ensemble simulated annealing, we obtain a quantitative description of the configurational space sampled by the two zinc knuckles, the linker and disordered termini in the absence of nucleic acids. We first compute the conformational ensemble (with an optimal size of three members) of an engineered nucleocapsid construct lacking the N- and C-termini that satisfies the experimental restraints, and then validate this ensemble, as well as characterize the disordered termini, using the experimental data from the full-length nucleocapsid construct. The experimental and computational strategy is generally applicable to multidomain proteins. Differential flexibility within the linker results in asymmetric motion of the zinc knuckles which may explain their functionally distinct roles despite high sequence identity. One of the configurations (populated at a level of ≈40 %) closely resembles that observed in various ligand-bound forms, providing evidence for conformational selection and a mechanistic link between protein dynamics and function. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Chest X-Ray

    Medline Plus

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

  19. X-ray sky

    International Nuclear Information System (INIS)

    Gruen, M.; Koubsky, P.

    1977-01-01

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

  20. Local hydrated structure of an Fe2+/Fe3+ aqueous solution: an investigation using a combination of molecular dynamics and X-ray absorption fine structure methods

    International Nuclear Information System (INIS)

    Ye Qing; Zhou Jing; Zhao Haifeng; Chen Xing; Chu Wangsheng; Zheng Xusheng; Marcelli, Augusto; Wu Ziyu

    2013-01-01

    The hydrated shell of both Fe 2+ and Fe 3+ aqueous solutions are investigated by using the molecular dynamics (MD) and X-ray absorption structure (XAS) methods. The MD simulations show that the first hydrated shells of both Fe 2+ and Fe 3+ are characterized by a regular octahedron with an Fe-O distance of 2.08Å for Fe 2+ and 1.96Å for Fe 3+ , and rule out the occurrence of a Jahn-Teller distortion in the hydrated shell of an Fe 2+ aqueous solution. The corresponding X-ray absorption near edge fine structure (XANES) calculation successfully reproduces all features in the XANES spectra in Fe 2+ and Fe 3+ aqueous solution. A feature that is located at energy 1 eV higher than the white line (WL) in an Fe 3+ aqueous solution may be assigned to the contribution of the charge transfer. (authors)

  1. Preparation, characterization and X-ray attenuation property of Gd2O3-based nanocomposites

    Science.gov (United States)

    Jayakumar, Sangeetha; Saravanan, T.; Philip, John

    2017-11-01

    In an attempt to develop an alternate to lead-based X-ray shielding material, we describe the X-ray attenuation property of nanocomposites containing Gd2O3 as nanofiller and silicone resin as matrix, prepared by a simple solution-casting technique. Gd2O3 nanoparticles of size 30 and 56 nm are used at concentrations of 25 and 2.5 wt%. The nanoparticles and the nanocomposites are characterized using X-ray diffraction (XRD) studies, small angle X-ray spectroscopy (SAXS), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and atomic force microscopy (AFM). The X-ray attenuation property of nanocomposites, studied using an industrial X-ray unit, shows that nanocomposites containing nanoparticles of size 56 nm (G2) exhibit better attenuation than nanocomposites containing nanoparticles of size 30 nm (G1), which is attributed to the greater interfacial interaction between the G2 nanofillers and silicone matrix. In the case of nanocomposites containing G1 nanoparticles, the interfacial interaction between the nanofiller and the matrix is so weak that it results in pulling out of nanofillers, causing voids in the matrix, which act as X-ray transparent region, thereby reducing the overall X-ray attenuation property of G1 nanocomposites. This is further corroborated from the AFM images of the nanocomposites. The weight loss and heat flow curves of pure silicone matrix and the nanocomposites containing Gd2O3 nanoparticles of size 30 and 56 nm show the degradation of silicone resin, due to chain scission, between 403 and 622 °C. The same onset temperature (403 °C) of degradation of matrix with and without nanoparticles shows that the addition of nanofillers to the matrix does not deteriorate the thermal stability of the matrix. This confirms the thermal stability of nanocomposites. Therefore, our study shows that nanocomposites containing G2 nanoparticles are potential candidates for the development of X-ray opaque fabric material.

  2. Investigation of optimal manufacturing process for freeze-dried formulations: Observation of frozen solutions by low temperature X-ray diffraction measurements

    International Nuclear Information System (INIS)

    Egawa, Hiroaki; Yonemochi, Etsuo; Terada, Katsuhide

    2005-01-01

    Freeze-drying is used for the production of sterile injections in the pharmaceutical industry. However, most pharmaceutical compounds are obtained as less stable amorphous form. Freeze crystallization by annealing is an effective method for pharmaceutical compounds that fail to crystallize in the freeze-drying process. Crystallization occurs in the frozen solution during the thermal treatment. In order to establish suitable annealing conditions efficiently, it is important to observe the crystallization process directly in the frozen solution. Recently, low temperature X-ray diffraction has been used to observe frozen solutions. In order to investigate the crystallization process kinetically, the temperature of the low temperature X-ray diffraction instrument must be accurately controlled. We calibrated the temperature of X-ray diffraction instrument by measuring eutectic temperatures of solutions for a series of compounds. Each eutectic crystal was observed in frozen solution with ice crystal below the eutectic temperature. Eutectic temperatures were detected by the decrease in diffraction intensity associated with heating from below the eutectic temperature. Good correlation was obtained between values in the literature and experimental values

  3. X-ray spectroscopy results for the pristine nanosilver solution and solution after undergoing the specific usage scenario

    Data.gov (United States)

    U.S. Environmental Protection Agency — The results demonstrate the Ag 3d5/2-3/2 spectrum of the pristine AgNPs. Furthermore, the XAS spectra from the analysis of the nanosilver solution (ASAP-AGX-32)...

  4. Chest X-Ray

    Medline Plus

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

  5. Chest X-Ray

    Medline Plus

    Full Text Available ... X-ray Transcript Welcome to Radiology Info dot org! Hello, I’m Dr. Geoffrey Rubin, a radiologist ... about chest x-rays, visit Radiology Info dot org. Thank you for your time! Spotlight Recently posted: ...

  6. X-ray apparatus

    International Nuclear Information System (INIS)

    Sell, L.J.

    1981-01-01

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

  7. X-ray - skeleton

    Science.gov (United States)

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

  8. Measurement of actinide concentration in solution samples from the NUCEF reprocessing facility by X-ray and low energy gamma-ray spectroscopy

    International Nuclear Information System (INIS)

    Howarth, P.J.A.; Uchiyama, Gunzo; Asakura, Toshihide; Sawada, Mutsumi; Hagiya, Hiromichi; Fujine, Sachio

    1999-01-01

    X-ray and low-energy gamma-ray spectroscopy has been used to measure actinide concentration within the backend nuclear fuel reprocessing research facility at NUCEF. Research on advanced reprocessing techniques at NUCEF is based on the PARC refinement of the PUREX process which aims to recover Am and Cm from the highly active waste stream and to control and partition Np and Tc. It is hoped that the PARC process will mitigate the environmental impact of the wastes and improve the economy of reprocessing. The main actinides for which assay is required are U, Pu, Np and Am and knowledge of these concentrations will enable the following to be determined: i.) evaluation of the distribution of actinides throughout the reprocessing facility ii.) verification of the simulated actinide distribution from chemical kinetic simulations of the PARC process and iii.) assurance of safety and control over migrant radioactive species. The research presented here shows that passive measurement of x-rays and low-energy gamma-rays from solution samples provides an accurate and non-destructive means for assaying the concentration. The measurement technique is based on the use of the characteristic low energy gamma-rays and internal conversion x-ray emission from actinides (11 keV to 22 keV). The x-ray emission is a few orders of magnitude more intense than the characteristic gamma-ray emission and can be easily detected from solutions. The experimental system described here can be used for solution monitoring to a minimum concentration of typically 10-6 M for Pu, 10-10 M for Am and 10-6 M for Np. (author)

  9. Chest X-Ray

    Medline Plus

    Full Text Available ... I’d like to talk with you about chest radiography also known as chest x-rays. Chest x-rays are the most ... far outweighs any risk. For more information about chest x-rays, visit Radiology Info dot org. Thank you for your time! ...

  10. Chest X-Ray

    Medline Plus

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

  11. Preparation and X-ray diffraction characterization of Th1-xBixO2-0.5x (where x= 0 to 0.5) solid solutions

    International Nuclear Information System (INIS)

    Kanrar, Buddhadev; Misra, N.L.

    2015-01-01

    Solid solutions of ThO 2 and Bi 2 O 3 were prepared by solid state reactions of these oxides. X-ray diffraction studies indicated that Bi +3 up to 50 at% can be dissolved in ThO 2 lattice. Rietveld refinement of the XRD patterns indicated single phase solid solutions up to 50 atom% of Bi +3 in ThO 2 lattice. The cell parameters of the solid solutions were found to decrease with increasing amount of Bi +3 in the lattice. (author)

  12. Time-resolved X-ray scattering by electronic wave packets: analytic solutions to the hydrogen atom

    DEFF Research Database (Denmark)

    Simmermacher, Mats; Henriksen, Niels Engholm; Møller, Klaus Braagaard

    2017-01-01

    Modern pulsed X-ray sources permit time-dependent measurements of dynamical changes in atoms and molecules via non-resonant scattering. The planning, analysis, and interpretation of such experiments, however, require a firm and elaborated theoretical framework. This paper provides a detailed...... description of time-resolved X-ray scattering by non-stationary electronic wave packets in atomic systems. A consistent application of the Waller-Hartree approximation is discussed and different contributions to the total differential scattering signal are identified and interpreted. Moreover......, it is demonstrated how the scattering signal of wave packets in the hydrogen atom can be expressed analytically. This permits simulations without numerical integration and establishes a benchmark for both efficiency and accuracy. Based on that, scattering patterns of an exemplary wave packet in the hydrogen atom...

  13. Small-angle scattering study of mesoscopic structures in charged gel and their evolution on dehydration

    DEFF Research Database (Denmark)

    Sugiyama, Masaaki; Annaka, Masahiko; Hara, Kazuhiro

    2003-01-01

    Mesoscopic structures, with length scales similar to10(2) Angstrom, were investigated by small-angle X-ray and neutron scattering (SAXS and SANS) in several N-isopropylacrylamide-sodium acrylate (NIPA-SA) copolymeric hydrogels with varying [NIPA]/[SA] ratios and water contents. The SAXS experimen...

  14. Shielding chalculations in x-rays installations for medical diagnosis. description of the method and computational solution

    International Nuclear Information System (INIS)

    Borroto Valdes, M.; Saez, D.G.

    1992-01-01

    Shielding requirements for x-rays diagnostic installations are investigated. The description of an entirely analytical method for calculation of thickness, based in the papers of Simpkin and NCRP49, is presented. Considerations described in specialized method to solving this problem. A program for microcomputer IBM and compatibles ones is available for estimation of minimum shielding requirements in lead, concrete and steel. Similar results were obtained from comparing with others authors

  15. Synchrotron-based in situ soft X-ray microscopy of Ag corrosion in aqueous chloride solution

    International Nuclear Information System (INIS)

    Bozzini, B; D'Urzo, L; Gianoncelli, A; Kaulich, B; Kiskinova, M; Prasciolu, M; Tadjeddine, A

    2009-01-01

    In this paper we report an in situ X-ray microscopy study of a model metal electrochemistry system, incorporating faradaic reactivity: the anodic corrosion and cathodic electrodeposition of Ag in aqueous systems. The information at sub-μm scale about morpho-chemical evolution of the electrified interface, provided by this novel electroanalytical approach fosters fundamental understanding of important issues concerning material fabrication and stability, which are crucial in developing the next generation electrochemical technologies, such as fuel cells and biosensors. The key methodology challenge faced in this pilot electrochemical experiments is combining a three-electrode configuration and wet environment, which required metal electrodes suitable for transmitting soft X-rays and a sealed cell allowing working in high vacuum. This has been solved via lithographic fabrication route fabricating 75 nm thick Ag electrodes and using Si 3 N 4 membranes as X-ray windows and electrode support. Imaging in the STXM mode with phase contrast allowed us to monitor the corrosion morphologies and metal outgrowth features. Localised thickness variation and the build-up of reaction products of electron density different from that of the starting material have been detected with high sensitivity.

  16. Butterfly Deformation Modes in a Photoexcited Pyrazolate-Bridged Pt Complex Measured by Time-Resolved X-Ray Scattering in Solution

    DEFF Research Database (Denmark)

    Haldrup, Kristoffer; Dohn, Asmus Ougaard; Shelby, Megan L.

    2016-01-01

    the monochromatic X-ray pulses at Beamline 11IDD of the Advanced Photon Source. The excited-state structural analysis of 1 was performed based on the results from both transient WAXS measurements and density functional theory calculations to shed light on the primary structural changes in its triplet metal-metal...... excited state has remained scarce. Using time-resolved wide-angle X-ray scattering (WAXS), the excited triplet state molecular structure of [Pt(ppy)(μ-t-Bu2pz)]2 (ppy = 2-phenylpyridine; t-Bu2pz = 3,5-di-tert-butylpyrazolate), complex 1, was obtained in a dilute (0.5 mM) toluene solution utilizing...

  17. Solution Structures of Highly Active Molecular Ir Water-Oxidation Catalysts from Density Functional Theory Combined with High-Energy X-ray Scattering and EXAFS Spectroscopy.

    Science.gov (United States)

    Yang, Ke R; Matula, Adam J; Kwon, Gihan; Hong, Jiyun; Sheehan, Stafford W; Thomsen, Julianne M; Brudvig, Gary W; Crabtree, Robert H; Tiede, David M; Chen, Lin X; Batista, Victor S

    2016-05-04

    The solution structures of highly active Ir water-oxidation catalysts are elucidated by combining density functional theory, high-energy X-ray scattering (HEXS), and extended X-ray absorption fine structure (EXAFS) spectroscopy. We find that the catalysts are Ir dimers with mono-μ-O cores and terminal anionic ligands, generated in situ through partial oxidation of a common catalyst precursor. The proposed structures are supported by (1)H and (17)O NMR, EPR, resonance Raman and UV-vis spectra, electrophoresis, etc. Our findings are particularly valuable to understand the mechanism of water oxidation by highly reactive Ir catalysts. Importantly, our DFT-EXAFS-HEXS methodology provides a new in situ technique for characterization of active species in catalytic systems.

  18. Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders.

    Science.gov (United States)

    Yun, Yifeng; Zou, Xiaodong; Hovmöller, Sven; Wan, Wei

    2015-03-01

    Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED) data collection, namely automated diffraction tomography (ADT) and rotation electron diffraction (RED), have been developed. Compared with X-ray diffraction (XRD) and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD) provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni-Se-O-Cl crystals, zeolites, germanates, metal-organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional ED methods

  19. Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders

    Directory of Open Access Journals (Sweden)

    Yifeng Yun

    2015-03-01

    Full Text Available Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED data collection, namely automated diffraction tomography (ADT and rotation electron diffraction (RED, have been developed. Compared with X-ray diffraction (XRD and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni–Se–O–Cl crystals, zeolites, germanates, metal–organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three

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

    International Nuclear Information System (INIS)

    Borbely, S.; Rosta, L.

    1999-04-01

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

  1. A small-angle neutron scattering study of the structure of graphitized carbon black aggregates in Triton X-100/water solutions

    DEFF Research Database (Denmark)

    Garamus, V.M.; Pedersen, J.S.

    1998-01-01

    concentration to a lower value. The CB aggregates have a fractal structure and the apparent fractal dimension is lower near the match point (75% heavy water). The scattering data are modelled using fractal-like aggregates (CB+surfactant), and voids in the CB particles and micelles. The data are fitted...... simultaneously for three different contrasts. The fractal dimension is found to be larger than 3 with the maximum size of the fractal aggregate being around 150-200 Angstrom. The primary CB particles have a broad size distribution with an average size of about 30-80 Angstrom. The surfactant coverage of the CB...... particles is 8% and is constant with varying CB and surfactant concentration. The volume fraction of the voids does not exceed 1% of the CB; The micelle structure is found to be the same as in surfactant/water solutions. (C) 1998 Elsevier Science B.V....

  2. Flash X-ray

    International Nuclear Information System (INIS)

    Sato, Eiichi

    2003-01-01

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

  3. Condensed, solution and gas phase behaviour of mono- and dinuclear 2,6-diacetylpyridine (dap) hydrazone copper complexes probed by X-ray, mass spectrometry and theoretical calculations.

    Science.gov (United States)

    Neto, Brenno A D; Viana, Barbara F L; Rodrigues, Thyago S; Lalli, Priscila M; Eberlin, Marcos N; da Silva, Wender A; de Oliveira, Heibbe C B; Gatto, Claudia C

    2013-08-28

    We describe the synthesis of novel mononuclear and dinuclear copper complexes and an investigation of their behaviour in solution using mass spectrometry (ESI-MS and ESI-MS/MS) and in the solid state using X-ray crystallography. The complexes were synthesized from two widely used diacetylpryridine (dap) ligands, i.e. 2,6-diacetylpyridinebis(benzoic acid hydrazone) and 2,6-diacetylpyridinebis(2-aminobenzoic acid hydrazone). Theoretical calculations (DFT) were used to predict the complex geometries of these new structures, their equilibrium in solution and energies associated with the transformations.

  4. Small angle neutron scattering studies of mixed micelles of sodium

    Indian Academy of Sciences (India)

    The aqueous solutions of sodium cumene sulphonate (NaCS) and its mixtures with each of cetyl trimethylammonium bromide (CTAB) and sodium dodecyl sulphate (SDS) are characterized by small angle neutron scattering (SANS). NaCS when added to CTAB solution leads to the formation of long rod-shaped micelles with ...

  5. Small-angle neutron scattering studies of nonionic surfactant: Effect

    Indian Academy of Sciences (India)

    Micellar solution of nonionic surfactant -dodecyloligo ethyleneoxide surfactant, decaoxyethylene monododecyl ether [CH3(CH2)11(OCH2CH2)10OH], C12E10 in D2O solution have been analysed by small-angle neutron scattering (SANS) at different temperatures (30, 45 and 60°C) both in the presence and absence of ...

  6. Combined operando X-ray diffraction–electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries

    Science.gov (United States)

    Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

    2015-01-01

    Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4. PMID:26345306

  7. Combined operando X-ray diffraction-electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries.

    Science.gov (United States)

    Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

    2015-09-08

    Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4.

  8. X-ray and neutron scattering on disordered nanosize clusters: a case study of lead-zirconate-titanate solid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Frantti, Johannes; Fujioka, Yukari [Finnish Research and Engineering, Helsinki (Finland)

    2015-04-01

    Defects and frequently used defect models of solids are reviewed. Signatures for identifying the disorder from x-ray and neutron scattering data are given. To give illustrative examples how technologically important defects contribute to x-ray and neutron scattering numerical method able to treat non-periodical solids possessing several simultaneous defect types is given for simulating scattering in nanosize disordered clusters. The approach takes particle size, shape, and defects into account and isolates element specific signals. As a case study a statistical approximation model for lead-zirconate titanate [Pb(Zr{sub x}Ti{sub 1-x})O{sub 3}, PZT] is introduced. PZT is a material possessing several defect types, including substitutional, displacement and surface defects. Spatial composition variation is taken into account by introducing a model in which the edge lengths of each cell depend on the distribution of Zr and Ti ions in the cluster. Spatially varying edge lengths and angles is referred to as microstrain. The model is applied to compute the scattering from ellipsoid shaped PZT clusters and to simulate the structural changes as a function of average composition. Two-phase co-existence range, the so called morphotropic phase boundary composition is given correctly. The composition at which the rhombohedral and tetragonal cells are equally abundant was x ∼ 0.51. Selected x-ray and neutron Bragg reflection intensities and line shapes were simulated. Examples of the effect of size and shape of the scattering clusters on diffraction patterns are given and the particle dimensions, computed through Scherrer equation, are compared with the exact cluster dimensions. Scattering from two types of 180 domains in spherical particles, one type assigned to Ti-rich PZT and the second to the MPB and Zr-rich PZT, is computed. We show how the method can be used for modelling polarization reversal. (copyright 2015 by WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Application of a radioactive sourced semi portable X-ray spectrometer to the solution of binary mix compositions

    International Nuclear Information System (INIS)

    Butcher, B.M.

    1988-01-01

    In many cases it is far more economically viable to transport individual constituents to a blending plant and produce a series of custom made products than to manufacture at site. This situation exists in many heavy chemical industries or on large building sites. In the cement industry inter-mixed or interground blends containing slag, fly ash, or limestone are produced. These mixes are designed to enhance certain physical properties and to reduce costs. This paper summarises experience of the application of portable isotope source X-ray analysers in achieving quality control of binary mixes

  10. X-ray astronomy

    International Nuclear Information System (INIS)

    Culhane, J.L.; Sanford, P.W.

    1981-01-01

    X-ray astronomy has been established as a powerful means of observing matter in its most extreme form. The energy liberated by sources discovered in our Galaxy has confirmed that collapsed stars of great density, and with intense gravitational fields, can be studied by making observations in the X-ray part of the electromagnetic spectrum. The astronomical objects which emit detectable X-rays include our own Sun and extend to quasars at the edge of the Universe. This book describes the history, techniques and results obtained in the first twenty-five years of exploration. Space rockets and satellites are essential for carrying the instruments above the Earth's atmosphere where it becomes possible to view the X-rays from stars and nebulae. The subject is covered in chapters, entitled: the birth of X-ray astronomy; the nature of X-radiation; X-rays from the Sun; solar-flare X-rays; X-rays from beyond the solar system; supernovae and their remnants; X-rays from binary stars; white dwarfs and neutron stars; black holes; X-rays from galaxies and quasars; clusters of galaxies; the observatories of the future. (author)

  11. X-ray holography

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  12. X-ray fluorescence holography.

    Science.gov (United States)

    Hayashi, Kouichi; Happo, Naohisa; Hosokawa, Shinya; Hu, Wen; Matsushita, Tomohiro

    2012-03-07

    X-ray fluorescence holography (XFH) is a method of atomic resolution holography which utilizes fluorescing atoms as a wave source or a monitor of the interference field within a crystal sample. It provides three-dimensional atomic images around a specified element and has a range of up to a few nm in real space. Because of this feature, XFH is expected to be used for medium-range local structural analysis, which cannot be performed by x-ray diffraction or x-ray absorption fine structure analysis. In this article, we explain the theory of XFH including solutions to the twin-image problem, an advanced measuring system, and data processing for the reconstruction of atomic images. Then, we briefly introduce our recent applications of this technique to the analysis of local lattice distortions in mixed crystals and nanometer-size clusters appearing in the low-temperature phase of a shape-memory alloy.

  13. X-ray fluorescence holography

    International Nuclear Information System (INIS)

    Hayashi, Kouichi; Happo, Naohisa; Hosokawa, Shinya; Hu Wen; Matsushita, Tomohiro

    2012-01-01

    X-ray fluorescence holography (XFH) is a method of atomic resolution holography which utilizes fluorescing atoms as a wave source or a monitor of the interference field within a crystal sample. It provides three-dimensional atomic images around a specified element and has a range of up to a few nm in real space. Because of this feature, XFH is expected to be used for medium-range local structural analysis, which cannot be performed by x-ray diffraction or x-ray absorption fine structure analysis. In this article, we explain the theory of XFH including solutions to the twin-image problem, an advanced measuring system, and data processing for the reconstruction of atomic images. Then, we briefly introduce our recent applications of this technique to the analysis of local lattice distortions in mixed crystals and nanometer-size clusters appearing in the low-temperature phase of a shape-memory alloy. (topical review)

  14. Providing x-rays

    International Nuclear Information System (INIS)

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

    1985-01-01

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

  15. Investigation of the interaction of Greek dolomitic marble with metal aqueous solutions using Rutherford backscattering and X-ray photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Godelitsas, A.; Kokkoris, M.; Misaelides, P.

    2005-01-01

    The interaction of dolomitic marble from Thassos Island (northern Aegean sea, Greece) with Co 2+ -, Cd 2+ -, Pb 2+ - and Cr 3+ - aqueous solutions (metal concentration: 1000 mgL -1 ) was investigated using Rutherford backscattering (RBS) and X-ray photoelectron spectroscopy (XPS). The initial material as well as the interaction products were also characterized by scanning electron microscopy (SEM/EDS), radioisotope induced X-ray fluorescence analysis (RI-XRFA), powder X-ray diffraction (Powder-XRD) and Fourier transform infra-red spectroscopy (FT-IR). The contact time of the samples with the aqueous solutions was one week and took place under ambient temperature. To our knowledge, the sorption of the above mentioned metals with dolomite (CaMg(CO 3 ) 2 ) has not yet been presented in the literature and the only data available concern the adsorption of Ca, Mg and Nd from NaCl solutions. The Thassos island dolomitic marble is a snow-white homogeneous carbonate metamorphic rock, with fine physicochemical and mechanical properties, currently used as natural building stone in many parts of the world (see http://www.thassosmarble.com), This dolomite-bearing material was also extensively used in the past as construction material of many .classical Greek and Roman sculptures and architectural elements; in 301 AD the Roman emperor Diocletian included 'Thassian marble' in the list of the 19 most expensive and important 'marbles' produced in the imperial quarries. Previous literature presented the isotopic analysis(δ 13 C, δ 18 O) and EPR studies (Mn 2+ and Fe 3+ ) of this stone. The obtained results indicated a limited Cd 2+ - and Co 2+ -sorption on the dissolved surface of the carbonate substrate, whereas, under the same experimental conditions, the Pb 2+ - and Cr 3+ -interaction is more intense leading to extended overgrowth of crystalline Pb-carbonates and surface precipitation of amorphous Cr-hydroxides/oxyhydroxides.

  16. Synchrotron X-ray Scattering of ZnO Nanorods: Periodic Ordering and Lattice Size

    International Nuclear Information System (INIS)

    Zhu, Z.; Andelman, T.; Yin, M.; Chen, T.; Ehrlich, S.; O'Brien, S.; Osgood, Jr. R.

    2005-01-01

    We demonstrate that synchrotron x-ray powder diffraction (XRD) is a powerful technique for studying the structure and self-organization of zinc-oxide nanostructures. Zinc-oxide nanorods were prepared by a solution-growth method that resulted in uniform nanorods with 2-nm diameter and lengths in the range 10-50 nm. These nanorods were structurally characterized by a combination of small-angle and wide-angle synchrotron XRD and transmission electron microscopy (TEM). Small-angle XRD and TEM were used to investigate nanorod self-assembly and the influence of surfactant/precursor ratio on self-assembly. Wide-angle XRD was used to study the evolution of nanorod growth as a function of synthesis time and surfactant/precursor ratio

  17. Looking for the best experimental conditions to detail the protein solvation shell in a binary aqueous solvent via small angle scattering

    International Nuclear Information System (INIS)

    Ortore, Maria Grazia; Sinibaldi, Raffaele; Spinozzi, Francesco; Carbini, Andrea; Carsughi, Flavio; Mariani, Paolo

    2009-01-01

    Protein hydration features attract particular interest in different fields, from biology up to physics, crossing chemistry and medicine. Particular attention is devoted to proteins dissolved in binary aqueous mixtures, since the presence of cosolvent can induce modifications in structural and functional properties. We have recently developed a methodology to obtain a quantitative description on protein solvation shell by a set of in-solution small angle scattering experiments, simultaneously analysed by a global-fit approach. In this paper, numerical simulations of small angle scattering curves are presented to figure out the sensitivity of the technique to different experimental conditions. Simulations concern two model proteins of different molecular weights and an unique cosolvent. A reliability test is introduced in order to find the best experimental conditions to be investigated, together with the most suitable scattering probe (neutrons or X-rays).

  18. State-dependent electron delocalization dynamics at the solute-solvent interface: soft-x-ray absorption spectroscopy and ab initio calculations.

    Science.gov (United States)

    Bokarev, Sergey I; Dantz, Marcus; Suljoti, Edlira; Kühn, Oliver; Aziz, Emad F

    2013-08-23

    Nonradiative decay channels in the L-edge fluorescence yield spectra from transition-metal-aqueous solutions give rise to spectral distortions with respect to x-ray transmission spectra. Their origin is unraveled here using partial and inverse partial fluorescence yields on the microjet combined with multireference ab initio electronic structure calculations. Comparing Fe2+, Fe3+, and Co2+ systems we demonstrate and quantify unequivocally the state-dependent electron delocalization within the manifold of d orbitals as one origin of this observation.

  19. X-ray microscopy in Aarhus

    International Nuclear Information System (INIS)

    Uggerhoej, Erik; Abraham-Peskir, Joanna V.

    2000-01-01

    The Aarhus imaging soft X-ray microscope is now a busy multi-user facility. The optical set-up will be described and project highlights discussed. a) Metal-induced structural changes in whole cells in solution. The effects of aluminum, copper, nickel and zinc on protozoa investigated by using a combination of light microscopy, confocal scanning laser microscopy and X-ray microscopy. b) Botanical studies by X-ray microscopy used to compliment electron microscopy studies. c) Sludge morphology and iron precipitation in Danish freshwater plants by combining X-ray, scanning electron and transmission electron microscopy

  20. X-ray interferometers

    International Nuclear Information System (INIS)

    Franks, A.

    1980-01-01

    An improved type of amplitude-division x-ray interferometer is described. The wavelength at which the interferometer can operate is variable, allowing the instrument to be used to measure x-ray wavelength, and the angle of inclination is variable for sample investigation. (U.K.)

  1. Extremity x-ray

    Science.gov (United States)

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

  2. X-rays utilization

    International Nuclear Information System (INIS)

    Rebigan, F.

    1979-03-01

    The modality of X-ray utilization in different activities and economy is given. One presents firstly quantities and units used in radiation dosimetry and other fields. One gives the generation of X-rays, their properties as well as the elements of radiation protection. The utilization characteristics of these radiations in different fields are finally given. (author)

  3. Chest X-Ray

    Medline Plus

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

  4. Small-angle neutron scattering instrument at MINT

    International Nuclear Information System (INIS)

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

    1996-01-01

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

  5. Look fast: Crystallization of conjugated molecules during solution shearing probed in-situ and in real time by X-ray scattering

    KAUST Repository

    Smilgies, Detlef Matthias; Li, Ruipeng; Giri, Gaurav; Chou, Kang Wei; Diao, Ying; Bao, Zhenan; Amassian, Aram

    2012-01-01

    High-speed solution shearing, in which a drop of dissolved material is spread by a coating knife onto the substrate, has emerged as a versatile, yet simple coating technique to prepare high-mobility organic thin film transistors. Solution shearing and subsequent drying and crystallization of a thin film of conjugated molecules is probed in situ using microbeam grazing incidence wide-angle X-ray scattering (μGIWAXS). We demonstrate the advantages of this approach to study solution based crystal nucleation and growth, and identify casting parameter combinations to cast highly ordered and laterally aligned molecular thin films. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Look fast: Crystallization of conjugated molecules during solution shearing probed in-situ and in real time by X-ray scattering

    KAUST Repository

    Smilgies, Detlef Matthias

    2012-12-20

    High-speed solution shearing, in which a drop of dissolved material is spread by a coating knife onto the substrate, has emerged as a versatile, yet simple coating technique to prepare high-mobility organic thin film transistors. Solution shearing and subsequent drying and crystallization of a thin film of conjugated molecules is probed in situ using microbeam grazing incidence wide-angle X-ray scattering (μGIWAXS). We demonstrate the advantages of this approach to study solution based crystal nucleation and growth, and identify casting parameter combinations to cast highly ordered and laterally aligned molecular thin films. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Quality regularities of dynamic X-ray diffraction in superlattices and films with variable gradient of deformation based on analysis of types of Takagi equation solutions

    International Nuclear Information System (INIS)

    Dyshekov, A.A.; Khapachev, Yu.P.

    1997-01-01

    It is proposed to use qualitative investigation methods of the differential Takagi equation solutions for the analysis of general properties of wave fields in deformed crystals. The physical interpretation of possible types of the Takagi equation solutions is considered briefly from the viewpoint of the stability theory. The type of solutions are defined by ratios between parameters involved in the equations set. For the Takagi equation these parameters are prescribed by the angular tuning from the precise Bragg angle as well as structural characteristics of the crystal and the deformation profile. The qualitative analysis for the problem of the dynamic X-ray diffraction is carried out for films with the variable deformation gradient and superlattices [ru

  8. Small-angle neutron-scattering experiments

    International Nuclear Information System (INIS)

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

    1981-04-01

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

  9. The BESSY X-ray microfocus beamline project

    International Nuclear Information System (INIS)

    Erko, A.; Schaefers, F.; Firsov, A.; Peatman, W.B.; Eberhardt, W.; Signorato, R.

    2004-01-01

    The design and construction of a beamline dedicated to X-ray absorption spectroscopy, X-ray fluorescence analysis, X-ray diffraction and X-ray small-angle scattering measurements with micron and submicron spatial resolution in the photon energy range of 1.9-30 keV are reported here. The main feature of the beamline is a combination of all these methods in one experimental station. The source will be a BESSY 7-T wavelength shifter, which is already in operation. Such a wavelength shifter with its continuous spectrum is an optimum source for these experiments. Glass capillaries and the combination of a linear Bragg-Fresnel lens and bimorph mirror were chosen as the special optical components in the beamline. This beamline will open for BESSY users the possibility to perform experiments on the same sample applying a microfocused X-ray beam in combination with advanced experimental methods

  10. X-ray crystallography

    Science.gov (United States)

    2001-01-01

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

  11. X-ray lasers

    CERN Document Server

    Elton, Raymond C

    2012-01-01

    The first in its field, this book is both an introduction to x-ray lasers and a how-to guide for specialists. It provides new entrants and others interested in the field with a comprehensive overview and describes useful examples of analysis and experiments as background and guidance for researchers undertaking new laser designs. In one succinct volume, X-Ray Lasers collects the knowledge and experience gained in two decades of x-ray laser development and conveys the exciting challenges and possibilities still to come._Add on for longer version of blurb_M>The reader is first introduced

  12. 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.)

  13. X-ray detector

    International Nuclear Information System (INIS)

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

    1977-01-01

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

  14. X-ray apparatus

    International Nuclear Information System (INIS)

    Grady, J.K.

    1985-01-01

    X-ray apparatus is described which has a shutter between the X-ray source and the patient. The shutter controls the level of radiation to which the patient is exposed instead of merely discontinuing the electric power supplied to the source. When the shutter is opened a radiation sensor senses the level of X-radiation. When a preset quantity of X-radiation has been measured an exposure control closes the shutter. Instead of using the radiation sensor, the integrated power supplied to the anode of the X-ray source may be measured. (author)

  15. Bone X-Ray (Radiography)

    Medline Plus

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

  16. Bone X-Ray (Radiography)

    Medline Plus

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

  17. X-ray examination apparatus

    NARCIS (Netherlands)

    2000-01-01

    The invention relates to an X-ray apparatus which includes an adjustable X-ray filter. In order to adjust an intensity profile of the X-ray beam, an X-ray absorbing liquid is transported to filter elements of the X-ray filter. Such transport is susceptible to gravitational forces which lead to an

  18. Bone X-Ray (Radiography)

    Medline Plus

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

  19. Bone X-Ray (Radiography)

    Science.gov (United States)

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

  20. Bone X-Ray (Radiography)

    Medline Plus

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