issue contents

Journal logoJOURNAL OF
ISSN: 1600-5767

April 2007 issue

Proceedings of the XIIIth International Conference on Small-Angle Scattering (Online Supplement)

Kyoto, Japan, 9-13 July 2006

Highlighted illustration

Plenary papers

J. Appl. Cryst. (2007). 40, s1-s9
doi: 10.1107/S0021889806055579
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Synchrotron radiation, by virtue of its special beam characteristics, has revived interest in small-angle X-ray scattering for hard condensed matter and materials science. New techniques have been developed and new scientific themes tackled, ranging from metallurgy to nanotechnology.

J. Appl. Cryst. (2007). 40, s10-s17
doi: 10.1107/S0021889807001409
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Advanced methods for the analysis of small-angle scattering data from solutions of biological macromolecules are reviewed.

J. Appl. Cryst. (2007). 40, s18-s22
doi: 10.1107/S0021889807007996
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Synchrotron X-ray diffuse scattering and photon correlation spectroscopy in reflection geometry were used to measure the structure and dynamic properties at the surface, interface and in the interior of supported polymer films.

J. Appl. Cryst. (2007). 40, s23-s27
doi: 10.1107/S0021889807003718
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Methods of contrast variation in X-ray and neutron scattering are reviewed.

Special sessions


J. Appl. Cryst. (2007). 40, s28-s33
doi: 10.1107/S0021889806056093
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Neutron spin echo spectroscopy reveals the two main reptation limiting processes: constraint release and contour length fluctuation on a molecular scale. The first direct observations of domain dynamics in biopolymers are presented.

J. Appl. Cryst. (2007). 40, s34-s37
doi: 10.1107/S0021889807009168
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Two-dimensional XPCS allows the dynamics of large wavectors in materials opaque to visible light to be probed. The self-diffusion constant of a colloidal dispersion is probed and compared with available models.

J. Appl. Cryst. (2007). 40, s38-s42
doi: 10.1107/S0021889807003561
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Interferences are observed in coherent X-ray small-angle scattering between a static reference and a fluctuating sample. Heterodyning makes possible the observation of Doppler shifts with sample drift velocities in the nanometres per second range.

J. Appl. Cryst. (2007). 40, s43-s47
doi: 10.1107/S0021889806054707
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Small-angle neutron scattering and dynamic light scattering have been complementarily employed in order to investigate the structure and dynamics of polymer gels. It is demonstrated that complementary use is necessary to explore the dynamics of polymer gels, particularly that of slide-ring gels in which cross-links can slide along the backbone polymer chain.

External fields

J. Appl. Cryst. (2007). 40, s48-s51
doi: 10.1107/S0021889806048874
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Flow-induced shish-kebab structure formation in ultrahigh-molecular-weight polyethylene (UHMWPE)/low-molecular-weight polyethylene blend melts was investigated by using synchrotron X-rays. The results confirmed that the formation of shish is due to the topological deformation of the UHMWPE entanglement network and the formation of shish can accelerate the kebab nucleation.

J. Appl. Cryst. (2007). 40, s52-s56
doi: 10.1107/S0021889806054823
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A short oversight of experiments where small-angle X-ray scattering was performed on samples which were kept in high magnetic fields is given. The samples are biological macromolecules, liquid crystals and crystalline materials.

J. Appl. Cryst. (2007). 40, s57-s61
doi: 10.1107/S0021889807001410
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A polarized small-angle scattering experiment with a concentrated magnetic fluid is described confirming dipolar chains and domains of hexagonal arrangements.

J. Appl. Cryst. (2007). 40, s62-s67
doi: 10.1107/S0021889806047650
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The decay of inter-particle order in Co-ferrofluid has been investigated for different inducing magnetic fields. Time constants have been calculated for the relaxation.

J. Appl. Cryst. (2007). 40, s68-s72
doi: 10.1107/S0021889807000441
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The magnetic responses of columnar discotic metallomesogens, cobalt octa(n-alkylthio)porphyrazine with different side-chain lengths (CoSx, where x is the peripheral n-alkyl chain length, x = 10, 12, 14), have been investigated by small-angle neutron scattering. The magnetic field strength required for the alignment of the columnar phase increased with the side-chain length x.

J. Appl. Cryst. (2007). 40, s73-s77
doi: 10.1107/S0021889807003445
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As a problem in open non-equilibrium phenomena, small-angle scattering studies of a chemical reaction at specific sites and reaction-induced self-assembly of the system which is induced by mixing two stable solutions of palladium(II) acetate [Pd(OAc)2] in N,N-dimethylformamide and the second-generation polyamidoamine dendrimer in methanol are presented.

Hierarchy/wide-Q range

J. Appl. Cryst. (2007). 40, s78-s82
doi: 10.1107/S0021889807006693
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A scanning X-ray imaging technique using the integrated small-angle scattering (SAXS) intensity is presented. The origin of the SAXS contrast is discussed for three biological materials: bone, eggshell and hair.

J. Appl. Cryst. (2007). 40, s83-s87
doi: 10.1107/S0021889806051995
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Synchrotron X-ray diffraction and electron microscopy data are presented for reconstituted protein systems from the bovine central nervous system, which reveal unexpected structures of hierarchical bionanotubes, not predicted by current electrostatic theories.

J. Appl. Cryst. (2007). 40, s88-s92
doi: 10.1107/S0021889807004153
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A simplified tube (hollow cylinder) form factor is developed and utilized to analyze ultra-small-angle X-ray scattering data obtained from multi-walled carbon nanotube/bismaleimide composite samples. The form factor is useful for distinguishing between hollow and solid cylinders as well for detecting the presence of aggregation of one-dimensional colloidal fillers in polymers.

J. Appl. Cryst. (2007). 40, s93-s96
doi: 10.1107/S0021889807001549
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Visualized analysis of SANS from a tert-butyl alcohol–water mixture has revealed that the concentration fluctuation is characterized by polydisperse mass fractals.

J. Appl. Cryst. (2007). 40, s97-s100
doi: 10.1107/S0021889806053507
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Multilevel aggregates with characteristic sizes covering four orders of magnitude, from 1 nm to 10 µm, formed upon cooling decane solutions of poly(ethylene-butene) random copolymers and wax-containing mixed solutions are investigated by combining three small-angle neutron scattering (SANS) techniques (conventional SANS, focusing SANS and ultra-SANS) with microscopy.

J. Appl. Cryst. (2007). 40, s101-s105
doi: 10.1107/S0021889807011727
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The hierarchical structure of an aqueous dispersion of niobate nanosheets was investigated by (ultra-)small-angle scattering methods.

New methods and devices

J. Appl. Cryst. (2007). 40, s106-s110
doi: 10.1107/S0021889806052149

J. Appl. Cryst. (2007). 40, s111-s115
doi: 10.1107/S0021889807005249
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Spin-echo small-angle neutron scattering is used to study the magnetic domain structure of an Ni layer on a Cu substrate. The experiments demonstrate the possibilities of this novel technique.

Parallel sessions

Alloys and ceramics

J. Appl. Cryst. (2007). 40, s116-s120
doi: 10.1107/S0021889807001859
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It is shown that natural and synthetic diamonds contain planar and three-dimensional defects, observable by small-angle neutron scattering. These defects appear after annealing and/or deformation of the diamonds.

J. Appl. Cryst. (2007). 40, s121-s125
doi: 10.1107/S0021889807000064
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Small-angle X-ray scattering analyses on {100} LiF platelets following irradiation with swift Pb and U ions have revealed continuous highly depleted electron densities close to the ion trajectories, suggesting local ion-induced decomposition of the crystal followed by release of mobile alteration products.

J. Appl. Cryst. (2007). 40, s126-s131
doi: 10.1107/S0021889807005493
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New magnesium–rare earth alloys, strengthened by a dense fine scale precipitation, have been designed for structural applications up to 523 K. A complementary study using small-angle X-ray scattering is presented here.

J. Appl. Cryst. (2007). 40, s132-s137
doi: 10.1107/S0021889807002609
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The contribution of molecular water aggregates in the small-angle X-ray scattering of quartz crystals was investigated as a function of the azimuth angle around the primary beam. The presence of Kossel lines randomly decorating the anisotropic two-dimensional pattern and the lack of a clear relationship between Porod invariant and OH content revealed that diffuse scattering plays an important role in the scattering of quartz crystal.

J. Appl. Cryst. (2007). 40, s138-s141
doi: 10.1107/S0021889807003524
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Microstructures in Zr–Cu–Al–Ni bulk metallic glasses consisting only of metallic elements have been examined by anomalous small-angle scattering at the Zr K edge. The cluster-like scattering was analysed in terms of composition fluctuation.

J. Appl. Cryst. (2007). 40, s142-s146
doi: 10.1107/S0021889807005110
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The microstructural effect of low-dose neutron irradiation in ferritic/martensitic steels has been investigated by means of small-angle neutron scattering: depending on the initial steel composition different microstructural evolutions are observed during post-irradiation tempering.

J. Appl. Cryst. (2007). 40, s147-s152
doi: 10.1107/S0021889806048382
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ZrO2–2.8 mol% Y2O3 powders synthesized by the gel-combustion route were investigated by small-angle X-ray scattering and other techniques. The nanoporous structures of these materials were characterized as functions of the nature of the organic fuel and of the calcination temperature.

Biological solution scattering

J. Appl. Cryst. (2007). 40, s153-s158
doi: 10.1107/S0021889807005936
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SAXS-based ab initio modelling of the capsids of isometric bacteriophages allows the solution structure of the constituent hollow spheres to be reconstructed reliably. For the shape of their free nucleic acid, however, other advanced modelling approaches are to be preferred.

J. Appl. Cryst. (2007). 40, s159-s164
doi: 10.1107/S0021889806045729
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By the complimentary use of small-angle X-ray and neutron scattering techniques, the permeability of water across a raft model membrane containing ganglioside (GD3) and the effect of monovalent cations (Na+ and K+) on the permeability have been investigated. The structures of GD3 micelle and GD3/cholesterol mixtures are also discussed.

J. Appl. Cryst. (2007). 40, s165-s169
doi: 10.1107/S0021889807001835
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Charge interaction and temperature effects on the solution structure of lysozyme are studied by small-angle X-ray scattering.

J. Appl. Cryst. (2007). 40, s170-s174
doi: 10.1107/S0021889807010229
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The solution structure of Ca2+/calmodulin complexed with a lentivirus lytic peptide 1 reveals a novel mode of molecular recognition. The result suggests that this region of the transmembrane glycoprotein is important to viral replication.

J. Appl. Cryst. (2007). 40, s175-s178
doi: 10.1107/S0021889807003354
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The change of the hydration shell of hen egg-white lysozyme during the unfolding–refolding process as a function temperature has been analysed. The decrease of the hydration-shell density starts from a lower temperature than the transition temperature of the collapse of the tertiary structure.

J. Appl. Cryst. (2007). 40, s179-s183
doi: 10.1107/S0021889807002117
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Small-angle X-ray scattering and nuclear magnetic resonance studies were performed to investigate the binding of trifluoperazine to Ca2+-free calmodulin with N- and C-terminal globular domains connected by a linker.

J. Appl. Cryst. (2007). 40, s184-s189
doi: 10.1107/S0021889807009211
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Using small-angle and wide-angle X-ray scattering techniques it has been possible to clarify the helix-to-sheet (cross-β) transition and the stacking process of the cross-β sheet of apomyoglobin as a model for amyloid.

J. Appl. Cryst. (2007). 40, s190-s194
doi: 10.1107/S0021889806055506
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A major upgrade of the X33 beamline at the European Molecular Biology Laboratory which has improved the beamline stability and data quality, shortened the measurement time and ensured user-friendly operation is reported.

J. Appl. Cryst. (2007). 40, s195-s199
doi: 10.1107/S0021889807003597

J. Appl. Cryst. (2007). 40, s200-s204
doi: 10.1107/S0021889807006838
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The size and shape of aggregates of human recombinant> αA- and αB-crystallins are investigated with small-angle neutron scattering and dynamic light scattering at 310 K and 288 K. The aggregates of αB-crystallin are stable at both temperatures but those of αA-crystallin are deformed at the lower temperature (288 K).

J. Appl. Cryst. (2007). 40, s205-s208
doi: 10.1107/S0021889807001987
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Using contrast variation by means of isomorphous replacement, the localization of dihalogenated phenols in multilamellar vesicles was determined, and was compared with the results of anomalous small-angle scattering.

J. Appl. Cryst. (2007). 40, s209-s212
doi: 10.1107/S0021889807009247
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The molecular assembly and chain conformation of a glycoprotein mucin are characterized by using small-angle scattering methods.

J. Appl. Cryst. (2007). 40, s213-s216
doi: 10.1107/S0021889807008278
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The chloride-ion concentration dependence of the molecular shape in the acid-denatured state of equine β-lactoglobulin was observed by small-angle X-ray scattering. The results indicated that the compact molten globule is transformed to an expanded conformation with decreasing chloride-ion concentration. Interestingly, this change accompanied the increase in the helix content as measured by circular dichroic spectra.

J. Appl. Cryst. (2007). 40, s217-s222
doi: 10.1107/S0021889807005821
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Solution X-ray and neutron scattering methods are briefly reviewed in view of their appeal and recent progress in data-analysis procedures. Specific examples are discussed highlighting the potential of the techniques and their future developments and applications to structural investigations in the post-genomics era.

J. Appl. Cryst. (2007). 40, s223-s228
doi: 10.1107/S0021889807002853
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New features of the small-angle scattering data analysis package ATSAS 2.1 that allow automated data processing and web-based access are described.

J. Appl. Cryst. (2007). 40, s229-s234
doi: 10.1107/S0021889807001707
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It is shown that bead reconstruction algorithms can be used to obtain low-resolution three-dimensional density maps for nucleic acids from SAXS data. In addition, it is shown that the reconstructed bead models can be used to define the molecular geometry in Poisson–Boltzmann calculations to accurately determine the excess number of ions bound under different solution conditions.

J. Appl. Cryst. (2007). 40, s235-s239
doi: 10.1107/S0021889807005791
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We present a method to separate the protein–detergent complex scattering signal from that of `empty' detergent micelles in small-angle X-ray scattering data of protein–detergent mixtures. The approach relies on singular value decomposition and fitting to data collected at different protein–detergent stoichiometries.

J. Appl. Cryst. (2007). 40, s240-s244
doi: 10.1107/S0021889807006218
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Microstructural characterization of 1,2-dilauroyl-sn-glycero-3-phosphatidyl-adenosine micellar solutions upon cyclohexane addition by SANS experiments with internal contrast variation.

J. Appl. Cryst. (2007). 40, s245-s249
doi: 10.1107/S002188980700252X
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A systematic evaluation of the accuracy of molecular mass determination of proteins using small-angle X-ray scattering.

Colloids, surfactants and liquids

J. Appl. Cryst. (2007). 40, s250-s253
doi: 10.1107/S0021889807009016
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The short-time diffusion of a magnetic charge-stabilized colloidal suspension in the absence of an external applied magnetic field has been investigated by means of X-ray photon correlation spectroscopy.

J. Appl. Cryst. (2007). 40, s254-s258
doi: 10.1107/S0021889807009600
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This work reports the synthesis and the characterization by small-angle scattering of polarized neutrons of ferrofluids consisting of ferrite nanoparticles coated by dodecanoic acid and dispersed in cyclohexane.

J. Appl. Cryst. (2007). 40, s259-s263
doi: 10.1107/S0021889807018882
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The gaps among the stacks of multilamellar vesicles used for the synthesis of nanoparticles are shown and characterized by ASAXS and freeze-fracture methods.

J. Appl. Cryst. (2007). 40, s264-s268
doi: 10.1107/S0021889807017888
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The small-angle X-ray scattering from dual-surfactant aqueous solutions made from sodium lauryl ether sulfate and coconut fatty acid amido propyl betaine was systematically measured as a function of the net sodium cation concentration and the surfactant concentration. The low-q behaviour of the form factor was consistent with long rigid cylinders while the middle- and high-q profiles fitted well with a core–shell cylinder model.

J. Appl. Cryst. (2007). 40, s269-s273
doi: 10.1107/S0021889807009181
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Mixed colloidal dispersions of clay platelets and magnetic nanoparticles were investigated using small-angle X-ray and neutron scattering. The main contribution to the scattering is due to the magnetic nanoparticles. The scattering intensities are proportional to the concentration of magnetic particles, thus from the scattering point of view the sample is a colloidal dispersion of non-interacting magnetic objects, although the laponite and magnetic particles clearly interact when the sample textures are observed in an optical microscope. The phase separation may be characterized as a liquid–gas transition.

J. Appl. Cryst. (2007). 40, s274-s278
doi: 10.1107/S0021889807008151
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The structure and oligomerization of sodium bis(2-ethylhexyl)sulfosuccinate water-in-oil microemulsion under the presence of monovalent and divalent salts in the water pool are dominated not only by the electrostatic effect between polar headgroups but also by the hydration effect by salts.

J. Appl. Cryst. (2007). 40, s279-s282
doi: 10.1107/S0021889807011958
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Examination of the relative intensity of the X-ray 220 reflection with respect to the 211 reference peak as a function of the alkoxy chain length of the title compounds enables the internal structure of the thermotropic Ia3d cubic phase to be clarified.

J. Appl. Cryst. (2007). 40, s283-s285
doi: 10.1107/S0021889807017852
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The dynamics of Au nanoparticles suspended in mixtures of water and glycerol are investigated by X-ray fluorescence correlation spectroscopy. The contrast of the measured time-correlation functions scales as expected with the Au particle concentration. The time constants for translational diffusion and sedimentation in water/glycerol show only qualitative agreement with the expected values.

J. Appl. Cryst. (2007). 40, s286-s291
doi: 10.1107/S0021889807008552
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Small-angle X-ray scattering is used to investigate the meso-structure of dry-pressed samples of nano-layered platelet-shaped clay particles, as water is absorbed into individual particles. The orientational order of the assembly is nematic. Orientation distributions are monitored and show a moderate decrease of this order with water uptake.

J. Appl. Cryst. (2007). 40, s292-s296
doi: 10.1107/S0021889807010825
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Precise characterization of the phase diagram for suspensions of sodium fluorohectorite colloids in saline solutions is achieved from small-angle X-ray scattering measurements. Radial intensity profiles are also addressed.

J. Appl. Cryst. (2007). 40, s297-s302
doi: 10.1107/S0021889806055191
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Structural models are developed for the metastable phases of saturated/unsaturated triacylglycerols appearing at the very beginning of crystallization from the melt based on experimental time-resolved SAXS/WAXS studies of isothermal crystallization in various fats.

J. Appl. Cryst. (2007). 40, s303-s306
doi: 10.1107/S0021889807010345
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The addition of colloidal particles between lamellar membrane slits induced a repulsive interlamellar interaction which showed a unique interlamellar distance dependence.

J. Appl. Cryst. (2007). 40, s307-s311
doi: 10.1107/S0021889807001483
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Aqueous solutions of 1,2-pentanediol, 1,5-pentanediol, 1,2-hexanediol and 1,6-hexanediol have been studied by small-angle neutron scattering, and the results analysed with the help of the Kirkwood–Buff formalism. The 1,2-hexanediol solutions exhibit the strongest attractive diol–diol interaction and the excess coordination numbers are in agreement with the possibility of forming micelles.

J. Appl. Cryst. (2007). 40, s312-s317
doi: 10.1107/S002188980700859X
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Sphingomyelin is one of the major sphingolipid components of many animal plasma membranes. SAXS and XRD studies revealed that N-lignocerol (C24:0) sphingomyelin bilayers have a ripple phase and an additional low-temperature stable phase.

J. Appl. Cryst. (2007). 40, s318-s320
doi: 10.1107/S0021889807008138
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Small-angle X-ray scattering measurements of water droplets in a mist were carried out using the BL15XU beamline at SPring-8.

J. Appl. Cryst. (2007). 40, s321-s326
doi: 10.1107/S0021889807006723
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An analytical model for the structure factor, based on an effective interaction potential made of an attractive Yukawa term plus a repulsive Yukawa term, has been applied to charged proteins and copolymer micellar solutions.

J. Appl. Cryst. (2007). 40, s327-s331
doi: 10.1107/S0021889807005201
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Using time-resolved small-angle neutron scattering it is possible to extract the equilibrium exchange kinetics of polymeric micelles. This paper provides insight into the effect of topological constraints on the expulsion time by comparing results from A-B diblock and A-B-A triblock copolymer micelles.

J. Appl. Cryst. (2007). 40, s332-s334
doi: 10.1107/S0021889807013568
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The time evolution of the small-angle scattering of the lamellar phase of a nonionic surfactant C16H33(OC2H4)7OH (C16E7) in D2O at a constant shear rate (0.3–30 s−1) is measured. The results indicate a discontinuous decrease in the repeat distance and so suggest some sort of transition.

Fibre diffraction

J. Appl. Cryst. (2007). 40, s335-s340
doi: 10.1107/S0021889807005523
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The depth-profiled ultrastructure of the collagen fibrillar matrix in the swollen human eye-bank cornea was studied by microbeam small-angle X-ray scattering at a spatial resolution of 25 µm to provide information about collagen fibril diameter, spacing and orientation.

Grazing-incidence small-angle scattering

J. Appl. Cryst. (2007). 40, s341-s345
doi: 10.1107/S0021889806048369
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Large-scale structures in polymer-blend films are probed by grazing-incidence ultra-small-angle X-ray scattering. By using flow the structural complexity is increased and sub-microbeam grazing-incidence small-angle X-ray scattering allows the local structure to be probed.

J. Appl. Cryst. (2007). 40, s346-s349
doi: 10.1107/S0021889807007716
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A gradient in a colloidal thin film prepared from solution is investigated using microbeam grazing-incidence small-angle X-ray scattering. A cross-over and oscillation between a complete layer and depleted regions are detected.

J. Appl. Cryst. (2007). 40, s350-s354
doi: 10.1107/S0021889806043755
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The morphology of nanocavities and {113} defects formed by implantation of neon and helium ions in Si(001) is investigated by means of grazing incidence small-angle X-ray scattering experiments.

J. Appl. Cryst. (2007). 40, s355-s360
doi: 10.1107/S0021889807001331
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Self-assembled films of hydrophobin HFBIII from the fungus Trichoderma reesei were studied at an air/water interface and on a solid substrate using grazing-incidence X-ray diffraction and reflectivity.

J. Appl. Cryst. (2007). 40, s361-s362
doi: 10.1107/S0021889806056184
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Poly[(n-nonyl-2-oxazoline)-b-(methyl-2-oxazoline)] diblock copolymers in aqueous solution form micelles of core-shell type. The core block is stretched, whereas the shell block is coiled.

J. Appl. Cryst. (2007). 40, s363-s366
doi: 10.1107/S0021889806053180