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PubMedDate not supplied

X-ray diffraction computed tomography.

Coherent scattering of x-ray photons leads to the phenomenon of x-ray diffraction, which is widely used for determining atomic structure in materials science. A technique [x-ray diffraction computed tomography (CT)] is described, analogous to conventional CT, in which the x-ray diffraction properties of a stack of two-dimensional object sections may be imaged. The technique has been investigated using a first generation (single pencil beam) CT scanner to measure small angle coherent scatter, in addition to the customary transmitted radiation. Diffraction data from a standard CT performance phantom obtained with this new technique and with an x-ray diffractometer are compared. The agreement is satisfactory bearing in mind the poor momentum resolution of our apparatus. The dose and sensitivity of x-ray diffraction CT are compared with those of conventional transmission CT. Diffraction patterns of some biological tissues and plastics presented in a companion paper indicate the potential of x-ray diffraction CT for tissue discrimination and material characterization. Finally, possibilities for refinement of the technique by improving the momentum resolution are discussed.

Computers↗

PubMed2001

The origins of stability of spontaneous vesicles.

Equilibrium unilamellar vesicles are stabilized by one of two distinct mechanisms depending on the value of the bending constant. Helfrich undulations ensure that the interbilayer potential is always repulsive when the bending constant, K, is of order k(B)T. When K k(B)T, unilamellar vesicles are stabilized by the spontaneous curvature that picks out a particular vesicle radius; other radii are disfavored energetically. We present measurements of the bilayer elastic constant and the spontaneous curvature, R(o), for three different systems of equilibrium vesicles by an analysis of the vesicle size distribution determined by cryo-transmission electron microscopy and small-angle neutron scattering. For cetyltrimethylammonium bromide (CTAB)/sodium octyl sulfonate catanionic vesicles, K =.7 k(B)T, suggesting that the unilamellar vesicles are stabilized by Helfrich-undulation repulsions. However, for CTAB and sodium perfluorooctanoate (FC(7)) vesicles, K = 6 k(B)T, suggesting stabilization by the energetic costs of deviations from the spontaneous curvature. Adding electrolyte to the sodium perfluorooctanoate/CTAB vesicles leads to vesicles with two bilayers; the attractive interactions between the bilayers can overcome the cost of small deviations from the spontaneous curvature to form two-layer vesicles, but larger deviations to form three and more layer vesicles are prohibited. Vesicles with a discrete numbers of bilayers at equilibrium are possible only for bilayers with a large bending modulus coupled with a spontaneous curvature.

Alkanesulfonic Acids↗

PubMed1993

Configurational distribution of denatured phosphoglycerate kinase.

Physiochemical characterization of the denatured states of proteins is important for a complete understanding of the factors stabilizing their folded conformations. Using a combination of small angle neutron scattering (SANS), statistical mechanical modelling and molecular mechanics calculations, we examine the configurational distribution of phosphoglycerate kinase denatured in 4 M guanidine hydrochloride solution. The denaturing of the protein produces a clear change in the form of the SANS profile and a large increase of the radius of gyration. In the statistical mechanical model, the region of contrast neutron scattering density associated with the protein is pictured as a chain of freely jointed spheres. The model is fitted to the SANS data for the denatured protein. It is found that a model with a small number of spheres cannot account for the higher resolution scattering, indicating an absence of detectable structuration; a good fit is found with 100 spheres of 8.5 A radius. Single configurations of the fitted chain of spheres are used as low-resolution bounds for model-building and molecular mechanics calculations to obtain plausible atomic-detail models of the denatured chain.

Computer Simulation↗

PubMed2001

An innovative digital imaging set-up allowing a low-dose approach to phase contrast applications in the medical field.

Recently, new imaging modalities based on the detection of weak phase perturbations effects, among which are phase contrast and diffraction imaging, have been developed by several researchers. Due to their high sensitivity to weakly absorbing details, these techniques seem to be very promising for applications in the medical field. On the other hand, digital radiology is undergoing a wide diffusion, and its benefits are presently very well understood. Up to now, however, the strong pixel size constraints associated with phase contrast pattern detection limited the possibility of exploiting the advantages of phase contrast in digital radiology applications. In this paper, an innovative setup capable of removing the pixel size constraints, and thus opening the way to low dose digital phase contrast imaging, is described. Furthermore, we introduce an imaging technique based on the detection of radiation scattered at small angles: the information extracted from the sample is increased at no dose expense. We believe that several radiological fields, mammography being the first important example, may benefit from the herein described innovative imaging techniques.

Diagnostic Imaging↗

PubMed1999

Thermal aggregation of patatin studied in situ.

In this work dynamic light scattering was used to study the thermal aggregation of patatin in situ, to elucidate the physical aggregation mechanism of the protein and to be able to relate the aggregation behavior to its structural properties. The dependence of the aggregation rates on the temperature and the ionic strength suggested a mechanism of slow coagulation, being both diffusion and chemically limited. The aggregation rate dependence on the protein concentration was in accordance with the mechanism proposed. The aggregation rates as obtained at temperatures ranging from 40 to 65 degrees C correlated well with unfolding of the protein at a secondary level. Small-angle neutron scattering and dynamic light scattering results were in good accordance; they revealed that native patatin has a cylindrical shape with a diameter and length of 5 and 9.8 nm, respectively.

Carboxylic Ester Hydrolases↗

PubMed2004

Effect of the hydrophilic size on the structural phases of aqueous nonionic gemini surfactant solutions.

Aggregate structures of aqueous nonionic Gemini surfactant solutions, alpha,alpha'-[2,4,7,9-tetramethyl-5-decyne-4,7-diyl]bis[omega-hydroxyl-polyoxyethylene] with three different length polyoxyethylenes (i.e., 10, 20, and 30 ethylene oxide monomers, denoted from now on as S-10, S-20, and S-30, respectively), are investigated using small angle neutron scattering, dynamic light scattering, and fluorescence spectroscopy. For S-10 at low surfactant concentrations (Cs < 0.9 wt %), large "clusters", with an average hydrodynamic radius (RH) > 40 nm, are found to coexist with monomers. At intermediate Cs (0.9 < Cs < 2 wt %), some clusters break down forming micelles, with an (RH) approximately 2-3 nm, while the remaining clusters coexist with micelles. Increasing Cs further (>2 wt %) results in a pure micellar phase with little or no clusters present. S-20 and S-30 mixtures, on the other hand, differ from S-10 in that irrespective of surfactant concentration, large clusters and small monomers/dimers are found to coexist, while there is no direct evidence for the presence of micelles.

Light↗

PubMed2000

Clipped random wave analysis of isometric lamellar microemulsions

We have made small angle neutron scattering studies of C10E4-D2O-octane isometric microemulsions in the lamellar phase at the hydrophile-lipophile balance temperature. The scattering intensity distributions were then analyzed with a particular choice of a spectral density function (SDF) derived by maximization of generalized entropy. The model agrees well with the measured intensities on an absolute scale, and allowed us to derive various length scales associated with the microemulsion mesoscopic structure as well as the average interfacial curvatures. We also used the experimentally determined SDF to generate a three-dimensional snapshot of the fluctuating microemulsion microstructure. Unlike conventional pictures of extended lamellar planes, we observed small domains which were internally lamellar but randomly oriented with respect to each other. Finally, we computed the probability distributions of the mean curvature H and the Gaussian curvature K on the oil-water interface. The former showed a symmetric distribution centered around H = 0, while the latter showed a skewed distribution peaked at a negative value of K, but with a wing extending to positive values.

Journal Article↗

PubMed2005

Phase behavior and local dynamics of concentrated triblock copolymer micelles.

We report a neutron-scattering study to characterize the ordering and local dynamics of spherical micelles formed by the triblock copolymer polyethylene oxide (PEO)--polypropylene oxide (PPO)--polyethylene oxide (Pluronic) in aqueous solution. The study focuses on two Pluronic species, F68 and F108, that have the same weight fraction of PEO but that differ in chain length by approximately a factor of 2. At sufficiently high concentration, both species undergo a sequence of phase changes with increasing temperature from dissolved chains to micelles with liquid-like order to a cubic crystal phase and finally back to a micelle liquid phase. A comparison of the phase diagrams constructed from small-angle neutron scattering indicates that crystallization is suppressed for shorter chain micelles due to fluctuation effects. The intermediate scattering function I(Q,t)I(Q,0) determined by neutron spin echo displays a line shape with two distinct relaxations. Comparisons between I(Q,t)I(Q,0) for fully hydrogenated F68 chains in D2O and for F68 with deuterated PEO blocks reveal that the slower relaxation corresponds to Rouse modes of the PPO segments in the concentrated micelle cores. The faster relaxation is identified with longitudinal diffusive modes in the PEO corona characteristic of a polymer brush.

Journal Article↗

PubMed2006

Phase separation in binary polymer/liquid crystal mixtures: network breaking and domain growth by coalescence-induced coalescence.

A small-angle light scattering (SALS) technique together with optical microscopy observation are used to investigate phase separation kinetics in films of low molecular weight thermotropic liquid crystal (4-cyano-4'-n-octyl-biphenyl, 8CB) with flexible polymer (polystyrene, PS). The growth of domains is studied as a function of time, film thickness, and film composition. The light scattering results are correlated with the images obtained by optical microscopy observation. In this paper, we study the breaking of a bicontinuous network of polymer in liquid crystal into droplets and their further growth via the coalescence-induced coalescence mechanism. The appearance of droplets in the system leads to a strong scattering at small wave vectors, while the bicontinuous network gives a peak at a nonzero wave vector. Superposition of these scattering intensities leads to the appearance of a second peak in the full scattering intensity signal, when the bicontinuous network starts to break up into disjointed elongated domains. Finally, both peaks merge into a single peak, which moves quickly toward zero wave vectors, indicating a complete transformation of elongated domains into spherical droplets of variable size. We found that the separation process does not depend on the size of the system. Irrespective of the sample thickness, the network breaks into fragments always at the same time after temperature quench. On the basis of morphological analysis, we found that the average size of the droplets which formed from the network grows with time, t, as t(alpha), alpha = 0.9 +/- 0.1, in the isotropic phase and in the nematic phase.

Journal Article↗

PubMedDate not supplied

Frozen spin targets in ribosomal structure research.

Polarized neutron scattering strongly depends on nuclear spin polarisation, particularly on proton spin polarisation. A single proton in a deuterated environment then is as efficient as 10 electrons in X-ray anomalous diffraction. Neutron scattering from the nuclear spin label is controlled by the polarisation of neutron spins and nuclear spins. Pure deuteron spin labels and proton spin labels are created by NMR saturation. We report on results obtained from the large subunit of E. coli ribosomes which have been obtained at the research reactor of GKSS using the polarized target facility developed by CERN. The nuclear spins were oriented with respect to an external field by dynamic nuclear polarisation. Proton spin polarisations of more than 80% were obtained in ribosomes at temperatures below 0.5 K. At T = 130 mK the relaxation time of the polarized target is one month (frozen spin target). Polarized small-angle neutron scattering of the in situ structure of rRNA and the total ribosomal protein (TP) has been determined from the frozen spin targets of the large ribosomal subunit, which has been deuterated in the TP and rRNA respectively. The results agree with those from neutron scattering in H2O/D2O mixtures obtained at room temperature. This is a necessary prerequisite for the planned determination of the in situ structure of individual ribosomal proteins and especially of that of ribosome bound mRNA and tRNAs.

Deuterium↗

PubMed2006

Aqueous block copolymer-surfactant mixtures and their ability in solubilizing chlorinated organic compounds. A thermodynamic and SANS study.

Within the topic of surfactant enhanced solubilization of additives sparingly soluble in water, volumetric, solubility, conductivity, and small-angle neutron scattering (SANS) experiments on mixtures composed of alpha,omega-dichloroalkane, surfactant, copolymer, and water were carried out at 298 K. The triblock copolymers (ethylene oxide)132(propylene oxide)50(ethylene oxide)132 (F108) and (ethylene oxide)76(propylene oxide)29(ethylene oxide)76 (F68) were chosen to investigate the role of the molecular weight keeping constant the hydrophilic/hydrophobic ratio. The selected surfactants are sodium decanoate (NaDec) and decyltrimethylammonium bromide (DeTAB) with comparable hydrophobicity and different charged heads. The alpha,omega-dichloroalkanes were chosen as contaminant prototypes. For the water + surfactant + copolymer mixtures, both the volume and the SANS results straightforwardly evidenced that (1) monomers of NaDec and copolymer unimers generate small mixed aggregates, (2) monomers of DeTAB combined with copolymer unimers do not form aggregates, and (3) unimeric copolymer is solubilized into NaDec and DeTAB micelles. The alpha,omeaga-dichloroalkanes presence induces the F108 aggregation even at very low copolymer composition. The addition of surfactant disintegrates the F108 aggregates and, consequently, the additive is expelled into the aqueous phase. Once F108 is in the unimeric state, it forms copolymer-micelle aggregates which incorporate the oil. In the case of F68 both the volumetric and the SANS data reveal that the additive does not alter the copolymer unimeric state. Moreover, they show that for the aqueous DeTAB-F68 system the additive trapping in both the copolymer-micelle aggregate and the pure micelles takes place being enhanced in the former aggregate in agreement with solubility experiments. For the NaDec-F68 mixtures, an additional solubilization process in the premicellar copolymer-surfactant microstructures occurs. SANS and conductivity data show that the additive incorporation into the mixed and the pure micelles does not essentially influence the structural properties of the aggregates.

Journal Article↗

PubMed2006

An off-axis magnetron-sputtering system for in situ studies of artificial superlattices growth by synchrotron radiation scattering.

A sputtering chamber for the growth of artificial superlattices of oxide-based materials is described. The chamber is designed to fit into a standard Huber eight-circle diffractometer. The chamber serves for investigation with synchrotron radiation of growth characteristics of oxide-based artificial superlattices in situ. Two Be windows of large area in the vacuum chamber enable measurement of reflections of X-rays at entrance and exit angles up to approximately 50 degrees . Large perpendicular momentum transfers are practical with this apparatus. The possibility of investigating X-ray scattering in situ is demonstrated by observation of the effects of the modulation length and the stacking period on the growth characteristics of BaTiO(3)/LaNiO(3) artificial superlattices.

Crystallization↗

PubMed2004

Structural and rheological properties of hydrophobically modified polysaccharide associative networks.

The phase behavior of hydrophobically modified chitosans (HMCs) in aqueous solution has been investigated using scattering and rheology experiments. We observed four regions on the phase diagram of the associative polymer: (i) a supernatant phase (unimers phase) at low polymer concentration; (ii) a dilute solution of intermolecularly bridged flowerlike micelles at intermediate concentration; (iii) an associative gel phase at high polymer content; and (iv) a phase separation. In the present paper, we discuss the structural and dynamical properties of the HMC associative networks (c > c*) at a fixed hydrophobic degree of substitution of 2% and fixed alkyl side chains (stickers) length C8 (domains iii and iv of the phase diagram). As the polymer concentration is increasing, a connecting network is formed from the percolation of bridges between micellar aggregates. In this regime, small-angle neutron scattering and light scattering measurements show that -50-nm flower aggregates are acting like junction points in the network. The effect of the concentration, the stress, and the shear on the structure of the network is discussed. In particular, we observe bridge-to-loop transitions and then the formation of microgels or a low-connected network under shear. Therefore, our results are compared to recent theoretical models and to the results reported for telechelic systems.

Hydrophobic and Hydrophilic Interactions↗

PubMed1998

Quantification of the collagen fibre architecture of human cranial dura mater.

The purpose of this study was to quantify and map the gross fibre architecture of the cranial dura mater (CDM) using small angle light scattering (SALS). In SALS, HeNe laser light is passed through the tissue, and the resultant scattering pattern is analysed to determine the preferred fibre direction and degree of orientation. The dura mater was found to be a complex structure with fibre orientations ranging from highly aligned to nearly random. In the temporal region, 80% of the samples (n = 20) were found to have regions composed of highly oriented fibres with a mean fibre direction of 6.3 degrees +/- 0.8 degree with respect to the sagittal plane (i.e. almost parallel to the superior sagittal sinus). These highly aligned regions were found in symmetric anatomical locations about the median sagittal sinus and had similar fibre orientations over both hemispheres. Although our sample size was small, we found that the size of the symmetric regions, which covered 14.4 +/- 1.6% of the total CDM area, was not influenced by subject's age or sex. The presence of these highly oriented fibre regions in CDM may be due to mechanical forces exerted on dura mater during its development. These forces may have induced realignment of the collagen fibres in the direction of tensile pull, although the exact basis for the unique gross fibre architecture of CDM remains unknown.

Brain↗

PubMed2006

Characterisation of bicontinuous cubic liquid crystalline systems of phytantriol and water using cryo field emission scanning electron microscopy (cryo FESEM).

Cubosomes are a novel lipid particulate delivery system currently being investigated for drug delivery purposes. The present study investigates bicontinuous cubic liquid crystalline systems (bulk phase and cubosomes) formed by phytantriol and water using cryo field emission scanning electron microscopy (cryo FESEM). Previously cubosomes have been characterized by cryo transmission electron microscopy (cryo TEM) with small angle X-ray diffraction (SAXS) confirming the bicontinuous liquid crystalline type. Bulk cubic phase and cubosomes were prepared from phytantriol and Pluronic F127 and analysed using cryo FESEM and SAXS. The micrographs showed the cubic phase had a tortuous, bicontinuous nature with a non-intersecting network of water channels. The cubosomes also show the same underlying tortuous structure entirely consistent with that of the bulk cubic phase and closely resemble the mathematical description of cubosomes described using nodal surface representation. The structure of both systems was confirmed using SAXS as a bicontinuous cubic liquid crystalline phase with Pn3m geometry. Cryo FESEM provides valuable insights into the morphological features of bicontinuous cubic liquid crystalline systems. The unique details shown provide strength to support the nodal surface representation of bicontinuous cubic liquid crystalline systems. Cryo FESEM provides a new technique to complement cryo TEM and SAXS for investigating their structure and function.

Cryoelectron Microscopy↗

PubMed2005

Effects of surfactant and temperature on rheological and structural properties of semidilute aqueous solutions of unmodified and hydrophobically modified alginate.

The dynamic and structural perturbations that result from the interactions between the anionic surfactant sodium dodecyl sulfate (SDS) and the hydrophobically modified biopolymer alginate (HM-alginate) have been studied with the aid of rheological methods, turbidimetry, and small-angle neutron scattering (SANS). The rheological results for a semidilute HM-alginate solution in the presence of SDS disclose strong interactions between HM-alginate and SDS at a low level of surfactant addition, and this feature is accompanied by enhanced turbidity. At higher surfactant concentrations the association complexes are disrupted. A strong temperature effect of the viscosity is observed in HM-alginate solutions at moderate SDS concentrations, where an elevated temperature leads to enhanced chain mobility, which promotes a breakup of the association complexes. The SANS results reveal a pronounced peak in the plot of scattered intensity versus wavevector q at intermediate q values for SDS concentrations above the critical micelle concentration (cmc). With contrast-matching conditions, using deuterated SDS instead of SDS, no interaction peak appears but an "upturn" in the scattered intensity is observed at small q value. The magnitude of this effect decreases with increasing surfactant concentration, showing clearly that SDS is capable of breaking up the large aggregates created.

Journal Article↗

PubMed2005

Micelle-to-vesicle transition of an iron-chelating microbial surfactant, marinobactin E.

Small-angle neutron scattering (SANS) and dynamic light scattering (DLS) techniques have been applied to study the self-assembly processes of a microbially produced siderophore, marinobactin E (ME). ME is one of a series of marinobactins A-E that facilitate Fe(III) acquisition by the source bacterium through coordination of Fe(III) by the marinobactin headgroup. ME is a six-amino-acid peptide amphiphile appended by palmitic acid (C16), and differs only in the nature of the fatty acid moiety from the other marinobactins. Apo-ME (uncoordinated ME) assembles to form micelles with an average diameter of 4.0 nm. Upon coordination of one equivalent of Fe(III), the mean micellar diameter of Fe(III)-ME shrinks to approximately 2.8 nm. However, in the presence of excess Fe(III), Fe(III)-ME undergoes a micelle-to-vesicle transition (MVT). At a small excess of Fe(III) over Fe(III)-ME (i.e., <1.2 Fe(III)/ME), a fraction of the Fe(III)-ME micelles rearrange into approximately 200 nm diameter unilamellar vesicles. At even greater Fe(III)/ME ratios (e.g., 2-3) multilamellar aggregates begin to emerge, consistent with either multilamellar vesicles or lamellar stacks. The MVT exhibited by ME may represent a unique mechanism by which marine bacteria may detect and sequester iron required for growth.

Iron Chelating Agents↗

PubMed1994

A quantitative model of the Escherichia coli 16 S RNA in the 30 S ribosomal subunit.

We use a computer-based protocol for automated structure refinement of large RNAs and ribonucleoproteins to propose a three-dimensional model for the Escherichia coli 16 S RNA in the 30 S ribosomal subunit along with the first quantitative estimates of the uncertainties in the model. Our models are based on the 16 S RNA secondary structure, the small angle neutron scatter map of 30 S proteins, tertiary RNA-RNA and RNA-protein contacts as suggested by cross-linking, chemical footprinting and other experimental studies, and electron microscopy data for the shape of the 30 S subunit and placement of 16 S RNA fragments, along with known motifs in RNA structure. In addition, some data on the interaction of the tRNAs/mRNA with the 16 S RNA were used to localize the active site. Since there are not enough structural data to derive a unique three-dimensional folding of the 16 S RNA, several different conformations can be generated to satisfy the experimental data. A set of seven models was refined to survey the range of acceptable conformations. These models were analyzed to deduce probable positions and orientations of the different helical segments that comprise the 16 S RNA in the Escherichia coli small subunit, and one consensus model from this set is presented here. An estimate of the reliability of our predicted structure is made using the variations between the models, and about 75% of 16 S RNA helical segments are localized to 15 A or less in their position in the small subunit. Our models show a distinct separation of the three major domains of the 16 S RNA. The 5' major domain and the central domain are clustered in the body of the 30 S subunit, whereas the 3' major domain is localized in the head of the subunit. Our modeling results are compared with models of the 16 S RNA proposed by other researchers, and are seen to be similar to the manually built models by Stern et al. and Brimacombe et al. with a few significant differences. The position of nucleotides implicated by footprinting and crosslinking data in tRNA and mRNA binding, and in subunit association are examined, and many of these sites are seen to lie along the 30 S subunit neck, cleft and the platform.

Base Sequence↗