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Results for “Scattering, Small Angle”

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At least 289 records · Page 16Linked to original sources

PubMed2003

De-mixing dynamics of a binary liquid system in a controlled-pore glass. A neutron spin-echo spectroscopy and small angle neutron scattering study.

The temperature-induced microphase separation of the binary liquid system iso-butyric acid+heavy water (iBA + D(2)O) in a mesoporous silica glass (CPG-10-75) of nominal pore width 7.5 nm was investigated by neutron spin-echo spectroscopy (NSE) and neutron small-angle scattering (SANS). Two mixtures of different composition were studied at different scattering angles at temperatures above and below the bulk phase transition temperature. The phase separation in the pore space is found to occur at a lower temperature than the bulk transition and extends over a significant temperature range. The effective diffusion coefficient derived from NSE at low scattering angles is found to decrease by one order of magnitude from 70 degrees C to 20 degrees C. This observation is attributed to the growing size of concentration fluctuations having a cut-off at ca. 8 nm, which corresponds to the mean pore size. The dynamics of the concentration fluctuations appears to be strongly influenced by the confinement in the pores, as it differs strongly from the bulk behaviour. These results are consistent with the preliminary results of the SANS study.

Journal Article↗

PubMedDate not supplied

Phase separation in a sheared gelatin/maltodextrin mixture studied by small-angle light scattering.

The influence of shear on the structure of a gelatin/maltodextrin mixture was investigated using small-angle light scattering both during phase separation and after phase separation was allowed to occur quiescently. In all cases, phase separation occurred via spinodal decomposition to form a droplet morphology, and a characteristic length scale was formed in the structure that was prevalent during shear, as well as in quiescent conditions. Below the critical shear rate for droplet breakup, shear accelerated the coarsening rate of the droplets. A transient regime of rapid hydrodynamic coarsening was present when shear was initiated after phase separation and at late times in all cases once the droplets attained a certain size. At the critical shear rate for droplet breakup (1 s(-1)), the rapid repetition of breakup and coarsening was postulated to occur, which enabled a microstructure consisting of elongated droplets with a narrow size distribution to form. When the shear rate enabled droplets to extend to such an extent that a percolated structure could form (10 s(-1)), then the structure was relatively stable and changed very slowly over time. At very high shear rates (100 s(-1)), droplet breakup was suppressed and a highly fibrillar morphology formed that was stable only while the system was under shear. Cessation of shear at high rates led to fiber breakup and the formation of many small droplets. For a given shear rate, the final microstructure appeared to be independent of the time that shear was started when the structure consisted of discrete droplets or fibers. When a percolated structure could form, however, the shear history appeared to be important.

Gelatin↗

PubMed1998

Repulsive interparticle interactions in a denatured protein solution revealed by small angle neutron scattering.

In order to investigate the effect of concentration in biological processes such as protein folding, small angle neutron scattering measurements were used to determine the second virial coefficient of solutions of both native and strongly denatured phosphoglycerate kinase and the radius of gyration of the protein at zero concentration. The value of the second virial coefficient is a good probe of the non-ideality of a solution. The present results show that the unfolding of the protein leads to a drastic change in the repulsive intermolecular interactions. We conclude that these interactions are due mainly to the behaviour of the denatured polypeptide chain as an excluded volume polymer.

Fungal Proteins↗

PubMed2005

Small-angle neutron scattering of ionic perfluoropolyether micellar solutions: role of counterions and temperature.

This paper reports a small-angle neutron scattering (SANS) characterization of perfluoropolyether (PFPE) aqueous micellar solutions with lithium, sodium, cesium and diethanol ammonium salts obtained from a chlorine terminated carboxylic acid and with two perfluoroisopropoxy units in the tail (n(2)). The counterion and temperature effects on the micelle formation and micellar growth extend our previous work on ammonium and potassium salts n(2) micellar solutions. Lithium, sodium, cesium and diethanol ammonium salts are studied at 0.1 and 0.2 M surfactant concentration in the temperature interval 28-67 degrees C. SANS spectra have been analyzed by a two-shell model for the micellar form factor and a screened Coulombic plus steric repulsion potential for the structure factor in the frame of the mean spherical approximation of a multicomponent system reduced to a generalized one component macroions system (GOCM). At 28 degrees C, for all the salts, the micelles are ellipsoidal with an axial ratio that increases from 1.6 to 4.2 as the counterion volume increases. The micellar core short axis is 13 A and the shell thickness 4.0 A for the alkali micelles, and 14 and 5.1 A for the diethanol ammonium micelles. Therefore, the core short axis mainly depends on the surfactant tail length and the shell thickness on the carboxylate polar head. The bulky diethanol ammonium counterion solely influences the shell thickness. Micellar charge and average aggregation number depend on concentration, temperature and counterion. At 28 degrees C, the fractional ionization decreases vs the counterion volume (or molecular weight) increase at constant concentration for both C = 0.1 M and C = 0.2 M. The increase of the counterion volume leads also to more ellipsoidal shapes. At C = 0.2 M, at 67 degrees C, for sodium and cesium micelles the axial ratio changes significantly, leading to spherical micelles with a core radius of 15 A, lower average aggregation number, and larger fractional ionization.

Journal Article↗

PubMed2006

Combining small angle neutron scattering (SANS) and fluorescence correlation spectroscopy (FCS) measurements to relate diffusion in agarose gels to structure.

Small angle neutron scattering (SANS) and fluorescence correlation spectroscopy (FCS) measurements were carried out on agarose hydrogels to link their microscopic structure to the diffusivity of solutes at different scales. SANS allowed for the determination of the distribution of void volumes within the gels. They were shown to be compatible with a random network of cylindrical fibers as described by the Ogston model. FCS measured solute diffusivity in spaces similar in size to the void volumes, and thus, the results reflected the gel heterogeneity. Solute diffusivity was predicted by modeling the gel as microscopic geometrical cells. Variations in the diffusivity of solutes of different sizes could be predicted from the structural parameters of the gel using theory, taking into account obstruction by cylindrical cells and solute hydrodynamics. Prediction of the FCS autocorrelation functions for solutes from a cell model demonstrated a lack of sensitivity of this technique for multicomponent analysis.

Biophysics↗

PubMed1995

Evidence for elongation of the helical pitch of the RecA filament upon ATP and ADP binding using small-angle neutron scattering.

Structural changes of the RecA filament upon binding of cofactors have been investigated by small-angle neutron scattering. Both ATP and ADP increased the helical pitch of the RecA homopolymer, which is observed to be 7 nm in the absence of any cofactor. The binding of ATP altered the pitch to 9 nm, whereas the binding of ADP only produced a pitch of 8.2 nm. The pitch determined for the RecA complex with the ATP analog adenosine 5'-[gamma-thio]triphosphate was similar to that found with ATP. Thus, at least three, somewhat different. RecA helical filamentous structures may form in solution. The binding of DNA to RecA did not alter the pitch significantly, indicating that the cofactor binding is the determining factor for the size of the helical pitch of the RecA filament. We also found that elongation of the helical pitch is a necessary, but not a sufficient condition, for the coprotease activity of RecA. The presence of acetate or glutamate ions is also required. The pitch of the ADP.RecA filament is in agreement with that found in the crystal structure. This correlation indicates that this structure corresponds to that of the ADP.RecA filament in solution, although this is not the species active in recombination.

Adenosine Diphosphate↗

PubMedDate not supplied

Small-angle light scattering and birefringence properties of chick cornea.

PURPOSE: Techniques employing polarized light propagation and scattering are useful in examining the cornea's lamellar structure. Recent advances in theoretical methods have significantly increased the ability to relate features of lamellar arrangements to measurements of transmitted polarized light. The chick cornea, because of its hypothesized structure of a gradual helical rotation of lamellar pairs, presents an interesting model for further development of this methodology. METHODS: Small-angle light scattering (SALS) and polarized transmission measurements were made on 7-week-old chick corneas under conditions that closely approximate the physiological state. Birefringence properties were determined from the transmission measurements and compared to the results of model calculations of polarized light propagating through lamellae organized according to the hypothesized structure for chick cornea. RESULTS: The I+ small-angle light scattering pattern had 4 cloverleaf lobes aligned with the crossed polarizer and analyzer axes. The lobes disappeared when the transcorneal pressure was increased from zero to 18 mmHg. Retardation measured at 18 mmHg was very small (approximately 0.01 microm). CONCLUSION: The disappearance of the I+ small-angle light scattering pattern when IOP is increased suggests that the lamellae undulate in their relaxed state and the undulations straighten when IOP is increased. Measured birefringence properties are consistent with the hypothesized lamellar structure.

Animals↗

PubMed2005

Novel self-assembly of amphiphilic copolymers into nanotubes: characterization by small-angle neutron scattering.

The self-assembly into nanotubes in solution of an amphiphilic copolymer is characterized by small-angle neutron scattering (SANS). This study confirmed the shape and the size of the tubular association and the 3-D association of the tubes predicted by molecular orbital theory. Moreover, the characterization of the stability of the association has revealed that the addition of a very small amount of salt to the solution increases the size of the association. When more salt is added, the size of the association decreases, and the structure is altered. The association was found to be independent of temperature and therefore is very stable.

Chemistry↗

PubMed2006

Surface versus confinement induced morphology transition in triblock copolymer films: a grazing incidence small angle neutron scattering investigation.

The internal nanostructure resulting from microphase separation in triblock copolymer films of polyparamethylstyrene-block-polystyrene-block-polyparamethylstyrene, P(pMS-b-Sd8-b-pMS), has been investigated with grazing incidence small angle neutron scattering (GISANS). X-ray reflectivity, grazing incidence small-angle X-ray scattering (GISAXS), optical microscopy and atomic force microscopy (AFM) complement the investigation. The influence of two limiting interfaces present in confinement is compared to the presence of only one surface. GISANS allows for the detection of structures in the very limited sample volume of confined films as well as for a depth sensitivity to probe the near free surface part of bulk films. With respect to the surface a perpendicular oriented lamella is observed. In contrast to the shrinkage of the characteristic lamellar spacing in confinement at the free surface, a slight increase is determined.

Journal Article↗

PubMed2005

Specular X-ray reflectivity and small angle neutron scattering for structure determination of ordered mesoporous dielectric films.

Specular X-ray reflectivity (SXR) and small-angle neutron scattering (SANS) are used to characterize the structure of a thin film containing cylindrical mesopores. The 3-D structure of the mesoporous film was determined from SANS measurements taken at multiple rotation angles between the incident beam and the film. The film was found to be composed of a randomly packed core and surface layers within which the hollow cylinders were regularly packed and oriented along the surface. The packing of the cylindrical mesopores was not hexagonal but rather rectangular with a conical angle of 55.7 degrees instead of 60 degrees expected for hexagonal packing. The extent of the planar orientation of the cylindrical mesopores within the surface layers was estimated from the width of the Bragg reflection in the SXR result to be about 25 repeating layers at both interfaces. This was further confirmed from cross-section transmission electron microscopy (TEM) results. The SXR results of this film exhibit an anomalous decrease in reflected intensity after each Bragg reflection. This anomaly in SXR can be modeled in a Parratt formulism using a depth profile composed of two characteristic lengths, the repeating distance among layers and the curvature of the density profile of each layer.

Journal Article↗

PubMed2005

Small-angle neutron scattering studies of an adsorbed non-ionic surfactant (C12E24) on hydrophobised silica particles in water.

Small-angle neutron scattering (SANS) studies of aqueous dispersions of Stöber silica particles (which have been hydrophobised by having 1-octadecanol grafted to their surface), carrying an adsorbed layer of the nonionic surfactant C12E24, in water, have been performed as a function of temperature. Using mixtures of D2O and H2O, the composition of the continuous phase was adjusted to have the same scattering length density as the silica particles. Hence, only the scattering from the 1-octadecanol and C12E24 layers was detected. The data have been analyzed using both a surface Guinier analysis and a two-layer structure model. It has been found that a step profile best describes the inner combined adsorbed layer (1-octadecanol grafted chains, plus the penetrating alkyl chains from the surfactant) and a semi-Gaussian profile the extended poly(ethylene oxide) outer layer. Both analyses demonstrated that the combined surface layer contracted with increasing temperature.

Journal Article↗

PubMed1994

The triple isotopic substitution method in small angle neutron scattering. Application to the study of the ternary complex EF-Tu.GTP.aminoacyl-tRNA.

The TIS (triple isotopic substitution) method in small angle neutron scattering was applied to determine the radius of gyration of polypeptide elongation factor Tu (EF-Tu) from E. coli associated with GDP and within the ternary complex EF-Tu.GTP.aminoacyl-tRNA. The results showed that, within errors of about 1 A, there is no change in the radius of gyration of the EF-Tu moiety upon ternary complex formation. Experiments were performed in H2O buffer, in which complex formation could be followed on an absolute scale because of the relatively large contrast of both protein and tRNA. The TIS method is based on the analysis of a scattering curve that is the difference between the scattering of two solutions containing appropriately deuterium labelled particles. A necessary condition for the application of the method is that the two solutions are identical in all respects except for the extent of deuterium label. The main properties of TIS that make it very useful for the study of complex particles in solution were confirmed by this study. These are the elimination of interparticle effects in the difference curve, the 'invisibility' of unlabelled parts of the particles and the independence of the difference scattering curve on the buffer 2H2O-H2O content. The last property is of particular interest for the study of interactions that may be influenced by 2H2O, since, contrary to classical contrast variation methods, TIS experiments can be performed in H2O buffer alone.

Guanosine Triphosphate↗

PubMed2005

Small-angle neutron scattering study of temperature-induced emulsion gelation: the role of sticky microgel particles.

In this work, small-angle neutron scattering (SANS) is used to probe the structural transformations that accompany temperature-induced gelation of emulsions stabilized by a temperature-responsive polymer. The latter is poly(NIPAM-co-PEGMa) (N-isopropylacrylamide and poly(ethyleneglycol) methacrylate) and contains 86 mol% NIPAM. Turbidity measurements revealed that poly(NIPAM-co-PEGMa) has a lower critical solution temperature (T(LCST)) of 36.5 degrees C in D(2)O. Aqueous polymer solutions were used to prepare perfluorodecalin-in-water emulsions (average droplet size of 6.9 mum). These emulsions formed gels at 50 degrees C. SANS measurements were performed on the poly(NIPAM-co-PEGMa) solutions and emulsions as a function of temperature. The emulsion was also prepared using a D2O/H2O mixture containing 72 vol% D2O in order to make scattering from the droplets negligible (on-contrast). The SANS data were analyzed using a combination of Porod and Ornstein-Zernike form factors. The results showed that the correlation length (xi) of the polymer scaled as xi approximately phi(p)(-0.68) at 32 degrees C, where phi(p) is the polymer volume fraction. The xi value increased for all systems as the temperature increased, which was attributed to a spinodal transition. At temperatures greater than T(LCST), the polymer solution changed to a polymer dispersion of poly(NIPAM-co-PEGMa) aggregates. The aggregates have features that are similar to microgel particles. The average size of these particles was estimated as 160-170 nm. The particles are "sticky" and are gel-forming. The on-contrast experiments performed using the emulsion indicated that the interfacial polymer chains condensed to give a relatively thick polymer layer at the perfluorodecalin-water interface at 50 degrees C. The gelled emulsions appear to consist of perfluorodecalin droplets with an encapsulating layer of collapsed polymer to which sticky microgel particles are adsorbed. The latter act as a "glue" between coated droplets in the emulsion gel.

Journal Article↗

PubMed2000

A study on structural and diffusion properties of porcine stratum corneum based on very small angle neutron scattering data.

PURPOSE: Generation of valuable information about the biphasic geometrical configuration of porcine stratum corneum from Very Small Angle Neutron Scattering (VSANS) data and investigation of its effect on the corresponding effective diffusivity. METHODS: Spectra of porcine stratum corneum are mathematically transformed in order to obtain the corresponding auto-correlation function (ACF). Model stratum corneum structures, matching this experimentally determined ACF, are then produced based on the "brick-and-mortar" configuration. The effective diffusivity through these model domains is calculated using an appropriate numerical method. RESULTS: The most appropriate geometry of porcine stratum corneum's lipid and protein phases in a "brick-and-mortar" configuration is quantitatively determined and correlated with the barrier properties (diffusivity) of the stratum corneum model structures. CONCLUSIONS: The ACF analysis indicates the most appropriate values for the dimensions of the corneocyte thickness and the surrounding lipid gap, while the corneocyte length is estimated from the diffusion study.

Animals↗

PubMed2004

Small-angle neutron scattering study on microstructure of poly(N-isopropylacrylamide)-block-poly(ethylene glycol) in water.

By employing small-angle neutron scattering (SANS), we investigated the microstructures of, poly(N-isopropylacrylamide) (PNIPA)-block-poly(ethylene glycol) (PEG) (NE) in deuterated water D2O, as related to macroscopic behaviors of fluidity, turbidity and synerisis. SANS revealed following results: (i) microphase separation occurs at around above 17 degrees C in a temperature range of transparent sol below 30 degrees C. In the microdomain appeared in the transparent sol state, both block chains of PNIPA and PEG are swollen by water; (ii) for the NE solution of polymer concentration W(p)>3.5% (w/v), corresponding to opaque gel above 30 degrees C, a percolated structure, i.e., network-like domain is formed by NE as a result of macrophase separation due to dehydration of the PNIPA chains. As the temperature increases toward 40 degrees C, the network domain is squeezed along a direction parallel to the NE interface, which leads to increase of the interfacial thickness given by swollen PEG chains and to the macroscopic synerisis behavior.

Acrylic Resins↗

PubMed2002

Diffusing wave spectroscopy and small-angle neutron scattering from concentrated colloidal suspensions.

We have studied the properties of dense colloidal suspensions with a combination of small-angle neutron scattering (SANS) and diffusing wave spectroscopy (DWS). Contrary to single light scattering, DWS provides dynamic information on length scales, from 1 to 100 nm, comparable to SANS. This offers a unique range of accessible length and time scales perfectly suited for the (noninvasive) investigation of highly concentrated systems. By this we obtain valuable information about the structural properties and the short-time diffusion of electrostatically stabilized, but strongly screened, hard-sphere-like colloidal suspensions with volume fractions up to 30%. We furthermore discuss the consequences of local structural ordering on the optical properties, such as optical density and polarization. Quantitative agreement is found when comparing transmission measurements (optical density) with parameter-free numerical calculations based on the structural characterization from SANS.

Biophysics↗

PubMed1984

Structure of the capsid of Kilham rat virus from small-angle neutron scattering.

The structure of empty capsids of Kilham rat virus, an autonomous parvovirus with icosahedral symmetry, was investigated by small-angle neutron scattering. From the forward scatter, the molecular weight was determined to be 4.0 X 10(6), and from the Guinier region, the radius of gyration was found to be 105 A in D2O and 104 A in H2O. On the basis of the capsid molecular weight and the molecular weights and relative abundances of the capsid proteins, we propose that the capsid has a triangulation number of 1. Extended scattering curves and mathematical modeling revealed that the capsid consists of two shells of protein, the inner shell extending from 58 to 91 A in D2O and from 50 to 91 A in H2O and containing 11% of the capsid scattering mass, and the outer shell extending to 121 A in H2O and D2O. The inner shell appears to have a higher content of basic amino acids than the outer shell, based on its lower scattering density in D2O than in H2O. We propose that all three capsid proteins contribute to the inner shell and that this basic region serves DNA binding and partial charge neutralization functions.

Amino Acids↗

PubMed1984

Small angle light scattering by large spheroids. Comparison with patterns from erythrocytes under shear.

The physical optics approximation has been used to compute small angle light scattering patterns from spheroids regarged as models for deformed red cells. According to their orientation, diagrams have been obtained whose fine structure can be very different from that resulting of the classical diffraction (existence of maxima and minima of intensity along the rings). Some experimental results for red cells suspensions under shear are shown which exhibit features very similar to the theoretical ones.

Erythrocytes↗