Science.gov

Sample records for angle scattering techniques

  1. Multiple small angle neutron scattering: A new two-dimensional ultrasmall angle neutron scattering technique

    SciTech Connect

    Gruenzweig, C.; Hils, T.; Muehlbauer, S.; Ay, M.; Lorenz, K.; Georgii, R.; Gaehler, R.; Boeni, P.

    2007-11-12

    We report on the demonstration experiment of the multiple small angle neutron scattering (MSANS) technique at a 5.6 m long neutron beam line, leading to a q resolution of 3x10{sup -4} A{sup -1}. The MSANS technique is based on two two-dimensional multihole apertures placed at the front end of the collimator and close to the sample, respectively. By choosing the proper MSANS geometry, individual diffraction patterns are superimposed leading to a large gain in intensity. Using MSANS as an option for standard small angle neutron scattering beam lines, the q resolution could be increased to 10{sup -5} A{sup -1} without dramatically sacrificing intensity.

  2. Scanning angle Raman spectroscopy: Investigation of Raman scatter enhancement techniques for chemical analysis

    SciTech Connect

    Meyer, Matthew W.

    2013-01-01

    This thesis outlines advancements in Raman scatter enhancement techniques by applying evanescent fields, standing-waves (waveguides) and surface enhancements to increase the generated mean square electric field, which is directly related to the intensity of Raman scattering. These techniques are accomplished by employing scanning angle Raman spectroscopy and surface enhanced Raman spectroscopy. A 1064 nm multichannel Raman spectrometer is discussed for chemical analysis of lignin. Extending dispersive multichannel Raman spectroscopy to 1064 nm reduces the fluorescence interference that can mask the weaker Raman scattering. Overall, these techniques help address the major obstacles in Raman spectroscopy for chemical analysis, which include the inherently weak Raman cross section and susceptibility to fluorescence interference.

  3. Development and prospects of Very Small Angle Neutron Scattering (VSANS) techniques

    NASA Astrophysics Data System (ADS)

    Xuo, Tai-Sen; Cheng, He; Chen, Yuan-Bo; Wang, Fang-Wei

    2016-07-01

    Very Small Angle Neutron Scattering (VSANS) is an upgrade of the traditional Small Angle Neutron Scattering (SANS) technique which can cover three orders of magnitude of length scale from one nanometer to one micrometer. It is a powerful tool for structure calibration in polymer science, biology, material science and condensed matter physics. Since the first VSANS instrument, D11 in Grenoble, was built in 1972, new collimation techniques, focusing optics (multi-beam converging apertures, material or magnetic lenses, and focusing mirrors) and higher resolution detectors combined with the long flight paths and long incident neutron wavelengths have been developed. In this paper, a detailed review is given of the development, principles and application conditions of various VSANS techniques. Then, beam current gain factors are calculated to evaluate those techniques. A VSANS design for the China Spallation Neutron Source (CSNS) is thereby presented. Supported by National Natural Science Foundation of China (21474119, 11305191)

  4. Small Angle Neutron Scattering

    SciTech Connect

    Urban, Volker S

    2012-01-01

    Small Angle Neutron Scattering (SANS) probes structural details at the nanometer scale in a non-destructive way. This article gives an introduction to scientists who have no prior small-angle scattering knowledge, but who seek a technique that allows elucidating structural information in challenging situations that thwart approaches by other methods. SANS is applicable to a wide variety of materials including metals and alloys, ceramics, concrete, glasses, polymers, composites and biological materials. Isotope and magnetic interactions provide unique methods for labeling and contrast variation to highlight specific structural features of interest. In situ studies of a material s responses to temperature, pressure, shear, magnetic and electric fields, etc., are feasible as a result of the high penetrating power of neutrons. SANS provides statistical information on significant structural features averaged over the probed sample volume, and one can use SANS to quantify with high precision the structural details that are observed, for example, in electron microscopy. Neutron scattering is non-destructive; there is no need to cut specimens into thin sections, and neutrons penetrate deeply, providing information on the bulk material, free from surface effects. The basic principles of a SANS experiment are fairly simple, but the measurement, analysis and interpretation of small angle scattering data involves theoretical concepts that are unique to the technique and that are not widely known. This article includes a concise description of the basics, as well as practical know-how that is essential for a successful SANS experiment.

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

    PubMed

    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 VV mode with the polarizer and analyzer parallel to each other and the HV mode having them perpendicular to each other. Using rotational and translational diffusion coefficients obtained under the HV mode yielded a nanocellulose length qualitatively consistent with that observed by TEM, whereas the length derived by the translational diffusion coefficient under the VV mode appeared to be overestimated.

  6. Using Small-Angle Scattering Techniques to Understand Mechanical Properties of Biopolymer-Based Biomaterials

    PubMed Central

    Hyland, Laura L.; Taraban, Marc B.

    2013-01-01

    The design and engineering of innovative biopolymer-based biomaterials for a variety of biomedical applications should be based on the understanding of the relationship between their nanoscale structure and mechanical properties. Down the road, such understanding could be fundamental to tune the properties of engineered tissues, extracellular matrices for cell delivery and proliferation/differentiation, etc. In this tutorial review, we attempt to show in what way biomaterial structural data can help to understand the bulk material properties. We begin with some background on common types of biopolymers used in biomaterials research, discuss some typical mechanical testing techniques and then review how others in the field of biomaterials have utilized small-angle scattering for material characterization. Detailed examples are then used to show the full range of possible characterization techniques available for biopolymer-based biomaterials. Future developments in the area of material characterization by small-angle scattering will undoubtedly facilitate the use of structural data to control the kinetics of assembly and final properties of prospective biomaterials. PMID:24273590

  7. Small angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Cousin, Fabrice

    2015-10-01

    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 spectrometer

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

    SciTech Connect

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

    2014-09-24

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

  9. Ultra Low-{kappa} Metrology Using X-Ray Reflectivity And Small-Angle X-Ray Scattering Techniques

    SciTech Connect

    Plantier, L.; Gonchond, J.-P.; Pernot, F.; Peled, A.; Yokhin, B.; Wyon, C.; Royer, J.-C.

    2007-09-26

    The automated metrology tool, combining X-ray reflectivity XRR and small-angle X-ray scattering SAXS has been demonstrated as a capable equipment to assess standard porous Ultra low-{kappa} (ULK) metrology. Therefore those techniques have enabled characterizations of several ULK used in sub-65 nm nodes integration. Standard ULK material for 65 nm node technology has been monitored through the whole C065 integration steps using those combined techniques.

  10. An overview of resid characterization by mass spectrometry and small angle scattering techniques.

    SciTech Connect

    Hunt, J. E.; Winans, R. E.

    1999-07-14

    The purpose of this presentation is to discuss what is known about the molecular structures found in petroleum resid from mass spectrometry and small angle neutron and X-ray scattering methods. The question about molecular size distributions and the occurrence of aggregation in the asphaltene fraction will be examined. Our understanding of this problem has evolved with the application of new analytical methods. Also, correlations with results from other approaches will be discussed. In addition, the issue of the nature of the heteroatom-containing molecules will be examined and the challenges that remain in this area.

  11. Strain induced directional coarsening in nickel based superalloys: Investigation on kinetics using the small angle neutron scattering (SANS) technique

    SciTech Connect

    Veron, M.; Bastie, P.

    1997-08-01

    Using the small angle neutron scattering technique, the authors have observed rafting in nickel based single crystal superalloys. Kinetics of morphological evolution of the precipitates have been studied in situ. Therefore the authors used a special furnace designed for the ageing of prestrained specimens under a neutron beam. The evolution of both the precipitate aspect ratio and the distance between precipitates confirms the importance of strain in the directional coarsening process. Results are presented and discussed regarding kinetics and microstructural aspects. In such conditions, rafts seem to be different from those obtained after a creep test.

  12. Asymmetrical flow field-flow fractionation with multi-angle light scattering and quasi-elastic light scattering for characterization of polymersomes: comparison with classical techniques.

    PubMed

    Till, Ugo; Gaucher-Delmas, Mireille; Saint-Aguet, Pascale; Hamon, Glenn; Marty, Jean-Daniel; Chassenieux, Christophe; Payré, Bruno; Goudounèche, Dominique; Mingotaud, Anne-Françoise; Violleau, Frédéric

    2014-12-01

    Polymersomes formed from amphiphilic block copolymers, such as poly(ethyleneoxide-b-ε-caprolactone) (PEO-b-PCL) or poly(ethyleneoxide-b-methylmethacrylate), were characterized by asymmetrical flow field-flow fractionation coupled with quasi-elastic light scattering (QELS), multi-angle light scattering (MALS), and refractive index detection, leading to the determination of their size, shape, and molecular weight. The method was cross-examined with more classical ones, like batch dynamic and static light scattering, electron microscopy, and atomic force microscopy. The results show good complementarities between all the techniques; asymmetrical flow field-flow fractionation being the most pertinent one when the sample exhibits several different types of population.

  13. VecDec4SAS program for analyzing the dynamic processes observed by the small-angle scattering technique

    NASA Astrophysics Data System (ADS)

    Molodenskii, D. S.

    2017-01-01

    A VecDec4SAS program has been developed to provide a fast and easy description of the dynamics of any process occurring in a nanoparticle solution observed by the small-angle scattering technique. The process should be characterized by the some conditional initial and final stages, in fractions of which all intermediate data are expanded. The program makes it possible to estimate the adequacy of two-basis approximation and indicate the presence of an additional process introducing a systematic error into the initial data. Scattering curves for human serum albumin protein in solutions with pH 7.4 and 3.0 and a concentration of 20 mg/mL, obtained on the DICSY station at the National Research Centre "Kurchatov Institute" in the solution temperature range from 25 to 70°C, were taken to be initial data to illustrate the potential of the program.

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

    PubMed Central

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

    2014-01-01

    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. PMID:25485128

  15. Angle resolved scatter measurement of bulk scattering in transparent ceramics

    NASA Astrophysics Data System (ADS)

    Sharma, Saurabh; Miller, J. Keith; Shori, Ramesh K.; Goorsky, Mark S.

    2015-02-01

    Bulk scattering in polycrystalline laser materials (PLM), due to non-uniform refractive index across the bulk, is regarded as the primary loss mechanism leading to degradation of laser performance with higher threshold and lower output power. The need for characterization techniques towards identifying bulk scatter and assessing the quality. Assessment of optical quality and the identification of bulk scatter have been by simple visual inspection of thin samples of PLMs, thus making the measurements highly subjective and inaccurate. Angle Resolved Scatter (ARS) measurement allows for the spatial mapping of scattered light at all possible angles about a sample, mapping the intensity for both forward scatter and back-scatter regions. The cumulative scattered light intensity, in the forward scatter direction, away from the specular beam is used for the comparison of bulk scattering between samples. This technique employ the detection of scattered light at all angles away from the specular beam directions and represented as a 2-D polar map. The high sensitivity of the ARS technique allows us to compare bulk scattering in different PLM samples which otherwise had similar transmitted beam wavefront distortions.

  16. Small‐angle X‐ray scattering as a useful supplementary technique to determine molecular masses of polyelectrolytes in solution

    PubMed Central

    Plazzotta, Beatrice; Diget, Jakob Stensgaard; Zhu, Kaizheng; Nyström, Bo

    2016-01-01

    ABSTRACT Determination of molecular masses of charged polymers is often nontrivial and most methods have their drawbacks. For polyelectrolytes, a new possibility for the determination of number‐average molecular masses is represented by small‐angle X‐ray scattering (SAXS) which allows fast determinations with a 10% accuracy. This is done by relating the mass to the position of a characteristic peak feature which arises in SAXS due to the local ordering caused by charge‐repulsions between polyelectrolytes. Advantages of the technique are the simplicity of data analysis, the independency from polymer architecture, and the low sample and time consumption. The method was tested on polyelectrolytes of various structures and chemical compositions, and the results were compared with those obtained from more conventional techniques, such as asymmetric flow field‐flow fractionation, gel permeation chromatography, and classical SAXS data analysis, showing that the accuracy of the suggested method is similar to that of the other techniques. © 2016 The Authors. Journal of Polymer Science Part B: Polymer Physics Published by Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2016, 54, 1913–1917 PMID:27840558

  17. Neutron spin echo scattering angle measurement (SESAME)

    SciTech Connect

    Pynn, R.; Fitzsimmons, M.R.; Fritzsche, H.; Gierlings, M.; Major, J.; Jason, A.

    2005-05-15

    We describe experiments in which the neutron spin echo technique is used to measure neutron scattering angles. We have implemented the technique, dubbed spin echo scattering angle measurement (SESAME), using thin films of Permalloy electrodeposited on silicon wafers as sources of the magnetic fields within which neutron spins precess. With 30-{mu}m-thick films we resolve neutron scattering angles to about 0.02 deg. with neutrons of 4.66 A wavelength. This allows us to probe correlation lengths up to 200 nm in an application to small angle neutron scattering. We also demonstrate that SESAME can be used to separate specular and diffuse neutron reflection from surfaces at grazing incidence. In both of these cases, SESAME can make measurements at higher neutron intensity than is available with conventional methods because the angular resolution achieved is independent of the divergence of the neutron beam. Finally, we discuss the conditions under which SESAME might be used to probe in-plane structure in thin films and show that the method has advantages for incident neutron angles close to the critical angle because multiple scattering is automatically accounted for.

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

    PubMed

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

    2015-07-10

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

  19. Anomalous and resonance small angle scattering: Revision

    SciTech Connect

    Epperson, J.E.; Thiyagarajan, P.

    1987-11-01

    Significant changes in the small angle scattered intensity can be induced by making measurements with radiation close to an absorption edge of an appropriate atomic species contained in the sample. These changes can be related quantitatively to the real and imaginary anomalous dispersion terms for the scattering factor (x-rays) or scattering length (neutrons). The physics inherent in these anomalous dispersion terms is first discussed before considering how they enter the relevant scattering theory. Two major areas of anomalous scattering research have emerged; macromolecules in solution and unmixing of metallic alloys. Research in each area is reviewed, illustrating both the feasibility and potential of these techniques. All the experimental results reported to date have been obtained with x-rays. However, it is pointed out that the formalism is the same for the analogue experiment with neutrons, and a number of suitable isotopes exist which exhibit resonance in an accessible range of energy. Potential applications of resonance small angle neutron scatterings are discussed. 54 refs., 8 figs., 1 tab.

  20. Anomalous and resonance small angle scattering

    SciTech Connect

    Epperson, J.E.; Thiyagarajan, P.

    1987-11-01

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

  1. Particle chaos and pitch angle scattering

    NASA Technical Reports Server (NTRS)

    Burkhart, G. R.; Dusenbery, P. B.; Speiser, T. W.

    1995-01-01

    Pitch angle scattering is a factor that helps determine the dawn-to-dusk current, controls particle energization, and it has also been used as a remote probe of the current sheet structure. Previous studies have interpreted their results under the exception that randomization will be greatest when the ratio of the two timescales of motion (gyration parallel to and perpendicular to the current sheet) is closet to one. Recently, the average expotential divergence rate (AEDR) has been calculated for particle motion in a hyperbolic current sheet (Chen, 1992). It is claimed that this AEDR measures the degree of chaos and therefore may be thought to measure the randomization. In contrast to previous expectations, the AEDR is not maximized when Kappa is approximately equal to 1 but instead increases with decreasing Kappa. Also contrary to previous expectations, the AEDR is dependent upon the parameter b(sub z). In response to the challenge to previous expectations that has been raised by this calculation of the AEDR, we have investigated the dependence of a measure of particle pitch angle scattering on both the parameters Kappa and b(sub z). We find that, as was previously expected, particle pitch angle scattering is maximized near Kappa = 1 provided that Kappa/b(sub z) greater than 1. In the opposite regime, Kappa/b(sub z) less than 1, we find that particle pitch angle scattering is still largest when the two timescales are equal, but the ratio of the timescales is proportional to b(sub z). In this second regime, particle pitch angle scattering is not due to randomization, but is instead due to a systematic pitch angle change. This result shows that particle pitch angle scattering need not be due to randomization and indicates how a measure of pitch angle scattering can exhibit a different behavior than a measure of chaos.

  2. Small Angle X-Ray Scattering Detector

    DOEpatents

    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., q.sub.max /q.sub.min.congruent.100.

  3. Multiple scattering technique lidar

    NASA Technical Reports Server (NTRS)

    Bissonnette, Luc R.

    1992-01-01

    The Bernouilli-Ricatti equation is based on the single scattering description of the lidar backscatter return. In practice, especially in low visibility conditions, the effects of multiple scattering can be significant. Instead of considering these multiple scattering effects as a nuisance, we propose here to use them to help resolve the problems of having to assume a backscatter-to-extinction relation and specifying a boundary value for a position far remote from the lidar station. To this end, we have built a four-field-of-view lidar receiver to measure the multiple scattering contributions. The system has been described in a number of publications that also discuss preliminary results illustrating the multiple scattering effects for various environmental conditions. Reported here are recent advances made in the development of a method of inverting the multiple scattering data for the determination of the aerosol scattering coefficient.

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

    NASA Astrophysics Data System (ADS)

    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

  5. Investigating hard sphere interactions through spin echo scattering angle measurement

    NASA Astrophysics Data System (ADS)

    Washington, Adam

    Spin Echo Scattering Angle Measurement (SESAME) allows neutron scattering instruments to perform real space measurements on large micron scale samples by encoding the scattering angle into the neutron's spin state via Larmor precession. I have built a SESAME instrument at the Low Energy Neutron Source. I have also assisted in the construction of a modular SESAME instrument on the ASTERIX beamline at Los Alamos National lab. The ability to tune these instruments has been proved mathematically and optimized and automated experimentally. Practical limits of the SESAME technique with respect to polarization analyzers, neutron spectra, Larmor elements, and data analysis were investigated. The SESAME technique was used to examine the interaction of hard spheres under depletion. Poly(methyl methacrylate) spheres suspended in decalin had previously been studied as a hard sphere solution. The interparticle correlations between the spheres were found to match the Percus-Yevick closure, as had been previously seen in dynamical light scattering experiments. To expand beyond pure hard spheres, 900kDa polystyrene was added to the solution in concentrations of less than 1% by mass. The steric effects of the polystyrene were expected to produce a short-range, attractive, "sticky" potential. Experiment showed, however, that the "sticky" potential was not a stable state and that the spheres would eventually form long range aggregates.

  6. Low-angle X-ray scattering from spices

    NASA Astrophysics Data System (ADS)

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

    2002-07-01

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

  7. Small angle neutron scattering using a triple axis spectrometer

    SciTech Connect

    Ahmend, F.U.; Kamal, I.; Yunus, S.M.

    1994-12-31

    SANS technique has been developed on a triple axis neutron spectrometer at TRIGA Mark II (3 MW) research reactor, AERE, Savar, Dhaka, Bangladesh. Double crystal (with very small mosaic spread {approximately} 1 min.) diffraction known as Bonse and Hart`s method has been employed in this technique. Such a device is a useful tool for small angle scattering in the Q range between 10{sup -5} and 10{sup -1} {Angstrom}{sup -1} and for real time experiments at short time scales. Therefore, large objects and large distance interparticle correlations can be investigated easily by this method. Test measurements using alumina (Al{sub 2}O{sub 3}) sample has been carried out to exploit this method. The radius of gyration has been determined and the data has been fitted to the scattering function of a sphere.

  8. Experimental methods in the study of neutron scattering at small angles

    SciTech Connect

    Dragolici, Cristian A.

    2014-11-24

    Small angle scattering (SAS) is the collective name given to the techniques of small angle neutron (SANS) and X-ray (SAXS) scattering. They offer the possibility to analyze particles without disturbing their natural environment. In each of these techniques radiation is elastically scattered by a sample and the resulting scattering pattern is analyzed to provide information about the size, shape and orientation of some component of the sample. Accordingly, a large number of methods and experimental patterns have been developed to ease the investigation of condensed matter by use of these techniques. Some of them are the discussed in this paper.

  9. Fractal Approach in Petrology: Combining Ultra-Small Angle (USANA) and Small Angle Neutron Scattering (SANS)

    SciTech Connect

    LoCelso, F.; Triolo, F.; Triolo, A.; Lin, J.S.; Lucido, G.; Triolo, R.

    1999-10-14

    Ultra small angle neutron scattering instruments have recently covered the gap between the size resolution available with conventional intermediate angle neutron scattering and small angle neutron scattering instruments on one side and optical microscopy on the other side. Rocks showing fractal behavior in over two decades of momentum transfer and seven orders of magnitude of intensity are examined and fractal parameters are extracted from the combined USANS and SANS curves.

  10. Coincidence measurements of electron-impact coherence parameters for e-He scattering in the full range of scattering angles

    SciTech Connect

    Klosowski, Lukasz; Piwinski, Mariusz; Dziczek, Dariusz; Pleskacz, Katarzyna; Chwirot, Stanislaw

    2009-12-15

    Electron impact coherence parameters for inelastic e-He scattering have been measured for the excitation to the 2 {sup 1}P{sub 1} state at collision energy of 100 eV. The experiment was conducted using angular correlation electron-photon coincidence technique with a magnetic angle changer allowing measurements in full range of scattering angles. The results are compared with other experimental data and theoretical predictions available for this collisional system.

  11. Spectral angle resolved scattering of thin film coatings.

    PubMed

    Schröder, Sven; Unglaub, David; Trost, Marcus; Cheng, Xinbin; Zhang, Jinlong; Duparré, Angela

    2014-02-01

    The light scattering of interference coatings is strongly dependent on the wavelength. In addition to the general strong increase of scattering as the wavelengths get shorter, dramatic scatter effects in and around the resonance regions can occur. This is discussed in detail for highly reflective and chirped mirrors. A new instrument is presented which enables spectral angle resolved scatter measurements of high-quality optical components to be performed between 250 and 1500 nm.

  12. Hierarchical Pore Morphology of Cretaceous Shale: A Small-Angle Neutron Scattering and Ultrasmall-Angle Neutron Scattering Study

    SciTech Connect

    Bahadur, J.; Melnichenko, Y. B.; Mastalerz, Maria; Furmann, Agnieszka; Clarkson, Chris R.

    2014-09-25

    Shale reservoirs are becoming an increasingly important source of oil and natural gas supply and a potential candidate for CO2 sequestration. Understanding the pore morphology in shale may provide clues to making gas extraction more efficient and cost-effective. The porosity of Cretaceous shale samples from Alberta, Canada, collected from different depths with varying mineralogical compositions, has been investigated by small- and ultrasmall-angle neutron scattering. Moreover these samples come from the Second White Specks and Belle Fourche formations, and their organic matter content ranges between 2 and 3%. The scattering length density of the shale specimens has been estimated using the chemical composition of the different mineral components. Scattering experiments reveal the presence of fractal and non-fractal pores. It has been shown that the porosity and specific surface area are dominated by the contribution from meso- and micropores. The fraction of closed porosity has been calculated by comparing the porosities estimated by He pycnometry and scattering techniques. There is no correlation between total porosity and mineral components, a strong correlation has been observed between closed porosity and major mineral components in the studied specimens.

  13. Hierarchical Pore Morphology of Cretaceous Shale: A Small-Angle Neutron Scattering and Ultrasmall-Angle Neutron Scattering Study

    DOE PAGES

    Bahadur, J.; Melnichenko, Y. B.; Mastalerz, Maria; ...

    2014-09-25

    Shale reservoirs are becoming an increasingly important source of oil and natural gas supply and a potential candidate for CO2 sequestration. Understanding the pore morphology in shale may provide clues to making gas extraction more efficient and cost-effective. The porosity of Cretaceous shale samples from Alberta, Canada, collected from different depths with varying mineralogical compositions, has been investigated by small- and ultrasmall-angle neutron scattering. Moreover these samples come from the Second White Specks and Belle Fourche formations, and their organic matter content ranges between 2 and 3%. The scattering length density of the shale specimens has been estimated using themore » chemical composition of the different mineral components. Scattering experiments reveal the presence of fractal and non-fractal pores. It has been shown that the porosity and specific surface area are dominated by the contribution from meso- and micropores. The fraction of closed porosity has been calculated by comparing the porosities estimated by He pycnometry and scattering techniques. There is no correlation between total porosity and mineral components, a strong correlation has been observed between closed porosity and major mineral components in the studied specimens.« less

  14. Cosmic-ray pitch-angle scattering in isotropic turbulence

    NASA Technical Reports Server (NTRS)

    Bieber, John W.; Smith, Charles W.; Matthaeus, William H.

    1988-01-01

    A dissipation range is incorporated in the turbulence model to reconcile the divergent conclusions from studies of cosmic-ray pitch-angle scattering in isotropic magnetic turbulence. The Fokker-Planck coefficient for pitch-angle scattering is calculated. It is shown that the slab form of the Fokker-Plank coefficient (Jokipii, 1966) is valid at very low energies, while the nonslab form (Fisk, 1974) is valid at intermediate energies.

  15. Collisionless pitch-angle scattering of runaway electrons

    NASA Astrophysics Data System (ADS)

    Liu, Jian; Wang, Yulei; Qin, Hong

    2016-06-01

    It is discovered that the tokamak field geometry generates a toroidicity induced broadening of the pitch-angle distribution of runaway electrons. This collisionless pitch-angle scattering is much stronger than the collisional scattering and invalidates the gyro-center model for runaway electrons. As a result, the energy limit of runaway electrons is found to be larger than the prediction of the gyro-center model and to depend heavily on the background magnetic field.

  16. A Discrete Scatterer Technique for Evaluating Electromagnetic Scattering from Trees

    DTIC Science & Technology

    2016-09-01

    ARL-TR-7799 ● SEP 2016 US Army Research Laboratory A Discrete Scatterer Technique for Evaluating Electromagnetic Scattering from...longer needed. Do not return it to the originator. ARL-TR-7799 ● SEP 2016 US Army Research Laboratory A Discrete Scatterer Technique ... Technique for Evaluating Electromagnetic Scattering from Trees 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S

  17. Radiation damage study using small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Rétfalvi, E.; Török, Gy; Rosta, L.

    2000-03-01

    Nuclear radiation provides important changes in the microstructure of metallic components of nuclear power plant and research reactors, influencing their mechanical properties. The investigation of this problem has primary interest for the safety and life-time of such nuclear installations. For the characterization of this kind of nanostructures small angle neutron scattering technique is a very useful tool. We have carried out experiments on samples of irradiated reactor vessel material and welded components of VVER-440-type reactors on the SANS instrument at the Budapest Research Reactor. In our measurements irradiated as well as non-irradiated samples were compared and magnetic field was applied for viewing the magnetic structure effects of the materials. A clear modification of the structure due to irradiation was obtained. Our data were analyzed by the ITP92 code, the inverse Fourier transform program of O. Glatter [1].

  18. Limits of applicability of the concept of scattering amplitude in small-angle scattering problems

    NASA Astrophysics Data System (ADS)

    Dzheparov, F. S.; Lvov, D. V.

    2014-01-01

    The applicability of the concept of scattering amplitude to the description of small-angle scattering experiments has been considered. An expression has been obtained for a scattered radiation flux on a detector under much milder conditions than the condition of Fraunhofer diffraction. The influence of incoherence of the source on the results has been evaluated.

  19. Emerging applications of small angle solution scattering in structural biology.

    PubMed

    Chaudhuri, Barnali N

    2015-03-01

    Small angle solution X-ray and neutron scattering recently resurfaced as powerful tools to address an array of biological problems including folding, intrinsic disorder, conformational transitions, macromolecular crowding, and self or hetero-assembling of biomacromolecules. In addition, small angle solution scattering complements crystallography, nuclear magnetic resonance spectroscopy, and other structural methods to aid in the structure determinations of multidomain or multicomponent proteins or nucleoprotein assemblies. Neutron scattering with hydrogen/deuterium contrast variation, or X-ray scattering with sucrose contrast variation to a certain extent, is a convenient tool for characterizing the organizations of two-component systems such as a nucleoprotein or a lipid-protein assembly. Time-resolved small and wide-angle solution scattering to study biological processes in real time, and the use of localized heavy-atom labeling and anomalous solution scattering for applications as FRET-like molecular rulers, are amongst promising newer developments. Despite the challenges in data analysis and interpretation, these X-ray/neutron solution scattering based approaches hold great promise for understanding a wide variety of complex processes prevalent in the biological milieu.

  20. Angle-resolved light scattering of individual rod-shaped bacteria based on Fourier transform light scattering.

    PubMed

    Jo, YoungJu; Jung, JaeHwang; Lee, Jee Woong; Shin, Della; Park, HyunJoo; Nam, Ki Tae; Park, Ji-Ho; Park, YongKeun

    2014-05-28

    Two-dimensional angle-resolved light scattering maps of individual rod-shaped bacteria are measured at the single-cell level. Using quantitative phase imaging and Fourier transform light scattering techniques, the light scattering patterns of individual bacteria in four rod-shaped species (Bacillus subtilis, Lactobacillus casei, Synechococcus elongatus, and Escherichia coli) are measured with unprecedented sensitivity in a broad angular range from -70° to 70°. The measured light scattering patterns are analyzed along the two principal axes of rod-shaped bacteria in order to systematically investigate the species-specific characteristics of anisotropic light scattering. In addition, the cellular dry mass of individual bacteria is calculated and used to demonstrate that the cell-to-cell variations in light scattering within bacterial species is related to the cellular dry mass and growth.

  1. Angle-resolved light scattering of individual rod-shaped bacteria based on Fourier transform light scattering

    PubMed Central

    Jo, YoungJu; Jung, JaeHwang; Lee, Jee Woong; Shin, Della; Park, HyunJoo; Nam, Ki Tae; Park, Ji-Ho; Park, YongKeun

    2014-01-01

    Two-dimensional angle-resolved light scattering maps of individual rod-shaped bacteria are measured at the single-cell level. Using quantitative phase imaging and Fourier transform light scattering techniques, the light scattering patterns of individual bacteria in four rod-shaped species (Bacillus subtilis, Lactobacillus casei, Synechococcus elongatus, and Escherichia coli) are measured with unprecedented sensitivity in a broad angular range from −70° to 70°. The measured light scattering patterns are analyzed along the two principal axes of rod-shaped bacteria in order to systematically investigate the species-specific characteristics of anisotropic light scattering. In addition, the cellular dry mass of individual bacteria is calculated and used to demonstrate that the cell-to-cell variations in light scattering within bacterial species is related to the cellular dry mass and growth. PMID:24867385

  2. Angle-resolved light scattering of individual rod-shaped bacteria based on Fourier transform light scattering

    NASA Astrophysics Data System (ADS)

    Jo, Youngju; Jung, Jaehwang; Lee, Jee Woong; Shin, Della; Park, Hyunjoo; Nam, Ki Tae; Park, Ji-Ho; Park, Yongkeun

    2014-05-01

    Two-dimensional angle-resolved light scattering maps of individual rod-shaped bacteria are measured at the single-cell level. Using quantitative phase imaging and Fourier transform light scattering techniques, the light scattering patterns of individual bacteria in four rod-shaped species (Bacillus subtilis, Lactobacillus casei, Synechococcus elongatus, and Escherichia coli) are measured with unprecedented sensitivity in a broad angular range from -70° to 70°. The measured light scattering patterns are analyzed along the two principal axes of rod-shaped bacteria in order to systematically investigate the species-specific characteristics of anisotropic light scattering. In addition, the cellular dry mass of individual bacteria is calculated and used to demonstrate that the cell-to-cell variations in light scattering within bacterial species is related to the cellular dry mass and growth.

  3. Small Angle Neutron Scattering at the National Institute of Standards and Technology

    PubMed Central

    Hammouda, B.; Krueger, S.; Glinka, C. J.

    1993-01-01

    The small angle neutron scattering technique is a valuable method for the characterization of morphology of various materials. It can probe inhomogeneities in the sample (whether occurring naturally or introduced through isotopic substitution) at a length scale from the atomic size (nanometers) to the macroscopic (micrometers) size. This work provides an overview of the small angle neutron scattering facilities at the National Institute of Standards and Technology and a review of the technique as it has been applied to polymer systems, biological macromolecules, ceramic, and metallic materials. Specific examples have been included. PMID:28053456

  4. Characterization of cationic polymers by asymmetric flow field-flow fractionation and multi-angle light scattering-A comparison with traditional techniques.

    PubMed

    Wagner, Michael; Pietsch, Christian; Tauhardt, Lutz; Schallon, Anja; Schubert, Ulrich S

    2014-01-17

    In the field of nanomedicine, cationic polymers are the subject of intensive research and represent promising carriers for genetic material. The detailed characterization of these carriers is essential since the efficiency of gene delivery strongly depends on the properties of the used polymer. Common characterization methods such as size exclusion chromatography (SEC) or mass spectrometry (MS) suffer from problems, e.g. missing standards, or even failed for cationic polymers. As an alternative, asymmetrical flow field-flow fractionation (AF4) was investigated. Additionally, analytical ultracentrifugation (AUC) and (1)H NMR spectroscopy, as well-established techniques, were applied to evaluate the results obtained by AF4. In this study, different polymers of molar masses between 10 and 120kgmol(-1) with varying amine functionalities in the side chain or in the polymer backbone were investigated. To this end, some of the most successful gene delivery agents, namely linear poly(ethylene imine) (LPEI) (only secondary amines in the backbone), branched poly(ethylene imine) (B-PEI) (secondary and tertiary amino groups in the backbone, primary amine end groups), and poly(l-lysine) (amide backbone and primary amine side chains), were characterized. Moreover, poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA), poly(2-(amino)ethyl methacrylate) (PAEMA), and poly(2-(tert-butylamino)ethyl methacrylate) (PtBAEMA) as polymers with primary, secondary, and tertiary amines in the side chain, have been investigated. Reliable results were obtained for all investigated polymers by AF4. In addition, important factors for all methods were evaluated, e.g. the influence of different elution buffers and AF4 membranes. Besides this, the correct determination of the partial specific volume and the suppression of the polyelectrolyte effect are the most critical issues for AUC investigations.

  5. Small-angle and surface scattering from porous and fractal materials.

    SciTech Connect

    Sinha, S. K.

    1998-09-18

    We review the basic theoretical methods used to treat small-angle scattering from porous materials, treated as general two-phase systems, and also the basic experimental techniques for carrying out such experiments. We discuss the special forms of the scattering when the materials exhibit mass or surface fractal behavior, and review the results of recent experiments on several types of porous media and also SANS experiments probing the phase behavior of binary fluid mixtures or polymer solutions confined in porous materials. Finally, we discuss the analogous technique of off-specular scattering from surfaces and interfaces which is used to study surface roughness of various kinds.

  6. SASBDB, a repository for biological small-angle scattering data

    PubMed Central

    Valentini, Erica; Kikhney, Alexey G.; Previtali, Gianpietro; Jeffries, Cy M.; Svergun, Dmitri I.

    2015-01-01

    Small-angle X-ray and neutron scattering (SAXS and SANS) are fundamental tools used to study the global shapes of proteins, nucleic acids, macromolecular complexes and assemblies in solution. Due to recent advances in instrumentation and computational methods, the quantity of experimental scattering data and subsequent publications is increasing dramatically. The need for a global repository allowing investigators to locate and access experimental scattering data and associated models was recently emphasized by the wwPDB small-angle scattering task force (SAStf). The small-angle scattering biological data bank (SASBDB) www.sasbdb.org has been designed in accordance with the plans of the SAStf as part of a future federated system of databases for biological SAXS and SANS. SASBDB is a comprehensive repository of freely accessible and fully searchable SAS experimental data and models that are deposited together with the relevant experimental conditions, sample details and instrument characteristics. At present the quality of deposited experimental data and the accuracy of models are manually curated, with future plans to integrate automated systems as the database expands. PMID:25352555

  7. Low frequency seabed scattering at low grazing angles.

    PubMed

    Zhou, Ji-Xun; Zhang, Xue-Zhen

    2012-04-01

    Low-frequency (LF) seabed scattering at low grazing angles (LGA) is almost impossible to directly measure in shallow water (SW), except through inversion from reverberation. The energy flux method for SW reverberation is briefly introduced in this paper. The closed-form expressions of reverberation in an isovelocity waveguide, derived from this method, indicate that in the three-halves law range interval multimode/ray sea bottom scattering with different incident and scattering angles in forming the reverberation may equivalently be represented by the bottom backscattering at a single range-dependent angle. This equivalent relationship is used to derive the bottom backscattering strength (BBS) as a function of angle and frequency. The LF&LGA BBS is derived in a frequency band of 200-2500 Hz and in a grazing angle range of 1.1°-14.0° from reverberation measurements at three sites with sandy bottoms. This is based on three previous works: (1) The closed-form expressions of SW reverberation [Zhou, (Chinese) Acta Acustica 5, 86-99 (1980)]; (2) the effective geo-acoustic model of sandy bottoms that follows the Biot model [Zhou et al., J. Acoust. Soc. Am. 125, 2847-2866 (2009)] and (3) A quality database of wideband reverberation level normalized to source level [Zhou and Zhang, IEEE J. Oceanic Eng. 30, 832-842 (2005)].

  8. Multiple magnetic scattering in small-angle neutron scattering of Nd–Fe–B nanocrystalline magnet

    PubMed Central

    Ueno, Tetsuro; Saito, Kotaro; Yano, Masao; Ito, Masaaki; Shoji, Tetsuya; Sakuma, Noritsugu; Kato, Akira; Manabe, Akira; Hashimoto, Ai; Gilbert, Elliot P.; Keiderling, Uwe; Ono, Kanta

    2016-01-01

    We have investigated the influence of multiple scattering on the magnetic small-angle neutron scattering (SANS) from a Nd–Fe–B nanocrystalline magnet. We performed sample-thickness- and neutron-wavelength-dependent SANS measurements, and observed the scattering vector dependence of the multiple magnetic scattering. It is revealed that significant multiple scattering exists in the magnetic scattering rather than the nuclear scattering of Nd–Fe–B nanocrystalline magnet. It is considered that the mean free path of the neutrons for magnetic scattering is rather short in Nd–Fe–B magnets. We analysed the SANS data by the phenomenological magnetic correlation model considering the magnetic microstructures and obtained the microstructural parameters. PMID:27321149

  9. Multiple magnetic scattering in small-angle neutron scattering of Nd-Fe-B nanocrystalline magnet

    NASA Astrophysics Data System (ADS)

    Ueno, Tetsuro; Saito, Kotaro; Yano, Masao; Ito, Masaaki; Shoji, Tetsuya; Sakuma, Noritsugu; Kato, Akira; Manabe, Akira; Hashimoto, Ai; Gilbert, Elliot P.; Keiderling, Uwe; Ono, Kanta

    2016-06-01

    We have investigated the influence of multiple scattering on the magnetic small-angle neutron scattering (SANS) from a Nd-Fe-B nanocrystalline magnet. We performed sample-thickness- and neutron-wavelength-dependent SANS measurements, and observed the scattering vector dependence of the multiple magnetic scattering. It is revealed that significant multiple scattering exists in the magnetic scattering rather than the nuclear scattering of Nd-Fe-B nanocrystalline magnet. It is considered that the mean free path of the neutrons for magnetic scattering is rather short in Nd-Fe-B magnets. We analysed the SANS data by the phenomenological magnetic correlation model considering the magnetic microstructures and obtained the microstructural parameters.

  10. Multiple magnetic scattering in small-angle neutron scattering of Nd-Fe-B nanocrystalline magnet.

    PubMed

    Ueno, Tetsuro; Saito, Kotaro; Yano, Masao; Ito, Masaaki; Shoji, Tetsuya; Sakuma, Noritsugu; Kato, Akira; Manabe, Akira; Hashimoto, Ai; Gilbert, Elliot P; Keiderling, Uwe; Ono, Kanta

    2016-06-20

    We have investigated the influence of multiple scattering on the magnetic small-angle neutron scattering (SANS) from a Nd-Fe-B nanocrystalline magnet. We performed sample-thickness- and neutron-wavelength-dependent SANS measurements, and observed the scattering vector dependence of the multiple magnetic scattering. It is revealed that significant multiple scattering exists in the magnetic scattering rather than the nuclear scattering of Nd-Fe-B nanocrystalline magnet. It is considered that the mean free path of the neutrons for magnetic scattering is rather short in Nd-Fe-B magnets. We analysed the SANS data by the phenomenological magnetic correlation model considering the magnetic microstructures and obtained the microstructural parameters.

  11. Stabilization of asphaltenes in aliphatic solvents using alkylbenzene-derived amphiphiles. 2. Study of the asphaltene-amphiphile interactions and structures using Fourier transform infrared spectroscopy and small-angle X-ray scattering techniques

    SciTech Connect

    Chang, C.L.; Fogler, H.S. )

    1994-06-01

    In the preceding paper in this issue, the influence of the chemical structure of a series of alkylbenzene-derived amphiphiles on the stabilization of asphaltenes was described. In this paper, we present the results of using Fourier transform infrared (FTIR) spectroscopy and small-angle X-ray scattering (SAXS) techniques to study the interaction between asphaltenes and two alkylbenzene-derived amphiphiles, p-alkylphenol and p-alkylbenzenesulfonic acid. FTIR spectroscopy was used to characterize and quantify the acid-base interactions between asphaltenes and amphiphiles. It was found that asphaltenes could hydrogen-bond to p-dodecylphenol amphiphiles. The hydrogen-bonding capacity of asphaltenes was estimated to be 1.6-2.0 mmol/g of asphaltene. On the other hand, the FTIR spectroscopic study indicated that asphaltenes had a complicated acid-base interaction with p-dodecylbenzenesulfonic acid (DBSA) amphiphiles with a stoichiometry of about 1.8 mmol of DBSA/g of asphaltene. The UV/vis spectroscopic study suggested that asphaltenes and DBSA could associate into large electronic conjugated complexes. Physical evidence of the association between asphaltenes and amphiphiles was obtained by SAXS measurements. 27 refs., 10 figs.

  12. Angle- and Spectral-Dependent Light Scattering from Plasmonic Nanocups

    SciTech Connect

    King, Nicholas S.; Li, Yang; Ayala-Orozco, Ciceron; Brannan, Travis; Nordlander, Peter; Halas, Naomi J.

    2011-09-27

    As optical frequency nanoantennas, reduced-symmetry plasmonic nanoparticles have light-scattering properties that depend strongly on geometry, orientation, and variations in dielectric environment. Here we investigate how these factors influence the spectral and angular dependence of light scattered by Au nanocups. A simple dielectric substrate causes the axial, electric dipole mode of the nanocup to deviate substantially from its characteristic cos² θ free space scattering profile, while the transverse, magnetic dipole mode remains remarkably insensitive to the presence of the substrate. Nanoscale irregularities of the nanocup rim and the local substrate permittivity have a surprisingly large effect on the spectral- and angle-dependent light-scattering properties of these structures.

  13. Windows for small-angle X-ray scattering cryostats.

    PubMed

    Lurio, Laurence; Mulders, Norbert; Paetkau, Mark; Jemian, Pete R; Narayanan, Suresh; Sandy, Alec

    2007-11-01

    To determine the suitability of commonly used windows for small-angle X-ray scattering, a range of materials, including Kapton, (aluminized) Mylar, beryllium, high-purity aluminium foil, mica and silicon nitride have been studied. At small wavevector transfers, Q, in the range 2 x 10(-3) to 0.2 nm(-1), the scattering from Kapton, mica and beryllium is reasonably well described by power laws in Q with exponents of -3.25, -3.6 and -3.9, respectively. There are large variations in the scattering from mica, but a freshly cleaved natural mica window was by far the weakest scatterer. For applications where radiation in the infrared or visible range should be blocked, aluminized Mylar is the most suitable material. Both Mylar and Kapton can be used to make very simple demountable superfluid-tight windows using indium O-ring seals.

  14. Branch Content in Hybrid Materials using Small-Angle Scattering

    NASA Astrophysics Data System (ADS)

    Beaucage, Greg

    2005-03-01

    Inorganic/organic hybrid materials often display ramified mass- fractal structures characterized by primary particle size, aggregate size, and mass-fractal dimension. Physical properties, such as mechanical and dynamic mechanical properties and electrical conductivity (in carbon composites for instance), can not be predicted using only these structural features since such properties are intimately tied to the degree and type of branching as shown by Witten [1]. Witten suggested the use of the minimum dimension, or the related connectivity dimension, to calculate mechanical response in these hybrid systems. A viable technique to quantify the minimum dimension and connectivity dimension in hybrid materials has, until recently, been absent from the literature. This presentation will discuss the use of small-angle x-ray and neutron scattering to describe branch content in hybrid materials [2] and will outline an approach to use the minimum dimension and connectivity dimension to predict static and dynamic mechanical properties for hybrid materials based on structure [1, 3]. 1. Witten TA, Rubinstein M, Colby RH Reinforcement of Rubber by Fractal Aggregates J Phys II 3 (3): 367-383 (1993). 2. Beaucage G Determination of branch fraction and minimum dimension of mass-fractal aggregates Phys Rev E 70 (3): art. no. 031401 Part 1 (2004). 3. Kohls DJ, Beaucage G Rational design of reinforced rubber Curr Opin Solid St M 6 (3): 183-194 (2002).

  15. Pulsed Laser Ablation-Induced Green Synthesis of TiO2 Nanoparticles and Application of Novel Small Angle X-Ray Scattering Technique for Nanoparticle Size and Size Distribution Analysis.

    PubMed

    Singh, Amandeep; Vihinen, Jorma; Frankberg, Erkka; Hyvärinen, Leo; Honkanen, Mari; Levänen, Erkki

    2016-12-01

    This paper aims to introduce small angle X-ray scattering (SAXS) as a promising technique for measuring size and size distribution of TiO2 nanoparticles. In this manuscript, pulsed laser ablation in liquids (PLAL) has been demonstrated as a quick and simple technique for synthesizing TiO2 nanoparticles directly into deionized water as a suspension from titanium targets. Spherical TiO2 nanoparticles with diameters in the range 4-35 nm were observed with transmission electron microscopy (TEM). X-ray diffraction (XRD) showed highly crystalline nanoparticles that comprised of two main photoactive phases of TiO2: anatase and rutile. However, presence of minor amounts of brookite was also reported. The traditional methods for nanoparticle size and size distribution analysis such as electron microscopy-based methods are time-consuming. In this study, we have proposed and validated SAXS as a promising method for characterization of laser-ablated TiO2 nanoparticles for their size and size distribution by comparing SAXS- and TEM-measured nanoparticle size and size distribution. SAXS- and TEM-measured size distributions closely followed each other for each sample, and size distributions in both showed maxima at the same nanoparticle size. The SAXS-measured nanoparticle diameters were slightly larger than the respective diameters measured by TEM. This was because SAXS measures an agglomerate consisting of several particles as one big particle which slightly increased the mean diameter. TEM- and SAXS-measured mean diameters when plotted together showed similar trend in the variation in the size as the laser power was changed which along with extremely similar size distributions for TEM and SAXS validated the application of SAXS for size distribution measurement of the synthesized TiO2 nanoparticles.

  16. Pulsed Laser Ablation-Induced Green Synthesis of TiO2 Nanoparticles and Application of Novel Small Angle X-Ray Scattering Technique for Nanoparticle Size and Size Distribution Analysis

    NASA Astrophysics Data System (ADS)

    Singh, Amandeep; Vihinen, Jorma; Frankberg, Erkka; Hyvärinen, Leo; Honkanen, Mari; Levänen, Erkki

    2016-10-01

    This paper aims to introduce small angle X-ray scattering (SAXS) as a promising technique for measuring size and size distribution of TiO2 nanoparticles. In this manuscript, pulsed laser ablation in liquids (PLAL) has been demonstrated as a quick and simple technique for synthesizing TiO2 nanoparticles directly into deionized water as a suspension from titanium targets. Spherical TiO2 nanoparticles with diameters in the range 4-35 nm were observed with transmission electron microscopy (TEM). X-ray diffraction (XRD) showed highly crystalline nanoparticles that comprised of two main photoactive phases of TiO2: anatase and rutile. However, presence of minor amounts of brookite was also reported. The traditional methods for nanoparticle size and size distribution analysis such as electron microscopy-based methods are time-consuming. In this study, we have proposed and validated SAXS as a promising method for characterization of laser-ablated TiO2 nanoparticles for their size and size distribution by comparing SAXS- and TEM-measured nanoparticle size and size distribution. SAXS- and TEM-measured size distributions closely followed each other for each sample, and size distributions in both showed maxima at the same nanoparticle size. The SAXS-measured nanoparticle diameters were slightly larger than the respective diameters measured by TEM. This was because SAXS measures an agglomerate consisting of several particles as one big particle which slightly increased the mean diameter. TEM- and SAXS-measured mean diameters when plotted together showed similar trend in the variation in the size as the laser power was changed which along with extremely similar size distributions for TEM and SAXS validated the application of SAXS for size distribution measurement of the synthesized TiO2 nanoparticles.

  17. Small-angle scattering and 3D structure interpretation.

    PubMed

    Trewhella, Jill

    2016-10-01

    This review focuses on advances in the application of solution small-angle scattering (SAS) in structural analysis of biomolecules and the complexes they form. Examples highlighted illustrate the unique contribution of SAS, using both X-rays and neutrons, in hybrid or integrative modelling methods. The increased information content when neutron scattering with contrast variation is used is a particular focus. Finally, progress toward an agreed reporting framework, the development of open data and model archives, and the importance of these initiatives is covered.

  18. Study of M1 and E1 excitations by high-resolution proton inelastic scattering measurement at forward angles

    SciTech Connect

    Tamii, A.; Adachi, T.; Hatanaka, K.; Hashimoto, H.; Kaneda, T.; Matsubara, H.; Okamura, H.; Sakemi, Y.; Shimizu, Y.; Tameshige, Y.; Yosoi, M.; Carter, J.; Dozono, M.; Fujita, H.; Fujita, Y.; Itoh, M.; Kawabata, T.; Nakanishi, K.; Sasamoto, Y.; Neumann-Cosel, P. von

    2007-06-13

    Experimental technique for measuring proton inelastic scattering with high-resolution at 295 MeV and at forward angles including zero degrees is described. The method is useful for extracting spin part of the M1 strength via nuclear excitation as well as E1 strength via Coulomb excitation. An excitation energy resolution of 20 keV, good scattering angle resolution, and low background condition have been achieved. The experimental technique was applied for several sd and pf shell nuclei.

  19. Inverse near-critical-angle scattering as a tool to characterize bubble clouds

    NASA Astrophysics Data System (ADS)

    Onofri, Fabrice R. A.; Krzysiek, Mariusz; Barbosa, Séverine; Wozniak, Mariusz; Mroczka, Janusz; Yuan, Yijia; Ren, Kuan-Fang

    2010-02-01

    Under real flow conditions, the critical-angle scattering of a spherical bubble is too noisy to obtain directly the bubble diameter and refractive index. To solve this problem and to limit the drawback of any counting technique, the critical angle refractometry and sizing (CARS) technique has been extended as a collective ensemble technique. As an inverse method it allows to get the size distribution and composition of a cloud of bubbles. In this paper we review the principle, the advantages and limits of this new optical particle characterization method.

  20. SANS (small-angle neutron scattering) from polymers and colloids

    SciTech Connect

    Hayter, J.B.

    1987-01-01

    Small-angle neutron scattering (SANS) has been remarkably successful in providing detailed quantitative structural information on complex everyday materials, such as polymers and colloids, which are often of considerable industrial as well as academic interest. This paper reviews some recent SANS experiments on polymers and colloids, including ferrofluids, and discusses the use of these apparently complex systems as general physical models of the liquid or solid state.

  1. Large-angle Bhabha scattering at LEP 1

    NASA Astrophysics Data System (ADS)

    Beenakker, Wim; Passarino, Giampiero

    1998-04-01

    A critical assessment is given of the theoretical uncertainty in the predicted cross-sections for large-angle Bhabha scattering at LEP 1, with or without t-channel subtraction. To this end a detailed comparison is presented of the results obtained with the programs ALIBABA and TOPAZ0. Differences in the implementation of the radiative corrections and the effect of missing higher-order terms are critically discussed. © 1998

  2. Wide-angle light scattering (WALS) for soot aggregate characterization

    SciTech Connect

    Oltmann, Hergen; Reimann, Joerg; Will, Stefan

    2010-03-15

    A novel set-up for the experimental determination of aggregate morphology in combustion processes based on elastic light scattering has been designed and realized. A key feature of this wide-angle light scattering (WALS) approach is an ellipsoidal mirror which is used to collect scattered light over a wide angular range of about 10-170 . The set-up employs a cw solid-state laser as light source and an intensified CCD-camera as detector. By means of the mirror the scattered light is imaged onto the detector allowing for a simultaneous acquisition of a full scattering diagram with a high angular resolution of about 0.6 . To demonstrate the performance of the approach, measurements for various sooting flames produced by premixed combustion in a flat flame burner were carried out, where the burner was operated with different equivalence ratios and fuels. It is shown that radii of gyration of soot particles may efficiently be obtained from an analysis of the scattering diagrams. (author)

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

    NASA Astrophysics Data System (ADS)

    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.

  4. Development of wide-angle 2D light scattering static cytometry

    NASA Astrophysics Data System (ADS)

    Xie, Linyan; Liu, Qiao; Shao, Changshun; Su, Xuantao

    2016-10-01

    We have recently developed a 2D light scattering static cytometer for cellular analysis in a label-free manner, which measures side scatter (SSC) light in the polar angular range from 79 to 101 degrees. Compared with conventional flow cytometry, our cytometric technique requires no fluorescent labeling of the cells, and static cytometry measurements can be performed without flow control. In this paper we present an improved label-free static cytometer that can obtain 2D light scattering patterns in a wider angular range. By illuminating the static microspheres on chip with a scanning optical fiber, wide-angle 2D light scattering patterns of single standard microspheres with a mean diameter of 3.87 μm are obtained. The 2D patterns of 3.87 μm microspheres contain both large-angle forward scatter (FSC) and SSC light in the polar angular range from 40 to 100 degrees, approximately. Experimental 2D patterns of 3.87 μm microspheres are in good agreement with Mie theory simulated ones. The wide-angle light scattering measurements may provide a better resolution for particle analysis as compared with the SSC measurements. Two dimensional light scattering patterns of HL-60 human acute leukemia cells are obtained by using our static cytometer. Compared with SSC 2D light scattering patterns, wide-angle 2D patterns contain richer information of the HL-60 cells. The obtaining of 2D light scattering patterns in a wide angular range could help to enhance the capabilities of our label-free static cytometry for cell analysis.

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

    NASA Technical Reports Server (NTRS)

    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

  6. The effect of pressure, isotopic (H/D) substitution, and other variables on miscibility in polymer-solvent systems. The nature of the demixing process; dynamic light scattering and small angle neutron scattering studies. Final report

    SciTech Connect

    Van Hook, W.A.

    2000-01-01

    A research program examining the effects of pressure, isotope substitution and other variables on miscibility in polymer solvent systems is described. The techniques employed included phase equilibrium measurements and dynamic light scattering and small angle neutron scattering.

  7. Small Angle X-ray Scattering for Nanoparticle Research.

    PubMed

    Li, Tao; Senesi, Andrew J; Lee, Byeongdu

    2016-09-28

    X-ray scattering is a structural characterization tool that has impacted diverse fields of study. It is unique in its ability to examine materials in real time and under realistic sample environments, enabling researchers to understand morphology at nanometer and angstrom length scales using complementary small and wide angle X-ray scattering (SAXS, WAXS), respectively. Herein, we focus on the use of SAXS to examine nanoscale particulate systems. We provide a theoretical foundation for X-ray scattering, considering both form factor and structure factor, as well as the use of correlation functions, which may be used to determine a particle's size, size distribution, shape, and organization into hierarchical structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well as the combination of SAXS with other X-ray and non-X-ray characterization tools. We conclude with an examination of several key areas of research where X-ray scattering has played a pivotal role, including in situ nanoparticle synthesis, nanoparticle assembly, and operando studies of catalysts and energy storage materials. Throughout this review we highlight the unique capabilities of X-ray scattering for structural characterization of materials in their native environment.

  8. Measuring the distribution of cellulose microfibril angles in primary cell walls by small angle X-ray scattering

    PubMed Central

    2014-01-01

    Background X-ray scattering is a well-established method for measuring cellulose microfibril angles in secondary cell walls. However, little data is available on the much thinner primary cell walls. Here, we show that microfibril orientation distributions can be determined by small angle X-ray scattering (SAXS) even in primary cell walls. The technique offers a number of advantages: samples can be analyzed in the native hydrated state without any preparation which minimizes the risk of artifacts and allows for fast data acquisition. The method provides data averaged over a specimen region, determined by the size of the used X-ray beam and, thus, yields the microfibril orientation distribution within this region. Results Cellulose microfibril orientation distributions were obtained for single cells of the alga Chara corallina, as well as for the multicellular hypocotyl of Arabidopsis thaliana. In both, Chara and Arabidopsis, distributions with a broad scattering around mean microfibril angles of approximately 0° and 90° towards the longitudinal axis of the cells were found. Conclusions With SAXS, the structure of primary cell walls can be analysed in their native state and new insights into the cellulose microfibril orientation of primary cell walls can be gained. The data shows that SAXS can serve as a valuable tool for the analysis of cellulose microfibril orientation in primary cell walls and, in consequence, add to the understanding of its mechanical behaviour and the intriguing mechanisms behind cell growth. PMID:25170343

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

    PubMed

    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.

  10. Survey of background scattering from materials found in small-angle neutron scattering

    PubMed Central

    Barker, J. G.; Mildner, D. F. R.

    2015-01-01

    Measurements and calculations of beam attenuation and background scattering for common materials placed in a neutron beam are presented over the temperature range of 300–700 K. Time-of-flight (TOF) measurements have also been made, to determine the fraction of the background that is either inelastic or quasi-elastic scattering as measured with a 3He detector. Other background sources considered include double Bragg diffraction from windows or samples, scattering from gases, and phonon scattering from solids. Background from the residual air in detector vacuum vessels and scattering from the 3He detector dome are presented. The thickness dependence of the multiple scattering correction for forward scattering from water is calculated. Inelastic phonon background scattering at small angles for crystalline solids is both modeled and compared with measurements. Methods of maximizing the signal-to-noise ratio by material selection, choice of sample thickness and wavelength, removal of inelastic background by TOF or Be filters, and removal of spin-flip scattering with polarized beam analysis are discussed. PMID:26306088

  11. Survey of background scattering from materials found in small-angle neutron scattering.

    PubMed

    Barker, J G; Mildner, D F R

    2015-08-01

    Measurements and calculations of beam attenuation and background scattering for common materials placed in a neutron beam are presented over the temperature range of 300-700 K. Time-of-flight (TOF) measurements have also been made, to determine the fraction of the background that is either inelastic or quasi-elastic scattering as measured with a (3)He detector. Other background sources considered include double Bragg diffraction from windows or samples, scattering from gases, and phonon scattering from solids. Background from the residual air in detector vacuum vessels and scattering from the (3)He detector dome are presented. The thickness dependence of the multiple scattering correction for forward scattering from water is calculated. Inelastic phonon background scattering at small angles for crystalline solids is both modeled and compared with measurements. Methods of maximizing the signal-to-noise ratio by material selection, choice of sample thickness and wavelength, removal of inelastic background by TOF or Be filters, and removal of spin-flip scattering with polarized beam analysis are discussed.

  12. Small-angle neutron scattering study of polymeric micellar structures

    SciTech Connect

    Wu, G.; Chu, B. ); Schneider, D.K. )

    1994-11-17

    Polymeric micellar structures formed by a PEO-PPO-PEO copolymer in o-xylene in the presence of water were investigated by small-angle neutron scattering. In order to reveal the detailed micellar structure, different contrasts among the micellar core, the micellar shell, and the dispersing medium (background) were constructed by selectively changing the protonated/deuterated combination of water and xylene. The micellar structure could be well described by a core-shell structure with the scattering behavior of the micellar shell being very similar to that of a star polymer. The solubilized water existed not only in the micellar core but also in the micellar shell. The volume fraction of a copolymer segments in the micellar shell was rather low, being of the order of 0.2. There seemed to be no sharp interface between the micellar core and the micellar shell. 25 refs., 11 figs., 4 tabs.

  13. Small-angle scattering study of Aspergillus awamori glycoprotein glucoamylase

    NASA Astrophysics Data System (ADS)

    Schmidt, A. E.; Shvetsov, A. V.; Kuklin, A. I.; Lebedev, D. V.; Surzhik, M. A.; Sergeev, V. R.; Isaev-Ivanov, V. V.

    2016-01-01

    Glucoamylase from fungus Aspergillus awamori is glycoside hydrolase that catalyzes the hydrolysis of α-1,4- and α-1,6-glucosidic bonds in glucose polymers and oligomers. This glycoprotein consists of a catalytic domain and a starch-binding domain connected by an O-glycosylated polypeptide chain. The conformation of the linker, the relative arrangement of the domains, and the structure of the full-length enzyme are unknown. The structure of the recombinant glucoamylase GA1 was studied by molecular modelling and small-angle neutron scattering (SANS) methods. The experimental SANS data provide evidence that glucoamylase exists as a monomer in solution and contains a glycoside component, which makes a substantial contribution to the scattering. The model of full-length glucoamylase, which was calculated without taking into account the effect of glycosylation, is consistent with the experimental data and has a radius of gyration of 33.4 ± 0.6 Å.

  14. Small-angle scattering study of Aspergillus awamori glycoprotein glucoamylase

    SciTech Connect

    Schmidt, A. E. Shvetsov, A. V.; Kuklin, A. I.; Lebedev, D. V.; Surzhik, M. A.; Sergeev, V. R.; Isaev-Ivanov, V. V.

    2016-01-15

    Glucoamylase from fungus Aspergillus awamori is glycoside hydrolase that catalyzes the hydrolysis of α-1,4- and α-1,6-glucosidic bonds in glucose polymers and oligomers. This glycoprotein consists of a catalytic domain and a starch-binding domain connected by an O-glycosylated polypeptide chain. The conformation of the linker, the relative arrangement of the domains, and the structure of the full-length enzyme are unknown. The structure of the recombinant glucoamylase GA1 was studied by molecular modelling and small-angle neutron scattering (SANS) methods. The experimental SANS data provide evidence that glucoamylase exists as a monomer in solution and contains a glycoside component, which makes a substantial contribution to the scattering. The model of full-length glucoamylase, which was calculated without taking into account the effect of glycosylation, is consistent with the experimental data and has a radius of gyration of 33.4 ± 0.6 Å.

  15. Ultra-small-angle neutron scattering with azimuthal asymmetry.

    PubMed

    Gu, X; Mildner, D F R

    2016-06-01

    Small-angle neutron scattering (SANS) measurements from thin sections of rock samples such as shales demand as great a scattering vector range as possible because the pores cover a wide range of sizes. The limitation of the scattering vector range for pinhole SANS requires slit-smeared ultra-SANS (USANS) measurements that need to be converted to pinhole geometry. The desmearing algorithm is only successful for azimuthally symmetric data. Scattering from samples cut parallel to the plane of bedding is symmetric, exhibiting circular contours on a two-dimensional detector. Samples cut perpendicular to the bedding show elliptically dependent contours with the long axis corresponding to the normal to the bedding plane. A method is given for converting such asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry SANS data. The aspect ratio from the SANS data is used to modify the slit-smeared USANS data to produce quasi-symmetric contours. Rotation of the sample about the incident beam may result in symmetric data but cannot extract the same information as obtained from pinhole geometry.

  16. Ultra-small-angle neutron scattering with azimuthal asymmetry

    SciTech Connect

    Gu, X.; Mildner, D. F. R.

    2016-05-16

    Small-angle neutron scattering (SANS) measurements from thin sections of rock samples such as shales demand as great a scattering vector range as possible because the pores cover a wide range of sizes. The limitation of the scattering vector range for pinhole SANS requires slit-smeared ultra-SANS (USANS) measurements that need to be converted to pinhole geometry. The desmearing algorithm is only successful for azimuthally symmetric data. Scattering from samples cut parallel to the plane of bedding is symmetric, exhibiting circular contours on a two-dimensional detector. Samples cut perpendicular to the bedding show elliptically dependent contours with the long axis corresponding to the normal to the bedding plane. A method is given for converting such asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry SANS data. Furthermore, the aspect ratio from the SANS data is used to modify the slit-smeared USANS data to produce quasi-symmetric contours. Rotation of the sample about the incident beam may result in symmetric data but cannot extract the same information as obtained from pinhole geometry.

  17. Ultra-small-angle neutron scattering with azimuthal asymmetry

    DOE PAGES

    Gu, X.; Mildner, D. F. R.

    2016-05-16

    Small-angle neutron scattering (SANS) measurements from thin sections of rock samples such as shales demand as great a scattering vector range as possible because the pores cover a wide range of sizes. The limitation of the scattering vector range for pinhole SANS requires slit-smeared ultra-SANS (USANS) measurements that need to be converted to pinhole geometry. The desmearing algorithm is only successful for azimuthally symmetric data. Scattering from samples cut parallel to the plane of bedding is symmetric, exhibiting circular contours on a two-dimensional detector. Samples cut perpendicular to the bedding show elliptically dependent contours with the long axis corresponding tomore » the normal to the bedding plane. A method is given for converting such asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry SANS data. Furthermore, the aspect ratio from the SANS data is used to modify the slit-smeared USANS data to produce quasi-symmetric contours. Rotation of the sample about the incident beam may result in symmetric data but cannot extract the same information as obtained from pinhole geometry.« less

  18. Characterization of photosynthetic supramolecular assemblies using small angle neutron scattering

    SciTech Connect

    Tiede, D.M.; Marone, P.; Wagner, A.M.; Thiyagarajan, P.

    1995-12-31

    We are using small angle neutron scattering (SANS) to resolve structural features of supramolecular assemblies of photosynthetic proteins in liquid and frozen solutions. SANS resolves the size, shape, and structural homogeneity of macromolecular assemblies in samples identical to those used for spectroscopic assays of photosynthetic function. Likely molecular structures of the supramolecular assemblies can be identified by comparing experimental scattering data with scattering profiles calculated for model supramolecular assemblies built from crystal structures of the individual proteins. SANS studies of the Rhodobacter sphaeroides reaction center, RC, presented here, show that the detergent solubilized RC exists in a variety of monomeric and aggregation states. The distribution between monomer and aggregate was found to depend strongly upon detergent, temperature and nature of additives, such as ethylene glycol used for low temperature spectroscopy and polyethylene glycol used for crystallization. Likely aggregate structures are being identified by fitting the experimental scattering profiles with those calculated for model aggregates built-up using the RC crystal structure. This work establishes the foundation for using SANS to identify intermediates in the RC crystallization pathways, and for determining likely structures of complexes formed between the RC and its physiological reaction partners, cytochrome c, and the LHI antenna complex.

  19. Ultra-small-angle neutron scattering with azimuthal asymmetry

    PubMed Central

    Gu, X.; Mildner, D. F. R.

    2016-01-01

    Small-angle neutron scattering (SANS) measurements from thin sections of rock samples such as shales demand as great a scattering vector range as possible because the pores cover a wide range of sizes. The limitation of the scattering vector range for pinhole SANS requires slit-smeared ultra-SANS (USANS) measurements that need to be converted to pinhole geometry. The desmearing algorithm is only successful for azimuthally symmetric data. Scattering from samples cut parallel to the plane of bedding is symmetric, exhibiting circular contours on a two-dimensional detector. Samples cut perpendicular to the bedding show elliptically dependent contours with the long axis corresponding to the normal to the bedding plane. A method is given for converting such asymmetric data collected on a double-crystal diffractometer for concatenation with the usual pinhole-geometry SANS data. The aspect ratio from the SANS data is used to modify the slit-smeared USANS data to produce quasi-symmetric contours. Rotation of the sample about the incident beam may result in symmetric data but cannot extract the same information as obtained from pinhole geometry. PMID:27275140

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

    SciTech Connect

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

    2007-01-19

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

  1. Dual-angle, self-calibrating Thomson scattering measurements in RFX-MOD

    SciTech Connect

    Giudicotti, L.

    2014-11-15

    In the multipoint Thomson scattering (TS) system of the RFX-MOD experiment the signals from a few spatial positions can be observed simultaneously under two different scattering angles. In addition the detection system uses optical multiplexing by signal delays in fiber optic cables of different length so that the two sets of TS signals can be observed by the same polychromator. Owing to the dependence of the TS spectrum on the scattering angle, it was then possible to implement self-calibrating TS measurements in which the electron temperature T{sub e}, the electron density n{sub e} and the relative calibration coefficients of spectral channels sensitivity C{sub i} were simultaneously determined by a suitable analysis of the two sets of TS data collected at the two angles. The analysis has shown that, in spite of the small difference in the spectra obtained at the two angles, reliable values of the relative calibration coefficients can be determined by the analysis of good S/N dual‑angle spectra recorded in a few tens of plasma shots. This analysis suggests that in RFX-MOD the calibration of the entire set of TS polychromators by means of the similar, dual-laser (Nd:YAG/Nd:YLF) TS technique, should be feasible.

  2. Dual-angle, self-calibrating Thomson scattering measurements in RFX-MOD

    NASA Astrophysics Data System (ADS)

    Giudicotti, L.; Pasqualotto, R.; Fassina, A.

    2014-11-01

    In the multipoint Thomson scattering (TS) system of the RFX-MOD experiment the signals from a few spatial positions can be observed simultaneously under two different scattering angles. In addition the detection system uses optical multiplexing by signal delays in fiber optic cables of different length so that the two sets of TS signals can be observed by the same polychromator. Owing to the dependence of the TS spectrum on the scattering angle, it was then possible to implement self-calibrating TS measurements in which the electron temperature Te, the electron density ne and the relative calibration coefficients of spectral channels sensitivity Ci were simultaneously determined by a suitable analysis of the two sets of TS data collected at the two angles. The analysis has shown that, in spite of the small difference in the spectra obtained at the two angles, reliable values of the relative calibration coefficients can be determined by the analysis of good S/N dual-angle spectra recorded in a few tens of plasma shots. This analysis suggests that in RFX-MOD the calibration of the entire set of TS polychromators by means of the similar, dual-laser (Nd:YAG/Nd:YLF) TS technique, should be feasible.

  3. Single-shot measurement of soot aggregate sizes by wide-angle light scattering (WALS)

    NASA Astrophysics Data System (ADS)

    Oltmann, H.; Reimann, J.; Will, S.

    2012-01-01

    The wide-angle light scattering (WALS) approach has been utilized for the measurement of soot aggregate sizes (radii of gyration) in flames on a single-shot basis. Key elements are a pulsed laser and an ellipsoidal mirror, which images the light scattered within a plane onto an intensified CCD camera, thus allowing for an instantaneous acquisition of a full scattering diagram with high resolution. Results for a laminar premixed flame exhibit good agreement with averaged data and demonstrate the feasibility of the method. The applicability of the technique to unsteady combustion processes is demonstrated by measuring aggregate sizes in a weakly turbulent jet-diffusion flame. In both cases light scattering results are verified by data obtained from electron microscopy analysis of sampled soot.

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

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

    PubMed Central

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

    2016-01-01

    Sensitivity to sub-pixel sample features has been demonstrated as a valuable capability of phase contrast x-ray imaging. Here, we report on a method to obtain angular-resolved small angle x-ray scattering distributions with edge-illumination- based imaging utilizing incoherent illumination from an x-ray tube. Our approach provides both the three established image modalities (absorption, differential phase and scatter strength), plus a number of additional contrasts related to unresolved sample features. The complementarity of these contrasts is experimentally validated by using different materials in powder form. As a significant application example we show that the extended complementary contrasts could allow the diagnosis of pulmonary emphysema in a murine model. In support of this, we demonstrate that the properties of the retrieved scattering distributions are consistent with the expectation of increased feature sizes related to pulmonary emphysema. Combined with the simplicity of implementation of edge-illumination, these findings suggest a high potential for exploiting extended sub-pixel contrasts in the diagnosis of lung diseases and beyond. PMID:27491917

  6. A polarization-based Thomson scattering technique for burning plasmas

    NASA Astrophysics Data System (ADS)

    Parke, E.; Mirnov, V. V.; Den Hartog, D. J.

    2014-02-01

    The traditional Thomson scattering diagnostic is based on measurement of the wavelength spectrum of scattered light, where electron temperature measurements are inferred from thermal broadening of the spectrum. At sufficiently high temperatures, especially those predicted for ITER and other burning plasmas, relativistic effects cause a change in the degree of polarization (P) of the scattered light; for fully polarized incident laser light, the scattered light becomes partially polarized. The resulting reduction of polarization is temperature dependent and has been proposed by other authors as a potential alternative to the traditional spectral decomposition technique. Following the previously developed Stokes vector approach, we analytically calculate the degree of polarization for incoherent Thomson scattering. For the first time, we obtain exact results valid for the full range of incident laser polarization states, scattering angles, and electron temperatures. While previous work focused only on linear polarization, we show that circularly polarized incident light optimizes the degree of depolarization for a wide range of temperatures relevant to burning plasmas. We discuss the feasibility of a polarization based Thomson scattering diagnostic for ITER-like plasmas with both linearly and circularly polarized light and compare to the traditional technique.

  7. LIGHT SCATTERING: Fast path-integration technique in simulation of light propagation through highly scattering objects

    NASA Astrophysics Data System (ADS)

    Voronov, Aleksandr V.; Tret'yakov, Evgeniy V.; Shuvalov, Vladimir V.

    2004-06-01

    Based on the path-integration technique and the Metropolis method, the original calculation scheme is developed for solving the problem of light propagation through highly scattering objects. The elimination of calculations of 'unnecessary' realisations and the phenomenological description of processes of multiple small-angle scattering provided a drastic increase (by nine and more orders of magnitude) in the calculation rate, retaining the specific features of the problem (consideration of spatial inhomogeneities, boundary conditions, etc.). The scheme allows one to verify other fast calculation algorithms and to obtain information required to reconstruct the internal structure of highly scattering objects (of size ~1000 scattered lengths and more) by the method of diffusion optical tomography.

  8. A novel small-angle neutron scattering detector geometry

    PubMed Central

    Kanaki, Kalliopi; Jackson, Andrew; Hall-Wilton, Richard; Piscitelli, Francesco; Kirstein, Oliver; Andersen, Ken H.

    2013-01-01

    A novel 2π detector geometry for small-angle neutron scattering (SANS) applications is presented and its theoretical performance evaluated. Such a novel geometry is ideally suited for a SANS instrument at the European Spallation Source (ESS). Motivated by the low availability and high price of 3He, the new concept utilizes gaseous detectors with 10B as the neutron converter. The shape of the detector is inspired by an optimization process based on the properties of the conversion material. Advantages over the detector geometry traditionally used on SANS instruments are discussed. The angular and time resolutions of the proposed detector concept are shown to satisfy the requirements of the particular SANS instrument. PMID:24046504

  9. Small angle neutron scattering studies of vesicle stability

    SciTech Connect

    Mang, J.T.; Hjelm, R.P.

    1997-10-01

    Small angle neutron scattering (SANS) was used to investigate the structure of mixed colloids of egg yolk phosphatidylcholine (EYPC) with the bile salt, cholylglycine (CG), in D{sub 2}O as a function of pressure (P) and temperature (T). At atmospheric pressure, the system forms an isotropic phase of mixed, single bilayer vesicles (SLV`s). Increasing the external hydrostatic pressure brought about significant changes in particle morphology. At T = 25 C, application of a pressure of 3.5 MPa resulted in the collapse of the SLV`s. Further increase of P, up to 51.8 MPa, resulted in a transition from a phase of ordered (stacked), collapsed vesicles to one of stacked, ribbon-like particles. A similar collapse of the vesicles was observed at higher temperature (T = 37 C) with increasing P, but at this temperature, no ribbon phase was found at the highest pressure explored.

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

    SciTech Connect

    Koerstgens, V.; Meier, R.; Ruderer, M. A.; Guo, S.; Chiang, H.-Y.; Mueller-Buschbaum, P.; Perlich, J.; Roth, S. V.; Gehrke, R.

    2012-07-15

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

  11. Small-angle X-ray scattering method to characterize molecular interactions: Proof of concept.

    PubMed

    Allec, Nicholas; Choi, Mina; Yesupriya, Nikhil; Szychowski, Brian; White, Michael R; Kann, Maricel G; Garcin, Elsa D; Daniel, Marie-Christine; Badano, Aldo

    2015-07-10

    Characterizing biomolecular interactions is crucial to the understanding of biological processes. Existing characterization methods have low spatial resolution, poor specificity, and some lack the capability for deep tissue imaging. We describe a novel technique that relies on small-angle X-ray scattering signatures from high-contrast molecular probes that correlate with the presence of biomolecular interactions. We describe a proof-of-concept study that uses a model system consisting of mixtures of monomer solutions of gold nanoparticles (GNPs) as the non-interacting species and solutions of GNP dimers linked with an organic molecule (dimethyl suberimidate) as the interacting species. We report estimates of the interaction fraction obtained with the proposed small-angle X-ray scattering characterization method exhibiting strong correlation with the known relative concentration of interacting and non-interacting species.

  12. Dual wavelength multiple-angle light scattering system for cryptosporidium detection

    NASA Astrophysics Data System (ADS)

    Buaprathoom, S.; Pedley, S.; Sweeney, S. J.

    2012-06-01

    A simple, dual wavelength, multiple-angle, light scattering system has been developed for detecting cryptosporidium suspended in water. Cryptosporidium is a coccidial protozoan parasite causing cryptosporidiosis; a diarrheal disease of varying severity. The parasite is transmitted by ingestion of contaminated water, particularly drinking-water, but also accidental ingestion of bathing-water, including swimming pools. It is therefore important to be able to detect these parasites quickly, so that remedial action can be taken to reduce the risk of infection. The proposed system combines multiple-angle scattering detection of a single and two wavelengths, to collect relative wavelength angle-resolved scattering phase functions from tested suspension, and multivariate data analysis techniques to obtain characterizing information of samples under investigation. The system was designed to be simple, portable and inexpensive. It employs two diode lasers (violet InGaN-based and red AlGaInP-based) as light sources and silicon photodiodes as detectors and optical components, all of which are readily available. The measured scattering patterns using the dual wavelength system showed that the relative wavelength angle-resolved scattering pattern of cryptosporidium oocysts was significantly different from other particles (e.g. polystyrene latex sphere, E.coli). The single wavelength set up was applied for cryptosporidium oocysts'size and relative refractive index measurement and differential measurement of the concentration of cryptosporidium oocysts suspended in water and mixed polystyrene latex sphere suspension. The measurement results showed good agreement with the control reference values. These results indicate that the proposed method could potentially be applied to online detection in a water quality control system.

  13. Small angle scattering methods to study porous materials under high uniaxial strain

    SciTech Connect

    Le Floch, Sylvie Balima, Félix; Pischedda, Vittoria; Legrand, Franck; San-Miguel, Alfonso

    2015-02-15

    We developed a high pressure cell for the in situ study of the porosity of solids under high uniaxial strain using neutron small angle scattering. The cell comprises a hydraulically actioned piston and a main body equipped with two single-crystal sapphire windows allowing for the neutron scattering of the sample. The sample cavity is designed to allow for a large volume variation as expected when compressing highly porous materials. We also implemented a loading protocol to adapt an existing diamond anvil cell for the study of porous materials by X-ray small angle scattering under high pressure. The two techniques are complementary as the radiation beam and the applied pressure are in one case perpendicular to each other (neutron cell) and in the other case parallel (X-ray cell). We will illustrate the use of these two techniques in the study of lamellar porous systems up to a maximum pressure of 0.1 GPa and 0.3 GPa for the neutron and X-ray cells, respectively. These devices allow obtaining information on the evolution of porosity with pressure in the pore dimension subdomain defined by the wave-numbers explored in the scattering process. The evolution with the applied load of such parameters as the fractal dimension of the pore-matrix interface or the apparent specific surface in expanded graphite and in expanded vermiculite is used to illustrate the use of the high pressure cells.

  14. Small angle scattering methods to study porous materials under high uniaxial strain

    NASA Astrophysics Data System (ADS)

    Le Floch, Sylvie; Balima, Félix; Pischedda, Vittoria; Legrand, Franck; San-Miguel, Alfonso

    2015-02-01

    We developed a high pressure cell for the in situ study of the porosity of solids under high uniaxial strain using neutron small angle scattering. The cell comprises a hydraulically actioned piston and a main body equipped with two single-crystal sapphire windows allowing for the neutron scattering of the sample. The sample cavity is designed to allow for a large volume variation as expected when compressing highly porous materials. We also implemented a loading protocol to adapt an existing diamond anvil cell for the study of porous materials by X-ray small angle scattering under high pressure. The two techniques are complementary as the radiation beam and the applied pressure are in one case perpendicular to each other (neutron cell) and in the other case parallel (X-ray cell). We will illustrate the use of these two techniques in the study of lamellar porous systems up to a maximum pressure of 0.1 GPa and 0.3 GPa for the neutron and X-ray cells, respectively. These devices allow obtaining information on the evolution of porosity with pressure in the pore dimension subdomain defined by the wave-numbers explored in the scattering process. The evolution with the applied load of such parameters as the fractal dimension of the pore-matrix interface or the apparent specific surface in expanded graphite and in expanded vermiculite is used to illustrate the use of the high pressure cells.

  15. Three dimensional scattering center imaging techniques

    NASA Technical Reports Server (NTRS)

    Younger, P. R.; Burnside, W. D.

    1991-01-01

    Two methods to image scattering centers in 3-D are presented. The first method uses 2-D images generated from Inverse Synthetic Aperture Radar (ISAR) measurements taken by two vertically offset antennas. This technique is shown to provide accurate 3-D imaging capability which can be added to an existing ISAR measurement system, requiring only the addition of a second antenna. The second technique uses target impulse responses generated from wideband radar measurements from three slightly different offset antennas. This technique is shown to identify the dominant scattering centers on a target in nearly real time. The number of measurements required to image a target using this technique is very small relative to traditional imaging techniques.

  16. Initial State Helicity Correlation in Wide Angle Compton Scattering

    NASA Astrophysics Data System (ADS)

    Day, Donal; Keller, Dustin; Zhang, Jixie

    2016-03-01

    Wide-angle Compton scattering (WACS) belongs to the family of exclusive processes, with large values of s, - t , and - u , that can reveal nucleon structure. In the pQCD version of WACS, three active quarks and two hard gluons are required to share the momentum. pQCD predictions for the WACS disagree with the cross sections currently available. In contrast, handbag mechanism calculations involving a single quark coupled to the spectator through GPDs, are compatible with the cross sections. Measurements of the longitudinal polarization transfer parameter KLL have been found to be inconsistent with the predictions of pQCD yet consistent with calculations within the handbag mechanism, at least at very large angles. There are handbag calculations, including quark and hadron helicity flip, which contradicts pQCD by finding that KLL ≠ALL . A measurement of ALL has been approved to run at Jefferson Lab and which has the potential to clarify the nature of the reaction mechanism in WACS and illuminate the role of quark orbital angular momentum. It will utilize a pure untagged bremsstrahlung photon beam and a longitudinally polarized proton target. After an introduction, the experiment will be described and the expected results presented.

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

    NASA Astrophysics Data System (ADS)

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

    2007-09-01

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

  18. Numerical Techniques for Scattering from Submerged Objects

    NASA Technical Reports Server (NTRS)

    Werby, M. F.; Tango, G. J.; Gaunaurd, G. C.

    1985-01-01

    To represent the final results in terms of matrices, one expands all appropriate physical quantities in terms of partial wave basis states. This includes expansions for the incident and scattered fields and the surface quantities. The method then utilizes the Huygen-Poincare integral representation for both the exterior and interior solutions, leading to the required matrix equations. One thus deals with matrix equations, the complexity of which depends on the nature of the problem. It is shown that in general a transition matrix T can be obtained relating the incident field A with the scattered field f having the form T = PQ(-1), where f = TA. The structure of Q can be quite complicated and can itself be composed of other matrix inversions such as arise from layered objects. Recent improvements in this method appropriate for a variety of physical problems are focused on, and on their implementation. Results are outlined from scattering simulations for very elongated submerged objects and resonance scattering from elastic solids and shells. The final improvement concerns eigenfunction expansions of surface terms, arising from solution of the interior problem, obtained via a preconditioning technique. This effectively reduces the problem to that of obtaining eigenvalues of a Hermitian operator. This formalism is reviewed for scattering from targets that are rigid, sound-soft, acoustic, elastic solids, elastic shells, and elastic layered objects. Two sets of the more interesting results are presented. The first concerns scattering from elongated objects, and the second to thin elastic spheroids.

  19. Grazing incidence wide angle x-ray scattering at the wiggler beamline BW4 of HASYLAB

    SciTech Connect

    Perlich, J.; Rubeck, J.; Botta, S.; Gehrke, R.; Roth, S. V.; Ruderer, M. A.; Prams, S. M.; Rawolle, M.; Zhong, Q.; Koerstgens, V.; Mueller-Buschbaum, P.

    2010-10-15

    We present an upgrade of the available measurement techniques at the wiggler beamline BW4 of the Hamburger Synchrotronstrahlungslabor (HASYLAB) to grazing incidence wide angle x-ray scattering (GIWAXS). GIWAXS refers to an x-ray diffraction method, which, based on the measurement geometry, is perfectly suited for the investigation of the material crystallinity of surfaces and thin films. It is shown that the overall experimental GIWAXS setup employing a movable CCD-detector provides the capability of reliable and reproducible diffraction measurements in grazing incidence geometry. Furthermore, the potential usage of an additional detector enables the simultaneous or successive measurement of GIWAXS and grazing incidence small angle x-ray scattering (GISAXS). The new capability is illustrated by the microbeam GIWAXS measurement of a thin film of the conjugated polymer poly(3-octylthiophene) (P3OT). The investigation reveals the semicrystalline nature of the P3OT film by a clear identification of the wide angle scattering reflexes up to the third order in the [100]-direction as well as the first order in the [010]-direction. The corresponding microbeam GISAXS measurement on the present morphology complements the characterization yielding the complete sample informa-tion from subnanometer up to micrometer length scales.

  20. Small-angle scattering and morphologies of ultra-flexible microemulsions.

    PubMed

    Prevost, Sylvain; Lopian, Tobias; Pleines, Maximilian; Diat, Olivier; Zemb, Thomas

    2016-12-01

    The phase diagrams of ternary mixtures of partly miscible solvents containing a hydrotropic co-solvent exhibit a variable miscibility gap and one critical point. This work investigates the entire monophasic region far from and near to the miscibility gap in octan-1-ol/ethanol/water, for which ultra-flexible micro-emulsions (UFMEs) are observed by small-angle scattering techniques. SWAXS (combined small- and wide-angle X-ray scattering) allows the elucidation of these types of structure. Three distinct areas can be identified in the phase diagram, with scattering data resembling those from direct, bicontinuous and reverse local structures. These UFMEs are far more polydisperse than their surfactant-based counterparts. Water-rich and solvent-rich domains are only delimited by a small excess of hydrotrope, instead of a well defined surfactant layer of fixed area per molecule. It is shown that all scattering spectra obtained for the nanostructured compositions can be modelled by a simple unified analytical model composed of two uncorrelated contributions. The main one is the Ornstein-Zernike formula for composition fluctuations which gives information about the pseudo-phase domain size. The second is a Lorentzian that captures the structure of at least one of the coexisting pseudo-phases. No Porod law can be measured in the SAXS domain. The proposed expression gives access to two characteristic sizes as well as one inter-aggregate distance.

  1. Small-angle scattering and morphologies of ultra-flexible microemulsions1

    PubMed Central

    Prevost, Sylvain; Lopian, Tobias; Pleines, Maximilian; Diat, Olivier; Zemb, Thomas

    2016-01-01

    The phase diagrams of ternary mixtures of partly miscible solvents containing a hydrotropic co-solvent exhibit a variable miscibility gap and one critical point. This work investigates the entire monophasic region far from and near to the miscibility gap in octan-1-ol/ethanol/water, for which ultra-flexible micro­emulsions (UFMEs) are observed by small-angle scattering techniques. SWAXS (combined small- and wide-angle X-ray scattering) allows the elucidation of these types of structure. Three distinct areas can be identified in the phase diagram, with scattering data resembling those from direct, bicontinuous and reverse local structures. These UFMEs are far more polydisperse than their surfactant-based counterparts. Water-rich and solvent-rich domains are only delimited by a small excess of hydrotrope, instead of a well defined surfactant layer of fixed area per molecule. It is shown that all scattering spectra obtained for the nanostructured compositions can be modelled by a simple unified analytical model composed of two uncorrelated contributions. The main one is the Ornstein–Zernike formula for composition fluctuations which gives information about the pseudo-phase domain size. The second is a Lorentzian that captures the structure of at least one of the coexisting pseudo-phases. No Porod law can be measured in the SAXS domain. The proposed expression gives access to two characteristic sizes as well as one inter-aggregate distance. PMID:27980512

  2. Sizing aerosolized fractal nanoparticle aggregates through Bayesian analysis of wide-angle light scattering (WALS) data

    NASA Astrophysics Data System (ADS)

    Huber, Franz J. T.; Will, Stefan; Daun, Kyle J.

    2016-11-01

    Inferring the size distribution of aerosolized fractal aggregates from the angular distribution of elastically scattered light is a mathematically ill-posed problem. This paper presents a procedure for analyzing Wide-Angle Light Scattering (WALS) data using Bayesian inference. The outcome is probability densities for the recovered size distribution and aggregate morphology parameters. This technique is applied to both synthetic data and experimental data collected on soot-laden aerosols, using a measurement equation derived from Rayleigh-Debye-Gans fractal aggregate (RDG-FA) theory. In the case of experimental data, the recovered aggregate size distribution parameters are generally consistent with TEM-derived values, but the accuracy is impaired by the well-known limited accuracy of RDG-FA theory. Finally, we show how this bias could potentially be avoided using the approximation error technique.

  3. Heparin's solution structure determined by small-angle neutron scattering.

    PubMed

    Rubinson, Kenneth A; Chen, Yin; Cress, Brady F; Zhang, Fuming; Linhardt, Robert J

    2016-12-01

    Heparin is a linear, anionic polysaccharide that is widely used as a clinical anticoagulant. Despite its discovery 100 years ago in 1916, the solution structure of heparin remains unknown. The solution shape of heparin has not previously been examined in water under a range of concentrations, and here is done so in D2 O solution using small-angle neutron scattering (SANS). Solutions of 10 kDa heparin-in the millimolar concentration range-were probed with SANS. Our results show that when sodium concentrations are equivalent to the polyelectrolyte's charge or up to a few hundred millimoles higher, the molecular structure of heparin is compact and the shape could be well modeled by a cylinder with a length three to four times its diameter. In the presence of molar concentrations of sodium, the molecule becomes extended to nearly its full length estimated from reported X-ray measurements on stretched fibers. This stretched form is not found in the presence of molar concentrations of potassium ions. In this high-potassium environment, the heparin molecules have the same shape as when its charges were mostly protonated at pD ≈ 0.5, that is, they are compact and approximately half the length of the extended molecules.

  4. Small angle elastic scattering of protons off of spinless nuclei

    SciTech Connect

    Ling, A.G.

    1988-07-01

    Elastic differential cross sections and analyzing powers for 800 MeV protons incident on /sup 12/C, /sup 40/Ca, and /sup 208/Pb in the momentum transfer range 20 MeV/c < q < 130 MeV/c have been measured. The data was taken with the High Resolution Spectrometer (HRS) at the Los Alamos Meson Physics Facility. Special delay-line drift chambers with dead regions for the beam to pass through them were used to obtain the data. Through the interference of the Coulomb and nuclear contributions to the differential cross section in the small angle region, the ratio of the real to imaginary part of the forward nuclear amplitude ..cap alpha../sub n/(0) = Ref/sub n/(0)/Imf/sub n/(0) is extracted. The importance of knowing this quantity at lower energies in order to study the differences between relativistic and non-relativistic scattering theories is discussed. 130 refs., 60 figs., 12 tabs.

  5. New Very Small Angle Neutron Scattering (VSANS) Instrument

    NASA Astrophysics Data System (ADS)

    Van Every, E.; Deyhim, A.; Kulesza, J.

    2016-09-01

    The design of a new Very Small Angle Neutron Scattering (VSANS) Instrument for use in National Institute of Standards And Technology (NIST) will be discussed. This instrument is similar to a shorter instrument we designed and delivered to ANSTO in Australia called the Bilby SANS instrument. The NIST VSANS and the ANSTO Bilby SANS instruments have very similar dimensions for length and diameter and have similar requirements for internal detector motion, top access port, walkway supports, and ports; however, the Bilby SANS instrument vacuum requirement was lower (7.5×10-5 Torr) and the entire (60,000 pound) vessel was required to move 1.5 meters on external rails with a repeatability of 100 um, which ADC achieved. The NIST VSANS length is 24 meter, internal diameter 2.3 meter with three internal carriages. The NIST VSANS instrument, which covers the usual SANS range will also allow configuration to cover the range between q ∼⃒ 10-4 A-1 to 10-3 A-1 with a sample beam current of (104 neutrons/s). The key requirements are a second position-sensitive detector system having a 1 mm pixel size and a longer sample-detector flight path of 20 m (i.e., a 40 m instrument).

  6. Small and Wide Angle X-ray Scattering studies of biological macromolecules in solution.

    PubMed

    Liu, Li; Boldon, Lauren; Urquhart, Melissa; Wang, Xiangyu

    2013-01-08

    In this paper, Small and Wide Angle X-ray Scattering (SWAXS) analysis of macromolecules is demonstrated through experimentation. SWAXS is a technique where X-rays are elastically scattered by an inhomogeneous sample in the nm-range at small angles (typically 0.1 - 5°) and wide angles (typically > 5°). This technique provides information about the shape, size, and distribution of macromolecules, characteristic distances of partially ordered materials, pore sizes, and surface-to-volume ratio. Small Angle X-ray Scattering (SAXS) is capable of delivering structural information of macromolecules between 1 and 200 nm, whereas Wide Angle X-ray Scattering (WAXS) can resolve even smaller Bragg spacing of samples between 0.33 nm and 0.49 nm based on the specific system setup and detector. The spacing is determined from Bragg's law and is dependent on the wavelength and incident angle. In a SWAXS experiment, the materials can be solid or liquid and may contain solid, liquid or gaseous domains (so-called particles) of the same or another material in any combination. SWAXS applications are very broad and include colloids of all types: metals, composites, cement, oil, polymers, plastics, proteins, foods, and pharmaceuticals. For solid samples, the thickness is limited to approximately 5 mm. Usage of a lab-based SWAXS instrument is detailed in this paper. With the available software (e.g., GNOM-ATSAS 2.3 package by D. Svergun EMBL-Hamburg and EasySWAXS software) for the SWAXS system, an experiment can be conducted to determine certain parameters of interest for the given sample. One example of a biological macromolecule experiment is the analysis of 2 wt% lysozyme in a water-based aqueous buffer which can be chosen and prepared through numerous methods. The preparation of the sample follows the guidelines below in the Preparation of the Sample section. Through SWAXS experimentation, important structural parameters of lysozyme, e.g. the radius of gyration, can be analyzed.

  7. Recent applications of small-angle neutron scattering in strongly interacting soft condensed matter

    NASA Astrophysics Data System (ADS)

    Wignall, G. D.; Melnichenko, Y. B.

    2005-08-01

    Before the application of small-angle neutron scattering (SANS) to the study of polymer structure, chain conformation studies were limited to light and small-angle x-ray scattering techniques, usually conducted in dilute solution owing to the difficulties of separating the inter- and intrachain contributions to the structure. The unique role of neutron scattering in soft condensed matter arises from the difference in the coherent scattering length between deuterium (bD = 0.67 × 10-12 cm) and hydrogen (bH = -0.37 × 10-12 cm), which results in a marked difference in scattering power (contrast) between molecules synthesized from normal (hydrogeneous) and deuterated monomer units. Thus, deuterium labelling techniques may be used to 'stain' molecules and make them 'visible' in the condensed state and other crowded environments, such as concentrated solutions of overlapping chains. For over two decades, SANS has proved to be a powerful tool for studies of structure-property relationships in polymeric systems and has made it possible to extract unique information about their size, shape, conformational changes and molecular associations. These applications are now so numerous that an exhaustive review of the field is no longer practical, so the authors propose to focus on the use of SANS for studies of strongly interacting soft matter systems. This paper will therefore discuss basic theory and practical aspects of the technique and will attempt to explain the physics of scattering with the minimum of unnecessary detail and mathematical rigour. Examples will be given to demonstrate the power of SANS and to show how it has helped to unveil universal aspects of the behaviour of macromolecules in such apparently diverse systems as polymer solutions, blends, polyelectrolytes and supercritical mixtures. The aim of the authors is to aid potential users who have a general scientific background, but no specialist knowledge of scattering, to understand the potential of the

  8. Small-Angle Neutron Scattering study of the NIST mAb reference material

    NASA Astrophysics Data System (ADS)

    Castellanos, Maria Monica; Liu, Yun; Krueger, Susan; Curtis, Joseph

    Monoclonal antibodies (mAbs) are of great interest to the biopharmaceutical industry because they can be engineered to target specific antigens. Due to their importance, the biomanufacturing initiative at NIST is developing an IgG1 mAb reference material `NIST mAb', which can be used by industry, academia, and regulatory authorities. As part of this collaborative effort, we aim at characterizing the reference material using neutron scattering techniques. We have studied the small-angle scattering profile of the NIST mAb in a histidine buffer at 0 and 150 mM NaCl. Using Monte Carlo simulations, we generate an ensemble of structures and calculate their theoretical scattering profile, which can be directly compared with experimental data. Moreover, we analyze the structure factor to understand the effect of solution conditions on the protein-protein interactions. Finally, we have measured the solution scattering of the NIST mAb, while simultaneously performing freeze/thaw cycles, in order to investigate if the solution structure was affected upon freezing. The results from neutron scattering not only support the development of the reference material, but also provide insights on its stability and guide efforts for its development under different formulations.

  9. Correlation between fractal dimension and surface characterization by small angle X-ray scattering in marble.

    PubMed

    Salinas-Nolasco, Manlio Favio; Méndez-Vivar, Juan

    2010-03-16

    Among several analysis techniques applied to the study of surface passivation using dicarboxylic acids, small angle X-ray scattering (SAXS) has proved to be relevant in the physicochemical interpretation of the surface association resulting between calcium carbonate and the molecular structure of malonic acid. It is possible to establish chemical affinity principles through bidimensional geometric analysis in terms of the fractal dimension obtained experimentally by SAXS. In this Article, we present results about the adsorption of malonic acid on calcite, using theoretical and mathematical principles of the fractal dimension.

  10. Spectral data of specular reflectance, narrow-angle transmittance and angle-resolved surface scattering of materials for solar concentrators.

    PubMed

    Good, Philipp; Cooper, Thomas; Querci, Marco; Wiik, Nicolay; Ambrosetti, Gianluca; Steinfeld, Aldo

    2016-03-01

    The spectral specular reflectance of conventional and novel reflective materials for solar concentrators is measured with an acceptance angle of 17.5 mrad over the wavelength range 300-2500 nm at incidence angles 15-60° using a spectroscopic goniometry system. The same experimental setup is used to determine the spectral narrow-angle transmittance of semi-transparent materials for solar collector covers at incidence angles 0-60°. In addition, the angle-resolved surface scattering of reflective materials is recorded by an area-scan CCD detector over the spectral range 350-1050 nm. A comprehensive summary, discussion, and interpretation of the results are included in the associated research article "Spectral reflectance, transmittance, and angular scattering of materials for solar concentrators" in Solar Energy Materials and Solar Cells.

  11. Spectral data of specular reflectance, narrow-angle transmittance and angle-resolved surface scattering of materials for solar concentrators

    PubMed Central

    Good, Philipp; Cooper, Thomas; Querci, Marco; Wiik, Nicolay; Ambrosetti, Gianluca; Steinfeld, Aldo

    2015-01-01

    The spectral specular reflectance of conventional and novel reflective materials for solar concentrators is measured with an acceptance angle of 17.5 mrad over the wavelength range 300−2500 nm at incidence angles 15–60° using a spectroscopic goniometry system. The same experimental setup is used to determine the spectral narrow-angle transmittance of semi-transparent materials for solar collector covers at incidence angles 0–60°. In addition, the angle-resolved surface scattering of reflective materials is recorded by an area-scan CCD detector over the spectral range 350–1050 nm. A comprehensive summary, discussion, and interpretation of the results are included in the associated research article “Spectral reflectance, transmittance, and angular scattering of materials for solar concentrators” in Solar Energy Materials and Solar Cells. PMID:26862556

  12. A new approach to quantification of metamorphism using ultra-small and small angle neutron scattering.

    SciTech Connect

    Anovitz, Lawrence {Larry} M; Lynn, Gary W; Cole, David R

    2009-12-01

    In this paper we report the results of a study using small angle and ultra-small angle neutron scattering techniques (SANS and USANS) to examine the evolution of carbonates during contact metamorphism. Data were obtained from samples collected along two transects in the metamorphosed Hueco limestone at the Marble Canyon, Texas, contact aureole. These samples were collected from the igneous contact out to {approx}1700 m. Scattering curves obtained from these samples show mass fractal behavior at low scattering vectors, and surface fractal behavior at high scattering vectors. Significant changes are observed in the surface and mass fractal dimensions as well as the correlation lengths (pore and grain sizes), surface area to volume ratio and surface Gibbs Free energy as a function of distance, including regions of the aureole outside the range of classic metamorphic petrology. A change from mass-fractal to non-fractal behavior is observed at larger scales near the outer boundary of the aureole that implies significant reorganization of pore distributions early in the metamorphic history. Surface fractal results suggest significant smoothing of grain boundaries, coupled with changes in pore sizes. A section of the scattering curve with a slope less than -4 appears at low-Q in metamorphosed samples, which is not present in unmetamorphosed samples. A strong spike in the surface area to volume ratio is observed in rocks near the mapped metamorphic limit, which is associated with reaction of small amounts of organic material to graphite. It may also represent an increase in pore volume or permeability, suggesting that a high permeability zone forms at the boundary of the aureole and moves outwards as metamorphism progresses. Neutron scattering data also correlate well with transmission electron microscopic (TEM) observations, which show formation of micro- and nanopores and microfractures during metamorphism. The scattering data are, however, quantifiable for a bulk rock

  13. Preparing monodisperse macromolecular samples for successful biological small-angle X-ray and neutron-scattering experiments.

    PubMed

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

    2016-11-01

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

  14. Laser desorption mass spectrometry and small angle neutron scattering of heavy fossil materials

    SciTech Connect

    Hunt, J.E.; Winans, R.E.; Thiyagarajan, P.

    1997-09-01

    The determination of the structural building blocks and the molecular weight range of heavy hydrocarbon materials is of crucial importance in research on their reactivity and for their processing. The chemically and physically heterogenous nature of heavy hydrocarbon materials, such as coals, heavy petroleum fractions, and residues, dictates that their structure and reactivity patterns be complicated. The problem is further complicated by the fact that the molecular structure and molecular weight distribution of these materials is not dependent on a single molecule, but on a complex mixture of molecules which vary among coals and heavy petroleum samples. Laser Desorption mass spectrometry (LDMS) is emerging as a technique for molecular weight determination having found widespread use in biological polymer research, but is still a relatively new technique in the fossil fuel area. Small angle neutron scattering (SANS) provides information on the size and shape of heavy fossil materials. SANS offers the advantages of high penetration power even in thick cells at high temperatures and high contrast for hydrocarbon systems dispersed in deuterated solvents. LDMS coupled with time of flight has the advantages of high sensitivity and transmission and high mass range. We have used LDMS to examine various heavy fossil-derived materials including: long chain hydrocarbons, asphaltenes from petroleum vacuum resids, and coals. This paper describes the application of laser desorption and small angle neutron scattering techniques to the analysis of components in coals, petroleum resids and unsaturated polymers.

  15. Angle-resolved scattering spectroscopy of explosives using an external cavity quantum cascade laser

    SciTech Connect

    Suter, Jonathan D.; Bernacki, Bruce E.; Phillips, Mark C.

    2012-04-01

    Investigation of angle-resolved scattering from solid explosives residues on a car door for non-contact sensing geometries. Illumination with a mid-infrared external cavity quantum cascade laser tuning between 7 and 8 microns was detected both with a sensitive single point detector and a hyperspectral imaging camera. Spectral scattering phenomena were discussed and possibilities for hyperspectral imaging at large scattering angles were outlined.

  16. Structural Analysis of the Flagellar Component Proteins in Solution by Small Angle X-Ray Scattering.

    PubMed

    Lee, Lawrence K

    2017-01-01

    Small angle X-ray scattering is an increasingly utilized method for characterizing the shape and structural properties of proteins in solution. The technique is amenable to very large protein complexes and to dynamic particles with different conformational states. It is therefore ideally suited to the analysis of some flagellar motor components. Indeed, we recently used the method to analyze the solution structure of the flagellar motor protein FliG, which when combined with high-resolution snapshots of conformational states from crystal structures, led to insights into conformational transitions that are important in mediating the self-assembly of the bacterial flagellar motor. Here, we describe procedures for X-ray scattering data collection of flagellar motor components, data analysis, and interpretation.

  17. Small-Angle X-Ray Scattering From RNA, Proteins, And Protein Complexes

    SciTech Connect

    Lipfert, Jan; Doniach, Sebastian; /Stanford U., Phys. Dept. /Stanford U., Appl. Phys. Dept. /SLAC, SSRL

    2007-09-18

    Small-angle X-ray scattering (SAXS) is increasingly used to characterize the structure and interactions of biological macromolecules and their complexes in solution. Although still a low-resolution technique, the advent of high-flux synchrotron sources and the development of algorithms for the reconstruction of 3-D electron density maps from 1-D scattering profiles have made possible the generation of useful low-resolution molecular models from SAXS data. Furthermore, SAXS is well suited for the study of unfolded or partially folded conformational ensembles as a function of time or solution conditions. Here, we review recently developed algorithms for 3-D structure modeling and applications to protein complexes. Furthermore, we discuss the emerging use of SAXS as a tool to study membrane protein-detergent complexes. SAXS is proving useful to study the folding of functional RNA molecules, and finally we discuss uses of SAXS to study ensembles of denatured proteins.

  18. Angle-resolved scattering spectroscopy of explosives using an external cavity quantum cascade laser

    NASA Astrophysics Data System (ADS)

    Suter, Jonathan D.; Bernacki, Bruce E.; Phillips, Mark C.

    2012-01-01

    We present a study of the spectral and angular dependence of the diffuse scatter of mid-infrared (MIR) laser light from explosives residues on surfaces. Experiments were performed using an external cavity quantum cascade laser (ECQCL) tunable between 7 and 8 μm (1270 to 1400 cm-1) for surface illumination. A mercury cadmium telluride (MCT) detector was used to detect backscattered spectra as a function of surface angle at a 2 meter standoff. A ferroelectric focal plane array was used to build hyperspectral images at a 0.5 meter standoff. Residues of RDX, tetryl, and TNT were investigated on surfaces including a painted car door for angles between zero (specular) and 50 degrees. We observe spectral signatures of the explosives in the diffuse scattering geometry which differ significantly from those observed in transmission geometries. Characterization of the scattered light spectra of explosives on surfaces will be essential for understanding the performance of standoff explosives detection instruments and developing robust spectral analysis techniques.

  19. Proton energy and scattering angle radiographs to improve proton treatment planning: a Monte Carlo study

    NASA Astrophysics Data System (ADS)

    Biegun, A. K.; Takatsu, J.; Nakaji, T.; van Goethem, M. J.; van der Graaf, E. R.; Koffeman, E. N.; Visser, J.; Brandenburg, S.

    2016-12-01

    The novel proton radiography imaging technique has a large potential to be used in direct measurement of the proton energy loss (proton stopping power, PSP) in various tissues in the patient. The uncertainty of PSPs, currently obtained from translation of X-ray Computed Tomography (xCT) images, should be minimized from 3-5% or higher to less than 1%, to make the treatment plan with proton beams more accurate, and thereby better treatment for the patient. With Geant4 we simulated a proton radiography detection system with two position-sensitive and residual energy detectors. A complex phantom filled with various materials (including tissue surrogates), was placed between the position sensitive detectors. The phantom was irradiated with 150 MeV protons and the energy loss radiograph and scattering angles were studied. Protons passing through different materials in the phantom lose energy, which was used to create a radiography image of the phantom. The multiple Coulomb scattering of a proton traversing different materials causes blurring of the image. To improve image quality and material identification in the phantom, we selected protons with small scattering angles. A good quality proton radiography image, in which various materials can be recognized accurately, and in combination with xCT can lead to more accurate relative stopping powers predictions.

  20. A novel full-angle scanning light scattering profiler to quantitatively evaluate forward and backward light scattering from intraocular lenses

    SciTech Connect

    Walker, Bennett N.; James, Robert H.; Ilev, Ilko K.; Calogero, Don

    2015-09-15

    Glare, glistenings, optical defects, dysphotopsia, and poor image quality are a few of the known deficiencies of intraocular lenses (IOLs). All of these optical phenomena are related to light scatter. However, the specific direction that light scatters makes a critical difference between debilitating glare and a slightly noticeable decrease in image quality. Consequently, quantifying the magnitude and direction of scattered light is essential to appropriately evaluate the safety and efficacy of IOLs. In this study, we introduce a full-angle scanning light scattering profiler (SLSP) as a novel approach capable of quantitatively evaluating the light scattering from IOLs with a nearly 360° view. The SLSP method can simulate in situ conditions by controlling the parameters of the light source including angle of incidence. This testing strategy will provide a more effective nonclinical approach for the evaluation of IOL light scatter.

  1. Elevation angle alignment of quasi optical receiver mirrors of collective Thomson scattering diagnostic by sawtooth measurementsa)

    NASA Astrophysics Data System (ADS)

    Moseev, D.; Meo, F.; Korsholm, S. B.; Bindslev, H.; Furtula, V.; Kantor, M.; Leipold, F.; Michelsen, P. K.; Nielsen, S. K.; Salewski, M.; Stejner, M.

    2012-10-01

    Localized measurements of the fast ion velocity distribution function and the plasma composition measurements are of significant interest for the fusion community. Collective Thomson scattering (CTS) diagnostics allow such measurements with spatial and temporal resolution. Localized measurements require a good alignment of the optical path in the transmission line. Monitoring the alignment during the experiment greatly benefits the confidence in the CTS measurements. An in situ technique for the assessment of the elevation angle alignment of the receiver is developed. Using the CTS diagnostic on TEXTOR without a source of probing radiation in discharges with sawtooth oscillations, an elevation angle misalignment of 0.9° was found with an accuracy of 0.25°.

  2. Contact angle and contact angle hysteresis measurements using the capillary bridge technique.

    PubMed

    Restagno, Frédéric; Poulard, Christophe; Cohen, Céline; Vagharchakian, Laurianne; Léger, Liliane

    2009-09-15

    A new experimental technique is proposed to easily measure both advancing and receding contact angles of a liquid on a solid surface, with unprecedented accuracy. The technique is based on the analysis of the evolution of a capillary bridge formed between a liquid bath and a solid surface (which needs to be spherical) when the distance between the surface and the liquid bath is slowly varied. The feasibility of the technique is demonstrated using a low-energy perfluorinated surface with two different test liquids (water and hexadecane). A detailed description of both experimental procedures and computational modeling are given, allowing one to determine contact angle values. It is shown that the origin of the high accuracy of this technique relies on the fact that the contact angles are automatically averaged over the whole periphery of the contact. This method appears to be particularly adapted to the characterization of surfaces with very low contact angle hysteresis.

  3. Small-Angle and Ultrasmall-Angle Neutron Scattering (SANS/USANS) Study of New Albany Shale: A Treatise on Microporosity

    SciTech Connect

    Bahadur, Jitendra; Radlinski, Andrzej P.; Melnichenko, Yuri B.; Mastalerz, Maria; Schimmelmann, Arndt

    2014-12-17

    We applied small-angle neutron scattering (SANS) and ultrasmall-angle neutron scattering (USANS) techniques to study the microstructure of several New Albany shales of different maturity. It has been established that the total porosity decreases with maturity and increases somewhat for post-mature samples. A new method of SANS data analysis was developed, which allows the extraction of information about the size range and number density of micropores from the relatively flat scattering intensity observed in the limit of the large scattering vector Q. Macropores and significant number of mesopores are surface fractals, and their structure can be described in terms of the polydisperse spheres (PDSP) model. The model-independent Porod invariant method was employed to estimate total porosity, and the results were compared with the PDSP model results. It has been demonstrated that independent evaluation of incoherent background is crucial for accurate interpretation of the scattering data in the limit of large Q-values. Moreover, pore volumes estimated by the N2 and CO2 adsorption, as well as via the mercury intrusion technique, have been compared with those measured by SANS/USANS, and possible reasons for the observed discrepancies are discussed.

  4. Small-Angle and Ultrasmall-Angle Neutron Scattering (SANS/USANS) Study of New Albany Shale: A Treatise on Microporosity

    DOE PAGES

    Bahadur, Jitendra; Radlinski, Andrzej P.; Melnichenko, Yuri B.; ...

    2014-12-17

    We applied small-angle neutron scattering (SANS) and ultrasmall-angle neutron scattering (USANS) techniques to study the microstructure of several New Albany shales of different maturity. It has been established that the total porosity decreases with maturity and increases somewhat for post-mature samples. A new method of SANS data analysis was developed, which allows the extraction of information about the size range and number density of micropores from the relatively flat scattering intensity observed in the limit of the large scattering vector Q. Macropores and significant number of mesopores are surface fractals, and their structure can be described in terms of themore » polydisperse spheres (PDSP) model. The model-independent Porod invariant method was employed to estimate total porosity, and the results were compared with the PDSP model results. It has been demonstrated that independent evaluation of incoherent background is crucial for accurate interpretation of the scattering data in the limit of large Q-values. Moreover, pore volumes estimated by the N2 and CO2 adsorption, as well as via the mercury intrusion technique, have been compared with those measured by SANS/USANS, and possible reasons for the observed discrepancies are discussed.« less

  5. SCT: a suite of programs for comparing atomistic models with small-angle scattering data.

    PubMed

    Wright, David W; Perkins, Stephen J

    2015-06-01

    Small-angle X-ray and neutron scattering techniques characterize proteins in solution and complement high-resolution structural studies. They are of particular utility when large proteins cannot be crystallized or when the structure is altered by solution conditions. Atomistic models of the averaged structure can be generated through constrained modelling, a technique in which known domain or subunit structures are combined with linker models to produce candidate global conformations. By randomizing the configuration adopted by the different elements of the model, thousands of candidate structures are produced. Next, theoretical scattering curves are generated for each model for trial-and-error fits to the experimental data. From these, a small family of best-fit models is identified. In order to facilitate both the computation of theoretical scattering curves from atomistic models and their comparison with experiment, the SCT suite of tools was developed. SCT also includes programs that provide sequence-based estimates of protein volume (either incorporating hydration or not) and add a hydration layer to models for X-ray scattering modelling. The original SCT software, written in Fortran, resulted in the first atomistic scattering structures to be deposited in the Protein Data Bank, and 77 structures for antibodies, complement proteins and anionic oligosaccharides were determined between 1998 and 2014. For the first time, this software is publicly available, alongside an easier-to-use reimplementation of the same algorithms in Python. Both versions of SCT have been released as open-source software under the Apache 2 license and are available for download from https://github.com/dww100/sct.

  6. How Random are Intrinsically Disordered Proteins? A Small Angle Scattering Perspective

    PubMed Central

    Receveur-Bréchot, Véronique; Durand, Dominique

    2012-01-01

    While the crucial role of intrinsically disordered proteins (IDPs) in the cell cycle is now recognized, deciphering their molecular mode of action at the structural level still remains highly challenging and requires a combination of many biophysical approaches. Among them, small angle X-ray scattering (SAXS) has been extremely successful in the last decade and has become an indispensable technique for addressing many of the fundamental questions regarding the activities of IDPs. After introducing some experimental issues specific to IDPs and in relation to the latest technical developments, this article presents the interest of the theory of polymer physics to evaluate the flexibility of fully disordered proteins. The different strategies to obtain 3-dimensional models of IDPs, free in solution and associated in a complex, are then reviewed. Indeed, recent computational advances have made it possible to readily extract maximum information from the scattering curve with a special emphasis on highly flexible systems, such as multidomain proteins and IDPs. Furthermore, integrated computational approaches now enable the generation of ensembles of conformers to translate the unique flexible characteristics of IDPs by taking into consideration the constraints of more and more various complementary experiment. In particular, a combination of SAXS with high-resolution techniques, such as x-ray crystallography and NMR, allows us to provide reliable models and to gain unique structural insights about the protein over multiple structural scales. The latest neutron scattering experiments also promise new advances in the study of the conformational changes of macromolecules involving more complex systems. PMID:22044150

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

    SciTech Connect

    Chehaidar, A.

    2015-09-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

    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.

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

    PubMed

    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. NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

    PubMed Central

    Zhang, Fan; Kline, R. Joseph; Guthrie, William F.; Ilavsky, Jan

    2017-01-01

    The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008–0.25 Å−1, together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments that employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. The validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification. PMID:28381972

  12. Role of Molecular Flexibility and Colloidal Descriptions of Proteins in Crowded Environments from Small-Angle Scattering.

    PubMed

    Castellanos, Maria Monica; Clark, Nicholas J; Watson, Max C; Krueger, Susan; McAuley, Arnold; Curtis, Joseph E

    2016-12-15

    Small-angle scattering is a powerful technique to study molecular conformation and interactions of proteins in solution and in amorphous solids. We have investigated the role of multiple protein configurations in the interaction parameters derived from small-angle scattering for proteins in concentrated solutions. In order to account for the wide configurational space sampled by proteins, we generate ensembles of atomistic structures for lysozyme and monoclonal antibodies, representing globular and flexible proteins, respectively. While recent work has argued that a colloidal approach is inadequate to model proteins, because of the large configurational space that they sample in solution, we find a range of length scales where colloidal models can be used to describe solution scattering data while simultaneously accounting for structural flexibility. We provide insights to determine the length scales where isotropic colloidal models can be used, and find smoothly varying sets of interaction parameters that encompass ensembles of structures. This approach may play an important role in the definition of long-range interactions in coarse-grained models of flexible proteins with experimental scattering constraints. Additionally, we apply the decoupling approximation to ensembles of lysozyme structures with atomistic detail and observe remarkably different results when using geometric solids, such as ellipsoids. The insights from this study provide guidelines for the analysis of small-angle scattering profiles of proteins in crowded environments.

  13. Broadband and Broad-Angle Low-Scattering Metasurface Based on Hybrid Optimization Algorithm

    PubMed Central

    Wang, Ke; Zhao, Jie; Cheng, Qiang; Dong, Di Sha; Cui, Tie Jun

    2014-01-01

    A broadband and broad-angle low-scattering metasurface is designed, fabricated, and characterized. Based on the optimization algorithm and far-field scattering pattern analysis, we propose a rapid and efficient method to design metasurfaces, which avoids the large amount of time-consuming electromagnetic simulations. Full-wave simulation and measurement results show that the proposed metasurface is insensitive to the polarization of incident waves, and presents good scattering-reduction properties for oblique incident waves. PMID:25089367

  14. Phospholipid Membrane Protection by Sugar Molecules during Dehydration—Insights into Molecular Mechanisms Using Scattering Techniques

    PubMed Central

    Garvey, Christopher J.; Lenné, Thomas; Koster, Karen L.; Kent, Ben; Bryant, Gary

    2013-01-01

    Scattering techniques have played a key role in our understanding of the structure and function of phospholipid membranes. These techniques have been applied widely to study how different molecules (e.g., cholesterol) can affect phospholipid membrane structure. However, there has been much less attention paid to the effects of molecules that remain in the aqueous phase. One important example is the role played by small solutes, particularly sugars, in protecting phospholipid membranes during drying or slow freezing. In this paper, we present new results and a general methodology, which illustrate how contrast variation small angle neutron scattering (SANS) and synchrotron-based X-ray scattering (small angle (SAXS) and wide angle (WAXS)) can be used to quantitatively understand the interactions between solutes and phospholipids. Specifically, we show the assignment of lipid phases with synchrotron SAXS and explain how SANS reveals the exclusion of sugars from the aqueous region in the particular example of hexagonal II phases formed by phospholipids. PMID:23584028

  15. Phospholipid Membrane Protection by Sugar Molecules during Dehydration-Insights into Molecular Mechanisms Using Scattering Techniques

    SciTech Connect

    Garvey, Christopher J.; Lenné, Thomas; Koster, Karen L.; Kent, Ben; Bryant, Gary

    2014-09-24

    Scattering techniques have played a key role in our understanding of the structure and function of phospholipid membranes. These techniques have been applied widely to study how different molecules (e.g., cholesterol) can affect phospholipid membrane structure. However, there has been much less attention paid to the effects of molecules that remain in the aqueous phase. One important example is the role played by small solutes, particularly sugars, in protecting phospholipid membranes during drying or slow freezing. In this paper, we present new results and a general methodology, which illustrate how contrast variation small angle neutron scattering (SANS) and synchrotron-based X-ray scattering (small angle (SAXS) and wide angle (WAXS)) can be used to quantitatively understand the interactions between solutes and phospholipids. Specifically, we show the assignment of lipid phases with synchrotron SAXS and explain how SANS reveals the exclusion of sugars from the aqueous region in the particular example of hexagonal II phases formed by phospholipids.

  16. Resonant scattering and resultant pitch angle evolution of relativistic electrons by plasmaspheric hiss

    NASA Astrophysics Data System (ADS)

    Ni, B.; Bortnik, J.; Thorne, R. M.; Ma, Q.; Chen, L.

    2013-12-01

    Adopting several realistic models for the wave distribution and ambient plasmaspheric density, we perform a comprehensive analysis to evaluate hiss-induced scattering coefficients, the relative role of each resonant harmonic, and the overall effect of hiss scattering on the pitch angle evolution and associated decay (loss) processes of relativistic electrons. The results show that scattering by the equatorial, highly oblique component of the hiss emission is negligible. A quasi-parallel propagating wave model of hiss emissions provides a good approximation for evaluation of scattering rates of ≤ 2 MeV electrons. However, realistic wave propagation angles as a function of latitude along the field line must be taken into account to accurately quantify the rates of hiss scattering above 2 MeV. Ambient plasma density is also a critical parameter that can influence hiss scattering rates and resultant pitch angle evolution of electron flux. While the first order cyclotron and the Landau resonances are dominant for hiss-induced scattering of less than 2 MeV electrons, higher order resonances become important and even dominant at intermediate equatorial pitch angles for ultra-relativistic (≥ 3 MeV) electrons. Hiss induced electron pitch angle evolution consistently shows a relatively rapid initial transport of electrons from high to lower pitch angles, with a gradual approach towards an equilibrium shape, and a final state where the entire distribution decays exponentially with time. Although hiss scattering rates near the loss cone control the pitch angle evolution and the ultimate loss of ultra-relativistic electrons, the presence of a scattering bottleneck (a pronounced drop in diffusion rate at intermediate pitch angles) significantly affects the loss rate and leads to characteristic top hat shaped pitch angle distributions at energies below ~1 MeV. Decay timescales are determined to be on the order of a few days, tens of days, and > 100 days for 500 keV, 2 Me

  17. Multi-angle Light Scattering Device for Aerosol Particle Detection

    DTIC Science & Technology

    2014-12-01

    SUBJECT TERMS b. ABSTRACT 2. REPORT TYPE 17. LIMITATION OF ABSTRACT 15. NUMBER OF PAGES 5d. PROJECT NUMBER 5e. TASK NUMBER 5f. WORK UNIT NUMBER...control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS. Kansas State University 2 Fairchild Hall Manhattan , KS 66506 -1100 31-Jul-2014...currently measuring scattering from Arizona road dust, various sizes of abrasive grits and planning soot studies, some cloud processed. The project

  18. Parity Violation in Forward Angle Elastic Electron-Proton Scattering

    SciTech Connect

    Miller, IV, Grady Wilson

    2001-01-01

    We have measured the parity-violating electroweak asymmetry in the elastic scattering of polarized electrons from the proton at Jefferson Laboratory. The kinematic point (θlab = 12.3 deg. and (Q2) = 0.48 (GeV/c)2) is chosen to provide sensitivity to the strange electric form factor GsE. A 3.36 GeV beam of longitudinally polarized electrons was scattered from protons in a liquid hydrogen target. The scattered flux was detected by a pair of spectrometers which focussed the elastically-scattered electrons onto total-absorption detectors. The detector signals were integrated and digitized by a custom data acquisition system. A feedback system reduced systematic errors by controlling helicity-correlated beam intensity differences at the sub-ppm (part per million) level. The experimental result, A = 14.5 +/- 2.0 (stat) ± 1.1 (syst) ppm, is consistent with the electroweak Standard Model with no additional contributions from strange quarks. In particular, the measurement implies GSE + 0.39 GsM = 0.023 ± 0.040 ± 0.026 (ζGnE), where the last uncertainty is due to the estimated uncertainty in the neutron electric form factor GnE . This result represents the first experimental constraint of the strange electric form factor.

  19. Multiple size scale structures in silica/siloxane composites studied by small-angle scattering

    SciTech Connect

    Beaucage, G.; Schaefer, D.W.; Ulibarri, T.; Black, E.

    1993-12-31

    The physical properties of in-situ produced composites, such as the TEOS-polysiloxane based systems, are directly related to the complex interaction of structural features from the nano- to macro-scopic scales. The nature of these structural interactions are a key element in understanding and controlling mechanical properties in these systems. We believe that the smallest scale structures, in the nanometer range, correlate with properties such as the modulus while large-scale structures on the micron scale effect failure in these materials. This paper discusses techniques for analysis of structural features and interrelation of structural features over these wide ranges of size using small-angle light, x-ray and neutron scattering. Combination of data from different instruments allows for characterization of the interaction between these different size scale features.

  20. Structure of nanocrystalline palladium and copper studied by small angle neutron scattering

    SciTech Connect

    Sanders, P.G.; Weertman, J.R.; Barker, J.G.

    1996-12-01

    The structure of nanocrystalline palladium and copper, made by inert gas condensation and compaction, was studied using small angle neutron scattering (SANS), optical microscopy, and scanning electron microscopy. The effects of annealing and warm compaction were also examined with these techniques. The SANS results were interpreted using a maximum entropy routine, combined with knowledge of the Archimedes density and hydrogen concentration determined by prompt gamma activation analysis (PGAA). Similar hydrogen concentrations were detected by SANS and PGAA. This hydrogen content, which was approximately 5 at.{percent} in samples compacted at room temperature, was reduced by both annealing and warm compaction. Defects in several size classes were observed, including missing grain pores ({approx_equal}1{endash}50 nm diameter) and defects of micrometer size. Warm compaction produced a lower number density of pores in nanocrystalline palladium, which led to increased density. The observed structure was correlated with Vickers microhardness and fracture surface morphology. {copyright} {ital 1996 Materials Research Society.}

  1. Angle-resolved spin wave band diagrams of square antidot lattices studied by Brillouin light scattering

    SciTech Connect

    Gubbiotti, G.; Tacchi, S.; Madami, M.; Carlotti, G.; Ding, J.; Adeyeye, A. O.

    2015-06-29

    The Brillouin light scattering technique has been exploited to study the angle-resolved spin wave band diagrams of squared Permalloy antidot lattice. Frequency dispersion of spin waves has been measured for a set of fixed wave vector magnitudes, while varying the wave vector in-plane orientation with respect to the applied magnetic field. The magnonic band gap between the two most dispersive modes exhibits a minimum value at an angular position, which exclusively depends on the product between the selected wave vector magnitude and the lattice constant of the array. The experimental data are in very good agreement with predictions obtained by dynamical matrix method calculations. The presented results are relevant for magnonic devices where the antidot lattice, acting as a diffraction grating, is exploited to achieve multidirectional spin wave emission.

  2. Study of the enzyme ascorbate oxidase by small angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Maritano, S.; Carsughi, F.; Fontana, M. P.; Marchesini, A.

    1996-09-01

    We report a study of the large scale structure of the "blue" copper enzyme ascorbate oxidase by small angle neutron scattering. The enzyme has been extracted from zucchini and studied in solutions of two different preparations. Contrast variation method was used by performing the measurements in water, heavy water and mixtures of H 2OD 2O. Our data show that, at least at the concentrations used here, the gyration radius of the enzyme is about 34 Å; with such a value our analysis is most consistent with a value of 70 KDa for the molecular weight of ascorbate oxidase in the conditions of our experiment. This is in contrast to the generally accepted value of 140 KDa, obtained by other techniques at high concentrations (e.g. greater than 2 mg ml -1). The possible origins of such a discrepancy are discussed.

  3. Toward a Taxonomy of the Denatured State: Small Angle Scattering Studies of Unfolded Proteins

    SciTech Connect

    Millett, I.S.; Doniach, S.; Plaxco, K.W.

    2005-02-15

    Despite the critical role the unfolded state plays in defining protein folding kinetics and thermodynamics (Berg et al., 2002; Dunker, 2002; Shortle, 2002; Wright and Dyson, 2002), our understanding of its detailed structure remains rather rudimentary; the heterogeneity of the unfolded ensemble renders difficult or impossible its study by traditional, atomic-level structural methods. Consequently, recent years have seen a significant expansion of small-angle X-ray and neutron scattering (SAXS and SANS, respectively) techniques that provide direct, albeit rotationally and time-averaged, measures of the geometric properties of the unfolded ensemble. These studies have reached a critical mass, allowing us for the first time to define general observations regarding the nature of the geometry - and possibly the chemistry and physics - of unfolded proteins.

  4. The crystallization of hectorite clays as monitored by small angle X-ray scattering and NMR

    SciTech Connect

    Carrado, K. A.; Xu, L.; Seifert, S.; Gregory, D.; Song, K.; Botto, R. E.

    1999-12-13

    The authors have probed the 48-hr crystallization of a magnesium silicate clay called hectorite. Small angle X-ray scattering (SAXS) at the Advanced Photon Source using aliquots ex situ has revealed that data is consistent with ex situ XRD, TGA, AFM, and IR data in that all these techniques see clay crystallite beginning to form in the first few hours of reaction. Tetraethylammonium (TEA) ions are used to aid crystallization and become incorporated as the exchange cations within the interlayers. {sup 13}C NMR shows that 80% of the final TEA loading is accomplished in the first 10 hrs. {sup 29}Si NMR displays a visible clay silicate peak after just 1 hr. In addition, the first in situ study of clay crystallization of any kind was performed by in situ SAXS. Results are consistent with the ex situ data as well as showing the sensitivity of SAXS to sol gel reactions occurring on the order of minutes.

  5. Micelle structural studies on oil solubilization by a small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Putra, Edy Giri Rachman; Seong, Baek Seok; Ikram, Abarrul

    2009-02-01

    A small-angle neutron scattering (SANS) technique was applied to reveal the micelle structural changes. The micelle structural changes of 0.3 M sodium dodecyl sulfate (SDS) concentration by addition of various oil, i.e. n-hexane, n-octane, and n-decane up to 60% (v/v) have been investigated. It was found that the size, aggregation number and the structures of the micelles changed exhibiting that the effective charge on the micelle decreases with an addition of oil. There was a small increase in minor axis of micelle while the correlation peak shifted to a lower momentum transfer Q and then to higher Q by a further oil addition.

  6. Membrane Structure Studies by Means of Small-Angle Neutron Scattering (SANS)

    SciTech Connect

    Knott, R. B.

    2008-03-17

    summary of membrane structure will be followed by an outline of the neutron scattering techniques used to understand membrane structure and dynamics. The emphasis will be on the small angle neutron scattering technique since there is a very powerful instrument at Serpong, however brief mention of other techniques will be included to demonstrate how a multidisciplinary approach is usually required.

  7. Measurement of energy spectra of small-angle scattering and distribution of optical microinhomogeneities in laser ceramics

    SciTech Connect

    Tverdokhleb, P E; Shepetkin, Yu A; Steinberg, I Sh; Belikov, A Yu; Vatnik, S M; Vedin, I A; Kurbatov, P F

    2014-06-30

    The energy spectra of small-angle light scattering from the samples of Nd:YAG ceramics and the spatial distributions of optical microinhomogeneities in them are measured. The spatial profiles of microinhomogeneities are found using the collinear heterodyne microprobe technique. Based on the obtained data, the comparison of noise and lasing characteristics of foreign and domestic samples of laser ceramics is carried out. (extreme light fields and their applications)

  8. Thermal degradation of M41S-class mesoporous sieves as revealed by small angle X-ray scattering

    SciTech Connect

    Hunt, J. E.; Xu, L.; Winans, R. E.; Seifert, S.

    2000-02-16

    The authors have studied the temperature stability of M41S class siliceous mesoporous materials loaded with carbonaceous material by temperature programmed small-angle X-ray scattering (TPSAXS) techniques. Results show the thermal structural instability of large pore pure silica sieve material with carbonaceous material (such as coal extracts) occluded within the pores of mesoporous 31 {angstrom} M41S materials. Unfilled pore M41S materials do not show thermal-related structural instability.

  9. Polarization Transfer in Wide-Angle Compton Scattering and Single-Pion Photoproduction from the Proton

    NASA Astrophysics Data System (ADS)

    Fanelli, C.; Cisbani, E.; Hamilton, D. J.; Salmé, G.; Wojtsekhowski, B.; Ahmidouch, A.; Annand, J. R. M.; Baghdasaryan, H.; Beaufait, J.; Bosted, P.; Brash, E. J.; Butuceanu, C.; Carter, P.; Christy, E.; Chudakov, E.; Danagoulian, S.; Day, D.; Degtyarenko, P.; Ent, R.; Fenker, H.; Fowler, M.; Frlez, E.; Gaskell, D.; Gilman, R.; Horn, T.; Huber, G. M.; de Jager, C. W.; Jensen, E.; Jones, M. K.; Kelleher, A.; Keppel, C.; Khandaker, M.; Kohl, M.; Kumbartzki, G.; Lassiter, S.; Li, Y.; Lindgren, R.; Lovelace, H.; Luo, W.; Mack, D.; Mamyan, V.; Margaziotis, D. J.; Markowitz, P.; Maxwell, J.; Mbianda, G.; Meekins, D.; Meziane, M.; Miller, J.; Mkrtchyan, A.; Mkrtchyan, H.; Mulholland, J.; Nelyubin, V.; Pentchev, L.; Perdrisat, C. F.; Piasetzky, E.; Prok, Y.; Puckett, A. J. R.; Punjabi, V.; Shabestari, M.; Shahinyan, A.; Slifer, K.; Smith, G.; Solvignon, P.; Subedi, R.; Wesselmann, F. R.; Wood, S.; Ye, Z.; Zheng, X.

    2015-10-01

    Wide-angle exclusive Compton scattering and single-pion photoproduction from the proton have been investigated via measurement of the polarization transfer from a circularly polarized photon beam to the recoil proton. The wide-angle Compton scattering polarization transfer was analyzed at an incident photon energy of 3.7 GeV at a proton scattering angle of θcmp=70 ° . The longitudinal transfer KLL, measured to be 0.645 ±0.059 ±0.048 , where the first error is statistical and the second is systematic, has the same sign as predicted for the reaction mechanism in which the photon interacts with a single quark carrying the spin of the proton. However, the observed value is ˜3 times larger than predicted by the generalized-parton-distribution-based calculations, which indicates a significant unknown contribution to the scattering amplitude.

  10. Polarization Transfer in Wide-Angle Compton Scattering and Single-Pion Photoproduction from the Proton.

    PubMed

    Fanelli, C; Cisbani, E; Hamilton, D J; Salmé, G; Wojtsekhowski, B; Ahmidouch, A; Annand, J R M; Baghdasaryan, H; Beaufait, J; Bosted, P; Brash, E J; Butuceanu, C; Carter, P; Christy, E; Chudakov, E; Danagoulian, S; Day, D; Degtyarenko, P; Ent, R; Fenker, H; Fowler, M; Frlez, E; Gaskell, D; Gilman, R; Horn, T; Huber, G M; de Jager, C W; Jensen, E; Jones, M K; Kelleher, A; Keppel, C; Khandaker, M; Kohl, M; Kumbartzki, G; Lassiter, S; Li, Y; Lindgren, R; Lovelace, H; Luo, W; Mack, D; Mamyan, V; Margaziotis, D J; Markowitz, P; Maxwell, J; Mbianda, G; Meekins, D; Meziane, M; Miller, J; Mkrtchyan, A; Mkrtchyan, H; Mulholland, J; Nelyubin, V; Pentchev, L; Perdrisat, C F; Piasetzky, E; Prok, Y; Puckett, A J R; Punjabi, V; Shabestari, M; Shahinyan, A; Slifer, K; Smith, G; Solvignon, P; Subedi, R; Wesselmann, F R; Wood, S; Ye, Z; Zheng, X

    2015-10-09

    Wide-angle exclusive Compton scattering and single-pion photoproduction from the proton have been investigated via measurement of the polarization transfer from a circularly polarized photon beam to the recoil proton. The wide-angle Compton scattering polarization transfer was analyzed at an incident photon energy of 3.7 GeV at a proton scattering angle of θ_{cm}^{p}=70°. The longitudinal transfer K_{LL}, measured to be 0.645±0.059±0.048, where the first error is statistical and the second is systematic, has the same sign as predicted for the reaction mechanism in which the photon interacts with a single quark carrying the spin of the proton. However, the observed value is ~3 times larger than predicted by the generalized-parton-distribution-based calculations, which indicates a significant unknown contribution to the scattering amplitude.

  11. Small-angle approximation to the transfer of narrow laser beams in anisotropic scattering media

    NASA Technical Reports Server (NTRS)

    Box, M. A.; Deepak, A.

    1981-01-01

    The broadening and the signal power detected of a laser beam traversing an anisotropic scattering medium were examined using the small-angle approximation to the radiative transfer equation in which photons suffering large-angle deflections are neglected. To obtain tractable answers, simple Gaussian and non-Gaussian functions for the scattering phase functions are assumed. Two other approximate approaches employed in the field to further simplify the small-angle approximation solutions are described, and the results obtained by one of them are compared with those obtained using small-angle approximation. An exact method for obtaining the contribution of each higher order scattering to the radiance field is examined but no results are presented.

  12. Energy-dispersive small-angle X-ray scattering with cone collimation using X-ray capillary optics

    NASA Astrophysics Data System (ADS)

    Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi

    2016-09-01

    Energy-dispersive small-angle X-ray scattering (ED-SAXS) with an innovative design of cone collimation based on an ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL) had been explored. Using this new cone collimation system, scattering angle 2θ has a theoretical minimum angle related to the mean half-opening angle of the hollow cone beam of 1.42 mrad, and with the usable X-ray energy ranging from 4 to 30 keV, the resulting observable scattering vector q is down to a minimum value of about 0.003 Å-1 (or a Bragg spacing of about 2100 Å). However, the absorption of lower energies by X-ray capillary optics, sample transmission, and detector response function limits the application range to lower energy. Cone collimation ED-SAXS experiments carried out on pure water, Lupolen, and in situ temperature-dependent measurement of diacetylenic acid/melamine micelle solid were presented at three different scattering angles 2θ of 0.18°, 0.70° and 1.18° to illustrate the new opportunities offered by this technique as well as its limitations. Also, a comparison has been made by replacing the PPXRL with a pinhole, and the result shows that cone collimation ED-SAXS based on ESBC with PPXRL was helpful in improving the signal-to-noise ratio (i.e., reducing the parasitic background scattering) than ESBC with a pinhole. The cone collimation instrument based on X-ray capillary optics could be considered as a promising tool to perform SAXS experiments, especially cone collimation ED-SAXS has potential application for the in situ temperature-dependent studying on the kinetics of phase transitions.

  13. Angle-Resolved Second-Harmonic Light Scattering from Colloidal Particles

    SciTech Connect

    Yang, N.; Angerer, W. E.; Yodh, A. G.

    2001-09-03

    We report angle-resolved second-harmonic generation (SHG) measurements from suspensions of centrosymmetric micron-size polystyrene spheres with surface-adsorbed dye (malachite green). The second-harmonic scattering profiles differ qualitatively from linear light scattering profiles of the same particles. We investigated these radiation patterns using several polarization configurations and particle diameters. We introduce a simple Rayleigh-Gans-Debye model to account for the SHG scattering anisotropy. The model compares favorably with our experimental data. Our measurements suggest scattering anisotropy may be used to isolate particle nonlinear optics from other bulk nonlinear optical effects in suspension.

  14. Numerical analysis of the Fokker-Planck equation with adiabatic focusing: Realistic pitch-angle scattering

    NASA Astrophysics Data System (ADS)

    Lasuik, J.; Fiege, J. D.; Shalchi, A.

    2017-01-01

    We solve the focused transport equation of cosmic rays numerically to investigate non-isotropic models of the pitch-angle scattering coefficient. In previous work, the Fokker-Planck equation was solved either analytically by using approximations, or by using a numerical approach together with simple models for the pitch-angle scattering coefficient. It is the purpose of the current article so compute particle distribution functions as well as the parallel diffusion coefficient by solving numerically the focused transport equation for a more realistic Fokker-Planck coefficient of pitch-angle scattering. Our analytical form for the scattering parameter is based on non-linear diffusion theory that takes into account realistic scattering at pitch-angles close to 90 ° . This general form contains the isotropic form as well as the quasi-linear limit as special cases. We show that the ratio of the diffusion coefficients with and without focusing sensitively depends on the ratio of the turbulent magnetic field and the mean field. The assumed form of the pitch-angle Fokker-Planck coefficient has an influence on the parallel diffusion coefficient. In all considered cases we found a reduction of the ratio of the diffusion coefficients if the ratio of magnetic fields is reduced.

  15. The dynamic duo: Combining NMR and small angle scattering in structural biology

    PubMed Central

    Hennig, Janosch; Sattler, Michael

    2014-01-01

    Structural biology provides essential information for elucidating molecular mechanisms that underlie biological function. Advances in hardware, sample preparation, experimental methods, and computational approaches now enable structural analysis of protein complexes with increasing complexity that more closely represent biologically entities in the cellular environment. Integrated multidisciplinary approaches are required to overcome limitations of individual methods and take advantage of complementary aspects provided by different structural biology techniques. Although X-ray crystallography remains the method of choice for structural analysis of large complexes, crystallization of flexible systems is often difficult and does typically not provide insights into conformational dynamics present in solution. Nuclear magnetic resonance spectroscopy (NMR) is well-suited to study dynamics at picosecond to second time scales, and to map binding interfaces even of large systems at residue resolution but suffers from poor sensitivity with increasing molecular weight. Small angle scattering (SAS) methods provide low resolution information in solution and can characterize dynamics and conformational equilibria complementary to crystallography and NMR. The combination of NMR, crystallography, and SAS is, thus, very useful for analysis of the structure and conformational dynamics of (large) protein complexes in solution. In high molecular weight systems, where NMR data are often sparse, SAS provides additional structural information and can differentiate between NMR-derived models. Scattering data can also validate the solution conformation of a crystal structure and indicate the presence of conformational equilibria. Here, we review current state-of-the-art approaches for combining NMR, crystallography, and SAS data to characterize protein complexes in solution. PMID:24687405

  16. Synchrotron-based small-angle X-ray scattering (SAXS) of proteins in solution

    PubMed Central

    Skou, Soren; Gillilan, Richard E

    2015-01-01

    Summary With recent advances in data analysis algorithms, X-ray detectors, and synchrotron sources, small-angle X-ray scattering (SAXS) has become much more accessible to the structural biology community than ever before. Although limited to ~10 Å resolution, SAXS can provide a wealth of structural information on biomolecules in solution and is compatible with a wide range of experimental conditions. SAXS is thus an attractive alternative when crystallography is not possible. Moreover, advanced usage of SAXS can provide unique insight into biomolecular behavior that can only be observed in solution, such as large conformational changes and transient protein-protein interactions. Unlike crystal diffraction data, however, solution scattering data are subtle in appearance, highly sensitive to sample quality and experimental errors, and easily misinterpreted. In addition, synchrotron beamlines that are dedicated to SAXS are often unfamiliar to the non-specialist. Here, we present a series of procedures that can be used for SAXS data collection and basic cross-checks designed to detect and avoid aggregation, concentration effects, radiation damage, buffer mismatch, and other common problems. The protein, human serum albumin (HSA), serves as a convenient and easily replicated example of just how subtle these problems can sometimes be, but also of how proper technique can yield pristine data even in problematic cases. Because typical data collection times at a synchrotron are only one to several days, we recommend that the sample purity, homogeneity, and solubility be extensively optimized prior to the experiment. PMID:24967622

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

    PubMed Central

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

    2016-01-01

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

  18. Using Small Angle Neutron Scattering on Glucose Oxidase immobilized on Single Layer Graphene

    NASA Astrophysics Data System (ADS)

    Rai, Durgesh; Gurusaran, M.; Qian, S.; Weiss, K.; Urban, V.; Li, P.; Ma, L.; Ajayan, P.; Narayanan, T.; Sekar, K.; Viswanathan, S.; Renugopalakrishanan, V.

    2015-03-01

    Reliable blood glucose monitoring using biosensors is valuable for health evaluations and medication in wake of chronic diabetic issues accompanying deviations from evolutionary human lifestyle. Glucose oxidase (GOx) is an ideal enzyme because of its specificity and the ability to electrochemically transduce from the enzymatic reaction. We use graphene-based electrode with GOx sensor matrix so that the emitted electrons from sensor matrix can flow across graphene nearly without scattering; crucial for constructing ultrasensitive-sensors. Thereafter, establishing a structure-property based relationships to tune the sensor topology with electrochemically output forms the main focus of the device development process. We have developed a methodology to obtain low-resolution hierarchical models of the aggregate matrix using Small Angle Neutron Scattering (SANS) technique. A Unified Fit model is used in tandem with GNOM, DAMMIN and DAMAVER to construct low-resolution models for GOx matrices. A detailed explanation of a general methodology for obtaining quantitative details aggregate structures along with qualitative models will be presented.

  19. Modeling detergent organization around aquaporin-0 using small-angle X-ray scattering.

    PubMed

    Berthaud, Alice; Manzi, John; Pérez, Javier; Mangenot, Stéphanie

    2012-06-20

    Solubilization of integral membrane proteins in aqueous solutions requires the presence of amphiphilic molecules like detergents. The transmembrane region of the proteins is then surrounded by a corona formed by these molecules, ensuring a hydrophilic outer surface. The presence of this corona has strongly hampered structural studies of solubilized membrane proteins by small-angle X-ray scattering (SAXS), a technique frequently used to monitor conformational changes of soluble proteins. Through the online combination of size exclusion chromatography, SAXS, and refractometry, we have determined a precise geometrical model of the n-dodecyl β-d-maltopyranoside corona surrounding aquaporin-0, the most abundant membrane protein of the eye lens. The SAXS data were well-fitted by a detergent corona shaped in an elliptical toroid around the crystal structure of the protein, similar to the elliptical shape recently reported for nanodiscs (Skar-Gislinge et al. J. Am. Chem. Soc. 2010, 132, 13713-13722). The torus thickness determined from the curve-fitting protocol is in excellent agreement with the thickness of a lipid bilayer, while the number of detergent molecules deduced from the volume of the torus compares well with those obtained on the same sample from refractometry and mass analysis based on SAXS forward scattering. For the first time, the partial specific volume of the detergent surrounding a protein was measured. The present protocol is a crucial step toward future conformational studies of membrane proteins in solution.

  20. Enhanced small-angle scattering connected to the Widom line in simulations of supercooled water

    NASA Astrophysics Data System (ADS)

    Wikfeldt, K. T.; Huang, C.; Nilsson, A.; Pettersson, L. G. M.

    2011-06-01

    We present extensive simulations on the TIP4P/2005 water model showing significantly enhanced small-angle scattering (SAS) in the supercooled regime. The SAS is related to the presence of a Widom line (TW) characterized by maxima in thermodynamic response functions and Ornstein-Zernike correlation length. Recent experimental small-angle x-ray scattering data [Huang et al., J. Chem. Phys. 133, 134504 (2010)], 10.1063/1.3495974 are excellently reproduced, albeit with an increasing temperature offset at lower temperatures. Assuming the same origin of the SAS in experiment and model this suggests the existence of a Widom line also in real supercooled water. Simulations performed at 1000 bar show an increased abruptness of a crossover from dominating high-density (HDL) to dominating low-density (LDL) liquid and strongly enhanced SAS associated with crossing TW, consistent with a recent determination of the critical pressure of TIP4P/2005 at 1350 bar. Furthermore, good agreement with experimental isothermal compressibilities at 1000, 1500, and 2000 bar shows that the high pressure supercooled thermodynamic behavior of water is well described by TIP4P/2005. Analysis of the tetrahedrality parameter Q reveals that the HDL-LDL structural transition is very sharp at 1000 bar, and that structural fluctuations become strongly coupled to density fluctuations upon approaching TW. Furthermore, the tetrahedrality distribution becomes bimodal at ambient temperatures, an observation that possibly provides a link between HDL-LDL fluctuations and the structural bimodality in liquid water indicated by x-ray spectroscopic techniques. Computed x-ray absorption spectra are indeed found to show sensitivity to the tetrahedrality parameter.

  1. Enhanced small-angle scattering connected to the Widom line in simulations of supercooled water.

    PubMed

    Wikfeldt, K T; Huang, C; Nilsson, A; Pettersson, L G M

    2011-06-07

    We present extensive simulations on the TIP4P∕2005 water model showing significantly enhanced small-angle scattering (SAS) in the supercooled regime. The SAS is related to the presence of a Widom line (T(W)) characterized by maxima in thermodynamic response functions and Ornstein-Zernike correlation length. Recent experimental small-angle x-ray scattering data [Huang et al., J. Chem. Phys. 133, 134504 (2010)] are excellently reproduced, albeit with an increasing temperature offset at lower temperatures. Assuming the same origin of the SAS in experiment and model this suggests the existence of a Widom line also in real supercooled water. Simulations performed at 1000 bar show an increased abruptness of a crossover from dominating high-density (HDL) to dominating low-density (LDL) liquid and strongly enhanced SAS associated with crossing T(W), consistent with a recent determination of the critical pressure of TIP4P∕2005 at 1350 bar. Furthermore, good agreement with experimental isothermal compressibilities at 1000, 1500, and 2000 bar shows that the high pressure supercooled thermodynamic behavior of water is well described by TIP4P∕2005. Analysis of the tetrahedrality parameter Q reveals that the HDL-LDL structural transition is very sharp at 1000 bar, and that structural fluctuations become strongly coupled to density fluctuations upon approaching T(W). Furthermore, the tetrahedrality distribution becomes bimodal at ambient temperatures, an observation that possibly provides a link between HDL-LDL fluctuations and the structural bimodality in liquid water indicated by x-ray spectroscopic techniques. Computed x-ray absorption spectra are indeed found to show sensitivity to the tetrahedrality parameter.

  2. A forward-angle-scattering method for the determination of optical constants and particle size distribution by collimated laser irradiation

    NASA Astrophysics Data System (ADS)

    Ren, Yatao; Qi, Hong; Yu, Xiaoying; Ruan, Liming

    2017-04-01

    This study examined the feasibility of using a secondary optimization technique and forward-angle-scattering method to retrieve optical constants (or complex refractive indices) and particle size distribution (PSD) simultaneously. In this work, two continuous wave lasers of different wavelengths were applied to irradiate the participating samples, and the scattered light of samples with different acceptance angles was obtained. First, the scattered signals within different acceptance angles were calculated by solving the radiative transfer equation. Then, the complex refractive index and PSD were retrieved simultaneously by applying quantum particle swarm optimization. However, the estimated results of PSD were inaccurate. Thus, a secondary optimization, which using the directional radiative intensity as input, was performed to improve the accuracy of PSD based on the first optimization process. Four commonly used kinds of monomodal PSD functions, i.e., the Rosin-Rammler, standard Normal, Logarithmic Normal, and Junge distribution, were retrieved. All results showed that the proposed technique can estimate the complex refractive index and PSD accurately.

  3. Noctilucent cloud polarimetry: Twilight measurements in a wide range of scattering angles

    NASA Astrophysics Data System (ADS)

    Ugolnikov, Oleg S.; Maslov, Igor A.; Kozelov, Boris V.; Dlugach, Janna M.

    2016-06-01

    Wide-field polarization measurements of the twilight sky background during several nights with bright and extended noctilucent clouds in central and northern Russia in 2014 and 2015 are used to build the phase dependence of the degree of polarization of sunlight scattered by cloud particles in a wide range of scattering angles (from 40° to 130°). This range covers the linear polarization maximum near 90° and large-angle slope of the curve. The polarization in this angle range is most sensitive to the particle size. The method of separation of scattering on cloud particles from the twilight background is presented. Results are compared with T-matrix simulations for different sizes and shapes of ice particles; the best-fit model radius of particles (0.06 μm) and maximum radius (about 0.1 μm) are estimated.

  4. Initial State Helicity Correlation in Wide Angle Compton Scattering

    NASA Astrophysics Data System (ADS)

    Zhang, Jixie; Day, Donal; Keller, Dustin; Rondon, Oscar

    2014-09-01

    The applicability of pQCD to exclusive reactions at medium energies is a subject of considerable interest. Real Compton scattering (RCS) has the potential to provide insight to this unsettled issue. In pQCD, three active quarks and two hard gluons are involved when describing RCS. But the cross sections do not agree with the pQCD predictions. In contrast, a handbag dominance model, involving only one single quark coupling to the spectator through generalized parton distributions (GPDs) does a good job of matching the cross section data. A measurement of the longitudinal polarization transfer parameter KLL was found inconsistent with predictions of pQCD yet consistent with calculations within the hand-bag mechanism. Further Miller's handbag approach, which including quark and hadron helicity flip, contradicts pQCD and others which demands that KLL =ALL , the initial state helicity correlation asymmetry, by finding that KLL ≠ALL . The first ever measurement of ALL has been proposed to run in Jefferson Lab's Hall C. This experiment will utilize an untagged bremsstrahlung photon beam and the longitudinally polarized UVA/JLAB proton target. After a brief introduction to the physics, the experiment will be described and the expected results presented.

  5. Initial State Helicity Correlation in Wide Angle Compton Scattering

    NASA Astrophysics Data System (ADS)

    Day, Donal; Keller, Dustin; Zhang, Jixie

    2015-04-01

    Whether pQCD can describe exclusive reactions at medium energies remains an area of active study. Real Compton scattering (RCS) has the potential to provide insight to this unsettled issue. A pQCD description of RCS requires the participation of three quarks and two hard gluons. However its predictions for the RCS cross sections disagree with data while calculations based on the handbag mechanism, involving a single quark coupled to the spectator through generalized parton distributions (GPDs), match the data well. The measured longitudinal polarization transfer parameter KLL is inconsistent with predictions of pQCD yet consistent with calculations of the handbag mechanism. Furthermore, Miller's approach, which includes quark and hadron helicity flip, contradicts pQCD where KLL =ALL , the initial state helicity correlation asymmetry, by finding that KLL ≠ALL . The first ever measurement of ALL (E12-14-006) has been approved to run in Jefferson Lab's Hall C and will be able to discriminate between the various models. E12-14-006 will utilize an untagged bremsstrahlung photon beam and the longitudinally polarized UVA/JLAB proton target. After a brief introduction to the physics, the experiment will be described and the expected results presented.

  6. High-resolution wide-angle X-ray scattering of protein solutions: effect of beam dose on protein integrity.

    PubMed

    Fischetti, Robert F; Rodi, Diane J; Mirza, Ahmed; Irving, Thomas C; Kondrashkina, Elena; Makowski, Lee

    2003-09-01

    Wide-angle X-ray scattering patterns from proteins in solution contain information relevant to the determination of protein fold. At relevant scattering angles, however, these data are weak, and the degree to which they might be used to categorize the fold of a protein is unknown. Preliminary work has been performed at the BioCAT insertion-device beamline at the Advanced Photon Source which demonstrates that one can collect X-ray scattering data from proteins in solution to spacings of at least 2.2 A (q = 2.8 A(-1)). These data are sensitive to protein conformational states, and are in good agreement with the scattering predicted by the program CRYSOL using the known three-dimensional atomic coordinates of the protein. An important issue in the exploitation of this technique as a tool for structural genomics is the extent to which the high intensity of X-rays available at third-generation synchrotron sources chemically or structurally damage proteins. Various data-collection protocols have been investigated demonstrating conditions under which structural degradation of even sensitive proteins can be minimized, making this technique a viable tool for protein fold categorization, the study of protein folding, unfolding, protein-ligand interactions and domain movement.

  7. Magnetic scattering in the simultaneous measurement of small-angle neutron scattering and Bragg edge transmission from steel.

    PubMed

    Oba, Yojiro; Morooka, Satoshi; Ohishi, Kazuki; Sato, Nobuhiro; Inoue, Rintaro; Adachi, Nozomu; Suzuki, Jun-Ichi; Tsuchiyama, Toshihiro; Gilbert, Elliot Paul; Sugiyama, Masaaki

    2016-10-01

    Pulsed neutron sources enable the simultaneous measurement of small-angle neutron scattering (SANS) and Bragg edge transmission. This simultaneous measurement is useful for microstructural characterization in steel. Since most steels are ferromagnetic, magnetic scattering contributions should be considered in both SANS and Bragg edge transmission analyses. An expression for the magnetic scattering contribution to Bragg edge transmission analysis has been derived. The analysis using this expression was applied to Cu steel. The ferrite crystallite size estimated from this Bragg edge transmission analysis with the magnetic scattering contribution was larger than that estimated using conventional expressions. This result indicates that magnetic scattering has to be taken into account for quantitative Bragg edge transmission analysis. In the SANS analysis, the ratio of magnetic to nuclear scattering contributions revealed that the precipitates consist of body-centered cubic Cu0.7Fe0.3 and pure Cu, which probably has 9R structure including elastic strain and vacancies. These results show that effective use of the magnetic scattering contribution allows detailed analyses of steel microstructure.

  8. Magnetic scattering in the simultaneous measurement of small-angle neutron scattering and Bragg edge transmission from steel1

    PubMed Central

    Oba, Yojiro; Morooka, Satoshi; Ohishi, Kazuki; Sato, Nobuhiro; Inoue, Rintaro; Adachi, Nozomu; Suzuki, Jun-ichi; Tsuchiyama, Toshihiro; Gilbert, Elliot Paul; Sugiyama, Masaaki

    2016-01-01

    Pulsed neutron sources enable the simultaneous measurement of small-angle neutron scattering (SANS) and Bragg edge transmission. This simultaneous measurement is useful for microstructural characterization in steel. Since most steels are ferromagnetic, magnetic scattering contributions should be considered in both SANS and Bragg edge transmission analyses. An expression for the magnetic scattering contribution to Bragg edge transmission analysis has been derived. The analysis using this expression was applied to Cu steel. The ferrite crystallite size estimated from this Bragg edge transmission analysis with the magnetic scattering contribution was larger than that estimated using conventional expressions. This result indicates that magnetic scattering has to be taken into account for quantitative Bragg edge transmission analysis. In the SANS analysis, the ratio of magnetic to nuclear scattering contributions revealed that the precipitates consist of body-centered cubic Cu0.7Fe0.3 and pure Cu, which probably has 9R structure including elastic strain and vacancies. These results show that effective use of the magnetic scattering contribution allows detailed analyses of steel microstructure. PMID:27738416

  9. X-ray small-angle scattering from sputtered CeO{sub 2}/C bilayers

    SciTech Connect

    Haviar, S.; Dubau, M.; Khalakhan, I.; Vorokhta, M.; Matolinova, I.; Matolin, V.; Vales, V.; Endres, J.; Holy, V.; Buljan, M.; Bernstorff, S.

    2013-01-14

    Surface and interface morphology of cerium oxide/carbon bilayers used as thin-film catalysts is studied by grazing-incidence small-angle x-ray scattering, scanning electron microscopy, and atomic-force microscopy, and the dependence of the structural parameters on the thicknesses of the constituting layers is investigated. The applicability of x-ray scattering and its advantages over standard analytical methods are discussed.

  10. The generation of Ganymede's diffuse aurora through pitch angle scattering

    NASA Astrophysics Data System (ADS)

    Tripathi, Arvind K.; Singhal, Rajendra P.; Singh, Onkar N., II

    2017-02-01

    Diffuse auroral intensities of neutral atomic oxygen OI λ1356 Å emission on Ganymede due to whistler mode waves are estimated. Pitch angle diffusion of magnetospheric electrons into the loss cone due to resonant wave-particle interaction of whistler mode waves is considered, and the resulting electron precipitation flux is calculated. The analytical yield spectrum approach is used for determining the energy deposition of electrons precipitating into the atmosphere of Ganymede. It is found that the intensities (4-30 R) calculated from the precipitation of magnetospheric electrons observed near Ganymede are inadequate to account for the observational intensities (≤ 100 R). This is in agreement with the conclusions reached in previous works. Some acceleration mechanism is required to energize the magnetospheric electrons. In the present work we consider the heating and acceleration of magnetospheric electrons by electrostatic waves. Two particle distribution functions (Maxwellian and kappa distribution) are used to simulate heating and acceleration of electrons. Precipitation of a Maxwellian distribution of electrons can produce about 70 R intensities of OI λ1356 Å emission for electron temperature of 150 eV. A kappa distribution can also yield a diffuse auroral intensity of similar magnitude for a characteristic energy of about 100 eV. The maximum contribution to the estimated intensity results from the dissociative excitation of O2. Contributions from the direct excitation of atomic oxygen and cascading in atomic oxygen are estimated to be only about 1 and 2 % of the total calculated intensity, respectively. The findings of this work are relevant for the present JUNO and future JUICE missions to Jupiter. These missions will provide new data on electron densities, electron temperature and whistler mode wave amplitudes in the magnetosphere of Jupiter near Ganymede.

  11. Analysis of photopolarimetric data of comets at small phase angles by rough surface scattering

    NASA Astrophysics Data System (ADS)

    Mukai, S.; Mukai, T.

    1990-07-01

    A comparison of cometary rough surface scattering model calculation results with observations has indicated that negative polarization is produced, over a phase-angle range of less than 20 deg, by the variation of polarization angle of reflected light due to a contribution from (1) different sites on large, rough particles, and/or (2) multiple internal reflection within small dielectric particles. The opposition effect in cometary comas is caused by large, rough particle reflection. The mixing model for cometary grains, encompassing small particles and large rough ones composed in both cases of slightly absorbing material, is seen as explaining the photopolarimetric data of comets in the backward-scattering region.

  12. Finite-size effect in light transmission through highly forward scattering media at grazing angles.

    PubMed

    Marinyuk, V V; Sheberstov, S V

    2016-03-01

    We present a theoretical study of light transmission through a disordered medium with large (compared to the light wavelength) inhomogeneities. Both numerical integration and analytic treatments of the radiative transfer equation are performed. An effect of the single-scattering phase function on the total transmittance is found in a subdiffusion thickness range. The effect reveals itself at grazing angles of incidence and originates from small-angle multiple scattering of light. A simple analytic formula for the total transmittance is derived. Our results are in good agreement with data of independent numerical calculations.

  13. Two-atom model in enhanced ion backscattering near 180/sup 0/ scattering angles

    SciTech Connect

    Oen, O.S.

    1981-06-01

    The recent discovery by Pronko, Appleton, Holland, and Wilson of an unusual enhancement of the yield of ions backscattered through angles close to 180/sup 0/ from the near surface regions of solids is investigated using a two-atom scattering model. The model predicts an enhancement effect in amorphous solids whose physical origin arises from the tolerance of path for those ions whose inward and outward trajectories lie in the vicinity of the critical impact parameter. Predictions are given of the dependence of the yield enhancement on the following parameters: ion energy, backscattering depth, exit angle, scattering potential, atomic numbers of projectile and target, and atomic density of target.

  14. Pitch angle scattering of relativistic electrons from stationary magnetic waves: Continuous Markov process and quasilinear theory

    SciTech Connect

    Lemons, Don S.

    2012-01-15

    We develop a Markov process theory of charged particle scattering from stationary, transverse, magnetic waves. We examine approximations that lead to quasilinear theory, in particular the resonant diffusion approximation. We find that, when appropriate, the resonant diffusion approximation simplifies the result of the weak turbulence approximation without significant further restricting the regime of applicability. We also explore a theory generated by expanding drift and diffusion rates in terms of a presumed small correlation time. This small correlation time expansion leads to results valid for relatively small pitch angle and large wave energy density - a regime that may govern pitch angle scattering of high-energy electrons into the geomagnetic loss cone.

  15. Do angles of obliquity apply to 30 degrees scattered radiation from megavoltage beams?

    PubMed

    Biggs, Peter J; Styczynski, John R

    2008-10-01

    The angle of obliquity is used in radiation shielding calculations to account for the longer path length x rays will see when obliquely incident on the protective barrier. According to the National Council on Radiation Protection and Measurements (NCRP), use of the angle of obliquity is explicitly assumed for primary radiation, so that an angle of obliquity for secondary radiation is never addressed. However, in the example section of the latest report, it specifically recommends against using an angle of obliquity for scattered radiation. To check this assumption, the existence or not of an angle of obliquity for scattered radiation has been investigated for bremsstrahlung x-ray beams of 4, 6, 10, 15, and 18 MV and for barriers consisting of concrete, lead, and steel using a Monte Carlo approach. The MCNP Monte Carlo code, v4.2C, has been used to generate scattered radiation at 30 degrees from a water phantom and incident on a secondary barrier at the same angle relative to the normal to the barrier. The barrier thickness was increased from zero to a thickness sufficient to reduce the fluence (f4 tally) to <10(-3). A transmission curve was created for each energy-barrier material combination by normalizing to zero thickness. The results for the first tenth-value layer (TVL) in concrete (5 energies) show an average angle of obliquity of 21.7 degrees +/- 5.6 degrees , and for the first two TVLs averaged 29.7 degrees +/- 3.9 degrees . The results for the first TVL in lead (3 energies) show an average angle of obliquity of 27.7 degrees +/- 4.0 degrees , and for the first two TVLs averaged 20.5 degrees +/- 5.8 degrees . There are no data in the NCRP reports for 30 degrees scattered radiation attenuated by steel with which to make a comparison.

  16. Ultrasmall Angle X-ray Scattering (USAXS) and Wide Angle X-ray Scattering (WAXS) Studies on the Complex Metal Hydride NaAlH4

    NASA Astrophysics Data System (ADS)

    Dobbins, Tabbetha; Bennett, Christopher; Torres, James; Ilavsky, Jan

    This research seeks to understand the role of ScCl , ZrCl , and VCl catalysts in NaAlH. We have examined these hydrides at multiple length scales using an X-ray scattering instrument which is capable of measuring scattering wave vector, Q, of 0.0001Å to 6.0 Å . The ultrasmall angle X-ray scattering (USAXS) instrument sector 9ID-D of the Advanced Photon Source (APS) simultaneously collects using USAXS, SAXS, and WAXS detectors. Studies were performed during in-situ heating up to 170C (just below the H desorption temperature for uncatalyzed NaAlH). Results showed that NaAlH has a surface fractal (highly porous) morphology. Isothermal studies performed at 30C, 65C, 100C, 135C, and 170C reveals changes at low Q (Q~0.001 Å to 0.01 Å) associated with highly interconnected intraparticle porosity which is suitably described by a power-law slope for a Gaussian polymer chain structure of p~2. At high scattering wave vector, Q~0.03 Å , the presence of a pore population which obeys Porod scattering and appears to have a size at 21nm is present. These fine pores increase in their population density as temperature is elevated. The WAXS data reveals thermal expansion to occur, but no solid state phase transformation to the product phase. Currently at NASA-Goddard.

  17. Application of electrically invisible antennas to the Modulated Scatterer Technique

    SciTech Connect

    Crocker, Dylan A.; Donnell, Kristen M.

    2015-09-16

    The modulated scatterer technique (MST) has shown promise for applications in microwave imaging, electric field mapping, and materials characterization. Traditionally, MST scatterers are dipoles centrally loaded with an element capable of modulation (e.g., a p-i-n diode). By modulating the load element, signals scattered from the MST scatterer are also modulated. However, due to the small size of such scatterers, it can be difficult to reliably detect the modulated signal. Increasing the modulation depth (MD; a parameter related to how well the scatterer modulates the scattered signal) may improve the detectability of the scattered signal. In an effort to improve the MD, the concept of electrically invisible antennas is applied to the design of MST scatterers. Our paper presents simulations and measurements of MST scatterers that have been designed to be electrically invisible during the reverse bias state of the modulated element (a p-i-n diode in this case), while producing detectable scattering during the forward bias state (i.e., operate in an electrically visible state). Furthermore, the results using the new design show significant improvement to the MD of the scattered signal as compared with a traditional MST scatterer (i.e., dipole centrally loaded with a p-i-n diode).

  18. Application of electrically invisible antennas to the Modulated Scatterer Technique

    DOE PAGES

    Crocker, Dylan A.; Donnell, Kristen M.

    2015-09-16

    The modulated scatterer technique (MST) has shown promise for applications in microwave imaging, electric field mapping, and materials characterization. Traditionally, MST scatterers are dipoles centrally loaded with an element capable of modulation (e.g., a p-i-n diode). By modulating the load element, signals scattered from the MST scatterer are also modulated. However, due to the small size of such scatterers, it can be difficult to reliably detect the modulated signal. Increasing the modulation depth (MD; a parameter related to how well the scatterer modulates the scattered signal) may improve the detectability of the scattered signal. In an effort to improve themore » MD, the concept of electrically invisible antennas is applied to the design of MST scatterers. Our paper presents simulations and measurements of MST scatterers that have been designed to be electrically invisible during the reverse bias state of the modulated element (a p-i-n diode in this case), while producing detectable scattering during the forward bias state (i.e., operate in an electrically visible state). Furthermore, the results using the new design show significant improvement to the MD of the scattered signal as compared with a traditional MST scatterer (i.e., dipole centrally loaded with a p-i-n diode).« less

  19. Determining Angle of Humeral Torsion Using Image Software Technique

    PubMed Central

    Sethi, Madhu; Vasudeva, Neelam

    2016-01-01

    Introduction Several researches have been done on the measurement of angles of humeral torsion in different parts of the world. Previously described methods were more complicated, not much accurate, cumbersome or required sophisticated instruments. Aim The present study was conducted with the aim to determine the angles of humeral torsion with a newer simple technique using digital images and image tool software. Materials and Methods A total of 250 dry normal adult human humeri were obtained from the bone bank of Department of Anatomy. The length and mid-shaft circumference of each bone was measured with the help of measuring tape. The angle of humeral torsion was measured directly from the digital images by the image analysis using Image Tool 3.0 software program. The data was analysed statistically with SPSS version 17 using unpaired t-test and Spearman’s rank order correlation coefficient. Results The mean angle of torsion was 64.57°±7.56°. On the right side it was 66.84°±9.69°, whereas, on the left side it was found to be 63.31±9.50°. The mean humeral length was 31.6 cm on right side and 30.33 cm on left side. Mid shaft circumference was 5.79 on right side and 5.63 cm on left side. No statistical differences were seen in angles between right and left humeri (p>0.001). Conclusion From our study, it was concluded that circumference of shaft is inversely proportional to angle of humeral torsion. The length and side of humerus has no relation with the humeral torsion. With advancement of digital technology, it is better to use new image softwares for anatomical studies. PMID:27891326

  20. On techniques for angle compensation in nonideal iris recognition.

    PubMed

    Schuckers, Stephanie A C; Schmid, Natalia A; Abhyankar, Aditya; Dorairaj, Vivekanand; Boyce, Christopher K; Hornak, Lawrence A

    2007-10-01

    The popularity of the iris biometric has grown considerably over the past two to three years. Most research has been focused on the development of new iris processing and recognition algorithms for frontal view iris images. However, a few challenging directions in iris research have been identified, including processing of a nonideal iris and iris at a distance. In this paper, we describe two nonideal iris recognition systems and analyze their performance. The word "nonideal" is used in the sense of compensating for off-angle occluded iris images. The system is designed to process nonideal iris images in two steps: 1) compensation for off-angle gaze direction and 2) processing and encoding of the rotated iris image. Two approaches are presented to account for angular variations in the iris images. In the first approach, we use Daugman's integrodifferential operator as an objective function to estimate the gaze direction. After the angle is estimated, the off-angle iris image undergoes geometric transformations involving the estimated angle and is further processed as if it were a frontal view image. The encoding technique developed for a frontal image is based on the application of the global independent component analysis. The second approach uses an angular deformation calibration model. The angular deformations are modeled, and calibration parameters are calculated. The proposed method consists of a closed-form solution, followed by an iterative optimization procedure. The images are projected on the plane closest to the base calibrated plane. Biorthogonal wavelets are used for encoding to perform iris recognition. We use a special dataset of the off-angle iris images to quantify the performance of the designed systems. A series of receiver operating characteristics demonstrate various effects on the performance of the nonideal-iris-based recognition system.

  1. A small angle neutron scattering study of mica based glass-ceramics with applications in dentistry

    NASA Astrophysics Data System (ADS)

    Kilcoyne, S. H.; Bentley, P. M.; Al-Jawad, M.; Bubb, N. L.; Al-Shammary, H. A. O.; Wood, D. J.

    2004-07-01

    We are currently developing machinable and load-bearing mica-based glass-ceramics for use in restorative dental surgery. In this paper we present the results of an ambient temperature small angle neutron scattering (SANS) study of several such ceramics with chemical compositions chosen to optimise machinability and strength. The SANS spectra are all dominated by scattering from the crystalline-amorphous phase interface and exhibit Q-4 dependence (Porod scattering) indicating that, on a 100Å scale, the surface of the crystals is smooth.

  2. Application of small-angle neutron scattering to the study of forces between magnetically chained monodisperse ferrofluid emulsion droplets

    SciTech Connect

    Jain, Dr Nirmesh; Liu, Dr C K; Hawkett, Dr B. S.; Warr, G. G.; Hamilton, William A

    2014-01-01

    The optical magnetic chaining technique (MCT) developed by Leal-Calderon, Bibette and co-workers in the 1990 s allows precise measurements of force profiles between droplets in monodisperse ferrofluid emulsions. However, the method lacks an in-situ determination of droplet size and therefore requires the combination of separately acquired measurements of droplet chain periodicity versus an applied magnetic field from optical Bragg scattering and droplet diameter inferred from dynamic light scattering (DLS) to recover surface force-distance profiles between the colloidal particles. Compound refractive lens (CRL) focussed small-angle scattering (SANS) MCT should result in more consistent measurements of droplet size (form factor measurements in the absence of field) and droplet chaining period (from structure factor peaks when the magnetic field is applied); and, with access to shorter length scales, extend force measurements to closer approaches than possible by optical measurements. We report on CRL-SANS measurements of monodisperse ferrofluid emulsion droplets aligned in straight chains by an applied field perpendicular to the incident beam direction. Analysis of the scattering from the closely spaced droplets required algorithms that carefully treated resolution and its effect on mean scattering vector magnitudes in order to determine droplet size and chain periods to sufficient accuracy. At lower applied fields scattering patterns indicate structural correlations transverse to the magnetic field direction due to the formation of intermediate structures in early chain growth.

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

    SciTech Connect

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

    2015-01-01

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

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

    PubMed

    Hopkins, Jesse B; Thorne, Robert E

    2016-06-01

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

  5. Analysis of the arriving-angle structure of the forward scattered wave on a vertical array in shallow water.

    PubMed

    He, Chuanlin; Yang, Kunde; Ma, Yuanliang; Lei, Bo

    2016-09-01

    The arriving-angle structure for the forward scattered wave on a vertical line array is obtained upon a modified scattering model in the Pekeris waveguide. The structure is investigated and interpreted by the array invariant theory combined with target induced modal coupling effect. Compared with that of the direct blast, the arriving-angle structure of the forward scattering wave owns multi-striations as well as an increased vertical array invariant. The forward scattered angle structure is dependent on the target position on the source-receiver line. Simulations indicate a potential separation for the forward scattered wave overwhelmed by the direct blast.

  6. Studying fractal geometry on submicron length scales by small-angle scattering

    SciTech Connect

    Wong, P.; Lin, J.

    1988-08-01

    Recent studies have shown that internal surfaces of porous geological materials, such as rocks and lignite coals, can be described by fractals down to atomic length scales. In this paper, the basic properties of self-similar and self-affine fractals are reviewed and how fractal dimensions can be measured by small-angle scattering experiments are discussed.

  7. Probing helium nano-bubble formation in tungsten with grazing incidence small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

    Helium nano-bubble formation in plasma facing materials has emerged as a major concern for the next-step fusion experiment ITER, where helium plasmas will be used during the tokamak's start-up phase. Here, we demonstrate that grazing incidence small-angle x-ray scattering is a powerful technique for the analysis of helium nano-bubble formation in tungsten. We measured helium bubbles with sizes between 1.5-2.5 nm in tungsten exposed to helium plasma at 700 °C, where a smaller number of larger bubbles were also observed. Depth distributions can be estimated by taking successive measurements across a range of x-ray incidence angles. Compared with traditional approaches in the field, such as transmission electron microscopy, this technique provides information across a much larger volume with high statistical precision, whilst also being non-destructive.

  8. Polarization transfer in wide-angle Compton scattering and single-pion photoproduction from the proton

    SciTech Connect

    Fanelli, Cristiano V.

    2015-10-06

    Wide-angle exclusive Compton scattering and single-pion photoproduction from the proton have been investigated via measurement of the polarization transfer from a circularly polarized photon beam to the recoil proton. The WACS polarization transfer was analyzed at an incident photon energy of 3.7 GeV at a proton scattering angle of θPcm = 70°. The longitudinal transfer KLL, measured to be 0.645 ± 0.059 ± 0.048, where the first error is statistical and the second is systematic, has the same sign as predicted for the reaction mechanism in which the photon interacts with a single quark carrying the spin of the proton. However, the observed value is ~3 times larger than predicted by the GPD-based calculations, which indicates a significant unknown contribution to the scattering amplitude.

  9. Polarization transfer in wide-angle Compton scattering and single-pion photoproduction from the proton

    DOE PAGES

    Fanelli, Cristiano V.

    2015-10-06

    Wide-angle exclusive Compton scattering and single-pion photoproduction from the proton have been investigated via measurement of the polarization transfer from a circularly polarized photon beam to the recoil proton. The WACS polarization transfer was analyzed at an incident photon energy of 3.7 GeV at a proton scattering angle of θPcm = 70°. The longitudinal transfer KLL, measured to be 0.645 ± 0.059 ± 0.048, where the first error is statistical and the second is systematic, has the same sign as predicted for the reaction mechanism in which the photon interacts with a single quark carrying the spin of the proton.more » However, the observed value is ~3 times larger than predicted by the GPD-based calculations, which indicates a significant unknown contribution to the scattering amplitude.« less

  10. Quantitative characterization of the contrast mechanisms of ultra-small angle x-ray scattering imaging.

    SciTech Connect

    Zhang, F.; Long, G. G.; Levine, L.E.; Ilavsky, J.; Jemain, P.R.; NIST

    2008-04-01

    A general treatment of X-ray imaging contrast for ultra-small-angle X-ray scattering (USAXS) imaging is presented; this approach makes use of phase propagation and dynamical diffraction theory to account quantitatively for the intensity distribution at the detector plane. Simulated results from a model system of micrometer-sized spherical SiO{sub 2} particles embedded in a polypropylene matrix show good agreement with experimental measurements. Simulations by means of a separate geometrical ray-tracing method also account for the features in the USAXS images and offer a complementary view of small-angle X-ray scattering as a contrast mechanism. The ray-tracing analysis indicates that refraction, in the form of Porod scattering, and, to a much lesser extent, X-ray reflection account for the USAXS imaging contrast.

  11. Small-angle neutron scattering studies from solutions of bovine nasal cartilage proteoglycan

    SciTech Connect

    Patel, A.; Stivala, S.S.; Damle, S.P.; Gregory, J.D.; Bunick, G.J.; Uberbacher, E.C.

    1985-08-01

    Small-angle neutron scattering, SANS, of the proteoglycan subunit of bovine nasal cartilage in 0.15N LiCl at 25/sup 0/C yielded the radius of gyration, R/sub g/, radius of gyration of the cross-section, R/sub q/, persistence length, a, and the molecular weight, M. The following values were obtained: M = 3.9 x 10/sup 6/, R/sub g/ = 745 A, R/sub q/ = 34.6 A and a = 35.2 A. These values compare favorably with those that were obtained from small angle x-ray scattering, SAXS, of a similar extract. The scattering curve of the proteoglycan subunit in D/sub 2/O showed a characteristic broad peak in the specified angular range similar to that observed from SAXS, thus confirming the polyelectrolyte nature of the proteoglycan. 15 refs., 3 figs., 1 tab. (DT)

  12. BIOISIS: Biological Macromolecules by Small Angle X-ray Scattering (SAXS)

    DOE Data Explorer

    Tainer, John [Scripps Research Institute; Hura, Greg [LBNL; Rambo, Robert P. [LBNL

    BIOISIS is an open access database dedicated to the study of biological macromolecules by small angle X-ray scattering (SAXS). BIOISIS aims to become the complete source for the deposition, distribution and maintenance of small angle X-ray scattering data and technologies. The database is designed around the concept of an ôexperimentö and relates a specific experiment to a set of genes, organisms, computational models and experimental data. As of May 2012, BIOSIS contains 7,118 genes covering four different organisms. Forty-two modeled structures are available. Clicking on a structures reveals scattering curves, experimental conditions, and experimental values. The data are collected at Beamline 12.3.1 of the Advanced Light Source (ALS).[Copied with editing from http://www.bioisis.net/about

  13. Scattering of surface plasmon polaritons by impedance barriers: Dependence on angle of incidence

    NASA Astrophysics Data System (ADS)

    Nikitin, A. Yu.; Brucoli, G.; García-Vidal, F. J.; Martín-Moreno, L.

    2008-05-01

    This paper studies theoretically surface plasmon polariton scattering by one-dimensional defects of metal surface impedance at oblique incidence. Surface impedance boundary conditions are used to formulate an integral equation which can be solved both analytically and numerically to yield the transmission, reflection, and out-of-plane cross section as a function of angle of incidence and other parameters. Numerical calculations, as well as analytical expressions, obtained within the Born approximation are presented. Green’s tensor approach is also applied so as to expand such analysis to region in which the surface impedance boundary conditions are not appropriate. We show that the angular dependencies for surface plasmon polariton scattering by impedance defects and by surface relief defects are essentially different. The angular dependency of surface plasmon polariton scattering by an impedance defect features an analog to Brewster’s angle that is explained in terms of dipole polarization of the defect.

  14. Scattering of nanowire surface plasmons coupled to quantum dots with azimuthal angle difference

    NASA Astrophysics Data System (ADS)

    Kuo, Po-Chen; Chen, Guang-Yin; Chen, Yueh-Nan

    2016-11-01

    Coherent scatterings of surface plasmons coupled to quantun dots have attracted great attention in plasmonics. Recently, an experiment has shown that the quantum dots located nearby a nanowire can be separated not only in distance, but also an angle ϕ along the cylindrical direction. Here, by using the real-space Hamiltonian and the transfer matrix method, we analytically obtain the transmission/reflection spectra of nanowire surface plasmons coupled to quantum dots with an azimuthal angle difference. We find that the scattering spectra can show completely different features due to different positions and azimuthal angles of the quantum dots. When additionally coupling a cavity to the dots, we obtain the Fano-like line shape in the transmission and reflection spectra due to the interference between the localized and delocalized modes.

  15. Scattering of nanowire surface plasmons coupled to quantum dots with azimuthal angle difference

    PubMed Central

    Kuo, Po-Chen; Chen, Guang-Yin; Chen, Yueh-Nan

    2016-01-01

    Coherent scatterings of surface plasmons coupled to quantun dots have attracted great attention in plasmonics. Recently, an experiment has shown that the quantum dots located nearby a nanowire can be separated not only in distance, but also an angle ϕ along the cylindrical direction. Here, by using the real-space Hamiltonian and the transfer matrix method, we analytically obtain the transmission/reflection spectra of nanowire surface plasmons coupled to quantum dots with an azimuthal angle difference. We find that the scattering spectra can show completely different features due to different positions and azimuthal angles of the quantum dots. When additionally coupling a cavity to the dots, we obtain the Fano-like line shape in the transmission and reflection spectra due to the interference between the localized and delocalized modes. PMID:27892942

  16. Pitch angle scattering of an energetic magnetized particle by a circularly polarized electromagnetic wave

    SciTech Connect

    Bellan, P. M.

    2013-04-15

    The interaction between a circularly polarized wave and an energetic gyrating particle is described using a relativistic pseudo-potential that is a function of the frequency mismatch. Analysis of the pseudo-potential provides a means for interpreting numerical results. The pseudo-potential profile depends on the initial mismatch, the normalized wave amplitude, and the initial angle between the wave magnetic field and the particle perpendicular velocity. For zero initial mismatch, the pseudo-potential consists of only one valley, but for finite mismatch, there can be two valleys separated by a hill. A large pitch angle scattering of the energetic electron can occur in the two-valley situation but fast scattering can also occur in a single valley. Examples relevant to magnetospheric whistler waves show that the energetic electron pitch angle can be deflected 5 Degree-Sign towards the loss cone when transiting a 10 ms long coherent wave packet having realistic parameters.

  17. Stochastic analysis of pitch angle scattering of charged particles by transverse magnetic waves

    SciTech Connect

    Lemons, Don S.; Liu Kaijun; Winske, Dan; Gary, S. Peter

    2009-11-15

    This paper describes a theory of the velocity space scattering of charged particles in a static magnetic field composed of a uniform background field and a sum of transverse, circularly polarized, magnetic waves. When that sum has many terms the autocorrelation time required for particle orbits to become effectively randomized is small compared with the time required for the particle velocity distribution to change significantly. In this regime the deterministic equations of motion can be transformed into stochastic differential equations of motion. The resulting stochastic velocity space scattering is described, in part, by a pitch angle diffusion rate that is a function of initial pitch angle and properties of the wave spectrum. Numerical solutions of the deterministic equations of motion agree with the theory at all pitch angles, for wave energy densities up to and above the energy density of the uniform field, and for different wave spectral shapes.

  18. Methods for analysis of size-exclusion chromatography-small-angle X-ray scattering and reconstruction of protein scattering.

    PubMed

    Malaby, Andrew W; Chakravarthy, Srinivas; Irving, Thomas C; Kathuria, Sagar V; Bilsel, Osman; Lambright, David G

    2015-08-01

    Size-exclusion chromatography in line with small-angle X-ray scattering (SEC-SAXS) has emerged as an important method for investigation of heterogeneous and self-associating systems, but presents specific challenges for data processing including buffer subtraction and analysis of overlapping peaks. This paper presents novel methods based on singular value decomposition (SVD) and Guinier-optimized linear combination (LC) to facilitate analysis of SEC-SAXS data sets and high-quality reconstruction of protein scattering directly from peak regions. It is shown that Guinier-optimized buffer subtraction can reduce common subtraction artifacts and that Guinier-optimized linear combination of significant SVD basis components improves signal-to-noise and allows reconstruction of protein scattering, even in the absence of matching buffer regions. In test cases with conventional SAXS data sets for cytochrome c and SEC-SAXS data sets for the small GTPase Arf6 and the Arf GTPase exchange factors Grp1 and cytohesin-1, SVD-LC consistently provided higher quality reconstruction of protein scattering than either direct or Guinier-optimized buffer subtraction. These methods have been implemented in the context of a Python-extensible Mac OS X application known as Data Evaluation and Likelihood Analysis (DELA), which provides convenient tools for data-set selection, beam intensity normalization, SVD, and other relevant processing and analytical procedures, as well as automated Python scripts for common SAXS analyses and Guinier-optimized reconstruction of protein scattering.

  19. Parameterization of structures in HE composites using surrogate materials: A small angle neutron scattering investigation

    SciTech Connect

    Mang, J.T.; Hjelm, R.P.; Skidmore, C.B.; Howe, P.M.

    1996-07-01

    High explosive materials used in the nuclear stockpile are composites of crystalline high explosives (HE) with binder materials, such as Estane. In such materials, there are naturally occurring density fluctuations (defects) due to cracks, internal (in the HE) and external (in the binder) voids and other artifacts of preparation. Changes in such defects due to material aging can affect the response of explosives due to shock, impact and thermal loading. Modeling efforts are attempting to provide quantitative descriptions of explosive response from the lowest ignition thresholds to the development of full blown detonations and explosions, however, adequate descriptions of these processes require accurate measurements of a number of structural parameters of the HE composite. Since different defects are believed to affect explosive sensitivity in different ways it is necessary to quantitatively differentiate between defect types. The authors report here preliminary results of SANS measurements on surrogates for HE materials. The objective of these measurements was to develop methodologies using SANS techniques to parameterize internal void size distributions in a surrogate material, sugar, to simulate an HE used in the stockpile, HMX. Sugar is a natural choice as a surrogate material, as it has the same crystal structure, has similar intragranular voids and has similar mechanical properties as HMX. It is used extensively as a mock material for explosives. Samples were used with two void size distributions: one with a sufficiently small mean particle size that only small occluded voids are present in significant concentrations, and one where the void sizes could be larger. By using methods in small-angle neutron scattering, they were able to isolate the scattering arising from particle-liquid interfaces and internal voids.

  20. Nano-Scale Morphology of Melanosomes Revealed by Small-Angle X-Ray Scattering

    PubMed Central

    Gorniak, Thomas; Haraszti, Tamas; Garamus, Vasyl M.; Buck, Andreas R.; Senkbeil, Tobias; Priebe, Marius; Hedberg-Buenz, Adam; Koehn, Demelza; Salditt, Tim; Grunze, Michael; Anderson, Michael G.; Rosenhahn, Axel

    2014-01-01

    Melanosomes are highly specialized organelles that produce and store the pigment melanin, thereby fulfilling essential functions within their host organism. Besides having obvious cosmetic consequences – determining the color of skin, hair and the iris – they contribute to photochemical protection from ultraviolet radiation, as well as to vision (by defining how much light enters the eye). Though melanosomes can be beneficial for health, abnormalities in their structure can lead to adverse effects. Knowledge of their ultrastructure will be crucial to gaining insight into the mechanisms that ultimately lead to melanosome-related diseases. However, due to their small size and electron-dense content, physiologically intact melanosomes are recalcitrant to study by common imaging techniques such as light and transmission electron microscopy. In contrast, X-ray-based methodologies offer both high spatial resolution and powerful penetrating capabilities, and thus are well suited to study the ultrastructure of electron-dense organelles in their natural, hydrated form. Here, we report on the application of small-angle X-ray scattering – a method effective in determining the three-dimensional structures of biomolecules – to whole, hydrated murine melanosomes. The use of complementary information from the scattering signal of a large ensemble of suspended organelles and from single, vitrified specimens revealed a melanosomal sub-structure whose surface and bulk properties differ in two commonly used inbred strains of laboratory mice. Whereas melanosomes in C57BL/6J mice have a well-defined surface and are densely packed with 40-nm units, their counterparts in DBA/2J mice feature a rough surface, are more granular and consist of 60-nm building blocks. The fact that these strains have different coat colors and distinct susceptibilities to pigment-related eye disease suggest that these differences in size and packing are of biological significance. PMID:24621581

  1. Effect of EMIC Wave Normal Angle Distribution on Relativistic Electron Scattering in Outer RB

    NASA Technical Reports Server (NTRS)

    Khazanov, G. V.; Gamayunov, K. V.

    2007-01-01

    We present the equatorial and bounce average pitch angle diffusion coefficients for scattering of relativistic electrons by the H+ mode of EMIC waves. Both the model (prescribed) and self consistent distributions over the wave normal angle are considered. The main results of our calculation can be summarized as follows: First, in comparison with field aligned waves, the intermediate and highly oblique waves reduce the pitch angle range subject to diffusion, and strongly suppress the scattering rate for low energy electrons (E less than 2 MeV). Second, for electron energies greater than 5 MeV, the |n| = 1 resonances operate only in a narrow region at large pitch-angles, and despite their greatest contribution in case of field aligned waves, cannot cause electron diffusion into the loss cone. For those energies, oblique waves at |n| greater than 1 resonances are more effective, extending the range of pitch angle diffusion down to the loss cone boundary, and increasing diffusion at small pitch angles by orders of magnitude.

  2. Atomistic modelling of scattering data in the Collaborative Computational Project for Small Angle Scattering (CCP-SAS).

    PubMed

    Perkins, Stephen J; Wright, David W; Zhang, Hailiang; Brookes, Emre H; Chen, Jianhan; Irving, Thomas C; Krueger, Susan; Barlow, David J; Edler, Karen J; Scott, David J; Terrill, Nicholas J; King, Stephen M; Butler, Paul D; Curtis, Joseph E

    2016-12-01

    The capabilities of current computer simulations provide a unique opportunity to model small-angle scattering (SAS) data at the atomistic level, and to include other structural constraints ranging from molecular and atomistic energetics to crystallography, electron microscopy and NMR. This extends the capabilities of solution scattering and provides deeper insights into the physics and chemistry of the systems studied. Realizing this potential, however, requires integrating the experimental data with a new generation of modelling software. To achieve this, the CCP-SAS collaboration (http://www.ccpsas.org/) is developing open-source, high-throughput and user-friendly software for the atomistic and coarse-grained molecular modelling of scattering data. Robust state-of-the-art molecular simulation engines and molecular dynamics and Monte Carlo force fields provide constraints to the solution structure inferred from the small-angle scattering data, which incorporates the known physical chemistry of the system. The implementation of this software suite involves a tiered approach in which GenApp provides the deployment infrastructure for running applications on both standard and high-performance computing hardware, and SASSIE provides a workflow framework into which modules can be plugged to prepare structures, carry out simulations, calculate theoretical scattering data and compare results with experimental data. GenApp produces the accessible web-based front end termed SASSIE-web, and GenApp and SASSIE also make community SAS codes available. Applications are illustrated by case studies: (i) inter-domain flexibility in two- to six-domain proteins as exemplified by HIV-1 Gag, MASP and ubiquitin; (ii) the hinge conformation in human IgG2 and IgA1 antibodies; (iii) the complex formed between a hexameric protein Hfq and mRNA; and (iv) synthetic 'bottlebrush' polymers.

  3. Atomistic modelling of scattering data in the Collaborative Computational Project for Small Angle Scattering (CCP-SAS)1

    PubMed Central

    Perkins, Stephen J.; Wright, David W.; Zhang, Hailiang; Brookes, Emre H.; Chen, Jianhan; Irving, Thomas C.; Krueger, Susan; Barlow, David J.; Edler, Karen J.; Scott, David J.; Terrill, Nicholas J.; King, Stephen M.; Butler, Paul D.; Curtis, Joseph E.

    2016-01-01

    The capabilities of current computer simulations provide a unique opportunity to model small-angle scattering (SAS) data at the atomistic level, and to include other structural constraints ranging from molecular and atomistic energetics to crystallography, electron microscopy and NMR. This extends the capabilities of solution scattering and provides deeper insights into the physics and chemistry of the systems studied. Realizing this potential, however, requires integrating the experimental data with a new generation of modelling software. To achieve this, the CCP-SAS collaboration (http://www.ccpsas.org/) is developing open-source, high-throughput and user-friendly software for the atomistic and coarse-grained molecular modelling of scattering data. Robust state-of-the-art molecular simulation engines and molecular dynamics and Monte Carlo force fields provide constraints to the solution structure inferred from the small-angle scattering data, which incorporates the known physical chemistry of the system. The implementation of this software suite involves a tiered approach in which GenApp provides the deployment infrastructure for running applications on both standard and high-performance computing hardware, and SASSIE provides a workflow framework into which modules can be plugged to prepare structures, carry out simulations, calculate theoretical scattering data and compare results with experimental data. GenApp produces the accessible web-based front end termed SASSIE-web, and GenApp and SASSIE also make community SAS codes available. Applications are illustrated by case studies: (i) inter-domain flexibility in two- to six-domain proteins as exemplified by HIV-1 Gag, MASP and ubiquitin; (ii) the hinge conformation in human IgG2 and IgA1 antibodies; (iii) the complex formed between a hexameric protein Hfq and mRNA; and (iv) synthetic ‘bottlebrush’ polymers. PMID:27980506

  4. PREFACE Proceedings of the XIV International Conference on Small-Angle Scattering, SAS-2009

    NASA Astrophysics Data System (ADS)

    King, Stephen; Terrill, Nicholas

    2010-10-01

    The XIV International Conference on Small-Angle Scattering, SAS-2009, was held in Oxford UK, 13-18 September 2009, and was jointly organised under the auspices of the International Union of Crystallography Commission on SAS by a team from the Diamond Light Source and the ISIS Pulsed Neutron Source - their first such joint venture - with help from the UK Science and Technology Facilities Council. It was the first time that this long running and successful series of conferences on the application, science and technology of small-angle scattering techniques had been staged in the UK. The UK has a proud heritage in small-angle scattering: as home to one of the world's first SANS instruments (at AERE Harwell), as the site of the world's first 2nd generation X-ray Synchrotron (the SRS at Daresbury with its suite of SAXS beamlines), and latterly as the location of the world's most successful pulsed source SANS instrument. Indeed, 2009 also marked the 25th Anniversary of neutron operations at ISIS and the opening of a Second Target Station. Whilst the SRS ceased operations in 2008, its mantle has been inherited by the Diamond synchrotron. Many delegates took the opportunity to visit both Diamond and ISIS during a conference excursion. Despite the prevailing global economic downturn, we were delighted that 434 delegates from 32 different countries were able to attend SAS-2009; two-thirds were drawn from the UK, Germany, Japan, the USA and France, but there were also sizeable contingents from Australia, Korea, Taiwan and South America. In many ways this geographical spread reflects the present and emerging distribution, respectively, of 3rd generation X-ray synchrotrons and high-flux neutron sources, although the scope of the conference was not solely limited to these probes. Financial support from the IUCr enabled us to grant bursaries to attend SAS-2009 to 12 delegates from emerging countries (Algeria, Argentina, Brazil, India, Nepal, Romania, Russia and the Ukraine). The

  5. The active layer morphology of organic solar cells probed with grazing incidence scattering techniques.

    PubMed

    Müller-Buschbaum, Peter

    2014-12-10

    Grazing incidence X-ray scattering (GIXS) provides unique insights into the morphology of active materials and thin film layers used in organic photovoltaic devices. With grazing incidence wide angle X-ray scattering (GIWAXS) the molecular arrangement of the material is probed. GIWAXS is sensitive to the crystalline parts and allows for the determination of the crystal structure and the orientation of the crystalline regions with respect to the electrodes. With grazing incidence small angle X-ray scattering (GISAXS) the nano-scale structure inside the films is probed. As GISAXS is sensitive to length scales from nanometers to several hundred nanometers, all relevant length scales of organic solar cells are detectable. After an introduction to GISAXS and GIWAXS, selected examples for application of both techniques to active layer materials are reviewed. The particular focus is on conjugated polymers, such as poly(3-hexylthiophene) (P3HT).

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

  7. Structural modeling of proteins by integrating small-angle x-ray scattering data

    NASA Astrophysics Data System (ADS)

    Zhang, Yong-Hui; Peng, Jun-Hui; Zhang, Zhi-Yong

    2015-12-01

    Elucidating the structure of large biomolecules such as multi-domain proteins or protein complexes is challenging due to their high flexibility in solution. Recently, an “integrative structural biology” approach has been proposed, which aims to determine the protein structure and characterize protein flexibility by combining complementary high- and low-resolution experimental data using computer simulations. Small-angle x-ray scattering (SAXS) is an efficient technique that can yield low-resolution structural information, including protein size and shape. Here, we review computational methods that integrate SAXS with other experimental datasets for structural modeling. Finally, we provide a case study of determination of the structure of a protein complex formed between the tandem SH3 domains in c-Cb1-associated protein and the proline-rich loop in human vinculin. Project supported by the National Key Basic Research Program of China (Grant Nos. 2013CB910203 and 2011CB911104), the National Natural Science Foundation of China (Grant No. 31270760), the Strategic Priority Research Program of the Chinese Academy of Sciences (Grant No. XDB08030102), and the Specialized Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20113402120013).

  8. X-ray Scattering Techniques for Characterization of Nanosystems in Lifescience

    SciTech Connect

    Saw, C K

    2005-04-11

    The intent of this chapter is to provide the basics of using x-ray diffraction techniques in order to obtain information on the structure and morphology of the nanosystems, and also to point out some of its strengths and weaknesses when compare to other characterization techniques. X-ray scattering examines over a wide range of density domains from a tenth to a thousandth angstrom. Essentially, this covers a whole range of condensed matter, including the structure and morphology of nanosystems, particularly useful for examining nanostructures in lifescience. This range of domain size requires both the wide-angle x-ray scattering (WAXS) and small-angle (SAXS) x-ray scattering techniques. Roughly WAXS covers from 2 nm down, and SAXS covers from .5 nm to 100 nm and possibly 1,000 nm for a finely tuned instrument. Brief theoretical description of both WAXS and SAXS will be given in this chapter. WAXS, by itself is a powerful technique in providing information on the crystallographic structure or lack of structure, atomic positions and sizes in a unit cell, to some extend, chemical compositions and as well as chemical stoichiometry. Examples of such experiments will also be given. In order to be able to describe the technique of x-ray scattering, some historical and theoretical background will be given in the hope of making this subject interesting and simple.

  9. Optical and Geometric Properties of Free Silica Nanoparticles Studied by Small-Angle X-Ray Scattering

    NASA Astrophysics Data System (ADS)

    Langer, Burkhard; Raschpichler, Christopher; Gruner, Mathias; Antonsson, Egill; Goroncy, Christian; Graf, Christina; Rühl, Eckart

    2016-09-01

    Elastic small-angle X-ray scattering (SAXS) of free silica (SiO2) nanoparticles is reported (d = 100-180 nm). The particles were prepared by a modified Stöber synthesis in narrow size distributions with controlled surface roughness and functionalization. Angle-resolved small-angle X-ray scattering patterns are shown to be sensitive to these changes in particle properties. It is reported that there is an exponential decrease in scattered X-ray intensity towards larger scattering angles as well as distinct oscillations, which is fully explained by Mie theory. Small-angle X-ray scattering of mesoporous nanoparticles with rough surfaces is compared to that of microporous nanoparticles with smooth surfaces, revealing distinct differences that are rationalized by diffuse scattering from nanoparticle pores in addition to the dominating contribution of Mie scattering. Furthermore, results from small-angle X-ray scattering experiments on functionalized silica nanoparticles are presented, where the incorporation of the dye fluorescein isothiocyanate is found to cause changes in the optical properties of the nanoparticles, as compared to non-functionalized samples. Small, but distinct deviations in particle size derived from electron microscopy and from small-angle X-ray scattering are observed. These are rationalized by particle shrinking occurring in electron microscopy as well as slight changes in optical properties of the nanoparticle samples.

  10. Quantitative analysis of angle-resolved scattering properties of ovarian tissue using optical coherence tomography

    PubMed Central

    Yang, Yi; Wang, Tianheng; Brewer, Molly

    2012-01-01

    Abstract. Angle-resolved optical scattering properties of ovarian tissue, on different optical coherence tomography (OCT) imaging planes, were quantitatively measured by fitting the compounded OCT A-lines into a single scattering model. Higher cross correlation value of angle-resolved scattering coefficients between different OCT imaging planes was found in normal ovaries than was present in malignant ovaries. The mean cross correlation coefficient (MCC) was introduced in this pilot study to characterize and differentiate normal, n=6, and malignant, n=4, ovaries. A specificity of 100 percent and a sensitivity of 100 percent were achieved by setting MCC threshold at 0.6. Collagen properties, within the OCT imaging penetration depth, were also qualitatively studied in terms of their content, structure and directivity. The homogeneous three-dimensional collagen fiber network, observed in the normal ovary, effectively explains the stronger cross correlation of angle-resolved scattering properties on different imaging planes while the heterogeneity, observed in the malignant ovary, suggests a weaker correlation. PMID:23085900

  11. Coherent Detector for Near-Angle Scattering and Polarization Characterization of Telescope Mirror Coatings

    NASA Technical Reports Server (NTRS)

    Macenka, Steven A.; Chipman, Russell A.; Daugherty, Brian J.; McClain, Stephen C.

    2012-01-01

    A report discusses the difficulty of measuring scattering properties of coated mirrors extremely close to the specular reflection peak. A prototype Optical Hetero dyne Near-angle Scatterometer (OHNS) was developed. Light from a long-coherence-length (>150 m) 532-nm laser is split into two arms. Acousto-optic modulators frequency shift the sample and reference beams, establishing a fixed beat frequency between the beams. The sample beam is directed at very high f/# onto a mirror sample, and the point spread function (PSF) formed after the mirror sample is scanned with a pinhole. This light is recombined by a non-polarizing beam splitter and measured through heterodyne detection with a spectrum analyzer. Polarizers control the illuminated and analyzed polarization states, allowing the polarization dependent scatter to be measured. The bidirectional reflective or scattering distribution function is normally measured through use of a scattering goniometer instrument. The instrumental beam width (collection angle span) over which the scatterometer responds is typically many degrees. The OHNS enables measurement at angles as small as the first Airy disk diameter.

  12. Solution structure and excitation energy transfer in phycobiliproteins of Acaryochloris marina investigated by small angle scattering.

    PubMed

    Golub, M; Combet, S; Wieland, D C F; Soloviov, D; Kuklin, A; Lokstein, H; Schmitt, F-J; Olliges, R; Hecht, M; Eckert, H-J; Pieper, J

    2017-04-01

    The structure of phycobiliproteins of the cyanobacterium Acaryochloris marina was investigated in buffer solution at physiological temperatures, i.e. under the same conditions applied in spectroscopic experiments, using small angle neutron scattering. The scattering data of intact phycobiliproteins in buffer solution containing phosphate can be well described using a cylindrical shape with a length of about 225Å and a diameter of approximately 100Å. This finding is qualitatively consistent with earlier electron microscopy studies reporting a rod-like shape of the phycobiliproteins with a length of about 250 (M. Chen et al., FEBS Letters 583, 2009, 2535) or 300Å (J. Marquart et al., FEBS Letters 410, 1997, 428). In contrast, phycobiliproteins dissolved in buffer lacking phosphate revealed a splitting of the rods into cylindrical subunits with a height of 28Å only, but also a pronounced sample aggregation. Complementary small angle neutron and X-ray scattering experiments on phycocyanin suggest that the cylindrical subunits may represent either trimeric phycocyanin or trimeric allophycocyanin. Our findings are in agreement with the assumption that a phycobiliprotein rod with a total height of about 225Å can accommodate seven trimeric phycocyanin subunits and one trimeric allophycocyanin subunit, each of which having a height of about 28Å. The structural information obtained by small angle neutron and X-ray scattering can be used to interpret variations in the low-energy region of the 4.5K absorption spectra of phycobiliproteins dissolved in buffer solutions containing and lacking phosphate, respectively.

  13. Small angle neutron scattering modeling of copper-rich precipitates in steel

    SciTech Connect

    Spooner, S.

    1997-11-01

    The magnetic to nuclear scattering intensity ratio observed in the scattering from copper rich precipitates in irradiated pressure vessel steels is much smaller than the value of 11.4 expected for a pure copper precipitate in iron. A model for precipitates in pressure vessel steels which matches the observed scattering typically incorporates manganese, nickel, silicon and other elements and it is assumed that the precipitate is non-magnetic. In the present work consideration is given to the effect of composition gradients and ferromagnetic penetration into the precipitate on the small angle scattering cross section for copper rich clusters as distinguished from conventional precipitates. The calculation is an extension of a scattering model for micelles which consist of shells of varying scattering density. A discrepancy between recent SANS scattering experiments on pressure vessel steels was found to be related to applied magnetic field strength. The assumption of cluster structure and its relation to atom probe FIM findings as well as the effects of insufficient field for magnetic saturation is discussed.

  14. Small angle neutron scattering modeling of copper-rich precipitates in steel

    SciTech Connect

    Spooner, S.

    1997-11-01

    The magnetic-to-nuclear scattering intensity ratio observed in the scattering from copper-rich precipitates in irradiated pressure vessel steels is much smaller than the value of 11.4 expected for a pure copper precipitate in iron. A model for precipitates in pressure vessel steels which matches the observed scattering typically incorporates manganese, nickel, silicon and other elements and it is assumed that the precipitate is non-magnetic. In the present work consideration is given to the effect of composition gradients and ferromagnetic penetration into the precipitate on the small angle scattering cross section for copper-rich clusters as distinguished from conventional precipitates. The calculation is an extension of a scattering model for micelles which consist of shells of varying scattering density. A discrepancy between recent SANS scattering experiments on pressure vessel shells was found to be related to applied magnetic field strength. The assumption of cluster structure and its relation to atom probe FIM findings as well as the effects of insufficient field for magnetic saturation is discussed.

  15. Small-angle x-ray scattering studies of the manganese stabilizing subunit in photosystem II.

    SciTech Connect

    Svensson, B.; Tiede, D. M.; Barry, B. A.; Univ. of Minnesota

    2002-08-29

    Small-angle X-ray scattering studies (SAXS) were used to determine the size, shape, and oligomeric composition of the manganese stabilizing protein (MSP) of photosystem II. This extrinsic protein subunit plays an important role in photosynthetic oxygen evolution. As its name implies, MSP stabilizes the tetranuclear Mn cluster of the water oxidation complex. Removal of MSP lowers activity and decreases the stability of active-site manganese. Reconstitution of MSP reverses these effects. In this study, MSP was extracted from spinach PSII membranes using CaCl{sub 2} or urea. Through the use of MALDI-TOF mass spectrometry, the molecular weight of MSP was determined to be 26.53 kDa. X-ray scattering results show that both samples display a monodisperse scattering pattern; this pattern is consistent with a homogeneous protein solution. The CaCl{sub 2} extracted and urea extracted MSP samples have radii of gyration of 25.9 {+-} 0.4 and 27.0 {+-} 0.01 {angstrom}, respectively. MSP is shown to be monomeric in solution. This was determined using a cytochrome c standard and the scattering intensity, extrapolated to zero scattering angle, which is proportional to the molecular weight. This SAXS study suggests that, in solution, MSP is a monomeric, elongated prolate ellipsoid with dimensions, 112 x 23 x 23 {angstrom}{sup 3} and an axial ratio of 4.8.

  16. Characterising density fluctuations in liquid yttria aluminates with small angle x-ray scattering

    SciTech Connect

    Greaves, G. Neville; Wilding, Martin C.; Vu Van, Quang; Majerus, Odile; Hennet, Louis

    2009-01-29

    Small angle x-ray scattering (SAXS) has been measured in the wavevector range 0.01scatter from longer range fluctuating volumes.

  17. Small angle X-ray scattering study of coal soot formation

    SciTech Connect

    Winans, R. E.; Parker, J. T.; Seifert, S.; Fletcher, T. H.

    2000-02-14

    The objective of this study is to examine, by small angle X-ray scattering (SAXS), the formation of soot from individual coal particle combustion in a methane flat flame burner. The SAXS instrument at the Basic Energy Sciences Synchrotron Radiation Center (BESSRC) at the Advanced Photon Source (APS) can be used to observe both the formation of spherules and clusters since it can access length scales of 6--6000 {angstrom}. The high X-ray flux enables rapid acquisition of scattering data of various regions of the flame. SAXS data reveal particle size, shape, surface areas, and surface roughness.

  18. Chaotic scattering of pitch angles in the current sheet of the magnetotail

    NASA Technical Reports Server (NTRS)

    Burkhart, G. R.; Chen, J.

    1992-01-01

    The modified Harris field model is used to investigate the process of pitch angle scattering by a current sheet. The relationship between the incoming asymptotic pitch angle alpha(in) and the outgoing asymptotic pitch angle alpha(out) is studied from first principles by numerically integrating the equation of motion. Evidence that charged particles undergo chaotic scattering by the current sheet is found. For fixed alpha(in), it is shown that alpha(out) exhibits sensitive dependence on the energy parameter in certain energy ranges. For a fixed energy parameter value in the same energy ranges, alpha(out) sensitively depends on alpha(in). For other energy values, alpha(out) does not show sensitive dependence on alpha(in) for most phase angles. A distribution of alpha(in) is mapped from the asymptotic region to the midplane, and it is found that the resulting particle distribution should have beam structures with well-collimated pitch angles near each resonance energy value. Implications for the particle distribution functions in the earth's magnetotail are discussed.

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

    NASA Astrophysics Data System (ADS)

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

    2008-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-11-01

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

  1. Note: A gel based imaging technique of the iridocorneal angle for evaluation of angle-closure glaucoma

    NASA Astrophysics Data System (ADS)

    Shinoj, V. K.; Murukeshan, V. M.; Baskaran, M.; Aung, T.

    2014-06-01

    Noninvasive medical imaging techniques have high potential in the field of ocular imaging research. Angle closure glaucoma is a major disease causing blindness and a possible way of detection is the examination of the anterior chamber angle in eyes. Here, a simple optical method for the evaluation of angle-closure glaucoma is proposed and illustrated. The light propagation from the region associated with the iridocorneal angle to the exterior of eye is considered analytically. The design of the gel assisted probe prototype is carried out and the imaging of iridocorneal angle is performed on an eye model.

  2. Angle-beam shear wave scattering from buried crack-like defects in bonded specimens

    NASA Astrophysics Data System (ADS)

    Maki, Carson T.; Michaels, Jennifer E.; Weng, Yu; Michaels, Thomas E.

    2017-02-01

    Ultrasonic wavefield imaging, which refers to the measurement of wave motion on a 2-D rectilinear grid resulting from a fixed source, has been previously applied to angle-beam shear wave propagation in simple plates with through-holes and far-surface notches. In this prior work, scattered waves were analyzed using baseline subtraction of wavefields acquired before and after a notch was introduced. In practice, however, defects of interest often occur between bonded layers and it is generally not possible to record data from the same specimen in both the undamaged and damaged states, even in the laboratory. Direct baseline subtraction of wavefields thus becomes impractical as a tool for analyzing scattering. This present work considers measurement and analysis of angle-beam waves in bonded specimens with and without buried defects originating from fastener holes. Data from fastener holes with and without simulated damage in the form of notches are compared, and it is shown that wavefield baseline subtraction, even after correcting for misalignment between scans, is ineffective for isolating scattering from the notch. A combination of frequency-wavenumber filtering and spatial windowing is proposed and implemented as an alternative approach to quantify scattering from damage. Despite unavoidable deviations from specimen-to-specimen caused by factors such as variations in bonding, transducer mounting, and fastener hole machining, it is shown that scattering from buried notches can be clearly visualized in recorded wavefield data of bonded plates containing a buried defect as opposed to "baseline" wavefield data taken from a nominally similar specimen with no defect present. Backscattering is further quantified in the form of scattering patterns at different scattering frames to quantify the effect of the notch on the total backscattered wavefield.

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

    PubMed Central

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

    2016-01-01

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

  4. Solution properties of a CO{sub 2}-soluble fluoropolymer via small angle neutron scattering

    SciTech Connect

    McClain, J.B.; Combes, J.R.; Romack, T.J.; Canelas, D.A.; Betts, D.E.; Samulski, E.T.; DeSimone, J.M.; Londono, D.; Wignall, G.D.

    1996-01-31

    In this communication, we report the first characterization of solutions of a high molecular weight polymer in supercritical CO{sub 2} by small-angle neutron scattering (SANS). It is shown that small-angle neutron scattering gives key molecular parameters of an amorphous fluoropolymer in supercritical CO{sub 2}, i.e., the molecular weight, radius of gyration, and second virial coefficient, and thereby gives insights into a polymer chain`s behavior in this unique solvent. The positive sign of the second virial coefficients indicate that this medium is a good solvent - there is no evidence of a collapsed chain conformation. In fact, we conclude from the SANS data that, in CO{sub 2}, the poly(FOA) chain dimensions are expanded relative to those characteristic of its melt. 29 refs., 2 figs., 1 tab.

  5. Failure of the multiple peaking approximation for fast capture processes at milliradian scattering angles

    SciTech Connect

    Houamer, Salim; Popov, Yuri V.; Dal Cappello, Claude

    2010-03-15

    The first Born approximation is examined for different fast capture processes for the p+He system at incident energies of about 1 MeV. Calculations have been performed for the singly differential cross section (SDCS) for scattering angles 0-0.5 mrad in the laboratory frame. In the case of transfer ionization, we observe that the two-step-2 mechanism has a dominant contribution to the SDCS for the kinematics considered in this work. The present investigation demonstrates that the multiple peaking approximation is a very crude method which fails to describe the SDCS even at scattering angles below 0.5 mrad. We have also presented a doubly differential cross section for the fixed emission energy of 600 eV and compared our results with other theoretical calculations and experiments.

  6. Photon spectra calculation for an Elekta linac beam using experimental scatter measurements and Monte Carlo techniques.

    PubMed

    Juste, B; Miro, R; Campayo, J M; Diez, S; Verdu, G

    2008-01-01

    The present work is centered in reconstructing by means of a scatter analysis method the primary beam photon spectrum of a linear accelerator. This technique is based on irradiating the isocenter of a rectangular block made of methacrylate placed at 100 cm distance from surface and measuring scattered particles around the plastic at several specific positions with different scatter angles. The MCNP5 Monte Carlo code has been used to simulate the particles transport of mono-energetic beams to register the scatter measurement after contact the attenuator. Measured ionization values allow calculating the spectrum as the sum of mono-energetic individual energy bins using the Schiff Bremsstrahlung model. The measurements have been made in an Elekta Precise linac using a 6 MeV photon beam. Relative depth and profile dose curves calculated in a water phantom using the reconstructed spectrum agree with experimentally measured dose data to within 3%.

  7. Grazing Angle Proton Scattering: Effects on Chandra and XMM-Newton X-Ray Telescopes

    DTIC Science & Technology

    2003-12-01

    these scattering models calculation . As expected the MCNPX results have broad, low are valid for moderately large angles of incidence, or cases energy...the incident particle will enter into the bulk MCNPX calculated values show a much larger energy losses material, if the particle trajectory is not...properties - Flmov FormuIa Calculation [ and will not change significantly for the mirror materials. SJ Oinc 0.20 MCNPX and Geant4 calculations

  8. Two-dimensional position-sensitive detectors for small-angle neutron scattering

    SciTech Connect

    McElhaney, S.A.; Vandermolen, R.I.

    1990-05-01

    In this paper, various detectors available for small angle neutron scattering (SANS) are discussed, along with some current developments being actively pursued. A section has been included to outline the various methodologies of position encoding/decoding with discussions on trends and limitations. Computer software/hardware vary greatly from institute and experiment and only a general discussion is given to this area. 85 refs., 33 figs.

  9. Angle-resolved surface-enhanced Raman scattering on metallic nanostructured plasmonic crystals.

    PubMed

    Baumberg, Jeremy J; Kelf, Timothy A; Sugawara, Yoshihiro; Cintra, Suzanne; Abdelsalam, Mamdouh E; Bartlett, Phillip N; Russell, Andrea E

    2005-11-01

    Surface-enhanced Raman scattering is an ideal tool for identifying molecules from the "fingerprint" of their molecular bonds; unfortunately, this process lacks a full microscopic understanding and, practically, is plagued with irreproducibility. Using nanostructured metal surfaces, we demonstrate strong correlations between plasmon resonances and Raman enhancements. Evidence for simultaneous ingoing and outgoing resonances in wavelength and angle sheds new light on the Raman enhancement process, allowing optimization of a new generation of reproducible Raman substrates.

  10. Small-Angle Neutron Scattering by the Magnetic Microstructure of Nanocrystalline Ferromagnets Near Saturation

    PubMed Central

    Weissmüller, J.; McMichael, R. D.; Michels, A.; Shull, R. D.

    1999-01-01

    The paper presents a theoretical analysis of elastic magnetic small-angle neutron scattering (SANS) due to the nonuniform magnetic microstructure in nanocrystalline ferromagnets. The reaction of the magnetization to the magnetocrystalline and magnetoelastic anisotropy fields is derived using the theory of micromagnetics. In the limit where the scattering volume is a single magnetic domain, and the magnetization is nearly aligned with the direction of the magnetic field, closed form solutions are given for the differential scattering cross-section as a function of the scattering vector and of the magnetic field. These expressions involve an anisotropy field scattering function, that depends only on the Fourier components of the anisotropy field microstructure, not on the applied field, and a micromagnetic response function for SANS, that can be computed from tabulated values of the materials parameters saturation magnetization and exchange stiffness constant or spin wave stiffness constant. Based on these results, it is suggested that the anisotropy field scattering function SH can be extracted from experimental SANS data. A sum rule for SH suggests measurement of the volumetric mean square anisotropy field. When magnetocrystalline anisotropy is dominant, then a mean grain size or the grain size distribution may be determined by analysis of SH.

  11. Method and Apparatus for Measuring Near-Angle Scattering of Mirror Coatings

    NASA Technical Reports Server (NTRS)

    Chipman, Russell A. (Inventor); Daugherty, Brian J. (Inventor); McClain, Stephen C. (Inventor); Macenka, Steven A. (Inventor)

    2013-01-01

    Disclosed herein is a method of determining the near angle scattering of a sample reflective surface comprising the steps of: a) splitting a beam of light having a coherence length of greater than or equal to about 2 meters into a sample beam and a reference beam; b) frequency shifting both the sample beam and the reference beam to produce a fixed beat frequency between the sample beam and the reference beam; c) directing the sample beam through a focusing lens and onto the sample reflective surface, d) reflecting the sample beam from the sample reflective surface through a detection restriction disposed on a movable stage; e) recombining the sample beam with the reference beam to form a recombined beam, followed by f) directing the recombined beam to a detector and performing heterodyne analysis on the recombined beam to measure the near-angle scattering of the sample reflective surface, wherein the position of the detection restriction relative to the sample beam is varied to occlude at least a portion of the sample beam to measure the near-angle scattering of the sample reflective surface. An apparatus according to the above method is also disclosed.

  12. Small-angle scatter tomography with a photon-counting detector array

    NASA Astrophysics Data System (ADS)

    Pang, Shuo; Zhu, Zheyuan; Wang, Ge; Cong, Wenxiang

    2016-05-01

    Small-angle x-ray scatter imaging has a high intrinsic contrast in cancer research and other applications, and provides information on molecular composition and micro-structure of the tissue. In general, the implementations of small-angle coherent scatter imaging can be divided into two main categories: direct tomography and angular dispersive computerized tomography. Based on the recent development of energy-discriminative photon-counting detector array, here we propose a computerized tomography setup based on energy-dispersive measurement with a photon-counting detector array. To show merits of the energy-dispersive approach, we have performed numerical tests with a phantom containing various tissue types, in comparison with the existing imaging approaches. The results show that with an energy resolution of ~6 keV, the energy dispersive tomography system with a broadband tabletop x-ray would outperform the angular dispersive system, which makes the x-ray small-angle scatter tomography promising for high-specificity tissue imaging.

  13. Pitch angle scattering by triggered emissions from the Siple Station wave injection experiment

    NASA Astrophysics Data System (ADS)

    Harid, V.; Golkowski, M.; Bell, T. F.; Cohen, M.; Inan, U. S.

    2012-12-01

    Nonlinear amplification of whistler mode waves in the Earth's magnetosphere , due to gyroresonance with energetic electrons, also known as the phenomena of VLF triggered emissions, has been investigated extensively with analytical formulations, experimental observations and computer simulations. However, the pitch angle scattering of typical triggered emission waveforms has not been specifically considered. Most authors consider particle scattering either in the presence of a monochromatic constant amplitude wave or a broadband incoherent but time-frequency homogenous emission. Although investigation of these two limiting cases has provided valuable insight into radiation belt dynamics, a large class of waves including triggered emissions and chorus do not fall under either of the two descriptions. The inherent symmetry of a constant amplitude monochromatic wave around the equator results in non-cumulative pitch angle change for a large population of electrons. Wave amplification generated during linear and nonlinear growth result in wave gradients that can have a more significant effect on particle pitch angle and energy. In addition, coherent frequency changing signals are capable of shifting the cyclotron resonance condition and significantly perturbing particle trajectories from their adiabatic motion. The wave-injection experiment at Siple Station, Antarctica was designed to study wave growth and triggering processes in the magnetosphere. Amplified signals from Siple Station often show both wave gradients as well advances in phase and frequency. Using a numerical test-particle simulation, we model the effect of typical Siple Station signals on pitch angle scattering and particle precipitation. Results show that triggered emission type wave forms are more efficient in producing large pitch angle changes in resonant particles.

  14. Electromagnetic Scattered Field Evaluation and Data Compression Using Imaging Techniques

    NASA Technical Reports Server (NTRS)

    Gupta, I. J.; Burnside, W. D.

    1996-01-01

    This is the final report on Project #727625 between The Ohio State University and NASA, Lewis Research Center, Cleveland, Ohio. Under this project, a data compression technique for scattered field data of electrically large targets is developed. The technique was applied to the scattered fields of two targets of interest. The backscattered fields of the scale models of these targets were measured in a ra compact range. For one of the targets, the backscattered fields were also calculated using XPATCH computer code. Using the technique all scattered field data sets were compressed successfully. A compression ratio of the order 40 was achieved. In this report, the technique is described briefly and some sample results are included.

  15. Convex and concave successions of power-law decays in small-angle scattering

    NASA Astrophysics Data System (ADS)

    Anitas, E. M.

    2016-08-01

    The small-angle scattering (SAS) structure factor from a new model of a 3D deterministic fractal in which the relative positions and the number of structural units vary with fractal iteration number is calculated. It is shown that, depending on the relative positions of scattering units inside the fractal, we can obtain various types of power-law successions, such as: convex/concave - when the absolute value of the scattering exponent of the first power-law decay is higher/smaller than that of the subsequent power- law decay, or any combination of them (i.e. convex-concave or concave-convex). The obtained results can explain experimental SAS (neutron or X-rays) data which are characterized by a succession of power-law decays of arbitrary length.

  16. Nucleon-nucleon scattering at small angles, measured at ANKE-COSY

    NASA Astrophysics Data System (ADS)

    Bagdasarian, Z.

    2016-03-01

    The most accepted approach to describe nucleon-nucleon (NN) interaction is the partial wave analysis (PWA), which translates various experimental observables to the common language of the partial waves. The reliable analysis relies not only on the quality experimental data, but also on the measurements of scattering observables over preferably the full angular range. Small angle scattering has been measured for six beam energies between 0.8 and 2.4 GeV using polarized proton beam incident on both proton and deuteron unpolarized targets at COSY-ANKE. This proceeding will report on the published and preliminary results for both pp and pn scattering from this and other recent experiments at ANKE. This study aims to provide the valuable observables to the SAID group in order to improve the phenomenological understanding of the nucleon-nucleon interaction.

  17. Generalized ISAR--part II: interferometric techniques for three-dimensional location of scatterers.

    PubMed

    Given, James A; Schmidt, William R

    2005-11-01

    This paper is the second part of a study dedicated to optimizing diagnostic inverse synthetic aperture radar (ISAR) studies of large naval vessels. The method developed here provides accurate determination of the position of important radio-frequency scatterers by combining accurate knowledge of ship position and orientation with specialized signal processing. The method allows for the simultaneous presence of substantial Doppler returns from both change of roll angle and change of aspect angle by introducing generalized ISAR ates. The first paper provides two modes of interpreting ISAR plots, one valid when roll Doppler is dominant, the other valid when the aspect angle Doppler is dominant. Here, we provide, for each type of ISAR plot technique, a corresponding interferometric ISAR (InSAR) technique. The former, aspect-angle dominated InSAR, is a generalization of standard InSAR; the latter, roll-angle dominated InSAR, seems to be new to this work. Both methods are shown to be efficient at identifying localized scatterers under simulation conditions.

  18. Bilayer thickness in unilamellar phosphatidylcholine vesicles: small-angle neutron scattering using contrast variation

    NASA Astrophysics Data System (ADS)

    Kučerka, N.; Uhríková, D.; Teixeira, J.; Balgavý, P.

    2004-07-01

    The thickness of the lipid bilayer in extruded unilamellar vesicles prepared from synthetic 1,2-diacyl-sn-glycero-3-phosphorylcholines with monounsaturated acyl chains (diCn:1PC, n=14-22) was studied at 30°C in the small-angle neutron scattering (SANS) experiment. Several contrasts of the neutron scattering length density between the aqueous phase and phospholipid bilayer of vesicles were used. The experimental data were evaluated using the small-angle form of the Kratky-Porod approximation ln[I(q)q2] vs. q2 of the SANS intensity I(q) in the appropriate range of scattering vector values q to obtain the bilayer radius of gyration Rg and its extrapolated value at infinite scattering contrast Rginf. The bilayer thickness parameter evaluated from a linear approximation of dependence of gyration radius on the inverse contrast was then obtained without using any bilayer structure model. The dependence of the thickness parameter dg≅120.5Rginf on the number n of acyl chain carbons was found to be linear with a slope of 1.8+/-0.2Å per one acyl chain carbon. This slope can be used in bilayer-protein interaction studies.

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

    NASA Astrophysics Data System (ADS)

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

    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 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.

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

    PubMed

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

    2016-07-01

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

  1. Thorough small-angle X-ray scattering analysis of the instability of liquid micro-jets in air.

    PubMed

    Marmiroli, Benedetta; Cacho-Nerin, Fernando; Sartori, Barbara; Pérez, Javier; Amenitsch, Heinz

    2014-01-01

    Liquid jets are of interest, both for their industrial relevance and for scientific applications (more important, in particular for X-rays, after the advent of free-electron lasers that require liquid jets as sample carrier). Instability mechanisms have been described theoretically and by numerical simulation, but confirmed by few experimental techniques. In fact, these are mainly based on cameras, which is limited by the imaging resolution, and on light scattering, which is hindered by absorption, reflection, Mie scattering and multiple scattering due to complex air/liquid interfaces during jet break-up. In this communication it is demonstrated that synchrotron small-angle X-ray scattering (SAXS) can give quantitative information on liquid jet dynamics at the nanoscale, by detecting time-dependent morphology and break-up length. Jets ejected from circular tubes of different diameters (100-450 µm) and speeds (0.7-21 m s(-1)) have been explored to cover the Rayleigh and first wind-induced regimes. Various solvents (water, ethanol, 2-propanol) and their mixtures have been examined. The determination of the liquid jet behaviour becomes essential, as it provides background data in subsequent studies of chemical and biological reactions using SAXS or X-ray diffraction based on synchrotron radiation and free-electron lasers.

  2. Nonuniformity in natural rubber as revealed by small-angle neutron scattering, small-angle X-ray scattering, and atomic force microscopy.

    PubMed

    Karino, Takeshi; Ikeda, Yuko; Yasuda, Yoritaka; Kohjiya, Shinzo; Shibayama, Mitsuhiro

    2007-02-01

    The microscopic structures of natural rubber (NR) and deproteinized NR (DPNR) were investigated by means of small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), and atomic force microscopy (AFM). They were compared to those of isoprene rubber (IR), which is a synthetic analogue of NR in terms of chemical structure without any non-rubber components like proteins. Comparisons of the structure and mechanical properties of NR, DPNR, and IR lead to the following conclusions. (i) The well-known facts, for example, the outstanding green strength of NR and strain-induced crystallization, are due not much to the presence of proteins but to other components such as the presence of phospholipids and/or the higher stereoregularity of NR. It also became clear the naturally residing proteins accelerate the upturn of stress at low strain. The protein phases work as cross-linking sites and reinforcing fillers in the rubbery matrix. (ii) The microscopic structures of NR were successfully reproduced by SANS intensity functions consisting of squared-Lorentz and Lorentz functions, indicating the presence of inhomogeneities in bulk and thermal concentration fluctuations in swollen state, respectively. On the other hand, IR rubbers were homogeneous in bulk. (iii) The inhomogeneities in NR are assigned to protein aggregates of the order of 200 A or larger. Although these aggregates are larger in size as well as in volume fraction than those of cross-link inhomogeneities introduced by cross-linking, they are removed by deproteinization. (iv) Swelling of both NR and IR networks introduces gel-like concentration fluctuations whose mesh size is of the order of 20 A.

  3. EDITORIAL Proceedings of the XIV International Conference on Small-Angle Scattering, SAS-2009

    NASA Astrophysics Data System (ADS)

    Ungar, Goran; Heenan, Richard

    2010-10-01

    There are 52 papers in these Proceedings. The papers are divided into 10 thematic sections and a section for invited papers and reviews. The sections and the respective section editors are given below. Section Editor(s) Invited Papers and Reviews Peter Griffiths, Wim Bras, Rudolf Winter Beamlines and Instrumentation Elliot Gilbert, Wim Bras, Nigel Rhodes Theory, Data processing and Modelling Jan Skov Pedersen, Carlo Knupp Biological Systems and Membranes Richard Heenan, Cameron Neylon Ceramics, Glasses and Porous Materials Rudolf Winter Colloids and Solutions Peter Griffiths Hierarchical Structures and Fibres Steve Eichhorn, Karen Edler Metallic and Magnetic Systems Armin Hoell Polymers Patrick Fairclough Time resolved Diffraction, Kinetic and Dynamical Studies João Cabral, Christoph Rau We are grateful to all section editors and the many anonymous referees for their invaluable effort which made the publication of the Proceedings possible. The refereeing process was strict and thorough, some papers were rejected and most were improved. The resulting compendium gives a good overview of recent developments in small-angle X-ray and neutron scattering theory, application, methods of analysis and instrumentation. Thus it should be a useful source of reference for a number of years to come. The papers are a good reflection of the material presented at the meeting. Because of the general high quality of the articles, it was difficult to decide which to highlight and be fair to all contributors. The following in particular have caught the attention of the editors. Highlighted papers A statistical survey of publications reporting the application of SAXS and SANS by Aldo Craievich (paper 012003) is recommended reading for anyone needing convincing about the vibrancy of this scientific field and the ever expanding use of these techniques. Two aspects of coherent X-ray scattering, made available by the advent of the 3rd generation synchrotron sources, are discussed in the

  4. Effect of EMIC Wave Normal Angle Distribution on Relativistic Electron Scattering

    NASA Technical Reports Server (NTRS)

    Gamayunov, K. V.; Khazanov, G. V.

    2006-01-01

    The flux level of outer-zone relativistic electrons (above 1 MeV) is extremely variable during geomagnetic storms, and controlled by a competition between acceleration and loss. Precipitation of these electrons due to resonant pitch-angle scattering by electromagnetic ion cyclotron (EMIC) waves is considered one of the major loss mechanisms. This mechanism was suggested in early theoretical studies more than three decades ago. However, direct experimental evidence of the wave role in relativistic electrons precipitation is difficult to obtain because of lack of concurrent measurements of precipitating electrons at low altitudes and the waves in a magnetically conjugate equatorial region. Recently, the data from balloon-borne X-ray instruments provided indirect but strong evidence on an efficiency of the EMIC wave induced loss for the outer-zone relativistic electrons. These observations stimulated theoretical studies that, particularly, demonstrated that EMIC wave induced pitch-angle diffusion of MeV electrons can operate in the strong diffusion limit and this mechanism can compete with relativistic electron depletion caused by the Dst effect during the initial and main phases of storm. Although an effectiveness of relativistic electron scattering by EMIC waves depends strongly on the wave spectral properties, the most favorable assumptions regarding wave characteristics has been made in all previous theoretical studies. Particularly, only quasi field-aligned EMIC waves have been considered as a driver for relativistic electron loss. At the same time, there is growing experimental and theoretical evidence that these waves can be highly oblique; EMIC wave energy can occupy not only the region of generation, i.e. the region of small wave normal angles, but also the entire wave normal angle region, and even only the region near 90 degrees. The latter can dramatically change he effectiveness of relativistic electron scattering by EMIC waves. In the present study, we

  5. Ternary systems of nonionic surfactant Brij 35, water and various simple alcohols: Structural investigations by small-angle X-ray scattering and dynamic light scattering.

    PubMed

    Tomsic, Matija; Bester-Rogac, Marija; Jamnik, Andrej; Kunz, Werner; Touraud, Didier; Bergmann, Alexander; Glatter, Otto

    2006-02-01

    Structural properties of ternary systems composed of nonionic surfactant dodecyl-poly(ethylene oxide-23) ether (C12E23, commercial name: Brij 35), water and various alcohols from ethanol to 1-decanol have been investigated using small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS) techniques. All measurements were performed at the temperature 25 degrees C. SAXS experimental data were put on absolute scale using water as a secondary standard. The data of water-rich mixtures at low to moderate surfactant concentrations were evaluated using the generalized indirect Fourier transformation method (GIFT), which is based on the simultaneous determination of the intra- and inter-particle scattering contributions. In this way, the size and the shape of interacting scattering particles in real space could be deduced. The systems with a relatively low surfactant concentration (5 mass%) were studied most extensively. In these cases, the water-rich regions of the phase diagrams could be investigated into more detail, since in the alcohol-rich regions problems with the GIFT evaluation of the SAXS data were encountered. The presented results demonstrate the level of structural details that can be obtained on the basis of scattering methods and point out the specific stages of data evaluation and interpretation where one must be extremely precautious. As such they reveal the inner structuration of the complex ternary systems of our present interest. In parallel, they also indicate that the longer chain alcohols actually behave as real oil phases in the studied systems, as one might expect, and also confirm the well-known properties of different short to medium chain alcohols that act as co-solvents and/or co-surfactants in microemulsion systems depending on their chain length.

  6. Monitoring simultaneously the growth of nanoparticles and aggregates by in situ ultra-small-angle x-ray scattering

    SciTech Connect

    Kammler, Hendrik K.; Beaucage, Gregory; Kohls, Douglas J.; Agashe, Nikhil; Ilavsky, Jan

    2005-03-01

    Ultra-small-angle x-ray scattering can provide information about primary particles and aggregates from a single scattering experiment. This technique is applied in situ to flame aerosol reactors for monitoring simultaneously the primary particle and aggregate growth dynamics of oxide nanoparticles in a flame. This was enabled through the use of a third generation synchrotron source (Advanced Photon Source, Argonne IL, USA) using specialized scattering instrumentation at the UNICAT facility which is capable of simultaneously measuring nanoscales to microscales (1 nm to 1 {mu}m). More specifically, the evolution of primary-particle diameter, mass-fractal dimension, geometric standard deviation, silica volume fraction, number concentration, radius of gyration of the aggregate, and number of primary particles per aggregate are measured along the flame axis for two different premixed flames. All these particle characteristics were derived from a single and nonintrusive measurement technique. Flame temperature profiles were measured in the presence of particles by in situ Fourier transform infrared spectroscopy and thermophoretic sampling was used to visualize particle growth with height above the burner as well as in the radial direction.

  7. Low Angle X-Ray Scattering Of Chloroplast With CKa Radiation

    NASA Astrophysics Data System (ADS)

    Paradies, Hasko H.

    1982-10-01

    The operational range of low angle x-ray scattering was extended to particles and structures of about 1 to 2µm by using CKa radiation with a wavelength of 44.7 A . For particles of about 1µm in diameter, the central scattering was not observed accurately with characteristic x rays such as CuKa. The size, shape, and hydration of chloroplasts have been measured by using low angle soft x-ray scattering with CKa radia-tion, emitted from a high power x-ray tube and from synchrotron radiation. Chloroplasts were found to have a radius of gyration of 2.15 +/- 0.5 um, corresponding to a particle diameter of 5.8 +/- 0.2 µm. The volume was calculated from Porod's invariant and was found to be 41.0 +/- 12.0 ttm3. Absolute measurements were performed directly, without weakening the primary beam, permitting the calculations of the mass of a chloroplast. The mass of the chloroplast was found to be 40.0 +/- 0.07 pg, containing 0.45 pg H20/pg chloroplast. The maximum enlargement of the chloroplast particle was determined from the pair distribution function and was found to be 5.8 +/- 0.2 Am. The central scattering for the chloroplast with a diameter of 6.0 um was observed within 20' of the scattering angle with CKa radiation. The origin of the difference from the nominal value in the Guinier region can be ascribed to the effect of interparticle interference when changing the density of the solvent to 10% glycerol. It should be pointed out that the use of this radiation and a synchrotron source enables us to obtain scattering of particles of Am size, almost free from the influence of the direct beam and parasitic scattering. Furthermore, by recording the intensity autocorrelation function, from which the weight average and number averaged radii of gyration, size, and size distribution can be obtained, we are enabled to study the relative dispersion from dilute particle dispersion within 0.01 arcsec and the physicochemical changes of whole cells and organelles with respect to

  8. Low Angle X-Ray Scattering Of Chloroplast With CK α-Radiation

    NASA Astrophysics Data System (ADS)

    Paradies, Hasko H.

    1982-03-01

    The operational range of low angle X-ray scattering was extended to particles and structures of about 1-2 μm by using CKα-radiation with a wavelength of 44.7 Å. For particles of about 1 μm in diameter, the central scattering was not observed accurately with characteristic X-rays such as CuKα. The size, shape and hydration of chloroplast have been measured by using low angle soft X-ray scattering with CKα-radiation, emitted from a high power X-ray tube and from synchrotron radiation. Chloroplasts were found to have a radius of gyration of 2.15 ± 0.5 μm, corresponding to a particle diameter of 5.8 ± 0.2 μm. The volume was calculated from Porod's invariant and was found to be 41.0 ± 12.0 μm3. Absolute measurements were performed directly, without weakening the primary beam, permitting the calculation of the mass of a chloroplast. The mass of the chloroplast was found to be 40.0 ± 0.07 pg, containing 0.45 pg H20/pg chloroplast. The maximum enlargement of the chloroplast particle was determined from the pair distribution function and was found to be 5.8 ± 0.2 pm. The central scattering for the chloroplast with a diameter of 6.0 μm was observed with-in 20' of the scattering angle with CKα-radiation. The origin of the difference from the nominal value in the Guinier region can be ascribed to the effect of interparticle interference when changing the density of the solvent to 10% glycerol. It should be pointed out that the use of this radiation and a synchrotron source enables us to obtain scattering of particles of μm size, almost free from the influence of the direct beam and parasitic scattering. Furthermore, by recording the intensity autocorrelation function, from which the weight average and number averaged radii of gyration, size and size distribution can be obtained, we are enabled to study the relative dispersion from dilute particle dispersion within 0.01 arcsec and the physico-chemical changes of whole cells and organelles with respect to aging

  9. Nanostructure surveys of macroscopic specimens by small-angle scattering tensor tomography.

    PubMed

    Liebi, Marianne; Georgiadis, Marios; Menzel, Andreas; Schneider, Philipp; Kohlbrecher, Joachim; Bunk, Oliver; Guizar-Sicairos, Manuel

    2015-11-19

    The mechanical properties of many materials are based on the macroscopic arrangement and orientation of their nanostructure. This nanostructure can be ordered over a range of length scales. In biology, the principle of hierarchical ordering is often used to maximize functionality, such as strength and robustness of the material, while minimizing weight and energy cost. Methods for nanoscale imaging provide direct visual access to the ultrastructure (nanoscale structure that is too small to be imaged using light microscopy), but the field of view is limited and does not easily allow a full correlative study of changes in the ultrastructure over a macroscopic sample. Other methods of probing ultrastructure ordering, such as small-angle scattering of X-rays or neutrons, can be applied to macroscopic samples; however, these scattering methods remain constrained to two-dimensional specimens or to isotropically oriented ultrastructures. These constraints limit the use of these methods for studying nanostructures with more complex orientation patterns, which are abundant in nature and materials science. Here, we introduce an imaging method that combines small-angle scattering with tensor tomography to probe nanoscale structures in three-dimensional macroscopic samples in a non-destructive way. We demonstrate the method by measuring the main orientation and the degree of orientation of nanoscale mineralized collagen fibrils in a human trabecula bone sample with a spatial resolution of 25 micrometres. Symmetries within the sample, such as the cylindrical symmetry commonly observed for mineralized collagen fibrils in bone, allow for tractable sampling requirements and numerical efficiency. Small-angle scattering tensor tomography is applicable to both biological and materials science specimens, and may be useful for understanding and characterizing smart or bio-inspired materials. Moreover, because the method is non-destructive, it is appropriate for in situ measurements and

  10. Nanostructure surveys of macroscopic specimens by small-angle scattering tensor tomography

    NASA Astrophysics Data System (ADS)

    Liebi, Marianne; Georgiadis, Marios; Menzel, Andreas; Schneider, Philipp; Kohlbrecher, Joachim; Bunk, Oliver; Guizar-Sicairos, Manuel

    2015-11-01

    The mechanical properties of many materials are based on the macroscopic arrangement and orientation of their nanostructure. This nanostructure can be ordered over a range of length scales. In biology, the principle of hierarchical ordering is often used to maximize functionality, such as strength and robustness of the material, while minimizing weight and energy cost. Methods for nanoscale imaging provide direct visual access to the ultrastructure (nanoscale structure that is too small to be imaged using light microscopy), but the field of view is limited and does not easily allow a full correlative study of changes in the ultrastructure over a macroscopic sample. Other methods of probing ultrastructure ordering, such as small-angle scattering of X-rays or neutrons, can be applied to macroscopic samples; however, these scattering methods remain constrained to two-dimensional specimens or to isotropically oriented ultrastructures. These constraints limit the use of these methods for studying nanostructures with more complex orientation patterns, which are abundant in nature and materials science. Here, we introduce an imaging method that combines small-angle scattering with tensor tomography to probe nanoscale structures in three-dimensional macroscopic samples in a non-destructive way. We demonstrate the method by measuring the main orientation and the degree of orientation of nanoscale mineralized collagen fibrils in a human trabecula bone sample with a spatial resolution of 25 micrometres. Symmetries within the sample, such as the cylindrical symmetry commonly observed for mineralized collagen fibrils in bone, allow for tractable sampling requirements and numerical efficiency. Small-angle scattering tensor tomography is applicable to both biological and materials science specimens, and may be useful for understanding and characterizing smart or bio-inspired materials. Moreover, because the method is non-destructive, it is appropriate for in situ measurements and

  11. Comparison of models and measurements of angle-resolved scatter from irregular aerosols

    NASA Astrophysics Data System (ADS)

    Milstein, Adam B.; Richardson, Jonathan M.

    2015-01-01

    We have developed and validated a method for modeling the elastic scattering properties of biological and inert aerosols of irregular shape at near- and mid-wave infrared wavelengths. The method, based on Gaussian random particles, calculates the ensemble-average optical cross section and Mueller scattering matrix, using the measured aerodynamic size distribution and previously-reported refractive index as inputs. The utility of the Gaussian particle model is that it is controlled by only two parameters (σ and Γ) which we have optimized such that the model best reproduces the full angle-resolved Mueller scattering matrices measured at λ=1.55 μm in the Standoff Aerosol Active Signature Testbed (SAAST). The method has been applied to wet-generated singlet biological spore samples, dry-generated biological spore clusters, and kaolin. The scattering computation is performed using the Discrete Dipole Approximation (DDA), which requires significant computational resources, and is thus implemented on LLGrid, a large parallel grid computer. For the cases presented, the best fit Gaussian particle model is in good qualitative correspondence with microscopy images of the corresponding class of particles. The measured and computed cross sections agree well within a factor of two overall, with certain cases bearing closer correspondence. In particular, the DDA reproduces the shape of the measured scatter function more accurately than Mie predictions. The DDA-computed depolarization factors are also in good agreement with measurement.

  12. Small angle light scattering characterization of single micrometric particles in microfluidic flows

    NASA Astrophysics Data System (ADS)

    Dannhauser, David; Romeo, Giovanni; Causa, Filippo; Netti, Paolo A.

    2013-04-01

    A CCD-camera based small angle light scattering (SALS) apparatus has been used to characterize single micrometric particles flowing in a micro-channel. The measured scattering vector spans the range 2x10-2 - 6:8x101μm-1. The incident laser light is collimated to a spot of about 50 μm in diameter at the sample position with a divergence lower than 0.045 rad. Such small collimated laser beam opens the possibility to perform on-line SALS of micron-sized particles flowing in micro-channels. By properly designing the micro-channel and using a viscoelastic liquid as suspending medium we are able to realize a precise 3D focusing of the target particles. The forward scattering emitted from the particle is collected by a lens with high numerical aperture. At the focal point of that lens a homemade beam stop is blocking the incident light. Finally, a second lens maps the scattered light on the CCD sensor, allowing to obtain far field images on short distances. Measurements with mono-disperse polystyrene particles, both in quiescent and in-flow conditions have been realized. Experiments in-flow allow to measure the single particle scattering. Results are validated by comparison with calculations based on the Lorenz-Mie theory. The quality of the measured intensity profiles confirms the possibility to use our apparatus in real multiplex applications, with particles down to 1 μm in radius.

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

    NASA Astrophysics Data System (ADS)

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

    1981-02-01

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

  14. Small-angle X-ray scattering from salt-free solutions of star-branched polyelectrolytes

    NASA Astrophysics Data System (ADS)

    Heinrich, M.; Rawiso, M.; Zilliox, J. G.; Lesieur, P.; Simon, J. P.

    2001-02-01

    The dispersion state of sodium-sulphonated polystyrene (ensuremathNaPSS) star-branched polyelectrolytes was investigated in salt-free aqueous solutions, by use of the small-angle X-ray scattering technique. With respect to polystyrene (PS) star-branched polymers of identical functionality, the ordering phenomenon occurring in the neighborhood of the overlap concentration c^* is reinforced and observed in a larger range of concentrations. Moreover, the degree of order is no longer maximum at c^* and is improved as the concentration decreases. The dispersion state is then mainly controlled by the electrostatic interaction. A crystalline order should therefore be achieved with stars of lower functionality, provided the electrostatic interaction is added to the osmotic repulsion. On the other hand, unusual scattering patterns are measured for aqueous solutions of ensuremathNaPSS star polyelectrolytes. Indeed, a diffuse scattering is revealed at high angles, in addition to the regular diffraction rings related to preferred interstar distances. It is similar to the broad scattering peak produced by semidilute solutions of ensuremathNaPSS linear polyelectrolytes and associated to the electrostatic correlation hole within the isotropic model. In the dilute regime (c< c^*), it is just an intramolecular characteristic and represents the electrostatic repulsion between arms belonging to the same star. In the semidilute regime (c> c^*), it also reflects the electrostatic repulsion between arms of distinct stars. So, as the concentration increases, it is mainly caused by the interpenetration of ensuremathNaPSS stars. Such an observation is in agreement with the composite structure earlier proposed by Daoud and Cotton for star semidilute solutions. For c> c^*, ensuremathNaPSS star aqueous solutions can therefore be pictured as effective stars immersed in a matrix formed by the overlap of the arm ends. With respect to the dilute regime, the effective stars are smaller; the higher

  15. A Laboratory Scale Critical-Dimension Small-Angle X-ray Scattering Instrument

    SciTech Connect

    Ho, Derek L.; Wang Chengqing; Lin, Eric K.; Jones, Ronald L.; Wu Wenli

    2007-09-26

    New methods for critical dimension (CD) measurements may be needed to enable the detailed characterization of nanoscale structures produced in the semiconductor industry and for nanotechnology applications. In earlier work, small angle x-ray scattering (SAXS) measurements with synchrotron sources have shown promise in meeting several grand challenges for CD metrology. However, it is not practical to depend upon x-ray synchrotron sources, which are large national facilities with limitations in the number of available instruments. To address this problem, a laboratory scale SAXS instrument for critical dimension measurements on periodic nanoscale patterns has been designed, installed, and tested. The system possesses two configurations, SAXS and ultra-small-angle x-ray scattering (USAXS), with a radiation target of either copper or molybdenum. With these configurations, the instrument is capable of accessing scattering angles that probe length scales ranging from ca. 0.5 nm to 2 {mu}m. In this work, we compare CD-SAXS measurements taken from a synchrotron-based SAXS at the Advanced Photon Source of the Argonne National Laboratory with those from the National Institute of Standards and Technology laboratory-scale SAXS instrument. The results from standard line/space gratings possessing periodic line-space patterns with CDs of tens to hundreds of nanometers show that the laboratory-scale system can quantitatively measure parameters, such as the pitch, line width, height, line-width roughness and sidewall angle. These results show that laboratory-scale measurements are feasible and can be used for research and development purposes or to assist calibration of optical scatterometry and CD-scanning electron microscopy instruments. The primary limitation of the measurement is that the data collection rate is unacceptably slow for production metrology because of the significantly lower x-ray beam fluxes currently available.

  16. Rupture and regeneration of colloidal crystals as studied by two-dimensional ultra-small-angle X-ray scattering.

    PubMed

    Konishi, Toshiki; Ise, Norio

    2006-11-21

    The structure of colloidal crystals of silica particles in water was studied by using the two-dimensional (2D) ultra-small-angle X-ray scattering (USAXS) technique. By violent shaking of the dispersion, large (body-centered cubic, bcc) crystals were broken into microcrystals while the lattice structure and lattice constant were preserved. The 2D-USAXS profiles revealed that the [111] direction of bcc microcrystals was parallel to the capillary axis and their orientational distribution with respect to the capillary axis was random. While a prepeak was observed in the one-dimensional USAXS measurements, no such peak was detected by the 2D-USAXS technique. The prepeak was concluded to be due to {110} being rotated by 54.7 degrees (the angle between [001] and [111]) from the capillary axis. The diffraction from the plane was out of the horizontal plane and was observed at a lower angle as a prepeak by detector scanning in the horizontal direction.

  17. Porosity of microporous zeolites A, X and ZSM-5 studied by small angle X-ray scattering and nitrogen adsorption

    NASA Astrophysics Data System (ADS)

    Du, Xiaoming; Wu, Erdong

    2007-09-01

    Small-angle X-ray scattering (SAXS) using synchrotron radiation and nitrogen adsorption have been applied to characterizations of porosities and microporous structures for the zeolites of NaA, KA, CaA, NaX and ZSM-5. Besides the information on the external morphology of the particles of the zeolites, the complementation of the two techniques has revealed rich and consistent structural and surface information on the molecular scale crystalline pores of these zeolites. Analyses of the data suggest that the determined sizes of the micropores imply the pore spaces occupied by the probe molecules of water in the SAXS and nitrogen in adsorption techniques, respectively. The microporous information of NaA and KA are difficult to obtain from nitrogen adsorption, due to the blocking of nitrogen by their narrow channels, but have been satisfactorily measured by SAXS. The factors causing variations of the measured values of the parameters in different analysis methods have been discussed.

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

    NASA Astrophysics Data System (ADS)

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

    2015-10-01

    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.

  19. A practical guide to small angle X-ray scattering (SAXS) of flexible and intrinsically disordered proteins.

    PubMed

    Kikhney, Alexey G; Svergun, Dmitri I

    2015-09-14

    Small-angle X-ray scattering (SAXS) is a biophysical method to study the overall shape and structural transitions of biological macromolecules in solution. SAXS provides low resolution information on the shape, conformation and assembly state of proteins, nucleic acids and various macromolecular complexes. The technique also offers powerful means for the quantitative analysis of flexible systems, including intrinsically disordered proteins (IDPs). Here, the basic principles of SAXS are presented, and profits and pitfalls of the characterization of multidomain flexible proteins and IDPs using SAXS are discussed from the practical point of view. Examples of the synergistic use of SAXS with high resolution methods like X-ray crystallography and nuclear magnetic resonance (NMR), as well as other experimental and in silico techniques to characterize completely, or partially unstructured proteins, are presented.

  20. SASfit: a tool for small-angle scattering data analysis using a library of analytical expressions

    PubMed Central

    Breßler, Ingo; Kohlbrecher, Joachim; Thünemann, Andreas F.

    2015-01-01

    SASfit is one of the mature programs for small-angle scattering data analysis and has been available for many years. This article describes the basic data processing and analysis workflow along with recent developments in the SASfit program package (version 0.94.6). They include (i) advanced algorithms for reduction of oversampled data sets, (ii) improved confidence assessment in the optimized model parameters and (iii) a flexible plug-in system for custom user-provided models. A scattering function of a mass fractal model of branched polymers in solution is provided as an example for implementing a plug-in. The new SASfit release is available for major platforms such as Windows, Linux and MacOS. To facilitate usage, it includes comprehensive indexed documentation as well as a web-based wiki for peer collaboration and online videos demonstrating basic usage. The use of SASfit is illustrated by interpretation of the small-angle X-ray scattering curves of monomodal gold nanoparticles (NIST reference material 8011) and bimodal silica nanoparticles (EU reference material ERM-FD-102). PMID:26500467

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

    SciTech Connect

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

    2015-02-15

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

  2. Mirroring within the Fokker-Planck formulation of cosmic ray pitch angle scattering in homogeneous magnetic turbulence

    NASA Technical Reports Server (NTRS)

    Goldstein, M. L.; Klimas, A. J.; Sandri, G.

    1974-01-01

    The Fokker-Planck coefficient for pitch angle scattering, appropriate for cosmic rays in homogeneous, stationary, magnetic turbulence, is computed from first principles. No assumptions are made concerning any special statistical symmetries the random field may have. This result can be used to compute the parallel diffusion coefficient for high energy cosmic rays moving in strong turbulence, or low energy cosmic rays moving in weak turbulence. Becuase of the generality of the magnetic turbulence which is allowed in this calculation, special interplanetary magnetic field features such as discontinuities, or particular wave modes, can be included rigorously. The reduction of this results to previously available expressions for the pitch angle scattering coefficient in random field models with special symmetries is discussed. The general existance of a Dirac delta function in the pitch angle scattering coefficient is demonstrated. It is proved that this delta function is the Fokker-Planck prediction for pitch angle scattering due to mirroring in the magnetic field.

  3. Triple energy window scatter correction technique in PET.

    PubMed

    Shao, L; Freifelder, R; Karp, J S

    1994-01-01

    A practical triple energy window technique (TEW) is proposed, which is based on using the information in two lower energy windows and one single calibration, to estimate the scatter within the photopeak window. The technique is basically a conventional dual-window technique plus a modification factor, which can partially compensate object-distribution dependent scatters. The modification factor is a function of two lower scatter windows of both the calibration phantom and the actual object. In order to evaluate the technique, a Monte Carlo simulation program, which simulates the PENN-PET scanner geometry, was used. Different phantom activity distributions and phantom sizes were tested to simulate brain studies, including uniform and nonuniform distributions. The results indicate that the TEW technique works well for a wide range of activity distributions and object sizes. The comparisons between the TEW and dual window techniques show better quantitative accuracy for the TEW, especially for different phantom sizes. The technique is also applied to experimental data from a PENN-PET scanner to test its practicality.

  4. A three-dimensional ray-driven attenuation, scatter and geometric response correction technique for SPECT in inhomogeneous media.

    PubMed

    Laurette, I; Zeng, G L; Welch, A; Christian, P E; Gullberg, G T

    2000-11-01

    The qualitative and quantitative accuracy of SPECT images is degraded by physical factors of attenuation, Compton scatter and spatially varying collimator geometric response. This paper presents a 3D ray-tracing technique for modelling attenuation, scatter and geometric response for SPECT imaging in an inhomogeneous attenuating medium. The model is incorporated into a three-dimensional projector-backprojector and used with the maximum-likelihood expectation-maximization algorithm for reconstruction of parallel-beam data. A transmission map is used to define the inhomogeneous attenuating and scattering object being imaged. The attenuation map defines the probability of photon attenuation between the source and the scattering site, the scattering angle at the scattering site and the probability of attenuation of the scattered photon between the scattering site and the detector. The probability of a photon being scattered through a given angle and being detected in the emission energy window is approximated using a Gaussian function. The parameters of this Gaussian function are determined using physical measurements of parallel-beam scatter line spread functions from a non-uniformly attenuating phantom. The 3D ray-tracing scatter projector-backprojector produces the scatter and primary components. Then, a 3D ray-tracing projector-backprojector is used to model the geometric response of the collimator. From Monte Carlo and physical phantom experiments, it is shown that the best results are obtained by simultaneously correcting attenuation, scatter and geometric response, compared with results obtained with only one or two of the three corrections. It is also shown that a 3D scatter model is more accurate than a 2D model. A transmission map is useful for obtaining measurements of attenuation and scatter in SPECT data, which can be used together with a model of the geometric response of the collimator to obtain corrected images with quantitative and diagnostically

  5. Self crowding of globular proteins studied by small-angle x-ray scattering.

    PubMed

    Goldenberg, David P; Argyle, Brian

    2014-02-18

    Small-angle x-ray scattering (SAXS) was used to study the behavior of equine metmyoglobin (Mb) and bovine pancreatic trypsin inhibitor (BPTI) at concentrations up to 0.4 and 0.15 g/mL, respectively, in solutions also containing 50% D2O and 1 M urea. For both proteins, significant effects because of interference between x-rays scattered by different molecules (interparticle interference) were observed, indicating nonideal behavior at high concentrations. The experimental data were analyzed by comparison of the observed scattering profiles with those predicted by crystal structures of the proteins and a hard-sphere fluid model used to represent steric exclusion effects. The Mb scattering data were well fit by the hard-sphere model using a sphere radius of 18 Å, only slightly smaller than that estimated from the three-dimensional structure (20 Å). In contrast, the scattering profiles for BPTI in phosphate buffer displayed substantially less pronounced interparticle interference than predicted by the hard-sphere model and the radius estimated from the known structure of the protein (15 Å). Replacing the phosphate buffer with 3-(N-morpolino)propane sulfonic acid (MOPS) led to increased interparticle interference, consistent with a larger effective radius and suggesting that phosphate ions may mediate attractive intermolecular interactions, as observed in some BPTI crystal structures, without the formation of stable oligomers. The scattering data were also used to estimate second virial coefficients for the two proteins: 2.0 ×10(-4) cm(3)mol/g(2) for Mb in phosphate buffer, 1.6 ×10(-4) cm(3)mol/g(2) for BPTI in phosphate buffer and 9.2 ×10(-4) cm(3)mol/g(2) for BPTI in MOPS. The results indicate that the behavior of Mb, which is nearly isoelectric under the conditions used, is well described by the hard-sphere model, but that of BPTI is considerably more complex and is likely influenced by both repulsive and attractive electrostatic interactions. The hard

  6. Self Crowding of Globular Proteins Studied by Small-Angle X-Ray Scattering

    PubMed Central

    Goldenberg, David P.; Argyle, Brian

    2014-01-01

    Small-angle x-ray scattering (SAXS) was used to study the behavior of equine metmyoglobin (Mb) and bovine pancreatic trypsin inhibitor (BPTI) at concentrations up to 0.4 and 0.15 g/mL, respectively, in solutions also containing 50% D2O and 1 M urea. For both proteins, significant effects because of interference between x-rays scattered by different molecules (interparticle interference) were observed, indicating nonideal behavior at high concentrations. The experimental data were analyzed by comparison of the observed scattering profiles with those predicted by crystal structures of the proteins and a hard-sphere fluid model used to represent steric exclusion effects. The Mb scattering data were well fit by the hard-sphere model using a sphere radius of 18 Å, only slightly smaller than that estimated from the three-dimensional structure (20 Å). In contrast, the scattering profiles for BPTI in phosphate buffer displayed substantially less pronounced interparticle interference than predicted by the hard-sphere model and the radius estimated from the known structure of the protein (15 Å). Replacing the phosphate buffer with 3-(N-morpolino)propane sulfonic acid (MOPS) led to increased interparticle interference, consistent with a larger effective radius and suggesting that phosphate ions may mediate attractive intermolecular interactions, as observed in some BPTI crystal structures, without the formation of stable oligomers. The scattering data were also used to estimate second virial coefficients for the two proteins: 2.0 ×10-4 cm3mol/g2 for Mb in phosphate buffer, 1.6 ×10-4 cm3mol/g2 for BPTI in phosphate buffer and 9.2 ×10-4 cm3mol/g2 for BPTI in MOPS. The results indicate that the behavior of Mb, which is nearly isoelectric under the conditions used, is well described by the hard-sphere model, but that of BPTI is considerably more complex and is likely influenced by both repulsive and attractive electrostatic interactions. The hard-sphere model may be

  7. Small-angle neutron scattering study of organic-phase aggregation in the TALSPEAK process.

    PubMed

    Grimes, Travis S; Jensen, Mark P; Debeer-Schmidt, Lisa; Littrell, Ken; Nash, Kenneth L

    2012-11-26

    The Trivalent Actinide-Lanthanide Separation by Phosphorus reagent Extraction from Aqueous Komplexes (TALSPEAK) process is a solvent extraction based method for separating trivalent lanthanides (Ln(3+)) from trivalent actinide cations in used nuclear fuel reprocessing. In conventional TALSPEAK, the extractant solution is di(2-ethylhexyl)phosphoric acid (HDEHP) in 1,4-diisopropylbenzene (DIPB). The aqueous medium is diethylenetriamine-N,N,N',N″,N″-pentaacetic acid (DTPA) in a concentrated lactic acid (HL) buffer. Lanthanides are extracted by HDEHP/DIPB, while the actinides remain in the aqueous phase as DTPA complexes. Lactic acid is extracted both independently of the lanthanides and as Ln/HL/HDEHP mixed complex(es). Previous results indicate that lanthanides are extracted both as the mixed complex and as a binary Ln(DEHP·HDEHP)(3) species. Small-angle neutron scattering (SANS) has been applied to study the self-organization properties of solute molecules in xylene solutions containing HDEHP, HL, selected lanthanide ions, and water. The scattering results demonstrate that the dominant HDEHP species is the hydrogen bonded dimer, (HDEHP)(2). Absent lanthanides, lactic acid is extracted as the 1:3 complex (HL·(HDEHP)(3)). Scattering in samples containing up to 0.005 M lanthanides (prepared by extracting lanthanides from aqueous media containing 1.0 M buffered lactic acid) indicates that the dominant metal complex is Ln(DEHP·HDEHP)(3). At 0.013 M extracted lanthanide, the scattering results indicate lower Ln:DEHP stoichiometry and larger scattering particles. At higher metal concentrations, the SANS results indicate large aggregates, the largest aggregates achieving a size equivalent to 20 HDEHP monomers as the primary scattering entity. Analysis of particle shapes indicates best fits with a uniform oblate spheroid particle. These results are discussed in connection with the results of a number of complementary observations that have been made on this system.

  8. Effects of the scatter in sunspot group tilt angles on the large-scale magnetic field at the solar surface

    SciTech Connect

    Jiang, J.; Cameron, R. H.; Schüssler, M.

    2014-08-10

    The tilt angles of sunspot groups represent the poloidal field source in Babcock-Leighton-type models of the solar dynamo and are crucial for the build-up and reversals of the polar fields in surface flux transport (SFT) simulations. The evolution of the polar field is a consequence of Hale's polarity rules, together with the tilt angle distribution which has a systematic component (Joy's law) and a random component (tilt-angle scatter). We determine the scatter using the observed tilt angle data and study the effects of this scatter on the evolution of the solar surface field using SFT simulations with flux input based upon the recorded sunspot groups. The tilt angle scatter is described in our simulations by a random component according to the observed distributions for different ranges of sunspot group size (total umbral area). By performing simulations with a number of different realizations of the scatter we study the effect of the tilt angle scatter on the global magnetic field, especially on the evolution of the axial dipole moment. The average axial dipole moment at the end of cycle 17 (a medium-amplitude cycle) from our simulations was 2.73 G. The tilt angle scatter leads to an uncertainty of 0.78 G (standard deviation). We also considered cycle 14 (a weak cycle) and cycle 19 (a strong cycle) and show that the standard deviation of the axial dipole moment is similar for all three cycles. The uncertainty mainly results from the big sunspot groups which emerge near the equator. In the framework of Babcock-Leighton dynamo models, the tilt angle scatter therefore constitutes a significant random factor in the cycle-to-cycle amplitude variability, which strongly limits the predictability of solar activity.

  9. Internal structures of agar-gelatin co-hydrogels by light scattering, small-angle neutron scattering and rheology.

    PubMed

    Santinath Singh, S; Aswal, V K; Bohidar, H B

    2011-06-01

    Internal structures of agar-gelatin co-hydrogels were investigated as a function of their volumetric mixing ratio, [Formula: see text] , 1.0 and 2.0 using dynamic light scattering (DLS), small-angle neutron scattering (SANS) and rheology. The degree of non-ergodicity ( X = 0.2 ± 0.02) , which was extracted as a heterodyne contribution from the measured dynamic structure factor data remained less than that of homogeneous solutions where ergodicity is expected (X = 10. The static structure factor, I(q) , results obtained from SANS were interpreted in the Guinier regime (low-q , which implied the existence of ≈ 250 nm long rod-like structures (double-helix bundles), and the power law (intermediate-q regions) yielded I (q) ~ q(−α) with α = 2.3 , 1.8 and 1.6 for r = 0.5 , 1.0 and 2.0. This is indicative of the presence of Gaussian chains at low r , while at r = 2 there was a propensity of rod-shaped structures. The gel strength and transition temperatures measured from frequency sweep and temperature ramp studies were suggestive of the presence of a stronger association between the two biopolymer networks at higher r . The results indicate that the internal structures of agar-gelatin co-hydrogels were highly dependent on the volumetric mixing ratio.

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

    PubMed Central

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

    2017-01-01

    A new model is proposed for the measurement errors incurred in typical small-angle X-ray scattering (SAXS) experiments, which takes into account the setup geometry and physics of the measurement process. The model accurately captures the experimentally determined errors from a large range of synchrotron and in-house anode-based measurements. Its most general formulation gives for the variance of the buffer-subtracted SAXS intensity σ2(q) = [I(q) + const.]/(kq), where I(q) is the scattering intensity as a function of the momentum transfer q; k and const. are fitting parameters that are characteristic of the experimental setup. The model gives a concrete procedure for calculating realistic measurement errors for simulated SAXS profiles. In addition, the results provide guidelines for optimizing SAXS measurements, which are in line with established procedures for SAXS experiments, and enable a quantitative evaluation of measurement errors. PMID:28381982

  11. Spin echo small angle neutron scattering using a continuously pumped {sup 3}He neutron polarisation analyser

    SciTech Connect

    Parnell, S. R.; Li, K.; Yan, H.; Stonaha, P.; Li, F.; Wang, T.; Baxter, D. V.; Snow, W. M.; Washington, A. L.; Walsh, A.; Chen, W. C.; Parnell, A. J.; Fairclough, J. P. A.; Pynn, R.

    2015-02-15

    We present a new instrument for spin echo small angle neutron scattering (SESANS) developed at the Low Energy Neutron Source at Indiana University. A description of the various instrument components is given along with the performance of these components. At the heart of the instrument are a series of resistive coils to encode the neutron trajectory into the neutron polarisation. These are shown to work well over a broad range of neutron wavelengths. Neutron polarisation analysis is accomplished using a continuously operating neutron spin filter polarised by Rb spin-exchange optical pumping of {sup 3}He. We describe the performance of the analyser along with a study of the {sup 3}He polarisation stability and its implications for SESANS measurements. Scattering from silica Stöber particles is investigated and agrees with samples run on similar instruments.

  12. Small-angle neutron scattering and molecular dynamics structural study of gelling DNA nanostars

    NASA Astrophysics Data System (ADS)

    Fernandez-Castanon, J.; Bomboi, F.; Rovigatti, L.; Zanatta, M.; Paciaroni, A.; Comez, L.; Porcar, L.; Jafta, C. J.; Fadda, G. C.; Bellini, T.; Sciortino, F.

    2016-08-01

    DNA oligomers with properly designed sequences self-assemble into well defined constructs. Here, we exploit this methodology to produce bulk quantities of tetravalent DNA nanostars (each one composed of 196 nucleotides) and to explore the structural signatures of their aggregation process. We report small-angle neutron scattering experiments focused on the evaluation of both the form factor and the temperature evolution of the scattered intensity at a nanostar concentration where the system forms a tetravalent equilibrium gel. We also perform molecular dynamics simulations of one isolated tetramer to evaluate the form factor numerically, without resorting to any approximate shape. The numerical form factor is found to be in very good agreement with the experimental one. Simulations predict an essentially temperature-independent form factor, offering the possibility to extract the effective structure factor and its evolution during the equilibrium gelation.

  13. Solution structures of calcium regulating proteins: A small-angle scattering study

    SciTech Connect

    Trewhella, J.; Heidorn, D.B.; Seeger, P.A.

    1987-11-01

    Small-angle X-ray scattering (SAXS) experiments have shown that the solution structures of two calcium-binding regulatory proteins, calmodulin and troponin C, are significantly different from their crystal structure forms. The structural differences occur in a region of calmodulin that is thought to bind to target enzymes;the calmodulin-enzyme complex is an initiator for many important biochemical processes. Calcium binding to calmodulin induces a conformational change that is a prerequisite for calmodulin binding to a target enzyme. SAXS data can characterize this conformational change and give insight into the mechanism of enzyme binding. Neutron resonance scattering promises to determine accurately the distances between calcium binding sites, thus providing important constraints on the structure of calmodulin in solution. 24 refs., 5 figs., 1 tab.

  14. Sample holder for small-angle x-ray scattering static and flow cell measurements

    SciTech Connect

    Lipfert, Jan; Millett, Ian S.; Seifert, Soenke; Doniach, Sebastian

    2006-04-15

    We present the design of a sample holder for small-angle x-ray scattering (SAXS) that can be used for both static and flow cell measurements, allowing to switch between these two types of measurement without having to realign the detector and camera geometry. The device makes possible high signal-to-noise experiments with sample volumes as small as 16 {mu}l and can be thermocontrolled using a standard circulating water bath. The setup has been used successfully for a range of biological SAXS measurements, including peptides, detergent micelles, membrane proteins, and nucleic acids. As a performance test, we present scattering data for horse heart cytochrome c, collected at the BESSRC CAT beam line 12-ID of the Advanced Photon Source. The design drawings are provided in the supplementary material.

  15. SEC-SANS: size exclusion chromatography combined in situ with small-angle neutron scattering1

    PubMed Central

    Jordan, Ashley; Jacques, Mark; Merrick, Catherine; Devos, Juliette; Forsyth, V. Trevor; Porcar, Lionel; Martel, Anne

    2016-01-01

    The first implementation and use of an in situ size exclusion chromatography (SEC) system on a small-angle neutron scattering instrument (SANS) is described. The possibility of deploying such a system for biological solution scattering at the Institut Laue–Langevin (ILL) has arisen from the fact that current day SANS instruments at ILL now allow datasets to be acquired using small sample volumes with exposure times that are often shorter than a minute. This capability is of particular importance for the study of unstable biological macromolecules where aggregation or denaturation issues are a major problem. The first use of SEC-SANS on ILL’s instrument D22 is described for a variety of proteins including one particularly aggregation-prone system. PMID:27980509

  16. Microstructural investigations on Russian reactor pressure vessel steels by small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Ulbricht, A.; Boehmert, J.; Strunz, P.; Dewhurst, C.; Mathon, M.-H.

    The effect of radiation embrittlement has a high safety significance for Russian VVER reactor pressure vessel steels. Heats of base and weld metals of the as-received state, irradiated state and post-irradiation annealed state were investigated using small-angle neutron scattering (SANS) to obtain insight about the microstructural features caused by fast neutron irradiation. The SANS intensities increase in the momentum transfer range between 0.8 and 3 nm-1 for all the material compositions in the irradiated state. The size distribution function of the irradiation-induced defect clusters has a pronounced maximum at 1 nm in radius. Their content varies between 0.1 and 0.7 vol.% dependent on material composition and increases with the neutron fluence. The comparison of nuclear and magnetic scattering indicates that the defects differ in their composition. Thermal annealing reduces the volume fraction of irradiation defect clusters.

  17. Deterministic fractals: extracting additional information from small-angle scattering data.

    PubMed

    Cherny, A Yu; Anitas, E M; Osipov, V A; Kuklin, A I

    2011-09-01

    The small-angle scattering curves of deterministic mass fractals are studied and analyzed in momentum space. In the fractal region, the curve I(q)q(D) is found to be log-periodic with good accuracy, and the period is equal to the scaling factor of the fractal. Here, D and I(q) are the fractal dimension and the scattering intensity, respectively. The number of periods of this curve coincides with the number of fractal iterations. We show that the log-periodicity of I(q)q(D) in the momentum space is related to the log-periodicity of the quantity g(r)r(3-D) in the real space, where g(r) is the pair distribution function. The minima and maxima positions of the scattering intensity are estimated explicitly by relating them to the pair distance distribution in real space. It is shown that the minima and maxima are damped with increasing polydispersity of the fractal sets; however, they remain quite pronounced even at sufficiently large values of polydispersity. A generalized self-similar Vicsek fractal with controllable fractal dimension is introduced, and its scattering properties are studied to illustrate the above findings. In contrast with the usual methods, the present analysis allows us to obtain not only the fractal dimension and the edges of the fractal region, but also the fractal iteration number, the scaling factor, and the number of structural units from which the fractal is composed.

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

    SciTech Connect

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

    2003-01-01

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

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

    PubMed Central

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

    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. 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. PMID:28381971

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

    SciTech Connect

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

    1988-03-25

    X-ray crystallographic studies of troponin C have revealed a novel protein structure consisting of two globular domains, each containing two Ca/sup 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/sup 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/sup 2 +/-facilitated dimerization of troponin C was observed. The data rule out large Ca/sup 2 +/-induced structural changes, indicating rather that the molecule with Ca/sup 2 +/ bound is only slightly more compact than the Ca/sup 2 +/-free molecule.

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

    PubMed

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

    2013-03-01

    In this work, the morphological and structural behaviors of poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) nanocomposites were investigated using small angle X-ray scattering (SAXS), wide angle X-ray diffraction (WAXD) and transmission electron microscopy (TEM). The nanocomposites with 1, 3 and 5 wt.% of organically modified montmorillonite Cloisite® 30B (OMMT) were prepared by melt processing in a twin screw extruder using two different processing conditions (low and high shear intensity). The lamellar long period of the polymer was lower for the nanocomposites, with high polydispersity values. However, the crystalline thickness increased with the clay content and was independent of the processing conditions. This behavior resulted in a high linear crystallinity of the nanocomposites with 3 and 5 wt.% OMMT. The disruption factor (β) was in agreement with the WAXD and TEM findings, indicating a good dispersion of the nanoparticles in the PHBV matrix with 3 wt.% of OMMT during the high shear intensity of melt processing.

  2. Structural characterization of a polymer substituted fullerene (flagellene) by small angle neutron scattering

    SciTech Connect

    Affholter, K.A.; Bunick, G.J.; Wignall, G.D.; Desimone, J.M.; Hunt, M.O. Jr.; Menceloglu, Y.Z.; Samulski, E.T.

    1994-12-31

    Small-angle neutron scattering (SANS) can structurally characterize fullerenes in solvents with strong SANS contrast (e.g. CS{sub 2}). Deuterated solvents (e.g. toluene-d{sub 8}) have a high scattering length density (SLD), which is close to that of C{sub 60} and C{sub 70} moieties. Hence, there is virtually no SANS contrast with the solvent and these particles are practically ``invisible`` in such media. On the other hand, the negative scattering length of hydrogen means that the SLD of H{sup 1}-containing materials is much lower, so they have strong contrast with toluene-d{sub 8}. Thus, SANS makes it possible to study the size and shapes of modified buckyballs such as the polymer-substituted fullerenes, or flagellenes. These consist of C{sub 60} cores to which 1-4 polystryene chains (with a molecular weight, MW {approx_equal} 2000) are attached. The extrapolated cross section at zero angle of scatter [d{Sigma}/d{Omega}(0)] is a function of the number of pendant chains, so SANS can be used to assess the number of ``arms`` which are covalently attached to the fullerene ``sphere.`` Close agreement ({plus_minus}4%) between measured and calculated values of d{Sigma}/d{Omega}(0) along with independent estimates of the radius of gyration (R{sub g}) and second virial coefficient (A{sub 2}) for a calibration linear polystyrene sample serves as a cross check on the validity of this methodology.

  3. [Evaluation of molecular weights of hyaluronate preparations by multi-angle laser light scattering].

    PubMed

    Yomota, Chikako

    2003-01-01

    Hyaluronate (HA), a glycosaminoglycan polysaccharide, has been used for osteoarthritis, periartritis of the shoulder and rheumatoid arthritis by intraarticular administration, and in ophthalmic surgery such as anterior segment surgery, and eye lotion. In this study, the molecular weight (Mw) of HA preparations were estimated by size-exclusion chromatography (SEC) system consisted of a refractometer (RI) and a multi-angle laser light scattering (MALS). From the results, it has been clarified that a successful characterization of HA samples with Mw up to 2 - 3 x 10(6) g/mol was possible by multidetector system.

  4. Cylindrical aggregates of chlorophylls studied by small-angle neutron scatter

    SciTech Connect

    Worcester, D.L.; Katz, J.J.

    1994-12-31

    Neutron small-angle scattering has demonstrated tubular chlorophyll aggregates formed by self-assembly of a variety of chlorophyll types in nonpolar solvents. The size and other properties of the tubular aggregates can be accounted for by stereochemical properties of the chlorophyll molecules. Features of some of the structures are remarkably similar to light harvesting chlorophyll complexes in vivo, particularly for photosynthetic bacteria. These nanotube chlorophyll structures may have applications as light harvesting biomaterials where efficient energy transfer occurs from an excited state which is highly delocalized.

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

  6. Study of structural irregularities of smectite clay systems by small-angle neutron scattering and adsorption

    NASA Astrophysics Data System (ADS)

    De Stefanis, A.; Tomlinson, A. A. G.; Steriotis, Th. A.; Charalambopoulou, G. Ch.; Keiderling, U.

    2007-04-01

    Small angle neutron scattering (SANS) and its contrast-matching variant are employed in order to determine structural properties (inter-pillar distances and mass/surface fractal dimensions of the clay layers and pillars) of a series of smectite natural clays (montmorillonite, beidellite, and bentonite) and their pillared and pillared/ion-exchanged analogues. Moreover, a comparative analysis with the adsorption data is carried out on the basis of a systematic study of the structural changes induced by a particular treatment or modification (e.g. pillaring) of the clay systems.

  7. Imaging method based on attenuation, refraction and ultra-small-angle-scattering of x-rays

    DOEpatents

    Wernick, Miles N.; Chapman, Leroy Dean; Oltulu, Oral; Zhong, Zhong

    2005-09-20

    A method for detecting an image of an object by measuring the intensity at a plurality of positions of a transmitted beam of x-ray radiation emitted from the object as a function of angle within the transmitted beam. The intensity measurements of the transmitted beam are obtained by a crystal analyzer positioned at a plurality of angular positions. The plurality of intensity measurements are used to determine the angular intensity spectrum of the transmitted beam. One or more parameters, such as an attenuation property, a refraction property and a scatter property, can be obtained from the angular intensity spectrum and used to display an image of the object.

  8. Small angle scattering polarization biopsy: a comparative analysis of various skin diseases

    NASA Astrophysics Data System (ADS)

    Zimnyakov, D. A.; Alonova, M. V.; Yermolenko, S. B.; Ivashko, P. V.; Reshetnikova, E. M.; Galkina, E. M.; Utz, S. R.

    2013-12-01

    An approach to differentiation of the morphological features of normal and pathological human epidermis on the base of statistical analysis of the local polarization states of laser light forward scattered by in-vitro tissue samples is discussed. The eccentricity and the azimuth angle of local polarization ellipses retrieved for various positions of the focused laser beam on the tissue surface, and the coefficient of collimated transmittance are considered as the diagnostic parameters for differentiation. The experimental data obtained with the psoriasis, discoid lupus erythematosus, alopecia, lichen planus, scabies, demodex, and normal skin samples are presented.

  9. Small-angle X-ray scattering probe of intermolecular interaction in red blood cells

    NASA Astrophysics Data System (ADS)

    Liu, Guan-Fen; Wang, We-Jia; Xu, Jia-Hua; Dong, Yu-Hui

    2015-03-01

    With high concentrations of hemoglobin (Hb) in red blood cells, self-interactions among these molecules could increase the propensities of their polymerization and aggregation. In the present work, high concentration Hb in solution and red blood cells were analyzed by small-angle X-ray scattering. Calculation of the effective structure factor indicates that the interaction of Hb molecules is the same when they are crowded together in both the cell and physiological saline. The Hb molecules stay individual without the formation of aggregates and clusters in cells. Supported by National Basic Research Program of China (2009CB918600) and National Natural Science Foundation of China (10979005)

  10. Clustering of water molecules in ultramicroporous carbon: In-situ small-angle neutron scattering

    SciTech Connect

    Bahadur, Jitendra; Contescu, Cristian I.; Rai, Durgesh K.; Gallego, Nidia C.; Melnichenko, Yuri B.

    2016-10-19

    The adsorption of water is central to most of the applications of microporous carbon as adsorbent material. We report early kinetics of water adsorption in the microporous carbon using in-situ small-angle neutron scattering. It is observed that adsorption of water occurs via cluster formation of molecules. Interestingly, the cluster size remains constant throughout the adsorption process whereas number density of clusters increases with time. The role of surface chemistry of microporous carbon on the early kinetics of adsorption process was also investigated. Lastly, the present study provides direct experimental evidence for cluster assisted adsorption of water molecules in microporous carbon (Do-Do model).

  11. Modeling and measurement of angle-beam wave propagation in a scatterer-free plate

    NASA Astrophysics Data System (ADS)

    Dawson, Alexander J.; Michaels, Jennifer E.; Michaels, Thomas E.

    2017-02-01

    Wavefield imaging has been shown to be a powerful tool for improving the understanding and characterization of wave propagation and scattering in plates. The complete measurement of surface displacement over a 2-D grid provided by wavefield imaging has the potential to serve as a useful means of validating ultrasonic models. Here, a preliminary study of ultrasonic angle-beam wave propagation in a scatterer-free plate using a combination of wavefield measurements and 2-D finite element models is described. Both wavefield imaging and finite element analysis are used to study the propagation of waves at a refracted angle of 56.8° propagating in a 6.35 mm thick aluminum plate. Wavefield imaging is performed using a laser vibrometer mounted on an XYZ scanning stage, which is programmed to move point-to-point on a rectilinear grid to acquire waveform data. The commercial finite element software package, PZFlex, which is specifically designed to handle large, complex ultrasonic problems, is used to create a 2-D cross-sectional model of the transducer and plate. For model validation, vertical surface displacements from both the wavefield measurements and the PZFlex finite element model are compared and found to be in excellent agreement. The validated PZFlex model is then used to explain the mechanism of Rayleigh wave generation by the angle-beam wedge. Since the wavefield measurements are restricted to the specimen surface, the cross-sectional PZFlex model is able to provide insights the wavefield data cannot. This study illustrates how information obtained from ultrasonic experiments and modeling results can be combined to improve understanding of angle-beam wave generation and propagation.

  12. Porosity and structural parameters of Karelian shungites according to the data of small-angle synchrotron radiation scattering and microscopy

    SciTech Connect

    Golubev, Ye. A. Ulyashev, V. V.; Veligzhanin, A. A.

    2016-01-15

    The nanoporosity and structure of natural carbons has been investigated on the example of Karelian carbon-rich shungites by comparing the data of small-angle synchrotron radiation scattering and highresolution microscopy. The analysis of small-angle scattering data is based on the model of scattering spheres with lognormal size distribution. It is found that the structure of samples from the Maksovo and Zazhogino deposits subjected to high temperatures in the geological medium and (also to a lesser extent) a sample from the Shunga deposit can be described as an aggregation of polydisperse scattering spheres with lognormal size distribution; the characteristic scatterer size is determined for them. A comparison with microscopy data shows that these scatterers are mainly associated with pores, and the character of their size distribution is similar to that previously established for nanoglobules in schungites.

  13. Critical dimension small angle X-ray scattering measurements of FinFET and 3D memory structures

    NASA Astrophysics Data System (ADS)

    Settens, Charles; Bunday, Benjamin; Thiel, Brad; Kline, R. Joseph; Sunday, Daniel; Wang, Chengqing; Wu, Wen-li; Matyi, Richard

    2013-04-01

    We have demonstrated that transmission critical dimension small angle X-ray scattering (CD-SAXS) provides high accuracy and precision CD measurements on advanced 3D microelectronic architectures. The competitive advantage of CD-SAXS over current 3D metrology methods such as optical scatterometry is that CD-SAXS is able to decouple and fit cross-section parameters without any significant parameter cross-correlations. As the industry aggressively scales beyond the 22 nm node, CD-SAXS can be used to quantitatively measure nanoscale deviations in the average crosssections of FinFETs and high-aspect ratio (HAR) memory devices. Fitting the average cross-section of 18:1 isolated HAR contact holes with an effective trapezoid model yielded an average pitch of 796.9 +/- 0.4 nm, top diameter of 70.3 +/- 0.9 nm, height of 1088 +/- 4 nm, and sidewall angle below 0.1°. Simulations of dense 40:1 HAR contact holes and FinFET fin-gate crossbar structures have been analyzed using CD-SAXS to inquire the theoretical precision of the technique to measure important process parameters such as fin CD, height, and sidewall angle; BOX etch recess, thickness of hafnium oxide and titanium nitride layers; gate CD, height, and sidewall angle; and hafnium oxide and titanium nitride etch recess. The simulations of HAR and FinFET structures mimic the characteristics of experimental data collected at a synchrotron x-ray source. Using the CD-SAXS simulator, we estimate the measurement capabilities for smaller similar structures expected at future nodes to predict the applicability of this technique to fulfill important CD metrology needs.

  14. Magnetic-field-dependent small-angle neutron scattering on random anisotropy ferromagnets

    NASA Astrophysics Data System (ADS)

    Michels, Andreas; Weissmüller, Jörg

    2008-06-01

    We report on the recently developed technique of magnetic-field-dependent small-angle neutron scattering (SANS), with attention to bulk ferromagnets exhibiting random magnetic anisotropy. In these materials, the various magnetic anisotropy fields (magnetocrystalline, magnetoelastic, and/or magnetostatic in origin) perturb the perfectly parallel spin alignment of the idealized ferromagnetic state. By varying the applied magnetic field, one can control one of the ordering terms which competes with the above-mentioned perturbing fields. Experiments which explore the ensuing reaction of the magnetization will therefore provide information not only on the field-dependent spin structure but, importantly, on the underlying magnetic interaction terms. This strategy, which underlies conventional studies of hysteresis loops in magnetometry, is here combined with magnetic SANS. While magnetometry generally records only a single scalar quantity, the integral magnetization, SANS provides access to a vastly richer data set, the Fourier spectrum of the response of the spin system as a function of the magnitude and orientation of the wave vector. The required data-analysis procedures have recently been established, and experiments on a number of magnetic materials, mostly nanocrystalline or nanocomposite metals, have been reported. Here, we summarize the theory of magnetic-field-dependent SANS along with the underlying description of random anisotropy magnets by micromagnetic theory. We review experiments which have explored the magnetic interaction parameters, the value of the exchange-stiffness constant as well as the Fourier components of the magnetic anisotropy field and of the magnetostatic stray field. A model-independent approach, based on the experimental autocorrelation function of the spin misalignment, provides access to the characteristic length of the spin misalignment. The field dependence of this quantity is in quantitative agreement with the predictions of

  15. A small-angle x-ray scattering system with a vertical layout

    NASA Astrophysics Data System (ADS)

    Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

    2014-12-01

    A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

  16. A small-angle x-ray scattering system with a vertical layout

    SciTech Connect

    Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

    2014-12-15

    A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

  17. Small-angle x-ray scattering study on the structure of microcrystalline and nanofibrillated cellulose

    NASA Astrophysics Data System (ADS)

    Leppänen, Kirsi; Pirkkalainen, Kari; Penttilä, Paavo; Sievänen, Jenni; Kotelnikova, Nina; Serimaa, Ritva

    2010-10-01

    The effects of different solvents on the structure of microcrystalline and nanofibrillated cellulose (MCC, NFC) were studied using small-angle x-ray scattering (SAXS). MCC was immersed in water, ethanol, and acetone, and NFC was immersed only in water and ethanol, but studied also in the form of foam-like water-NFC-gel in wet, air-dried and re-wet states. The solvent affected the average chord length, which reveals the typical length scale of the structure of the sample: 2.4 ± 0.1 nm was obtained for MCC-water, 2.5 ± 0.1 nm for re-wet NFC-gel, 1.6 ± 0.1 nm for MCC-ethanol, 1.2 ± 0.1 nm for NFC-ethanol, and 1.3 ± 0.1 nm for MCC-acetone. The specific surface of cellulose increased strongly when MCC and NFC were immersed in the solvents compared to dry cellulose. The specific surface of cellulose was determined to be larger for NFC-water than MCC-water, and slightly larger for dry NFC powder than for dry MCC, which can be explained by the fact that the width of cellulose crystallites perpendicular to the cellulose chain direction was slightly larger in MCC than in NFC on the basis of wide-angle x-ray scattering results.

  18. A small-angle x-ray scattering system with a vertical layout.

    PubMed

    Wang, Zhen; Chen, Xiaowei; Meng, Lingpu; Cui, Kunpeng; Wu, Lihui; Li, Liangbin

    2014-12-01

    A small-angle x-ray scattering (SAXS) system with a vertical layout (V-SAXS) has been designed and constructed for in situ detection on nanostructures, which is well suitable for in situ study on self-assembly of nanoparticles at liquid interface and polymer processing. A steel-tower frame on a reinforced basement is built as the supporting skeleton for scattering beam path and detector platform, ensuring the system a high working stability and a high operating accuracy. A micro-focus x-ray source combining parabolic three-dimensional multi-layer mirror and scatteringless collimation system provides a highly parallel beam, which allows us to detect the very small angle range. With a sample-to-detector distance of 7 m, the largest measurable length scale is 420 nm in real space. With a large sample zone, it is possible to install different experimental setups such as film stretching machine, which makes the system perfect to follow the microstructures evolution of materials during processing. The capability of the V-SAXS on in situ study is tested with a drying experiment of a free latex droplet, which confirms our initial design.

  19. Magnetic design evolution in perpendicular magnetic recording media as revealed by resonant small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Wang, Tianhan; Mehta, Virat; Ikeda, Yoshihiro; Do, Hoa; Takano, Kentaro; Florez, Sylvia; Terris, Bruce D.; Wu, Benny; Graves, Catherine; Shu, Michael; Rick, Ramon; Scherz, Andreas; Stöhr, Joachim; Hellwig, Olav

    2013-09-01

    We analyze the magnetic design for different generations of perpendicular magnetic recording (PMR) media using resonant soft x-ray small angle x-ray scattering. This technique allows us to simultaneously extract in a single experiment the key structural and magnetic parameters, i.e., lateral structural grain and magnetic cluster sizes as well as their distributions. We find that earlier PMR media generations relied on an initial reduction in the magnetic cluster size down to the grain level of the high anisotropy granular base layer, while very recent media designs introduce more exchange decoupling also within the softer laterally continuous cap layer. We highlight that this recent development allows optimizing magnetic cluster size and magnetic cluster size distribution within the composite media system for maximum achievable area density, while keeping the structural grain size roughly constant.

  20. Morphology of crystalline-amorphous olefin block copolymers in solution characterized by small-angle neutron scattering and microscopy.

    PubMed

    Radulescu, Aurel; Goerigk, Günter; Fetters, Lewis; Richter, Dieter

    2015-12-01

    The single-chain properties and self-assembly behavior in dilute solution of olefin block copolymers obtained by chain-shuttling technology and consisting of alternating crystallizable and amorphous ethylene/1-octene blocks were investigated by pinhole and focusing small-angle neutron scattering techniques, optical microscopy in bright-field and crossed-polarizer modes, and differential scanning calorimetry. The complex hydrocarbon soluble (precipitant free) macro-aggregates formed with decreasing temperature are characterized by spherulitic textures. The spherulites yield, on one hand, a morphology that depends on the chain structure properties and, on the other hand, multiple structural levels with a hierarchical organization that ranges from 10 Å up to tens of micrometres. This morphology displays peculiarities dictated by the polydisperse character of these materials.

  1. Morphology of crystalline–amorphous olefin block copolymers in solution characterized by small-angle neutron scattering and microscopy

    PubMed Central

    Radulescu, Aurel; Goerigk, Günter; Fetters, Lewis; Richter, Dieter

    2015-01-01

    The single-chain properties and self-assembly behavior in dilute solution of olefin block copolymers obtained by chain-shuttling technology and consisting of alternating crystallizable and amorphous ethylene/1-octene blocks were investigated by pinhole and focusing small-angle neutron scattering techniques, optical microscopy in bright-field and crossed-polarizer modes, and differential scanning calorimetry. The complex hydrocarbon soluble (precipitant free) macro-aggregates formed with decreasing temperature are characterized by spherulitic textures. The spherulites yield, on one hand, a morphology that depends on the chain structure properties and, on the other hand, multiple structural levels with a hierarchical organization that ranges from 10 Å up to tens of micrometres. This morphology displays peculiarities dictated by the polydisperse character of these materials. PMID:26664344

  2. Preliminary experiments on apparatus for in situ studies of microwave-driven reactions by small angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Whittaker, A. G.; Harrison, A.; Oakley, G. S.; Youngson, I. D.; Heenan, R. K.; King, S. M.

    2001-01-01

    In this article we describe apparatus for the study of the microwave-driven growth of particles in solution by in situ small angle neutron scattering (SANS). This apparatus has enabled the first preliminary experiments using microwave-activated in situ diffraction. We take iron oxide as the prototype system, but the technique may be extended to a wide variety of chemical reactions that deposit solids from solution. The key features of the apparatus are a microwave cavity with a modular construction that may be adapted to the geometric constraints of the diffractometer, and a computer-controlled microwave generator that may be set to maintain either constant pressure or temperature in the reaction vessel. In this particular piece of equipment the reaction vessel is adapted so that part of the sample fills a cell of identical construction to those commonly used in SANS measurements for optimal transmission of the neutron beam.

  3. Characterization of oligomerization of a peptide from the ebola virus glycoprotein by small-angle neutron scattering

    SciTech Connect

    Egorov, V. V.; Gorshkov, A. N.; Murugova, T. N.; Vasin, A. V.; Lebedev, D. V.; Isaev-Ivanov, V. V.; Kiselev, O. I.

    2016-01-15

    Transmission electron microscopy (TEM) and small-angle neutron scattering (SANS) studies showed that model peptides QNALVCGLRQ (G33) and QNALVCGLRG (G31) corresponding to region 551–560 of the GP protein of the Sudan Ebola virus are prone to oligomerization in solution. Both peptides can form amyloid-like fibrills. The G33 peptide forms fibrils within one day of incubation, whereas the fibrillogenesis of the G31 peptide is observed only after incubation for several months. The possible role of the observed processes in the pathogenesis and the possibility of applying a combination of the TEM and SANS techniques to search for new compounds that are able to influence the protein oligomerization are discussed.

  4. From Non-equilibrium to Equilibrium: Micellar Kinetics seen by Time-resolved Small-angle Scattering

    NASA Astrophysics Data System (ADS)

    Lund, Reidar

    The kinetic pathways of self-assembled nanostructures are not fully understood. Time-resolved small-angle X-ray/neutron scattering (TR-SAXS/SANS) is powerful technique1 that allows kinetics processes such as nucleation processes2,3 and morphological transitions4,5 to be followed with structural resolution over time scales starting from milliseconds. Neutrons offer the additional advantage of facile contrast variation through H/D substitution schemes, which also allow equilibrium processes such as molecular exchange and diffusion to be studied1 , 6 , 7. Here we will highlight the current capabilities of TR-SAS and show results on the kinetics of polymeric micelles. We will address how the understanding of kinetic pathways can be used control the nanostructure.

  5. Characterization of oligomerization of a peptide from the ebola virus glycoprotein by small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Egorov, V. V.; Gorshkov, A. N.; Murugova, T. N.; Vasin, A. V.; Lebedev, D. V.; Isaev-Ivanov, V. V.; Kiselev, O. I.

    2016-01-01

    Transmission electron microscopy (TEM) and small-angle neutron scattering (SANS) studies showed that model peptides QNALVCGLRQ (G33) and QNALVCGLRG (G31) corresponding to region 551-560 of the GP protein of the Sudan Ebola virus are prone to oligomerization in solution. Both peptides can form amyloid-like fibrills. The G33 peptide forms fibrils within one day of incubation, whereas the fibrillogenesis of the G31 peptide is observed only after incubation for several months. The possible role of the observed processes in the pathogenesis and the possibility of applying a combination of the TEM and SANS techniques to search for new compounds that are able to influence the protein oligomerization are discussed.

  6. Characterization of Protein Flexibility Using Small-Angle X-Ray Scattering and Amplified Collective Motion Simulations

    PubMed Central

    Wen, Bin; Peng, Junhui; Zuo, Xiaobing; Gong, Qingguo; Zhang, Zhiyong

    2014-01-01

    Large-scale flexibility within a multidomain protein often plays an important role in its biological function. Despite its inherent low resolution, small-angle x-ray scattering (SAXS) is well suited to investigate protein flexibility and determine, with the help of computational modeling, what kinds of protein conformations would coexist in solution. In this article, we develop a tool that combines SAXS data with a previously developed sampling technique called amplified collective motions (ACM) to elucidate structures of highly dynamic multidomain proteins in solution. We demonstrate the use of this tool in two proteins, bacteriophage T4 lysozyme and tandem WW domains of the formin-binding protein 21. The ACM simulations can sample the conformational space of proteins much more extensively than standard molecular dynamics (MD) simulations. Therefore, conformations generated by ACM are significantly better at reproducing the SAXS data than are those from MD simulations. PMID:25140431

  7. Anomalous Small Angle X-Ray Scattering Simulations: Proof of Concept for Distance Measurements for Nanoparticle-Labelled Biomacromolecules in Solution

    PubMed Central

    Pinfield, Valerie J.; Scott, David J.

    2014-01-01

    Anomalous small angle X-ray scattering can in principle be used to determine distances between metal label species on biological molecules. Previous experimental studies in the past were unable to distinguish the label-label scattering contribution from that of the molecule, because of the use of atomic labels; these labels contribute only a small proportion of the total scattering signal. However, with the development of nanocrystal labels (of 50–100 atoms) there is the possibility for a renewed attempt at applying anomalous small angle X-ray scattering for distance measurement. This is because the contribution to the scattered signal is necessarily considerably stronger than for atomic labels. Here we demonstrate through simulations, the feasibility of the technique to determine the end-to-end distances of labelled nucleic acid molecules as well as other internal distances mimicking a labelled DNA binding protein if the labels are dissimilar metal nanocrystals. Of crucial importance is the ratio of mass of the nanocrystals to that of the labelled macromolecule, as well as the level of statistical errors in the scattering intensity measurements. The mathematics behind the distance determination process is presented, along with a fitting routine than incorporates maximum entropy regularisation. PMID:24759797

  8. The measurement capabilities of cross-sectional profile of Nanoimprint template pattern using small angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Yamanaka, Eiji; Taniguchi, Rikiya; Itoh, Masamitsu; Omote, Kazuhiko; Ito, Yoshiyasu; Ogata, Kiyoshi; Hayashi, Naoya

    2016-05-01

    Nanoimprint lithography (NIL) is one of the most potential candidates for the next generation lithography for semiconductor. It will achieve the lithography with high resolution and low cost. High resolution of NIL will be determined by a high definition template. Nanoimprint lithography will faithfully transfer the pattern of NIL template to the wafer. Cross-sectional profile of the template pattern will greatly affect the resist profile on the wafer. Therefore, the management of the cross-sectional profile is essential. Grazing incidence small angle x-ray scattering (GI-SAXS) technique has been proposed as one of the method for measuring cross-sectional profile of periodic nanostructure pattern. Incident x-rays are irradiated to the sample surface with very low glancing angle. It is close to the critical angle of the total reflection of the x-ray. The scattered x-rays from the surface structure are detected on a two-dimensional detector. The observed intensity is discrete in the horizontal (2θ) direction. It is due to the periodicity of the structure, and diffraction is observed only when the diffraction condition is satisfied. In the vertical (β) direction, the diffraction intensity pattern shows interference fringes reflected to height and shape of the structure. Features of the measurement using x-ray are that the optical constant for the materials are well known, and it is possible to calculate a specific diffraction intensity pattern based on a certain model of the cross-sectional profile. The surface structure is estimated by to collate the calculated diffraction intensity pattern that sequentially while changing the model parameters with the measured diffraction intensity pattern. Furthermore, GI-SAXS technique can be measured an object in a non-destructive. It suggests the potential to be an effective tool for product quality assurance. We have developed a cross-sectional profile measurement of quartz template pattern using GI-SAXS technique. In this

  9. Nuclear effects on ion heating within the small-angle charged-particle elastic-scattering regime

    NASA Astrophysics Data System (ADS)

    Andrade, A.; Hale, G. M.

    1984-10-01

    The effects of nuclear forces (in contrast to pure Coulomb interaction) on the ion heating rate which results from small-angle scattering processes between charged particles in plasmas are investigated within the framework of Fokker-Planck theory. These effects are included through the addition of analytic Coulomb-nuclear interference and nuclear elastic cross sections in the scattering integrals of the dynamical friction coefficient and dispersion tensor. It is found that corrections to traditional Fokker-Planck predictions of the ion-ion energy exchange rate can be calculated and that these corrections are sensitive to the choice of the maximum scattering angle defining the cutoff between small- and large-angle scattering.

  10. Fast computation of high energy elastic collision scattering angle for electric propulsion plume simulation

    NASA Astrophysics Data System (ADS)

    Araki, Samuel J.

    2016-11-01

    In the plumes of Hall thrusters and ion thrusters, high energy ions experience elastic collisions with slow neutral atoms. These collisions involve a process of momentum exchange, altering the initial velocity vectors of the collision pair. In addition to the momentum exchange process, ions and atoms can exchange electrons, resulting in slow charge-exchange ions and fast atoms. In these simulations, it is particularly important to accurately perform computations of ion-atom elastic collisions in determining the plume current profile and assessing the integration of spacecraft components. The existing models are currently capable of accurate calculation but are not fast enough such that the calculation can be a bottleneck of plume simulations. This study investigates methods to accelerate an ion-atom elastic collision calculation that includes both momentum- and charge-exchange processes. The scattering angles are pre-computed through a classical approach with ab initio spin-orbit free potential and are stored in a two-dimensional array as functions of impact parameter and energy. When performing a collision calculation for an ion-atom pair, the scattering angle is computed by a table lookup and multiple linear interpolations, given the relative energy and randomly determined impact parameter. In order to further accelerate the calculations, the number of collision calculations is reduced by properly defining two cut-off cross-sections for the elastic scattering. In the MCC method, the target atom needs to be sampled; however, it is confirmed that initial target atom velocity does not play a significant role in typical electric propulsion plume simulations such that the sampling process is unnecessary. With these implementations, the computational run-time to perform a collision calculation is reduced significantly compared to previous methods, while retaining the accuracy of the high fidelity models.

  11. Small-angle neutron scattering reveals the assembly mode and oligomeric architecture of TET, a large, dodecameric aminopeptidase

    SciTech Connect

    Appolaire, Alexandre; Girard, Eric; Colombo, Matteo; Durá, M. Asunción; Moulin, Martine; Härtlein, Michael; Franzetti, Bruno; Gabel, Frank

    2014-11-01

    The present work illustrates that small-angle neutron scattering, deuteration and contrast variation, combined with in vitro particle reconstruction, constitutes a very efficient approach to determine subunit architectures in large, symmetric protein complexes. In the case of the 468 kDa heterododecameric TET peptidase machine, it was demonstrated that the assembly of the 12 subunits is a highly controlled process and represents a way to optimize the catalytic efficiency of the enzyme. The specific self-association of proteins into oligomeric complexes is a common phenomenon in biological systems to optimize and regulate their function. However, de novo structure determination of these important complexes is often very challenging for atomic-resolution techniques. Furthermore, in the case of homo-oligomeric complexes, or complexes with very similar building blocks, the respective positions of subunits and their assembly pathways are difficult to determine using many structural biology techniques. Here, an elegant and powerful approach based on small-angle neutron scattering is applied, in combination with deuterium labelling and contrast variation, to elucidate the oligomeric organization of the quaternary structure and the assembly pathways of 468 kDa, hetero-oligomeric and symmetric Pyrococcus horikoshii TET2–TET3 aminopeptidase complexes. The results reveal that the topology of the PhTET2 and PhTET3 dimeric building blocks within the complexes is not casual but rather suggests that their quaternary arrangement optimizes the catalytic efficiency towards peptide substrates. This approach bears important potential for the determination of quaternary structures and assembly pathways of large oligomeric and symmetric complexes in biological systems.

  12. Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering

    PubMed Central

    Gurnon, A. Kate; Godfrin, P. Douglas; Wagner, Norman J.; Eberle, Aaron P. R.; Butler, Paul; Porcar, Lionel

    2014-01-01

    A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is presented. The SANS shear cell consists of a concentric cylinder Couette geometry that is sealed and rotating about a horizontal axis so that the vorticity direction of the flow field is aligned with the neutron beam enabling scattering from the 1-2 plane of shear (velocity-velocity gradient, respectively). This approach is an advance over previous shear cell sample environments as there is a strong coupling between the bulk rheology and microstructural features in the 1-2 plane of shear. Flow-instabilities, such as shear banding, can also be studied by spatially resolved measurements. This is accomplished in this sample environment by using a narrow aperture for the neutron beam and scanning along the velocity gradient direction. Time resolved experiments, such as flow start-ups and large amplitude oscillatory shear flow are also possible by synchronization of the shear motion and time-resolved detection of scattered neutrons. Representative results using the methods outlined here demonstrate the useful nature of spatial resolution for measuring the microstructure of a wormlike micelle solution that exhibits shear banding, a phenomenon that can only be investigated by resolving the structure along the velocity gradient direction. Finally, potential improvements to the current design are discussed along with suggestions for supplementary experiments as motivation for future experiments on a broad range of complex fluids in a variety of shear motions. PMID:24561395

  13. Measuring material microstructure under flow using 1-2 plane flow-small angle neutron scattering.

    PubMed

    Gurnon, A Kate; Godfrin, P Douglas; Wagner, Norman J; Eberle, Aaron P R; Butler, Paul; Porcar, Lionel

    2014-02-06

    A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is presented. The SANS shear cell consists of a concentric cylinder Couette geometry that is sealed and rotating about a horizontal axis so that the vorticity direction of the flow field is aligned with the neutron beam enabling scattering from the 1-2 plane of shear (velocity-velocity gradient, respectively). This approach is an advance over previous shear cell sample environments as there is a strong coupling between the bulk rheology and microstructural features in the 1-2 plane of shear. Flow-instabilities, such as shear banding, can also be studied by spatially resolved measurements. This is accomplished in this sample environment by using a narrow aperture for the neutron beam and scanning along the velocity gradient direction. Time resolved experiments, such as flow start-ups and large amplitude oscillatory shear flow are also possible by synchronization of the shear motion and time-resolved detection of scattered neutrons. Representative results using the methods outlined here demonstrate the useful nature of spatial resolution for measuring the microstructure of a wormlike micelle solution that exhibits shear banding, a phenomenon that can only be investigated by resolving the structure along the velocity gradient direction. Finally, potential improvements to the current design are discussed along with suggestions for supplementary experiments as motivation for future experiments on a broad range of complex fluids in a variety of shear motions.

  14. Small-Angle Scattering of X-Rays from Extragalactic Sources by Dust in Intervening Galaxies

    NASA Astrophysics Data System (ADS)

    Miralda-Escudé, Jordi

    1999-02-01

    Gamma-ray bursts are now known to be a cosmological population of objects, which are often accompanied by X-ray and optical afterglows. The total energy emitted in the afterglow can be similar to the energy radiated in the gamma-ray burst itself. If a galaxy containing a large column density of dust is near the line of sight to a gamma-ray burst, small-angle scattering of the X-rays due to diffraction by the dust grains will give rise to an X-ray echo of the afterglow. A measurement of the angular size of the echo at a certain time after the afterglow is observed yields a combination of the angular diameter distances to the scattering galaxy and the gamma-ray burst that can be used to constrain cosmological models in the same way as a time delay in a gravitational lens. The scattering galaxy will generally cause gravitational lensing as well, and this should modify the shape of the X-ray echo from a circular ring. The main difficulty in detecting this phenomenon is the very low flux expected for the echo. The flux can be increased when the gamma-ray burst is highly magnified by gravitational lensing, or when the deflecting galaxy is at low redshift. X-ray echoes of continuous (but variable) sources, such as quasars, may also be detectable with high-resolution instruments and would allow similar measurements.

  15. Large-area proportional counter camera for the US National Small-Angle Neutron Scattering Facility

    SciTech Connect

    Abele, R.K.; Allin, G.W.; Clay, W.T.; Fowler, C.E.; Kopp, M.K.

    1980-01-01

    An engineering model of a multiwire position-sensitive proportional-counter (PSPC) was developed, tested, and installed at the US National Small-Angle Neutron Scattering Facility at ORNL. The PSPC is based on the RC-encoding and time-difference decoding method to measure the spatial coordinates of the interaction loci of individual scattered neutrons. The active area of the PSPC is 65 cm x 65 cm, and the active depth is 3.6 cm. The spatial uncertainty in both coordinates is approx. 1.0 cm (fwhm) for thermal neutrons; thus, a matrix of 64 x 64 picture elements is resolved. The count rate capability for randomly detected neutrons is 10/sup 4/ counts per second, with < 3% coincidence loss. The PSPC gas composition is 63% /sup 3/He, 32% Xe, and 5% CO/sub 2/ at an absolute pressure of approx. 3 x 10/sup 5/ Pa (3 atm). The detection efficiency is approx. 90% for the 0.475-nm (4.75-A) neutrons used in the scattering experiments.

  16. Estimation and modeling of coal pore accessibility using small angle neutron scattering

    DOE PAGES

    Zhang, Rui; Liu, Shimin; Bahadur, Jitendra; ...

    2015-09-04

    Gas diffusion in coal is controlled by nano-structure of the pores. The interconnectivity of pores not only determines the dynamics of gas transport in the coal matrix but also influences the mechanical strength. In this study, small angle neutron scattering (SANS) was employed to quantify pore accessibility for two coal samples, one of sub-bituminous rank and the other of anthracite rank. Moreover, a theoretical pore accessibility model was proposed based on scattering intensities under both vacuum and zero average contrast (ZAC) conditions. Our results show that scattering intensity decreases with increasing gas pressure using deuterated methane (CD4) at low Qmore » values for both coals. Pores smaller than 40 nm in radius are less accessible for anthracite than sub-bituminous coal. On the contrary, when the pore radius is larger than 40 nm, the pore accessibility of anthracite becomes larger than that of sub-bituminous coal. Only 20% of pores are accessible to CD4 for anthracite and 37% for sub-bituminous coal, where the pore radius is 16 nm. For these two coals, pore accessibility and pore radius follows a power-law relationship.« less

  17. BACKWARD ANGLE STRUCTURE IN THE 20Ne+28Si QUASIELASTIC SCATTERING

    NASA Astrophysics Data System (ADS)

    Sgouros, O.; Soukeras, V.; Pakou, A.; Patronis, N.; Zerva, K.; Keeley, N.; Strojek, I.; Trzcińska, A.; Piasecki, E.; Rusek, K.; Stiliaris, E.; Mazzocco, M.

    2013-10-01

    New data for the quasielastic scattering of 20Ne from a 28Si target at incident energies of 42.5 MeV and 52.3 MeV and for the 28Si(20Ne, 24Mg)24Mg, 28Si(20Ne, 16O)32S and 28Si(20Ne, 12C)36Ar transfer reactions at 52.3 MeV are reported. Oscillations are observed in the backward angle quasielastic scattering data at 52.3 MeV and the 28Si(20Ne, 12C)36Ar transfer cross-sections are of the same magnitude as those for single-α stripping. Coupled reaction channels (CRC) calculations are unable to describe either the quasielastic or the 28Si(20Ne, 12C)36Ar transfer data assuming a sequential α transfer process with α-particle form factors from the literature. The addition of direct 8Be cluster transfer can provide a reasonable description of both data sets, but only with much larger spectroscopic factors than suggested by simple structure calculations or the large 8Be emission thresholds of 20Ne, 28Si and 36Ar, suggesting that the observed structure is of resonance-like origin. An optical model analysis of the quasielastic scattering data is also reported.

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

    SciTech Connect

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

    2015-09-07

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

  19. Estimation and modeling of coal pore accessibility using small angle neutron scattering

    SciTech Connect

    Zhang, Rui; Liu, Shimin; Bahadur, Jitendra; Elsworth, Derek; Melnichenko, Yuri; He, Lilin; Wang, Yi

    2015-09-04

    Gas diffusion in coal is controlled by nano-structure of the pores. The interconnectivity of pores not only determines the dynamics of gas transport in the coal matrix but also influences the mechanical strength. In this study, small angle neutron scattering (SANS) was employed to quantify pore accessibility for two coal samples, one of sub-bituminous rank and the other of anthracite rank. Moreover, a theoretical pore accessibility model was proposed based on scattering intensities under both vacuum and zero average contrast (ZAC) conditions. Our results show that scattering intensity decreases with increasing gas pressure using deuterated methane (CD4) at low Q values for both coals. Pores smaller than 40 nm in radius are less accessible for anthracite than sub-bituminous coal. On the contrary, when the pore radius is larger than 40 nm, the pore accessibility of anthracite becomes larger than that of sub-bituminous coal. Only 20% of pores are accessible to CD4 for anthracite and 37% for sub-bituminous coal, where the pore radius is 16 nm. For these two coals, pore accessibility and pore radius follows a power-law relationship.

  20. Workshop on Research Techniques in Wave Propagation and Scattering

    NASA Astrophysics Data System (ADS)

    Varadan, V. V.; Varadan, V. K.

    1983-05-01

    A Workshop/Symposium on Research Techniques in Wave Propagation and Scattering was held at the Ohio State University October 18-21, 1982. This workshop was co-sponsored with the generous financial support of the U.S. Army Research Office, U.S. Office of Naval Research, the Center for Welding Research, O.S.U., and the Department of Engineering Mechanics, O.S.U. The workshop format consisted of a core of a general lectures of fifty minutes duration each and several shorter contributions that were of twenty minutes duration each. In addition, there were three panel discussions. The general lectures were of an expository nature on fundamental concepts and basic analytical/numerical techniques for the solution of wave scattering and propagation problems. The speakers were noted for their contribution to these techniques and in many cases have pioneered the techniques that they elaborated upon. These lectures were invaluable to the participants since they were of a pedagogical nature and easily understood by even those not very familiar with the particular method. The written version of many of these lectures will appear in a four volume Handbook on Acoustic, Electromagnetic and Elastic Wave Scattering to be published by North Holland as a separate project.

  1. Application of GPC/LALLS to cellulose research. [Gel permeation chromatography/low-angle laser light scattering

    SciTech Connect

    Cael, J.J.; Cietek, D.J.; Kolpak, F.J.

    1983-01-01

    The techniques of gel permeation chromatography and low-angle laser light scattering (GPC/LALLS) have been combined for absolute determination of cellulose molecular weights and molecular weight distributions (MWD). The GPC/LALLS technique has been applied to tetrahydrofuran (THF) solutions of cellulose tricarbanilate (CTC) derivatives prepared from celluloses having a wide range of molecular weights. The molecular weight data obtained are consistent with values determined by intrinsic viscosity methods; and as a consequence of the absolute nature of this technique, Mark-Houswink coefficients can be predicted from a single, broad-distribution, linear homopolymer without recourse to tedious and time-consuming fractional precipitation methods. A unique application of the technique has been in correlating GPC/LALLS molecular weight data with the viscosity of nonderivatized celluloses dissolved in 0.5 M cupiethylenediamine hydroxide (CuEn). The procedure yields an absolute viscosity-molecular weight relationship which is comparable with a similar relationship originally derived from cellulose nitrates. The results indicate that the weight-average degree of polymerization (DP/sub w/) for CTC preparations is considerably greater than that obtained from cellulose nitrates, and this discrepancy, in DP/sub w/ has been attributed to errors in the Mark-Houwink coefficients for the cellulose nitrate-acetone system. 25 references, 9 figures, 7 tables.

  2. NEUTRON SPECTROSCOPY BY DOUBLE SCATTER AND ASSOCIATED PARTICLE TECHNIQUES.

    SciTech Connect

    DIOSZEGI,I.

    2007-10-28

    Multiple detectors can provide [1,2] both directional and spectroscopic information. Neutron spectra may be obtained by neutron double scatter (DSNS), or the spontaneous fission associated particle (AP) technique. Spontaneous fission results in the creation of fission fragments and the release of gamma rays and neutrons. As these occur at the same instant, they are correlated in time. Thus gamma ray detection can start a timing sequence relative to a neutron detector where the time difference is dominated by neutron time-of-flight. In this paper we describe these techniques and compare experimental results with Monte Carlo calculations.

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

    PubMed Central

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

    2015-01-01

    We review recent developments in the rapidly growing field of membrane biophysics, with a focus on the structural properties of single lipid bilayers determined by different scattering techniques, namely neutron and X-ray scattering. The need for accurate lipid structural properties is emphasized by the sometimes conflicting results found in the literature, even in the case of the most studied lipid bilayers. Increasingly, accurate and detailed structural models require more experimental data, such as those from contrast varied neutron scattering and X-ray scattering experiments that are jointly refined with molecular dynamics simulations. This experimental and computational approach produces robust bilayer structural parameters that enable insights, for example, into the interplay between collective membrane properties and its components (e.g., hydrocarbon chain length and unsaturation, and lipid headgroup composition). From model studies such as these, one is better able to appreciate how a real biological membrane can be tuned by balancing the contributions from the lipid’s different moieties (e.g., acyl chains, headgroups, backbones, etc.). PMID:26402708

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

    SciTech Connect

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

    2015-09-21

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

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

    DOE PAGES

    Kučerka, Norbert; Heberle, Frederick A.; Pan, Jianjun; ...

    2015-09-21

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

  6. The structure of Sindbis virus produced from vertebrate and invertabrate hosts determined by small angle neutron scattering

    SciTech Connect

    He, Lilin; Piper, Amanda; Meilleur, Flora; Myles, Dean A A; Hernandez, Raquel; Brown, Dennis; Heller, William T

    2010-01-01

    The complex natural cycle of vectored viruses that transition between host species, such as between insects and mammals, makes understanding the full life cycle of the virus an incredibly complex problem. Sindbis virus, an arbovirus and prototypic alphavirus having an inner protein shell and an outer glycoprotein coat separated by a lipid membrane, is one example of a vectored virus that transitions between vertebrate and insect hosts. While evidence of host-specific differences in Sindbis virus has been observed, no work has been performed to characterize the impact of the host species on the structure of the virus. Here, we report the first study of the structural differences between Sindbis viruses grown in mammalian and insect cells, which were determined by small-angle neutron scattering (SANS), a nondestructive technique that did not decrease the infectivity of the Sindbis virus particles studied. The scattering data and modeling showed that, while the radial position of the lipid bilayer did not change significantly, it was possible to conclude that it did have significantly more cholesterol when the virus was grown in mammalian cells. Additionally, the outer protein coat was found to be more extended in the mammalian Sindbis virus. The SANS data also demonstrated that the RNA and nucleocapsid protein share a closer interaction in the mammalian-cell-grown virus than in the virus from insect cells.

  7. Spatial distribution of intra-molecular water and polymeric components in polyelectrolyte dendrimers revealed by small angle scattering investigations

    SciTech Connect

    Chen, Chun-Yu; Chen, Wei-Ren; Herwig, Kenneth W; Hong, Kunlun; Li, Xin; Liu, Emily; Liu, Yun; Smith, Gregory Scott; Wu, Bin; Yang, Jun; Do, Changwoo

    2011-01-01

    An experimental scheme using contrast variation small angle neutron scattering technique (SANS), is developed to investigate the structural characteristics of amine-terminated poly(amidoamine) dendrimers (PAMAM) solutions. The focus is placed on understanding the dependence of intra-dendrimer water and polymer distribution on molecular protonation, which can be precisely adjusted by tuning the pH value of solution. Assuming the spherical symmetry in the spatial arrangement of the constituent component of dendrimer, and the atomic ratio of hydrogen-to-deuterium for the solvent residing within the cavities of dendrimer is identical to that for the solvent outside dendrimer, the intra-dendrimer water distribution along the radial direction can be determined based on the model of coherent scattering cross section developed in this work. Moreover, our result clearly reveals an outward relocation of the peripheral groups, as well as the enhanced intra-dendrimer hydration, upon increasing the molecular protonation and therefore allows the determination of segmental backfolding in a quantitative manner. The connection between these charge-induced structural changes and our recently observed progressively active segmental dynamics is also discussed.

  8. NOTE: Characterization of cirrhosis and hepatocellular carcinoma using low-angle x-ray scattering signatures of serum

    NASA Astrophysics Data System (ADS)

    Elshemey, Wael M.; Desouky, Omar S.; Mohammed, Mohammed S.; Elsayed, Anwar A.; El-houseini, Motawa E.

    2003-09-01

    The diagnosis of hepatocellular carcinoma (HCC) usually occurs at late stages in the disease when there are few effective treatment options. The measurement of the concentration of tumour markers in the serum of patients is a complementary tool frequently used for the interpretation of diagnostic imaging results. It is also used as a prognostic tool for the detection of cancer. Unfortunately, the sensitivity of tumour markers is still low and many times it yields normal results for cirrhotic and HCC patients. In the current work, the detection possibility of the structural changes in serum proteins accompanying cirrhosis and HCC is investigated using a low-angle x-ray scattering (LAXS) technique. The results show that there are significant differences in the LAXS profiles of cirrhosis and HCC lyophilized serum samples compared to normal. The changes in shape, total counts and position of the first scattering peak at 4.8°, which was previously reported to be sensitive to the structural changes in protein, showed the most characteristic deviations from normal serum. The present results are promising and would offer a potentially helpful complementary tool for monitoring cirrhosis and HCC.

  9. New developments in the ATSAS program package for small-angle scattering data analysis

    PubMed Central

    Petoukhov, Maxim V.; Franke, Daniel; Shkumatov, Alexander V.; Tria, Giancarlo; Kikhney, Alexey G.; Gajda, Michal; Gorba, Christian; Mertens, Haydyn D. T.; Konarev, Petr V.; Svergun, Dmitri I.

    2012-01-01

    New developments in the program package ATSAS (version 2.4) for the processing and analysis of isotropic small-angle X-ray and neutron scattering data are described. They include (i) multiplatform data manipulation and display tools, (ii) programs for automated data processing and calculation of overall parameters, (iii) improved usage of high- and low-resolution models from other structural methods, (iv) new algorithms to build three-dimensional models from weakly interacting oligomeric systems and complexes, and (v) enhanced tools to analyse data from mixtures and flexible systems. The new ATSAS release includes installers for current major platforms (Windows, Linux and Mac OSX) and provides improved indexed user documentation. The web-related developments, including a user discussion forum and a widened online access to run ATSAS programs, are also presented. PMID:25484842

  10. Small-angle scattering as a tool to study the thermal denaturation of DNA

    NASA Astrophysics Data System (ADS)

    Wood, Kathleen; Knott, Robert; Tonchev, Ognyan; Angelov, Dimitar; Theodorakopoulos, Nikos; Peyrard, Michel

    2014-10-01

    DNA thermal denaturation is the breaking of the base pairs, leading to a splitting of the two strands of the double helix. While it is easy to measure the fraction of open base pairs (f) vs. temperature, determining the fraction (p) of fully open molecules is much harder. Previously, the simultaneous recording of f and p could only be achieved for special sequences. We show that small-angle scattering of X-rays or neutrons allows the measurement of p for any sequence. We illustrate the method with a SAXS investigation of two sequences designed to exhibit different melting profiles and compare the SAXS data with nano-calorimetric measurements of the melting curve.

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

    SciTech Connect

    Abramova, V. V.; Sinitskii, A. S.; Grigor'eva, N. A.; Grigor'ev, S. V.; Belov, D. V.; Petukhov, A. V.; Mistonov, A. A.; Vasil'eva, A. V.; Tret'yakov, Yu. D.

    2009-07-15

    The results of an ultrasmall-angle X-ray scattering study of iron(III) oxide inverse opal thin films are presented. The photonic crystals examined are shown to have fcc structure with amount of stacking faults varying among the samples. The method used in this study makes it possible to easily distinguish between samples with predominantly twinned fcc structure and nearly perfect fcc stacking. The difference observed between samples fabricated under identical conditions is attributed to random layer stacking in the self-assembled colloidal crystals used as templates for fabricating the inverse opals. The present method provides a versatile tool for analyzing photonic crystal structure in studies of inverse opals made of various materials, colloidal crystals, and three-dimensional photonic crystals of other types.

  12. Small angle x-ray scattering and electron microscopy of nanoparticles formed in an electrical arc

    NASA Astrophysics Data System (ADS)

    Carvou, E.; Garrec, J. L. Le; Pérez, J.; Praquin, J.; Djeddi, M.; Mitchell, J. B. A.

    2013-03-01

    Small Angle X-ray Scattering has been used to characterize nanoparticles generated by electrical arcing between metallic (AgSnO2) electrodes. The particles are found to have diameters between 30 and 40 nm and display smooth surfaces suggesting that they are either in liquid form or have solidified from the liquid state. Particles collected around the electrodes were analyzed by Transmission Electron Microscopy and were seen to be much larger than those seen in the SAXS measurement, to be spherical in form and composed of silver metal with irregular tin oxide particles deposited on their surface. Mixed metal nanoparticles can have important practical applications and the use of mixed sintered electrodes may be a direct method for their production.

  13. Small-angle neutron scattering from polymer hydrogels with memory effect for medicine immobilization

    SciTech Connect

    Kulvelis, Yu. V. Lebedev, V. T.; Trunov, V. A.; Pavlyuchenko, V. N.; Ivanchev, S. S.; Primachenko, O. N.; Khaikin, S. Ya.

    2011-12-15

    Hydrogels synthesized based on cross-linked copolymers of 2-hydroxyethyl methacrylate and functional monomers (acrylic acid or dimethylaminoethyl methacrylate), having a memory effect with respect to target medicine (cefazolin), have been investigated by small-angle neutron scattering. The hydrogels are found to have a two-level structural organization: large (up to 100 nm) aggregates filled with network cells (4-7 nm in size). The structural differences in the anionic, cationic, and amphiphilic hydrogels and the relationship between their structure and the ability of hydrogels to absorb moisture are shown. A relationship between the memory effect during cefazolin immobilization and the internal structure of hydrogels, depending on their composition and type of functional groups, is established.

  14. Small-angle Scattering Study of Mesoscopic Structures in Charged Gel and Their Evolution in Dehydration

    SciTech Connect

    Sugiyama, M.; Annaka, M.; Hara, K.; Vigild, M. E.; Wignall, George D

    2003-01-01

    Mesoscopic structures, with length scales {approx}10{sup 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 experiments reveal that, depending upon the [NIPA]/[SA] ratio, the dehydrated NIPA-SA gel shows two mesoscopic structures: one consists of randomly distributed SA-rich islands in NIPA matrix, while the other is a microphase-separated structure, composed of NIPA-rich and SA-rich domains. In addition, the SANS experiments reveal the mesoscopic structural features during the dehydration process. As the concentration of the network polymers increases, NIPA-rich and water-rich domains segregate in the gel. Then, an electrostatic interaction between the segregated domains induces a microphase-separated structure in the limit of the dehydrated NIPA-SA gel.

  15. Direct detection of resonant electron pitch angle scattering by whistler waves in a laboratory plasma.

    PubMed

    Van Compernolle, B; Bortnik, J; Pribyl, P; Gekelman, W; Nakamoto, M; Tao, X; Thorne, R M

    2014-04-11

    Resonant interactions between energetic electrons and whistler mode waves are an essential ingredient in the space environment, and in particular in controlling the dynamic variability of Earth's natural radiation belts, which is a topic of extreme interest at the moment. Although the theory describing resonant wave-particle interaction has been present for several decades, it has not been hitherto tested in a controlled laboratory setting. In the present Letter we report on the first laboratory experiment to directly detect resonant pitch angle scattering of energetic (∼keV) electrons due to whistler mode waves. We show that the whistler mode wave deflects energetic electrons at precisely the predicted resonant energy, and that varying both the maximum beam energy, and the wave frequency, alters the energetic electron beam very close to the resonant energy.

  16. Aggregates structure analysis of petroleum asphaltenes with small-angle neutron scattering.

    SciTech Connect

    Tanaka, R.; Hunt, J. E.; Winans, R. E.; Thiyagarajan, P.; Sato, S.; Takanohashi, T.; Idemitsu Kosan Co.; National Institute of Advanced Industrial Science and Technology

    2003-01-01

    The objective of this study is to examine changes in the structures of petroleum asphaltene aggregates in situ with small-angle neutron scattering (SANS). Asphaltenes were isolated from three different crude oils: Maya, Khafji, and Iranian Light. An aliquot of the 5 wt % asphaltene solution in deuterated Decalin, 1-methylnaphthalene, or quinoline was loaded in a special stainless steel cell for SANS measurements. SANS data measured at various temperatures from 25 to 350 {sup o}C showed various topological features different with asphaltene or solvent species. A fractal network was formed only with asphaltene of Maya in Decalin, and it remained even at 350 {sup o}C. In all of the solvents, asphaltenes aggregate in the form of a prolate ellipsoid with a high aspect ratio at 25 {sup o}C and got smaller with increasing temperature. That became a compact sphere with the size of around 25 {angstrom} in radius at 350 {sup o}C.

  17. Waveguide detection of right-angle-scattered light in flow cytometry

    DOEpatents

    Mariella, Jr., Raymond P.

    2000-01-01

    A transparent flow cell is used as an index-guided optical waveguide. A detector for the flow cell but not the liquid stream detects the Right-Angle-Scattered (RAS) Light exiting from one end of the flow cell. The detector(s) could view the trapped RAS light from the flow cell either directly or through intermediate optical light guides. If the light exits one end of the flow cell, then the other end of the flow cell can be given a high-reflectivity coating to approximately double the amount of light collected. This system is more robust in its alignment than the traditional flow cytometry systems which use imaging optics, such as microscope objectives.

  18. A precise measurement of the weak mixing angle in neutrino-nucleon scattering

    NASA Astrophysics Data System (ADS)

    Zeller, Geralyn P.

    This dissertation reports a precise determination of the weak mixing angle, sin2 thetaW, from measurement of the ratios of neutral current to charged current neutrino deep inelastic cross sections. High statistics samples of separately collected neutrino and antineutrino events, resulting from exposure to the Fermilab neutrino beam during the period from 1996 to 1997, allowed the reduction of systematic errors associated with charm production and other sources. The final value, sin 2 thetaW(on shell) = 0.2277 +/- 0.0013 (stat) +/- 0.0009 (syst), lies three standard deviations above the standard model prediction. The measurement is currently the most precise determination of sin2 theta W in neutrino-nucleon scattering, surpassing its predecessors by a factor of two in precision. A model independent analysis recasts the same data into a measurement of effective left and right handed neutral current quark couplings.

  19. Robust, high-throughput solution structural analyses by small angle X-ray scattering (SAXS)

    SciTech Connect

    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.

  20. Small-angle x-ray scattering study of polymer structure: Carbosilane dendrimers in hexane solution

    NASA Astrophysics Data System (ADS)

    Shtykova, E. V.; Feigin, L. A.; Volkov, V. V.; Malakhova, Yu. N.; Streltsov, D. R.; Buzin, A. I.; Chvalun, S. N.; Katarzhanova, E. Yu.; Ignatieva, G. M.; Muzafarov, A. M.

    2016-09-01

    The three-dimensional organization of monodisperse hyper-branched macromolecules of regular structure—carbosilane dendrimers of zero, third, and sixth generations—has been studied by small-angle X-ray scattering (SAXS) in solution. The use of modern methods of SAXS data interpretation, including ab initio modeling, has made it possible to determine the internal architecture of the dendrimers in dependence of the generation number and the number of cyclosiloxane end groups (forming the shell of dendritic macromolecules) and show dendrimers to be spherical. The structural results give grounds to consider carbosilane dendrimers promising objects for forming crystals with subsequent structural analysis and determining their structure with high resolution, as well as for designing new materials to be used in various dendrimer-based technological applications.

  1. Use of anomalous small angle x-ray scattering to investigate microstructural features in complex alloys

    SciTech Connect

    Weertman, J.R.

    1988-08-01

    This report covers the last 5 months of the second year of this grant and the first 8 months of the third year. The research thrust of this grant has been directed into two areas. The principal effort has been spent in an investigation of the use of anomalous small angle x-ray scattering (ASAXS) to observe changes in the microstructure of a relatively complex alloy produced by high temperature deformation or aging. The second effort involves a study of the high temperature behavior of several ferritic steels. During this past year we have been examining the effect of environment (air vs vacuum) on the high temperature strength of Fe9Cr1Mo modified by the addition of small amounts of V and Nb.

  2. Scattering angle dependence of electron impact excitation: Intensity variation within a vibrational progression

    SciTech Connect

    Dillon, M.; Kimura, M. ); Buenker, R.J.; Hirsch, G.; Li, Y.; Chantranupong, L. )

    1995-01-22

    Intensity distributions of electronic transitions in O[sub 2] and CO within a vibrational progression resulting from electron impact excitation are studied theoretically and experimentally. The [ital multireference] [ital single]- [ital and] [ital double]-[ital excitation] [ital configuration] [ital interaction] (MRD-CI) method is used to elucidate details of selected electronic transitions. In particular, the adiabatic MRD-CI approach can account for the variation of the Franck--Condon envelope with scattering angle that has been reported for the [ital B] [sup 1][Sigma][sup +][l arrow][ital X] [sup 1][Sigma][sup +] transition in CO and also was recently observed in the [ital B][prime] [sup 3][Sigma][sup [minus

  3. Small angle neutron scattering (SANS and V-SANS) study of asphaltene aggregates in crude oil.

    PubMed

    Headen, Thomas F; Boek, Edo S; Stellbrink, Jörg; Scheven, Ulrich M

    2009-01-06

    We report small angle neutron scattering (SANS) experiments on two crude oils. Analysis of the high-Q SANS region has probed the asphaltene aggregates in the nanometer length scale. We find that the radius of gyration decreases with increasing temperature. We show that SANS measurements on crude oils give similar aggregate sizes to those found from SANS measurements of asphaltenes redispersed in deuterated toluene. The combined use of SANS and V-SANS on crude oil samples has allowed the determination of the radius of gyration of large scale asphaltene aggregates of approximately 0.45 microm. This has been achieved by the fitting of Beaucage functions over two size regimes. Analysis of the fitted Beaucage functions at very low-Q has shown that the large scale aggregates are not simply made by aggregation of all the smaller nanoaggregates. Instead, they are two different aggregates coexisting.

  4. Study of (Cyclic Peptide)-Polymer Conjugate Assemblies by Small-Angle Neutron Scattering.

    PubMed

    Koh, Ming Liang; FitzGerald, Paul A; Warr, Gregory G; Jolliffe, Katrina A; Perrier, Sébastien

    2016-12-19

    We present a fundamental study into the self-assembly of (cyclic peptide)-polymer conjugates as a versatile supramolecular motif to engineer nanotubes with defined structure and dimensions, as characterised in solution using small-angle neutron scattering (SANS). This work demonstrates the ability of the grafted polymer to stabilise and/or promote the formation of unaggregated nanotubes by the direct comparison to the unconjugated cyclic peptide precursor. This ideal case permitted a further study into the growth mechanism of self-assembling cyclic peptides, allowing an estimation of the cooperativity. Furthermore, we show the dependency of the nanostructure on the polymer and peptide chemical functionality in solvent mixtures that vary in the ability to compete with the intermolecular associations between cyclic peptides and ability to solvate the polymer shell.

  5. Small angle x-ray scattering studies of carbon anodes used in lithium rechargeable batteries.

    SciTech Connect

    Sandi, G.; Carrado, K. A.; Winans, R. E.; Seifert, S.; Johnson, C. S.

    1999-11-16

    In ANL laboratories, disordered carbons with predictable surface area and porosity properties have been prepared using inorganic templates containing well defined pore sizes. The carbons have been tested in electrochemical cells as anodes in lithium secondary batteries. They deliver high specific capacity and display excellent performance in terms of the number of cycles run. In situ small angle X-ray scattering (SAXS) during electrochemical cycling was carried out at the Advanced Photon Source, at ANL. In order to monitor the carbon electrode structural changes upon cycling, an electrochemical cell was specially designed to allow for the application of electrical current and the collection of SAXS data at the same time. Results show that upon cycling the structure of the carbon remains unchanged, which is desirable in reversible systems.

  6. Elucidating the Molecular Deformation Mechanism of Entangled Polymers in Fast Flow by Small Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Wang, Yangyang; Sanchez-Diaz, Luis; Cheng, Shiwang; Hong, Kunlun; Chen, Wei-Ren; Liu, Jianning; Lin, Panpan; Wang, Shi-Qing

    Understanding the viscoelastic properties of polymers is of fundamental and practical importance because of the vast and ever expanding demand of polymeric materials in daily life. Our current theoretical framework for describing the nonlinear flow behavior of entangled polymers is built upon the tube model pioneered by de Gennes, Doi, and Edwards. In this work, we critically examine the central hypothesis of the tube model for nonlinear rheology using small angle neutron scattering (SANS). While the tube model envisions a unique non-affine elastic deformation mechanism for entangled polymers, our SANS measurements show that the evolution of chain conformation of a well-entangled polystyrene melt closely follows the affine deformation mechanism in uniaxial extension, even when the Rouse Weissenberg number is much smaller than unity. This result provides a key clue for understanding the molecular deformation mechanism of entangled polymers in fast flow. Several implications from our analysis will be discussed in this talk.

  7. Measurement of the absolute differential cross section of proton–proton elastic scattering at small angles

    DOE PAGES

    Mchedlishvili, D.; Chiladze, D.; Dymov, S.; ...

    2016-02-03

    The differential cross section for proton-proton elastic scattering has been measured at a beam kinetic energy of 1.0 GeV and in 200 MeV steps from 1.6 to 2.8 GeV for centre-of-mass angles in the range from 12°-16° to 25°-30°, depending on the energy. A precision in the overall normalisation of typically 3% was achieved by studying the energy losses of the circulating beam of the COSY storage ring as it passed repeatedly through the windowless hydrogen target of the ANKE magnetic spectrometer. It is shown that the data have a significant impact upon the results of a partial wave analysis.more » Furthermore, after extrapolating the differential cross sections to the forward direction, the results are broadly compatible with the predictions of forward dispersion relations.« less

  8. Measurement of the absolute differential cross section of proton–proton elastic scattering at small angles

    SciTech Connect

    Mchedlishvili, D.; Chiladze, D.; Dymov, S.; Bagdasarian, Z.; Barsov, S.; Gebel, R.; Gou, B.; Hartmann, M.; Kacharava, A.; Keshelashvili, I.; Khoukaz, A.; Kulessa, P.; Kulikov, A.; Lehrach, A.; Lomidze, N.; Lorentz, B.; Maier, R.; Macharashvili, G.; Merzliakov, S.; Mikirtychyants, S.; Nioradze, M.; Ohm, H.; Prasuhn, D.; Rathmann, F.; Serdyuk, V.; Schroer, D.; Shmakova, V.; Stassen, R.; Stein, H. J.; Stockhorst, H.; Strakovsky, I. I.; Stroher, H.; Tabidze, M.; Taschner, A.; Trusov, S.; Tsirkov, D.; Uzikov, Yu.; Valdau, Yu.; Wilkin, C.; Workman, R. L.; Wustner, P.

    2016-02-03

    The differential cross section for proton-proton elastic scattering has been measured at a beam kinetic energy of 1.0 GeV and in 200 MeV steps from 1.6 to 2.8 GeV for centre-of-mass angles in the range from 12°-16° to 25°-30°, depending on the energy. A precision in the overall normalisation of typically 3% was achieved by studying the energy losses of the circulating beam of the COSY storage ring as it passed repeatedly through the windowless hydrogen target of the ANKE magnetic spectrometer. It is shown that the data have a significant impact upon the results of a partial wave analysis. Furthermore, after extrapolating the differential cross sections to the forward direction, the results are broadly compatible with the predictions of forward dispersion relations.

  9. Small-angle neutron scattering of nanocrystalline gadolinium and holmium with random paramagnetic susceptibility

    NASA Astrophysics Data System (ADS)

    Döbrich, Frank; Bick, Jens-Peter; Birringer, Rainer; Wolff, Matthias; Kohlbrecher, Joachim; Michels, Andreas

    2015-02-01

    A neutron study of nanocrystalline terbium (Balaji G et al 2008 Phys. Rev. Lett. 100 227202) has shown that the randomly oriented anisotropy of the paramagnetic susceptibility tensor may lead to strongly correlated nanoscale spin disorder in the paramagnetic state which can be probed very effectively by magnetic small-angle neutron scattering (SANS). In principle, this scenario is also applicable to other rare-earth metals and the size of the effect is expected to scale with the strength of the anisotropy in the paramagnetic state. Here, we report SANS results (in the paramagnetic state) on nanocrystalline inert-gas condensed samples of Gd and Ho, which represent the cases of low and high anisotropy, respectively.

  10. Riboswitch Conformations Revealed by Small-Angle X-Ray Scattering

    PubMed Central

    Lipfert, Jan; Herschlag, Daniel; Doniach, Sebastian

    2015-01-01

    Summary Riboswitches are functional RNA molecules that control gene expression through conformational changes in response to small-molecule ligand binding. In addition, riboswitch 3D structure, like that of other RNA molecules, is dependent on cation–RNA interactions as the RNA backbone is highly negatively charged. Here, we show how small-angle X-ray scattering (SAXS) can be used to probe RNA conformations as a function of ligand and ion concentration. In a recent study of a glycine-binding tandem aptamer from Vibrio cholerae, we have used SAXS data and thermodynamic modeling to investigate how Mg2+-dependent folding and glycine binding are energetically coupled. In addition, we have employed ab initio shape reconstruction algorithms to obtain low-resolution models of the riboswitch structure from SAXS data under different solution conditions. PMID:19381558

  11. Small angle neutron scattering as fingerprinting of ancient potteries from Sicily (Southern Italy)

    SciTech Connect

    Barone, G.; Mazzoleni, P.; Crupi, V.; Majolino, D.; Venuti, V.; Teixeira, J.

    2009-09-01

    Small angle neutron scattering measurements have been carried out in order to investigate, in microdestructive way, the mesoscopic structure of a variety of potteries of relevance to cultural heritage coming from different Sicilian (Southern Italy) archeological sites belonging to the 'Strait of Messina' area and dated back to 7th-3rd century B.C. Data have been compared with the mesoscopic parameters extracted for two series of clayey sediments typical of the Strait of Messina area and fired under controlled conditions. The observed agreement between the features of reference and archeological samples allowed us to estimate the maximum firing temperature of the latter. Information on the pore sizes was obtained by the use of the concept of fractal surface, and compared with porosimetry results.

  12. A stress-controlled shear cell for small-angle light scattering and microscopy

    NASA Astrophysics Data System (ADS)

    Aime, S.; Ramos, L.; Fromental, J. M.; Prévot, G.; Jelinek, R.; Cipelletti, L.

    2016-12-01

    We develop and test a stress-controlled, parallel plates shear cell that can be coupled to an optical microscope or a small angle light scattering setup, for simultaneous investigation of the rheological response and the microscopic structure of soft materials under an imposed shear stress. In order to minimize friction, the cell is based on an air bearing linear stage, the stress is applied through a contactless magnetic actuator, and the strain is measured through optical sensors. We discuss the contributions of inertia and of the small residual friction to the measured signal and demonstrate the performance of our device in both oscillating and step stress experiments on a variety of viscoelastic materials.

  13. Small angle neutron scattering study to determine the structure of high strength hydrogels.

    NASA Astrophysics Data System (ADS)

    Tominaga, Taiki; Tirumala, Vijay R.; Lin, Eric K.; Wu, Wen-Li; Gong, Jian Ping; Furukawa, Hidemitsu; Osada, Yoshihito

    2006-03-01

    Hydrogels are swollen polymer networks containing more than 90% water. Most hydrogels, however, are mechanically too weak to be used as load bearing devices. Gong et al. have overcome this problem by synthesizing hydrogels with a double network (DN) structure. Modifying the polyelectrolyte network structure by polymerization of high molecular weight uncharged polymer in situ, resulted in orders of magnitude increase in their load bearing ability. Despite 90% water, these tough gels exhibit a fracture stress of 170 kg/cm^2, similar to that of articular cartilage found in the bone-joints of human body. In this work, we determined the structure of DN-gels using small angle neutron scattering. Structural origins for high toughness found in DN-gels were then examined by comparing the structure of DN-gels with that of pure polyelectrolyte network and polyacrylamide solution.

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

    NASA Astrophysics Data System (ADS)

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

    2011-03-01

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

  15. Clustering of water molecules in ultramicroporous carbon: In-situ small-angle neutron scattering

    DOE PAGES

    Bahadur, Jitendra; Contescu, Cristian I.; Rai, Durgesh K.; ...

    2016-10-19

    The adsorption of water is central to most of the applications of microporous carbon as adsorbent material. We report early kinetics of water adsorption in the microporous carbon using in-situ small-angle neutron scattering. It is observed that adsorption of water occurs via cluster formation of molecules. Interestingly, the cluster size remains constant throughout the adsorption process whereas number density of clusters increases with time. The role of surface chemistry of microporous carbon on the early kinetics of adsorption process was also investigated. Lastly, the present study provides direct experimental evidence for cluster assisted adsorption of water molecules in microporous carbonmore » (Do-Do model).« less

  16. Quantitative impact of small angle forward scatter on whole blood oximetry using a Beer-Lambert absorbance model.

    PubMed

    LeBlanc, Serge Emile; Atanya, Monica; Burns, Kevin; Munger, Rejean

    2011-04-21

    It is well known that red blood cell scattering has an impact on whole blood oximetry as well as in vivo retinal oxygen saturation measurements. The goal of this study was to quantify the impact of small angle forward scatter on whole blood oximetry for scattering angles found in retinal oximetry light paths. Transmittance spectra of whole blood were measured in two different experimental setups: one that included small angle scatter in the transmitted signal and one that measured the transmitted signal only, at absorbance path lengths of 25, 50, 100, 250 and 500 µm. Oxygen saturation was determined by multiple linear regression in the 520-600 nm wavelength range and compared between path lengths and experimental setups. Mean calculated oxygen saturation differences between setups were greater than 10% at every absorbance path length. The deviations to the Beer-Lambert absorbance model had different spectral dependences between experimental setups, with the highest deviations found in the 520-540 nm range when scatter was added to the transmitted signal. These results are consistent with other models of forward scatter that predict different spectral dependences of the red blood cell scattering cross-section and haemoglobin extinction coefficients in this wavelength range.

  17. Investigation on the structure of water/AOT/IPM/alcohols reverse micelles by conductivity, dynamic light scattering, and small angle X-ray scattering.

    PubMed

    Zhang, Xiaoguang; Chen, Yingjun; Liu, Jiexiang; Zhao, Chuanzhuang; Zhang, Haijiao

    2012-03-29

    We have systematically investigated the effect of alcohols (ethanol, propanol, butanol, and pentanol) on the structure of the water/AOT/IPM system using conductivity, dynamic light scattering (DLS), and small-angle X-ray scattering (SAXS) techniques. The results show that no percolation phenomenon is observed in the water/AOT/IPM system, whereas the addition of ethanol (propanol and butanol) induces apparently percolation. The threshold water content (W(p)) depends closely on the alcohol type and concentration. The effect of alcohols on the conductance behavior is discussed from the physical properties of alcohols, the interfacial flexibility, and the attractive interactions between droplets. The hydrodynamic diameter of droplets (d(H)) obtained from DLS increases markedly with the increase in water content (W(0)); however, it decreases gradually with increasing alcohol chain length and concentration. SAXS measurements display distinctly the shoulder, the low hump peaks, and the heavy tail phenomenon in the pair distance distribution function p(r) profile, which rely strongly on the alcohol species and its concentration. The gyration radius (R(g)) increases with increasing W(0), and decreases with the increase of alcohol chain length and concentration. Schematic diagram of the conductance mechanism of water/AOT/IPM/alcohol systems is primarily depicted. Three different phases of the discrete droplets, the oligomers, and the isolated ellipsoidal droplets existed in the different W(0) ranges correspond to three different stages in the conductivity-W(0) curve. Coupling the structure characteristics of reverse micelles obtained from DLS and SAXS techniques with conductivity could be greatly helpful to deeply understand the percolation mechanism of water/AOT/IPM/alcohols systems.

  18. A technique for estimating 4D-CBCT using prior knowledge and limited-angle projections

    SciTech Connect

    Zhang, You; Yin, Fang-Fang; Ren, Lei; Segars, W. Paul

    2013-12-15

    in estimated and “ground-truth” onboard images for MM-only, FD-only, and MM-FD techniques were 60.10% (±27.17%)/4.9 mm (±3.0 mm), 96.07% (±31.48%)/12.1 mm (±3.9 mm) and 11.45% (±9.37%)/1.3 mm (±1.3 mm), respectively. For orthogonal-view 30°-each scan angle, the corresponding results were 59.16% (±26.66%)/4.9 mm (±3.0 mm), 75.98% (±27.21%)/9.9 mm (±4.0 mm), and 5.22% (±2.12%)/0.5 mm (±0.4 mm). For single-view scan angles of 3°, 30°, and 60°, the results for MM-FD technique were 32.77% (±17.87%)/3.2 mm (±2.2 mm), 24.57% (±18.18%)/2.9 mm (±2.0 mm), and 10.48% (±9.50%)/1.1 mm (±1.3 mm), respectively. For projection angular-sampling-intervals of 0.6°, 1.2°, and 2.5° with the orthogonal-view 30°-each scan angle, the MM-FD technique generated similar VPD (maximum deviation 2.91%) and COMS (maximum deviation 0.6 mm), while sparser sampling yielded larger VPD/COMS. With equal number of projections, the estimation results using scattered 360° scan angle were slightly better than those using orthogonal-view 30°-each scan angle. The estimation accuracy of MM-FD technique declined as noise level increased.Conclusions: The MM-FD technique substantially improves the estimation accuracy for onboard 4D-CBCT using prior planning 4D-CT and limited-angle projections, compared to the MM-only and FD-only techniques. It can potentially be used for the inter/intrafractional 4D-localization verification.

  19. Accuracy and efficiency considerations for wide-angle wavefield extrapolators and scattering operators

    NASA Astrophysics Data System (ADS)

    Thomson, C. J.

    2005-10-01

    Several observations are made concerning the numerical implementation of wide-angle one-way wave equations, using for illustration scalar waves obeying the Helmholtz equation in two space dimensions. This simple case permits clear identification of a sequence of physically motivated approximations of use when the mathematically exact pseudo-differential operator (PSDO) one-way method is applied. As intuition suggests, these approximations largely depend on the medium gradients in the direction transverse to the main propagation direction. A key point is that narrow-angle approximations are to be avoided in the interests of accuracy. Another key consideration stems from the fact that the so-called `standard-ordering' PSDO indicates how lateral interpolation of the velocity structure can significantly reduce computational costs associated with the Fourier or plane-wave synthesis lying at the heart of the calculations. A third important point is that the PSDO theory shows what approximations are necessary in order to generate an exponential one-way propagator for the laterally varying case, representing the intuitive extension of classical integral-transform solutions for a laterally homogeneous medium. This exponential propagator permits larger forward stepsizes. Numerical comparisons with Helmholtz (i.e. full) wave-equation finite-difference solutions are presented for various canonical problems. These include propagation along an interfacial gradient, the effects of a compact inclusion and the formation of extended transmitted and backscattered wave trains by model roughness. The ideas extend to the 3-D, generally anisotropic case and to multiple scattering by invariant embedding. It is concluded that the method is very competitive, striking a new balance between simplifying approximations and computational labour. Complicated wave-scattering effects are retained without the need for expensive global solutions, providing a robust and flexible modelling tool.

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

    NASA Astrophysics Data System (ADS)

    Lambard, Jacques; Lesieur, Pierre; Zemb, Thomas

    1992-06-01

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

  1. Methods for magnetic resonance analysis using magic angle technique

    DOEpatents

    Hu, Jian Zhi [Richland, WA; Wind, Robert A [Kennewick, WA; Minard, Kevin R [Kennewick, WA; Majors, Paul D [Kennewick, WA

    2011-11-22

    Methods of performing a magnetic resonance analysis of a biological object are disclosed that include placing the object in a main magnetic field (that has a static field direction) and in a radio frequency field; rotating the object at a frequency of less than about 100 Hz around an axis positioned at an angle of about 54.degree.44' relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a phase-corrected magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. In particular embodiments the method includes pulsing the radio frequency to provide at least two of a spatially selective read pulse, a spatially selective phase pulse, and a spatially selective storage pulse. Further disclosed methods provide pulse sequences that provide extended imaging capabilities, such as chemical shift imaging or multiple-voxel data acquisition.

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

    PubMed Central

    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. PMID:25721341

  3. Resolution of ab initio shapes determined from small-angle scattering.

    PubMed

    Tuukkanen, Anne T; Kleywegt, Gerard J; Svergun, Dmitri I

    2016-11-01

    Spatial resolution is an important characteristic of structural models, and the authors of structures determined by X-ray crystallography or electron cryo-microscopy always provide the resolution upon publication and deposition. Small-angle scattering of X-rays or neutrons (SAS) has recently become a mainstream structural method providing the overall three-dimensional structures of proteins, nucleic acids and complexes in solution. However, no quantitative resolution measure is available for SAS-derived models, which significantly hampers their validation and further use. Here, a method is derived for resolution assessment for ab initio shape reconstruction from scattering data. The inherent variability of the ab initio shapes is utilized and it is demonstrated how their average Fourier shell correlation function is related to the model resolution. The method is validated against simulated data for proteins with known high-resolution structures and its efficiency is demonstrated in applications to experimental data. It is proposed that henceforth the resolution be reported in publications and depositions of ab initio SAS models.

  4. Investigation of the tripoli porous structure by small-angle neutron scattering

    SciTech Connect

    Avdeev, M. V.; Blagoveshchenskii, N. M.; Garamus, V. M.; Novikov, A. G. Puchkov, A. V.

    2011-12-15

    The characteristics of the tripoli porous structure have been investigated by small-angle neutron scattering (SANS). Tripoli is a finely porous sedimentary rock formed by small spherical opal particles. Its main component is aqueous silica SiO{sub 2} {center_dot} nH{sub 2}O (80-90%). Tripoli is widely used in practice as a working medium for sorption filters and in some other commercial and construction technologies. The shape of the experimental SANS curves indicates the presence of small and large pores in tripoli. The small-pore size was estimated to be {approx}100 Angstrom-Sign . The size of large pores turned out to be beyond the range of neutron wave vector transfers Q that are available for the instrument used; however, their size was indirectly estimated to be {approx}(2000-2500) Angstrom-Sign . The pores of both groups behave as surfacetype fractal scatterers with the fractal dimension D {approx} 2.2-2.6. The densities of pores of these two groups differ by approximately three orders of magnitude ({approx}10{sup 16} and {approx}10{sup 13} cm{sup -3} for small and large pores, respectively); the fraction of large pores amounts to 70-80% of the total pore volume. The found pore characteristics (their densities, sizes, and relative volumes) are in satisfactory agreement (when a comparison is possible) with the absorption data.

  5. Small angle neutron scattering study of fatigue induced grain boundary cavities

    SciTech Connect

    Page, R.; Roth, M.; Weertman, J.R.

    1982-07-01

    Small angle neutron scattering (SANS) has been used to study grain boundary cavitation in high purity copper fatigued at elevated temperatures. SANS is an extremely sensitive method for observing cavities. Void volume fractions of less than 10/sup -6/ can be detected. Analysis of scattering data yields values for the total void volume per unit volume and the total number of voids in a fatigued sample. The size distribution of the voids also can be calculated. From a series of specimens, each fatigued under identical conditions but for varying lengths of time, it is possible to obtain the void nucleation rate and the rate of growth of the total void volume and of the individual voids. Extrapolation of curves of void volume fraction vs time of fatigue to zero time shows that cavitation begins upon commencement of fatiguing without any measurable incubation time. Void nucleation is continuous throughout fatigue Calculated values of the individual void growth rate agree very well, as regards time dependence, temperature dependence, and even absolute value, with growth rates derived from a theory of fatigueinduced cavitation based on transient effects in vacancy diffusion.

  6. Solution Properties of 1,3-Cyclohexadiene Polymers by Small Angle Neutron and Light Scattering

    SciTech Connect

    Yun, Seok I; Melnichenko, Yuri B; Wignall, George D; Hong, Kunlun; Mays, Jimmy; Britt, Phillip F; Terao, Ken; Nakamura, Yo

    2006-01-01

    1,3-Cyclohexdiene polymers (PCHD) and their derivatives are of interest due to the six-member rings in the main chain, which are expected to impart higher mechanical strength and better thermal and chemical stability, as compared to common vinyl polymers. For example, hydrogenated PCHD has the highest glass transition temperature (T{sub g} {approx} 231 C) of all hydrocarbon polymers, and it also shows good heat, weather, impact, abrasion, and chemical resistance as well as low water absorption. In addition, PCHD has unique photochemical properties, such as excellent transparency, due to the isolated double bonds in the main chain. Also, block copolymers containing PCHD show unusual phase separation behavior. For example, a styrene/1,3-CHD block copolymer (PS-b-PCHD) with 50 vol % CHD (1,4/1,2 {approx} 95/5) exhibits a core-shell or hollow cylinder morphology, while a typical styrene/acyclic diene (isoprene or butadiene) block copolymer with similar composition exhibits a lamellar structure. Such phase behavior and many other properties strongly depend on the conformation of the polymer in solution or bulk. However, almost no data have been reported on the conformation of PCHD, probably because of the lack of well-defined and well-characterized samples. Here we report solution properties of PCHD in tetrahydrofuran (THF) and chloroform by multiangle laser light scattering, viscometry, and small-angle neutron scattering (SANS).

  7. Characterization of Athabasca Asphaltenes Separated Physically and Chemically Using Small-Angle X-Ray Scattering

    NASA Astrophysics Data System (ADS)

    Amundarain Hurtado, Jesus Leonardo

    Athabasca asphaltenes were characterized using small-angle X-ray scattering (SAXS) with synchrotron radiation. Two methods were used to separate asphaltenes from Athabasca bitumen. Conventional chemical separation by precipitation with n-pentane, and physical separation realized by passing bitumen through a zirconia membrane with a 20 nm average pore size. The Athabasca permeates and chemically separated samples were dispersed in 1-methylnaphtalene and n-dodecane, with temperature and asphaltene concentration ranges of 50-310 °C and 1-8 wt. %, respectively. Two approaches were also taken in the analysis of the SAXS emissions. A model-independent approach provided radii of gyration and scattering coefficients. A model-dependent fit provided size distributions for asphaltenes aggregates assuming that they are dense and spherical. Physically and chemically separated asphaltenes showed significant differences in nominal size and structure, and their structural properties exhibited different temperature dependencies. The results challenge the merits of using chemically separated asphaltene properties as a basis for asphaltene property prediction in crude oil/bitumen.

  8. New Insights into Pore Characteristics and Hydrocarbon Generation of Shale Using Small-Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Ding, M.; Hartl, M.; Wang, Y.; Hjelm, R.

    2014-12-01

    Pore size, distribution, connectivity, and shape as well as hydrocarbon saturation and composition reflect the history of hydrocarbon maturation and migration. However, characterization of the underlying factors and processes controlling hydrocarbons behavior in tight rocks is extremely limited, especially lacking of direct experimental observations. We have studied the pore characteristics of marine and lacustrine shale from the Erdos basin, China during laboratory pyrolysis using small-angle neutron scattering (SANS). Our SANS results show that scattering intensity of smaller pores (< 20 nm)/larger Q values of shale samples increase systematically as temperature increase during pyrolysis from 250 oC to 600oC (Fig.1a). These results in combination with hydrocarbon fractions measurements during the same process (Fig. 1b) provide a quantitative relation between pore characteristics and hydrocarbons generation. Our results indicate that hydrocarbon expulsion primarily causes the observed changes in smaller pores. They also demonstrate that due to its sensitivity to hydrogen, SANS locates all pores whether the pore is filled or not with hydrocarbons. Thus, SANS is particularly suited for probing hydrocarbon behavior in tight shale reservoirs and the factors that impact their pore dynamics for the petroleum industry.

  9. Resolution of ab initio shapes determined from small-angle scattering

    PubMed Central

    Tuukkanen, Anne T.; Kleywegt, Gerard J.; Svergun, Dmitri I.

    2016-01-01

    Spatial resolution is an important characteristic of structural models, and the authors of structures determined by X-ray crystallography or electron cryo-microscopy always provide the resolution upon publication and deposition. Small-angle scattering of X-rays or neutrons (SAS) has recently become a mainstream structural method providing the overall three-dimensional structures of proteins, nucleic acids and complexes in solution. However, no quantitative resolution measure is available for SAS-derived models, which significantly hampers their validation and further use. Here, a method is derived for resolution assessment for ab initio shape reconstruction from scattering data. The inherent variability of the ab initio shapes is utilized and it is demonstrated how their average Fourier shell correlation function is related to the model resolution. The method is validated against simulated data for proteins with known high-resolution structures and its efficiency is demonstrated in applications to experimental data. It is proposed that henceforth the resolution be reported in publications and depositions of ab initio SAS models. PMID:27840683

  10. Small-angle neutron scattering correlation functions of bulk magnetic materials

    PubMed Central

    Mettus, Denis; Michels, Andreas

    2015-01-01

    On the basis of the continuum theory of micromagnetics, the correlation function of the spin-misalignment small-angle neutron scattering cross section of bulk ferromagnets (e.g. elemental polycrystalline ferromagnets, soft and hard magnetic nanocomposites, nanoporous ferromagnets, or magnetic steels) is computed. For such materials, the spin disorder which is related to spatial variations in the saturation magnetization and magnetic anisotropy field results in strong spin-misalignment scattering dΣM/dΩ along the forward direction. When the applied magnetic field is perpendicular to the incoming neutron beam, the characteristics of dΣM/dΩ (e.g. the angular anisotropy on a two-dimensional detector or the asymptotic power-law exponent) are determined by the ratio of magnetic anisotropy field strength H p to the jump ΔM in the saturation magnetization at internal interfaces. Here, the corresponding one- and two-dimensional real-space correlations are analyzed as a function of applied magnetic field, the ratio H p/ΔM, the single-particle form factor and the particle volume fraction. Finally, the theoretical results for the correlation function are compared with experimental data on nanocrystalline cobalt and nickel. PMID:26500464

  11. Miscibility Study of PCBM/P3EHT Organic Photovoltaics via Small Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Yin, Wen; McCulloch, Bryan; Segalman, Rachel; Dadmun, Mark

    2011-03-01

    Organic photovoltaics (OPV) attracted considerable interest as lightweight, inexpensive, and easily processable replacement of inorganic photovoltaics. Current results indicate that the morphology of these photovoltaic materials is essential to their solar energy conversion efficiency but a detailed and fundamental understanding is absent. In this paper, the miscibility and structure of P3EHT/PCBM composites with varying PCBM loading level are investigated via small angle neutron scattering (SANS). With P3EHT having a melting temperature below 100°C, SANS experiments of the blends are conducted above the melting point to unequivocally determine the miscibility of PCBM and P3EHT without the added complexity of polymer crystals. Our SANS results show that blends with 20 and 50 wt% PCBM exhibit dramatically larger scattering at low-Q regime relative to 10 and 15wt% PCBM samples. This result implies that the miscibility limit of PCBM and P3EHT lies between 15:85 and 20:80. Further analysis is underway to correlate these results to OPV efficiency.

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

    SciTech Connect

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

    2012-02-07

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

  13. Small Angle Neutron-Scattering Studies of the Core Structure of Intact Neurosecretory Vesicles.

    NASA Astrophysics Data System (ADS)

    Krueger, Susan Takacs

    Small angle neutron scattering (SANS) was used to study the state of the dense cores within intact neurosecretory vesicles. These vesicles transport the neurophysin proteins, along with their associated hormones, oxytocin or vasopressin, from the posterior pituitary gland to the bloodstream, where the entire vesicle contents are released. Knowledge of the vesicle core structure is important in developing an understanding of this release mechanism. Since the core constituents exist in a dense state at concentrations which cannot be reproduced (in solution) in the laboratory, a new method was developed to determine the core structure from SANS experiments performed on intact neurosecretory vesicles. These studies were complemented by biochemical assays performed to determine the role, if any, played by phospholipids in the interactions between the core constituents. H_2O/D_2 O ratio in the solvent can be adjusted, using the method of contrast variation, such that the scattering due to the vesicle membranes is minimized, thus emphasizing the scattering originating from the cores. The applicability of this method for examining the interior of biological vesicles was tested by performing an initial study on human red blood cells, which are similar in structure to other biological vesicles. Changes in intermolecular hemoglobin interactions, occurring when the ionic strength of the solvent was varied or when the cells were deoxygenated, were examined. The results agreed with those expected for dense protein solutions, indicating that the method developed was suitable for the study of hemoglobin within the cells. Similar SANS studies were then performed on intact neurosecretory vesicles. The experimental results were inconsistent with model calculations which assumed that the cores consisted of small, densely-packed particles or large, globular aggregates. Although a unique model could not be determined, the data suggest that the core constituents form long aggregates of

  14. Size And Shape of Detergent Micelles Determined By Small-Angle X-Ray Scattering

    SciTech Connect

    Lipfert, Jan; Columbus, Linda; Chu, Vincent B.; Lesley, Scott A.; Doniach, Sebastian; /Stanford U., Phys. Dept. /Stanford U., Appl. Phys. Dept. /SLAC, SSRL /Pasteur Inst., Paris /Scripps Res. Inst. /Novartis Res. Found.

    2009-04-29

    We present a systematic analysis of the aggregation number and shape of micelles formed by nine detergents commonly used in the study of membrane proteins. Small-angle X-ray scattering measurements are reported for glucosides with 8 and 9 alkyl carbons (OG/NG), maltosides and phosphocholines with 10 and 12 alkyl carbons (DM/DDM and FC-10/FC-12), 1,2-dihexanoyl-sn-glycero-phosphocholine (DHPC), 1-palmitoyl-2-hydroxy-sn-glycero-3-[phospho-rac-(1-glycerol)] (LPPG), and 3-[(3-cholamidopropyl)dimethylammonio]-1-propane sulfonate (CHAPS). The SAXS intensities are well described by two-component ellipsoid models, with a dense outer shell corresponding to the detergent head groups and a less electron dense hydrophobic core. These models provide an intermediate resolution view of micelle size and shape. In addition, we show that Guinier analysis of the forward scattering intensity can be used to obtain an independent and model-free measurement of the micelle aggregation number and radius of gyration. This approach has the advantage of being easily generalizable to protein-detergent complexes, where simple geometric models are inapplicable. Furthermore, we have discovered that the position of the second maximum in the scattering intensity provides a direct measurement of the characteristic head group-head group spacing across the micelle core. Our results for the micellar aggregation numbers and dimensions agree favorably with literature values as far as they are available. We de novo determine the shape of FC-10, FC-12, DM, LPPG, and CHAPS micelles and the aggregation numbers of FC-10 and OG to be ca. 50 and 250, respectively. Combined, these data provide a comprehensive view of the determinants of micelle formation and serve as a starting point to correlate detergent properties with detergent-protein interactions.

  15. Screen anticancer drug in vitro using resonance light scattering technique.

    PubMed

    Chen, Zhanguang; Liu, Guoliang; Chen, Meizhen; Xu, Benjie; Peng, Yurui; Chen, Maohuai; Wu, Mingyao

    2009-02-15

    An in vitro screening model using resonance light scattering (RLS) technique with 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide (MTT) reagent as the reactive probe to target cancer cell was firstly developed. In this model, MTT was reduced by viable cancer cells to produce a purple formazan. Cell viability was proportional to the number of formazan induced strong light scattering signal. The inhibition rate of anticancer drug was found to vary inversely with the H(22)-MTT system RLS intensity. So it was intuitive to see the sequence of the tumor suppressive activity of six anticancer drugs without data processing by RLS/MTT screening spectra. Compared with the traditional MTT method, this method has high sensitivity, low detection limit and quite intuitive screening results which were identical to those obtained from the MTT colorimetric assay.

  16. The effect of the shape function on small-angle scattering analysis by the maximum entropy method

    SciTech Connect

    Jemian, P.R.; Allen, A.J. |

    1992-09-15

    Analysis of small-angle scattering data to obtain a particle size distribution is dependent upon the shape function used to model the scattering. Using a maximum entropy analysis of small-angle scattering data, the effect of shape function selection on obtained size distribution is demonstrated using three different shape functions to describe the same scattering data from each of two steels. The alloys have been revealed by electron microscopy to contain a distribution of randomly oriented and mainly non-interacting, irregular, ellipsoidal precipitates. Comparison is made between the different forms of the shape function. Effect of an incident wavelength distribution is also shown. The importance of testing appropriate shape functions and validating these against other microstructural studies is discussed.

  17. Small angle neutron scattering for the structural study of intrinsically disordered proteins in solution: a practical guide.

    PubMed

    Gabel, Frank

    2012-01-01

    Small angle neutron scattering (SANS) allows studying bio-macromolecular structures and interactions in solution. It is particularly well-suited to study structural properties of intrinsically disordered proteins (IDPs) over a wide range of length-scales ranging from global aspects (radii of gyration and molecular weight) down to short-distance properties (e.g., cross-sectional analysis). In this book chapter, we provide a practical guide on how to carry out SANS experiments on IDPs and discuss the complementary aspects and strengths of SANS with respect to small angle X-ray scattering (SAXS).

  18. Multiaxial deformation of polyethylene and polyethylene/clay nanocomposites: In situ synchrotron small angle and wide angle X-ray scattering study

    SciTech Connect

    Gurun, Bilge; Bucknall, David G.; Thio, Yonathan S.; Teoh, Chin Ching; Harkin-Jones, Eileen

    2013-01-10

    A unique in situ multiaxial deformation device has been designed and built specifically for simultaneous synchrotron small angle X-ray scattering (SAXS) and wide angle X-ray scattering (WAXS) measurements. SAXS and WAXS patterns of high-density polyethylene (HDPE) and HDPE/clay nanocomposites were measured in real time during in situ multiaxial deformation at room temperature and at 55 C. It was observed that the morphological evolution of polyethylene is affected by the existence of clay platelets as well as the deformation temperature and strain rate. Martensitic transformation of orthorhombic into monoclinic crystal phases was observed under strain in HDPE, which is delayed and hindered in the presence of clay nanoplatelets. From the SAXS measurements, it was observed that the thickness of the interlamellar amorphous region increased with increasing strain, which is due to elongation of the amorphous chains. The increase in amorphous layer thickness is slightly higher for the nanocomposites compared to the neat polymer.

  19. Onset and Nature of Fracture of Uniaxially Compressed Gun Propellants. A Small Angle Neutron and X-ray Scattering Study

    DTIC Science & Technology

    1993-08-01

    Avogadro constant , Di is the mass density of material i, the sums are over the k atom types in material i, nk is the number of atoms of type k, Wk is the...subsequent analysis. This includes the ability to obtain averages for constant scattering angle (0) as functions of the azimuthal angle (0). If radial...values for the B specimen are plotted against axial orientation with strain level for each curve remaining constant . The general trend indicated is an

  20. Studies of Particle Sedimentation by Novel Scattering Techniques

    NASA Technical Reports Server (NTRS)

    Tong, Penger

    2000-01-01

    The four-year grant began May 1, 1996 (5-1-96 to 4-30-00, $100,000/year). We have finished 4 major research projects and published 10 papers during this grant period. An important aspect of this research has been the education of students at graduate and undergraduate levels. They have been fully involved in the research described below: 1. Polymer-induced depletion interaction in colloid-polymer mixtures. 2. Colloidal sedimentation in polymer solutions. 3. Velocity fluctuations in particle sedimentation. New laser light scattering techniques for velocity difference measurements.

  1. Technique to measure contact angle of micro/nanodroplets using atomic force microscopy

    SciTech Connect

    Jung, Yong Chae; Bhushan, Bharat

    2008-07-15

    Contact angle is the primary parameter that characterizes wetting; however, the measurement techniques have been limited to droplets with a diameter as low as about 50 {mu}m. The authors developed an atomic force microscopy-based technique to measure the contact angle of micro- and nanodroplets deposited using a modified nanoscale dispensing tip. The obtained contact angle results were compared with those of a macrodroplet (2.1 mm diameter). It was found that the contact angle on various surfaces decreases with decreasing the droplet size.

  2. An ultra-high vacuum chamber for scattering experiments featuring in-vacuum continuous in-plane variation of the angle between entrance and exit vacuum ports

    NASA Astrophysics Data System (ADS)

    Englund, Carl-Johan; Agâker, Marcus; Fredriksson, Pierre; Olsson, Anders; Johansson, Niklas; Rubensson, Jan-Erik; Nordgren, Joseph

    2015-09-01

    A concept that enables in-vacuum continuous variation of the angle between two ports in one plane has been developed and implemented. The vacuum chamber allows for measuring scattering cross sections as a function of scattering angle and is intended for resonant inelastic X-ray scattering experiments. The angle between the ports can be varied in the range of 30°-150°, while the pressure change is less than 2 × 10-10 mbars.

  3. An ultra-high vacuum chamber for scattering experiments featuring in-vacuum continuous in-plane variation of the angle between entrance and exit vacuum ports

    SciTech Connect

    Englund, Carl-Johan; Agåker, Marcus Fredriksson, Pierre; Olsson, Anders; Johansson, Niklas; Rubensson, Jan-Erik; Nordgren, Joseph

    2015-09-15

    A concept that enables in-vacuum continuous variation of the angle between two ports in one plane has been developed and implemented. The vacuum chamber allows for measuring scattering cross sections as a function of scattering angle and is intended for resonant inelastic X-ray scattering experiments. The angle between the ports can be varied in the range of 30°-150°, while the pressure change is less than 2 × 10{sup −10} mbars.

  4. A summary of the low angle x-ray atomic scattering factors which have been measured by the critical voltage effect in High Energy Electron Diffraction (HEED)

    SciTech Connect

    Fox, A.G.; Fisher, R.M.

    1987-08-01

    A tabulated summary of all the accurate (/approximately/0.1%) low-angle x-ray atomic scattering (form) factors which have been determined by the systematic critical voltage technique in HEED is presented. For low atomic number elements (Z/approx lt/40) the low angle form factors can be significantly different to best free atom values, and so the best band structure calculated and/or x-ray measured form factors consistent with the critical voltage measurements are also indicated. At intermediate atomic numbers Zapprox. =40..-->..50 only the very low-angle form factors appear to be different to the best free atom values, and even then only by a small amount. For heavy elements (Z/approx lt/70) the best free atom form factors appear to agree very closely with the critical voltage measured values and so, in this case, critical voltage measurements give very accurate measurements of Debye-Waller factors. 48 refs.

  5. Structure of spontaneously formed solid-electrolyte interphase on lithiated graphite determined using small-angle neutron scattering

    DOE PAGES

    Sacci, Robert L.; Banuelos, Jose Leobardo; Veith, Gabriel M.; ...

    2015-03-25

    We report the first small-angle neutron scattering of a chemically formed solid-electrolyte interphase from LixC6 reacting with ethylene carbonate/dimethyl carbon solvent. This provides a different and perhaps simpler view of SEI formation than the usual electrochemically-driven reaction. We show that an organic layer coats the graphite particles filling in micro-pores and is polymeric in nature being 1-3 nm thick. We used inelastic neutron scattering to probe the chemistry, and we found that the SEI showed similar inelastic scattering to polyethylene oxide.

  6. A recoil detector for the measurement of antiproton-proton elastic scattering at angles close to 90°

    NASA Astrophysics Data System (ADS)

    Hu, Q.; Bechstedt, U.; Gillitzer, A.; Grzonka, D.; Khoukaz, A.; Klehr, F.; Lehrach, A.; Prasuhn, D.; Ritman, J.; Sefzick, T.; Stockmanns, T.; Täschner, A.; Wuestner, P.; Xu, H.

    2014-10-01

    The design and construction of a recoil detector for the measurement of recoil protons of antiproton-proton elastic scattering at scattering angles close to are described. The performance of the recoil detector has been tested in the laboratory with radioactive sources and at COSY with proton beams by measuring proton-proton elastic scattering. The results of laboratory tests and commissioning with beam are presented. Excellent energy resolution and proper working performance of the recoil detector validate the conceptual design of the KOALA experiment at HESR to provide the cross section data needed to achieve a precise luminosity determination at the PANDA experiment.

  7. Small-angle neutron scattering data on C{sub 60} clusters in weakly polar solutions of fullerenes

    SciTech Connect

    Tropin, T. V. Avdeev, M. V.; Aksenov, V. L.

    2007-05-15

    Solutions of fullerence C{sub 60} in carbon disulfide CS{sub 2} have been investigated by small-angle neutron scattering. Combination of solubility, contrast, and incoherent scattering make it possible to measure and analyze the relatively small scattering cross section of this system. Along with single fullerene molecules, a small amount of large fullerene clusters (more than 100 A in size) is found in these solutions. The formation of these clusters depends on the procedure of solution preparation. The size distribution functions of clusters are compared with the results of the phenomenological cluster model of fullerene solubility.

  8. High-speed reference-beam-angle control technique for holographic memory drive

    NASA Astrophysics Data System (ADS)

    Yamada, Ken-ichiro; Ogata, Takeshi; Hosaka, Makoto; Fujita, Koji; Okuyama, Atsushi

    2016-09-01

    We developed a holographic memory drive for next-generation optical memory. In this study, we present the key technology for achieving a high-speed transfer rate for reproduction, that is, a high-speed control technique for the reference beam angle. In reproduction in a holographic memory drive, there is the issue that the optimum reference beam angle during reproduction varies owing to distortion of the medium. The distortion is caused by, for example, temperature variation, beam irradiation, and moisture absorption. Therefore, a reference-beam-angle control technique to position the reference beam at the optimum angle is crucial. We developed a new optical system that generates an angle-error-signal to detect the optimum reference beam angle. To achieve the high-speed control technique using the new optical system, we developed a new control technique called adaptive final-state control (AFSC) that adds a second control input to the first one derived from conventional final-state control (FSC) at the time of angle-error-signal detection. We established an actual experimental system employing AFSC to achieve moving control between each page (Page Seek) within 300 µs. In sequential multiple Page Seeks, we were able to realize positioning to the optimum angles of the reference beam that maximize the diffracted beam intensity. We expect that applying the new control technique to the holographic memory drive will enable a giga-bit/s-class transfer rate.

  9. A planar Mie scattering visualization technique for turbo machinery application

    NASA Astrophysics Data System (ADS)

    Gawehn, Thomas; Schodl, Richard

    2007-12-01

    A planar Mie scattering technique is described which allows for the systematical analysis of three-dimensional shock configurations without the need for velocity measurements. For that, small particles are added to the flow upstream of the shock and illuminated by a laser light sheet. The scattered light is captured by a CCD camera so that the position of the shock wave can be determined from the increase of the light intensity across the shock. To analyze the three-dimensional structure of a shock wave, the light sheet is moved perpendicular to the flow direction. The measurement technique is applied to both a supersonic wedge flow at Ma = 2.43 and a more complex shock wave configuration in a transonic cascade flow at Ma = 1.09. The gathered results are conclusive with Schlieren photographs, numerical simulations and surface pressure measurements. As the chosen setup allows the application to test sections with restricted optical access and a synchronization of the image capturing process with an external triggering signal, the three-dimensional shock configurations inside a transonic compressor rotor can also be visualized.

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

    SciTech Connect

    Settens, Charles M.

    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.

  11. A mobile system for a comprehensive online-characterization of nanoparticle aggregates based on wide-angle light scattering and laser-induced incandescence.

    PubMed

    Huber, Franz J T; Altenhoff, Michael; Will, Stefan

    2016-05-01

    A mobile demonstrator for the comprehensive online-characterization of gas-borne nanoparticle aggregates is presented. Two optical measurement techniques are combined, both utilizing a pulsed Nd:YAG laser as light source. Aggregate size and fractal dimension are measured by Wide-Angle Light Scattering (WALS). An ellipsoidal mirror images elastically scattered light from scattering angles between 10° and 165° onto a CCD-camera chip resulting in an almost complete scattering diagram with high angular resolution. Primary particle size and volume fraction are measured by time-resolved Laser-Induced Incandescence (TiRe-LII). Here, particles are heated up to about 3000 K by the short laser pulse, the enhanced thermal radiation signal is detected with gated photomultiplier tubes. Analysis of the signal decay time and maximum LII-signal allows for the determination of primary particle diameter and volume fraction. The performance of the system is demonstrated by combined measurements on soot nanoparticle aggregates from a soot aerosol generator. Particle and aggregate sizes are varied by using different equivalence ratios of the combustion in the generator. Soot volume fraction can be adjusted by different levels of dilution with air. Online-measurements were carried out demonstrating the favorable performance of the system and the potential for industrial applications such as process control and product development. The particle properties obtained are confirmed through transmission electron microscopy analysis on representative samples.

  12. A mobile system for a comprehensive online-characterization of nanoparticle aggregates based on wide-angle light scattering and laser-induced incandescence

    NASA Astrophysics Data System (ADS)

    Huber, Franz J. T.; Altenhoff, Michael; Will, Stefan

    2016-05-01

    A mobile demonstrator for the comprehensive online-characterization of gas-borne nanoparticle aggregates is presented. Two optical measurement techniques are combined, both utilizing a pulsed Nd:YAG laser as light source. Aggregate size and fractal dimension are measured by Wide-Angle Light Scattering (WALS). An ellipsoidal mirror images elastically scattered light from scattering angles between 10° and 165° onto a CCD-camera chip resulting in an almost complete scattering diagram with high angular resolution. Primary particle size and volume fraction are measured by time-resolved Laser-Induced Incandescence (TiRe-LII). Here, particles are heated up to about 3000 K by the short laser pulse, the enhanced thermal radiation signal is detected with gated photomultiplier tubes. Analysis of the signal decay time and maximum LII-signal allows for the determination of primary particle diameter and volume fraction. The performance of the system is demonstrated by combined measurements on soot nanoparticle aggregates from a soot aerosol generator. Particle and aggregate sizes are varied by using different equivalence ratios of the combustion in the generator. Soot volume fraction can be adjusted by different levels of dilution with air. Online-measurements were carried out demonstrating the favorable performance of the system and the potential for industrial applications such as process control and product development. The particle properties obtained are confirmed through transmission electron microscopy analysis on representative samples.

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

    SciTech Connect

    Chen, Lingling

    1996-04-01

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

  14. Analysis of the data from Compton X-ray polarimeters which measure the azimuthal and polar scattering angles

    NASA Astrophysics Data System (ADS)

    Krawczynski, H.

    2011-05-01

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

  15. Carbide precipitates in solution-quenched PH13-8 Mo stainless steel: A small-angle neutron scattering investigation

    NASA Astrophysics Data System (ADS)

    Sen, D.; Patra, A. K.; Mazumder, S.; Mittra, J.; Dey, G. K.; de, P. K.

    2004-08-01

    This paper deals with the small-angle neutron scattering (SANS) investigation on solution-quenched PH13-8 Mo stainless steel. From the nature of the variation of the functionality of the profiles for varying specimen thickness and also from the transmission electron microscopy (TEM), it has been established that the small-angle scattering signal predominantly originates from the block-like metallic carbide precipitates in the specimen. The contribution due to double Bragg reflection is not significant in the present case. The single scattering profile has been extracted from the experimental profiles corresponding to different values of specimen thickness. In order to avoid complexity and non-uniqueness of the multi-parameter minimization for randomly oriented polydisperse block-like precipitate model, the data have been analyzed assuming randomly oriented polydisperse cylindrical particle model with a locked aspect ratio.

  16. The new small-angle neutron scattering instrument SANS-1 at MLZ-characterization and first results

    NASA Astrophysics Data System (ADS)

    Mühlbauer, S.; Heinemann, A.; Wilhelm, A.; Karge, L.; Ostermann, A.; Defendi, I.; Schreyer, A.; Petry, W.; Gilles, R.

    2016-10-01

    A thorough characterization of the key features of the new small-angle neutron scattering instrument SANS-1 at MLZ, a joint project of Technische Universität München and Helmholtz Zentrum Geesthacht, is presented. Measurements of the neutron beam profile, divergency and flux are given for various positions along the instrument including the sample position, and agree well with Monte Carlo simulations of SANS-1 using the program McStas. Secondly, the polarization option of SANS-1 is characterized for a broad wavelength band. A key feature of SANS-1 is the large accessible Q-range facilitated by the sideways movement of the detector. Particular attention is hence paid to the effects that arise due to large scattering angles on the detector where a standard cos3 solid angle correction is no longer applicable. Finally the performance of the instrument is characterized by a set of standard samples.

  17. Evolution of the pore structure during the early stages of the alkali-activation reaction: An in situ small-angle neutron scattering investigation

    DOE PAGES

    White, Claire E.; Olds, Daniel P.; Hartl, Monika; ...

    2017-02-01

    The long-term durability of cement-based materials is influenced by the pore structure and associated permeability at the sub-micrometre length scale. With the emergence of new types of sustainable cements in recent decades, there is a pressing need to be able to predict the durability of these new materials, and therefore nondestructive experimental techniques capable of characterizing the evolution of the pore structure are increasingly crucial for investigating cement durability. Here, small-angle neutron scattering is used to analyze the evolution of the pore structure in alkali-activated materials over the initial 24 h of reaction in order to assess the characteristic poremore » sizes that emerge during these short time scales. By using a unified fitting approach for data modeling, information on the pore size and surface roughness is obtained for a variety of precursor chemistries and morphologies (metakaolin- and slag-based pastes). Furthermore, the impact of activator chemistry is elucidatedviathe analysis of pastes synthesized using hydroxide- and silicate-based activators. It is found that the main aspect influencing the size of pores that are accessible using small-angle neutron scattering analysis (approximately 10–500 Å in diameter) is the availability of free silica in the activating solution, which leads to a more refined pore structure with smaller average pore size. Furthermore, as the reaction progresses the gel pores visible using this scattering technique are seen to increase in size.« less

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

    PubMed Central

    Rambo, Robert P.; Tainer, John A.

    2010-01-01

    Defining the shape, conformation, or assembly state of an RNA in solution often requires multiple investigative tools ranging from nucleotide analog interference mapping to X-ray crystallography. A key addition to this toolbox is small-angle X-ray scattering (SAXS). SAXS provides direct structural information regarding the size, shape, and flexibility of the particle in solution and has proven powerful for analyses of RNA structures with minimal requirements for sample concentration and volumes. In principle, SAXS can provide reliable data on small and large RNA molecules. In practice, SAXS investigations of RNA samples can show inconsistencies that suggest limitations in the SAXS experimental analyses or problems with the samples. Here, we show through investigations on the SAM-I riboswitch, the Group I intron P4-P6 domain, 30S ribosomal subunit from Sulfolobus solfataricus (30S), brome mosaic virus tRNA-like structure (BMV TLS), Thermotoga maritima asd lysine riboswitch, the recombinant tRNAval, and yeast tRNAphe that many problems with SAXS experiments on RNA samples derive from heterogeneity of the folded RNA. Furthermore, we propose and test a general approach to reducing these sample limitations for accurate SAXS analyses of RNA. Together our method and results show that SAXS with synchrotron radiation has great potential to provide accurate RNA shapes, conformations, and assembly states in solution that inform RNA biological functions in fundamental ways. PMID:20106957

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

    PubMed Central

    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. PMID:25615859

  20. Search for small-angle neutron scattering in MnO at 1700K

    SciTech Connect

    Routbort, J.L.; Epperson, J.E.; Klippert, T.E.; Goretta, K.C.

    1986-01-01

    A preliminary small-angle scattering (SANS) experiment has been performed on MnO single crystal at the Intense Pulsed Neutron Source. The experiment was preformed at 1700/sup 0/K at oxygen partial pressures of 2.2 x 10/sup -4/, 1 x 10/sup 2/, and 2 x 10/sup 2/ Pa, which resulted in deviations from stoichiometry of about 0.0015, 0.082, and 0.127. No statistically significant change in SANS was observed at this temperature with the pressure changes. Neither was any significant change observed in the wavelength-dependent sample transmission, also measured in-situ as a function of pressure. Therefore, either clustering of cation vacancies is negligible in MnO for these conditions, or the clusters are smaller than about 5 A. Of proposed cluster configurations, only the existence of the smallest (4:1, 6:2, or possible 8:3) appears to be consistent with these results.

  1. Structure parameters of synaptic vesicles quantified by small-angle x-ray scattering.

    PubMed

    Castorph, Simon; Riedel, Dietmar; Arleth, Lise; Sztucki, Michael; Jahn, Reinhard; Holt, Matthew; Salditt, Tim

    2010-04-07

    Synaptic vesicles (SVs) are small, membrane-bound organelles that are found in the synaptic terminal of neurons, and which are crucial in neurotransmission. After a rise in internal [Ca(2+)] during neuronal stimulation, SVs fuse with the plasma membrane releasing their neurotransmitter content, which then signals neighboring neurons. SVs are subsequently recycled and refilled with neurotransmitter for further rounds of release. Recently, tremendous progress has been made in elucidating the molecular composition of SVs, as well as putative protein-protein interactions. However, what is lacking is an empirical description of SV structure at the supramolecular level-which is necessary to enable us to fully understand the processes of membrane fusion, retrieval, and recycling. Using small-angle x-ray scattering, we have directly investigated the size and structure of purified SVs. From this information, we deduced detailed size and density parameters for the protein layers responsible for SV function, as well as information about the lipid bilayer. To achieve a convincing model fit, a laterally anisotropic structure for the protein shell is needed, as a rotationally symmetric density profile does not explain the data. Not only does our model confirm many of the preexisting ideas concerning SV structure, but also for the first time, to our knowledge, it indicates structural refinements, such as the presence of protein microdomains.

  2. Comparative analysis of the nucleosome structure of cell nuclei by small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Isaev-Ivanov, V. V.; Lebedev, D. V.; Lauter, H.; Pantina, R. A.; Kuklin, A. I.; Islamov, A. Kh.; Filatov, M. V.

    2010-05-01

    The nucleosome structure in native nuclei of normal (chicken erythrocyte and rat leukocyte nuclei) and anomalously proliferating (the human cervical adenocarcinoma cell line HeLa and the Chinese hamster fibroblast cell line A238) cells has been investigated using small-angle neutron scattering. The experimental results obtained allow one to make the inference that the parameters of the nucleosome structure for the chicken erythrocyte and rat leukocyte nuclei (on average over the nucleus) are close to the universally accepted values and that the distance distribution function is bimodal. The bimodality of the distance distribution function reflects a narrow distribution of distances between nucleosomes (on average over the nucleus) at the fibril level of the chromatin organization. The histone core of the nucleosome structure in the nuclei of the HeLa and A238 cells (on average over the nucleus) is considerably less compact than that in the chicken erythrocyte and rat leukocyte nuclei, and the distance distribution function does not exhibit indications of the bimodality.

  3. Modeling and small-angle neutron scattering spectra of chromatin supernucleosomal structures at genome scale

    NASA Astrophysics Data System (ADS)

    Ilatovskiy, Andrey V.; Lebedev, Dmitry V.; Filatov, Michael V.; Grigoriev, Mikhail; Petukhov, Michael G.; Isaev-Ivanov, Vladimir V.

    2011-11-01

    Eukaryotic genome is a highly compacted nucleoprotein complex organized in a hierarchical structure based on nucleosomes. Detailed organization of this structure remains unknown. In the present work we developed algorithms for geometry modeling of the supernucleosomal chromatin structure and for computing distance distribution functions and small-angle neutron scattering (SANS) spectra of the genome-scale (˜106 nucleosomes) chromatin structure at residue resolution. Our physical nucleosome model was based on the mononucleosome crystal structure. A nucleosome was assumed to be rigid within a local coordinate system. Interface parameters between nucleosomes can be set for each nucleosome independently. Pair distance distributions were computed with Monte Carlo simulation. SANS spectra were calculated with Fourier transformation of weighted distance distribution; the concentration of heavy water in solvent and probability of H/D exchange were taken into account. Two main modes of supernucleosomal structure generation were used. In a free generation mode all interface parameters were chosen randomly, whereas nucleosome self-intersections were not allowed. The second generation mode (generation in volume) enabled spherical or cubical wall restrictions. It was shown that calculated SANS spectra for a number of our models were in general agreement with available experimental data.

  4. Percolating bulk-heterostructures from neutron reflectometry and small angle scattering data

    NASA Astrophysics Data System (ADS)

    Olds, Daniel; Duxbury, Phillip

    2013-03-01

    We present a novel algorithm for efficiently calculating the simulated small angle scattering data of any discretized morphological model of arbitrary scale and resolution, referred to as the distribution function method (DFM). Unlike standard SAS fitting methods, the DFM algorithm allows for the calculation of form factors and structure factors from complex nanoscale morphologies commonly encountered in many modern polymeric and nanoparticle based systems, which have no exact analytical corollary. The computational efficiency of the DFM algorithm suggests it's use in morphological model refinement. We will present a number of simple examples to demonstrate the accuracy and limits of the algorithm, followed by an example of incorporation of the DFM algorithm into reverse Monte Carlo structural refinement of bulk-heterojunction two-phase morphologies, such as those commonly found in organic photovoltaic devices. We will show that morphological features introduced via direct incorporation of experimental neutron reflectometry and SANS data to the models has a direct effect on the results of device simulations. The authors thank CORE-CM at Michigan State University for it's funding of this research.

  5. Small-angle light scattering by airborne particulates: Environnement S.A. continuous particulate monitor

    NASA Astrophysics Data System (ADS)

    Renard, Jean-Baptiste; Thaury, Claire; Mineau, Jean-Luc; Gaubicher, Bertrand

    2010-08-01

    Airborne particulate matter may have an effect on human health. It is therefore necessary to determine and control in real time the evolution of the concentration and mass of particulates in the ambient air. These parameters can be obtained using optical methods. We propose here a new instrument, 'CPM' (continuous particulate monitor), for the measurement of light scattered by ambient particulates at small angles. This geometry allows simultaneous and separate detections of PM10, PM2.5 and PM1 fractions of airborne particulate matter, with no influence of their chemical nature and without using theoretical calculations. The ambient air is collected through a standard sampling head (PM10 inlet according to EN 12341, PM2.5 inlet according to EN 14907; or PM1, TSP inlets, standard US EPA inlets). The analysis of the first measurements demonstrates that this new instrument can detect, for each of the seven defined size ranges, real-time variations of particulate content in the ambient air. The measured concentrations (expressed in number per liter) can be converted into total mass concentrations (expressed in micrograms per cubic meter) of all fractions of airborne particulate matters sampled by the system. Periodic comparison with a beta-attenuation mass monitor (MP101M Beta Gauge Analyzer from Environnement S.A. company) allows the calculation of a calibration factor as a function of the mean particulate density that is used for this conversion. It is then possible to provide real-time relative variations of aerosol mass concentration.

  6. Small-angle neutron scattering study of radiation-induced defects in synthetic quartz

    SciTech Connect

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

    2006-12-15

    The supraatomic structure of single crystals of synthetic quartz was studied by thermal neutron small-angle scattering in the initial state (dislocation densities 54 and 570 cm{sup -2}) and after irradiation in the WWR-M reactor (Petersburg Nuclear Physics Institute) by fast neutrons with energies E{sub n} > 0.1 MeV at fluences F{sub n} = 0.2 x 10{sup 17} -5 x 10{sup 18} neutrons/cm{sup 2}. It is established that fast neutrons form point, linear, and volume defects in the lattice throughout the entire volume of a sample. Large-volume structures-amorphous-phase nuclei-reach sizes of {approx}100 nm in quartz, while occupying a small total volume of {approx}0.3% even at the maximum fluence 5 x 10{sup 18} neutrons/cm{sup 2}. The main fraction of the damaged volume (up to 5%) corresponds to point (with a radius of gyration of 1-2 nm) and linear defects, giving a comparable contribution ({approx}1-4%). The extended linear structures with a radius of 2 nm, even at a moderate fluence of 7.7 x 10{sup 17} neutrons/cm{sup 2}, have a significant total length per volume unit ({approx}10{sup 11} cm/cm{sup 3}) and can form a connected network with a cell {approx}30 nm in size in the sample. Foreign atoms and molecules can migrate through channels of this network.

  7. Nature of radiation defects in synthetic quartz according to the small-angle neutron scattering data

    SciTech Connect

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

    2007-05-15

    The supraatomic structure of single crystals of synthetic quartz in the initial state with a dislocation density of 570 cm{sup -2} and after irradiation in the VVR-M reactor at the Petersburg Nuclear Physics Institute with fast neutrons having the energy E{sub n} > 1 MeV in the range of fluences F{sub n} = 7.7 x 10{sup 17} -2.1 x 10{sup 20} neutrons/cm{sup 2} has been studied by small-angle scattering of thermal neutrons. It is established that fast neutrons form point, linear, and volume lattice defects throughout the entire sample volume. Large-volume structures (nuclei of the amorphous phase) in quartz, reaching {approx}100 nm in size, occupy a small total volume ({approx}1.5%) even at the maximum fluence 2.1 x 10{sup 20} neutrons/cm{sup 2}. The majority of damage is related to the point defects with the radius of gyration of 1-2 nm and linear defects, which give comparable contributions up to several percent.

  8. Pore distributions in nanocrystalline metals from small-angle neutron scattering

    SciTech Connect

    Sanders, P.G.; Weertman, J.R.; Eastman, J.A.

    1998-07-24

    Recent upgrades in inert-gas condensation processing equipment have produced nanocrystalline metal samples with high densities and low-impurity levels. Typical Cu and Pd samples have densities {ge}98% of theoretical and oxygen and hydrogen impurity concentrations {le}0.5 at. %. Lower porosity and impurity levels may make it difficult to produce and maintain samples with the smallest nanocrystalline grain sizes. These improved samples were studied by small-angle neutron scattering (SANS) to determine the volume fraction and size distribution of pores. Excellent correlation was obtained between the total volume fraction of pores and the Archimedes density for Pd, signifying that most of the pores were relatively small and in the detectability range of SANS ({approx}1--100 nm). Nanocrystalline Cu is shown to exhibit a wider pore size distribution. For Pd, the average pore sizes were slightly smaller than the average grain size, while for Cu the pore size and grain size were about the same. Both materials exhibited a trend of increasing pore size with increasing grain size. In terms of processing prerequisites, the principal condition for the production of high-density nanocrystalline Cu is an exceptionally clean synthesis environment, while nanocrystalline Pd requires compaction at elevated temperatures. These differences are the result of Cu having both a lower melting point and a greater susceptibility to contamination by gaseous impurities such as oxygen.

  9. Conformational Changes and Flexibility of DNA Devices Observed by Small-Angle X-ray Scattering.

    PubMed

    Bruetzel, Linda K; Gerling, Thomas; Sedlak, Steffen M; Walker, Philipp U; Zheng, Wenjun; Dietz, Hendrik; Lipfert, Jan

    2016-08-10

    Self-assembled DNA origami nanostructures enable the creation of precisely defined shapes at the molecular scale. Dynamic DNA devices that are capable of switching between defined conformations could afford completely novel functionalities for diagnostic, therapeutic, or engineering applications. Developing such objects benefits strongly from experimental feedback about conformational changes and 3D structures, ideally in solution, free of potential biases from surface attachment or labeling. Here, we demonstrate that small-angle X-ray scattering (SAXS) can quantitatively resolve the conformational changes of a DNA origami two-state switch device as a function of the ionic strength of the solution. In addition, we show how SAXS data allow for refinement of the predicted idealized three-dimensional structure of the DNA object using a normal mode approach based on an elastic network model. The results reveal deviations from the idealized design geometries that are otherwise difficult to resolve. Our results establish SAXS as a powerful tool to investigate conformational changes and solution structures of DNA origami and we anticipate our methodology to be broadly applicable to increasingly complex DNA and RNA devices.

  10. Structural formation of huntingtin-like aggregates probed by small-angle neutron scattering

    SciTech Connect

    Stanley, Christopher B; Perevozchikova, Tatiana; Berthelier-Jung, Valerie M

    2011-01-01

    In several neurodegenerative disorders, including Huntington s disease (HD), aspects concerning the earliest of protein structures that form along the aggregation pathway have increasingly gained attention since these particular species are likely to be neurotoxic. We used time-resolved small-angle neutron scattering (SANS) to probe in solution these transient structures formed by peptides having the N-terminal sequence context of mutant huntingtin (Htt) exon 1. We obtained snapshots of the formed aggregates as the kinetic reaction ensued to yield quantitative information on their size and mass. At the early stage, small precursor species with an initial radius of gyration (Rg) of 16.1 5.9 and average mass of a dimer to trimer were monitored. Structural growth was treated as two modes with a transition from three-dimensional early aggregate formation to two-dimensional fibril growth and association. Our SANS results on the internal structure of the mature fibrils demonstrate loose packing with about 1 peptide per 4.75 -sheet repeat distance, which is shown to be quantitatively consistent with a -helix model. This research provides new insights into the structures forming along the pathway of Htt exon 1 aggregation and should assist in determining the role that precursors play in neuronal toxicity.

  11. Synchrotron radiation small angle scattering studies of d(TTAGGG)4 oligomer in solution

    NASA Astrophysics Data System (ADS)

    Kozak, Maciej; Wlodarczyk, Agnieszka; Dobek, Andrzej

    2009-10-01

    Telomeric DNA sequences play a crucial role in maintaining chromosome stability and integrity. In human chromosomes telomeres are composed of tandem (TTAGGG)n repeats. The structural parameters and low-resolution structure of a synthetic d(TTAGGG)4 oligomer in solution has been studied in the absence and in the presence of potassium cations, with the use of the small angle scattering of synchrotron radiation. The radii of gyration RG, calculated for d(TTAGGG)4 oligomer (in 10 mM Tris/HCl pH 7.3) was 1.42 nm, while RG, (in 10 mM Tris/HCl pH 7.3; 0.1 mM KCl) was 1.32 nm. The pair distance distribution function, P(r), yielded a maximum dimension of 4.55and 4.35 nm for solutions in the absence and the presence of potassium cations. On the basis of SAXS data, the low-resolution structure in solution has been reconstructed using ab inito methods.

  12. Use of anomalous small angle x-ray scattering to investigate microstructural features in complex alloys

    SciTech Connect

    Weertman, J.R.

    1990-08-01

    The research thrust has been directed into two areas. The principal effort has been spent in an investigation of the use of anomalous small angle x-ray scattering (ASAXS) to observe changes in the microstructure of a relatively complex alloy produced by high temperature deformation or aging. A second effort involves a study of the high temperature behavior of several ferritic steels. In particular, we are investigating the precursors and earliest stages of fatigue crack initiation, especially how initiation is affected by hold times and by environment. We have been studying carbides in two ferritic steel alloys. The first is Fe9CrlMo modified by the addition of small amounts of the strong carbide formers, V and Nb. This alloy, which has been studied at ORNL and in the course of this grant, is used in power-generating equipment. The second alloy is AF1410 (primarily Fel4Col0Ni), an ultra high-strength, high toughness steel. 8 figs.,

  13. Insight into asphaltene nanoaggregate structure inferred by small angle neutron and X-ray scattering.

    PubMed

    Eyssautier, Joëlle; Levitz, Pierre; Espinat, Didier; Jestin, Jacques; Gummel, Jérémie; Grillo, Isabelle; Barré, Loïc

    2011-06-02

    Complementary neutron and X-ray small angle scattering results give prominent information on the asphaltene nanostructure. Precise SANS and SAXS measurements on a large q-scale were performed on the same dilute asphaltene-toluene solution, and absolute intensity scaling was carried out. Direct comparison of neutron and X-ray spectra enables description of a fractal organization made from the aggregation of small entities of 16 kDa, exhibiting an internal fine structure. Neutron contrast variation experiments enhance the description of this nanoaggregate in terms of core-shell disk organization, giving insight into core and shell dimensions and chemical compositions. The nanoaggregates are best described by a disk of total radius 32 Å with 30% polydispersity and a height of 6.7 Å. Composition and density calculations show that the core is a dense and aromatic structure, contrary to the shell, which is highly aliphatic. These results show a good agreement with the general view of the Yen model (Yen, T. F.; et al. Anal. Chem.1961, 33, 1587-1594) and as for the modified Yen model (Mullins, O. C. Energy Fuels2010, 24, 2179-2207), provide characteristic dimensions of the asphaltene nanoaggregate in good solvent.

  14. Interactive graphical system for small-angle scattering analysis of polydisperse systems

    NASA Astrophysics Data System (ADS)

    Konarev, P. V.; Volkov, V. V.; Svergun, D. I.

    2016-09-01

    A program suite for one-dimensional small-angle scattering analysis of polydisperse systems and multiple data sets is presented. The main program, POLYSAS, has a menu-driven graphical user interface calling computational modules from ATSAS package to perform data treatment and analysis. The graphical menu interface allows one to process multiple (time, concentration or temperature-dependent) data sets and interactively change the parameters for the data modelling using sliders. The graphical representation of the data is done via the Winteracter-based program SASPLOT. The package is designed for the analysis of polydisperse systems and mixtures, and permits one to obtain size distributions and evaluate the volume fractions of the components using linear and non-linear fitting algorithms as well as model-independent singular value decomposition. The use of the POLYSAS package is illustrated by the recent examples of its application to study concentration-dependent oligomeric states of proteins and time kinetics of polymer micelles for anticancer drug delivery.

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

    DOE PAGES

    Grant, Thomas D.; Luft, Joseph R.; Carter, Lester G.; ...

    2015-01-23

    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 targetsmore » for which high-resolution structures have been determined via X-ray crystallography or nuclear magnetic resonance (NMR) spectroscopy. 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.« less

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

    SciTech Connect

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

    2015-01-23

    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. 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.

  17. Ensemble Activation of G-Protein -Coupled Receptors Revealed by Small-Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Chu, Xiang-Qiang; Perera, Suchithranga; Shrestha, Utsab; Chawla, Udeep; Struts, Andrey; Qian, Shuo; Brown, Michael

    2014-03-01

    Rhodopsin is a G-protein -coupled receptor (GPCR) involved in visual light perception and occurs naturally in a membrane lipid environment. Rhodopsin photoactivation yields cis-trans isomerization of retinal giving equilibrium between inactive Meta-I and active Meta-II states. Does photoactivation lead to a single Meta-II conformation, or do substates exist as described by an ensemble-activation mechanism (EAM)? We use small-angle neutron scattering (SANS) to investigate conformational changes in rhodopsin-detergent and rhodopsin-lipid complexes upon photoactivation. Meta-I state is stabilized in CHAPS-solubilized rhodopsin, while Meta-II is trapped in DDM-solubilized rhodopsin. SANS data are acquired from 80% D2O solutions and at contrast-matching points for both DDM and CHAPS samples. Our experiments demonstrate that for detergent-solubilized rhodopsin, SANS with contrast variation can detect structural differences between the rhodopsin dark-state, Meta-I, Meta-II, and ligand-free opsin states. Dark-state rhodopsin has more conformational flexibility in DDM micelles compared to CHAPS, which is consistent with an ensemble of activated Meta-II states. Furthermore, time-resolved SANS enables study of the time-dependent structural transitions between Meta-I and Meta-II, which is crucial to understanding the ensemble-based activation.

  18. Small-Angle Neutron Scattering and Spontaneous Formation of Unilamellar Vesicles: Potential Vehicles for Drug Delivery

    NASA Astrophysics Data System (ADS)

    Katsaras, John

    2004-03-01

    Unilamellar vesicles (ULVs) are single-bilayer shells with radii commonly between 10 and 100 nm, and are widely used as model membranes, drug delivery systems, microreactors and substrates for a variety of enzymes and proteins. A common method of making ULVs is the extrusion of multilamellar vesicles (MLVs) through synthetic membranes of known pore size. These extruded ULVs are invariably unstable and in due time, revert back to MLVs. Over the years there have been reports of the spontaneous formation of stable ULVs in surfactant, lipid, and lipid/detergent mixtures. These ULVs have sometimes been shown to be monodisperse and their radii were found, almost without exception, to vary with concentration. We have carried-out small-angle neutron scattering (SANS) experiments on a biomimetic system composed of the phospholipids dimyristoyl and dihexanoyl phosphorylcholine (DMPC and DHPC, respectively). Doping DMPC/DHPC multilamellar vesicles with either the negatively charged lipid dimyristoyl phosphorylglycerol (DMPG, net charge -1) or the divalent cation, calcium (Ca2+) leads to the spontaneous formation of monodisperse unilamellar vesicles whose radii are concentration independent, in contrast to previous experimental observations.

  19. Small Angle Neutron Scattering Reveals pH-dependent Conformational Changes in Trichoderma reesei Cellobiohydrolase I

    PubMed Central

    Pingali, Sai Venkatesh; O'Neill, Hugh M.; McGaughey, Joseph; Urban, Volker S.; Rempe, Caroline S.; Petridis, Loukas; Smith, Jeremy C.; Evans, Barbara R.; Heller, William T.

    2011-01-01

    Cellobiohydrolase I (Cel7A) of the fungus Trichoderma reesei (now classified as an anamorph of Hypocrea jecorina) hydrolyzes crystalline cellulose to soluble sugars, making it of key interest for producing fermentable sugars from biomass for biofuel production. The activity of the enzyme is pH-dependent, with its highest activity occurring at pH 4–5. To probe the response of the solution structure of Cel7A to changes in pH, we measured small angle neutron scattering of it in a series of solutions having pH values of 7.0, 6.0, 5.3, and 4.2. As the pH decreases from 7.0 to 5.3, the enzyme structure remains well defined, possessing a spatial differentiation between the cellulose binding domain and the catalytic core that only changes subtly. At pH 4.2, the solution conformation of the enzyme changes to a structure that is intermediate between a properly folded enzyme and a denatured, unfolded state, yet the secondary structure of the enzyme is essentially unaltered. The results indicate that at the pH of optimal activity, the catalytic core of the enzyme adopts a structure in which the compact packing typical of a fully folded polypeptide chain is disrupted and suggest that the increased range of structures afforded by this disordered state plays an important role in the increased activity of Cel7A through conformational selection. PMID:21784865

  20. Microstructure of 3D-Printed Polymer Composites Investigated by Small-Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Kang, Tae Hui; Compton, Brett G.; Heller, William T.; Urban, Voker S.; Duty, Chad E.; Do, Changwoo

    Polymer composites printed from the large scale printer at Manufacturing Demonstration Facility at Oak Ridge National Laboratory have been investigated by small-angle neutron scattering (SANS). For the Acrylonitrile Butadiene Styrene (ABS)/Carbon Fiber (CF) composites, the microstructure of polymer domains and the alignment of CF have been characterized across the layer from the printed piece. CF shows strong anisotropic alignment along the printing direction due to the flow of polymer melt at the nozzle. Order parameter of the anisotropy which ranges from -0.11 to -0.06 exhibits strong correlation with the position within the layer: stronger alignment near the layer interface. It is also confirmed that the existence of CF reduces the polymer domain correlation length significantly and reinforces the mechanical strength of the polymer composites. For the Epoxy/nano-clay platelet composites, the effect of processing condition, nozzle size, and the addition of the another filler, Silicon Carbide (SC), have been investigated by SANS. Nano-clay platelet shows strong anisotropic alignment along the printing direction as well. Order parameter of the anisotropy varies according to nozzle size and presence of the SC, and difference disappears at high Q region. Scientific User Facilities Division and Materials Sciences and Energy Division, Office of Basic Energy Sciences, U.S. Department of Energy.

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

    PubMed Central

    Skou, Magda; Skou, Søren; Jensen, Thomas G.; Vestergaard, Bente; Gillilan, Richard E.

    2014-01-01

    Owing to the demand for low sample consumption and automated sample changing capabilities at synchrotron small-angle X-ray (solution) scattering (SAXS) beamlines, X-ray microfluidics is receiving continuously increasing attention. Here, a remote-controlled microfluidic device is presented for simultaneous SAXS and ultraviolet absorption measurements during protein dialysis, integrated directly on a SAXS beamline. Microfluidic dialysis can be used for monitoring structural changes in response to buffer exchange or, as demonstrated, protein concentration. By collecting X-ray data during the concentration procedure, the risk of inducing protein aggregation due to excessive concentration and storage is eliminated, resulting in reduced sample consumption and improved data quality. The proof of concept demonstrates the effect of halted or continuous flow in the microfluidic device. No sample aggregation was induced by the concentration process at the levels achieved in these experiments. Simulations of fluid dynamics and transport properties within the device strongly suggest that aggregates, and possibly even higher-order oligomers, are preferentially retained by the device, resulting in incidental sample purification. Hence, this versatile microfluidic device enables investigation of experimentally induced structural changes under dynamically controllable sample conditions. PMID:25242913

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

    SciTech Connect

    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.

  3. Small Angle Neutron Scattering (SANS) Studies on the Structural Evolution of Pyromellitamide Self-assembled Gels

    SciTech Connect

    Scott, Jamieson; Tong, Katie; William, Hamilton; He, Lilin; James, Michael; Thordarson, Pall; Boukhalfa, Sofiane

    2014-10-31

    The kinetics of aggregation of two pyromellitamide gelators; tetrabutyl- (C4) and tetrahexylpyromellitamide (C6), in deuterated cyclohexane has been investigated by small angle neutron scattering (SANS) for up to six days. The purpose of this study was to improve our understanding of how self-assembled gels are formed. Short-term (< 3 hour) time scales revealed multiple phases with the data for the tetrabutylpyromellitamide C4 indicating one dimensional stacking and aggregation corresponding to a multi-fiber braided cluster arrangement that is about 35 Å in diameter. The corresponding tetrahexylpyromellitamide C6 data suggests that the C6 also forms one-dimensional stacks but that these aggregate to a thicker multi-fiber braided cluster that have a diameter of 61.8 Å. Over a longer period of time, the radius, persistence length and contour length all continue to increase in 6 days after cooling. This data suggests that structural changes in self-assembled gels occur over a period exceeding several days and that fairly subtle changes in the structure (e.g. tail-length) can influence the packing of molecules in self-assembled gels on the single-to-few fiber bundle stage.

  4. Small Angle Neutron Scattering (SANS) Studies on the Structural Evolution of Pyromellitamide Self-assembled Gels

    DOE PAGES

    Scott, Jamieson; Tong, Katie; William, Hamilton; ...

    2014-10-31

    The kinetics of aggregation of two pyromellitamide gelators; tetrabutyl- (C4) and tetrahexylpyromellitamide (C6), in deuterated cyclohexane has been investigated by small angle neutron scattering (SANS) for up to six days. The purpose of this study was to improve our understanding of how self-assembled gels are formed. Short-term (< 3 hour) time scales revealed multiple phases with the data for the tetrabutylpyromellitamide C4 indicating one dimensional stacking and aggregation corresponding to a multi-fiber braided cluster arrangement that is about 35 Å in diameter. The corresponding tetrahexylpyromellitamide C6 data suggests that the C6 also forms one-dimensional stacks but that these aggregate tomore » a thicker multi-fiber braided cluster that have a diameter of 61.8 Å. Over a longer period of time, the radius, persistence length and contour length all continue to increase in 6 days after cooling. This data suggests that structural changes in self-assembled gels occur over a period exceeding several days and that fairly subtle changes in the structure (e.g. tail-length) can influence the packing of molecules in self-assembled gels on the single-to-few fiber bundle stage.« less

  5. Small-angle neutron scattering reveals a pH-dependent conformational change in cellobiohydrolase I

    SciTech Connect

    Pingali, Sai Venkatesh; O'Neill, Hugh Michael; McGaughey, Joseph; Urban, Volker S; Myles, Dean A A; Petridis, Loukas; Smith, Jeremy C; Evans, Barbara R; Heller, William T

    2011-01-01

    Cellobiohydrolase I (Cel7A) of the fungus Trichoderma reesei (now classified as an anamorph of Hypocrea jecorina) hydrolyzes crystalline cellulose to soluble sugars, making it of key interest for producing fermentable sugars from biomass for biofuel production. The activity of the enzyme is pH-dependent, with its highest activity occurring at pH 4-5. To probe the response of the solution structure of Cel7A to changes in pH, we measured small angle neutron scattering of it in a series of solutions having pH values of 7.0, 6.0, 5.3, and 4.2. As the pH decreases from 7.0 to 5.3, the enzyme structure remains well defined, possessing a spatial differentiation between the cellulose binding domain and the catalytic core that only changes subtly. At pH 4.2, the solution conformation of the enzyme changes to a structure that is intermediate between a properly folded enzyme and a denatured, unfolded state, yet the secondary structure of the enzyme is essentially unaltered. The results indicate that at the pH of optimal activity, the catalytic core of the enzyme adopts a structure in which the compact packing typical of a fully folded polypeptide chain is disrupted and suggest that the increased range of structures afforded by this disordered state plays an important role in the increased activity of Cel7A through conformational selection.

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

    NASA Astrophysics Data System (ADS)

    Howell, Steven C.

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

  7. Modeling the Structure of RNA Molecules with Small-Angle X-Ray Scattering Data

    PubMed Central

    Gajda, Michal Jan; Martinez Zapien, Denise; Uchikawa, Emiko; Dock-Bregeon, Anne-Catherine

    2013-01-01

    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. PMID:24223750

  8. Investigation of the interaction of dimethyl sulfoxide with lipid membranes by small-angle neutron scattering

    SciTech Connect

    Gorshkova, J. E. Gordeliy, V. I.

    2007-05-15

    The influence of dimethyl sulfoxide (CH{sub 3}){sub 2}SO (DMSO) on the structure of membranes of 1,2-dimiristoyl-sn-glycero-3-phosphatidylcholine (DMPC) in an excess of a water-DMSO solvent is investigated over a wide range of DMSO molar concentrations 0.0 {<=} X{sub DMSO} {<=} 1.0 at temperatures T = 12.5 and 55 deg. C. The dependences of the repeat distance d of multilamellar membranes and the thickness d{sub b} of single vesicles on the molar concentration X{sub DMSO} in the L{sub {beta}}{sub '} gel and L{sub {alpha}} liquid-crystalline phases are determined by small-angle neutron scattering. The intermembrane distance d{sub s} is determined from the repeat distance d and the membrane thickness d{sub b}. It is shown that an increase in the molar concentration X{sub DMSO} leads to a considerable decrease in the intermembrane distance and that, at X{sub DMSO} = 0.4, the neighboring membranes are virtually in steric contact with each other. The use of the deuterated phospholipid (DMSO-D6) and the contrast variation method makes it possible, for the first time, to determine the number of DMSO molecules strongly bound to the membrane.

  9. Molecular weight-gyration radius relation of globular proteins: a comparison of light scattering, small-angle X-ray scattering and structure-based data.

    PubMed

    Smilgies, Detlef-M; Folta-Stogniew, Ewa

    2015-10-01

    The molecular weight-gyration radius relation for a number of globular proteins based on experimental light scattering data is compared with small-angle X-ray scattering data recently published by Mylonas & Svergun [J. Appl. Cryst. (2007 ▸), 40, s245-s249]. In addition, other recent experimental data and theoretical calculations are reviewed. It is found that the MW-Rg relation for the globular proteins is well represented by a power law with an exponent of 0.37 (2).

  10. Method to study sample object size limit of small-angle x-ray scattering computed tomography

    NASA Astrophysics Data System (ADS)

    Choi, Mina; Ghammraoui, Bahaa; Badal, Andreu; Badano, Aldo

    2016-03-01

    Small-angle x-ray scattering (SAXS) imaging is an emerging medical tool that can be used for in vivo detailed tissue characterization and has the potential to provide added contrast to conventional x-ray projection and CT imaging. We used a publicly available MC-GPU code to simulate x-ray trajectories in a SAXS-CT geometry for a target material embedded in a water background material with varying sample sizes (1, 3, 5, and 10 mm). Our target materials were water solution of gold nanoparticle (GNP) spheres with a radius of 6 nm and a water solution with dissolved serum albumin (BSA) proteins due to their well-characterized scatter profiles at small angles and highly scattering properties. The background material was water. Our objective is to study how the reconstructed scatter profile degrades at larger target imaging depths and increasing sample sizes. We have found that scatter profiles of the GNP in water can still be reconstructed at depths up to 5 mm embedded at the center of a 10 mm sample. Scatter profiles of BSA in water were also reconstructed at depths up to 5 mm in a 10 mm sample but with noticeable signal degradation as compared to the GNP sample. This work presents a method to study the sample size limits for future SAXS-CT imaging systems.

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

    NASA Astrophysics Data System (ADS)

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

    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.

  12. DARA: a web server for rapid search of structural neighbours using solution small angle X-ray scattering data

    PubMed Central

    Kikhney, Alexey G.; Panjkovich, Alejandro; Sokolova, Anna V.; Svergun, Dmitri I.

    2016-01-01

    Motivation: Small angle X-ray scattering (SAXS) is an established method for studying biological macromolecules in solution, whereby the experimental scattering patterns relate to the quaternary and tertiary structure of the macromolecule. Here we present DARA, a web-server, that queries over 150 000 scattering profiles pre-computed from the high resolution models of macromolecules and biological assemblies in the Protein Data Bank, to rapidly find nearest neighbours of a given experimental or theoretical SAXS pattern. Identification of the best scattering equivalents provides a straightforward and automated way of structural assessment of macromolecules based on a SAXS profile. DARA results are useful e.g. for fold recognition and finding of biologically active oligomers. Availability and implementation: http://dara.embl-hamburg.de/ Contact: svergun@embl-hamburg.de PMID:26504146

  13. Deformation of poly(methyl methacrylate)-poly(ethylene oxide) blends: a molecular characterization by small-angle neutron scattering

    SciTech Connect

    Lefebvre, J.M.R.; Porter, S.; Wignall, G.D.

    1986-01-01

    The deformation behavior of miscible amorphous/amorphous PMMA/PEO blends has been compared to that of pure PMMA. Small-angle neutron scattering experiments have been performed on labeled systems made of PEO + D-PMMA + H-PMMA. Characteristic molecular parameters such as radius of gyration R/sub g/, molecular weight M/sub w/ and interaction parameter X have been extracted from the coherent scattering cross sections. Molecular anisotropy is measured on the solid state coextruded samples and the observed drawing efficiency is compared to the results of shrinkage tests. In the case of PMMA/PEO blends, anomalous scattering behavior precludes any quantitative interpretation of the scattering patterns, but revealed important structural changes upon drawing, namely a deformation-induced phase separation.

  14. Coherent Rayleigh-Brillouin scattering as a flow diagnostic technique

    SciTech Connect

    Graul, J. S.; Lilly, T. C.

    2014-12-09

    Broadband coherent Rayleigh-Brillouin scattering (CRBS) was used to measure translational gas temperatures for nitrogen at the ambient pressure of 0.8 atm using a purpose-built Fabry-Perot etalon spectrometer. Temperatures derived from the CRBS spectral analysis were compared with experimentally-measured temperatures, and were found to be, on average, within 2% of the experimentally-measured value. Axial flow velocities from a double jet at a pressure ratio of 0.38 were also measured by looking at the Doppler shift of the CRBS line shape. With recent developments in chirped laser technology and the capacity of CRBS to simultaneously provide thermodynamic and bulk flow information, the CRBS line shape acquisition and analysis technique presented here may allow for future time-resolved, characterization of aerospace flows.

  15. Guanidine hydrochloride denaturation of dopamine-induced α-synuclein oligomers: a small-angle X-ray scattering study.

    PubMed

    Pham, Chi L L; Kirby, Nigel; Wood, Kathleen; Ryan, Timothy; Roberts, Blaine; Sokolova, Anna; Barnham, Kevin J; Masters, Colin L; Knott, Robert B; Cappai, Roberto; Curtain, Cyril C; Rekas, Agata

    2014-01-01

    Alpha-synuclein (α-syn) forms the amyloid-containing Lewy bodies found in the brain in Parkinson's disease. The neurotransmitter dopamine (DA) reacts with α-syn to form SDS-resistant soluble, non-amyloid, and melanin-containing oligomers. Their toxicity is debated, as is the nature of their structure and their relation to amyloid-forming conformers of α-syn. The small-angle X-ray scattering technique in combination with modeling by the ensemble optimization method showed that the un-reacted native protein populated three broad classes of conformer, while reaction with DA gave a restricted ensemble range suggesting that the rigid melanin molecule played an important part in their structure. We found that 6 M guanidine hydrochloride did not dissociate α-syn DA-reacted dimers and trimers, suggesting covalent linkages. The pathological significance of covalent association is that if they are non-toxic, the oligomers would act as a sink for toxic excess DA and α-syn; if toxic, their stability could enhance their toxicity. We argue it is essential, therefore, to resolve the question of whether they are toxic or not.

  16. Positron Annihilation Spectroscopy and Small Angle Neutron Scattering Characterization of Nanostructural Features in Irradiated Fe-Cu-Mn Alloys

    SciTech Connect

    Wirth, B D; Asoka-Kumar, P; Howell, R H; Odette, G R; Sterne, P A

    2001-01-01

    Radiation embrittlement of nuclear reactor pressure vessel steels results from a high number density of nanometer sized Cu-Mn-Ni rich precipitates (CRPs) and sub-nanometer matrix features, thought to be vacancy-solute cluster complexes (VSC). However, questions exist regarding both the composition of the precipitates and the defect character and composition of the matrix features. We present results of positron annihilation spectroscopy (PAS) and small angle neutron scattering (SANS) characterization of irradiated and thermally aged Fe-Cu and Fe-Cu-Mn alloys. These complementary techniques provide insight into the composition and character of both types of nanoscale features. The SANS measurements indicate populations of CRPs and VSCs in both alloys. The CRPs are coarser in the Fe-Cu alloy and the number densities of CRP and VSC increase with the addition of Mn. The PAS involved measuring both the positron lifetimes and the Doppler broadened annihilation spectra in the high momentum region to provide elemental sensitivity at the annihilation site. The spectra in Fe-Cu-Mn specimens thermally aged to peak hardness at 450 C and irradiated at 288 C are nearly identical to elemental Cu. Positron lifetime and spectrum measurements in Fe-Cu specimens irradiated at 288 C clearly show the existence of long lifetime ({approx}500 ps) open volume defects, which also contain Cu. Thus the SANS and PAS provide a self-consistent picture of nanostructures composed of CRPs and VSCs and tend to discount high Fe concentrations in the CRPs.

  17. Small angle neutron scattering study of sodium dodecyl sulfate micellar growth driven by addition of a hydrotropic salt.

    PubMed

    Hassan, P A; Fritz, Gerhard; Kaler, Eric W

    2003-01-01

    The structures of aggregates formed in aqueous solutions of an anionic surfactant, sodium dodecyl sulfate (SDS), with the addition of a cationic hydrotropic salt, p-toluidine hydrochloride (PTHC), have been investigated by small angle neutron scattering (SANS). The SANS spectra exhibit a pronounced peak at low salt concentration, indicating the presence of repulsive intermicellar interactions. Model-independent real space information about the structure is obtained from a generalized indirect Fourier transformation (GIFT) technique in combination with a suitable model for the interparticle structure factor. The interparticle interaction is captured using the rescaled mean spherical approximation (RMSA) closure relation and a Yukawa form of the interaction potential. Further quantification of the geometrical parameters of the micelles was achieved by a complete fit of the SANS data using a prolate ellipsoidal form factor and the RMSA structure factor. The present study shows that PTHC induces a decrease in the fractional charge of the micelles due to adsorption at the micellar surface and consequent growth of the SDS micelles from nearly globular to rodlike as the concentration of PTHC increases.

  18. Aluminum Nitride Grown by Atomic Layer Epitaxy Characterized with Real-Time Grazing Incidence Small Angle X-ray Scattering

    NASA Astrophysics Data System (ADS)

    Anderson, Virginia; Nepal, Neeraj; Johnson, Scooter; Robinson, Zachary; Demasi, Alexander; Hite, Jennifer; Ludwig, Karl; Eddy, Charles

    Aluminum nitride, gallium nitride, and indium nitride are being considered for many applications, and are currently being used commercially for LEDs. These III-nitride films are conventionally deposited by metalorganic chemical vapor deposition and molecular beam epitaxy. Research into depositing III-nitrides with atomic layer epitaxy (ALE) is underway as it is a fabrication friendly technique for thin films at lower temperatures. AlN deposited with ALE at 500°C have been shown to have good crystallinity, but relatively high carbon and oxygen impurities, and understanding the film deposition mechanism is an ongoing project. Grazing incidence small angle x-ray scattering (GISAXS) is sensitive to surface features, making it useful for real time monitoring of deposition processes. AlN was monitored by GISAXS while being deposited with ALE using trimethylaluminum and hydrogen/nitrogen plasma at the Brookhaven National Synchrotron Light Source and the Cornell High Energy Synchrotron Source. The GISAXS of AlN ALE at nominally 400°C, 450°C, and 500°C was compared to ex situ characterization with XPS and AFM.

  19. Kinetics of copper growth on graphene revealed by time-resolved small-angle x-ray scattering

    NASA Astrophysics Data System (ADS)

    Hodas, M.; Siffalovic, P.; Jergel, M.; Pelletta, M.; Halahovets, Y.; Vegso, K.; Kotlar, M.; Majkova, E.

    2017-01-01

    Metal growth on graphene has many applications. Transition metals are known to favor three-dimensional (3D) cluster growth on graphene. Copper is of particular interest for cost-effective surface-supported catalysis applications and as a contact material in electronics. This paper presents an in situ real-time study of Cu growth kinetics on graphene covering all stages preceding formation of a continuous film performed by laboratory-based grazing-incidence small-angle x-ray scattering (GISAXS) technique. In particular, nucleation and 3D cluster growth, coalescence, and percolation stages were identified. The cluster nucleation saturates after reaching a density of 1012c m-2 at ≈1 monolayer thickness. A Kratky plot and a paracrystal model with cumulative structural disorder were necessary to evaluate properly cluster growth and coalescence, respectively. The power law scaling constants 0.27 ±0.05 and 0.81 ±0.02 of the temporal evolution of Cu cluster size suggest the growth of isolated clusters and dynamic cluster coalescence keeping the cluster shape, respectively. Coalescence and percolation thresholds occur at Cu thicknesses of 2 ±0.4 and 8.8 ±0.7 nm , respectively. This paper demonstrates the potential of laboratory-based in situ GISAXS as a vital diagnostic tool for tailoring a large variety of Cu nanostructures on graphene based on an in situ Cu growth monitoring which is applicable in a broad range of deposition times.

  20. Structural Evolution of Polylactide Molecular Bottlebrushes: Kinetics Study by Size Exclusion Chromatography, Small Angle Neutron Scattering and Simulations

    SciTech Connect

    Pickel, Deanna L; Kilbey, II, S Michael; Uhrig, David; Hong, Kunlun; Carrillo, Jan-Michael Y; Sumpter, Bobby G; Ahn, Suk-Kyun; Han, Youngkyu; Kim, Dr. Tae-Hwan; Smith, Gregory Scott; Do, Changwoo

    2014-01-01

    Structural evolution from poly(lactide) (PLA) macromonomer to resultant PLA molecular bottlebrush during ring opening metathesis polymerization (ROMP) was investigated for the first time by combining size exclusion chromatography (SEC), small-angle neutron scattering (SANS) and coarse-grained molecular dynamics (CG-MD) simulations. Multiple aliquots were collected at various reaction times during ROMP, and subsequently analyzed by SEC and SANS. The two complementary techniques enable the understanding of systematic changes in conversion, molecular weight and dispersity as well as structural details of PLA molecular bottlebrushes. CG-MD simulation not only predicts the experimental observations, but it also provides further insight into the analysis and interpretation of data obtained in SEC and SANS experiments. We find that PLA molecular bottlebrushes undergo three conformational transitions with increasing conversion (i.e., increasing the backbone length): (1) from an elongated to a globular shape due to longer side chain at lower conversion, (2) from a globular to an elongated shape at intermediate conversion caused by excluded volume of PLA side chain, and (3) the saturation of contour length at higher conversion due to chain transfer reactions.

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

    NASA Astrophysics Data System (ADS)

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

    2016-11-01

    The structural features of polyacrylonitrile and pitch-based carbon fibers were analyzed from a comprehensive point of view by X-ray measurements and related techniques. The results indicated that the undulating graphite ribbon with embedded microvoid was the main structural unit for graphitic fibers. The void's parameters for these fibers could be obtained directly by small-angle X-ray scattering following the classic method deduced based on the typical two-phase system (i.e., Porod's law, Guinier's law and Debye's law). The non-graphitic fibers, however, were composed of two-dimensional turbostratic crystallites in the aggregation of microfibril and thus had a quasi two-phase structure (microfibril, interfibrillar amorphous structure and microvoid embedded within the microfibril). The extended Debye or Beaucage model in this case should be applied in order to obtain the structural parameters. It also revealed that the quasi two-phase system would complete its transformation to two-phase system during high-temperature graphitization. Therefore, the degree of graphitization was speculated to be the essential indicator distinguishing graphitic fibers from non-graphitic ones and would be helpful in understanding the transformation of structural features during the graphitization of carbon fibers.

  2. Structural characterization of irreversibly adsorbed polymer layers at the polymer/solid interface - In-situ grazing incidence angle x-ray scattering studies

    NASA Astrophysics Data System (ADS)

    Jiang, Naisheng; Chen, Fen; Chen, Xiameng; Han, Zexi; Liang, Chen; Gin, Peter; Asada, Mitsunori; Endoh, Maya; Koga, Tad

    2012-02-01

    In recent years, great attention has been paid to irreversibly adsorbed polymer layers formed on solid substrates since they can modify various properties of polymeric materials confined at the nanometer scale. In this talk, by the combined use of in-situ grazing incidence small angle x-ray scattering and x-ray reflectivity techniques, we aim to characterize the detailed structures of the adsorbed layers composed of different homopolymers (polystyrene, polybutadiene, poly (ethylene oxide), and poly (methyl methacrylate)) prepared on silicon substrates. We will highlight the generality/differences in the structures, leading to a better understanding of the formation process of the adsorbed layers at the impenetrable solid interfaces.

  3. Investigation of the structure of unilamellar dimyristoylphosphatidylcholine vesicles in aqueous sucrose solutions by small-angle neutron and X-ray scattering

    SciTech Connect

    Kiselev, M. A. Zemlyanaya, E. V.; Zhabitskaya, E. I.; Aksenov, V. L.

    2015-01-15

    The structure of a polydispersed population of unilamellar dimyristoylphosphatidylcholine (DMPC) vesicles in sucrose solutions has been investigated by small-angle neutron scattering (SANS) and small-angle X-ray scattering (SAXS). Calculations within the model of separated form factors (SFF) show that the structure of the vesicle system depends strongly on the sucrose concentration.

  4. A method for determining transmembrane helix association and orientation in detergent micelles using small angle x-ray scattering.

    PubMed Central

    Bu, Z; Engelman, D M

    1999-01-01

    Solution small angle x-ray scattering can be used to study the association of transmembrane proteins solubilized in detergent micelles. We have used the alpha-helical transmembrane domain of the human erythrocyte glycophorin A (GpA) fused to the carboxyl terminus of monomeric staphylococcal nuclease (SN/GpA) as a model system for study. By matching the average electron density of the detergent micelles to that of the buffer solution, the micelle contribution to the small angle scattering vanishes, and the molecular weight and the radius of gyration of the proteins can be determined. SN/GpA has been found to dimerize in a zwitterionic detergent micelle, N-dodecyl-N,N-(dimethylammonio)butyrate (DDMAB), whose average electron density naturally matches the electron density of an aqueous buffer. The dimerization occurs through the transmembrane domains of GpA. With the aid of the nuclease domain scattering, the orientation of the helices within a dimer can be determined to be parallel by radius of gyration analysis. The association constant of a mutant (G83I) that weakens the GpA dimerization has been determined to be 24 microM in the DDMAB environment. The experimental methods established here could be used to apply solution small angle x-ray scattering to studying the association and interactions of other membrane proteins. PMID:10423450

  5. Ultra small angle x-ray scattering in complex mixtures of triacylglycerols

    NASA Astrophysics Data System (ADS)

    Peyronel, Fernanda; Quinn, Bonnie; Marangoni, Alejandro G.; Pink, David A.

    2014-11-01

    Ultra-small angle x-ray scattering (USAXS) has been used to elucidate, in situ, the aggregation structure of unsheared model edible oils. Each system comprised one or two solid lipids and a combination of liquid lipids. The 3D nano- to micro-structures of each system were characterized. The length scale investigated, using the Bonse-Hart camera at beamline ID-15D at the Advanced Photon Source, ANL, ranged from 300 Å-10 µm. Using the Unified Fit model, level-1 analysis showed that the scatterers were 2D objects with either a smooth, a rough, or a diffuse surface. These 2D objects had an average radius of gyration Rg1 between 200-1500 Å. Level-2 analysis displayed a slope between -1 and -2. Use of the Guinier-Porod model gave s ≈ 1 thus showing that it was cylinders (TAGwoods) aggregating with fractal dimension 1 ≤ D2 ≤ 2. D2 = 1 is consistent with 1D structures formed from TAGwoods, while D2 = 2 implies that the TAGwoods had formed structures characteristic of diffusion or reaction limited cluster-cluster aggregation (DLCA/RLCA). These aggregates exhibited radii of gyration, Rg2, between 2500 and 6500 Å. Level-3 analyses showed diffuse surfaces, for most of the systems. These interpretations are in accord with theoretical models which studied crystalline nano-platelets (CNPs) coated with nano-scale layers arising from phase separation at the CNP surfaces. These layers could be due to either liquid-liquid phase separation with the CNPs coated, uniformly or non-uniformly, by a diffuse layer of TAGs, or solid-liquid phase separation with the CNPs coated by a rough layer of crystallites. A fundamental understanding of the self-organizing structures arising in these systems helps advance the characterization of fat crystal networks from nanometres to micrometres. This research can be used to design novel fat structures that use healthier fats via nano- and meso-scale structural engineering.

  6. Focused-ion-beam-fabricated homogeneous acute-angled Au nanorods for surface-enhanced Raman scattering

    NASA Astrophysics Data System (ADS)

    Sivashanmugan, Kundan; Liao, Jiunn-Der; Haochih Liu, Bernard

    2015-05-01

    Well-ordered acute-angled Au nanorod (NR) arrays were fabricated using a focused ion beam (FIB) (fibAu_NR). The angle between the NRs and the substrate was tilted at 30-90°. A fibAu_NR with an angle of less than 90° significantly increased the effect of surface-enhanced Raman scattering, which was evaluated using low-concentration rose bengal (<10-5 M) as the molecular test probe. The results show that an angled NR surface produces a strong local electromagnetic effect owing to a large number of Raman active sites. In addition, an optimized fibAu_NR was found to distinguish cyanuric acid in milk solution with good reproducibility.

  7. Contact angle hysteresis on polymer substrates established with various experimental techniques, its interpretation, and quantitative characterization.

    PubMed

    Bormashenko, Edward; Bormashenko, Yelena; Whyman, Gene; Pogreb, Roman; Musin, Albina; Jager, Rachel; Barkay, Zahava

    2008-04-15

    The effect of contact angle hysteresis (CAH) was studied on various polymer substrates with traditional and new experimental techniques. The new experimental technique presented in the article is based on the slow deformation of the droplet, thus CAH is studied under the constant volume of the drop in contrast to existing techniques when the volume of the drop is changed under the measurement. The energy of hysteresis was calculated in the framework of the improved Extrand approach. The advancing contact angle established with a new technique is in a good agreement with that measured with the needle-syringe method. The receding angles measured with three experimental techniques demonstrated a very significant discrepancy. The force pinning the triple line responsible for hysteresis was calculated.

  8. The effect of chiropractic techniques on the Cobb angle in idiopathic scoliosis arising in adolescence.

    PubMed

    Byun, Sunghak; Han, Dongwook

    2016-04-01

    [Purpose] The purpose of this study was to examine whether chiropractic techniques would reduce the curvature of idiopathic scoliosis, which commonly occurs in elementary school children. [Subjects] The subjects of this study were 5 healthy elementary students who listened to an explanation of the study methods and purpose of the study and agreed to participate in the experiment. [Methods] The Cobb angle was measured by taking an X-ray (FCT-1, Dongmun, Goyangsi, Republic of Korea) taken from the rear, using X-ray film. The method of intervention this study used was application of chiropractic techniques. Spinal correction was carried out for 30 minutes per session, which included soft tissue massage, 3 times a week for 8 weeks. [Results] It was established that the Cobb angle was noticeably decreased after 4 weeks of the intervention. Post Hoc analysis revealed that the Cobb angle noticeably decreased after 4 weeks compared with the Cobb angle before the chiropractic techniques were applied. However, no significant difference in Cobb angle was evident after the fourth week. [Conclusion] This study demonstrated that chiropractic techniques can effectively reduce the Cobb angle within as little as 4 weeks. So, we can confirm that the chiropractic techniques were effective for reducing the curvature of idiopathic scoliosis.

  9. The effect of chiropractic techniques on the Cobb angle in idiopathic scoliosis arising in adolescence

    PubMed Central

    Byun, Sunghak; Han, Dongwook

    2016-01-01

    [Purpose] The purpose of this study was to examine whether chiropractic techniques would reduce the curvature of idiopathic scoliosis, which commonly occurs in elementary school children. [Subjects] The subjects of this study were 5 healthy elementary students who listened to an explanation of the study methods and purpose of the study and agreed to participate in the experiment. [Methods] The Cobb angle was measured by taking an X-ray (FCT-1, Dongmun, Goyangsi, Republic of Korea) taken from the rear, using X-ray film. The method of intervention this study used was application of chiropractic techniques. Spinal correction was carried out for 30 minutes per session, which included soft tissue massage, 3 times a week for 8 weeks. [Results] It was established that the Cobb angle was noticeably decreased after 4 weeks of the intervention. Post Hoc analysis revealed that the Cobb angle noticeably decreased after 4 weeks compared with the Cobb angle before the chiropractic techniques were applied. However, no significant difference in Cobb angle was evident after the fourth week. [Conclusion] This study demonstrated that chiropractic techniques can effectively reduce the Cobb angle within as little as 4 weeks. So, we can confirm that the chiropractic techniques were effective for reducing the curvature of idiopathic scoliosis. PMID:27190435

  10. Changes of creatine kinase structure upon ligand binding as seen by small-angle scattering

    NASA Astrophysics Data System (ADS)

    Forstner, Michael; Kriechbaum, Manfred; Laggner, Peter; Wallimann, Theo

    1996-09-01

    Small-angle X-ray and neutron scattering have been used to investigate structural changes upon binding of individual substrates or a transition state analogue complex (TSAC), consisting of Mg-ADP, creatine and KNO 3 to creatine kinase isoenzymes (dimeric M-CK and octameric Mi-CK) and monomeric arginine kinase (AK). Considerable changes in the shape and the size of the molecules occurred upon binding of Mg-ATP and TSAC, whereas creatine alone had only a small effect. In Mi-CK, the radius of gyration was reduced from 55.6 Å (free enzyme) to 48.9 Å (enzyme + Mg-ATP) and to 48.2 Å (enzyme + TSAC). The experiments performed with M-CK showed similar changes from 28.0 Å (free enzyme) to 25.6 Å (enzyme + Mg-ATP) and to 25.5 Å (enzyme + TSAC). Creatine alone did not lead to significant changes in the radii of gyration, nor did free ATP or ADP. AK showed the same behaviour: a change of the radius of gyration from 21.5 Å (free enzyme) to 19.7 Å (enzyme + MG-ATP), whereas with arginine alone only a minor change could be observed. The primary change in structure as seen with monomeric AK seems to be a magnesium-nucleotide induced domain movement relative to each other, whereas the effect of substrate may be of local order only. In creatine kinase, however, further movements must be involved in the large conformational change.

  11. Small-angle neutron scattering study of structure and kinetics of temperature-induced protein gelation.

    PubMed

    Chodankar, S; Aswal, V K; Kohlbrecher, J; Vavrin, R; Wagh, A G

    2009-02-01

    The phase diagram, structural evolution, and kinetics of temperature-induced protein gelation of protein Bovine Serum Albumin (BSA) have been studied as a function of solution pH and protein concentration. The protein gelation temperature represents the onset of turbidity in the protein solution, which increases significantly with increasing pH beyond the isoelectric pH of the protein molecule. On the other hand, the gelation temperature decreases with an increase in protein concentration only in the low-protein-concentration regime and shows a small increasing trend at higher protein concentrations. The structural evolution and kinetics of protein gelation have been studied using small-angle neutron scattering. The structure of the protein molecule remains stable up to temperatures very close to the gelation temperature. On increasing the temperature above the gelation temperature, the protein solution exhibits a fractal structure, an indication of gel formation due to aggregation. The fractal dimension of the gel increases with increasing temperature, suggesting an increase in branching between the aggregates, which leads to stronger gels. The increase in both solution pH and protein concentration is found to delay the growth in the fractal structure and its saturation. The kinetics of gelation has been studied using the temperature-jump process of heating. It is found that the structure of the protein gels remains invariant after the heating time ( approximately 1 min), indicating a rapid formation of gel structure within this time. The protein gels prepared through gradual and temperature-jump heating routes do not always show the same structure. In particular, at higher temperatures (e.g., 85 degrees C ), while gradual heating shows a fractal structure, there is collapse of such fractal structure during temperature-jump heating.

  12. Small-angle neutron scattering studies of hemoglobin confined inside silica tubes of varying sizes.

    PubMed

    Mandal, Soumit S; Cristiglio, Viviana; Lindner, Peter; Bhattacharyya, Aninda J

    2014-02-03

    In addition to the chemical nature of the surface, the dimensions of the confining host exert a significant influence on confined protein structures; this results in immense biological implications, especially those concerning the enzymatic activities of the protein. This study probes the structure of hemoglobin (Hb), a model protein, confined inside silica tubes with pore diameters that vary by one order of magnitude (≈20-200 nm). The effect of confinement on the protein structure is probed by comparison with the structure of the protein in solution. Small-angle neutron scattering (SANS), which provides information on protein tertiary and quaternary structures, is employed to study the influence of the tube pore diameter on the structure and configuration of the confined protein in detail. Confinement significantly influences the structural stability of Hb and the structure depends on the Si-tube pore diameter. The high radius of gyration (Rg) and polydispersity of Hb in the 20 nm diameter Si-tube indicates that Hb undergoes a significant amount of aggregation. However, for Si-tube diameters greater or equal to 100 nm, the Rg of Hb is found to be in very close proximity to that obtained from the protein data bank (PDB) reported structure (Rg of native Hb=23.8 Å). This strongly indicates that the protein has a preference for the more native-like non-aggregated state if confined inside tubes of diameter greater or equal to 100 nm. Further insight into the Hb structure is obtained from the distance distribution function, p(r), and ab initio models calculated from the SANS patterns. These also suggest that the Si-tube size is a key parameter for protein stability and structure.

  13. Nanostructure in block copolymer solutions: Rheology and small-angle neutron scattering

    SciTech Connect

    Habas, Jean-Pierre; Pavie, Emmanuel; Perreur, Christelle; Lapp, Alain; Peyrelasse, Jean

    2004-12-01

    Triblock copolymers composed of poly(ethylene oxide) (PEO) and poly(propylene oxide) (PPO) present an amphiphilic character in aqueous solutions. Since PPO is less hydrophilic than PEO and since their solubilities decrease when the temperature increases, the copolymers self-assemble spontaneously, forming micelles at moderate temperatures. For higher temperatures or concentrations, the copolymers or the micelles are ordered because of repulsive interactions and form lyotropic liquid crystalline phases. These are phases of very great viscosity with the aspect of gels, and transitions between different crystalline phases can occur at fixed concentration during an increase of temperature. We studied solutions of three different copolymers. The first two have a star structure. They are both composed of four branches (EO){sub x}(PO){sub y} fixed on an ethylene diamine, but differ by the values of x and y. Their commercial name is Tetronic 908 (x=114, y=21) and Tetronic 704 (x=16, y=18). The third copolymer (EO){sub 37}(PO){sub 56}(EO){sub 37} is linear and is known under the name of Pluronic P105. The measurements of the shear complex elastic modulus according to the temperature is used to determine the temperatures of the different transitions. Then, small-angle neutron scattering on samples under flow and true crystallographic arguments make it possible to identify the nature of the crystalline phases. For the systems studied, we show that the branched copolymers form only one type of liquid crystalline phase, which is bcc for the T908 and lamellar for the T704. For the linear copolymer, it is possible to identify three transitions: micellar solution to hexagonal phase, hexagonal phase to body-centered cubic phase, and finally body-centered cubic phase to lamellar phase.

  14. Small-Angle Neutron Scattering Studies of Magnetic Correlation Lengths in Nanoparticle Assemblies

    NASA Astrophysics Data System (ADS)

    Majetich, Sara

    2009-03-01

    Small-angle neutron scattering (SANS) measurements of ordered arrays of surfactant-coated magnetic nanoparticle reveal characteristic length scales associated with interparticle and intraparticle magnetic ordering. The high degree of uniformity in the monodisperse nanoparticle size and spacing leads to a pronounced diffraction peak and allows for a straightforward determination of these length scales [1]. There are notable differences in these length scales depending on the particle moment, which depends on the material (Fe, Co, Fe3O4) and diameter, and also on whether the metal particle core is surrounded by an oxide shell. For 8.5 nm particles containing an Fe core and thick Fe3O4 shell, evidence of a spin flop phase is seen in the magnetite shell when a field is applied , but not when the shell thickness is ˜0.5 nm [2]. 8.0 nm particles with an e-Co core and 0.75 nm CoO shell show no exchange bias effects while similar particles with a 2 nm thick shell so significant training effects below 90 K. Polarized SANS studied of 7 nm Fe3O4 nanoparticle assemblies show the ability to resolve the magnetization components in 3D. [4pt] [1] M. Sachan, C. Bonnoit, S. A. Majetich, Y. Ijiri, P. O. Mensah-Bonsu, J. A. Borchers, and J. J. Rhyne, Appl. Phys. Lett. 92, 152503 (2008). [0pt] [2] Yumi Ijiri, Christopher V. Kelly, Julie A. Borchers, James J. Rhyne, Dorothy F. Farrell, Sara A. Majetich, Appl. Phys. Lett. 86, 243102-243104 (2005). [0pt] [3] K. L. Krycka, R. Booth, J. A. Borchers, W. C. Chen, C. Conlon, T. Gentile, C. Hogg, Y. Ijiri, M. Laver, B. B. Maranville, S. A. Majetich, J. Rhyne, and S. M. Watson, Physica B (submitted).

  15. Structure and properties of aqueous methylcellulose gels by small-angle neutron scattering.

    PubMed

    Chatterjee, Tirtha; Nakatani, Alan I; Adden, Roland; Brackhagen, Meinolf; Redwine, David; Shen, Hongwei; Li, Yongfu; Wilson, Tricia; Sammler, Robert L

    2012-10-08

    Cold, semidilute, aqueous solutions of methylcellulose (MC) are known to undergo thermoreversible gelation when warmed. This study focuses on two MC materials with much different gelation performance (gel temperature and hot gel modulus) even though they have similar metrics of their coarse-grained chemical structure (degree-of-methylether substitution and molecular weight distribution). Small-angle neutron scattering (SANS) experiments were conducted to probe the structure of the aqueous MC materials at pre- and postgel temperatures. One material (MC1, higher gel temperature) exhibited a single almost temperature-insensitive gel characteristic length scale (ζ(c) = 1090 ± 50 Å) at postgelation temperatures. This length scale is thought to be the gel blob size between network junctions. It also coincides with the length scale between entanglement sites measured with rheology studies at pregel temperatures. The other material (MC2, lower gel temperature) exhibited two distinct length scales at all temperatures. The larger length scale decreased as temperature increased. Its value (ζ(c1) = 1046 ± 19 Å) at the lowest pregel temperature was indistinguishable from that measured for MC1, and reached a limiting value (ζ(c1) = 450 ± 19 Å) at high temperature. The smaller length scale (ζ(c2) = 120 to 240 Å) increased slightly as temperature increased, but remained on the order of the chain persistence length (130 Å) measured at pregel temperatures. The smaller blob size (ζ(c1)) of MC2 suggests a higher bond energy or a stiffer connectivity between network junctions. Moreover, the number density of these blobs, at the same reduced temperature with respect to the gel temperature, is orders of magnitude higher for the MC2 gels. Presumably, the smaller gel length scale and higher number density lead to higher hot gel modulus for the low gel temperature material.

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

    PubMed

    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.

  17. Evidence for Three-Dimensional Radiative Effects in MODIS Cloud Optical Depths Retrieved at Back Scattering View Angles

    NASA Technical Reports Server (NTRS)

    Varnai, Tamas; Marshak, Alexander

    2003-01-01

    This study addresses the question whether 1D radiative transfer theory describes well the angular distribution of shortwave cloud reflection. The statistical analysis of a large set of MODIS observations indicates that in oblique backward scattering directions, cloud reflection is stronger than 1D theory would predict. After considering a variety of possible causes, the paper concludes that the most likely reason for the increase lies in 3D radiative interactions. The results' main implication is that cloud optical depths retrieved at back scattering view angles larger than about 50 degrees tend to be overestimated and should be used only with great caution.

  18. Single-crystal CVD diamonds as small-angle X-ray scattering windows for high-pressure research.

    PubMed

    Wang, Suntao; Meng, Yu-Fei; Ando, Nozomi; Tate, Mark; Krasnicki, Szczesny; Yan, Chih-Shiue; Liang, Qi; Lai, Joseph; Mao, Ho-Kwang; Gruner, Sol M; Hemley, Russell J

    2012-06-01

    Small-angle X-ray scattering (SAXS) was performed on single-crystal chemical vapor deposition (CVD) diamonds with low nitrogen concentrations, which were fabricated by microwave plasma-assisted chemical vapor deposition at high growth rates. High optical quality undoped 500 µm-thick single-crystal CVD diamonds grown without intentional nitrogen addition proved to be excellent as windows on SAXS cells, yielding parasitic scattering no more intense than a 7.5 µm-thick Kapton film. A single-crystal CVD diamond window was successfully used in a high-pressure SAXS cell.

  19. A Study of Cross-linked Regions of Poly(Vinyl Alcohol) Gels by Small-Angle Neutron Scattering

    NASA Astrophysics Data System (ADS)

    Lawrence, Mathias B.; Desa, J. A. E.; Aswal, V. K.

    2011-07-01

    A poly(vinyl alcohol)-borax cross-linked hydrogel has been studied by Small Angle Neutron Scattering as a function of borax concentration in the wave-vector transfer (Q) range of 0.017 Å-1 to 0.36 Å-1. It is found that as the concentration of borax increases, so does the intensity of scattering in this range. Beyond a borax concentration of 2 mg/ml, the increase in cross-linked PVA chains leads to cross-linked units larger than 150 Å as evidenced by a reduction in intensity in the lower Q region.

  20. Integral indicatrix of light scattering from {open_quotes}soft{close_quotes} spherical particles in the region of small angles

    SciTech Connect

    Lopatin, V.N.; Shapovalov, K.A.

    1995-05-01

    The integral indicatrix of light scattering from a {open_quotes}soft{close_quotes} spherical particle is studied as a function of the phase shift. It is shown analytically in the WKB approximation and numerically on the basis of the Mie theory and the WKB approximation that the dependence of the integral indicatrix on the phase shift is similar to that for the factor of light scattering efficiency. Asymptotic expressions for the integral indicatrix are obtained for large diffraction parameters in the limiting cases of small and large phase shifts in the region of small angles. 8 refs., 3 figs.

  1. Synchrotron radiation-based x-ray reflection and scattering techniques for dimensional nanometrology

    NASA Astrophysics Data System (ADS)

    Krumrey, Michael; Gleber, Gudrun; Scholze, Frank; Wernecke, Jan

    2011-09-01

    Nanoobjects have at least one dimension in the range from 1 to 100 nm. Thus, if radiation is used for dimensional metrology, it should preferably have a wavelength in or below this range. For example, x-ray reflectometry (XRR) using x-ray tubes with Cu Kα radiation is widely used for layer thickness measurements with relative uncertainties of about 1%. By using different monochromator beamlines in the laboratory of PTB at the synchrotron radiation facility BESSY II, any x-ray wavelength from several nanometers down to about 0.1 nm can be selected for dimensional measurements in the nanometer range. Here, XRR is performed at wavelengths in the vicinity of an absorption edge of the chemical elements involved in order to enhance the contrast for layer systems like SiO2/Si which are difficult to resolve with Cu Kα radiation. By using longer wavelengths of around 2 nm, even an oxide layer and a thin carbonaceous contamination layer on a strongly curved spherical surface were separated, as required for measurements at 95 mm diameter silicon spheres within the international Avogadro project for the new definition of the kilogram. For nanoparticles in suspension, small angle x-ray scattering (SAXS) is the method of choice for dimensional metrology. This ensemble technique requires intense, monochromatic x-rays of low divergence. From the scattering pattern, the particle diameter and the size distribution are obtained. Moreover, the dimensional properties of nanostructured surfaces and nanoparticles on surfaces have been studied by grazing incidence SAXS (GISAXS), combining small angle scattering with the reflection geometry known from XRR. The diameters of gold nanoparticles obtained by SAXS and GISAXS are in very good agreement.

  2. Silver behenate as a calibration standard of grazing-incidence small-angle X-ray scattering

    SciTech Connect

    Lee, Byeongdu; Lo, Chieh-Tsung; Seifert, Soenke; Winans, Randall E.

    2006-09-12

    Grazing-incidence small-angle X-ray scattering (GISAXS) patterns of a silver behenate composite film, which has a typical layered structure, are described. The peak position of the film in the GISAXS pattern was varied depending on the incident angle, which was well described by taking into account the refraction and the reflection effects. Since the refractive index of samples depends on sample preparation, it is recommended that the measurement of silver behenate as a standard be done in conventional transmission mode to avoid any complexity.

  3. 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)

    SciTech Connect

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

    2012-10-15

    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.

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

    SciTech Connect

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

    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.

  5. A study of the effect of formalin preservation on normal and cancerous breast tissues using small angle X-ray scattering (SAXS)

    NASA Astrophysics Data System (ADS)

    Changizi, V.; Wilkinson, S.; Hall, C. J.; Grossmann, G.

    2006-09-01

    Small angle X-ray scattering (SAXS) has the ability to provide information on a molecular and supra-molecular scale from biological tissue specimens. It has been postulated that this information will be useful in providing histopathological diagnoses for certain diseases of the breast. In this category, we include cancer, a major health problem for a number of populations around the world. So far studies in our group have been made using flash-frozen tissue samples. This limits the range and ease of use of the technique. If we were able to obtain the same information from preserved tissues then a more extensive use of SAXS diagnosis would be possible. Here we report on the first investigations into this possibility. In the research reported in this paper, 84 human breast biopsies including cancer and normal tissues were obtained from human patients. Small angle scatter data were collected at station 2.1 of the SRS at the Daresbury Laboratory, UK using a beam size of 0.25 mm 2 at the sample and a wavelength of 1.54 Å. The sample to detector distance was 2000 mm. The results verify that there is a quantifiable difference between the scatter curves from flash-frozen cancer and normal breast tissue in the range of scatter vector Q between 0.4 and 0.7 nm -1. After preserving the tissues in formalin, the difference between the normal and cancerous tissues is less marked. The preservation of the tissue in formalin can essentially mask the effects that disease would have on the tissue supra-molecular structure rendering the preserved specimens of less useful for this histopathology technique.

  6. Grazing-incidence small-angle X-ray scattering: application to the study of quantum dot lattices

    SciTech Connect

    Buljan, Maja Radić, Nikola; Bernstorff, Sigrid; Dražić, Goran; Bogdanović-Radović, Iva; Holý, Václav

    2012-01-01

    The modelling of grazing-incidence small-angle X-ray scattering (GISAXS) from three-dimensional quantum dot lattices is described. The ordering of quantum dots in three-dimensional quantum dot lattices is investigated by grazing-incidence small-angle X-ray scattering (GISAXS). Theoretical models describing GISAXS intensity distributions for three general classes of lattices of quantum dots are proposed. The classes differ in the type of disorder of the positions of the quantum dots. The models enable full structure determination, including lattice type, lattice parameters, the type and degree of disorder in the quantum dot positions and the distributions of the quantum dot sizes. Applications of the developed models are demonstrated using experimentally measured data from several types of quantum dot lattices formed by a self-assembly process.

  7. Scattering attributes of one-dimensional semiconducting oxide nanomaterials individually probed for varying light-matter interaction angles

    PubMed Central

    Choi, Daniel S.; Singh, Manpreet; Zhou, Hebing; Milchak, Marissa; Hahm, Jong-in

    2015-01-01

    We report the characteristic optical responses of one-dimensional semiconducting oxide nanomaterials by examining the individual nanorods (NRs) of ZnO, SnO2, indium tin oxide, and zinc tin oxide under precisely controlled, light-matter interaction geometry. Scattering signals from a large set of NRs of the different types are evaluated spatially along the NR length while varying the NR tilt angle, incident light polarization, and analyzer rotation. Subsequently, we identify material-indiscriminate, NR tilt angle- and incident polarization-dependent scattering behaviors exhibiting continuous, intermittent, and discrete responses. The insight gained from this study can advance our fundamental understanding of the optical behaviors of the technologically useful nanomaterials and, at the same time, promote the development of highly miniaturized, photonic and bio-optical devices utilizing the spatially controllable, optical responses of the individual semiconducting oxide NRs. PMID:26549887

  8. Concept for a time-of-flight Small Angle Neutron Scattering instrument at the European Spallation Source

    NASA Astrophysics Data System (ADS)

    Jaksch, S.; Martin-Rodriguez, D.; Ostermann, A.; Jestin, J.; Duarte Pinto, S.; Bouwman, W. G.; Uher, J.; Engels, R.; Frielinghaus, H.

    2014-10-01

    A new Small Angle Neutron Scattering instrument is proposed for the European Spallation Source. The pulsed source requires a time-of-flight analysis of the gathered neutrons at the detector. The optimal instrument length is found to be rather large, which allows for a polarizer and a versatile collimation. The polarizer allows for studying magnetic samples and incoherent background subtraction. The wide collimation will host VSANS and SESANS options that increase the resolution of the instrument towards μm and tens of μm, respectively. Two 1 m2 area detectors will cover a large solid angle simultaneously. The expected gains for this new instrument will lie in the range between 20 and 36, depending on the assessment criteria, when compared to up-to-date reactor based instruments. This will open new perspectives for fast kinetics, weakly scattering samples, and multi-dimensional contrast variation studies.

  9. Performance of the micro-PIC gaseous area detector in small-angle X-ray scattering experiments.

    PubMed

    Hattori, Kaori; Tsuchiya, Ken'ichi; Ito, Kazuki; Okada, Yoko; Fujii, Kotaro; Kubo, Hidetoshi; Miuchi, Kentaro; Takata, Masaki; Tanimori, Toru; Uekusa, Hidehiro

    2009-03-01

    The application of a two-dimensional photon-counting detector based on a micro-pixel gas chamber (micro-PIC) to high-resolution small-angle X-ray scattering (SAXS), and its performance, are reported. The micro-PIC is a micro-pattern gaseous detector fabricated by printed circuit board technology. This article describes the performance of the micro-PIC in SAXS experiments at SPring-8. A dynamic range of >10(5) was obtained for X-ray scattering from a polystyrene sphere solution. A maximum counting rate of up to 5 MHz was observed with good linearity and without saturation. For a diffraction pattern of collagen, weak peaks were observed in the high-angle region in one accumulation of photons.

  10. Characterizing the Morphologies of Mechanically Manipulated Multiwall Carbon Nanotube Films by Small-Angle X-ray Scattering

    SciTech Connect

    Wang,B.; Bennett, R.; Verploegen, E.; Hart, A.; Cohen, R.

    2007-01-01

    We used small-angle X-ray scattering (SAXS) to quantitatively characterize the morphological characteristics of pristine and mechanically manipulated multiwall carbon nanotube (MWCNT) films. We determined that CNT diameters measured near the edges of a film were smaller compared to those measured in the interior. Uniaxially compressed MWCNT films exhibited a buckling deformation that was observable both in scanning electron microscopy (SEM) and SAXS. CNT films were also converted into cellular foams of CNTs through capillarity-induced densification. By examining spatially- and time-resolved SAXS data for the cellular foams, we identified low angle features in the scattering curves that correspond to the average spacing between CNTs, demonstrating that SAXS is a useful method for monitoring the packing density of CNTs in a film. For all of the morphologies that were examined (aligned, disordered, compressed, and densified), SAXS data showed good correspondence with SEM images.

  11. Modulated heterodyne light scattering set-up for measuring long relaxation time at small and wide angle

    NASA Astrophysics Data System (ADS)

    Leone, Nancy; Villari, Valentina; Micali, Norberto

    2012-08-01

    We present a simple, compact, and versatile experimental setup working in the heterodyne detection mode with modulation of the reference beam. The system is implemented with a collection optics based on a unimodal optical fiber coupler. This choice allows the heterodyne to be used in a wide range of scattering angles, even for very small ones, without losing the optical beating. The apparatus can be successfully used to study translational diffusive dynamics of dispersed particles at scattering angles smaller than 5° and it is suitable for exploring slow relaxation processes in sub-Hertz frequency domain, for example, in glass-forming systems. It is also possible to measure the electrophoretic mobility by applying an electric field into a charged particles solution.

  12. Scattering attributes of one-dimensional semiconducting oxide nanomaterials individually probed for varying light-matter interaction angles

    SciTech Connect

    Choi, Daniel S.; Singh, Manpreet; Zhou, Hebing; Milchak, Marissa; Hahm, Jong-in

    2015-10-12

    We report the characteristic optical responses of one-dimensional semiconducting oxide nanomaterials by examining the individual nanorods (NRs) of ZnO, SnO{sub 2}, indium tin oxide, and zinc tin oxide under precisely controlled, light-matter interaction geometry. Scattering signals from a large set of NRs of the different types are evaluated spatially along the NR length while varying the NR tilt angle, incident light polarization, and analyzer rotation. Subsequently, we identify material-indiscriminate, NR tilt angle- and incident polarization-dependent scattering behaviors exhibiting continuous, intermittent, and discrete responses. The insight gained from this study can advance our fundamental understanding of the optical behaviors of the technologically useful nanomaterials and, at the same time, promote the development of highly miniaturized, photonic and bio-optical devices utilizing the spatially controllable, optical responses of the individual semiconducting oxide NRs.

  13. Grazing incidence small-angle X-ray scattering microtomography demonstrated on a self-ordered dried drop of nanoparticles.

    PubMed

    Kuhlmann, Marion; Feldkamp, Jan M; Patommel, Jens; Roth, Stephan V; Timmann, Andreas; Gehrke, Rainer; Müller-Buschbaum, Peter; Schroer, Christian G

    2009-07-07

    We combine grazing-incidence small-angle X-ray scattering (GISAXS) with scanning X-ray microtomography to investigate the nanostructure in a dried gold/polystyrene nanocomposite drop. Local GISAXS structure factors are reconstructed at each position on the surface of this two-dimensionally heterogeneous sample with 30 microm pixel size. Evidence for four types of self-assembled colloidal crystalline structures is provided by the reconstructed data of the drop demonstrating the feasibility of the method.

  14. Monte-Carlo simulation of an ultra small-angle neutron scattering instrument based on Soller slits

    SciTech Connect

    Rieker, T.; Hubbard, P.

    1997-09-01

    Monte Carlo simulations are used to investigate an ultra small-angle neutron scattering instrument for use at a pulsed source based on a Soller slit collimator and analyzer. The simulations show that for a q{sub min} of {approximately}le-4 {angstrom}{sup -1} (15 {angstrom} neutrons) a few tenths of a percent of the incident flux is transmitted through both collimators at q=0.

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

    NASA Astrophysics Data System (ADS)

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

    2010-10-01

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

  16. Nanostructured metallic rear reflectors for thin solar cells: balancing parasitic absorption in metal and large-angle scattering

    NASA Astrophysics Data System (ADS)

    Disney, Claire E. R.; Pillai, Supriya; Green, Martin A.

    2015-12-01

    Rear reflectors for solar cells comprised of metal films with periodic arrays of nanoscale features on their surface can provide significantly enhanced light trapping in the absorber layer. However these structures can also result in significantly increased parasitic absorption into the metal layer at various wavelengths of light. Conversely these highly absorbing resonances can also coincide with the wavelengths which display the largest enhancement to the cell's photocurrent. As such it is important to understand the underlying causes for such photocurrent enhancements and losses in the metal in order to design the optimum structure for use. 3D Finite-difference-time-domain simulations have been used to model a variety of structures and analyze the spatial distribution of absorption within different materials which make up the structure, the angles at which light will be scattered from the rear surface, as well as the idealized short circuit current from each structure integrated across the AM1.5 spectrum. These reveal the properties of these modes at resonant wavelengths at which absorption into both materials is enhanced. Despite the enhanced coupling of light into the metal at these wavelengths, the amount of light scattered back into the absorber at large angles is also significantly boosted. For a large variety of geometries, the impact of this large angle scattering dominates leading to significant increases to a cell's photocurrent. Our simulations allow us to understand the contributions of multiple plasmonic effects occurring in such structures, allowing selection of the most suitable geometries to achieve large-angle scattering in a desired wavelength range.

  17. Distribution of transport current in a type-II superconductor studied by small-angle neutron scattering.

    PubMed

    Pautrat, A; Goupil, C; Simon, Ch; Charalambous, D; Forgan, E M; Lazard, G; Mathieu, P; Brûlet, A

    2003-02-28

    We report small-angle neutron scattering measurements on the vortex lattice in a PbIn polycrystal in the presence of an applied current. Using the rocking curves as a probe of the distribution of current in the sample, we observe that vortex pinning is due to the surface roughness. This leads to a surface current that persists in the flux-flow region. We show the influence of surface treatments on the distribution of this current.

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

    NASA Astrophysics Data System (ADS)

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

    2014-12-01

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

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

    SciTech Connect

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

    2014-12-14

    A new method is introduced to compute X-ray solution scattering profiles from atomic models of macromolecules. The three-dimensional version of the Reference Interaction Site Model (RISM) from liquid-state statistical mechanics is employed to compute the solvent distribution around the solute, including both water and ions. X-ray scattering profiles are computed from this distribution together with the solute geometry. We describe an efficient procedure for performing this calculation employing a Lebedev grid for the angular averaging. The intensity profiles (which involve no adjustable parameters) match experiment and molecular dynamics simulations up to wide angle for two proteins (lysozyme and myoglobin) in water, as well as the small-angle profiles for a dozen biomolecules taken from the BioIsis.net database. The RISM model is especially well-suited for studies of nucleic acids in salt solution. Use of fiber-diffraction models for the structure of duplex DNA in solution yields close agreement with the observed scattering profiles in both the small and wide angle scattering (SAXS and WAXS) regimes. In addition, computed profiles of anomalous SAXS signals (for Rb{sup +} and Sr{sup 2+}) emphasize the ionic contribution to scattering and are in reasonable agreement with experiment. In cases where an absolute calibration of the experimental data at q = 0 is available, one can extract a count of the excess number of waters and ions; computed values depend on the closure that is assumed in the solution of the Ornstein–Zernike equations, with results from the Kovalenko–Hirata closure being closest to experiment for the cases studied here.

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

    PubMed Central

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

    2014-01-01

    A new method is introduced to compute X-ray solution scattering profiles from atomic models of macromolecules. The three-dimensional version of the Reference Interaction Site Model (RISM) from liquid-state statistical mechanics is employed to compute the solvent distribution around the solute, including both water and ions. X-ray scattering profiles are computed from this distribution together with the solute geometry. We describe an efficient procedure for performing this calculation employing a Lebedev grid for the angular averaging. The intensity profiles (which involve no adjustable parameters) match experiment and molecular dynamics simulations up to wide angle for two proteins (lysozyme and myoglobin) in water, as well as the small-angle profiles for a dozen biomolecules taken from the BioIsis.net database. The RISM model is especially well-suited for studies of nucleic acids in salt solution. Use of fiber-diffraction models for the structure of duplex DNA in solution yields close agreement with the observed scattering profiles in both the small and wide angle scattering (SAXS and WAXS) regimes. In addition, computed profiles of anomalous SAXS signals (for Rb+ and Sr2+) emphasize the ionic contribution to scattering and are in reasonable agreement with experiment. In cases where an absolute calibration of the experimental data at q = 0 is available, one can extract a count of the excess number of waters and ions; computed values depend on the closure that is assumed in the solution of the Ornstein–Zernike equations, with results from the Kovalenko–Hirata closure being closest to experiment for the cases studied here. PMID:25494779

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

    SciTech Connect

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

    2016-05-24

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

  2. First in situ evidence of electron pitch angle scattering due to magnetic field line curvature in the Ion diffusion region

    NASA Astrophysics Data System (ADS)

    Zhang, Y. C.; Shen, C.; Marchaudon, A.; Rong, Z. J.; Lavraud, B.; Fazakerley, A.; Yao, Z.; Mihaljcic, B.; Ji, Y.; Ma, Y. H.; Liu, Z. X.

    2016-05-01

    Theory predicts that the first adiabatic invariant of a charged particle may be violated in a region of highly curved field lines, leading to significant pitch angle scattering for particles whose gyroradius are comparable to the radius of the magnetic field line curvature. This scattering generates more isotropic particle distribution functions, with important impacts on the presence or absence of plasma instabilities. Using magnetic curvature analysis based on multipoint Cluster spacecraft observations, we present the first investigation of magnetic curvature in the vicinity of an ion diffusion region where reconnected field lines are highly curved. Electrons at energies > 8 keV show a clear pitch angle ordering between bidirectional and trapped distribution in surrounding regions, while we show that in the more central part of the ion diffusion region electrons above such energies become isotropic. By contrast, colder electrons (~1 keV) retain their bidirectional character throughout the diffusion regions. The calculated adiabatic parameter K2 for these electrons is in agreement with theory. This study provides the first observational evidence for particle pitch angle scattering due to magnetic field lines with well characterized curvature in a space plasma.

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  4. Particle sizing by measurement of forward-scattered light at two angles

    NASA Technical Reports Server (NTRS)

    Buchele, D. R.

    1983-01-01

    Fundamental and practical limitations to particle sizing by measurement of forward scattered light are presented. Methods to minimize the limitations are described. Two types of instruments are compared.

  5. Small-angle light scattering from polymer-dispersed liquid-crystal films

    SciTech Connect

    Loiko, V. A. Maschke, U.; Zyryanov, V. Ya.; Konkolovich, A. V.; Misckevich, A. A.

    2008-10-15

    A method is developed for modeling and computing the angular distribution of light scattered forward from a single-layer polymer-dispersed liquid-crystal (PDLC) film. The method is based on effective-medium approximation, anomalous diffraction approximation, and far-field single-scattering approximation. The angular distribution of forward-scattered light is analyzed for PDLC films with droplet size larger than the optical wavelength. The method can be used to study field-and temperature-induced phase transitions in LC droplets with cylindrical symmetry by measuring polarized scattered light intensity.

  6. Distribution angle control of a light-emitting diode downlight lens with high color uniformity using a scattering polymer

    NASA Astrophysics Data System (ADS)

    Mochizuki, Keiichi; Oosumi, Kazumasa; Koizumi, Fumiaki; Shinohara, Yoshinori; Tagaya, Akihiro; Koike, Yasuhiro

    2015-06-01

    We have proposed a light-emitting diode (LED) downlight lens that is made of a highly scattered optical transmission (HSOT) polymer. The HSOT polymer contains optimized heterogeneous structures that produce homogeneously scattered light with forward directivity. The full width at half maximum of the illuminance distribution angle can be increased from 16.7° to 37.9° as the concentration of the scattering particles in the HSOT polymer LED downlight lenses of identical shape is increased from 0.015 to 0.100 wt%. The colors in an illuminated area are highly uniform, which is not discernible by the human eye, with a high output efficiency greater than 85 %.

  7. Cell growth characteristics from angle- and polarization-resolved light scattering: Prospects for two-dimensional correlation analysis

    NASA Astrophysics Data System (ADS)

    Herran Cuspinera, Roxana M.; Hore, Dennis K.

    2016-11-01

    We highlight the potential of generalized two-dimensional correlation analysis for the fingerprinting of cell growth in solution monitored by light scattering, where the synchronous and asynchronous responses serve as a sensitive marker for the effect of growth conditions on the distribution of cell morphologies. The polarization of the scattered light varies according to the cell size distribution, and so the changes in the polarization over time are an excellent indicator of the dynamic growth conditions. However, direct comparison of the polarization-, time-, and angle-resolved signals between different experiments is hindered by the subtle changes in the data, and the inability to easily adapt models to account for these differences. Using Mie scattering simulations of different growth conditions, and some preliminary experimental data for a single set of conditions, we illustrate that correlation analysis provides rapid and sensitive qualitative markers of growth characteristics.

  8. A potential for overestimating the absolute magnitudes of second virial coefficients by small-angle X-ray scattering.

    PubMed

    Scott, David J; Patel, Trushar R; Winzor, Donald J

    2013-04-15

    Theoretical consideration is given to the effect of cosolutes (including buffer and electrolyte components) on the determination of second virial coefficients for proteins by small-angle X-ray scattering (SAXS)-a factor overlooked in current analyses in terms of expressions for a two-component system. A potential deficiency of existing practices is illustrated by reassessment of published results on the effect of polyethylene glycol concentration on the second virial coefficient for urate oxidase. This error reflects the substitution of I(0,c3,0), the scattering intensity in the limit of zero scattering angle and solute concentration, for I(0,0,0), the corresponding parameter in the limit of zero cosolute concentration (c3) as well. Published static light scattering results on the dependence of the apparent molecular weight of ovalbumin on buffer concentration are extrapolated to zero concentration to obtain the true value (M2) and thereby establish the feasibility of obtaining the analogous SAXS parameter, I(0,0,0), experimentally.

  9. Anomalous small angle x-ray scattering studies of amorphous metal-germanium alloys

    SciTech Connect

    Rice, M.

    1993-12-01

    This dissertation addresses the issue of composition modulation in sputtered amorphous metal-germanium thin films with the aim of understanding the intermediate range structure of these films as a function of composition. The investigative tool used in this work is anomalous small-angle X-ray scattering (ASAXS). The primary focus of this investigation is the amorphous iron-germanium (a-Fe{sub x}Ge{sub 100-x}) system with particular emphasis on the semiconductor-rich regime. Brief excursions are made into the amorphous tungsten-germanium (a-W{sub x}Ge{sub 100-x}) and the amorphous molybdenum-germanium (a-Mo{sub x}Ge{sub 100-x}) systems. All three systems exhibit an amorphous structure over a broad composition range extending from pure amorphous germanium to approximately 70 atomic percent metal when prepared as sputtered films. Across this composition range the structures change from the open, covalently bonded, tetrahedral network of pure a-Ge to densely packed metals. The structural changes are accompanied by a semiconductor-metal transition in all three systems as well as a ferromagnetic transition in the a-Fe{sub x}Ge{sub 100-x} system and a superconducting transition in the a-Mo{sub x}Ge{sub 100-x} system. A long standing question, particularly in the a-Fe{sub x}Ge{sub 100-x} and the a-Mo{sub x}Ge{sub 100-x} systems, has been whether the structural changes (and therefore the accompanying electrical and magnetic transitions) are accomplished by homogeneous alloy formation or phase separation. The application of ASAXS to this problem proves unambiguously that fine scale composition modulations, as distinct from the simple density fluctuations that arise from cracks and voids, are present in the a-Fe{sub x}Ge{sub 100-x}, a-W{sub x}Ge{sub 100-x}, and a-Mo{sub x}Ge{sub 100-x} systems in the semiconductor-metal transition region. Furthermore, ASAXS shows that germanium is distributed uniformly throughout each sample in the x<25 regime of all three systems.

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

    USGS Publications Warehouse

    Shang, C.; Rice, J.A.; Eberl, D.D.; Lin, S.-J.

    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 extrapolation 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 A??. The SAXS results are compared with those obtained by X-ray diffraction peak broadening methods. It was found that the power-law exponent (??) obtained by fitting the data in the region of q = 0.1 -0.6 nm-1 to the power law (I = Ioq-??) 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 ?? <4.0.

  11. A simple procedure to evaluate the efficiency of bio-macromolecular rigid-body refinement by small-angle scattering.

    PubMed

    Gabel, Frank

    2012-01-01

    A simple and rapid procedure is presented that enables evaluation and visualization of refinement efficiency for bio-macromolecular complexes consisting of two subunits in a given orientation by using small-angle scattering. Subunit orientations within a complex can be provided in practice by NMR residual dipolar couplings, an approach that has been combined with increasing success to complement small-angle data. The procedure is illustrated by applying it to several systems composed of two simple geometric bodies (ellipsoids) and to protein complexes from the protein data bank that vary in subunit size and anisometry. The effects of the experimental small-angle scattering range (Q-range) and data noise level on the refinement efficiency are investigated and discussed. The procedure can be used in two ways: (1) either as a quick preliminary test to probe the refinement capacity expected for a given bio-macromolecular complex prior to sophisticated and time-consuming experiments and data analysis, or (2) as an a posteriori check of the stability and accuracy of a refined model and for illustration of the residual degrees of freedom of the subunit positions that are in agreement with both small-angle data and restraints on subunit orientation (as provided, e.g., by NMR).

  12. Modern integral equation techniques for quantum reactive scattering theory

    SciTech Connect

    Auerbach, Scott Michael

    1993-11-01

    Rigorous calculations of cross sections and rate constants for elementary gas phase chemical reactions are performed for comparison with experiment, to ensure that our picture of the chemical reaction is complete. We focus on the H/D+H2 → H2/DH + H reaction, and use the time independent integral equation technique in quantum reactive scattering theory. We examine the sensitivity of H+H2 state resolved integral cross sections σ{sub v'j',vj}(E) for the transitions (v = 0,j = 0) to (v'} = 1,j' = 1,3), to the difference between the Liu-Siegbahn-Truhlar-Horowitz (LSTH) and double many body expansion (DMBE) ab initio potential energy surfaces (PES). This sensitivity analysis is performed to determine the origin of a large discrepancy between experimental cross sections with sharply peaked energy dependence and theoretical ones with smooth energy dependence. We find that the LSTH and DMBE PESs give virtually identical cross sections, which lends credence to the theoretical energy dependence.

  13. Dynamics of intermediate filament assembly followed in micro-flow by small angle X-ray scattering.

    PubMed

    Brennich, Martha Elisabeth; Nolting, Jens-Friedrich; Dammann, Christian; Nöding, Bernd; Bauch, Susanne; Herrmann, Harald; Pfohl, Thomas; Köster, Sarah

    2011-02-21

    The assembly of intermediate filaments (IFs) is a complex process that can be recapitulated through a series of distinct steps in vitro. The combination of microfluidics and small angle X-ray scattering (SAXS) provides a powerful tool to investigate the kinetics of this process on the relevant timescales. Microfluidic mixers based on the principle of hydrodynamic focusing allow for precise control of the mixing of proteins and smaller reagents like ions. Here, we present a multi-layer device that prevents proteins from adsorbing to the channel walls by engulfing the protein jet with a fluid layer of buffer. To ensure compatibility with SAXS, the device is fabricated from UV-curable adhesive (NOA 81). To demonstrate the successful prevention of contact between the protein jet and the channel walls we measure the distribution of a fluorescent dye in the device by confocal microscopy at various flow speeds and compare the results to finite element method (FEM) simulations. The prevention of contact enables the investigation of the assembly of IFs in flow by gradually increasing the salt concentration in the protein jet. The diffusion of salt into the jet can be determined by FEM simulations. SAXS data are collected at different positions in the jet, corresponding to different salt concentrations, and they reveal distinct differences between the earliest assembly states. We find that the mean square radius of gyration perpendicular to the filament axis increases from 13 nm(2) to 58 nm(2) upon assembly. Thereby we provide dynamic structural data of a complex assembly process that was amenable up to now only by microscopic techniques.

  14. Global small-angle X-ray scattering data analysis for multilamellar vesicles: the evolution of the scattering density profile model

    PubMed Central

    Heftberger, Peter; Kollmitzer, Benjamin; Heberle, Frederick A.; Pan, Jianjun; Rappolt, Michael; Amenitsch, Heinz; Kučerka, Norbert; Katsaras, John; Pabst, Georg

    2014-01-01

    The highly successful scattering density profile (SDP) model, used to jointly analyze small-angle X-ray and neutron scattering data from unilamellar vesicles, has been adapted for use with data from fully hydrated, liquid crystalline multilamellar vesicles (MLVs). Using a genetic algorithm, this new method is capable of providing high-resolution structural information, as well as determining bilayer elastic bending fluctuations from standalone X-ray data. Structural parameters such as bilayer thickness and area per lipid were determined for a series of saturated and unsaturated lipids, as well as binary mixtures with cholesterol. The results are in good agreement with previously reported SDP data, which used both neutron and X-ray data. The inclusion of deuterated and non-deuterated MLV neutron data in the analysis improved the lipid backbone information but did not improve, within experimental error, the structural data regarding bilayer thickness and area per lipid. PMID:24587787

  15. A scatter-corrected list-mode reconstruction and a practical scatter/random approximation technique for dynamic PET imaging

    NASA Astrophysics Data System (ADS)

    Cheng, Ju-Chieh Kevin; Rahmim, Arman; Blinder, Stephan; Camborde, Marie-Laure; Raywood, Kelvin; Sossi, Vesna

    2007-04-01

    We describe an ordinary Poisson list-mode expectation maximization (OP-LMEM) algorithm with a sinogram-based scatter correction method based on the single scatter simulation (SSS) technique and a random correction method based on the variance-reduced delayed-coincidence technique. We also describe a practical approximate scatter and random-estimation approach for dynamic PET studies based on a time-averaged scatter and random estimate followed by scaling according to the global numbers of true coincidences and randoms for each temporal frame. The quantitative accuracy achieved using OP-LMEM was compared to that obtained using the histogram-mode 3D ordinary Poisson ordered subset expectation maximization (3D-OP) algorithm with similar scatter and random correction methods, and they showed excellent agreement. The accuracy of the approximated scatter and random estimates was tested by comparing time activity curves (TACs) as well as the spatial scatter distribution from dynamic non-human primate studies obtained from the conventional (frame-based) approach and those obtained from the approximate approach. An excellent agreement was found, and the time required for the calculation of scatter and random estimates in the dynamic studies became much less dependent on the number of frames (we achieved a nearly four times faster performance on the scatter and random estimates by applying the proposed method). The precision of the scatter fraction was also demonstrated for the conventional and the approximate approach using phantom studies. This work was supported by the Canadian Institute of Health Research, a TRIUMF Life Science Grant, the Natural Sciences and Engineering Research Council of Canada UFA (V Sossi) and the Michael Smith Foundation for Health Research Scholarship (V Sossi).

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

    PubMed

    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.

  17. A large-solid-angle X-ray Raman scattering spectrometer at ID20 of the European Synchrotron Radiation Facility.

    PubMed

    Huotari, S; Sahle, Ch J; Henriquet, Ch; Al-Zein, A; Martel, K; Simonelli, L; Verbeni, R; Gonzalez, H; Lagier, M C; Ponchut, C; Moretti Sala, M; Krisch, M; Monaco, G

    2017-03-01

    An end-station for X-ray Raman scattering spectroscopy at beamline ID20 of the European Synchrotron Radiation Facility is described. This end-station is dedicated to the study of shallow core electronic excitations using non-resonant inelastic X-ray scattering. The spectrometer has 72 spherically bent analyzer crystals arranged in six modular groups of 12 analyzer crystals each for a combined maximum flexibility and large solid angle of detection. Each of the six analyzer modules houses one pixelated area detector allowing for X-ray Raman scattering based imaging and efficient separation of the desired signal from the sample and spurious scattering from the often used complicated sample environments. This new end-station provides an unprecedented instrument for X-ray Raman scattering, which is a spectroscopic tool of great interest for the study of low-energy X-ray absorption spectra in materials under in situ conditions, such as in operando batteries and fuel cells, in situ catalytic reactions, and extreme pressure and temperature conditions.

  18. Multi-angle static and dynamic light scattering investigation of lysozyme association: From crystallization to liquid liquid phase separation

    NASA Astrophysics Data System (ADS)

    Onuma, Kazuo; Kanzaki, Noriko

    2007-06-01

    The association of hen egg white lysozyme was observed using time-resolved multi-angle static and dynamic light scattering. In solutions containing 1.2 M of NaCl with a pH of 4.6 buffered by 50 mM of NaAc, and maintained at 20C, the apparent molecular weight Mw, and gyration radius Rg, of lysozyme aggregates were measured at 0.3-5-s intervals for various lysozyme concentrations from 8 to 32 mg/mL using static light scattering. At 32 mg/mL, liquid-liquid phase separation (LLPS) occurred. The (Kc/ΔR(q)) vs. q2 plot had a non-linear shape with a maximum at a particular q2, indicating that the aggregate size distribution was within a narrow range. This had not been observed in our previous studies of high-molecular-weight proteins. The dynamic light scattering data were consistent with those of static light scattering; i.e., CONTIN analysis showed clear bimodal (monomer and aggregate) distributions. Fractal dimension analysis of the aggregates with the protein concentration showed that the inner structure of the scatterer formed during LLPS was rigid in the final stage, which supports a two-step nucleation model.

  19. Dynamic small angle x-ray scattering study of stressed Kevlar 49 epoxy composites

    SciTech Connect

    Lee, J.S.; Fellers, J.F.; Tang, M.Y.; Lin, J.S.

    1985-01-01

    The highly crosslinked epoxy resins gave rise to isotropic scattering patterns and applying tensile stresses resulted in very little scattering changes. The dynamic scattering studies on the epoxy resins indicate the failure process as a catastrophic dynamic process with fractures initiating from surface or internal flaws. The crack propagates across the whole sample in a very short time to complete failure. The Kevlar fibers are microporous giving rise to equatorially elongated anisotropic scattering patterns. These microvoids can be partially filled by liquid epoxy. Based on comparisons of the volume fraction of the microvoids obtained by SAXS absolute intensity measurements and by the density measurements, two sizes of microvoids are present in the Kevlar 49 fibers - one in the range of 10 to 20 nm and the other much larger. Applying tensile stresses results in an increase in the scattering intensities and in the volume fraction of smaller microvoids. The average radius of gyration of these microvoids remained constant, and hence the number of these smaller microvoids must have increased in order to account for increased scattering intensities. It is thus concluded that the failure of Kevlar 49 fibers is accompanied by the increase in number of smaller microvoids and the enlargement of the larger microvoids along the fiber axis direction. The reinforced epoxy composites of low volume fraction unidirectional Kevlar 49 fiber gave rise to anisotropic scattering patterns perpendicular to the fiber axis direction, and it is believed this scattering is due to voids within the fibers and voids entrapped along the fiber matrix interface during processing. The dynamic scattering studies on the composites indicate the failure as a catastrophic dynamic process, fracture initiating in the epoxy matrix and the fibers not being able to carry the load, thus failing catastrophically as well. The failure is thus instantaneous once incipient failure occurs.

  20. A study of effective atomic number and electron density of gel dosimeters and human tissues for scattering of gamma rays: momentum transfer, energy and scattering angle dependence.

    PubMed

    Kurudirek, Murat

    2016-11-01

    The objective of this work was to study water- and tissue-equivalent properties of some gel dosimeters, human tissues and water, for scattering of photons using the effective atomic number (Z eff). The Rayleigh to Compton scattering ratio (R/C) was used to obtain Z eff and electron density (N e ) of gel dosimeters, human tissues and water considering a 10(-2)-10(9) momentum transfer, q (Å(-1)). In the present work, a logarithmic interpolation procedure was used to estimate R/C as well as Z eff of the chosen materials in a wide scattering angle (1°-180°) and energy range (0.001-100 MeV). The Z eff of the chosen materials was found to increase as momentum transfer increases, for q > ~1 Å(-1). At fixed scattering angle and energy, Z eff of the material first increases and then becomes constant for high momentum transfers (q ≥ 3 Å(-1)), which indicates that Z eff is almost independent of energy and scattering angle for the chosen materials. Based on the Z eff data and the continuous momentum transfer range (10(-2)-10(9) Å(-1)), MAGIC, PAGAT and soft tissue were found to be water-equivalent materials, since their differences (%) relative to water are significantly low (≤3.2 % for MAGIC up to 10(3) Å(-1), ≤2.9 % for PAGAT up to 10(9) Å(-1), and ≤3.8 % for soft tissue up to 10(9) Å(-1)), while the Fricke gel was not found to be water equivalent. PAGAT was found to be a soft tissue-equivalent material in the entire momentum transfer range (<4.3 %), while MAGAT has shown to be tissue equivalent for brain (≤8.1 % up to 10 Å(-1)) and lung (<8.2 % up to 10 Å(-1)) tissues. The Fricke gel dosimeter has shown to be adipose tissue equivalent for most of the momentum range considered (<10 %).