Dispersion of Rod-like Particles of Nafion in Salt-Free Water/1-Propanol and Water/Ethanol Solutions.

PubMed

Yamaguchi, Makoto; Matsunaga, Takuro; Amemiya, Kazuki; Ohira, Akihiro; Hasegawa, Naoki; Shinohara, Kazuhiko; Ando, Masaki; Yoshida, Toshihiko

2014-12-26

The dispersion of perfluorinated sulfonic acid ionomers in catalyst inks is an important factor controlling the performance of catalyst layers in membrane electrode assemblies of proton exchange membrane fuel cells (PEMFCs). The effect of water/alcohol composition on the dispersion of H-Nafion in water/1-propanol and water/ethanol solutions was studied by dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), and (19)F nuclear magnetic resonance ((19)F NMR) spectroscopy. Hydrodynamic radii calculated from DLS decay profiles and the radii and interparticle distance of rod-like particles derived from SAXS profiles showed almost the same dependence on alcohol concentration. 1-Propanol was more effective than ethanol to induce changes in the characteristic lengths of the rod-like particles. The motional narrowing in the (19)F NMR spectra by addition of 1-propanol indicates selective solvation of the rod-like particles. We suppose this might have decreased their radii and induced their elongation, which eventually led to extension of the ordered regions as observed in the hydrodynamic radii. Our study helps to clarify the dispersion of Nafion in aqueous alcohol solutions, which has implications for the performance of PEMFCs.

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

NASA Astrophysics Data System (ADS)

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

2017-08-01

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

Colloidal properties of sodium caseinate-stabilized nanoemulsions prepared by a combination of a high-energy homogenization and evaporative ripening methods.

PubMed

Montes de Oca-Ávalos, J M; Candal, R J; Herrera, M L

2017-10-01

Nanoemulsions stabilized by sodium caseinate (NaCas) were prepared using a combination of a high-energy homogenization and evaporative ripening methods. The effects of protein concentration and sucrose addition on physical properties were analyzed by dynamic light scattering (DLS), Turbiscan analysis, confocal laser scanning microscopy (CLSM) and small angle X-ray scattering (SAXS). Droplets sizes were smaller (~100nm in diameter) than the ones obtained by other methods (200 to 2000nm in diameter). The stability behavior was also different. These emulsions were not destabilized by creaming. As droplets were so small, gravitational forces were negligible. On the contrary, when they showed destabilization the main mechanism was flocculation. Stability of nanoemulsions increased with increasing protein concentrations. Nanoemulsions with 3 or 4wt% NaCas were slightly turbid systems that remained stable for at least two months. According to SAXS and Turbiscan results, aggregates remained in the nano range showing small tendency to aggregation. In those systems, interactive forces were weak due to the small diameter of flocs. Copyright © 2017 Elsevier Ltd. All rights reserved.

A New Clinical Instrument for The Early Detection of Cataract Using Dynamic Light Scattering and Corneal Topography

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Datiles, Manuel B., III; King, James F.

2000-01-01

A growing cataract can be detected at the molecular level using the technique of dynamic light scattering (DLS). However, the success of this method in clinical use depends upon the precise control of the scattering volume inside a patient's eye and especially during patient's repeat visits. This is important because the scattering volume (cross-over region between the scattered fight and incident light) inside the eye in a high-quality DLS set-up is very small (few microns in dimension). This precise control holds the key for success in the longitudinal studies of cataract and during anti-cataract drug screening. We have circumvented these problems by fabricating a new DLS fiber optic probe with a working distance of 40 mm and by mounting it inside a cone of a corneal analyzer. This analyzer is frequently used in mapping the corneal topography during PRK (photorefractive keratectomy) and LASIK (laser in situ keratomileusis) procedures in shaping of the cornea to correct myopia. This new instrument and some preliminary clinical tests on one of us (RRA) showing the data reproducibility are described.

New clinical instrument for the early detection of cataract using dynamic light scattering and corneal topography

NASA Astrophysics Data System (ADS)

Ansari, Rafat R.; Datiles, Manuel B., III; King, James F.

2000-06-01

A growing cataract can be detected at the molecular level using the technique of dynamic light scattering (DLS). However, the success of this method in clinical use depends upon the precise control of the scattering volume inside a patient's eye and especially during patient's repeat visits. This is important because the scattering volume (cross-over region between the scattered light and incident light) inside the eye in a high-quality DLS set-up is very small (few microns in dimension). This precise control holds the key for success in the longitudinal studies of cataract and during anti-cataract drug screening. We have circumvented these problems by fabricating a new DLS fiber optic probe with a working distance of 40 mm and by mounting it inside a cone of a corneal analyzer. This analyzer is frequently used in mapping the corneal topography during PRK (photorefractive keratectomy) and LASIK (laser in situ keratomileusis) procedures in shaping of the cornea to correct myopia. This new instrument and some preliminary clinical tests on one of us (RRA) showing the data reproducibility are described.

Thermoreversible gelation of poly(vinylidene fluoride) in phthalates: the influence of aliphatic chain length of solvents.

PubMed

Yadav, P Jaya Prakash; Ghosh, Goutam; Maiti, Biswajit; Aswal, Vinod K; Goyal, P S; Maiti, Pralay

2008-04-17

Thermoreversible gelation of poly(vinylidene fluoride) (PVDF) has been studied in a new series of solvents (phthalates), for example, dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), and dihexyl phthalate (DHP) as a function of temperature and polymer concentration, both by test tube tilting and dynamic light scattering (DLS) method. The effect of aliphatic chain length (n) of diesters on the gelation kinetics, structure/microstructure and morphology of PVDF gels has been examined. Gelation rate was found to increase with increasing aliphatic chain length of diester. DLS results indicate that the sol-gel transformation proceeds via two-steps: first, microgel domains were formed, and then the infinite three-dimensional (3D) network is established by connecting microgels through polymer chains. The crystallites are responsible for 3D network for gelation in phthalates, and alpha-polymorph is formed during gelation producing higher amount of crystallinity with increasing aliphatic chain length of diester. Morphology of the networks of dried gels in different phthalates showed that fibril thickness and lateral dimensions decrease with higher homologues of phthalates. The scattering intensity is fitted with Debye-Bueche model in small-angle neutron scattering and suggested that both the correlation length and interlamellar spacing increases with n. A model has been proposed, based on electronic structure calculations, to explain the conformation of PVDF chain in presence of various phthalates and their complexes, which offer the cause of higher gelation rate for longer aliphatic chain length.

Surfactant induced stabilization of nano liquid crystalline (dodecane-phytantriol) droplet

NASA Astrophysics Data System (ADS)

Abbas, S.; Saha, Debasish; Kumar, Sugam; Aswal, V. K.; Kohlbrecher, J.

2018-04-01

The study of formation and stabilization of dodecane-phytantriol (DPT) microemulsions using ionic and nonionic surfactants are investigated. Small Angle Neutron Scattering (SANS) and Dynamic Light Scattering (DLS) techniques have been employed to study the resulting structures of the micro emulsion droplets. We show the formation of stable microemulsion droplets with absence of lyotropic liquid crystalline phase on addition of nonionic surfactant C12E10. The oil to surfactant ratio plays the crucial role in formation of stable droplet and its size. The dense presence of C12E10 molecules between microemulsion droplets protect them from coalescence while less number of C12E10 between the surface of droplets easily triggers the coalescence process. The interaction with both anionic (SDS) as well as cationic (DTAB) surfactants with DPT phase leads to formation of microemulsion droplets with lyotropic liquid crystalline phase.

Interaction of celecoxib with membranes: the role of membrane biophysics on its therapeutic and toxic effects.

PubMed

Pereira-Leite, Catarina; Nunes, Cláudia; Lima, José L F C; Reis, Salette; Lúcio, Marlene

2012-11-26

The present work provides a biophysical characterization of the interaction of celecoxib, a cyclo-oxigenase-2 selective nonsteroidal anti-inflammatory drug, with membranes using liposomes, constituted by phosphatidylcholines, as membrane model systems. In order to mimic biological conditions, the experiments were performed at physiological pH (7.4); at an acidic pH to mimic the conditions of the inflamed cells (5.0); and at different membrane physical states (gel, ripple, and fluid phase). Important information regarding the celecoxib-membrane interactions was gathered by the complementary biophysical techniques: derivative spectrophotometry was used to determine liposome/water partition coefficient of celecoxib; dynamic light scattering (DLS) measurements were performed to study the influence of celecoxib on lipid main phase transition temperature; fluorescence binding measurements were made to assess the location of celecoxib within the membrane; and small-angle and wide-angle X-ray scattering (SAXS and WAXS) were used to assess the changes in the structure and order of phosphatidylcholine bilayers caused by the presence of celecoxib. The overall results obtained indicate that celecoxib greatly interacts with membranes. Briefly, celecoxib exhibits a high liposome/water partition coefficient that is non-pH-dependent, but the location of celecoxib within the membrane is pH-dependent. In fact, celecoxib is more deeply located inside the membrane at pH 5.0, while it locates closer to the surface at pH 7.4. DLS, SAXS, and WAXS results have shown a high membrane fluidization in the presence of celecoxib, especially at pH 7.4. Overall, the current study can contribute to a biophysical characterization of the celecoxib-membrane interaction. The relevance of the gathered results will be discussed in terms of the reported celecoxib therapeutic and toxic effects.

Synthesis of Thermoresponsive Amphiphilic Polyurethane Gel as a New Cell Printing Material near Body Temperature.

PubMed

Tsai, Yi-Chun; Li, Suming; Hu, Shiaw-Guang; Chang, Wen-Chi; Jeng, U-Ser; Hsu, Shan-hui

2015-12-23

Waterborne polyurethane (PU) based on poly(ε-caprolactone) (PCL) diol and a second oligodiol containing amphiphilic blocks was synthesized in this study. The microstructure was characterized by dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), and rheological measurement of the PU dispersion. The surface hydrophilicity measurement, infrared spectroscopy, wide-angle X-ray diffraction, mechanical and thermal analyses were conducted in solid state. It was observed that the presence of a small amount of amphiphilic blocks in the soft segment resulted in significant changes in microstructure. When 90 mol % PCL diol and 10 mol % amphiphilic blocks of poly(l-lactide)-poly(ethylene oxide) (PLLA-PEO) diol were used as the soft segment, the synthesized PU had a water contact angle of ∼24° and degree of crystallinity of ∼14%. The dispersion had a low viscosity below room temperature. As the temperature was raised to body temperature (37 °C), the dispersion rapidly (∼170 s) underwent sol-gel transition with excellent gel modulus (G' ≈ 6.5 kPa) in 20 min. PU dispersions with a solid content of 25-30% could be easily mixed with cells in sol state, extruded by a 3D printer, and deposited layer by layer as a gel. Cells remained alive and proliferating in the printed hydrogel scaffold. We expect that the development of novel thermoresponsive PU system can be used as smart injectable hydrogel and applied as a new type of bio-3D printing ink.

Variability of single-leg versus double-leg stance radiographs in the varus knee.

PubMed

Chen, Andrew; Rich, Valerie; Bain, Elizabeth; Sterett, William I

2009-07-01

We evaluated measured radiographic parameter variability between single-leg stance (SLS) and double-leg stance (DLS) radiographs in patients with varus knee malalignment, indicated for high tibial osteotomy. Fifty-three consecutive knees (mean, 49 years; range, 18-79 years) were evaluated for varus thrust. SLS and DLS radiographs were obtained. A single blinded observer measured mechanical axis angles and weight-bearing line (WBL) deviation using a goniometer. Mechanical axis angles averaged 9.1 degrees (DLS) and 11.3 degrees (SLS). SLS radiographs averaged 9% greater WBL medialization than did DLS. Medial opening averaged 16.4 mm (DLS) and 18.8 mm (SLS). DLS and SLS radiographs showed no significant differences in patients without varus thrust. Patients with varus thrust demonstrated differences in mechanical axis angles (DLS, 9.4 degrees; SLS, 12.2 degrees), WBL deviation (12.1% less), medialization (DLS), and medial opening necessary for correction (DLS, 16.6 mm; SLS, 20.3 mm). In varus thrust, SLS radiographs more closely replicate dynamic knee malalignment, possibly providing more accurate measurements of angular deformity.

One-step analysis of DNA/chitosan complexes by field-flow fractionation reveals particle size and free chitosan content.

PubMed

Ma, Pei Lian; Buschmann, Michael D; Winnik, Françoise M

2010-03-08

The composition of samples obtained upon complexation of DNA with chitosan was analyzed by asymmetrical flow field flow fractionation (AF4) with online UV-visible, multiangle light scattering (MALS), and dynamic light scattering (DLS) detectors. A chitosan labeled with rhodamine B to facilitate UV-vis detection of the polycation was complexed with DNA under conditions commonly used for transfection (chitosan glucosamine to DNA phosphate molar ratio of 5). AF4 analysis revealed that 73% of the chitosan-rhodamine remained free in the dispersion and that the DNA/chitosan complexes had a broad size distribution ranging from 20 to 160 nm in hydrodynamic radius. The accuracy of the data was assessed by comparison with data from batch-mode DLS and scanning electron microscopy. The AF4 combined with DLS allowed the characterization of small particles that were not detected by conventional batch-mode DLS. The AF4 analysis will prove to be an important tool in the field of gene therapy because it readily provides, in a single measurement, three important physicochemical parameters of the complexes: the amount of unbound polycation, the hydrodynamic size of the complexes, and their size distribution.

Kinetics of aggregation in charged nanoparticle solutions driven by different mechanisms

NASA Astrophysics Data System (ADS)

Abbas, S.; Yadav, I.; Kumar, Sugam; Aswal, V. K.; Kohlbrecher, J.

2017-05-01

The structure and kinetics during aggregation of anionic silica nanoparticles as induced through different mechanisms have been studied by dynamic light scattering (DLS) and small-angle neutron scattering (SANS). Three different additives, namely an electrolyte (NaCl), cationic protein (lysozyme) and non-ionic surfactant (C12E10) were used to initiate nanoparticle aggregation. Electrolyte induced aggregation can be explained by DLVO interaction, whereas depletion interaction (non-DLVO interaction) is found responsible for nanoparticle aggregation in case of non-ionic surfactant. Unlike these two cases, strong electrostatic attraction between nanoparticle and oppositely charged protein results into protein-mediated nanoparticle aggregation. The electrolyte induced aggregation show quite slow aggregation rate whereas protein mediated as well as surfactant induced aggregation takes place almost instantaneously. The significant differences observed in the kinetics are explained based on range of interactions responsible for the aggregation. In spite of differences in mechanism and kinetics, the nanoparticle clusters are found to have similar fractal morphology (fractal dimension ˜ 2.5) in all the three cases.

Interaction of lysozyme protein with different sized silica nanoparticles and their resultant structures

NASA Astrophysics Data System (ADS)

Yadav, Indresh; Aswal, V. K.; Kohlbrecher, J.

2016-05-01

The interaction of model protein-lysozyme with three different sized anionic silica nanoparticles has been studied by UV-vis spectroscopy, dynamic light scattering (DLS) and small-angle neutron scattering (SANS). The surface area and curvature of the nanoparticles change with size, which significantly influence their interaction with protein. The lysozyme adsorbs on the surface of the nanoparticles due to electrostatic attraction and leads to the phase transformation from one phase (clear) to two-phase (turbid) of the nanoparticle-protein system. The dominance of lysozyme induced short-range attraction over long-range electrostatic repulsion between nanoparticles is responsible for phase transformation and modeled by the two-Yukawa potential. The magnitude of the attractive interaction increases with the size of the nanoparticles as a result the phase transformation commences relatively at lower concentration of lysozyme. The structure of the nanoparticle-protein system in two-phase is characterized by the diffusion limited aggregate type of mass fractal morphology.

Interaction of lysozyme protein with different sized silica nanoparticles and their resultant structures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yadav, Indresh, E-mail: iykumarindresh288@gmail.com; Aswal, V. K.; Kohlbrecher, J.

The interaction of model protein-lysozyme with three different sized anionic silica nanoparticles has been studied by UV-vis spectroscopy, dynamic light scattering (DLS) and small-angle neutron scattering (SANS). The surface area and curvature of the nanoparticles change with size, which significantly influence their interaction with protein. The lysozyme adsorbs on the surface of the nanoparticles due to electrostatic attraction and leads to the phase transformation from one phase (clear) to two-phase (turbid) of the nanoparticle-protein system. The dominance of lysozyme induced short-range attraction over long-range electrostatic repulsion between nanoparticles is responsible for phase transformation and modeled by the two-Yukawa potential. Themore » magnitude of the attractive interaction increases with the size of the nanoparticles as a result the phase transformation commences relatively at lower concentration of lysozyme. The structure of the nanoparticle-protein system in two-phase is characterized by the diffusion limited aggregate type of mass fractal morphology.« less

Techniques for Accurate Sizing of Gold Nanoparticles Using Dynamic Light Scattering with Particular Application to Chemical and Biological Sensing Based on Aggregate Formation.

PubMed

Zheng, Tianyu; Bott, Steven; Huo, Qun

2016-08-24

Gold nanoparticles (AuNPs) have found broad applications in chemical and biological sensing, catalysis, biomolecular imaging, in vitro diagnostics, cancer therapy, and many other areas. Dynamic light scattering (DLS) is an analytical tool used routinely for nanoparticle size measurement and analysis. Due to its relatively low cost and ease of operation in comparison to other more sophisticated techniques, DLS is the primary choice of instrumentation for analyzing the size and size distribution of nanoparticle suspensions. However, many DLS users are unfamiliar with the principles behind the DLS measurement and are unware of some of the intrinsic limitations as well as the unique capabilities of this technique. The lack of sufficient understanding of DLS often leads to inappropriate experimental design and misinterpretation of the data. In this study, we performed DLS analyses on a series of citrate-stabilized AuNPs with diameters ranging from 10 to 100 nm. Our study shows that the measured hydrodynamic diameters of the AuNPs can vary significantly with concentration and incident laser power. The scattered light intensity of the AuNPs has a nearly sixth order power law increase with diameter, and the enormous scattered light intensity of AuNPs with diameters around or exceeding 80 nm causes a substantial multiple scattering effect in conventional DLS instruments. The effect leads to significant errors in the reported average hydrodynamic diameter of the AuNPs when the measurements are analyzed in the conventional way, without accounting for the multiple scattering. We present here some useful methods to obtain the accurate hydrodynamic size of the AuNPs using DLS. We also demonstrate and explain an extremely powerful aspect of DLS-its exceptional sensitivity in detecting gold nanoparticle aggregate formation, and the use of this unique capability for chemical and biological sensing applications.

Reference materials and representative test materials to develop nanoparticle characterization methods: the NanoChOp project case

NASA Astrophysics Data System (ADS)

Roebben, Gert; Kestens, Vikram; Varga, Zoltan; Charoud-Got, Jean; Ramaye, Yannic; Gollwitzer, Christian; Bartczak, Dorota; Geißler, Daniel; Noble, James; Mazoua, Stéphane; Meeus, Nele; Corbisier, Philippe; Palmai, Marcell; Mihály, Judith; Krumrey, Michael; Davies, Julie; Resch-Genger, Ute; Kumarswami, Neelam; Minelli, Caterina; Sikora, Aneta; Goenaga-Infante, Heidi

2015-10-01

This paper describes the production and characteristics of the nanoparticle test materials prepared for common use in the collaborative research project NanoChOp (Chemical and optical characterisation of nanomaterials in biological systems), in casu suspensions of silica nanoparticles and CdSe/CdS/ZnS quantum dots. This paper is the first to illustrate how to assess whether nanoparticle test materials meet the requirements of a 'reference material' (ISO Guide 30:2015) or rather those of the recently defined category of 'representative test material' (ISO TS 16195:2013). The NanoChOp test materials were investigated with small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and centrifugal liquid sedimentation (CLS) to establish whether they complied with the required monomodal particle size distribution. The presence of impurities, aggregates, agglomerates and viable microorganisms in the suspensions was investigated with DLS, CLS, optical and electron microscopy and via plating on nutrient agar. Suitability of surface functionalization was investigated with attenuated total reflection Fourier transform infrared spectrometry (ATR-FTIR) and via the capacity of the nanoparticles to be fluorescently labeled or to bind antibodies. Between-unit homogeneity and stability were investigated in terms of particle size and zeta potential. This paper shows that only based on the outcome of a detailed characterization process one can raise the status of a test material to representative test material or reference material, and how this status depends on its intended use.

Small angle neutron scattering study of nano sized microstructure in Fe-Cr ODS steels for gen IV in-core applications.

PubMed

Han, Young-Soo; Mao, Xiadong; Jang, Jinsung

2013-11-01

The nano-sized microstructures in Fe-Cr oxide dispersion strengthened steel for Gen IV in-core applications were studied using small angle neutron scattering. The oxide dispersion strengthened steel was manufactured through hot isostatic pressing with various chemical compositions and fabrication conditions. Small angle neutron scattering experiments were performed using a 40 m small angle neutron scattering instrument at HANARO. Nano sized microstructures, namely, yttrium oxides and Cr-oxides were quantitatively analyzed by small angle neutron scattering. The yttrium oxides and Cr-oxides were also observed by transmission electron microscopy. The microstructural analysis results from small angle neutron scattering were compared with those obtained by transmission electron microscopy. The effects of the chemical compositions and fabrication conditions on the microstructure were investigated in relation to the quantitative microstructural analysis results obtained by small angle neutron scattering. The volume fraction of Y-oxide increases after fabrication, and this result is considered to be due to the formation of non-stochiometric Y-Ti-oxides.

Preparation, purification, and characterization of aminopropyl-functionalized silica sol.

PubMed

Pálmai, Marcell; Nagy, Lívia Naszályi; Mihály, Judith; Varga, Zoltán; Tárkányi, Gábor; Mizsei, Réka; Szigyártó, Imola Csilla; Kiss, Teréz; Kremmer, Tibor; Bóta, Attila

2013-01-15

A new, simple, and "green" method was developed for the surface modification of 20 nm diameter Stöber silica particles with 3-aminopropyl(diethoxy)methylsilane in ethanol. The bulk polycondensation of the reagent was inhibited and the stability of the sol preserved by adding a small amount of glacial acetic acid after appropriate reaction time. Centrifugation, ultrafiltration, and dialysis were compared in order to choose a convenient purification technique that allows the separation of unreacted silylating agent from the nanoparticles without destabilizing the sol. The exchange of the solvent to acidic water during the purification yielded a stable colloid, as well. Structural and morphological analysis of the obtained aminopropyl silica was performed using transmission electron microscopy (TEM), dynamic light scattering (DLS) and zeta potential measurements, Fourier-transform infrared (FTIR), (13)C and (29)Si MAS nuclear magnetic resonance (NMR) spectroscopies, as well as small angle X-ray scattering (SAXS). Our investigations revealed that the silica nanoparticle surfaces were partially covered with aminopropyl groups, and multilayer adsorption followed by polycondensation of the silylating reagent was successfully avoided. The resulting stable aminopropyl silica sol (ethanolic or aqueous) is suitable for biomedical uses due to its purity. Copyright © 2012 Elsevier Inc. All rights reserved.

Protein–Protein Interactions in Dilute to Concentrated Solutions: α-Chymotrypsinogen in Acidic Conditions

PubMed Central

2015-01-01

Protein–protein interactions were investigated for α-chymotrypsinogen by static and dynamic light scattering (SLS and DLS, respectively), as well as small-angle neutron scattering (SANS), as a function of protein and salt concentration at acidic conditions. Net protein–protein interactions were probed via the Kirkwood–Buff integral G22 and the static structure factor S(q) from SLS and SANS data. G22 was obtained by regressing the Rayleigh ratio versus protein concentration with a local Taylor series approach, which does not require one to assume the underlying form or nature of intermolecular interactions. In addition, G22 and S(q) were further analyzed by traditional methods involving fits to effective interaction potentials. Although the fitted model parameters were not always physically realistic, the numerical values for G22 and S(q → 0) were in good agreement from SLS and SANS as a function of protein concentration. In the dilute regime, fitted G22 values agreed with those obtained via the osmotic second virial coefficient B22 and showed that electrostatic interactions are the dominant contribution for colloidal interactions in α-chymotrypsinogen solutions. However, as protein concentration increases, the strength of protein–protein interactions decreases, with a more pronounced decrease at low salt concentrations. The results are consistent with an effective “crowding” or excluded volume contribution to G22 due to the long-ranged electrostatic repulsions that are prominent even at the moderate range of protein concentrations used here (<40 g/L). These apparent crowding effects were confirmed and quantified by assessing the hydrodynamic factor H(q → 0), which is obtained by combining measurements of the collective diffusion coefficient from DLS data with measurements of S(q → 0). H(q → 0) was significantly less than that for a corresponding hard-sphere system and showed that hydrodynamic nonidealities can lead to qualitatively incorrect conclusions regarding B22, G22, and static protein–protein interactions if one uses only DLS to assess protein interactions. PMID:24810917

Solution Behavior and Activity of a Halophilic Esterase under High Salt Concentration

PubMed Central

Rao, Lang; Zhao, Xiubo; Pan, Fang; Li, Yin; Xue, Yanfen; Ma, Yanhe; Lu, Jian R.

2009-01-01

Background Halophiles are extremophiles that thrive in environments with very high concentrations of salt. Although the salt reliance and physiology of these extremophiles have been widely investigated, the molecular working mechanisms of their enzymes under salty conditions have been little explored. Methodology/Principal Findings A halophilic esterolytic enzyme LipC derived from archeaon Haloarcula marismortui was overexpressed from Escherichia coli BL21. The purified enzyme showed a range of hydrolytic activity towards the substrates of p-nitrophenyl esters with different alkyl chains (n = 2−16), with the highest activity being observed for p-nitrophenyl acetate, consistent with the basic character of an esterase. The optimal esterase activities were found to be at pH 9.5 and [NaCl] = 3.4 M or [KCl] = 3.0 M and at around 45°C. Interestingly, the hydrolysis activity showed a clear reversibility against changes in salt concentration. At the ambient temperature of 22°C, enzyme systems working under the optimal salt concentrations were very stable against time. Increase in temperature increased the activity but reduced its stability. Circular dichroism (CD), dynamic light scattering (DLS) and small angle neutron scattering (SANS) were deployed to determine the physical states of LipC in solution. As the salt concentration increased, DLS revealed substantial increase in aggregate sizes, but CD measurements revealed the maximal retention of the α-helical structure at the salt concentration matching the optimal activity. These observations were supported by SANS analysis that revealed the highest proportion of unimers and dimers around the optimal salt concentration, although the coexistent larger aggregates showed a trend of increasing size with salt concentration, consistent with the DLS data. Conclusions/Significance The solution α-helical structure and activity relation also matched the highest proportion of enzyme unimers and dimers. Given that all the solutions studied were structurally inhomogeneous, it is important for future work to understand how the LipC's solution aggregation affected its activity. PMID:19759821

Static structures and dynamics of hemoglobin vesicle (HBV) developed as a transfusion alternative.

PubMed

Sato, Takaaki; Sakai, Hiromi; Sou, Keitaro; Medebach, Martin; Glatter, Otto; Tsuchida, Eishun

2009-06-18

Hemoglobin vesicle (HbV) is an artificial oxygen carrier that encapsulates solution of purified and highly concentrated (ca. 38 g dL(-1)) human hemoglobin. Its exceptionally high concentration as a liposomal product (ca. 40% volume fraction) achieves an oxygen-carrying capacity comparable to that of blood. We use small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS) to investigate the hierarchical structures and dynamics of HbVs in concentrated suspensions. SAXS data revealed unilamellar shell structure and internal density profile of the artificial cell membrane for Hb encapsulation. The SAXS intensity of HbV at scattering vector q > 0.5 nm(-1) manifests dissolution states of the encapsulated Hbs in the inner aqueous phase of the vesicle having ca. 240 nm diameter. The peak position as well as the height and width of static structure factor of Hb before and after encapsulation are almost identical, demonstrating the preserved protein-protein interactions in the confined space. To overcome multiple scattering from turbid samples, we employed thin layer-cell DLS combined with the so-called bruteforce and echo techniques, which allows us to observe collective diffusion dynamics of HbVs without dilution. A pronounced slowdown of the HbV diffusion and eventual emergence of dynamically arrested state in the presence of high-concentration plasma substitutes (water-soluble polymers), such as dextran, modified fluid gelatin, and hydroxylethyl starch, can be explained by depletion interaction. A significantly weaker effect of recombinant human serum albumin on HbV flocculation and viscosity enhancement than those induced by other polymers is clearly attributed to the specificity as a protein; its compact structure efficiently reduces the reservoir polymer volume fraction that determines the depth of the attractive potential between HbVs. These phenomena are technically essential for controlling the suspension rheology, which is advantageous for versatile clinical applications.

Note: Evaluation of slurry particle size analyzers for chemical mechanical planarization process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jang, Sunjae; Kulkarni, Atul; Qin, Hongyi

In the chemical mechanical planarization (CMP) process, slurry particle size is important because large particles can cause defects. Hence, selection of an appropriate particle measuring system is necessary in the CMP process. In this study, a scanning mobility particle sizer (SMPS) and dynamic light scattering (DLS) were compared for particle size distribution (PSD) measurements. In addition, the actual particle size and shape were confirmed by transmission electron microscope (TEM) results. SMPS classifies the particle size according to the electrical mobility, and measures the particle concentration (single particle measurement). On the other hand, the DLS measures the particle size distribution bymore » analyzing scattered light from multiple particles (multiple particle measurement). For the slurry particles selected for evaluation, it is observed that SMPS shows bi-modal particle sizes 30 nm and 80 nm, which closely matches with the TEM measurements, whereas DLS shows only single mode distribution in the range of 90 nm to 100 nm and showing incapability of measuring small particles. Hence, SMPS can be a better choice for the evaluation of CMP slurry particle size and concentration measurements.« less

Total synthesis of isotopically enriched Si-29 silica NPs as potential spikes for isotope dilution quantification of natural silica NPs.

PubMed

Pálmai, Marcell; Szalay, Roland; Bartczak, Dorota; Varga, Zoltán; Nagy, Lívia Naszályi; Gollwitzer, Christian; Krumrey, Michael; Goenaga-Infante, Heidi

2015-05-01

A new method was developed for the preparation of highly monodisperse isotopically enriched Si-29 silica nanoparticles ((29)Si-silica NPs) with the purpose of using them as spikes for isotope dilution mass spectrometry (IDMS) quantification of silica NPs with natural isotopic distribution. Si-29 tetraethyl orthosilicate ((29)Si-TEOS), the silica precursor was prepared in two steps starting from elementary silicon-29 pellets. In the first step Si-29 silicon tetrachloride ((29)SiCl4) was prepared by heating elementary silicon-29 in chlorine gas stream. By using a multistep cooling system and the dilution of the volatile and moisture-sensitive (29)SiCl4 in carbon tetrachloride as inert medium we managed to reduce product loss caused by evaporation. (29)Si-TEOS was obtained by treating (29)SiCl4 with absolute ethanol. Structural characterisation of (29)Si-TEOS was performed by using (1)H and (13)C nuclear magnetic resonance (NMR) spectroscopy and Fourier-transform infrared (FTIR) spectroscopy. For the NP preparation, a basic amino acid catalysis route was used and the resulting NPs were analysed using transmission electron microscopy (TEM), small angle X-ray scattering (SAXS), dynamic light scattering (DLS) and zeta potential measurements. Finally, the feasibility of using enriched NPs for on-line field-flow fractionation coupled with multi-angle light scattering and inductively coupled plasma mass spectrometry (FFF/MALS/ICP-MS) has been demonstrated. Copyright © 2015 Elsevier Inc. All rights reserved.

Dynamic light scattering in ophthalmology: results of in vitro and in vivo experiments.

PubMed

Fankhauser, Franz

2006-01-01

To calibrate new dynamic light scattering (DLS) devices in defined solutions and post mortem porcine and human eyes. To examine all segments of the eye and to become familiar with the usage of the technique in living subjects. METHODS, DESIGN: Three new DLS devices for the usage in patients were developed. Mono-disperse solutions, poly-disperse solutions, gels, post mortem porcine and human eyes as well as healthy volunteers were studied. The detected signals were inverted into autocorrelation functions. We constructed three DLS devices appropriate for in vitro as well as in vivo examinations. In mono disperse solution precise disintegration rates could be calculated. In poly-disperse solutions, in gel and in the vitreous the results did not correlate with movements of individual particles but we could calculate characteristics of the complete scattering system. In vivo measurements demonstrated that DLS can be used in all human eye segments. DLS is a unique technique. With DLS the molecular composition of eye segments can be studied in living subjects. This can be used to understand the molecular basis of severe eye diseases. The presented data demonstrate that DLS delivers reproducible data from all eye segments. It is possible to study the molecular structures of eye segments in living subjects. The developed devices were proved successfully in vitro as well as in vivo. Limitations are the low specificity of DLS and its sensitivity to background noise. Now clinical studies are necessary to demonstrate potential diagnostic benefits of DLS in specific eye diseases.

Interactions and release of two palmitoyl peptides from phytantriol cubosomes.

PubMed

Akhlaghi, Seyedeh Parinaz; Loh, Watson

2017-08-01

Phytantriol cubosomes loaded with two palmitoyl peptides (Palpepcubes), namely GHKcube and GQPRcube, were prepared using an ultrasonication protocol. The Palpepcubes dimensions were characterized by dynamic light scattering (DLS) and cryo-transmission electron microscopy (cryo-TEM). Small-angle X-ray scattering (SAXS) analyses revealed that the bicontinuous cubic structure remained even at palmitoyl peptide contents as high as 5wt.%, with an increase in the cell parameter from approximately 6.5 to 7.2nm. Isothermal titration calorimetry (ITC) was used to elucidate the interactions between the blank cubosomes and the palmitoyl peptides, revealing an exothermic process of interaction. Moreover, the in vitro release of the palmitoyl peptides from the Palpepcubes was studied using a dialysis method coupled with liquid chromatography-mass spectrometry (LC/MS) technique, in which a sustained release of up to a few days was observed. Finally, the stability of the aqueous solutions of the palmitoyl peptides and the Palpepcubes kept at room temperature and at low temperature (4°C) was studied by LC/MS method, indicating that incorporation into cubosomes increases the peptide stability significantly. Copyright © 2017 Elsevier B.V. All rights reserved.

pH-sensitive niosomes: Effects on cytotoxicity and on inflammation and pain in murine models.

PubMed

Rinaldi, Federica; Del Favero, Elena; Rondelli, Valeria; Pieretti, Stefano; Bogni, Alessia; Ponti, Jessica; Rossi, François; Di Marzio, Luisa; Paolino, Donatella; Marianecci, Carlotta; Carafa, Maria

2017-12-01

pH-sensitive nonionic surfactant vesicles (niosomes) by polysorbate-20 (Tween-20) or polysorbate-20 derivatized by glycine (added as pH sensitive agent), were developed to deliver Ibuprofen (IBU) and Lidocaine (LID). For the physical-chemical characterization of vesicles (mean size, size distribution, zeta potential, vesicle morphology, bilayer properties and stability) dynamic light scattering (DLS), small angle X-ray scattering and fluorescence studies were performed. Potential cytotoxicity was evaluated on immortalized human keratinocyte cells (HaCaT) and on immortalized mouse fibroblasts Balb/3T3. In vivo antinociceptive activity (formalin test) and anti-inflammatory activity tests (paw edema induced by zymosan) in murine models were performed on drug-loaded niosomes. pH-sensitive niosomes were stable in the presence of 0 and 10% fetal bovine serum, non-cytotoxic and able to modify IBU or LID pharmacological activity in vivo. The synthesis of stimuli responsive surfactant, as an alternative to add pH-sensitive molecules to niosomes, could represent a promising delivery strategy for anesthetic and anti-inflammatory drugs.

Controlling block copolymer phase behavior using ionic surfactant

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ray, D.; Aswal, V. K.

2016-05-23

The phase behavior of poly(ethylene oxide)-poly(propylene oxide-poly(ethylene oxide) PEO-PPO-PEO triblock copolymer [P85 (EO{sub 26}PO{sub 39}EO{sub 26})] in presence of anionic surfactant sodium dodecyl sulfate (SDS) in aqueous solution as a function of temperature has been studied using dynamic light scattering (DLS) and small-angle neutron scattering (SANS). The measurements have been carried out for fixed concentrations (1 wt%) of block copolymer and surfactants. Each of the individual components (block copolymer and surfactant) and the nanoparticle–surfactant mixed system have been examined at varying temperature. The block copolymer P85 forms spherical micelles at room temperature whereas shows sphere-to-rod like micelle transition at highermore » temperatures. On the other hand, SDS surfactant forms ellipsoidal micelles over a wide temperature range. Interestingly, it is found that phase behavior of mixed micellar system (P85 + SDS) as a function of temperature is drastically different from that of P85, giving the control over the temperature-dependent phase behavior of block copolymers.« less

Microstructure of Amorphous and Semi-Crystalline Polymers.

DTIC Science & Technology

1981-06-07

of these materials. Further, the occurrence of nodular structures is difficult to reconcile with the results of studies of small angle neutron ...scattering and small angle neutron scattering studies of the same materials. Based on the combined results of these studies , it is suggested that the nodular...relevance here were reviewed by Flory.’ In addition to these, the results of studies using small angle neutron scattering’ and wide angle X-ray scattering

Monte Carlo calculation of large and small-angle electron scattering in air

NASA Astrophysics Data System (ADS)

Cohen, B. I.; Higginson, D. P.; Eng, C. D.; Farmer, W. A.; Friedman, A.; Grote, D. P.; Larson, D. J.

2017-11-01

A Monte Carlo method for angle scattering of electrons in air that accommodates the small-angle multiple scattering and larger-angle single scattering limits is introduced. The algorithm is designed for use in a particle-in-cell simulation of electron transport and electromagnetic wave effects in air. The method is illustrated in example calculations.

Systematic analysis of protein–detergent complexes applying dynamic light scattering to optimize solutions for crystallization trials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meyer, Arne; Dierks, Karsten; XtalConcepts, Marlowring 19, 22525 Hamburg

Application of in situ dynamic light scattering to solutions of protein–detergent complexes permits characterization of these complexes in samples as small as 2 µl in volume. Detergents are widely used for the isolation and solubilization of membrane proteins to support crystallization and structure determination. Detergents are amphiphilic molecules that form micelles once the characteristic critical micelle concentration (CMC) is achieved and can solubilize membrane proteins by the formation of micelles around them. The results are presented of a study of micelle formation observed by in situ dynamic light-scattering (DLS) analyses performed on selected detergent solutions using a newly designed advancedmore » hardware device. DLS was initially applied in situ to detergent samples with a total volume of approximately 2 µl. When measured with DLS, pure detergents show a monodisperse radial distribution in water at concentrations exceeding the CMC. A series of all-transn-alkyl-β-d-maltopyranosides, from n-hexyl to n-tetradecyl, were used in the investigations. The results obtained verify that the application of DLS in situ is capable of distinguishing differences in the hydrodynamic radii of micelles formed by detergents differing in length by only a single CH{sub 2} group in their aliphatic tails. Subsequently, DLS was applied to investigate the distribution of hydrodynamic radii of membrane proteins and selected water-insoluble proteins in presence of detergent micelles. The results confirm that stable protein–detergent complexes were prepared for (i) bacteriorhodopsin and (ii) FetA in complex with a ligand as examples of transmembrane proteins. A fusion of maltose-binding protein and the Duck hepatitis B virus X protein was added to this investigation as an example of a non-membrane-associated protein with low water solubility. The increased solubility of this protein in the presence of detergent could be monitored, as well as the progress of proteolytic cleavage to separate the fusion partners. This study demonstrates the potential of in situ DLS to optimize solutions of protein–detergent complexes for crystallization applications.« less

Monte Carlo calculation of large and small-angle electron scattering in air

DOE PAGES

Cohen, B. I.; Higginson, D. P.; Eng, C. D.; ...

2017-08-12

A Monte Carlo method for angle scattering of electrons in air that accommodates the small-angle multiple scattering and larger-angle single scattering limits is introduced. In this work, the algorithm is designed for use in a particle-in-cell simulation of electron transport and electromagnetic wave effects in air. The method is illustrated in example calculations.

Dynamic light scattering: A fast and reliable method to analyze bacterial growth during the lag phase.

PubMed

Vargas, Susana; Millán-Chiu, Blanca E; Arvizu-Medrano, Sofía M; Loske, Achim M; Rodríguez, Rogelio

2017-06-01

A comparison between plate counting (PC) and dynamic light scattering (DLS) is reported. PC is the standard technique to determine bacterial population as a function of time; however, this method has drawbacks, such as the cumbersome preparation and handling of samples, as well as the long time required to obtain results. Alternative methods based on optical density are faster, but do not distinguish viable from non-viable cells. These inconveniences are overcome by using DLS. Two different bacteria strains were considered: Escherichia coli and Staphylococcus aureus. DLS was performed at two different illuminating conditions: continuous and intermittent. By the increment of particle size as a function of time, it was possible to observe cell division and the formation of aggregates containing very few bacteria. The scattered intensity profiles showed the lag phase and the transition to the exponential phase of growth, providing a quantity proportional to viable bacteria concentration. The results revealed a clear and linear correlation in both lag and exponential phase, between the Log 10 (colony-forming units/mL) from PC and the Log 10 of the scattered intensity I s from DLS. These correlations provide a good support to use DLS as an alternative technique to determine bacterial population. Copyright © 2017 Elsevier B.V. All rights reserved.

Protein Analysis by Dynamic Light Scattering: Methods and Techniques for Students

ERIC Educational Resources Information Center

Lorber, Bernard; Fischer, Frederic; Bailly, Marc; Roy, Herve; Kern, Daniel

2012-01-01

Dynamic light scattering (DLS) analyses are routinely used in biology laboratories to detect aggregates in macromolecular solutions, to determine the size of proteins, nucleic acids, and complexes or to monitor the binding of ligands. This article is written for graduate and undergraduate students with access to DLS and for faculty members who…

Investigation of the structure of unilamellar dimyristoylphosphatidylcholine vesicles in aqueous sucrose solutions by small-angle neutron and X-ray scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kiselev, M. A., E-mail: elena@jinr.ru; Zemlyanaya, E. V.; Zhabitskaya, E. I.

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.

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

DOE PAGES

Allen, Andrew J.; Zhang, Fan; Kline, R. Joseph; ...

2017-03-07

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 thatmore » employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. As a result, 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.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allen, Andrew J.; Zhang, Fan; Kline, R. Joseph

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 thatmore » employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. As a result, 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.« less

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

PubMed

Allen, Andrew J; Zhang, Fan; Kline, R Joseph; Guthrie, William F; Ilavsky, Jan

2017-04-01

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.

Flocculation and aggregation in a microgravity environment (FAME)

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Dhadwal, Harbans S.; Suh, Kwang I.

1994-01-01

An experiment to study flocculation phenomena in the constrained microgravity environment of a space shuttle or space station is described. The small size and light weight experiment easily fits in a Spacelab Glovebox. Using an integrated fiber optic dynamic light scattering (DLS) system we obtain high precision particle size measurements from dispersions of colloidal particles within seconds, needs no onboard optical alignment, no index matching fluid, and offers sample mixing and shear melting capabilities to study aggregation (flocculation and coagulation) phenomena under both quiescent and controlled agitation conditions. The experimental system can easily be adapted for other microgravity experiments requiring the use of DLS. Preliminary results of ground-based study are reported.

Self-assembled stable sponge-type nanocarries for Brucea javanica oil delivery.

PubMed

Zou, Aihua; Li, Yawen; Chen, Yiyin; Angelova, Angelina; Garamus, Vasil M; Li, Na; Drechsler, Markus; Angelov, Borislav; Gong, Yabin

2017-05-01

Sponge-type nanocarriers (spongosomes) are produced upon dispersion of a liquid crystalline sponge phase formed by self-assembly of an amphiphilic lipid in excess aqueous phase. The inner organization of the spongosomes is built-up by randomly ordered bicontinuous lipid membranes and their surfaces are stabilized by alginate chains providing stealth properties and colloidal stability. The present study elaborates spongosomes for improved encapsulation of Brucea javanica oil (BJO), a traditional Chinese medicine that may strongly inhibit proliferation and metastasis of various cancers. The inner structural organization and the morphology characteristics of BJO-loaded nanocarriers at varying quantities of BJO were determined by cryogenic transmission electron microscopy (Cryo-TEM), small angle X-ray scattering (SAXS) and dynamic light scattering (DLS). Additionally, the drug loading and drug release profiles for BJO-loaded spongosome systems also were determined. We found that the sponge-type liquid crystalline lipid membrane organization provides encapsulation efficiency rate of BJO as high as 90%. In vitro cytotoxicity and apoptosis study of BJO spongosome nanoparticles with A549 cells demonstrated enhanced anti-tumor efficiency. These results suggest potential clinical applications of the obtained safe spongosome formulations. Copyright © 2017 Elsevier B.V. All rights reserved.

Multimeric species in equilibrium in detergent-solubilized Na,K-ATPase.

PubMed

Yoneda, Juliana Sakamoto; Scanavachi, Gustavo; Sebinelli, Heitor Gobbi; Borges, Júlio Cesar; Barbosa, Leandro R S; Ciancaglini, Pietro; Itri, Rosangela

2016-08-01

In this work, we find an equilibrium between different Na,K-ATPase (NKA) oligomeric species solubilized in a non-ionic detergent C12E8 by means of Dynamic Light Scattering (DLS), Analytical Ultracentrifugation (AUC), Small Angle X-ray Scattering (SAXS), Spectrophotometry (absorption at 280/350nm) and enzymatic activity assay. The NKA sample after chromatography purification presented seven different populations as identified by AUC, with monomers and tetramers amounting to ∼55% of the total protein mass in solution. These two species constituted less than 40% of the total protein mass after increasing the NKA concentration. Removal of higher-order oligomer/aggregate species from the NKA solution using 220nm-pore filter resulted in an increase of the specific enzymatic activity. Nevertheless, the enzyme forms new large aggregates over an elapsed time of 20h. The results thus point out that C12E8-solubilized NKA is in a dynamic equilibrium of monomers, tetramers and high-order oligomers/subunit aggregates. These latter have low or null activity. High amount of detergent leads to the dissociation of NKA into smaller aggregates with no enzymatic activity. Copyright © 2016. Published by Elsevier B.V.

Sizing of colloidal particle and protein molecules in a hanging fluid drop

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Suh, Kwang I.

1995-01-01

We report non-invasive particle size measurements of polystyrene latex colloidal particles and bovine serum albumin (BSA) protein molecules suspended in tiny hanging fluid drops of 30 micro-Liter volume using a newly designed fiber optic probe. The probe is based upon the principles of the technique of dynamic light scattering (DLS). The motivation for this work comes from growing protein crystals in outer space. Protein crystals have been grown previously in hanging drops in microgravity experiments on-board the space shuttle orbiter. However, obtaining quantitative information on nucleation and growth of the protein crystals in real time has always been a desired goal, but hitherto not achieved. Several protein researchers have shown interest in using DLS to monitor crystal growth process in a droplet, but elaborate instrumentation and optical alignment problems have made in-situ applications difficult. We demonstrate that such an experiment is now possible. Our system offers fast (5 seconds) determination of particle size, utilize safe levels of very low laser power (less than or equal to 0.2 mW), a small scattering volume (approximately 2 x 10(exp -5) cu mm) and high spatial coherence (Beta) values. This is a major step forward when compared to currently available DLS systems.

Charactrisation of particle assemblies by 3D cross correlation light scattering and diffusing wave spectroscopy

NASA Astrophysics Data System (ADS)

Scheffold, Frank

2014-08-01

To characterize the structural and dynamic properties of soft materials and small particles, information on the relevant mesoscopic length scales is required. Such information is often obtained from traditional static and dynamic light scattering (SLS/DLS) experiments in the single scattering regime. In many dense systems, however, these powerful techniques frequently fail due to strong multiple scattering of light. Here I will discuss some experimental innovations that have emerged over the last decade. New methods such as 3D static and dynamic light scattering (3D LS) as well as diffusing wave spectroscopy (DWS) can cover a much extended range of experimental parameters ranging from dilute polymer solutions, colloidal suspensions to extremely opaque viscoelastic emulsions.

A Fiber Optic Probe for Monitoring Protein Aggregation, Nucleation, and Crystallization

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Suh, Kwang I.; Arabshahi, Alireza; Wilson, William W.; Bray, Terry L.; DeLucas, Lawrence J.

1996-01-01

Protein crystals are experimentally grown in hanging drops in microgravity experiments on-board the Space Shuttle orbiter. The technique of dynamic light scattering (DLS) can be used to monitor crystal growth process in hanging droplets (approx. 30 (L)) in microgravity experiments, but elaborate instrumentation and optical alignment problems have made in-situ applications difficult. In this paper we demonstrate that such experiments are now feasible. We apply a newly developed fiber optic probe to various earth and space (micro- gravity) bound protein crystallization system configurations to test its capability. These include conventional batch (cuvette or capillary) systems, hanging drop method in a six-pack hanging drop vapor diffusion apparatus (HDVDA), a modified HDVDA for temperature- induced nucleation and aggregation studies, and a newly envisioned dynamically controlled vapor diffusion system (DCVDS) configuration. Our compact system exploits the principles of DLS and offers a fast (within a few seconds) means of quantitatively and non-invasively monitoring the various growth stages of protein crystallization. In addition to DLS capability, the probe can also be used for performing single-angle static light scattering measurements. It utilizes extremely low levels of laser power (approx. few (W)) without a need of having any optical alignment and vibration isolation. The compact probe is also equipped with a miniaturized microscope for visualization of macroscopic protein crystals. This new optical diagnostic system opens up enormous opportunity for exploring new ways to grow good quality crystals suitable for x-ray crystallographic analysis and may help develop a concrete scientific basis for understanding the process of crystallization.

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

PubMed

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

2012-05-17

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

Multiple-Fiber-Optic Probe For Light-Scattering Measurements

NASA Technical Reports Server (NTRS)

Dhadwal, Harbans Singh; Ansari, Rafat R.

1996-01-01

Multiple-fiber-optical probe developed for use in measuring light scattered at various angles from specimens of materials. Designed for both static and dynamic light-scattering measurements of colloidal dispersions. Probe compact, rugged unit containing no moving parts and remains stationary during operation. Not restricted to operation in controlled, research-laboratory environment. Positioned inside or outside light-scattering chamber. Provides simultaneous measurements at small angular intervals over range of angles, made to include small scattering angles by orienting probe in appropriate direction.

Dynamic light scattering as an objective noninvasive method in veterinary ophthalmic diagnosis and research

NASA Astrophysics Data System (ADS)

Dubin, Stephen; Ansari, Rafat R.; Tulp, Orien; Steinberg, Sheldon; Koch, Seth; DellaVecchia, Michael A.; Cozmi, Mihaela; Victor, Mary

1999-06-01

The absence of verbal feedback, available from most human patients, is a major limitation in veterinary diagnosis in general and in the evaluation of ophthalmic lens opacity in particular. A novel compact dynamic light scattering (DLS) instrument, developed at NASA, offers significant mitigation to this limitation. It not only yields objective repeatable non-invasive estimation of lens opacity but also provides insight into the nature of chemical and physical alternations in the lens and other eye structures. For example, DLS measurements of the cataractous lens may be interpreted in terms of alpha crystalline protein size. In contrast to most conventional methods, the examination results are numerical and readily accommodate statistical analysis. We present results of DLS measurements in laboratory rabbits with naphthalene induced cataracts, rodents with genetically conditioned hypertension and/or diabetes mellitus; as well as applications of the DLS method in clinical veterinary patients. Use of DLS in examination of phacoemulsification fluid, urine and other biological materials, and potential applications in ocular toxically will also be discussed.

Small-angle X-ray scattering (SAXS) studies of the structure of mesoporous silicas

NASA Astrophysics Data System (ADS)

Zienkiewicz-Strzałka, M.; Skibińska, M.; Pikus, S.

2017-11-01

Mesoporous ordered silica nanostructures show strong interaction with X-ray radiation in the range of small-angles. Small-angle X-ray scattering (SAXS) measurements based on the elastically scattered X-rays are important in analysis of condensed matter. In the case of mesoporous silica materials SAXS technique provides information on the distribution of electron density in the mesoporous material, in particular describing their structure and size of the unit cell as well as type of ordered structure and finally their parameters. The characterization of nanopowder materials, nanocomposites and porous materials by Small-Angle X-ray Scattering seems to be valuable and useful. In presented work, the SAXS investigation of structures from the group of mesoporous ordered silicates was performed. This work has an objective to prepare functional materials modified by noble metal ions and nanoparticles and using the small-angle X-ray scattering to illustrate their properties. We report the new procedure for describing mesoporous materials belonging to SBA-15 and MCM-41 family modified by platinum, palladium and silver nanoparticles, based on detailed analysis of characteristic peaks in the small-angle range of X-ray scattering. This procedure allows to obtained the most useful parameters for mesoporous materials characterization and their successfully compare with experimental measurements reducing the time and material consumption with good precision for particles and pores with a size below 10 nm.

Irena : tool suite for modeling and analysis of small-angle scattering.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ilavsky, J.; Jemian, P.

2009-04-01

Irena, a tool suite for analysis of both X-ray and neutron small-angle scattering (SAS) data within the commercial Igor Pro application, brings together a comprehensive suite of tools useful for investigations in materials science, physics, chemistry, polymer science and other fields. In addition to Guinier and Porod fits, the suite combines a variety of advanced SAS data evaluation tools for the modeling of size distribution in the dilute limit using maximum entropy and other methods, dilute limit small-angle scattering from multiple non-interacting populations of scatterers, the pair-distance distribution function, a unified fit, the Debye-Bueche model, the reflectivity (X-ray and neutron)more » using Parratt's formalism, and small-angle diffraction. There are also a number of support tools, such as a data import/export tool supporting a broad sampling of common data formats, a data modification tool, a presentation-quality graphics tool optimized for small-angle scattering data, and a neutron and X-ray scattering contrast calculator. These tools are brought together into one suite with consistent interfaces and functionality. The suite allows robust automated note recording and saving of parameters during export.« less

A review of exosome separation techniques and characterization of B16-F10 mouse melanoma exosomes with AF4-UV-MALS-DLS-TEM.

PubMed

Petersen, Kevin E; Manangon, Eliana; Hood, Joshua L; Wickline, Samuel A; Fernandez, Diego P; Johnson, William P; Gale, Bruce K

2014-12-01

Exosomes participate in cancer metastasis, but studying them presents unique challenges as a result of their small size and purification difficulties. Asymmetrical field flow fractionation with in-line ultraviolet absorbance, dynamic light scattering, and multi-angle light scattering was applied to the size separation and characterization of non-labeled B16-F10 exosomes from an aggressive mouse melanoma cell culture line. Fractions were collected and further analyzed using batch mode dynamic light scattering, transmission electron microscopy and compared with known size standards. Fractogram peak positions and computed radii show good agreement between samples and across fractions. Ultraviolet absorbance fractograms in combination with transmission electron micrographs were able to resolve subtle heterogeneity of vesicle retention times between separate batches of B16-F10 exosomes collected several weeks apart. Further, asymmetrical field flow fractionation also effectively separated B16-F10 exosomes into vesicle subpopulations by size. Overall, the flow field flow fractionation instrument combined with multiple detectors was able to rapidly characterize and separate exosomes to a degree not previously demonstrated. These approaches have the potential to facilitate a greater understanding of exosome function by subtype, as well as ultimately allow for "label-free" isolation of large scale clinical exosomes for the purpose of developing future exosome-based diagnostics and therapeutics.

A review of exosome separation techniques and characterization of B16-F10 mouse melanoma exosomes with AF4-UV-MALS-DLS-TEM

PubMed Central

Manangon, Eliana; Hood, Joshua L.; Wickline, Samuel A.; Fernandez, Diego P.; Johnson, William P.; Gale, Bruce K.

2015-01-01

Exosomes participate in cancer metastasis, but studying them presents unique challenges as a result of their small size and purification difficulties. Asymmetrical field flow fractionation with in-line ultraviolet absorbance, dynamic light scattering, and multi-angle light scattering was applied to the size separation and characterization of non-labeled B16-F10 exosomes from an aggressive mouse melanoma cell culture line. Fractions were collected and further analyzed using batch mode dynamic light scattering, transmission electron microscopy and compared with known size standards. Fractogram peak positions and computed radii show good agreement between samples and across fractions. Ultraviolet absorbance fractograms in combination with transmission electron micrographs were able to resolve subtle heterogeneity of vesicle retention times between separate batches of B16-F10 exosomes collected several weeks apart. Further, asymmetrical field flow fractionation also effectively separated B16-F10 exosomes into vesicle subpopulations by size. Overall, the flow field flow fractionation instrument combined with multiple detectors was able to rapidly characterize and separate exosomes to a degree not previously demonstrated. These approaches have the potential to facilitate a greater understanding of exosome function by subtype, as well as ultimately allow for “label-free” isolation of large scale clinical exosomes for the purpose of developing future exosome-based diagnostics and therapeutics. PMID:25084738

Primary Data Treatment Software for Position-Sensitive Detector of Small-Angle Neutron Scattering Spectrometer in the Isotropic Pattern Scattering Case

NASA Astrophysics Data System (ADS)

Soloviev, Alexei; Kutuzov, Sergei; Ivankov, Olexander; Kuklin, Alexander

2018-02-01

A new data converter has been created for the new position-sensitive detector (PSD) of small-angle neutron scattering (SANS) spectrometer YuMO. In the isotropic pattern scattering case, it provides the possibility for processing PSD data with the SAS data processing program that has already been in use.

Characterization of magnetic nanoparticle by dynamic light scattering

PubMed Central

2013-01-01

Here we provide a complete review on the use of dynamic light scattering (DLS) to study the size distribution and colloidal stability of magnetic nanoparticles (MNPs). The mathematical analysis involved in obtaining size information from the correlation function and the calculation of Z-average are introduced. Contributions from various variables, such as surface coating, size differences, and concentration of particles, are elaborated within the context of measurement data. Comparison with other sizing techniques, such as transmission electron microscopy and dark-field microscopy, revealed both the advantages and disadvantages of DLS in measuring the size of magnetic nanoparticles. The self-assembly process of MNP with anisotropic structure can also be monitored effectively by DLS. PMID:24011350

CONTIN XPCS: software for inverse transform analysis of X-ray photon correlation spectroscopy dynamics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andrews, Ross N.; Narayanan, Suresh; Zhang, Fan

X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) reveal materials dynamics using coherent scattering, with XPCS permitting the investigation of dynamics in a more diverse array of materials than DLS. Heterogeneous dynamics occur in many material systems. The authors' recent work has shown how classic tools employed in the DLS analysis of heterogeneous dynamics can be extended to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. The present work describes the software implementation of inverse transform analysis of XPCS data. This software, calledCONTIN XPCS, is an extension of traditionalCONTINanalysis and accommodates the various dynamics encountered inmore » equilibrium XPCS measurements.« less

CONTIN XPCS: software for inverse transform analysis of X-ray photon correlation spectroscopy dynamics

DOE PAGES

Andrews, Ross N.; Narayanan, Suresh; Zhang, Fan; ...

2018-02-01

X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) reveal materials dynamics using coherent scattering, with XPCS permitting the investigation of dynamics in a more diverse array of materials than DLS. Heterogeneous dynamics occur in many material systems. The authors' recent work has shown how classic tools employed in the DLS analysis of heterogeneous dynamics can be extended to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. The present work describes the software implementation of inverse transform analysis of XPCS data. This software, calledCONTIN XPCS, is an extension of traditionalCONTINanalysis and accommodates the various dynamics encountered inmore » equilibrium XPCS measurements.« less

A Method for Identifying Small-Molecule Aggregators Using Photonic Crystal Biosensor Microplates

PubMed Central

Chan, Leo L.; Lidstone, Erich A.; Finch, Kristin E.; Heeres, James T.; Hergenrother, Paul J.; Cunningham, Brian T.

2010-01-01

Small molecules identified through high-throughput screens are an essential element in pharmaceutical discovery programs. It is now recognized that a substantial fraction of small molecules exhibit aggregating behavior leading to false positive results in many screening assays, typically due to nonspecific attachment to target proteins. Therefore, the ability to efficiently identify compounds within a screening library that aggregate can streamline the screening process by eliminating unsuitable molecules from further consideration. In this work, we show that photonic crystal (PC) optical biosensor microplate technology can be used to identify and quantify small-molecule aggregation. A group of aggregators and nonaggregators were tested using the PC technology, and measurements were compared with those gathered by three alternative methods: dynamic light scattering (DLS), an α-chymotrypsin colorimetric assay, and scanning electron microscopy (SEM). The PC biosensor measurements of aggregation were confirmed by visual observation using SEM, and were in general agreement with the α-chymotrypsin assay. DLS measurements, in contrast, demonstrated inconsistent readings for many compounds that are found to form aggregates in shapes, very different from the classical spherical particles assumed in DLS modeling. As a label-free detection method, the PC biosensor aggregation assay is simple to implement and provides a quantitative direct measurement of the mass density of material adsorbed to the transducer surface, whereas the microplate-based sensor format enables compatibility with high-throughput automated liquid-handling methods used in pharmaceutical screening. PMID:20930952

Adsorption of Small Cationic Nanoparticles onto Large Anionic Particles from Aqueous Solution: A Model System for Understanding Pigment Dispersion and the Problem of Effective Particle Density.

PubMed

North, S M; Jones, E R; Smith, G N; Mykhaylyk, O O; Annable, T; Armes, S P

2017-02-07

The present study focuses on the use of copolymer nanoparticles as a dispersant for a model pigment (silica). Reversible addition-fragmentation chain transfer (RAFT) alcoholic dispersion polymerization was used to synthesize sterically stabilized diblock copolymer nanoparticles. The steric stabilizer block was poly(2-(dimethylamino)ethyl methacrylate) (PDMA) and the core-forming block was poly(benzyl methacrylate) (PBzMA). The mean degrees of polymerization for the PDMA and PBzMA blocks were 71 and 100, respectively. Transmission electron microscopy (TEM) studies confirmed a near-monodisperse spherical morphology, while dynamic light scattering (DLS) studies indicated an intensity-average diameter of 30 nm. Small-angle X-ray scattering (SAXS) reported a volume-average diameter of 29 ± 0.5 nm and a mean aggregation number of 154. Aqueous electrophoresis measurements confirmed that these PDMA 71 -PBzMA 100 nanoparticles acquired cationic character when transferred from ethanol to water as a result of protonation of the weakly basic PDMA chains. Electrostatic adsorption of these nanoparticles from aqueous solution onto 470 nm silica particles led to either flocculation at submonolayer coverage or steric stabilization at or above monolayer coverage, as judged by DLS. This technique indicated that saturation coverage was achieved on addition of approximately 465 copolymer nanoparticles per silica particle, which corresponds to a fractional surface coverage of around 0.42. These adsorption data were corroborated using thermogravimetry, UV spectroscopy and X-ray photoelectron spectroscopy. TEM studies indicated that the cationic nanoparticles remained intact on the silica surface after electrostatic adsorption, while aqueous electrophoresis confirmed that surface charge reversal occurred below pH 7. The relatively thick layer of adsorbed nanoparticles led to a significant reduction in the effective particle density of the silica particles from 1.99 g cm -3 to approximately 1.74 g cm -3 , as judged by disk centrifuge photosedimentometry (DCP). Combining the DCP and SAXS data suggests that essentially no deformation of the PBzMA cores occurs during nanoparticle adsorption onto the silica particles.

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Effects of macromolecular crowding on the structure of a protein complex: A small-angle scattering study of superoxide dismutase

DOE PAGES

Rajapaksha, Ajith; Stanley, Christopher B.; Todd, Brian A.

2015-02-17

Macromolecular crowding can alter the structure and function of biological macromolecules. We used small angle scattering (SAS) to measure the change in size of a protein complex, superoxide dismutase (SOD), induced by macromolecular crowding. Crowding was induced using 400 MW polyethylene glycol (PEG), triethylene glycol (TEG), methyl- -glucoside ( -MG) and trimethylamine N-oxide (TMAO). Parallel small angle neutron scattering (SANS) and small angle x-ray scattering (SAXS) allowed us to unambiguously attribute apparent changes in radius of gyration to changes in the structure of SOD. For a 40% PEG solution, we find that the volume of SOD was reduced by 9%.more » Considering the osmotic pressure due to PEG, this deformation corresponds to a highly compressible structure. SAXS done in the presence of TEG suggests that for further deformation beyond a 9% decrease in volume the resistance to deformation may increase dramatically.« less

Surface Modifier-Free Organic-Inorganic Hybridization To Produce Optically Transparent and Highly Refractive Bulk Materials Composed of Epoxy Resins and ZrO2 Nanoparticles.

PubMed

Enomoto, Kazushi; Kikuchi, Moriya; Narumi, Atsushi; Kawaguchi, Seigou

2018-04-25

Surface modifier-free hybridization of ZrO 2 nanoparticles (NPs) with epoxy-based polymers is demonstrated for the first time to afford highly transparent and refractive bulk materials. This is achieved by a unique and versatile hybridization via the one-pot direct phase transfer of ZrO 2 NPs from water to epoxy monomers without any aggregation followed by curing with anhydride. Three types of representative epoxy monomers, bisphenol A diglycidyl ether (BADGE), 3,4-epoxycyclohexylmethyl-3',4'-epoxycyclohexane carboxylate (CEL), and 1,3,5-tris(3-(oxiran-2-yl)propyl)-1,3,5-triazinane-2,4,6-trione (TEPIC), are used to produce transparent viscous dispersions. The resulting ZrO 2 NPs are thoroughly characterized using dynamic light scattering (DLS), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR), and solid-state 13 C CP/MAS NMR measurements. The results from DLS and TEM analyses indicate nanodispersion of ZrO 2 into epoxy monomers as a continuous medium. A surface modification mechanism and the binding fashion during phase transfer are proposed based on the FT-IR and solid-state 13 C CP/MAS NMR measurements. Epoxy-based hybrid materials with high transparency and refractive index are successfully fabricated by heat curing or polymerizing a mixture of monomers containing epoxy-functionalized ZrO 2 NPs and methylhexahydrophthalic anhydride in the presence of a phosphoric catalyst. The TEM and small-angle X-ray scattering measurements of the hybrids show a nanodispersion of ZrO 2 in the epoxy networks. The refractive index at 594 nm ( n 594 ) increases up to 1.765 for BADGE-based hybrids, 1.667 for CEL-based hybrids, and 1.693 for TEPIC-based hybrids. Their refractive indices and Abbe's numbers are quantitatively described by the Lorentz-Lorenz effective medium expansion theory. Their transmissivity is also reasonably explained using Fresnel refraction, Rayleigh scattering, and the Lambert-Beer theories. This surface modifier-free hybridization provides a versatile, fascinating, and promising method for synthesizing a variety of epoxy-based hybrid materials.

Application of dynamic light scattering for studying the evolution of micro- and nano-droplets

NASA Astrophysics Data System (ADS)

Derkachov, G.; Jakubczyk, D.; Kolwas, K.; Shopa, Y.; Woźniak, M.; Wojciechowski, T.

2018-01-01

The dynamic light scattering (DLS) technique was used for studying the processes of aggregation of spherical SiO2 particles in various diethylene glycol (DEG) suspensions. The suspensions were studied in a cuvette, in a millimeter-sized droplet and in a micrometer-sized droplet. For the first time DLS signals for droplets of picolitre volume, levitated in an electrodynamic quadrupole trap, were obtained. It is shown that the correlation analysis of light scattered from a micro-droplet allows monitoring the changes of its internal structure, as well as its motions: trap-constricted Brownian motions and random rotations.

Spider Silk-CBD-Cellulose Nanocrystal Composites: Mechanism of Assembly

PubMed Central

Meirovitch, Sigal; Shtein, Zvi; Ben-Shalom, Tal; Lapidot, Shaul; Tamburu, Carmen; Hu, Xiao; Kluge, Jonathan A.; Raviv, Uri; Kaplan, David L.; Shoseyov, Oded

2016-01-01

The fabrication of cellulose-spider silk bio-nanocomposites comprised of cellulose nanocrystals (CNCs) and recombinant spider silk protein fused to a cellulose binding domain (CBD) is described. Silk-CBD successfully binds cellulose, and unlike recombinant silk alone, silk-CBD self-assembles into microfibrils even in the absence of CNCs. Silk-CBD-CNC composite sponges and films show changes in internal structure and CNC alignment related to the addition of silk-CBD. The silk-CBD sponges exhibit improved thermal and structural characteristics in comparison to control recombinant spider silk sponges. The glass transition temperature (Tg) of the silk-CBD sponge was higher than the control silk sponge and similar to native dragline spider silk fibers. Gel filtration analysis, dynamic light scattering (DLS), small angle X-ray scattering (SAXS) and cryo-transmission electron microscopy (TEM) indicated that silk-CBD, but not the recombinant silk control, formed a nematic liquid crystalline phase similar to that observed in native spider silk during the silk spinning process. Silk-CBD microfibrils spontaneously formed in solution upon ultrasonication. We suggest a model for silk-CBD assembly that implicates CBD in the central role of driving the dimerization of spider silk monomers, a process essential to the molecular assembly of spider-silk nanofibers and silk-CNC composites. PMID:27649169

Self-similar assemblies of globular whey proteins at the air-water interface: effect of the structure.

PubMed

Mahmoudi, Najet; Gaillard, Cédric; Boué, François; Axelos, Monique A V; Riaublanc, Alain

2010-05-01

We investigated the structure of heat-induced assemblies of whey globular proteins using small angle neutron scattering (SANS), static and dynamic light scattering (SLS and DLS), and cryogenic transmission electron microscopy (Cryo-TEM). Whey protein molecules self-assemble in fractal aggregates with a structure density depending on the electrostatic interactions. We determined the static and dynamic properties of interfacial layer formed by the protein assemblies, upon adsorption and spreading at the air-water interface using surface film balance and interfacial dilatational rheology. Upon spreading, all whey protein systems show a power-law scaling behavior of the surface pressure versus concentration in the semi-dilute surface concentration regime, with an exponent ranging from 5.5 to 9 depending on the electrostatic interactions and the aggregation state. The dilatational modulus derived from surface pressure isotherms shows a main peak at 6-8 mN/m, generally considered to be the onset of a conformational change in the monolayer, and a second peak or a shoulder at 15 mN/m. Long-time adsorption kinetics give similar results for both the native whey proteins and the corresponding self-similar assemblies, with a systematic effect of the ionic strength. Copyright 2010 Elsevier Inc. All rights reserved.

Spider Silk-CBD-Cellulose Nanocrystal Composites: Mechanism of Assembly.

PubMed

Meirovitch, Sigal; Shtein, Zvi; Ben-Shalom, Tal; Lapidot, Shaul; Tamburu, Carmen; Hu, Xiao; Kluge, Jonathan A; Raviv, Uri; Kaplan, David L; Shoseyov, Oded

2016-09-18

The fabrication of cellulose-spider silk bio-nanocomposites comprised of cellulose nanocrystals (CNCs) and recombinant spider silk protein fused to a cellulose binding domain (CBD) is described. Silk-CBD successfully binds cellulose, and unlike recombinant silk alone, silk-CBD self-assembles into microfibrils even in the absence of CNCs. Silk-CBD-CNC composite sponges and films show changes in internal structure and CNC alignment related to the addition of silk-CBD. The silk-CBD sponges exhibit improved thermal and structural characteristics in comparison to control recombinant spider silk sponges. The glass transition temperature (Tg) of the silk-CBD sponge was higher than the control silk sponge and similar to native dragline spider silk fibers. Gel filtration analysis, dynamic light scattering (DLS), small angle X-ray scattering (SAXS) and cryo-transmission electron microscopy (TEM) indicated that silk-CBD, but not the recombinant silk control, formed a nematic liquid crystalline phase similar to that observed in native spider silk during the silk spinning process. Silk-CBD microfibrils spontaneously formed in solution upon ultrasonication. We suggest a model for silk-CBD assembly that implicates CBD in the central role of driving the dimerization of spider silk monomers, a process essential to the molecular assembly of spider-silk nanofibers and silk-CNC composites.

SMALL ANGLE SCATTERING OF X-RAYS BY PLASTICALLY DEFORMED SINGLE CRYSTALS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Robinson, W.H.; Smoluchowski, R.

1959-05-01

The small-angle scattering of x rays from single crystals of magnesium plastically deformed by simple shear was measured in the angular range of 4' to 5 deg . The crystals were subjected to both unidirectional and cyclic shear stresses applied along the STAl 1 2-bar 0! direction. Thin slices of the deformed single crystals were prepared using strainfree cutting and polishing techniques. The thin slices had orientations such that the slip direction was either parallel or perpendicular to the incident x-ray beam in order to observe any anisotropy in the scattering that might be due to dislocations. It was foundmore » that those samples which contained deformation twins within the irradiated volume produced rather large scattered intensity. This scattered intensity is interpreted as being due to double Bragg scattering. The scattered intensity from other specimens was attributed to surface scattering. No evidence for small angle scattering by dislocations was found. (auth)« less

Self-aggregation of sodium dodecyl sulfate within (choline chloride + urea) deep eutectic solvent.

PubMed

Pal, Mahi; Rai, Rewa; Yadav, Anita; Khanna, Rajesh; Baker, Gary A; Pandey, Siddharth

2014-11-11

Deep eutectic solvents (DESs) have shown tremendous promise as green solvents with low toxicity and cost. Understanding molecular aggregation processes within DESs will not only enhance the application potential of these solvents but also help alleviate some of the limitations associated with them. Among DESs, those comprising choline chloride and appropriate hydrogen-bond donors are inexpensive and easy to prepare. On the basis of fluorescence probe, electrical conductivity, and surface tension experiments, we present the first clear lines of evidence for self-aggregation of an anionic surfactant within a DES containing a small fraction of water. Namely, well-defined assemblies of sodium dodecyl sulfate (SDS) apparently form in the archetype DES Reline comprising a 1:2 molar mixture of choline chloride and urea. Significant enhancement in the solubility of organic solvents that are otherwise not miscible in choline chloride-based DESs is achieved within Reline in the presence of SDS. The remarkably improved solubility of cyclohexane within SDS-added Reline is attributed to the presence of spontaneously formed cyclohexane-in-Reline microemulsions by SDS under ambient conditions. Surface tension, dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), density, and dynamic viscosity measurements along with responses from the fluorescence dipolarity and microfluidity probes of pyrene and 1,3-bis(1-pyrenyl)propane are employed to characterize these aggregates. Such water-free oil-in-DES microemulsions are appropriately sized to be considered as a new type of nanoreactor.

Small-angle x-ray scattering investigations of extrudates

NASA Astrophysics Data System (ADS)

Pikus, Stanislaw; Jamroz, Jerzy

1997-02-01

The small-angle X-ray scattering investigations of the extrudes are presented. The investigations of the different samples of starch by means of the SAXS indicate the new possibilities for using this method for extrudates examination. Results obtained by SAXS method of close dependance between intensity SAXS scattering and characteristic parameters of the extrudates were shown.

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.

Size-dependent interaction of silica nanoparticles with lysozyme and bovine serum albumin proteins

NASA Astrophysics Data System (ADS)

Yadav, Indresh; Aswal, Vinod K.; Kohlbrecher, Joachim

2016-05-01

The interaction of three different sized (diameter 10, 18, and 28 nm) anionic silica nanoparticles with two model proteins—cationic lysozyme [molecular weight (MW) 14.7 kDa)] and anionic bovine serum albumin (BSA) (MW 66.4 kDa) has been studied by UV-vis spectroscopy, dynamic light scattering (DLS), and small-angle neutron scattering (SANS). The adsorption behavior of proteins on the nanoparticles, measured by UV-vis spectroscopy, is found to be very different for lysozyme and BSA. Lysozyme adsorbs strongly on the nanoparticles and shows exponential behavior as a function of lysozyme concentration irrespective of the nanoparticle size. The total amount of adsorbed lysozyme, as governed by the surface-to-volume ratio, increases on lowering the size of the nanoparticles for a fixed volume fraction of the nanoparticles. On the other hand, BSA does not show any adsorption for all the different sizes of the nanoparticles. Despite having different interactions, both proteins induce similar phase behavior where the nanoparticle-protein system transforms from one phase (clear) to two phase (turbid) as a function of protein concentration. The phase behavior is modified towards the lower concentrations for both proteins with increasing the nanoparticle size. DLS suggests that the phase behavior arises as a result of the nanoparticles' aggregation on the addition of proteins. The size-dependent modifications in the interaction potential, responsible for the phase behavior, have been determined by SANS data as modeled using the two-Yukawa potential accounting for the repulsive and attractive interactions in the systems. The protein-induced interaction between the nanoparticles is found to be short-range attraction for lysozyme and long-range attraction for BSA. The magnitude of attractive interaction irrespective of protein type is enhanced with increase in the size of the nanoparticles. The total (attractive+repulsive) potential leading to two-phase formation is found to be more attractive for larger sized nanoparticles. The nanoparticle aggregates are characterized by mass fractal.

Structural evolution of photocrosslinked silk fibroin and silk fibroin-based hybrid hydrogels: A small angle and ultra-small angle scattering investigation.

PubMed

Whittaker, Jasmin L; Balu, Rajkamal; Knott, Robert; de Campo, Liliana; Mata, Jitendra P; Rehm, Christine; Hill, Anita J; Dutta, Naba K; Roy Choudhury, Namita

2018-07-15

Regenerated Bombyx mori silk fibroin (RSF) is a widely recognized protein for biomedical applications; however, its hierarchical gel structure is poorly understood. In this paper, the hierarchical structure of photocrosslinked RSF and RSF-based hybrid hydrogel systems: (i) RSF/Rec1-resilin and (ii) RSF/poly(N-vinylcaprolactam (PVCL) is reported for the first time using small-angle scattering (SAS) techniques. The structure of RSF in dilute to concentrated solution to fabricated hydrogels were characterized using small angle X-ray scattering (SAXS), small angle neutron scattering (SANS) and ultra-small angle neutron scattering (USANS) techniques. The RSF hydrogel exhibited three distinctive structural characteristics: (i) a Porod region in the length scale of 2 to 3nm due to hydrophobic domains (containing β-sheets) which exhibits sharp interfaces with the amorphous matrix of the hydrogel and the solvent, (ii) a Guinier region in the length scale of 4 to 20nm due to hydrophilic domains (containing turns and random coil), and (iii) a Porod-like region in the length scale of few micrometers due to water pores/channels exhibiting fractal-like characteristics. Addition of Rec1-resilin or PVCL to RSF and subsequent crosslinking systematically increased the nanoscale size of hydrophobic and hydrophilic domains, whereas decreased the homogeneity of pore size distribution in the microscale. The presented results have implications on the fundamental understanding of the structure-property relationship of RSF-based hydrogels. Copyright © 2018. Published by Elsevier B.V.

Stabilizing Off-pathway Oligomers by Polyphenol Nanoassemblies for IAPP Aggregation Inhibition

NASA Astrophysics Data System (ADS)

Nedumpully-Govindan, Praveen; Kakinen, Aleksandr; Pilkington, Emily H.; Davis, Thomas P.; Chun Ke, Pu; Ding, Feng

2016-01-01

Experimental studies have shown that many naturally occurring polyphenols have inhibitory effect on the aggregation of several proteins. Here, we use discrete molecular dynamics (DMD) simulations and high-throughput dynamic light scattering (DLS) experiments to study the anti-aggregation effects of two polyphenols, curcumin and resveratrol, on the aggregation of islet amyloid polypeptide (IAPP or amylin). Our DMD simulations suggest that the aggregation inhibition is caused by stabilization of small molecular weight IAPP off-pathway oligomers by the polyphenols. Our analysis indicates that IAPP-polyphenol hydrogen bonds and π-π stacking combined with hydrophobic interactions are responsible for the stabilization of oligomers. The presence of small oligomers is confirmed with DLS measurements in which nanometer-sized oligomers are found to be stable for up to 7.5 hours, the time frame within which IAPP aggregates in the absence of polyphenols. Our study offers a general anti-aggregation mechanism for polyphenols, and further provides a computational framework for the future design of anti-amyloid aggregation therapeutics.

Pinhole-type two-dimensional ultra-small-angle X-ray scattering on the micrometer scale

PubMed Central

Kishimoto, Hiroyuki; Shinohara, Yuya; Suzuki, Yoshio; Takeuchi, Akihisa; Yagi, Naoto; Amemiya, Yoshiyuki

2014-01-01

A pinhole-type two-dimensional ultra-small-angle X-ray scattering set-up at a so-called medium-length beamline at SPring-8 is reported. A long sample-to-detector distance, 160.5 m, can be used at this beamline and a small-angle resolution of 0.25 µm−1 was thereby achieved at an X-ray energy of 8 keV. PMID:24365910

Effective phase function of light scattered at small angles by polydisperse particulate media

NASA Astrophysics Data System (ADS)

Turcu, I.

2008-06-01

Particles with typical dimensions higher than the light wavelength and relative refraction indexes close to one, scatter light mainly in the forward direction where the scattered light intensity has a narrow peak. For particulate media accomplishing these requirements the light scattered at small angles in a far-field detecting set-up can be described analytically by an effective phase function (EPF) even in the multiple scattering regime. The EPF model which was built for monodispersed systems has been extended to polydispersed media. The main ingredients consist in the replacement of the single particle phase function and of the optical thickness with their corresponding averaged values. Using a Gamma particle size distribution (PSD) as a testing model, the effect of polydispersity was systematically investigated. The increase of the average radius or/and of the PSD standard deviation leads to the decrease of the angular spreading of the small angle scattered light.

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

PubMed Central

Duff, Anthony P.; Durand, Dominique; Gabel, Frank; Hendrickson, Wayne A.; Hura, Greg L.; Jacques, David A.; Kirby, Nigel M.; Kwan, Ann H.; Pérez, Javier; Pollack, Lois; Ryan, Timothy M.; Sali, Andrej; Schneidman-Duhovny, Dina; Vachette, Patrice; Westbrook, John

2017-01-01

In 2012, preliminary guidelines were published addressing sample quality, data acquisition and reduction, presentation of scattering data and validation, and modelling for biomolecular small-angle scattering (SAS) experiments. Bio­molecular SAS has since continued to grow and authors have increasingly adopted the preliminary guidelines. In parallel, integrative/hybrid determination of biomolecular structures is a rapidly growing field that is expanding the scope of structural biology. For SAS to contribute maximally to this field, it is essential to ensure open access to the information required for evaluation of the quality of SAS samples and data, as well as the validity of SAS-based structural models. To this end, the preliminary guidelines for data presentation in a publication are reviewed and updated, and the deposition of data and associated models in a public archive is recommended. These guidelines and recommendations have been prepared in consultation with the members of the International Union of Crystallography (IUCr) Small-Angle Scattering and Journals Commissions, the Worldwide Protein Data Bank (wwPDB) Small-Angle Scattering Validation Task Force and additional experts in the field. PMID:28876235

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Utilizing dynamic light scattering as a process analytical technology for protein folding and aggregation monitoring in vaccine manufacturing.

PubMed

Yu, Zhou; Reid, Jennifer C; Yang, Yan-Ping

2013-12-01

Protein aggregation is a common challenge in the manufacturing of biological products. It is possible to minimize the extent of aggregation through timely measurement and in-depth characterization of aggregation. In this study, we demonstrated the use of dynamic light scattering (DLS) to monitor inclusion body (IB) solubilization, protein refolding, and aggregation near the production line of a recombinant protein-based vaccine candidate. Our results were in good agreement with those measured by size-exclusion chromatography. DLS was also used to characterize the mechanism of aggregation. As DLS is a quick, nonperturbing technology, it can potentially be used as an at-line process analytical technology to ensure complete IB solubilization and aggregate-free refolding. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association.

A full-angle Monte-Carlo scattering technique including cumulative and single-event Rutherford scattering in plasmas [Theory of cumulative large-angle collisions in plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Higginson, Drew P.

Here, we describe and justify a full-angle scattering (FAS) method to faithfully reproduce the accumulated differential angular Rutherford scattering probability distribution function (pdf) of particles in a plasma. The FAS method splits the scattering events into two regions. At small angles it is described by cumulative scattering events resulting, via the central limit theorem, in a Gaussian-like pdf; at larger angles it is described by single-event scatters and retains a pdf that follows the form of the Rutherford differential cross-section. The FAS method is verified using discrete Monte-Carlo scattering simulations run at small timesteps to include each individual scattering event.more » We identify the FAS regime of interest as where the ratio of temporal/spatial scale-of-interest to slowing-down time/length is from 10 -3 to 0.3–0.7; the upper limit corresponds to Coulomb logarithm of 20–2, respectively. Two test problems, high-velocity interpenetrating plasma flows and keV-temperature ion equilibration, are used to highlight systems where including FAS is important to capture relevant physics.« less

A full-angle Monte-Carlo scattering technique including cumulative and single-event Rutherford scattering in plasmas [Theory of cumulative large-angle collisions in plasmas

DOE PAGES

Higginson, Drew P.

2017-08-12

Here, we describe and justify a full-angle scattering (FAS) method to faithfully reproduce the accumulated differential angular Rutherford scattering probability distribution function (pdf) of particles in a plasma. The FAS method splits the scattering events into two regions. At small angles it is described by cumulative scattering events resulting, via the central limit theorem, in a Gaussian-like pdf; at larger angles it is described by single-event scatters and retains a pdf that follows the form of the Rutherford differential cross-section. The FAS method is verified using discrete Monte-Carlo scattering simulations run at small timesteps to include each individual scattering event.more » We identify the FAS regime of interest as where the ratio of temporal/spatial scale-of-interest to slowing-down time/length is from 10 -3 to 0.3–0.7; the upper limit corresponds to Coulomb logarithm of 20–2, respectively. Two test problems, high-velocity interpenetrating plasma flows and keV-temperature ion equilibration, are used to highlight systems where including FAS is important to capture relevant physics.« less

The Small-Angle Neutron Scattering Data Analysis of the Phospholipid Transport Nanosystem Structure

NASA Astrophysics Data System (ADS)

Zemlyanaya, E. V.; Kiselev, M. A.; Zhabitskaya, E. I.; Aksenov, V. L.; Ipatova, O. M.; Ivankov, O. I.

2018-05-01

The small-angle neutron scattering technique (SANS) is employed for investigation of structure of the phospholipid transport nanosystem (PTNS) elaborated in the V.N.Orekhovich Institute of Biomedical Chemistry (Moscow, Russia). The SANS spectra have been measured at the YuMO small-angle spectrometer of IBR-2 reactor (Joint Institute of Nuclear Research, Dubna, Russia). Basic characteristics of polydispersed population of PTNS unilamellar vesicles (average radius of vesicles, polydispersity, thickness of membrane, etc.) have been determined in three cases of the PTNS concentrations in D2O: 5%, 10%, and 25%. Numerical analysis is based on the separated form factors method (SFF). The results are discussed in comparison with the results of analysis of the small-angle X-ray scattering spectra collected at the Kurchatov Synchrotron Radiation Source of the National Research Center “Kurchatov Institute” (Moscow, Russia).

More Fluorous Surface Modifier Makes it Less Oleophobic: Fluorinated-Siloxane Copolymer/PDMS Coatings

PubMed Central

Zhang, Wei; Zheng, Ying; Orsini, Lorenzo; Morelli, Andrea; Galli, Giancarlo; Chiellini, Emo; Carpenter, Everett E.; Wynne, Kenneth J.

2010-01-01

A copolyacrylate with semifluorinated and polydimethylsiloxane side chains (D5-3) was used as a surface modifier for a condensation cured PDMS coating. The decyl fluorous group is represented by “D”; “5” is a 5 kDa silicone, and “3” the mole ratio of fluorous to silicone side chain. Wetting behavior was assessed by dynamic contact angle (DCA) analysis using isopropanol, which differentiates silicone and fluorous wetting behavior. Interestingly, a maximum in surface oleophobicity was found at low D5-3 concentration (0.4 wt%). Higher concentrations result in decreased oleophobicity reflected in decreased contact angles. To understand this unexpected observation, dynamic light scattering (DLS) studies were initiated on a model system consisting of hydroxyl-terminated PDMS (18 kDa) containing varying amounts of D5-3. DLS revealed D5-3 aggregation as a function of temperature and concentration. A model is proposed by which D5-3 surface concentration is depleted via phase separation favoring D5-3 aggregation at concentrations >0.4 wt%, that is, the CMC. This model suggests increasing aggregate / micelle concentrations at increased D5-3 concentration. Bulk morphologies studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM) support this model by showing increased aggregate concentrations with increased D5-3 >0.4 wt%. PMID:20000339

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.

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

Numerical reproduction and explanation of road surface mirages under grazing-angle scattering.

PubMed

Lu, Jia; Zhou, Huaichun

2017-07-01

The mirror-like reflection image of the road surface under grazing-angle scattering can be easily observed in daily life. It was suggested that road surface mirages may occur due to a light-enhancing effect of the rough surface under grazing-angle scattering. The main purpose of this work is to explain the light-enhancing mechanism of rough surfaces under grazing-angle scattering. The off-specular reflection from a random rough magnesium oxide ceramic surface is analyzed by using the geometric optics approximation method. Then, the geometric optics approximation method is employed to develop a theoretical model to predict the observation effect of the grazing-angle scattering phenomenon of the road surface. The rough surface is assumed to consist of small-scale rough surface facets. The road surface mirage is reproduced from a large number of small-scale rough surface facets within the eye's resolution limit at grazing scattering angles, as the average bidirectional reflectance distribution function value at the bright location is about twice that of the surface in front of the mirage. It is suggested that the light-enhancing effect of the rough surface under grazing-angle scattering is not proper to be termed as "off-specular reflection," since it has nothing to do with the "specular" direction with respect to the incident direction.

Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering

NASA Astrophysics Data System (ADS)

Yan, Yong; Qian, Shuo; Garrison, Ben; Smith, Tyler; Kim, Peter

2018-04-01

A nondestructive neutron scattering method to precisely measure the hydrogen content in high-temperature steam-oxidized Zircaloy-4 cladding was developed. Zircaloy-4 cladding was used to produce hydrided specimens with hydrogen content up to ≈500 wppm. Following hydrogen charging, the hydrogen content of the hydrided specimens was measured using the vacuum hot extraction method, by which the samples with desired hydrogen concentrations were selected for the neutron study. The hydrided samples were then oxidized in steam up to ≈6.0 wt. % at 1100 °C. Optical microscopy shows that our hydriding procedure results in uniform distribution of circumferential hydrides across the wall thickness, and uniform oxide layers were formed on the sample surfaces by the steam oxidation. Small- and wide-angle neutron scattering were simultaneously performed to provide a quick (less than an hour per sample) measurement of the hydrogen content in various types of hydrided and oxidized Zircaloy-4. Our study demonstrates that the hydrogen in pre-oxidized Zircaloy-4 cladding can be measured very accurately by both small- and wide-angle neutron scattering. For steam-oxidized samples, the small-angle neutron scattering is contaminated with coherent scattering from additional structural features induced by the steam oxidation. However, the scattering intensity of the wide-angle neutron scattering increases proportionally with the hydrogen charged in the samples. The hydrogen content and wide-angle neutron scattering intensity are highly linearly correlated for the oxidized cladding samples examined in this work, and can be used to precisely determine the hydrogen content in steam-oxidized Zircaloy-4 samples. Hydrogen contents determined by neutron scattering of oxidation samples were also found to be consistent with the results of chemical analysis within acceptable margins for error.

Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering

DOE PAGES

Yan, Yong; Qian, Shuo; Garrison, Ben; ...

2018-04-15

In this study, a nondestructive neutron scattering method to precisely measure the hydrogen content in high-temperature steam-oxidized Zircaloy-4 cladding was developed. Zircaloy-4 cladding was used to produce hydrided specimens with hydrogen content up to ≈500 wppm. Following hydrogen charging, the hydrogen content of the hydrided specimens was measured using the vacuum hot extraction method, by which the samples with desired hydrogen concentrations were selected for the neutron study. The hydrided samples were then oxidized in steam up to ≈6.0wt. % at 1100°C. Optical microscopy shows that our hydriding procedure results in uniform distribution of circumferential hydrides across the wall thickness,more » and uniform oxide layers were formed on the sample surfaces by the steam oxidation. Small- and wide-angle neutron scattering were simultaneously performed to provide a quick (less than an hour per sample) measurement of the hydrogen content in various types of hydrided and oxidized Zircaloy-4. Our study demonstrates that the hydrogen in pre-oxidized Zircaloy-4 cladding can be measured very accurately by both small- and wide-angle neutron scattering. For steam-oxidized samples, the small-angle neutron scattering is contaminated with coherent scattering from additional structural features induced by the steam oxidation. However, the scattering intensity of the wide-angle neutron scattering increases proportionally with the hydrogen charged in the samples. The hydrogen content and wide-angle neutron scattering intensity are highly linearly correlated for the oxidized cladding samples examined in this work, and can be used to precisely determine the hydrogen content in steam-oxidized Zircaloy-4 samples. Hydrogen contents determined by neutron scattering of oxidation samples were also found to be consistent with the results of chemical analysis within acceptable margins for error.« less

Nondestructive hydrogen analysis of steam-oxidized Zircaloy-4 by wide-angle neutron scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, Yong; Qian, Shuo; Garrison, Ben

In this study, a nondestructive neutron scattering method to precisely measure the hydrogen content in high-temperature steam-oxidized Zircaloy-4 cladding was developed. Zircaloy-4 cladding was used to produce hydrided specimens with hydrogen content up to ≈500 wppm. Following hydrogen charging, the hydrogen content of the hydrided specimens was measured using the vacuum hot extraction method, by which the samples with desired hydrogen concentrations were selected for the neutron study. The hydrided samples were then oxidized in steam up to ≈6.0wt. % at 1100°C. Optical microscopy shows that our hydriding procedure results in uniform distribution of circumferential hydrides across the wall thickness,more » and uniform oxide layers were formed on the sample surfaces by the steam oxidation. Small- and wide-angle neutron scattering were simultaneously performed to provide a quick (less than an hour per sample) measurement of the hydrogen content in various types of hydrided and oxidized Zircaloy-4. Our study demonstrates that the hydrogen in pre-oxidized Zircaloy-4 cladding can be measured very accurately by both small- and wide-angle neutron scattering. For steam-oxidized samples, the small-angle neutron scattering is contaminated with coherent scattering from additional structural features induced by the steam oxidation. However, the scattering intensity of the wide-angle neutron scattering increases proportionally with the hydrogen charged in the samples. The hydrogen content and wide-angle neutron scattering intensity are highly linearly correlated for the oxidized cladding samples examined in this work, and can be used to precisely determine the hydrogen content in steam-oxidized Zircaloy-4 samples. Hydrogen contents determined by neutron scattering of oxidation samples were also found to be consistent with the results of chemical analysis within acceptable margins for error.« less

A full-angle Monte-Carlo scattering technique including cumulative and single-event Rutherford scattering in plasmas

NASA Astrophysics Data System (ADS)

Higginson, Drew P.

2017-11-01

We describe and justify a full-angle scattering (FAS) method to faithfully reproduce the accumulated differential angular Rutherford scattering probability distribution function (pdf) of particles in a plasma. The FAS method splits the scattering events into two regions. At small angles it is described by cumulative scattering events resulting, via the central limit theorem, in a Gaussian-like pdf; at larger angles it is described by single-event scatters and retains a pdf that follows the form of the Rutherford differential cross-section. The FAS method is verified using discrete Monte-Carlo scattering simulations run at small timesteps to include each individual scattering event. We identify the FAS regime of interest as where the ratio of temporal/spatial scale-of-interest to slowing-down time/length is from 10-3 to 0.3-0.7; the upper limit corresponds to Coulomb logarithm of 20-2, respectively. Two test problems, high-velocity interpenetrating plasma flows and keV-temperature ion equilibration, are used to highlight systems where including FAS is important to capture relevant physics.

Nanospheres with a smectic hydrophobic core and an amorphous PEG hydrophilic shell: structural changes and implications for drug delivery

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murthy, N. Sanjeeva; Zhang, Zheng; Borsadia, Siddharth

The structural changes in nanospheres with a crystalline core and an amorphous diffuse shell were investigated by small-angle neutron scattering (SANS), small-, medium-, and wide-angle X-ray scattering (SAXS, MAXS and WAXS), and differential scanning calorimetry (DSC).

Advanced analysis of polymer emulsions: Particle size and particle size distribution by field-flow fractionation and dynamic light scattering.

PubMed

Makan, Ashwell C; Spallek, Markus J; du Toit, Madeleine; Klein, Thorsten; Pasch, Harald

2016-04-15

Field flow fractionation (FFF) is an advanced fractionation technique for the analyses of very sensitive particles. In this study, different FFF techniques were used for the fractionation and analysis of polymer emulsions/latexes. As model systems, a pure acrylic emulsion and emulsions containing titanium dioxide were prepared and analyzed. An acrylic emulsion polymerization was conducted, continuously sampled from the reactor and subsequently analyzed to determine the particle size, radius of gyration in specific, of the latex particles throughout the polymerization reaction. Asymmetrical flow field-flow fractionation (AF4) and sedimentation field-flow fractionation (SdFFF), coupled to a multidetector system, multi-angle laser light scattering (MALLS), ultraviolet (UV) and refractive index (RI), respectively, were used to investigate the evolution of particle sizes and particle size distributions (PSDs) as the polymerization progressed. The obtained particle sizes were compared against batch-mode dynamic light scattering (DLS). Results indicated differences between AF4 and DLS results due to DLS taking hydration layers into account, whereas both AF4 and SdFFF were coupled to MALLS detection, hence not taking the hydration layer into account for size determination. SdFFF has additional separation capabilities with a much higher resolution compared to AF4. The calculated radii values were 5 nm larger for SdFFF measurements for each analyzed sample against the corresponding AF4 values. Additionally a low particle size shoulder was observed for SdFFF indicating bimodality in the reactor very early during the polymerization reaction. Furthermore, different emulsions were mixed with inorganic species used as additives in cosmetics and coatings such as TiO2. These complex mixtures of species were analyzed to investigate the retention and particle interaction behavior under different AF4 experimental conditions, such as the mobile phase. The AF4 system was coupled online to inductively coupled plasma mass spectrometry (ICP-MS) for elemental speciation and identification of the inorganic additive. SdFFF had a larger separation power to distinguish different particle size populations whereas AF4 had the capability of separating the organic particles and inorganic TiO2 particles, with high resolution. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Multifractal detrended fluctuation analysis of intensity time series of photons scattered by tracer particles within a polymeric gel

NASA Astrophysics Data System (ADS)

Telesca, Luciano; Haro-Pérez, Catalina; Moreno-Torres, L. Rebeca; Ramirez-Rojas, Alejandro

2018-01-01

Some properties of spatial confinement of tracer colloidal particles within polyacrylamide dispersions are studied by means of the well-known dynamic light scattering (DLS) technique. DLS allows obtaining sequences of elapsed times of scattered photons. In this work, the aqueous polyacrylamide dispersion has no crosslinking and the volume fraction occupied by the tracer particles is 0.02 %. Our experimental setup provides two sequences of photons scattered by the same scattering volume that corresponds to two simultaneous experiments (Channel A and Channel B). By integration of these sequences, the intensity time series are obtained. We find that both channels are antipersistent with Hurst exponent, H ∼0.43 and 0.36, respectively. The antipersistence of the intensity time series indicates a subdiffusive dynamics of the tracers in the polymeric network, which is in agreement with the time dependence of the tracer's mean square displacement.

Informing the improvement of forest products durability using small angle neutron scattering

Treesearch

Nayomi Plaza Rodriguez; Sai Venkatesh Pingali; Shuo Qian; William T. Heller; Joseph E. Jakes

2016-01-01

A better understanding of how wood nanostructure swells with moisture is needed to accelerate the development of forest products with enhanced moisture durability. Despite its suitability to study nanostructures, small angle neutron scattering (SANS) remains an underutilized tool in forest products research. Nanoscale moisture-induced structural changes in intact and...

Scattering from fractals

NASA Astrophysics Data System (ADS)

Hurd, Alan J.

The realization that structures in Nature often can be described by Mandelbrot's fractals has led to a revolution in many areas of physics. The interaction of waves with fractal systems has, understandably, become intensely studied since scattering is the method of choice to probe delicate fractal structures such as chainlike particle aggregates. Not all of these waves are electromagnetic. Neutron scattering, for example, is an important complementary tool to structural studies by X-ray and light scattering. Since the phenomenology of small-angle neutron scattering (SANS), as it is applied to fractal systems, is identical to that of small-angle X-ray scattering (SAXS), it falls within the scope of this paper.

Side-to-side differences in lower extremity biomechanics during multi-directional jump landing in volleyball athletes.

PubMed

Sinsurin, Komsak; Srisangboriboon, Sarun; Vachalathiti, Roongtiwa

2017-07-01

Side-to-side differences of lower extremities may influence the likelihood of injury. Moreover, adding the complexity of jump-landing direction would help to explain lower extremity control during sport activities. The aim was to determine the effects of limb dominance and jump-landing direction on lower extremity biomechanics. Nineteen female volleyball athletes participated. Both dominant limbs (DLs) and non-dominant limbs (NLs) were examined in single-leg jump-landing tests in four directions, including forward (0°), diagonal (30° and 60°), and lateral (90°) directions. Kinematic marker trajectories and ground reaction forces were collected using a 10 camera Vicon system and an AMTI force plate. Repeated measures ANOVA (2 × 4, limb × direction) was used to analyse. The finding showed that, at peak vertical GRF, a significant interaction of limb dominance and direction effects was found in the hip flexion angle and lower extremity joint kinetics (p < .05). NLs and DLs exhibited significantly different strategies while landing in various directions. Significantly higher increase of ankle dorsiflexion angle was observed in lateral direction compared to other directions for both DLs and NLs (p < .05). Increasingly using ankle dorsiflexion was observed from the forward to the lateral direction for both DLs and NLs. However, NLs and DLs preferentially used different strategies of joint moment organization to respond to similar VGRFs in various directions. The response pattern of DLs might not be effective and may expose DLs to a higher injury risk, especially with regard to landing with awkward posture compared with NLs.

NaCl-triggered self-assembly of hydrophilic poloxamine block copolymers.

PubMed

Bahadur, Anita; Cabana-Montenegro, Sonia; Aswal, Vinod Kumar; Lage, Emilio V; Sandez-Macho, Isabel; Concheiro, Angel; Alvarez-Lorenzo, Carmen; Bahadur, Pratap

2015-10-15

Tetronic 1307 (T1307) is a hydrophilic poloxamine (HLB>24) with a high molecular mass owing to its long PEO and PPO blocks. In spite of good biocompatibility, its use as a component of drug delivery systems is limited by its high critical micelle concentration (CMC) and temperature (CMT). The aim of this work was to elucidate whether the addition of NaCl or the combination of salts and temperature may bring T1307 micellization and gelling features into more practically useful values. Increasing NaCl concentration in the 0.154 M (isotonic) to 2M (hypertonic) range made the copolymer more hydrophobic and more prone to self-assemble into unimodal micelles, as observed by means of π-A isotherms, (1)H NMR, dynamic light scattering (DLS), small-angle neutron scattering (SANS), and pyrene fluorescence. The decrease in CMC and CMT observed for T1307 in 0.5 M NaCl medium (tolerable hypertonic solution), compared to water, notably favored the solubility of hydrophobic drugs such as curcumin and quercetin. Moreover, phase diagram, intrinsic viscosity and sol-to-gel transition were markedly affected by NaCl concentration. Overall, the strong dependence of T1307 self-assembly features on NaCl opens interesting possibilities for tuning the performance of T1307 as a component of nanocarriers and in situ gelling systems. Copyright © 2015 Elsevier B.V. All rights reserved.

Functional and structural characterization of a novel putative cysteine protease cell wall-modifying multi-domain enzyme selected from a microbial metagenome.

PubMed

Faheem, Muhammad; Martins-de-Sa, Diogo; Vidal, Julia F D; Álvares, Alice C M; Brandão-Neto, José; Bird, Louise E; Tully, Mark D; von Delft, Frank; Souto, Betulia M; Quirino, Betania F; Freitas, Sonia M; Barbosa, João Alexandre R G

2016-12-09

A current metagenomics focus is to interpret and transform collected genomic data into biological information. By combining structural, functional and genomic data we have assessed a novel bacterial protein selected from a carbohydrate-related activity screen in a microbial metagenomic library from Capra hircus (domestic goat) gut. This uncharacterized protein was predicted as a bacterial cell wall-modifying enzyme (CWME) and shown to contain four domains: an N-terminal, a cysteine protease, a peptidoglycan-binding and an SH3 bacterial domain. We successfully cloned, expressed and purified this putative cysteine protease (PCP), which presented autoproteolytic activity and inhibition by protease inhibitors. We observed cell wall hydrolytic activity and ampicillin binding capacity, a characteristic of most bacterial CWME. Fluorimetric binding analysis yielded a K b of 1.8 × 10 5  M -1 for ampicillin. Small-angle X-ray scattering (SAXS) showed a maximum particle dimension of 95 Å with a real-space R g of 28.35 Å. The elongated molecular envelope corroborates the dynamic light scattering (DLS) estimated size. Furthermore, homology modeling and SAXS allowed the construction of a model that explains the stability and secondary structural changes observed by circular dichroism (CD). In short, we report a novel cell wall-modifying autoproteolytic PCP with insight into its biochemical, biophysical and structural features.

A simple and rapid creatinine sensing via DLS selectivity, using calix[4]arene thiol functionalized gold nanoparticles.

PubMed

Sutariya, Pinkesh G; Pandya, Alok; Lodha, Anand; Menon, Shobhana K

2016-01-15

A new, simple, ultra-sensitive and selective approach has been reported for the "on spot" colorimetric detection of creatinine based on calix[4]arene functionalized gold nanoparticles (AuNPs) with excellent discrimination in the presence of other biomolecules. The lower detection limit of the method is 2.16nM. The gold nanoparticles and p-tert-butylcalix[4]arene were synthesized by microwave assisted method. Specifically, in our study, we used dynamic light scattering (DLS) which is a powerful method for the determination of small changes in particle size, improved selectivity and sensitivity of the creatinine detection system over colorimetric method. The nanoassembly is characterized by Transmission electron microscopy (TEM), DLS, UV-vis and ESI-MS spectroscopy, which demonstrates the binding affinity due its ability of hydrogen bonding and electrostatic interaction between -NH group of creatinine and pSDSC4. It exhibits fast response time (<60s) to creatinine and has long shelf-life (>5 weeks). The developed pSDSC4-AuNPs based creatinine biosensor will be established as simple, reliable and accurate tool for the determination of creatinine in human urine samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Quasi-Elastic Light Scattering in Ophthalmology

NASA Astrophysics Data System (ADS)

Ansari, Rafat R.

The eye is not just a "window to the soul"; it can also be a "window to the human body." The eye is built like a camera. Light which travels from the cornea to the retina traverses through tissues that are representative of nearly every tissue type and fluid type in the human body. Therefore, it is possible to diagnose ocular and systemic diseases through the eye. Quasi-elastic light scattering (QELS) also known as dynamic light scattering (DLS) is a laboratory technique routinely used in the characterization of macromolecular dispersions. QELS instrumentation has now become more compact, sensitive, flexible, and easy to use. These developments have made QELS/DLS an important tool in ophthalmic research where disease can be detected early and noninvasively before the clinical symptoms appear.

Changes of polarimetric scattering characteristics of ALOS PALSAR caused by the 2011 Eruption of Shinmoe-dake Volcano

NASA Astrophysics Data System (ADS)

Ohkura, Hiroshi

Full polarimetric SAR images of ALOS PALSAR of Shinmoe-dake volcano in Japan were analyzed. The volcano erupted in January, 2011 and volcano ash deposited more than 10 cm in 12 km (2) and 1 m in 2 km (2) . Two images before and after the eruption were compared based on a point view of the four-component scattering model to detect changes of polarimetric scattering characteristics. The main detected changes are as follows. Total power of the four-component scattering model decreased on a farslope after the eruption. An incident angle on a farslope is larger than the angle on a foreslope. Decrease of surface roughness due to deposited volcanic ashes makes back-scattering smaller in the area of a larger incidence angle. However the rate of the double-bounce component got higher in a forest at the foot of a mountain slope and on a plain, where the ground surface is almost horizontal and the incident angle is relatively-large. Decrease of roughness of the forest floor increases forward scattering on the floor of the larger incident angle. This increases the double-bounced scattering due to bouncing back between the forest floor and trunks which stand "perpendicularly" on the almost horizontal forest floor. The rate of the surface scattering component got higher around an area where layover occurred. In the study area, most of layovers occurred at a ridge where an incidence angle was small. Decrease of surface roughness due to the ash deposit increases the surface scattering power in the area of the small incidence angle.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 pitchmore » angle scattering of high-energy electrons into the geomagnetic loss cone.« less

Measurement of shear-induced diffusion of red blood cells using dynamic light scattering-optical coherence tomography

NASA Astrophysics Data System (ADS)

Tang, Jianbo; Erdener, Sefik Evren; Li, Baoqiang; Fu, Buyin; Sakadzic, Sava; Carp, Stefan A.; Lee, Jonghwan; Boas, David A.

2018-02-01

Dynamic Light Scattering-Optical Coherence Tomography (DLS-OCT) takes the advantages of using DLS to measure particle flow and diffusion within an OCT resolution-constrained 3D volume, enabling the simultaneous measurements of absolute RBC velocity and diffusion coefficient with high spatial resolution. In this work, we applied DLS-OCT to measure both RBC velocity and the shear-induced diffusion coefficient within penetrating venules of the somatosensory cortex of anesthetized mice. Blood flow laminar profile measurements indicate a blunted laminar flow profile, and the degree of blunting decreases with increasing vessel diameter. The measured shear-induced diffusion coefficient was proportional to the flow shear rate with a magnitude of 0.1 to 0.5 × 10-6 mm2 . These results provide important experimental support for the recent theoretical explanation for why DCS is dominantly sensitive to RBC diffusive motion.

CONTIN XPCS: Software for Inverse Transform Analysis of X-Ray Photon Correlation Spectroscopy Dynamics

PubMed Central

Narayanan, Suresh; Zhang, Fan; Kuzmenko, Ivan; Ilavsky, Jan

2018-01-01

X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) both reveal dynamics using coherent scattering, but X-rays permit investigating of dynamics in a much more diverse array of materials. Heterogeneous dynamics occur in many such materials, and we showed how classic tools employed in analysis of heterogeneous DLS dynamics extend to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. This work presents the software implementation of inverse transform analysis of XPCS data called CONTIN XPCS, an extension of traditional CONTIN that accommodates dynamics encountered in equilibrium XPCS measurements. PMID:29875507

CONTIN XPCS: Software for Inverse Transform Analysis of X-Ray Photon Correlation Spectroscopy Dynamics.

PubMed

Andrews, Ross N; Narayanan, Suresh; Zhang, Fan; Kuzmenko, Ivan; Ilavsky, Jan

2018-02-01

X-ray photon correlation spectroscopy (XPCS) and dynamic light scattering (DLS) both reveal dynamics using coherent scattering, but X-rays permit investigating of dynamics in a much more diverse array of materials. Heterogeneous dynamics occur in many such materials, and we showed how classic tools employed in analysis of heterogeneous DLS dynamics extend to XPCS, revealing additional information that conventional Kohlrausch exponential fitting obscures. This work presents the software implementation of inverse transform analysis of XPCS data called CONTIN XPCS, an extension of traditional CONTIN that accommodates dynamics encountered in equilibrium XPCS measurements.

A Hierarchical Algorithm for Fast Debye Summation with Applications to Small Angle Scattering

PubMed Central

Gumerov, Nail A.; Berlin, Konstantin; Fushman, David; Duraiswami, Ramani

2012-01-01

Debye summation, which involves the summation of sinc functions of distances between all pair of atoms in three dimensional space, arises in computations performed in crystallography, small/wide angle X-ray scattering (SAXS/WAXS) and small angle neutron scattering (SANS). Direct evaluation of Debye summation has quadratic complexity, which results in computational bottleneck when determining crystal properties, or running structure refinement protocols that involve SAXS or SANS, even for moderately sized molecules. We present a fast approximation algorithm that efficiently computes the summation to any prescribed accuracy ε in linear time. The algorithm is similar to the fast multipole method (FMM), and is based on a hierarchical spatial decomposition of the molecule coupled with local harmonic expansions and translation of these expansions. An even more efficient implementation is possible when the scattering profile is all that is required, as in small angle scattering reconstruction (SAS) of macromolecules. We examine the relationship of the proposed algorithm to existing approximate methods for profile computations, and show that these methods may result in inaccurate profile computations, unless an error bound derived in this paper is used. Our theoretical and computational results show orders of magnitude improvement in computation complexity over existing methods, while maintaining prescribed accuracy. PMID:22707386

Precision determination of electron scattering angle by differential nuclear recoil energy method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liyanage, N.; Saenboonruang, K.

2015-12-01

The accurate determination of the scattered electron angle is crucial to electron scattering experiments, both with open-geometry large-acceptance spectrometers and ones with dipole-type magnetic spectrometers for electron detection. In particular, for small central-angle experiments using dipole-type magnetic spectrometers, in which surveys are used to measure the spectrometer angle with respect to the primary electron beam, the importance of the scattering angle determination is emphasized. However, given the complexities of large experiments and spectrometers, the accuracy of such surveys is limited and insufficient to meet demands of some experiments. In this article, we present a new technique for determination of themore » electron scattering angle based on an accurate measurement of the primary beam energy and the principle of differential nuclear recoil. This technique was used to determine the scattering angle for several experiments carried out at the Experimental Hall A, Jefferson Lab. Results have shown that the new technique greatly improved the accuracy of the angle determination compared to surveys.« less

Precision Determination of Electron Scattering Angle by Differential Nuclear Recoil Energy Method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liyanage, Nilanga; Saenboonruang, Kiadtisak

2015-09-01

The accurate determination of the scattered electron angle is crucial to electron scattering experiments, both with open-geometry large-acceptance spectrometers and ones with dipole-type magnetic spectrometers for electron detection. In particular, for small central-angle experiments using dipole-type magnetic spectrometers, in which surveys are used to measure the spectrometer angle with respect to the primary electron beam, the importance of the scattering angle determination is emphasized. However, given the complexities of large experiments and spectrometers, the accuracy of such surveys is limited and insufficient to meet demands of some experiments. In this article, we present a new technique for determination of themore » electron scattering angle based on an accurate measurement of the primary beam energy and the principle of differential nuclear recoil. This technique was used to determine the scattering angle for several experiments carried out at the Experimental Hall A, Jefferson Lab. Results have shown that the new technique greatly improved the accuracy of the angle determination compared to surveys.« less

Thermalization after/during reheating

NASA Astrophysics Data System (ADS)

Harigaya, Keisuke; Mukaida, Kyohei

2014-05-01

If reheating of the Universe takes place via Planck-suppressed decay, it seems that the thermalization of produced particles might be delayed, since they have large energy/small number densities and number violating large angle scatterings which decrease the momentum of particles by large amount are inefficient correspondingly. In this paper, we study the thermalization of such "under occupied" decay products in detail, following recent developments in understanding the thermalization of non-abelian plasma. Contrary to the above naive expectation, it is shown that in most cases thermalization after/during reheating occurs instantaneously by properly taking account of scatterings with small angles and of particles with small momenta. In particular, the condition for instantaneous thermalization before the completion of reheating is found to be , which is much milder than that obtained in previous works with small angle scatterings taken into account.

Quantitative molecular characterization of bovine vitreous and lens with non-invasive dynamic light scattering

NASA Technical Reports Server (NTRS)

Ansari, R. R.; Suh, K. I.; Dunker, S.; Kitaya, N.; Sebag, J.

2001-01-01

The non-invasive technique of dynamic light scattering (DLS) was used to quantitatively characterize vitreous and lens structure on a molecular level by measuring the sizes of the predominant particles and mapping the three-dimensional topographic distribution of these structural macromolecules in three spatial dimensions. The results of DLS measurements in five fresh adult bovine eyes were compared to DLS measurements in model solutions of hyaluronan (HA) and collagen (Coll). In the bovine eyes DLS measurements were obtained from excised samples of gel and liquid vitreous and compared to the model solutions. Measurements in whole vitreous were obtained at multiple points posterior to the lens to generate a three-dimensional 'map' of molecular structure. The macromolecule distribution in bovine lens was similarly characterized.In each bovine vitreous (Bo Vit) specimen, DLS predominantly detected two distinct particles, which differed in diffusion properties and hence size. Comparisons with model vitreous solutions demonstrated that these most likely corresponded to the Coll and HA components of vitreous. Three-dimensional mapping of Bo Vit found heterogeneity throughout the vitreous body, with different particle size distributions for Coll and HA at different loci. In contrast, the three-dimensional distribution of lens macromolecules was more homogeneous. Thus, the non-invasive DLS technique can quantitate the average sizes of vitreous and lens macromolecules and map their three-dimensional distribution. This method to assess quantitatively the macromolecular structure of vitreous and lens should be useful for clinical as well as experimental applications in health and disease. Copyright 2001 Academic Press.

Synthesis and Small-Angle X-Ray Scattering Investigations of Ureido-Pyrimidone Hydrogen Bonding Star and Linear Poly(ethylene-co-propylene)s

DTIC Science & Technology

2006-02-01

Synthesis and Small-Angle X-ray Scattering Investigations of Ureido- Pyrimidone Hydrogen Bonding Star and Linear Poly(ethylene-co-propylene)s...Scattering Investigations of Ureido- Pyrimidone Hydrogen Bonding Star and Linear Poly(ethylene-co-propylene)s Frederick L. Beyer Weapons and...control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS. 1. REPORT DATE (DD-MM-YYYY) February 2006 2 . REPORT TYPE Interim 3. DATES

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

Structural and mechanical properties of cardiolipin lipid bilayers determined using neutron spin echo, small angle neutron and X-ray scattering, and molecular dynamics simulations

DOE PAGES

Pan, Jianjun; Cheng, Xiaolin; Sharp, Melissa; ...

2014-10-29

We report that the detailed structural and mechanical properties of a tetraoleoyl cardiolipin (TOCL) bilayer were determined using neutron spin echo (NSE) spectroscopy, small angle neutron and X-ray scattering (SANS and SAXS, respectively), and molecular dynamics (MD) simulations. We used MD simulations to develop a scattering density profile (SDP) model, which was then utilized to jointly refine SANS and SAXS data. In addition to commonly reported lipid bilayer structural parameters, component distributions were obtained, including the volume probability, electron density and neutron scattering length density.

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.

FINAL REPORT: DOE CONTRACT NUMBER FG0205ER64026 Biological Neutron Scattering: A Collaboration with the Oak Ridge Center for Structural Molecular Biology

DOE Office of Scientific and Technical Information (OSTI.GOV)

Trewhella, Jill

2011-01-12

The overarching goal of this project was to promote applications of small-angle scattering in structural molecular biology by providing model examples of cutting edge applications that demonstrate the unique capabilities and potential of the DOE national user facilities at Oak Ridge, especially the newly commissioned BioSANS. The approach taken was three-fold: (1) to engage in high impact collaborative research projects that would benefit from small-angle neutron scattering to both demonstrate the power of the technique while expanding the potential user community; (2) to provide access to scattering facilities established at the University of Utah to as broad a set ofmore » researchers as possible to increase the expertise in small-angle scattering generally; and (3) to develop new methods and tools for small-angle scattering. To these ends, three major research collaborations were pursued that resulted in a significant body of published work where neutron scattering and contrast variation played a major role. These major collaborations involved studies of protein complexes involved in (1) bacterial transcription regulation and adaptive response (a DOE/BER priority area); (2) regulation of cardiac muscle; and (3) neuronal disorders. In addition, to broaden the impact of the project, smaller collaborative efforts were supported that used either small-angle X-ray or neutron scattering. Finally, the DOE supported facilities at the University of Utah were made available to researchers on a service basis and a number of independent groups took advantage of this opportunity. In all of this work, there was an emphasis on the training of students and post docs in scattering techniques, and a set of publications (a book chapter, a review, and an encyclopedia article) were produced to guide the non-specialist potential user of scattering techniques in successful applications of the techniques. We also developed a suite of user friendly web-based computational tools currently being accessed world-wide by researchers as an aid in neutron scattering data interpretation. In all, these collaborative projects and resulted in 29 original refereed journal articles published between 2005 and 2010 and engaged groups from at least 14 Universities (10 US, 4 international) and 3 National Laboratories (2 US, 1 international). An important final initiative from this project was to begin a process for international community agreement on a set of standards for the publication of biomolecular small-angle scattering data. This initiative is being championed with the International Union of Crystallography and has engaged a number of Journal Editors and is a very important step in the maturing of this now burgeoning field.« less

Field-induced self-assembly of iron oxide nanoparticles investigated using small-angle neutron scattering.

PubMed

Fu, Zhendong; Xiao, Yinguo; Feoktystov, Artem; Pipich, Vitaliy; Appavou, Marie-Sousai; Su, Yixi; Feng, Erxi; Jin, Wentao; Brückel, Thomas

2016-11-03

The magnetic-field-induced assembly of magnetic nanoparticles (NPs) provides a unique and flexible strategy in the design and fabrication of functional nanostructures and devices. We have investigated the field-induced self-assembly of core-shell iron oxide NPs dispersed in toluene by means of small-angle neutron scattering (SANS). The form factor of the core-shell NPs was characterized and analyzed using SANS with polarized neutrons. Large-scale aggregates of iron oxide NPs formed above 0.02 T as indicated by very-small-angle neutron scattering measurements. A three-dimensional long-range ordered superlattice of iron oxide NPs was revealed under the application of a moderate magnetic field. The crystal structure of the superlattice has been identified to be face-centred cubic.

Multiple Acquisition InSAR Analysis: Persistent Scatterer and Small Baseline Approaches

NASA Astrophysics Data System (ADS)

Hooper, A.

2006-12-01

InSAR techniques that process data from multiple acquisitions enable us to form time series of deformation and also allow us to reduce error terms present in single interferograms. There are currently two broad categories of methods that deal with multiple images: persistent scatterer methods and small baseline methods. The persistent scatterer approach relies on identifying pixels whose scattering properties vary little with time and look angle. Pixels that are dominated by a singular scatterer best meet these criteria; therefore, images are processed at full resolution to both increase the chance of there being only one dominant scatterer present, and to reduce the contribution from other scatterers within each pixel. In images where most pixels contain multiple scatterers of similar strength, even at the highest possible resolution, the persistent scatterer approach is less optimal, as the scattering characteristics of these pixels vary substantially with look angle. In this case, an approach that interferes only pairs of images for which the difference in look angle is small makes better sense, and resolution can be sacrificed to reduce the effects of the look angle difference by band-pass filtering. This is the small baseline approach. Existing small baseline methods depend on forming a series of multilooked interferograms and unwrapping each one individually. This approach fails to take advantage of two of the benefits of processing multiple acquisitions, however, which are usually embodied in persistent scatterer methods: the ability to find and extract the phase for single-look pixels with good signal-to-noise ratio that are surrounded by noisy pixels, and the ability to unwrap more robustly in three dimensions, the third dimension being that of time. We have developed, therefore, a new small baseline method to select individual single-look pixels that behave coherently in time, so that isolated stable pixels may be found. After correction for various error terms, the phase values of the selected pixels are unwrapped using a new three-dimensional algorithm. We apply our small baseline method to an area in southern Iceland that includes Katla and Eyjafjallajökull volcanoes, and retrieve a time series of deformation that shows transient deformation due to intrusion of magma beneath Eyjafjallajökull. We also process the data using the Stanford method for persistent scatterers (StaMPS) for comparison.

Study of the gel films of Acetobacter Xylinum cellulose and its modified samples by {sup 1}H NMR cryoporometry and small-angle X-ray scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Babushkina, T. A.; Klimova, T. P.; Shtykova, E. V.

2010-03-15

Gel films of Acetobacter Xylinum cellulose and its modified samples have been investigated by 1H nuclear magnetic resonance (NMR) cryoporometry and small-angle X-ray scattering. The joint use of these two methods made it possible to characterize the sizes of aqueous pores in gel films and estimate the sizes of structural inhomogeneities before and after the sorption of polyvinylpyrrolidone and Se{sub 0} nanoparticles (stabilized by polyvinylpyrrolidone) into the films. According to small-angle X-ray scattering data, the sizes of inhomogeneities in a gel film change only slightly upon the sorption of polyvinylpyrrolidone and nanoparticles. The impregnated material is sorbed into water-filled cavitiesmore » that are present in the gel film. {sup 1}H NMR cryoporometry allowed us to reveal the details of changes in the sizes of small aqueous pores during modifications.« less

Structure and Interaction in the pH-Dependent Phase Behavior of Nanoparticle-Protein Systems.

PubMed

Yadav, Indresh; Kumar, Sugam; Aswal, Vinod K; Kohlbrecher, Joachim

2017-02-07

The pH-dependent structure and interaction of anionic silica nanoparticles (diameter 18 nm) with two globular model proteins, lysozyme and bovine serum albumin (BSA), have been studied. Cationic lysozyme adsorbs strongly on the nanoparticles, and the adsorption follows exponential growth as a function of lysozyme concentration, where the saturation value increases as pH approaches the isoelectric point (IEP) of lysozyme. By contrast, irrespective of pH, anionic BSA does not show any adsorption. Despite having a different nature of interactions, both proteins render a similar phase behavior where nanoparticle-protein systems transform from being one-phase (clear) to two-phase (turbid) above a critical protein concentration (CPC). The measurements have been carried out for a fixed concentration of silica nanoparticles (1 wt %) with varying protein concentrations (0-5 wt %). The CPC is found to be much higher for BSA than for lysozyme and increases for lysozyme but decreases for BSA as pH approaches their respective IEPs. The structure and interaction in these systems have been examined using dynamic light scattering (DLS) and small-angle neutron scattering (SANS). The effective hydrodynamic size of the nanoparticles measured using DLS increases with protein concentration and is related to the aggregation of the nanoparticles above the CPC. The propensity of the nanoparticles to aggregate is suppressed for lysozyme and enhanced for BSA as pH approached their respective IEPs. This behavior is understood from SANS data through the interaction potential determined by the interplay of electrostatic repulsion with a short-range attraction for lysozyme and long-range attraction for BSA. The nanoparticle aggregation is caused by charge neutralization by the oppositely charged lysozyme and through depletion for similarly charged BSA. Lysozyme-mediated attractive interaction decreases as pH approaches the IEP because of a decrease in the charge on the protein. In the case of BSA, a decrease in the BSA-BSA repulsion enhances the depletion attraction between the nanoparticles as pH is shifted toward the IEP. The morphology of the nanoparticle aggregates is found to be mass fractal.

Imaging electrical conductivity, permeability, and/or permittivity contrasts using the Born Scattering Inversion (BSI)

NASA Astrophysics Data System (ADS)

Darrh, A.; Downs, C. M.; Poppeliers, C.

2017-12-01

Born Scattering Inversion (BSI) of electromagnetic (EM) data is a geophysical imaging methodology for mapping weak conductivity, permeability, and/or permittivity contrasts in the subsurface. The high computational cost of full waveform inversion is reduced by adopting the First Born Approximation for scattered EM fields. This linearizes the inverse problem in terms of Born scattering amplitudes for a set of effective EM body sources within a 3D imaging volume. Estimation of scatterer amplitudes is subsequently achieved by solving the normal equations. Our present BSI numerical experiments entail Fourier transforming real-valued synthetic EM data to the frequency-domain, and minimizing the L2 residual between complex-valued observed and predicted data. We are testing the ability of BSI to resolve simple scattering models. For our initial experiments, synthetic data are acquired by three-component (3C) electric field receivers distributed on a plane above a single point electric dipole within a homogeneous and isotropic wholespace. To suppress artifacts, candidate Born scatterer locations are confined to a volume beneath the receiver array. Also, we explore two different numerical linear algebra algorithms for solving the normal equations: Damped Least Squares (DLS), and Non-Negative Least Squares (NNLS). Results from NNLS accurately recover the source location only for a large dense 3C receiver array, but fail when the array is decimated, or is restricted to horizontal component data. Using all receiver stations and all components per station, NNLS results are relatively insensitive to a sub-sampled frequency spectrum, suggesting that coarse frequency-domain sampling may be adequate for good target resolution. Results from DLS are insensitive to diminishing array density, but contain spatially oscillatory structure. DLS-generated images are consistently centered at the known point source location, despite an abundance of surrounding structure.

Protection against UV and X-ray cataracts using dynamic light scattering

NASA Technical Reports Server (NTRS)

Giblin, Frank J.

2005-01-01

Static and dynamic light scattering (SLS and DLS) analysis was used to investigate the aggregation of lens proteins in a hyperbaric oxygen (HBO)/guinea pig in vivo model for nuclear cataract. Nuclear cataract, an opacity which occurs in the center of the lens, is a major type of human maturity-onset cataract for which the cause is not well-understood. HBO is commonly used in major hospitals for treating complications such as poor wound healing due to impaired blood circulation. It is known that treatment of human patients with HBO for extended periods of time can produce nuclear cataract. Guinea pigs, initially 18 months old, were treated with HBO (2.5 atm of 100% O2 for 2.5 hr) 3x per week for 7 months to increase tie level of lens nuclear light scattering. Age-matched animals were used for controls. The eyes of the animals were analyzed in vivo using an integrated static and DLS fiber optic probe in collaboration with the NASA group. DLS in vivo was used to measure the size of lens proteins at 50 different locations across the optical axis of the guinea pig lens.

Small-angle neutron scattering investigations of Co-doped iron oxide nanoparticles. Preliminary results

NASA Astrophysics Data System (ADS)

Creanga, Dorina; Balasoiu, Maria; Soloviov, Dmitro; Balasoiu-Gaina, Alexandra-Maria; Puscasu, Emil; Lupu, Nicoleta; Stan, Cristina

2018-03-01

Preliminary small-angle neutron scattering investigations on aqueous suspensions of several cobalt doped ferrites (CoxFe3-xO4, x=0; 0.5; 1) nanoparticles prepared by chemical co-precipitation method, are reported. The measurements were accomplished at the YuMO instrument in function at the IBR-2 reactor. Results of intermediary data treatment are presented and discussed.

Small-angle neutron scattering study of a monoclonal antibody using free-energy constraints.

PubMed

Clark, Nicholas J; Zhang, Hailiang; Krueger, Susan; Lee, Hyo Jin; Ketchem, Randal R; Kerwin, Bruce; Kanapuram, Sekhar R; Treuheit, Michael J; McAuley, Arnold; Curtis, Joseph E

2013-11-14

Monoclonal antibodies (mAbs) contain hinge-like regions that enable structural flexibility of globular domains that have a direct effect on biological function. A subclass of mAbs, IgG2, have several interchain disulfide bonds in the hinge region that could potentially limit structural flexibility of the globular domains and affect the overall configuration space available to the mAb. We have characterized human IgG2 mAb in solution via small-angle neutron scattering (SANS) and interpreted the scattering data using atomistic models. Molecular Monte Carlo combined with molecular dynamics simulations of a model mAb indicate that a wide range of structural configurations are plausible, spanning radius of gyration values from ∼39 to ∼55 Å. Structural ensembles and representative single structure solutions were derived by comparison of theoretical SANS profiles of mAb models to experimental SANS data. Additionally, molecular mechanical and solvation free-energy calculations were carried out on the ensemble of best-fitting mAb structures. The results of this study indicate that low-resolution techniques like small-angle scattering combined with atomistic molecular simulations with free-energy analysis may be helpful to determine the types of intramolecular interactions that influence function and could lead to deleterious changes to mAb structure. This methodology will be useful to analyze small-angle scattering data of many macromolecular systems.

Geant4 simulations of soft proton scattering in X-ray optics. A tentative validation using laboratory measurements

NASA Astrophysics Data System (ADS)

Fioretti, Valentina; Mineo, Teresa; Bulgarelli, Andrea; Dondero, Paolo; Ivanchenko, Vladimir; Lei, Fan; Lotti, Simone; Macculi, Claudio; Mantero, Alfonso

2017-12-01

Low energy protons (< 300 keV) can enter the field of view of X-ray telescopes, scatter on their mirror surfaces at small incident angles, and deposit energy on the detector. This phenomenon can cause intense background flares at the focal plane decreasing the mission observing time (e.g. the XMM-Newton mission) or in the most extreme cases, damaging the X-ray detector. A correct modelization of the physics process responsible for the grazing angle scattering processes is mandatory to evaluate the impact of such events on the performance (e.g. observation time, sensitivity) of future X-ray telescopes as the ESA ATHENA mission. The Remizovich model describes particles reflected by solids at glancing angles in terms of the Boltzmann transport equation using the diffuse approximation and the model of continuous slowing down in energy. For the first time this solution, in the approximation of no energy losses, is implemented, verified, and qualitatively validated on top of the Geant4 release 10.2, with the possibility to add a constant energy loss to each interaction. This implementation is verified by comparing the simulated proton distribution to both the theoretical probability distribution and with independent ray-tracing simulations. Both the new scattering physics and the Coulomb scattering already built in the official Geant4 distribution are used to reproduce the latest experimental results on grazing angle proton scattering. At 250 keV multiple scattering delivers large proton angles and it is not consistent with the observation. Among the tested models, the single scattering seems to better reproduce the scattering efficiency at the three energies but energy loss obtained at small scattering angles is significantly lower than the experimental values. In general, the energy losses obtained in the experiment are higher than what obtained by the simulation. The experimental data are not completely representative of the soft proton scattering experienced by current X-ray telescopes because of the lack of measurements at low energies (< 200 keV) and small reflection angles, so we are not able to address any of the tested models as the one that can certainly reproduce the scattering behavior of low energy protons expected for the ATHENA mission. We can, however, discard multiple scattering as the model able to reproduce soft proton funnelling, and affirm that Coulomb single scattering can represent, until further measurements at lower energies are available, the best approximation of the proton scattered angular distribution at the exit of X-ray optics.

Primary particle diameter differentiation and bimodality identification by five analytical methods using gold nanoparticle size distributions synthesized by pulsed laser ablation in liquids

NASA Astrophysics Data System (ADS)

Letzel, Alexander; Gökce, Bilal; Menzel, Andreas; Plech, Anton; Barcikowski, Stephan

2018-03-01

For a known material, the size distribution of a nanoparticle colloid is a crucial parameter that defines its properties. However, measured size distributions are not easy to interpret as one has to consider weighting (e.g. by light absorption, scattering intensity, volume, surface, number) and the way size information was gained. The radius of a suspended nanoparticle can be given as e.g. sphere equivalent, hydrodynamic, Feret or radius of gyration. In this study, gold nanoparticles in water are synthesized by pulsed-laser ablation (LAL) and fragmentation (LFL) in liquids and characterized by various techniques (scanning transmission electron microscopy (STEM), small-angle X-ray scattering (SAXS), analytical disc centrifugation (ADC), dynamic light scattering (DLS) and UV-vis spectroscopy with Mie-Gans Theory) to study the comparability of different analytical techniques and determine the method that is preferable for a given task related to laser-generated nanoparticles. In particular, laser-generated colloids are known to be bimodal and/or polydisperse, but bimodality is sometimes not analytically resolved in literature. In addition, frequently reported small size shifts of the primary particle mode around 10 nm needs evaluation of its statistical significance related to the analytical method. Closely related to earlier studies on SAXS, different colloids in defined proportions are mixed and their size as a function of the nominal mixing ratio is analyzed. It is found that the derived particle size is independent of the nominal mixing ratio if the colloid size fractions do not overlap considerably. Conversely, the obtained size for colloids with overlapping size fractions strongly depends on the nominal mixing ratio since most methods cannot distinguish between such fractions. Overall, SAXS and ADC are very accurate methods for particle size analysis. Further, the ability of different methods to determine the nominal mixing ratio of sizes fractions is studied experimentally.

Characterization of nano-sized oxides in Fe-12Cr oxide-dispersion-strengthened ferritic steel using small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Han, Young-Soo; Mao, Xiaodong; Jang, Jinsung; Kim, Tae-Kyu

2015-04-01

The ferritic ODS steel was manufactured by hot isostatic pressing and heat treatment. The nano-sized microstructures such as yttrium oxides and Cr oxides were quantitatively analyzed by small-angle neutron scattering (SANS). The effects of the fabrication conditions on the nano-sized microstructure were investigated in relation to the quantitative analysis results obtained by SANS. The ratio between magnetic and nuclear scattering components was calculated, and the characteristics of the nano-sized yttrium oxides are discussed based on the SANS analysis results.

Small-angle scattering from 3D Sierpinski tetrahedron generated using chaos game

NASA Astrophysics Data System (ADS)

Slyamov, Azat

2017-12-01

We approximate a three dimensional version of deterministic Sierpinski gasket (SG), also known as Sierpinski tetrahedron (ST), by using the chaos game representation (CGR). Structural properties of the fractal, generated by both deterministic and CGR algorithms are determined using small-angle scattering (SAS) technique. We calculate the corresponding monodisperse structure factor of ST, using an optimized Debye formula. We show that scattering from CGR of ST recovers basic fractal properties, such as fractal dimension, iteration number, scaling factor, overall size of the system and the number of units composing the fractal.

Analysis of small-angle X-ray scattering data in the presence of significant instrumental smearing

PubMed Central

Bergenholtz, Johan; Ulama, Jeanette; Zackrisson Oskolkova, Malin

2016-01-01

A laboratory-scale small-angle X-ray scattering instrument with pinhole collimation has been used to assess smearing effects due to instrumental resolution. A new, numerically efficient method to smear ideal model intensities is developed and presented. It allows for directly using measured profiles of isotropic but otherwise arbitrary beams in smearing calculations. Samples of low-polydispersity polymer spheres have been used to show that scattering data can in this way be quantitatively modeled even when there is substantial distortion due to instrumental resolution. PMID:26937235

Small-angle neutron scattering study of the structure of mixed micellar solutions based on heptaethylene glycol monotetradecyl ether and cesium dodecyl sulfate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rajewska, A., E-mail: aldonar@jinr.ru; Medrzycka, K.; Hallmann, E.

2016-01-15

The micellization in mixed aqueous systems based on a nonionic surfactant, heptaethylene glycol monotetradecyl ether (C{sub 14}E{sub 7}), and an anionic surfactant, cesium dodecyl sulfate, has been investigated by small-angle neutron scattering. Preliminary data on the behavior of the C{sub 14}E{sub 7} aqueous solutions (with three concentrations, 0.17, 0.5, and 1%) mixed with a small amount of anionic surfactant, cesium dodecyl sulfate, are reported.

Complementary uses of small angle X-ray scattering and X-ray crystallography.

PubMed

Pillon, Monica C; Guarné, Alba

2017-11-01

Most proteins function within networks and, therefore, protein interactions are central to protein function. Although stable macromolecular machines have been extensively studied, dynamic protein interactions remain poorly understood. Small-angle X-ray scattering probes the size, shape and dynamics of proteins in solution at low resolution and can be used to study samples in a large range of molecular weights. Therefore, it has emerged as a powerful technique to study the structure and dynamics of biomolecular systems and bridge fragmented information obtained using high-resolution techniques. Here we review how small-angle X-ray scattering can be combined with other structural biology techniques to study protein dynamics. This article is part of a Special Issue entitled: Biophysics in Canada, edited by Lewis Kay, John Baenziger, Albert Berghuis and Peter Tieleman. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed Central

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

2015-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Inverse Transformation: Unleashing Spatially Heterogeneous Dynamics with an Alternative Approach to XPCS Data Analysis.

PubMed

Andrews, Ross N; Narayanan, Suresh; Zhang, Fan; Kuzmenko, Ivan; Ilavsky, Jan

2018-02-01

X-ray photon correlation spectroscopy (XPCS), an extension of dynamic light scattering (DLS) in the X-ray regime, detects temporal intensity fluctuations of coherent speckles and provides scattering vector-dependent sample dynamics at length scales smaller than DLS. The penetrating power of X-rays enables probing dynamics in a broad array of materials with XPCS, including polymers, glasses and metal alloys, where attempts to describe the dynamics with a simple exponential fit usually fails. In these cases, the prevailing XPCS data analysis approach employs stretched or compressed exponential decay functions (Kohlrausch functions), which implicitly assume homogeneous dynamics. In this paper, we propose an alternative analysis scheme based upon inverse Laplace or Gaussian transformation for elucidating heterogeneous distributions of dynamic time scales in XPCS, an approach analogous to the CONTIN algorithm widely accepted in the analysis of DLS from polydisperse and multimodal systems. Using XPCS data measured from colloidal gels, we demonstrate the inverse transform approach reveals hidden multimodal dynamics in materials, unleashing the full potential of XPCS.

Inverse Transformation: Unleashing Spatially Heterogeneous Dynamics with an Alternative Approach to XPCS Data Analysis

PubMed Central

Andrews, Ross N.; Narayanan, Suresh; Zhang, Fan; Kuzmenko, Ivan; Ilavsky, Jan

2018-01-01

X-ray photon correlation spectroscopy (XPCS), an extension of dynamic light scattering (DLS) in the X-ray regime, detects temporal intensity fluctuations of coherent speckles and provides scattering vector-dependent sample dynamics at length scales smaller than DLS. The penetrating power of X-rays enables probing dynamics in a broad array of materials with XPCS, including polymers, glasses and metal alloys, where attempts to describe the dynamics with a simple exponential fit usually fails. In these cases, the prevailing XPCS data analysis approach employs stretched or compressed exponential decay functions (Kohlrausch functions), which implicitly assume homogeneous dynamics. In this paper, we propose an alternative analysis scheme based upon inverse Laplace or Gaussian transformation for elucidating heterogeneous distributions of dynamic time scales in XPCS, an approach analogous to the CONTIN algorithm widely accepted in the analysis of DLS from polydisperse and multimodal systems. Using XPCS data measured from colloidal gels, we demonstrate the inverse transform approach reveals hidden multimodal dynamics in materials, unleashing the full potential of XPCS. PMID:29875506

A Fast Hyperspectral Vector Radiative Transfer Model in UV to IR spectral bands

NASA Astrophysics Data System (ADS)

Ding, J.; Yang, P.; Sun, B.; Kattawar, G. W.; Platnick, S. E.; Meyer, K.; Wang, C.

2016-12-01

We develop a fast hyperspectral vector radiative transfer model with a spectral range from UV to IR with 5 nm resolutions. This model can simulate top of the atmosphere (TOA) diffuse radiance and polarized reflectance by considering gas absorption, Rayleigh scattering, and aerosol and cloud scattering. The absorption component considers several major atmospheric absorbers such as water vapor, CO2, O3, and O2 including both line and continuum absorptions. A regression-based method is used to parameterize the layer effective optical thickness for each gas, which substantially increases the computation efficiency for absorption while maintaining high accuracy. This method is over 500 times faster than the existing line-by-line method. The scattering component uses the successive order of scattering (SOS) method. For Rayleigh scattering, convergence is fast due to the small optical thickness of atmospheric gases. For cloud and aerosol layers, a small-angle approximation method is used in SOS calculations. The scattering process is divided into two parts, a forward part and a diffuse part. The scattering in the small-angle range in the forward direction is approximated as forward scattering. A cloud or aerosol layer is divided into thin layers. As the ray propagates through each thin layer, a portion diverges as diffuse radiation, while the remainder continues propagating in forward direction. The computed diffuse radiance is the sum of all of the diffuse parts. The small-angle approximation makes the SOS calculation converge rapidly even in a thick cloud layer.

Small-Angle Neutron Scattering on Crosslink Distribution of Epoxy Networks.

DTIC Science & Technology

1985-10-01

distinct second phase or heterogeneity has been detected. Small- angle X-ray scattering (SAXS), 1 nuclear magnetic resonance (NMR) ,2 electron ... paramagnetic resonance (EPR),3 and glass transition 4temperature (Tg) measurements reveal a second phase which is attri- . buted to a heterogeneous...FUNDING/SPONSORING lab. OFFICE SYMBOL 9. PROCUREMENT INSTRUMENT IDENTIFICATION NUMBER * ORGANIZATION I (If applticable)j F3361 5-84-C-5020 * Bc ADDRESS

Contribution of double scattering to structural coloration in quasiordered nanostructures of bird feathers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Noh, Heeso; Liew, Seng Fatt; Saranathan, Vinodkumar

2010-07-28

We measured the polarization- and angle-resolved optical scattering and reflection spectra of the quasiordered nanostructures in the bird feather barbs. In addition to the primary peak that originates from single scattering, we observed a secondary peak which exhibits depolarization and distinct angular dispersion. We explained the secondary peak in terms of double scattering, i.e., light is scattered successively twice by the structure. The two sequential single-scattering events are considered uncorrelated. Using the Fourier power spectra of the nanostructures obtained from the small-angle x-ray scattering experiment, we calculated the double scattering of light in various directions. The double-scattering spectrum is broadermore » than the single-scattering spectrum, and it splits into two subpeaks at larger scattering angle. The good agreement between the simulation results and the experimental data confirms that double scattering of light makes a significant contribution to the structural color.« less

Celecoxib Encapsulation in β-Casein Micelles: Structure, Interactions, and Conformation.

PubMed

Turovsky, Tanya; Khalfin, Rafail; Kababya, Shifi; Schmidt, Asher; Barenholz, Yechezkel; Danino, Dganit

2015-07-07

β-Casein is a 24 kDa natural protein that has an open conformation and almost no folded or secondary structure, and thus is classified as an intrinsically unstructured protein. At neutral pH, β-casein has an amphiphilic character. Therefore, in contrast to most unstructured proteins that remain monomeric in solution, β-casein self-assembles into well-defined core-shell micelles. We recently developed these micelles as potential carriers for oral administration of poorly water-soluble pharmaceuticals, using celecoxib as a model drug. Herein we present deep and precise insight into the physicochemical characteristics of the protein-drug formulation, both in bulk solution and in dry form, emphasizing drug conformation, packing properties and aggregation state. In addition, the formulation is extensively studied in terms of structure and morphology, protein/drug interactions and physical stability. Particularly, NMR measurements indicated strong drug-protein interactions and noncrystalline drug conformation, which is expected to improve drug solubility and bioavailability. Small-angle X-ray scattering (SAXS) and cryogenic transmission electron microscopy (cryo-TEM) were combined for nanostructural characterization, proving that drug-protein interactions lead to well-defined spheroidal micelles that become puffier and denser upon drug loading. Dynamice light scattering (DLS), turbidity measurements, and visual observations complemented the analysis for determining formulation structure, interactions, and stability. Additionally, it was shown that the loaded micelles retain their properties through freeze-drying and rehydration, providing long-term physical and chemical stability. Altogether, the formulation seems greatly promising for oral drug delivery.

The influence of novel gemini surfactants containing cycloalkyl side-chains on the structural phases of DNA in solution.

PubMed

Pietralik, Zuzanna; Kumita, Janet R; Dobson, Christopher M; Kozak, Maciej

2015-07-01

Very important to gene therapy is the delivery system of the nucleic acids (called a vector), which will enhance the efficiency of the transport of new DNA into cells whilst protecting against damage. A promising alternative to the currently used viral vectors are the systems based on amphiphilic compounds - lipoplexes. Among them, gemini surfactants, which consist of two hydrophobic chains and two cationic heads connected by a linker - spacer group, appear to be promising candidates. The subject of this study involves two gemini surfactants, alkoxy derivatives of bis-imidazolium quaternary salts, differing in the length of their spacer groups and how they interact with two types of salmon sperm DNA (low and high molecular weight (MW)) or plasmid DNA (pDNA). The mixtures of gemini surfactants with nucleic acids of differing p/n ratios (positive-to-negative charge ratio) were characterised by small angle X-ray scattering (SAXS) of synchrotron radiation, dynamic light scattering (DLS), circular dichroism (CD) spectroscopy, atomic force microscopy (AFM), transmission electron microscopy (TEM) and gel electrophoresis techniques. This analysis allows for the selection of the most suitable and promising candidates for non-viral vectors in gene therapy, determination of the conditions needed to form stable complexes, identification of conformational changes in the DNA molecules upon interactions with gemini surfactants and in some cases, determination of the structures formed in these lipoplexes. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Implementation of a small-angle scattering model in MCNPX for very cold neutron reflector studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grammer, Kyle B.; Gallmeier, Franz X.

Current neutron moderator media do not sufficiently moderate neutrons below the cold neutron regime into the very cold neutron (VCN) regime that is desirable for some physics applications. Nesvizhevsky et al [1] have demonstrated that nanodiamond powder efficiently reflect VCN via small angle scattering. He suggests that these effects could be exploited to boost the neutron output of a VCN moderator. Simulation studies of nanoparticle reflectors are being investigated as part of the development of a VCN source option for the SNS second target station. We are pursuing an expansion of the MCNPX code by implementation of an analytical small-anglemore » scattering function [2], which is adaptable by scattering particle sizes, distributions, and packing fractions in order to supplement currently existing scattering kernels. The analytical model and preliminary studies using MCNPX will be discussed.« less

Effect of calcium/sodium ion exchange on the osmotic properties and structure of polyelectrolyte gels.

PubMed

Horkay, Ferenc; Basser, Peter J; Hecht, Anne-Marie; Geissler, Erik

2015-12-01

We discuss the main findings of a long-term research program exploring the consequences of sodium/calcium ion exchange on the macroscopic osmotic and elastic properties, and the microscopic structure of representative synthetic polyelectrolyte (sodium polyacrylate, (polyacrylic acid)) and biopolymer gels (DNA). A common feature of these gels is that above a threshold calcium ion concentration, they exhibit a reversible volume phase transition. At the macroscopic level, the concentration dependence of the osmotic pressure shows that calcium ions influence primarily the third-order interaction term in the Flory-Huggins model of polymer solutions. Mechanical tests reveal that the elastic modulus is practically unaffected by the presence of calcium ions, indicating that ion bridging does not create permanent cross-links. At the microscopic level, small-angle neutron scattering shows that polyacrylic acid and DNA gels exhibit qualitatively similar structural features in spite of important differences (e.g. chain flexibility and chemical composition) between the two polymers. The main effect of calcium ions is that the neutron scattering intensity increases due to the decrease in the osmotic modulus. At the level of the counterion cloud around dissolved macroions, anomalous small-angle X-ray scattering measurements made on DNA indicate that divalent ions form a cylindrical sheath enveloping the chain, but they are not localized. Small-angle neutron scattering and small-angle X-ray scattering provide complementary information on the structure and interactions in polymer solutions and gels. © IMechE 2015.

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.

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

Probing the Complex Architecture of Multimodular Carbohydrate-Active Enzymes Using a Combination of Small Angle X-Ray Scattering and X-Ray Crystallography.

PubMed

Czjzek, Mirjam; Ficko-Blean, Elizabeth

2017-01-01

The various modules in multimodular carbohydrate-active enzymes (CAZymes) may function in catalysis, carbohydrate binding, protein-protein interactions or as linkers. Here, we describe how combining the biophysical techniques of Small Angle X-ray Scattering (SAXS) and macromolecular X-ray crystallography (XRC) provides a powerful tool for examination into questions related to overall structural organization of ultra multimodular CAZymes.

Study of High Temperature Failure Mechanisms in Ceramics

DTIC Science & Technology

1988-06-01

The major experimental 4 techniques employed in the program are the use of small- angle neutron scattering to characterize cavity nucleation and growth...creep crackgrowth. Of particular interest are the development of a stochastic model of grainboundary sliding and a micromechanical model that relates...Accession For NTIS GF.A&I DTIC T,’ IDi st ribut Ion’ ;i Avillii~diii l l= (~~ I. RESEARCH OBJECTIVES I. Utilize small- angle neutron scattering to

Grazing-incidence small angle x-ray scattering studies of nanoscale polymer gratings

NASA Astrophysics Data System (ADS)

Doxastakis, Manolis; Suh, Hyo Seon; Chen, Xuanxuan; Rincon Delgadillo, Paulina A.; Wan, Lingshu; Williamson, Lance; Jiang, Zhang; Strzalka, Joseph; Wang, Jin; Chen, Wei; Ferrier, Nicola; Ramirez-Hernandez, Abelardo; de Pablo, Juan J.; Gronheid, Roel; Nealey, Paul

2015-03-01

Grazing-Incidence Small Angle X-ray Scattering (GISAXS) offers the ability to probe large sample areas, providing three-dimensional structural information at high detail in a thin film geometry. In this study we exploit the application of GISAXS to structures formed at one step of the LiNe (Liu-Nealey) flow using chemical patterns for directed self-assembly of block copolymer films. Experiments conducted at the Argonne National Laboratory provided scattering patterns probing film characteristics at both parallel and normal directions to the surface. We demonstrate the application of new computational methods to construct models based on scattering measured. Such analysis allows for extraction of structural characteristics at unprecedented detail.

Diffraction scattering computed tomography: a window into the structures of complex nanomaterials

PubMed Central

Birkbak, M. E.; Leemreize, H.; Frølich, S.; Stock, S. R.

2015-01-01

Modern functional nanomaterials and devices are increasingly composed of multiple phases arranged in three dimensions over several length scales. Therefore there is a pressing demand for improved methods for structural characterization of such complex materials. An excellent emerging technique that addresses this problem is diffraction/scattering computed tomography (DSCT). DSCT combines the merits of diffraction and/or small angle scattering with computed tomography to allow imaging the interior of materials based on the diffraction or small angle scattering signals. This allows, e.g., one to distinguish the distributions of polymorphs in complex mixtures. Here we review this technique and give examples of how it can shed light on modern nanoscale materials. PMID:26505175

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.

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

NASA Astrophysics Data System (ADS)

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

1993-04-01

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

Sagittal plane analysis of the spine and pelvis in degenerative lumbar scoliosis.

PubMed

Han, Fei; Weishi, Li; Zhuoran, Sun; Qingwei, Ma; Zhongqiang, Chen

2017-01-01

Previous studies have reported the normative values of pelvic sagittal parameters, but no study has analyzed the sagittal spino-pelvic alignment in degenerative lumbar scoliosis (DLS) and its role in the pathogenesis. Retrospective analysis was applied to 104 patients with DLS, together with 100 cases of asymptomatic young adults as a control group and another control group consisting of 145 cases with cervical spondylosis. The coronal and sagittal parameters were measured on the anteroposterior and lateral radiograph of the whole spine in the DLS group as well as in the two control groups. Statistical analysis showed that the DLS group had a higher pelvic incidence (PI) value (50.5° ± 10.2°), than the normal control group (with PI 47.2° ± 8.8°) and the cervical spondylosis group (46.9° ± 9.1°). In DLS group, there were 38 cases (36.5%) complicated with degenerative lumbar spondylolisthesis, who had higher PI values than patients without it. Besides, the lumbar lordosis (LL) and sacral slope (SS) of DLS group were lower; the scoliosis Cobb's angle was correlated with pelvic tilt (PT); thoracic kyphosis was correlated with LL, SS, and PT; and LL was correlated with other sagittal parameters. Patients with DLS may have a higher PI, which may impact the pathogenesis of DLS. A high PI value is probably associated with the high prevalence of degenerative lumbar spondylolisthesis among DLS patients. In DLS patients, the lumbar spine maintains the ability of regulating the sagittal balance, and the regulation depends more on thoracic curve.

Characterization of Inherent Particles and Mechanism of Thermal Stress Induced Particle Formation in HSV-2 Viral Vaccine Candidate.

PubMed

Li, Lillian; Kirkitadze, Marina; Bhandal, Kamaljit; Roque, Cristopher; Yang, Eric; Carpick, Bruce; Rahman, Nausheen

2017-11-10

Vaccine formulations may contain visible and/or subvisible particles, which can vary in both size and morphology. Extrinsic particles, which are particles not part of the product such as foreign contaminants, are generally considered undesirable and should be eliminated or controlled in injectable products. However, biological products, in particular vaccines, may also contain particles that are inherent to the product. Here we focus on the characterization of visible and subvisible particles in a live, replication-deficient viral vaccine candidate against HSV genital herpes in an early developmental stage. HSV-2 viral vaccine was characterized using a panel of analytical methods, including Fourier transform infrared spectroscopy (FTIR), sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE), Western blot, liquid chromatography-mass spectrometry (LC-MS), light microscopy, transmission electron microscopy (TEM), micro-flow imaging (MFI), dynamic light scattering (DLS), right angle light scattering (RALS), and intrinsic fluorescence. Particles in HSV-2 vaccine typically ranged from hundreds of nanometers to hundreds of micrometers in size and were determined to be inherent to the product. The infectious titer did not correlate with any trend in subvisible particle concentration and size distribution as shown by DLS, MFI, and TEM under stressed conditions. This suggested that particle changes in the submicron range were related to HSV-2 virion structure and had direct impact on biological activity. It was also observed that subvisible and visible particles could induce aggregation in the viral product. The temperature induced aggregation was observed by RALS, intrinsic fluorescence, and DLS. The increase of subvisible particle size with temperature could be fitted to a two-step thermokinetic model. Visible and subvisible particles were found to be inherent to the HSV-2 viral vaccine product. The mechanism of protein aggregation was discussed and a two-step thermokinetic aggregation profile was proposed. The approaches reported in this study may be applied to a variety of vaccines and other biological products, as a way to assess the consistency of the manufacturing process and identify key product quality attributes. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Long Periodic Structure of a Room-Temperature Ionic Liquid by High-Pressure Small-Angle X-Ray Scattering and Wide-Angle X-Ray Scattering: 1-Decyl-3-Methylimidazolium Chloride.

PubMed

Abe, Hiroshi; Hamaya, Nozomu; Koyama, Yoshihiro; Kishimura, Hiroaki; Takekiyo, Takahiro; Yoshimura, Yukihiro; Wakabayashi, Daisuke; Funamori, Nobumasa; Matsuishi, Kiyoto

2018-04-23

The Bragg reflections of 1-decyl-3-methylimidazolium chloride ([C 10 mim][Cl]), a room-temperature ionic liquid, are observed in a lowly scattered wavevector (q) region using high-pressure (HP) small-angle X-ray scattering methods. The HP crystal of [C 10 mim][Cl] was characterized by an extremely long periodic structure. The peak position at the lowest q (1.4 nm -1 ) was different from that of the prepeak observed in the liquid state (2.3 nm -1 ). Simultaneously, Bragg reflections at high-q were detected using HP wide-angle X-ray scattering. The longest lattice constant was estimated to be 4.3 nm using structural analysis. The crystal structure of HP differed from that of the low-temperature (LT) crystal and the LT liquid crystal. With increasing pressure, Bragg reflections in the high-q component became much broader, and were accompanied by phase transition, although those in the low-q component were observed to be relatively sharp. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

CONTINUOUS ROTATION SCATTERING CHAMBER

DOEpatents

Verba, J.W.; Hawrylak, R.A.

1963-08-01

An evacuated scattering chamber for use in observing nuclear reaction products produced therein over a wide range of scattering angles from an incoming horizontal beam that bombards a target in the chamber is described. A helically moving member that couples the chamber to a detector permits a rapid and broad change of observation angles without breaching the vacuum in the chamber. Also, small inlet and outlet openings are provided whose size remains substantially constant. (auth)

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 N 2 and CO 2 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

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 N 2 and CO 2 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

On the analysis of time-of-flight spin-echo modulated dark-field imaging data

NASA Astrophysics Data System (ADS)

Sales, Morten; Plomp, Jeroen; Bouwman, Wim G.; Tremsin, Anton S.; Habicht, Klaus; Strobl, Markus

2017-06-01

Spin-Echo Modulated Small Angle Neutron Scattering with spatial resolution, i.e. quantitative Spin-Echo Dark Field Imaging, is an emerging technique coupling neutron imaging with spatially resolved quantitative small angle scattering information. However, the currently achieved relatively large modulation periods of the order of millimeters are superimposed to the images of the samples. So far this required an independent reduction and analyses of the image and scattering information encoded in the measured data and is involving extensive curve fitting routines. Apart from requiring a priori decisions potentially limiting the information content that is extractable also a straightforward judgment of the data quality and information content is hindered. In contrast we propose a significantly simplified routine directly applied to the measured data, which does not only allow an immediate first assessment of data quality and delaying decisions on potentially information content limiting further reduction steps to a later and better informed state, but also, as results suggest, generally better analyses. In addition the method enables to drop the spatial resolution detector requirement for non-spatially resolved Spin-Echo Modulated Small Angle Neutron Scattering.

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

PubMed

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

2015-10-01

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).

Effect of degassing on the aggregation of carbon nanotubes dispersed in water

NASA Astrophysics Data System (ADS)

Chen, C.-J.; Huang, J.-R.; Hwang, I.-S.; Choi, H. J.; Lai, P.-Y.; Chan, C. K.

2017-10-01

Dynamic light scattering (DLS) along with centrifugation and shaking tests reveal that dissolved gases can significantly affect the aggregation behavior of carbon nanotubes (CNTs) dispersed in water. The CNTs in non-degassed samples form loose, stable networks having the DLS result reminiscent of semidilute polymer solutions, whereas the CNTs in degassed samples aggregate to form Brownian colloids that sediment quickly. Interestingly, the CNTs dispersed in acetone, with or without degassing, also behave like semidilute polymers in DLS experiments. We propose a surface nanobubble-assisted mechanism to explain the observed aggregation behaviors. Our work signifies that dissolved gases may play an important role in determining hydrophobicity and biomolecular functions in aqueous environments.

Inverse transformation: unleashing spatially heterogeneous dynamics with an alternative approach to XPCS data analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andrews, Ross N.; Narayanan, Suresh; Zhang, Fan

X-ray photon correlation spectroscopy (XPCS), an extension of dynamic light scattering (DLS) in the X-ray regime, detects temporal intensity fluctuations of coherent speckles and provides scattering-vector-dependent sample dynamics at length scales smaller than DLS. The penetrating power of X-rays enables XPCS to probe the dynamics in a broad array of materials, including polymers, glasses and metal alloys, where attempts to describe the dynamics with a simple exponential fit usually fail. In these cases, the prevailing XPCS data analysis approach employs stretched or compressed exponential decay functions (Kohlrausch functions), which implicitly assume homogeneous dynamics. This paper proposes an alternative analysis schememore » based upon inverse Laplace or Gaussian transformation for elucidating heterogeneous distributions of dynamic time scales in XPCS, an approach analogous to the CONTIN algorithm widely accepted in the analysis of DLS from polydisperse and multimodal systems. In conclusion, using XPCS data measured from colloidal gels, it is demonstrated that the inverse transform approach reveals hidden multimodal dynamics in materials, unleashing the full potential of XPCS.« less

Inverse transformation: unleashing spatially heterogeneous dynamics with an alternative approach to XPCS data analysis

DOE PAGES

Andrews, Ross N.; Narayanan, Suresh; Zhang, Fan; ...

2018-02-01

X-ray photon correlation spectroscopy (XPCS), an extension of dynamic light scattering (DLS) in the X-ray regime, detects temporal intensity fluctuations of coherent speckles and provides scattering-vector-dependent sample dynamics at length scales smaller than DLS. The penetrating power of X-rays enables XPCS to probe the dynamics in a broad array of materials, including polymers, glasses and metal alloys, where attempts to describe the dynamics with a simple exponential fit usually fail. In these cases, the prevailing XPCS data analysis approach employs stretched or compressed exponential decay functions (Kohlrausch functions), which implicitly assume homogeneous dynamics. This paper proposes an alternative analysis schememore » based upon inverse Laplace or Gaussian transformation for elucidating heterogeneous distributions of dynamic time scales in XPCS, an approach analogous to the CONTIN algorithm widely accepted in the analysis of DLS from polydisperse and multimodal systems. In conclusion, using XPCS data measured from colloidal gels, it is demonstrated that the inverse transform approach reveals hidden multimodal dynamics in materials, unleashing the full potential of XPCS.« less

Highly sensitive and selective dynamic light-scattering assay for TNT detection using p-ATP attached gold nanoparticle.

PubMed

Dasary, Samuel S R; Senapati, Dulal; Singh, Anant Kumar; Anjaneyulu, Yerramilli; Yu, Hongtao; Ray, Paresh Chandra

2010-12-01

TNT is one of the most commonly used nitro aromatic explosives for landmines of military and terrorist activities. As a result, there is an urgent need for rapid and reliable methods for the detection of trace amount of TNT for screenings in airport, analysis of forensic samples, and environmental analysis. Driven by the need to detect trace amounts of TNT from environmental samples, this article demonstrates a label-free, highly selective, and ultrasensitive para-aminothiophenol (p-ATP) modified gold nanoparticle based dynamic light scattering (DLS) probe for TNT recognition in 100 pico molar (pM) level from ethanol:acetonitile mixture solution. Because of the formation of strong π-donor-acceptor interaction between TNT and p-ATP, para-aminothiophenol attached gold nanoparticles undergo aggregation in the presence of TNT, which changes the DLS intensity tremendously. A detailed mechanism for significant DLS intensity change has been discussed. Our experimental results show that TNT can be detected quickly and accurately without any dye tagging in 100 pM level with excellent discrimination against other nitro compounds.

Structures and interactions among globular proteins above the isoelectric point in the presence of divalent ions: A small angle neutron scattering and dynamic light scattering study

NASA Astrophysics Data System (ADS)

Kundu, Sarathi; Pandit, Subhankar; Abbas, Sohrab; Aswal, V. K.; Kohlbrecher, J.

2018-02-01

Small angle neutron scattering study reveals that at pD ≈ 7.0, above the isoelectric point of the globular protein Bovine Serum Albumin (BSA), in the presence of different divalent ions (Mg2+, Ca2+, Sr2+ and Ba2+), the short-range attractive interaction remains nearly constant and the intermediate-range repulsive interaction decreases with increasing salt concentration up to a certain concentration value but after that remains unchanged. However, for the monovalent ion (Na+), repulsive interaction decreases gradually up to 1 M salt concentration. Dynamic light scattering study shows that for all ions, diffusion coefficient of BSA decreases with increasing salt concentration and then nearly saturates.

Characterization of Gd loaded chitosan-TPP nanohydrogels by a multi-technique approach combining dynamic light scattering (DLS), asymetrical flow-field-flow-fractionation (AF4) and atomic force microscopy (AFM) and design of positive contrast agents for molecular resonance imaging (MRI)

NASA Astrophysics Data System (ADS)

Rigaux, G.; Gheran, C. V.; Callewaert, M.; Cadiou, C.; Voicu, S. N.; Dinischiotu, A.; Andry, M. C.; Vander Elst, L.; Laurent, S.; Muller, R. N.; Berquand, A.; Molinari, M.; Huclier-Markai, S.; Chuburu, F.

2017-02-01

Chitosan CS—tripolyphosphate TPP/hyaluronic acid HA nanohydrogels loaded with gadolinium chelates (GdDOTA ⊂ CS-TPP/HA NGs) synthesized by ionic gelation were designed for lymph node (LN) MRI. In order to be efficiently drained to LNs, nanogels (NGs) needed to exhibit a diameter ϕ < 100 nm. For that, formulation parameters were tuned, using (i) CS of two different molecular weights (51 and 37 kDa) and (ii) variable CS/TPP ratio (2 < CS/TPP < 8). Characterization of NG size distribution by dynamic light scattering (DLS) and asymetrical flow-field-flow-fractionation (AF4) showed discrepancies since DLS diameters were consistently above 200 nm while AF4 showed individual nano-objects with ϕ < 100 nm. Such a difference could be correlated to the presence of aggregates inherent to ionic gelation. This point was clarified by atomic force microscopy (AFM) in liquid mode which highlighted the main presence of individual nano-objects in nanosuspensions. Thus, combination of DLS, AF4 and AFM provided a more precise characterization of GdDOTA ⊂ CS-TPP/HA nanohydrogels which, in turn, allowed to select formulations leading to NGs of suitable mean sizes showing good MRI efficiency and negligible toxicity.

Small-Angle X-ray Scattering (SAXS) Instrument Performance and Validation Using Silver Nanoparticles

DTIC Science & Technology

2016-12-01

Intercalibration of small-angle X- Ray and neutron-scattering data. Journal of Applied Crystallography . 1988;21:629–638. 7. Zhang F, Ilavsky J, Long GG...Materials Transactions A. 2009;41:1151–1158. 8. Kusz J, Bohm H. Performance of a confocal multilayer X-ray optic. Journal of Applied Crystallography ...Journal of Applied Crystallography . 2004;37:369–380. 10. Orthaber D, Bergmann A, Glatter O. SAXS experiments on absolute scale with Kratky systems using

Small Angle X ray Scattering (SAXS) Instrument Performance and Validation Using Silver Nanoparticles

DTIC Science & Technology

2016-12-01

Intercalibration of small-angle X- Ray and neutron-scattering data. Journal of Applied Crystallography . 1988;21:629–638. 7. Zhang F, Ilavsky J, Long GG...Materials Transactions A. 2009;41:1151–1158. 8. Kusz J, Bohm H. Performance of a confocal multilayer X-ray optic. Journal of Applied Crystallography ...Journal of Applied Crystallography . 2004;37:369–380. 10. Orthaber D, Bergmann A, Glatter O. SAXS experiments on absolute scale with Kratky systems using

Electron-cyclotron wave scattering by edge density fluctuations in ITER

NASA Astrophysics Data System (ADS)

Tsironis, Christos; Peeters, Arthur G.; Isliker, Heinz; Strintzi, Dafni; Chatziantonaki, Ioanna; Vlahos, Loukas

2009-11-01

The effect of edge turbulence on the electron-cyclotron wave propagation in ITER is investigated with emphasis on wave scattering, beam broadening, and its influence on localized heating and current drive. A wave used for electron-cyclotron current drive (ECCD) must cross the edge of the plasma, where density fluctuations can be large enough to bring on wave scattering. The scattering angle due to the density fluctuations is small, but the beam propagates over a distance of several meters up to the resonance layer and even small angle scattering leads to a deviation of several centimeters at the deposition location. Since the localization of ECCD is crucial for the control of neoclassical tearing modes, this issue is of great importance to the ITER design. The wave scattering process is described on the basis of a Fokker-Planck equation, where the diffusion coefficient is calculated analytically as well as computed numerically using a ray tracing code.

Interpretation of small-angle diffraction experiments on opal-like photonic crystals

NASA Astrophysics Data System (ADS)

Marlow, F.; Muldarisnur, M.; Sharifi, P.; Zabel, H.

2011-08-01

Comprehensive structural information on artificial opals involving the deviations from the strongly dominating face-centered cubic structure is still missing. Recent structure investigations with neutrons and synchrotron sources have shown a high degree of order but also a number of unexpected scattering features. Here, we point out that the exclusion of the allowed 002-type diffraction peaks by a small atomic form factor is not obvious and that surface scattering has to be included as a possible source for the diffraction peaks. Our neutron diffraction data indicate that surface scattering is the main reason for the smallest-angle peaks in the diffraction patterns.

Derivation of phase functions from multiply scattered sunlight transmitted through a hazy atmosphere

NASA Technical Reports Server (NTRS)

Weinman, J. A.; Twitty, J. T.; Browning, S. R.; Herman, B. M.

1975-01-01

The intensity of sunlight multiply scattered in model atmospheres is derived from the equation of radiative transfer by an analytical small-angle approximation. The approximate analytical solutions are compared to rigorous numerical solutions of the same problem. Results obtained from an aerosol-laden model atmosphere are presented. Agreement between the rigorous and the approximate solutions is found to be within a few per cent. The analytical solution to the problem which considers an aerosol-laden atmosphere is then inverted to yield a phase function which describes a single scattering event at small angles. The effect of noisy data on the derived phase function is discussed.

A modified Rayleigh-Gans-Debye formula for small angle X-ray scattering by interstellar dust grains

NASA Astrophysics Data System (ADS)

Sharma, Subodh K.

2015-05-01

A widely used approximation in studies relating to small angle differential scattering cross-section of X-rays scattered by interstellar dust grains is the well known Rayleigh-Gans-Debye approximation (RGDA). The validity of this approximation, however, is limited only to X-ray energies greater than about 1 keV. At lower energies, this approximation overestimates the exact results. In this paper a modification to the RGDA is suggested. It is shown that a combination of the RGDA with Ramsauer approximation retains the formal simplicity of the RGDA and also yields good agreement with Mie computations at all X-ray energies.

Mechanical Properties versus Morphology of Ordered Polymers. Volume III. Part I

DTIC Science & Technology

1982-08-01

measured by wide angle x-ray scattering and differential scanning calorimetry, is unrelated to the diffuse scattered intensity [62]. Cellulose acetate which...increasing void fraction, in air swollen cellulose . Comparison of the volume fraction of voids calculated from the SAXS integrated intensity with...1964). 63. P.H. Hermans, D. Heikens, and A. Weidinger, "A Quantitative Investigation on the X-Ray Small Angle Scattering of Cellulose Fibers. Part II

New noninvasive index for evaluation of the vascular age of healthy and sick people

NASA Astrophysics Data System (ADS)

Fine, Ilya; Kuznik, Boris I.; Kaminsky, Alexander V.; Shenkman, Louis; Kustovsjya, Evgeniya M.; Maximova, Olga G.

2012-08-01

We conducted a study on 861 healthy and sick subjects and demonstrated that some calculated parameters based on measurement of the dynamic light scattering (DLS) signal from the finger correlate highly with chronological age ranging from 1.5 to 85 years old. Measurements of DLS signals were obtained during both occlusion and nonocclusion of blood flow in the finger. For the nonocclusion case we found that the low-frequency component of the DLS signal significantly correlates with the biological age while the high-frequency component of the DLS signal resembles the arterial pulse-wave and does correlate with age. However, the most prominent correlation between the DLS characteristics and age was noted with the stasis stage measurements. We propose that the observed age-related phenomena are caused by alterations in local blood viscosity and interactions of the endothelial cells with erythrocytes. Further, a new noninvasive index based on the age-related optical characteristics was introduced. This noninvasive index may be used as a research and diagnostic tool to examine the endothelial and thrombolytic properties of the vascular system.

New noninvasive index for evaluation of the vascular age of healthy and sick people.

PubMed

Fine, Ilya; Kuznik, Boris I; Kaminsky, Alexander V; Shenkman, Louis; Kustovsjya, Evgeniya M; Elena, Evgeniya M; Maximova, Olga G

2012-08-01

We conducted a study on 861 healthy and sick subjects and demonstrated that some calculated parameters based on measurement of the dynamic light scattering (DLS) signal from the finger correlate highly with chronological age ranging from 1.5 to 85 years old. Measurements of DLS signals were obtained during both occlusion and nonocclusion of blood flow in the finger. For the nonocclusion case we found that the low-frequency component of the DLS signal significantly correlates with the biological age while the high-frequency component of the DLS signal resembles the arterial pulse-wave and does correlate with age. However, the most prominent correlation between the DLS characteristics and age was noted with the stasis stage measurements. We propose that the observed age-related phenomena are caused by alterations in local blood viscosity and interactions of the endothelial cells with erythrocytes. Further, a new noninvasive index based on the age-related optical characteristics was introduced. This noninvasive index may be used as a research and diagnostic tool to examine the endothelial and thrombolytic properties of the vascular system.

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.

Structure of Carbon Nanotube Porins in Lipid Bilayers: An in Situ Small-Angle X-ray Scattering (SAXS) Study [Atomic-level structure of carbon nanotube porins in lipid bilayers: an in-situ small-angle x-ray scattering (SAXS) study

DOE PAGES

Tran, Ich C.; Tunuguntla, Ramya H.; Kim, Kyunghoon; ...

2016-06-20

Carbon nanotube porins (CNTPs), small segments of carbon nanotubes capable of forming defined pores in lipid membranes, are important future components for bionanoelectronic devices as they could provide a robust analog of biological membrane channels. Furthermore, in order to control the incorporation of these CNT channels into lipid bilayers, it is important to understand the structure of the CNTPs before and after insertion into the lipid bilayer as well as the impact of such insertion on the bilayer structure. Here we employed a noninvasive in situ probe, small-angle X-ray scattering, to study the integration of CNT porins into dioleoylphosphatidylcholine bilayers.more » These results show that CNTPs in solution are stabilized by a monolayer of lipid molecules wrapped around their outer surface. We also demonstrate that insertion of CNTPs into the lipid bilayer results in decreased bilayer thickness with the magnitude of this effect increasing with the concentration of CNTPs.« less

X-ray and Neutron Scattering Study of the Formation of Core–Shell-Type Polyoxometalates

DOE PAGES

Yin, Panchao; Wu, Bin; Mamontov, Eugene; ...

2016-02-05

A typical type of core-shell polyoxometalates can be obtained through the Keggin-type polyoxometalate-templated growth of a layer of spherical shell structure of {Mo 72Fe 30}. Small angle X-ray scattering is used to study the structural features and stability of the core-shell structures in aqueous solutions. Time-resolved small angle X-ray scattering is applied to monitor the synthetic reactions and a three-stage formation mechanism is proposed to describe the synthesis of the core-shell polyoxometalates based on the monitoring results. Quasi-elastic and inelastic neutron scattering are used to probe the dynamics of water molecules in the core-shell structures and two different types ofmore » water molecules, the confined and structured water, are observed. These water molecules play an important role in bridging core and shell structures and stabilizing the cluster structures. A typical type of core shell polyoxometalates can be obtained through the Keggin-type polyoxometalate-templated growth of a layer of spherical shell structure of {Mo 72Fe 30}. Small-angle X-ray scattering is used to study the structural features and stability of the core shell structures in aqueous solutions. Time-resolved small-angle X-ray scattering is applied to monitor the synthetic reactions, and a three-stage formation mechanism is proposed to describe the synthesis of the core shell polyoxometalates based on the monitoring results. New protocols have been developed by fitting the X-ray data with custom physical models, which provide more convincing, objective, and completed data interpretation. Quasi-elastic and inelastic neutron scattering are used to probe the dynamics of water molecules in the core shell structures, and two different types of water molecules, the confined and structured water, are observed. These water molecules play an important role in bridging core and shell structures and stabilizing the cluster structures.« less

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. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

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. Copyright © 2013 Elsevier Inc. All rights reserved.

Total internal reflection and dynamic light scattering microscopy of gels

NASA Astrophysics Data System (ADS)

Gregor, Brian F.

Two different techniques which apply optical microscopy in novel ways to the study of biological systems and materials were built and applied to several samples. The first is a system for adapting the well-known technique of dynamic light scattering (DLS) to an optical microscope. This can detect and scatter light from very small volumes, as compared to standard DLS which studies light scattering from volumes 1000x larger. The small scattering volume also allows for the observation of nonergodic dynamics in appropriate samples. Porcine gastric mucin (PGM) forms a gel at low pH which lines the epithelial cell layer and acts as a protective barrier against the acidic stomach environment. The dynamics and microscopic viscosity of PGM at different pH levels is studied using polystyrene microspheres as tracer particles. The microscopic viscosity and microrheological properties of the commercial basement membrane Matrigel are also studied with this instrument. Matrigel is frequently used to culture cells and its properties remain poorly determined. Well-characterized and purely synthetic Matrigel substitutes will need to have the correct rheological and morphological characteristics. The second instrument designed and built is a microscope which uses an interferometry technique to achieve an improvement in resolution 2.5x better in one dimension than the Abbe diffraction limit. The technique is based upon the interference of the evanescent field generated on the surface of a prism by a laser in a total internal reflection geometry. The enhanced resolution is demonstrated with fluorescent samples. Additionally. Raman imaging microscopy is demonstrated using the evanescent field in resonant and non-resonant samples, although attempts at applying the enhanced resolution technique to the Raman images were ultimately unsuccessful. Applications of this instrument include high resolution imaging of cell membranes and macroscopic structures in gels and proteins. Finally, a third section incorporating previous research on simulations of complex fluids is included. Two dimensional simulations of oil, water, and surfactant mixtures were computed with a lattice gas method. The simulated systems were randomly mixed and then the temperature was quenched to a predetermined point. Spontaneous micellization is observed for a narrow range of temperature quenches, and the overall growth rate of macroscopic structure is found to follow a Vogel-Fulcher growth law.

Offshell quantum electrodynamics

NASA Astrophysics Data System (ADS)

Land, Martin; Horwitz, Lawrence P.

2013-04-01

In this paper, we develop the quantum field theory of off-shell electromagnetism, and use it to calculate the Møller scattering cross-section. This calculation leads to qualitative deviations from the usual scattering cross-sections, which are, however, small effects, but may be visible at small angles near the forward direction.

Effect of solvent and temperature on the size distribution of casein micelles measured by dynamic light scattering.

PubMed

Beliciu, C M; Moraru, C I

2009-05-01

The objectives of this study were to investigate the effect of the solvent on the accuracy of casein micelle particle size determination by dynamic light scattering (DLS) at different temperatures and to establish a clear protocol for these measurements. Dynamic light scattering analyses were performed at 6, 20, and 50 degrees C using a 90Plus Nanoparticle Size Analyzer (Brookhaven Instruments, Holtsville, NY). Raw and pasteurized skim milk were used as sources of casein micelles. Simulated milk ultrafiltrate, ultrafiltered water, and permeate obtained by ultrafiltration of skim milk using a 10-kDa cutoff membrane were used as solvents. The pH, ionic concentration, refractive index, and viscosity of all solvents were determined. The solvents were evaluated by DLS to ensure that they did not have a significant influence on the results of the particle size measurements. Experimental protocols were developed for accurate measurement of particle sizes in all solvents and experimental conditions. All measurements had good reproducibility, with coefficients of variation below 5%. Both the solvent and the temperature had a significant effect on the measured effective diameter of the casein micelles. When ultrafiltered permeate was used as a solvent, the particle size and polydispersity of casein micelles decreased as temperature increased. The effective diameter of casein micelles from raw skim milk diluted with ultrafiltered permeate was 176.4 +/- 5.3 nm at 6 degrees C, 177.4 +/- 1.9 nm at 20 degrees C, and 137.3 +/- 2.7 nm at 50 degrees C. This trend was justified by the increased strength of hydrophobic bonds with increasing temperature. Overall, the results of this study suggest that the most suitable solvent for the DLS analyses of casein micelles was casein-depleted ultrafiltered permeate. Dilution with water led to micelle dissociation, which significantly affected the DLS measurements, especially at 6 and 20 degrees C. Simulated milk ultrafiltrate seemed to give accurate results only at 20 degrees C. Results obtained in simulated milk ultrafiltrate at 6 degrees C could not be explained based on the known effects of temperature on the casein micelle, whereas at 50 degrees C, precipitation of amorphous calcium phosphate affected the DLS measurement.

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 CO 2 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 usingmore » 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.« less

Scattering from phase-separated vesicles. I. An analytical form factor for multiple static domains

DOE PAGES

Heberle, Frederick A.; Anghel, Vinicius N. P.; Katsaras, John

2015-08-18

This is the first in a series of studies considering elastic scattering from laterally heterogeneous lipid vesicles containing multiple domains. Unique among biophysical tools, small-angle neutron scattering can in principle give detailed information about the size, shape and spatial arrangement of domains. A general theory for scattering from laterally heterogeneous vesicles is presented, and the analytical form factor for static domains with arbitrary spatial configuration is derived, including a simplification for uniformly sized round domains. The validity of the model, including series truncation effects, is assessed by comparison with simulated data obtained from a Monte Carlo method. Several aspects ofmore » the analytical solution for scattering intensity are discussed in the context of small-angle neutron scattering data, including the effect of varying domain size and number, as well as solvent contrast. Finally, the analysis indicates that effects of domain formation are most pronounced when the vesicle's average scattering length density matches that of the surrounding solvent.« less

Performance of SMARTer at Very Low Scattering Vector q-Range Revealed by Monodisperse Nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Putra, E. Giri Rachman; Ikram, A.; Bharoto

2008-03-17

A monodisperse nanoparticle sample of polystyrene has been employed to determine performance of the 36 meter small-angle neutron scattering (SANS) BATAN spectrometer (SMARTer) at the Neutron Scattering Laboratory (NSL)--Serpong, Indonesia, in a very low scattering vector q-range. Detector position at 18 m from sample position, beam stopper of 50 mm in diameter, neutron wavelength of 5.66 A as well as 18 m-long collimator had been set up to achieve very low scattering vector q-range of SMARTer. A polydisperse smeared-spherical particle model was applied to fit the corrected small-angle scattering data of monodisperse polystyrene nanoparticle sample. The mean average of particlemore » radius of 610 A, volume fraction of 0.0026, and polydispersity of 0.1 were obtained from the fitting results. The experiment results from SMARTer are comparable to SANS-J, JAEA - Japan and it is revealed that SMARTer is powerfully able to achieve the lowest scattering vector down to 0.002 A{sup -1}.« less

Protein-Containing Lipid Bilayers Intercalated with Size-Matched Mesoporous Silica Thin Films

DOE PAGES

Isaksson, Simon; Watkins, Erik Benjamin; Browning, Kathryn L.; ...

2016-11-23

Here, proteins are key components in a multitude of biological processes, of which the functions carried out by transmembrane (membrane-spanning) proteins are especially demanding for investigations. This is because this class of protein needs to be incorporated into a lipid bilayer representing its native environment, and in addition, many experimental conditions also require a solid support for stabilization and analytical purposes. The solid support substrate may, however, limit the protein functionality due to protein–material interactions and a lack of physical space. We have in this work tailored the pore size and pore ordering of a mesoporous silica thin film tomore » match the native cell-membrane arrangement of the transmembrane protein human aquaporin 4 (hAQP4). Using neutron reflectivity (NR), we provide evidence of how substrate pores host the bulky water-soluble domain of hAQP4, which is shown to extend 7.2 nm into the pores of the substrate. Complementary surface analytical tools, including quartz crystal microbalance with dissipation monitoring (QCM-D) and fluorescence microscopy, revealed successful protein-containing supported lipid bilayer (pSLB) formation on mesoporous silica substrates, whereas pSLB formation was hampered on nonporous silica. Additionally, electron microscopy (TEM and SEM), light scattering (DLS and stopped-flow), and small-angle X-ray scattering (SAXS) were employed to provide a comprehensive characterization of this novel hybrid organic–inorganic interface, the tailoring of which is likely to be generally applicable to improve the function and stability of a broad range of membrane proteins containing water-soluble domains.« less

Relating structure and flow of soft colloids

NASA Astrophysics Data System (ADS)

Kundu, S. K.; Gupta, S.; Stellbrink, J.; Willner, L.; Richter, D.

2013-11-01

To relate the complex macroscopic flow of soft colloids to details of its microscopic equilibrium and non-equilibrium structure is still one big challenge in soft matter science. We investigated several well-defined colloidal model systems like star polymers or diblock copolymer micelles by linear/non-linear rheology, static/dynamic light scattering (SLS/DLS) and small angle neutron scattering (SANS). In addition, in-situ SANS experiments during shear (Rheo-SANS) revealed directly shear induced structural changes on a microscopic level. Varying the molecular architecture of the individual colloidal particle as well as particle-particle interactions and covering at the same time a broad concentration range from the very dilute to highly concentrated, glassy regime, we could separate contributions from intra- and inter-particle softness. Both can be precisely "tuned" by varying systematically the functionality, 6 ≤ f≤ 64, for star polymers or aggregation number, 30 ≤ N agg ≤ 1000 for diblock copolymer micelles, as well as the degree of polymerization of the individual polymer arm 100 ≤ D p ≤ 3000. In dilute solutions, the characteristic shear rate at which deformation of the soft colloid is observed can be related to the Zimm time of the polymeric corona. In concentrated solutions, we validated a generalized Stokes-Einstein approach to describe the increase in macroscopic viscosity and mesoscopic self diffusion coefficient on approaching the glassy regime. Both can be explained in terms of an ultra-soft interaction potential. Moreover, non-equilibrium structure factors are obtained by Rheo-SANS. All experimental results are in excellent quantitative agreement with recent theoretical predictions.

Protein-Containing Lipid Bilayers Intercalated with Size-Matched Mesoporous Silica Thin Films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Isaksson, Simon; Watkins, Erik Benjamin; Browning, Kathryn L.

Here, proteins are key components in a multitude of biological processes, of which the functions carried out by transmembrane (membrane-spanning) proteins are especially demanding for investigations. This is because this class of protein needs to be incorporated into a lipid bilayer representing its native environment, and in addition, many experimental conditions also require a solid support for stabilization and analytical purposes. The solid support substrate may, however, limit the protein functionality due to protein–material interactions and a lack of physical space. We have in this work tailored the pore size and pore ordering of a mesoporous silica thin film tomore » match the native cell-membrane arrangement of the transmembrane protein human aquaporin 4 (hAQP4). Using neutron reflectivity (NR), we provide evidence of how substrate pores host the bulky water-soluble domain of hAQP4, which is shown to extend 7.2 nm into the pores of the substrate. Complementary surface analytical tools, including quartz crystal microbalance with dissipation monitoring (QCM-D) and fluorescence microscopy, revealed successful protein-containing supported lipid bilayer (pSLB) formation on mesoporous silica substrates, whereas pSLB formation was hampered on nonporous silica. Additionally, electron microscopy (TEM and SEM), light scattering (DLS and stopped-flow), and small-angle X-ray scattering (SAXS) were employed to provide a comprehensive characterization of this novel hybrid organic–inorganic interface, the tailoring of which is likely to be generally applicable to improve the function and stability of a broad range of membrane proteins containing water-soluble domains.« less

Distance within colloidal dimers probed by rotation-induced oscillations of scattered light.

PubMed

van Vliembergen, Roland W L; van IJzendoorn, Leo J; Prins, Menno W J

2016-01-25

Aggregation processes of colloidal particles are of broad scientific and technological relevance. The earliest stage of aggregation, when dimers appear in an ensemble of single particles, is very important to characterize because it opens routes for further aggregation processes. Furthermore, it represents the most sensitive phase of diagnostic aggregation assays. Here, we characterize dimers by rotating them in a magnetic field and by recording the angle dependence of light scattering. At small scattering angles, the scattering cross section can be approximated by the total cross-sectional area of the dimer. In contrast, at scattering angles around 90 degrees, we reveal that the dependence of the scattering cross section on the dimer angle shows a series of peaks per single 2π rotation of the dimers. These characteristics originate from optical interactions between the two particles, as we have verified with two-particle Mie scattering simulations. We have studied in detail the angular positions of the peaks. It appears from simulations that the influence of particle size polydispersity, Brownian rotation and refractive index on the angular positions of the peaks is relatively small. However, the angular positions of the peaks strongly depend on the distance between the particles. We find a good correspondence between measured data and calculations for a gap of 180 nm between particles having a diameter of 1 micrometer. The experiment and simulations pave the way for extracting distance-specific data from ensembles of dimerizing colloidal particles, with application for sensitive diagnostic aggregation assays.

Recent results from the NN-interaction studies with polarized beams and targets at ANKE-COSY

NASA Astrophysics Data System (ADS)

Dymov, Sergey

2016-02-01

Adding to the nucleon-nucleon scattering database is one of the major priorities of the ANKE collaboration. Such data are necessary ingredients, not only for the understanding of nuclear forces, but also for the description of meson production and other nuclear reactions at intermediate energies. By measuring the cross section, deuteron analysing powers, and spin-correlation parameters in the dp → {pp}sn reaction, where {pp}s represents the 1S0 state, information has been obtained on small-angle neutron-proton spin-flip charge-exchange amplitudes. The measurements of pp elastic scattering by the COSY-EDDA have had a major impact on the partial wave analysis of this reaction above 1 GeV. However, these experiments only extended over the central region of c.m. angles, 300 < θcm < 1500, that has left major ambiguities in the phase shift analysis by the SAID group. In contrast, the small angle region is accessible at ANKE-COSY, that allowed measurement of the differential cross section and the analysing power at 50 < θcm < 300 in the 0.8 — 2.8 GeV energy range. The data on the pn elastic scattering are much more scarce than those of pp, especially in the region above 1.15 GeV. The study of the dp → {pp}s n reaction provides the information about the pn elastic scattering at large angles. The small angle scattering was studied with the polarized proton COSY beam and an unpolarised deuterium gas target. The detection the spectator proton in the ANKE vertex silicon detector allowed to use the deuterium target as an effective neutron one. The analysing powers of the process were obtained at six beam energies from 0.8 to 2.4 GeV.

Biological Small Angle Scattering: Techniques, Strategies and Tips

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chaudhuri, Barnali; Muñoz, Inés G.; Urban, Volker S.

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

Small Angle Neutron Scattering Observation of Chain Retraction after a Large Step Deformation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blanchard, A.; Heinrich, M.; Pyckhout-Hintzen, W.

The process of retraction in entangled linear chains after a fast nonlinear stretch was detected from time-resolved but quenched small angle neutron scattering (SANS) experiments on long, well-entangled polyisoprene chains. The statically obtained SANS data cover the relevant time regime for retraction, and they provide a direct, microscopic verification of this nonlinear process as predicted by the tube model. Clear, quantitative agreement is found with recent theories of contour length fluctuations and convective constraint release, using parameters obtained mainly from linear rheology. The theory captures the full range of scattering vectors once the crossover to fluctuations on length scales belowmore » the tube diameter is accounted for.« less

Correlating hydrodynamic radii with that of two-dimensional nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yue, Yuan; Kan, Yuwei; Clearfield, Abraham

2015-12-21

Dynamic light scattering (DLS) is one of the most adapted methods to measure the size of nanoparticles, as referred to the hydrodynamic radii (R{sub h}). However, the R{sub h} represents only that of three-dimensional spherical nanoparticles. In the present research, the size of two-dimensional (2D) nanoparticles of yttrium oxide (Y{sub 2}O{sub 3}) and zirconium phosphate (ZrP) was evaluated through comparing their hydrodynamic diameters via DLS with lateral sizes obtained using scanning and transmission electron microscopy. We demonstrate that the hydrodynamic radii are correlated with the lateral sizes of both square and circle shaped 2D nanoparticles. Two proportional coefficients, i.e., correctingmore » factors, are proposed for the Brownian motion status of 2D nanoparticles. The correction is possible by simplifying the calculation of integrals in the case of small thickness approximation. The correcting factor has great significance for investigating the translational diffusion behavior of 2D nanoparticles in a liquid and in effective and low-cost measurement in terms of size and morphology of shape-specific nanoparticles.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Vaerenbergh, Pierre; Léonardon, Joachim; Sztucki, Michael

2016-07-27

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

In-situ small-angle x-ray scattering study of nanoparticles in the plasma plume induced by pulsed laser irradiation of metallic targets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lavisse, L.; Jouvard, J.-M.; Girault, M.

2012-04-16

Small angle x-ray scattering was used to probe in-situ the formation of nanoparticles in the plasma plume generated by pulsed laser irradiation of a titanium metal surface under atmospheric conditions. The size and morphology of the nanoparticles were characterized as function of laser irradiance. Two families of nanoparticles were identified with sizes on the order of 10 and 70 nm, respectively. These results were confirmed by ex-situ transmission electron microscopy experiments.

Anomalous small-angle scattering as a way to solve the Babinet principle problem

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boiko, M. E., E-mail: m.e.boiko@mail.ioffe.ru; Sharkov, M. D.; Boiko, A. M.

2013-12-15

X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

Polymer Based Molecular Composites. Volume 171. Materials Research Society Symposium Proceedings Held in Boston, Massachusetts on 27-30 November 1989

DTIC Science & Technology

1990-09-01

231 Harry L. Frisch PART V: IONOMERS/STRUCTURE SMALL ANGLE X - RAY SCATTERING ON POLY(ETHYLENE-METHACRYLIC ACID) LEAD AND LEAD SULFIDE IONOMERS 237...E.J. Kramer, R.J. Composto, R.S. Stein, T.P. Russell, G.P. Felcher, A. Mansour, and A. Karim * td:tt Papet Vil X - RAY REFLECTIVITY AND FLUORESCENCE...Sammann DETERMINATION OF PARTICLE SIZE OF A DISPERSED PHASE BY SMALL-ANGLE X - RAY SCATTERING 413 Frank C. Wilson *Invited Paper ix SYNTHESIS AND

Anomalous small-angle scattering as a way to solve the Babinet principle problem

NASA Astrophysics Data System (ADS)

Boiko, M. E.; Sharkov, M. D.; Boiko, A. M.; Bobyl, A. V.

2013-12-01

X-ray absorption spectra (XAS) have been used to determine the absorption edges of atoms present in a sample under study. A series of small-angle X-ray scattering (SAXS) measurements using different monochromatic X-ray beams at different wavelengths near the absorption edges is performed to solve the Babinet principle problem. The sizes of clusters containing atoms determined by the method of XAS were defined in SAXS experiments. In contrast to differential X-ray porosimetry, anomalous SAXS makes it possible to determine sizes of clusters of different atomic compositions.

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

NASA Astrophysics Data System (ADS)

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

2016-02-01

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

Effects of the environmental factors on the casein micelle structure studied by cryo transmission electron microscopy and small-angle x-ray scattering/ultrasmall-angle x-ray scattering

NASA Astrophysics Data System (ADS)

Marchin, Stéphane; Putaux, Jean-Luc; Pignon, Frédéric; Léonil, Joëlle

2007-01-01

Casein micelles are colloidal protein-calcium-transport complexes whose structure has not been unequivocally elucidated. This study used small-angle x-ray scattering (SAXS) and ultrasmall angle x-ray scattering (USAXS) as well as cryo transmission electron microscopy (cryo-TEM) to provide fine structural details on their structure. Cryo-TEM observations of native casein micelles fractionated by differential centrifugation showed that colloidal calcium phosphate appeared as nanoclusters with a diameter of about 2.5nm. They were uniformly distributed in a homogeneous tangled web of caseins and were primarily responsible for the intensity distribution in the SAXS profiles at the highest q vectors corresponding to the internal structure of the casein micelles. A specific demineralization of casein micelles by decreasing the pH from 6.7 to 5.2 resulted in a reduced granular aspect of the micelles observed by cryo-TEM and the existence of a characteristic point of inflection in SAXS profiles. This supports the hypothesis that the smaller substructures detected by SAXS are colloidal calcium phosphate nanoclusters rather than putative submicelles.

Small-angle x-ray scattering measurement of a mist of ethanol nanodroplets: An approach to understanding ultrasonic separation of ethanol-water mixtures

NASA Astrophysics Data System (ADS)

Yano, Yohko F.; Matsuura, Kazuo; Fukazu, Tetsuo; Abe, Fusatsugu; Wakisaka, Akihiro; Kobara, Hitomi; Kaneko, Kazuyuki; Kumagai, Atsushi; Katsuya, Yoshio; Tanaka, Masahiko

2007-07-01

Small-angle x-ray scattering measurements using a brilliant x-ray source revealed nanometer sized liquid droplets in a mist formed by ultrasonic atomization. Ultrasonic atomization of ethanol-water mixtures produced a combination of water-rich droplets of micrometer order and ethanol-rich droplets as small as 1nm, which is 10-3 times smaller than the predicted size. These sizes were also obtained for mists generated from the pure liquids. These results will help to clarify the mechanism of "ultrasonic ethanol separation," which has the potential to become an alternative to distillation.

Submicron Protein Particle Characterization using Resistive Pulse Sensing and Conventional Light Scattering Based Approaches.

PubMed

Barnett, Gregory V; Perhacs, Julia M; Das, Tapan K; Kar, Sambit R

2018-02-08

Characterizing submicron protein particles (approximately 0.1-1μm) is challenging due to a limited number of suitable instruments capable of monitoring a relatively large continuum of particle size and concentration. In this work, we report for the first time the characterization of submicron protein particles using the high size resolution technique of resistive pulse sensing (RPS). Resistive pulse sensing, dynamic light scattering and size-exclusion chromatography with in-line multi-angle light scattering (SEC-MALS) are performed on protein and placebo formulations, polystyrene size standards, placebo formulations spiked with silicone oil, and protein formulations stressed via freeze-thaw cycling, thermal incubation, and acid treatment. A method is developed for monitoring submicron protein particles using RPS. The suitable particle concentration range for RPS is found to be approximately 4 × 10 7 -1 × 10 11 particles/mL using polystyrene size standards. Particle size distributions by RPS are consistent with hydrodynamic diameter distributions from batch DLS and to radius of gyration profiles from SEC-MALS. RPS particle size distributions provide an estimate of particle counts and better size resolution compared to light scattering. RPS is applicable for characterizing submicron particles in protein formulations with a high degree of size polydispersity. Data on submicron particle distributions provide insights into particles formation under different stresses encountered during biologics drug development.

Visualization of Individual Images in Patterned Organic-Inorganic Multilayers Using GISAXS-CT.

PubMed

Ogawa, Hiroki; Nishikawa, Yukihiro; Takenaka, Mikihito; Fujiwara, Akihiko; Nakanishi, Yohei; Tsujii, Yoshinobu; Takata, Masaki; Kanaya, Toshiji

2017-05-16

Using grazing-incidence small-angle scattering (GISAXS) with computed tomography (CT), we have individually reconstructed the spatial distribution of a thin gold (Au) layer buried under a thin poly(styrene-b-2-vinylpyridine) (PS-b-P2VP) layer. Owing to the difference between total reflection angles of Au and PS-b-P2VP, the scattering profiles for Au nanoparticles and self-assembled nanostructures of PS-b-P2VP could be independently obtained by changing the X-ray angle of incidence. Reconstruction of scattering profiles allows one to separately characterize spatial distributions in Au and PS-b-P2VP nanostructures.

Integrated instrument for dynamic light scattering and natural fluorescence measurements

NASA Astrophysics Data System (ADS)

Rovati, Luigi; Pollonini, Luca; Ansari, Rafat R.

2001-06-01

Over the past two decades, great efforts have been made in ophthalmology to use optical techniques based on dynamic light scattering and tissue natural fluorescence for early (at molecular level) diagnosis of ocular pathologies. In our previous studies, the relationship between the corneal AF and DLS decay widths of ocular tissues were established by performing measurements on diabetes mellitus patients. In those studies, corneal AF mean intensities were significantly correlated with DLS decay width measurements for each diabetic retinopathy grade in the vitreous and in the cornea. This suggested that the quality of the diagnosis could be significantly improved by properly combining these two powerful techniques into a single instrument. Our approach is based on modifying a commercial scanning ocular fluorometer (Fluorotron Master, Ocumetrics Inc., CA, USA) to include both techniques in the same scanning unit. This configuration provides both DLS and AF real time measurements from the same ocular volume: they can be located in each section of the optical axis of the eye from the cornea to the retina. In this paper, the optical setup of the new system is described and preliminary in-vitro and in-vivo measurements are presented.

Dynamic light scattering as an efficient tool to study glyconanoparticle-lectin interactions.

PubMed

Wang, Xin; Ramström, Olof; Yan, Mingdi

2011-10-21

Glyconanomaterials, an emerging class of bio-functional nanomaterials, have shown promise in detecting, imaging and targeting proteins, bacteria, and cells. In this article, we report that dynamic light scattering (DLS) can be used as an efficient tool to study glyconanoparticle (GNP)--lectin interactions. Silica and Au nanoparticles (NPs) conjugated with D-mannose (Man) and D-galactose (Gal) were treated with the lectins Concanavalin A (Con A) and Ricinus communis agglutinin (RCA(120)), and the hydrodynamic volumes of the resulting aggregates were measured by DLS. The results showed that the particle size grew with increasing lectin concentration. The limit of detection (LOD) was determined to be 2.9 nM for Con A with Man-conjugated and 6.6 nM for RCA(120) with Gal-conjugated silica NPs (35 nm), respectively. The binding affinity was also determined by DLS and the results showed 3-4 orders of magnitude higher affinity of GNPs than the free ligands with lectins. The assay sensitivity and affinity were particle size dependent and decreased with increasing particle diameter. Because the method relies on the particle size growth, it is therefore general and can be applied to nanomaterials of different compositions.

Structured water in polyelectrolyte dendrimers: Understanding small angle neutron scattering results through atomistic simulation

NASA Astrophysics Data System (ADS)

Wu, Bin; Kerkeni, Boutheïna; Egami, Takeshi; Do, Changwoo; Liu, Yun; Wang, Yongmei; Porcar, Lionel; Hong, Kunlun; Smith, Sean C.; Liu, Emily L.; Smith, Gregory S.; Chen, Wei-Ren

2012-04-01

Based on atomistic molecular dynamics (MD) simulations, the small angle neutron scattering (SANS) intensity behavior of a single generation-4 polyelectrolyte polyamidoamine starburst dendrimer is investigated at different levels of molecular protonation. The SANS form factor, P(Q), and Debye autocorrelation function, γ(r), are calculated from the equilibrium MD trajectory based on a mathematical approach proposed in this work. The consistency found in comparison against previously published experimental findings (W.-R. Chen, L. Porcar, Y. Liu, P. D. Butler, and L. J. Magid, Macromolecules 40, 5887 (2007)) leads to a link between the neutron scattering experiment and MD computation, and fresh perspectives. The simulations enable scattering calculations of not only the hydrocarbons but also the contribution from the scattering length density fluctuations caused by structured, confined water within the dendrimer. Based on our computational results, we explore the validity of using radius of gyration RG for microstructure characterization of a polyelectrolyte dendrimer from the scattering perspective.

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

NASA Astrophysics Data System (ADS)

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

2013-06-01

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

Minimally invasive decompression surgery for lumbar spinal stenosis with degenerative scoliosis: Predictive factors of radiographic and clinical outcomes.

PubMed

Minamide, Akihito; Yoshida, Munehito; Iwahashi, Hiroki; Simpson, Andrew K; Yamada, Hiroshi; Hashizume, Hiroshi; Nakagawa, Yukihiro; Iwasaki, Hiroshi; Tsutsui, Shunji; Kagotani, Ryohei; Sonekatsu, Mayumi; Sasaki, Takahide; Shinto, Kazunori; Deguchi, Tsuyoshi

2017-05-01

There is ongoing controversy regarding the most appropriate surgical treatment for lumbar spinal stenosis (LSS) with concurrent degenerative lumbar scoliosis (DLS): decompression alone, decompression with limited spinal fusion, or long spinal fusion for deformity correction. The coexistence of degenerative stenosis and deformity is a common scenario; Nonetheless, selecting the appropriate surgical intervention requires thorough understanding of the patients clinical symptomatology as well as radiographic parameters. Minimally invasive (MIS) decompression surgery was performed for LSS patients with DLS. The aims of this study were (1) to investigate the clinical outcomes of MIS decompression surgery in LSS patients with DLS, and (2) to identify the predictive factors for both radiographic and clinical outcomes after MIS surgery. 438 consecutive patients were enrolled in this study. Inclusion criteria was evidence of LSS and DLS with coronal curvature measuring greater than 10°. The Japanese Orthopaedic Association (JOA) score, JOA recovery rate, low back pain (LBP), and radiographic features were evaluated preoperatively and at over 2 years postoperatively. Of the 438 patients, 122 were included in final analysis, with a mean follow-up of 2.4 years. The JOA recovery rate was 47.6%. LBP was significantly improved at final follow-up. Cobb angle was maintained for 2 years postoperatively (p = 0.159). Clinical outcomes in foraminal stenosis patients were significantly related to sex, preoperative high Cobb angle and progression of scoliosis (p = 0.008). In the severe scoliosis patients, the JOA recovery was 44%, and was significantly depended on progression of scoliosis (Cobb angle: preoperation 29.6°, 2-years follow-up 36.9°) and mismatch between the pelvic incidence (PI) and the lumbar lordosis (LL) (preoperative PI-LL 35.5 ± 21.2°) (p = 0.028). This study investigated clinical outcomes of MIS decompression surgery in LSS patients with DLS. The predictive risk factors of clinical outcomes were severe scoliosis, foramina stenosis, progressive scoliosis and large mismatch of PI-LL. Copyright © 2016 The Japanese Orthopaedic Association. All rights reserved.

The effects of burial diagenesis on multiscale porosity in the St. Peter Sandstone: An imaging, small-angle, and ultra-small-angle neutron scattering analysis

DOE PAGES

Anovitz, Lawrence M.; Freiburg, Jared T.; Wasbrough, Matthew; ...

2017-11-06

To examine the effects of burial diagenesis on heirarchical pore structures in sandstone and compare those with the effects of overgrowth formation, we obtained samples of St. Peter Sandstone from drill cores obtained in the Illinois and Michigan Basins. The multiscale pore structure of rocks in sedimentary reservoirs and the mineralogy associated with those pores are critical factors for estimating reservoir properties, including fluid mass in place, permeability, and capillary pressures, as well as geochemical interactions between the rock and the fluid. The combination of small- and ultra-small-angle neutron scattering with backscattered electron or X ray-computed tomographic imaging, or both,more » provided a means by which pore structures were quantified at scales ranging from aproximately 1 nm to 1 cm—seven orders of magnitude. Larger scale (>10 µm) porosity showed the expected logarithmic decrease in porosity with depth, although there was significant variation in each sample group. However, small- and ultra-small-angle neutron scattering data showed that the proportion of small-scale porosity increased with depth. Porosity distributions were not continuous, but consisted of a series of log normal-like distributions at several distinct scales within these rocks. Fractal dimensions at larger scales decreased (surfaces smoothed) with increasing depth, and those at smaller scales increased (surfaces roughened) and pores become more isolated (higher lacunarity). Furthermore, data suggest that changes in pore-size distributions are controlled by both physical (compaction) and chemical effects (precipitation, cementation, dissolution).« less

The effects of burial diagenesis on multiscale porosity in the St. Peter Sandstone: An imaging, small-angle, and ultra-small-angle neutron scattering analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anovitz, Lawrence M.; Freiburg, Jared T.; Wasbrough, Matthew

To examine the effects of burial diagenesis on heirarchical pore structures in sandstone and compare those with the effects of overgrowth formation, we obtained samples of St. Peter Sandstone from drill cores obtained in the Illinois and Michigan Basins. The multiscale pore structure of rocks in sedimentary reservoirs and the mineralogy associated with those pores are critical factors for estimating reservoir properties, including fluid mass in place, permeability, and capillary pressures, as well as geochemical interactions between the rock and the fluid. The combination of small- and ultra-small-angle neutron scattering with backscattered electron or X ray-computed tomographic imaging, or both,more » provided a means by which pore structures were quantified at scales ranging from aproximately 1 nm to 1 cm—seven orders of magnitude. Larger scale (>10 µm) porosity showed the expected logarithmic decrease in porosity with depth, although there was significant variation in each sample group. However, small- and ultra-small-angle neutron scattering data showed that the proportion of small-scale porosity increased with depth. Porosity distributions were not continuous, but consisted of a series of log normal-like distributions at several distinct scales within these rocks. Fractal dimensions at larger scales decreased (surfaces smoothed) with increasing depth, and those at smaller scales increased (surfaces roughened) and pores become more isolated (higher lacunarity). Furthermore, data suggest that changes in pore-size distributions are controlled by both physical (compaction) and chemical effects (precipitation, cementation, dissolution).« less

Extinction, emission, and scattering spectroscopy of 5-50 nm citrate-coated gold nanoparticles: An argument for curvature effects on aggregation

NASA Astrophysics Data System (ADS)

Esfahani, Milad Rabbani; Pallem, Vasanta L.; Stretz, Holly A.; Wells, Martha J. M.

2017-03-01

The interaction of macromolecules with gold nanoparticles (GNPs) is of interest in the emerging field of biomedical and environmental detection devices. However, the physicochemical properties, including spectra, of GNPs in aqueous solution in the absence of metal-macromolecular interactions must first be considered before their activity in biological and environmental systems can be understood. The specific objective of this research was to experimentally illuminate the role of nanoparticle core size on the spectral (simultaneous consideration of extinction, emission, and scattering) versus aggregation behaviors of citrate-coated GNPs (CT-GNPs). It is difficult to find in the literature systematic simultaneous presentation of scattering, emission, and extinction spectra, including the UV range, and thus the present work will aid those who would use such particles for spectroscopic related separations or sensors. The spectroscopic behavior of CT-GNPs with different core sizes (5, 10, 30, and 50 nm) was studied in ultra-pure water at pH 6.0-6.5 employing UV-visible extinction, excitation-emission matrix (EEM), resonance Rayleigh scattering, and dynamic light scattering (DLS) spectroscopies. The CT-GNP-5 and CT-GNP-10 samples aggregated, absorbed light, and emitted light. In contrast, the CT-GNP-30 and CT-GNP-50 samples did not aggregate and did not emit light, but scattered light intensely. Multimodal peaks were observed in the intensity-based DLS spectra of CT-GNP-5 and CT-GNP-10 samples. Monomodal peaks in the volume-based DLS spectra overestimated particle diameters by 60% and 30% for the CT-GNP-5 and CT-GNP-10 samples, respectively, but underestimated diameters by 10% and 4% for the CT-GNP-30 and CT-GNP-50 samples. The volume-based DLS spectra indicated that dimer and trimer aggregates contributed most to the overall volume of particles in the 5- and 10-nm CT-GNPs, whereas the CT-GNP-30 and CT-GNP-50 samples did not aggregate. Here, we discuss the potential influence that differences in preparation, ionic strength, zeta potential, and conformation of adsorbed citrate anions (due to surface curvature of corona) may exert on the aggregation and spectral observations in these data. In particular, the severe surface curvature of the 5- and 10-nm GNP corona may affect the efficiency of the di-/tribasic citrate compatiblizer molecule to shield the core from interactions with light and from GNP-GNP homoaggregation.

How Noniridescent Colors Are Generated by Quasi-ordered Structures of Bird Feathers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Noh, Heeso; Liew, Seng Fatt; Saranathan, Vinodkumar

2012-03-26

We investigate the mechanism of structural coloration by quasi-ordered nanostructures in bird feather barbs. Small-angle X-ray scattering (SAXS) data reveal the structures are isotropic and have short-range order on length scales comparable to optical wavelengths. We perform angle-resolved reflection and scattering spectrometry to fully characterize the colors under directional and omni-directional illumination of white light. Under directional lighting, the colors change with the angle between the directions of illumination and observation. The angular dispersion of the primary peaks in the scattering/reflection spectra can be well explained by constructive interference of light that is scattered only once in the quasi-ordered structures.more » Using the Fourier power spectra of structure from the SAXS data we calculate optical scattering spectra and explain why the light scattering peak is the highest in the backscattering direction. Under omni-directional lighting, colors from the quasi-ordered structures are invariant with the viewing angle. The non-iridescent coloration results from the isotropic nature of structures instead of strong backscattering.« less

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.

Vesicle Adhesion and Fusion Studied by Small-Angle X-Ray Scattering.

PubMed

Komorowski, Karlo; Salditt, Annalena; Xu, Yihui; Yavuz, Halenur; Brennich, Martha; Jahn, Reinhard; Salditt, Tim

2018-04-24

We have studied the adhesion state (also denoted by docking state) of lipid vesicles as induced by the divalent ions Ca 2+ or Mg 2+ at well-controlled ion concentration, lipid composition, and charge density. The bilayer structure and the interbilayer distance in the docking state were analyzed by small-angle x-ray scattering. A strong adhesion state was observed for DOPC:DOPS vesicles, indicating like-charge attraction resulting from ion correlations. The observed interbilayer separations of ∼1.6 nm agree quantitatively with the predictions of electrostatics in the strong coupling regime. Although this phenomenon was observed when mixing anionic and zwitterionic (or neutral) lipids, pure anionic membranes (DOPS) with highest charge density σ resulted in a direct phase transition to a multilamellar state, which must be accompanied by rupture and fusion of vesicles. To extend the structural assay toward protein-controlled docking and fusion, we have characterized reconstituted N-ethylmaleimide-sensitive factor attachment protein receptors in controlled proteoliposome suspensions by small-angle x-ray scattering. Copyright © 2018 Biophysical Society. Published by Elsevier Inc. All rights reserved.

Role of solution structure in self-assembly of conjugated block copolymer thin films

DOE PAGES

Brady, Michael A.; Ku, Sung -Yu; Perez, Louis A.; ...

2016-10-24

Conjugated block copolymers provide a pathway to achieve thermally stable nanostructured thin films for organic solar cells. We characterized the structural evolution of poly(3-hexylthiophene)- block-poly(diketopyrrolopyrrole–terthiophene) (P3HT- b-DPPT-T) from solution to nanostructured thin films. Aggregation of the DPPT-T block of P3HT- b-DPPT-T was found in solution by small-angle X-ray scattering with the P3HT block remaining well-solvated. The nanostructure in thin films was determined using a combination of wide and small-angle X-ray scattering techniques as a function of processing conditions. The structure in solution controlled the initial nanostructure in spin-cast thin films, allowing subsequent thermal annealing processes to further improve the ordering.more » In contrast to the results for thin films, nanostructural ordering was not observed in the bulk samples by small-angle X-ray scattering. Finally, these results suggest the importance of controlling solvent induced aggregation in forming nanostructured thin films of conjugated block copolymers.« less

Wavelength-independent constant period spin-echo modulated small angle neutron scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sales, Morten, E-mail: lsp260@alumni.ku.dk; Plomp, Jeroen; Bouwman, Wim

2016-06-15

Spin-Echo Modulated Small Angle Neutron Scattering (SEMSANS) in Time-of-Flight (ToF) mode has been shown to be a promising technique for measuring (very) small angle neutron scattering (SANS) signals and performing quantitative Dark-Field Imaging (DFI), i.e., SANS with 2D spatial resolution. However, the wavelength dependence of the modulation period in the ToF spin-echo mode has so far limited the useful modulation periods to those resolvable with the limited spatial resolution of the detectors available. Here we present our results of an approach to keep the period of the induced modulation constant for the wavelengths utilised in ToF. This is achieved bymore » ramping the magnetic fields in the coils responsible for creating the spatially modulated beam in synchronisation with the neutron pulse, thus keeping the modulation period constant for all wavelengths. Such a setup enables the decoupling of the spatial detector resolution from the resolution of the modulation period by the use of slits or gratings in analogy to the approach in grating-based neutron DFI.« less

Direct comparison of Fe-Cr unmixing characterization by atom probe tomography and small angle scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Couturier, Laurent, E-mail: laurent.couturier55@ho

The fine microstructure obtained by unmixing of a solid solution either by classical precipitation or spinodal decomposition is often characterized either by small angle scattering or atom probe tomography. This article shows that a common data analysis framework can be used to analyze data obtained from these two techniques. An example of the application of this common analysis is given for characterization of the unmixing of the Fe-Cr matrix of a 15-5 PH stainless steel during long-term ageing at 350 °C and 400 °C. A direct comparison of the Cr composition fluctuations amplitudes and characteristic lengths obtained with both techniquesmore » is made showing a quantitative agreement for the fluctuation amplitudes. The origin of the discrepancy remaining for the characteristic lengths is discussed. - Highlights: •Common analysis framework for atom probe tomography and small angle scattering •Comparison of same microstructural characteristics obtained using both techniques •Good correlation of Cr composition fluctuations amplitudes from both techniques •Good correlation of Cr composition fluctuations amplitudes with classic V parameter.« less

Role of solution structure in self-assembly of conjugated block copolymer thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brady, Michael A.; Ku, Sung -Yu; Perez, Louis A.

Conjugated block copolymers provide a pathway to achieve thermally stable nanostructured thin films for organic solar cells. We characterized the structural evolution of poly(3-hexylthiophene)- block-poly(diketopyrrolopyrrole–terthiophene) (P3HT- b-DPPT-T) from solution to nanostructured thin films. Aggregation of the DPPT-T block of P3HT- b-DPPT-T was found in solution by small-angle X-ray scattering with the P3HT block remaining well-solvated. The nanostructure in thin films was determined using a combination of wide and small-angle X-ray scattering techniques as a function of processing conditions. The structure in solution controlled the initial nanostructure in spin-cast thin films, allowing subsequent thermal annealing processes to further improve the ordering.more » In contrast to the results for thin films, nanostructural ordering was not observed in the bulk samples by small-angle X-ray scattering. Finally, these results suggest the importance of controlling solvent induced aggregation in forming nanostructured thin films of conjugated block copolymers.« less

DNA-magnetic Particle Binding Analysis by Dynamic and Electrophoretic Light Scattering.

PubMed

Haddad, Yazan; Dostalova, Simona; Kudr, Jiri; Zitka, Ondrej; Heger, Zbynek; Adam, Vojtech

2017-11-09

Isolation of DNA using magnetic particles is a field of high importance in biotechnology and molecular biology research. This protocol describes the evaluation of DNA-magnetic particles binding via dynamic light scattering (DLS) and electrophoretic light scattering (ELS). Analysis by DLS provides valuable information on the physicochemical properties of particles including particle size, polydispersity, and zeta potential. The latter describes the surface charge of the particle which plays major role in electrostatic binding of materials such as DNA. Here, a comparative analysis exploits three chemical modifications of nanoparticles and microparticles and their effects on DNA binding and elution. Chemical modifications by branched polyethylenimine, tetraethyl orthosilicate and (3-aminopropyl)triethoxysilane are investigated. Since DNA exhibits a negative charge, it is expected that zeta potential of particle surface will decrease upon binding of DNA. Forming of clusters should also affect particle size. In order to investigate the efficiency of these particles in isolation and elution of DNA, the particles are mixed with DNA in low pH (~6), high ionic strength and dehydration environment. Particles are washed on magnet and then DNA is eluted by Tris-HCl buffer (pH = 8). DNA copy number is estimated using quantitative polymerase chain reaction (PCR). Zeta potential, particle size, polydispersity and quantitative PCR data are evaluated and compared. DLS is an insightful and supporting method of analysis that adds a new perspective to the process of screening of particles for DNA isolation.

Fiber-Optic Imaging Probe Developed for Space Used to Detect Diabetes Through the Eye

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Chenault, Michelle V.; Datiles, Manuel B., III; Sebag, J.; Suh, Kwang I.

2000-01-01

Approximately 16 million Americans have diabetes mellitus, which can severely impair eyesight by causing cataracts, diabetic retinopathy, and glaucoma. Cataracts are 1.6 times more common in people with diabetes than in those without diabetes, and cataract extraction is the only surgical treatment. In many cases, diabetes-related ocular pathologies go undiagnosed until visual function is compromised. This ongoing pilot project seeks to study the progression of diabetes in a unique animal model by monitoring changes in the lens with a safe, sensitive, dynamic light-scattering probe. Dynamic light scattering (DLS), has the potential to diagnose cataracts at the molecular level. Recently, a new DLS fiber-optic probe was developed at the NASA Glenn Research Center at Lewis Field for noncontact, accurate, and extremely sensitive particle-sizing measurements in fluid dispersions and suspensions (ref. 1). This compact, portable, and rugged probe is free of optical alignment, offers point-and-shoot operation for various online field applications and challenging environments, and yet is extremely flexible in regards to sample container sizes, materials, and shapes. No external vibration isolation and no index matching are required. It can measure particles as small as 1 nm and as large as few micrometers in a wide concentration range from very dilute (waterlike) dispersions to very turbid (milklike) suspensions. It is safe and fast to use, since it only requires very low laser power (10 nW to 3 mW) with very short data acquisition times (2 to 10 sec).

Detection of vapor nanobubbles by small angle neutron scattering (SANS)

NASA Astrophysics Data System (ADS)

Popov, Emilian; He, Lilin; Dominguez-Ontiveros, Elvis; Melnichenko, Yuri

2018-04-01

Experiments using boiling water on untreated (roughness 100-300 nm) metal surfaces using small-angle neutron scattering (SANS) show the appearance of structures that are 50-70 nm in size when boiling is present. The scattering signal disappears when the boiling ceases, and no change in the signal is detected at any surface temperature condition below saturation. This confirms that the signal is caused by vapor nanobubbles. Two boiling regimes are evaluated herein that differ by the degree of subcooling (3-10 °C). A polydisperse spherical model with a log-normal distribution fits the SANS data well. The size distribution indicates that a large number of nanobubbles exist on the surface during boiling, and some of them grow into large bubbles.

A microstructural comparison of two nuclear-grade martensitic steels using small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Coppola, R.; Fiori, F.; Little, E. A.; Magnani, M.

1997-06-01

Results are presented of a small-angle neutron scattering (SANS) study on two 10-13% Cr martensitic stainless steels of interest for nuclear applications, viz. DIN 1.4914 (MANET specification, for fusion reactors) and AISI 410. The investigation has focussed principally on microstructural effects associated with the differences in chromium content between the two alloys. The size distribution functions determined from nuclear and magnetic SANS components for the two steels given identical heat treatments are in accord with an interpretation based on the presence of ˜ 1 nm size CCr aggregates in the microstructure. Much larger (˜ 10 nm) scattering inhomogeneities with different magnetic contrast are also present and tentatively identified as carbides.

Application of support vector regression for optimization of vibration flow field of high-density polyethylene melts characterized by small angle light scattering

NASA Astrophysics Data System (ADS)

Xian, Guangming

2018-03-01

In this paper, the vibration flow field parameters of polymer melts in a visual slit die are optimized by using intelligent algorithm. Experimental small angle light scattering (SALS) patterns are shown to characterize the processing process. In order to capture the scattered light, a polarizer and an analyzer are placed before and after the polymer melts. The results reported in this study are obtained using high-density polyethylene (HDPE) with rotation speed at 28 rpm. In addition, support vector regression (SVR) analytical method is introduced for optimization the parameters of vibration flow field. This work establishes the general applicability of SVR for predicting the optimal parameters of vibration flow field.

Small angle scattering from protein/sugar conjugates

NASA Astrophysics Data System (ADS)

Jackson, Andrew; White, John

2006-11-01

The Maillard reaction between free amine groups on proteins and sugars is well known. We have examined the effect of the reaction of the casein group of milk proteins with sugars on their nanoscale structure and aggregation. The small angle neutron scattering from beta casein and sodium caseinate and their sugar conjugates have been studied as a function of solution concentration. At high conjugate concentration (greater than ca. 5 mg/ml) the addition of sugar reduces supra-micellar aggregation of the protein whilst at lower concentration, where the protein is expected to be deaggregated already, little effect is seen. Guinier analysis of the scattering data show a radius of gyration of around 75 A˚ for beta casein in solution and around 80 A˚ for the sucrose conjugate.

Investigations of the fabrication and the surface-enhanced Raman scattering detection applications for tapered fiber probes prepared with the laser-induced chemical deposition method.

PubMed

Fan, Qunfang; Cao, Jie; Liu, Ye; Yao, Bo; Mao, Qinghe

2013-09-01

The process of depositing nanoparticles onto tapered fiber probes with the laser-induced chemical deposition method (LICDM) and the surface-enhanced Raman scattering (SERS) detection performance of the prepared probes are experimentally investigated in this paper. Our results show that the nanoparticle-deposited tapered fiber probes prepared with the LICDM method depend strongly on the value of the cone angle. For small-angle tapered probes the nanoparticle-deposited areas are only focused at the taper tips, because the taper surfaces are mainly covered by a relatively low-intensity evanescent field. By lengthening the reaction time or increasing the induced power or solution concentration, it is still possible to deposit nanoparticles on small-angle tapers with the light-scattering effect. With 4-aminothiophenol as the testing molecule, it was found that for given preparation conditions, the cone angles for the tapered probes with the highest SERS spectral intensities for different excitation laser powers are almost the same. However, such an optimal cone angle is determined by the combined effects of both the localized surface plasmon resonance strength and the transmission loss generated by the nanoparticles deposited.

Character of the opposition effect and negative polarization

NASA Technical Reports Server (NTRS)

Pieters, Carle M.; Shkuratov, Yu. G.; Stankevich, D. G.

1991-01-01

Photometric and polarimetric properties at small phase angles were measured for silicates with controlled surface properties in order to distinguish properties that are associated with surface reflection from those that are associated with multiple scattering from internal grain boundaries. These data provide insight into the causes and conditions of photometric properties observed at small phase angles for dark bodies of the solar system. Obsidian was chosen to represent a silicate dielectric with no internal scattering boundaries. Because obsidian is free of internal scatterers, light reflected from both the rough and smooth obsidian samples is almost entirely single and multiple Fresnel reflections form surface facets with no body component. Surface structure alone cannot produce an opposition effect. Comparison of the obsidian and basalt results indicates that for an opposition effect to occur, surface texture must be both rough and contain internal scattering interfaces. Although the negative polarization observed for the obsidian samples indicates single and multiple reflections are part of negative polarization, the longer inversion angle of the multigrain inversion samples implies that internal reflections must also contribute a significant negative polarization component.

Reflective small angle electron scattering to characterize nanostructures on opaque substrates

NASA Astrophysics Data System (ADS)

Friedman, Lawrence H.; Wu, Wen-Li; Fu, Wei-En; Chien, Yunsan

2017-09-01

Feature sizes in integrated circuits (ICs) are often at the scale of 10 nm and are ever shrinking. ICs appearing in today's computers and hand held devices are perhaps the most prominent examples. These smaller feature sizes demand equivalent advances in fast and accurate dimensional metrology for both development and manufacturing. Techniques in use and continuing to be developed include X-ray based techniques, optical scattering, and of course the electron and scanning probe microscopy techniques. Each of these techniques has their advantages and limitations. Here, the use of small angle electron beam scattering measurements in a reflection mode (RSAES) to characterize the dimensions and the shape of nanostructures on flat and opaque substrates is demonstrated using both experimental and theoretical evidence. In RSAES, focused electrons are scattered at angles smaller than 1 ° with the assistance of electron optics typically used in transmission electron microscopy. A proof-of-concept experiment is combined with rigorous electron reflection simulations to demonstrate the efficiency and accuracy of RSAES as a method of non-destructive measurement of shapes of features less than 10 nm in size on flat and opaque substrates.

Reflective Small Angle Electron Scattering to Characterize Nanostructures on Opaque Substrates.

PubMed

Friedman, Lawrence H; Wu, Wen-Li; Fu, Wei-En; Chien, Yunsan

2017-09-01

Features sizes in integrated circuits (ICs) are often at the scale of 10 nm and are ever shrinking. ICs appearing in today's computers and hand held devices are perhaps the most prominent examples. These smaller feature sizes demand equivalent advances in fast and accurate dimensional metrology for both development and manufacturing. Techniques in use and continuing to be developed include X-ray based techniques, optical scattering and of course the electron and scanning probe microscopy techniques. Each of these techniques have their advantages and limitations. Here the use of small angle electron beam scattering measurements in a reflection mode (RSAES) to characterize the dimensions and the shape of nanostructures on flat and opaque substrates is demonstrated using both experimental and theoretical evidence. In RSAES, focused electrons are scattered at angles smaller than 1° with the assistance of electron optics typically used in transmission electron microscopy. A proof-of-concept experiment is combined with rigorous electron reflection simulations to demonstrate the efficiency and accuracy of RSAES as a method of non-destructive measurement of shapes of features less than 10 nm in size on flat and opaque substrates.

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.

A stress-controlled shear cell for small-angle light scattering and microscopy.

PubMed

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.

Digenetic Changes in Macro- to Nano-Scale Porosity in the St. Peter Sandstone:L An (Ultra) Small Angle Neutron Scattering and Backscattered Electron Imagining Analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anovitz, Lawrence; Cole, David; Rother, Gernot

2013-01-01

Small- and Ultra-Small Angle Neutron Scattering (SANS and USANS) provide powerful tools for quantitative analysis of porous rocks, yielding bulk statistical information over a wide range of length scales. This study utilized (U)SANS to characterize shallowly buried quartz arenites from the St. Peter Sandstone. Backscattered electron imaging was also used to extend the data to larger scales. These samples contain significant volumes of large-scale porosity, modified by quartz overgrowths, and neutron scattering results show significant sub-micron porosity. While previous scattering data from sandstones suggest scattering is dominated by surface fractal behavior over many orders of magnitude, careful analysis of ourmore » data shows both fractal and pseudo-fractal behavior. The scattering curves are composed of subtle steps, modeled as polydispersed assemblages of pores with log-normal distributions. However, in some samples an additional surface-fractal overprint is present, while in others there is no such structure, and scattering can be explained by summation of non-fractal structures. Combined with our work on other rock-types, these data suggest that microporosity is more prevalent, and may play a much more important role than previously thought in fluid/rock interactions.« less

Nanoscale femtosecond imaging of transient hot solid density plasmas with elemental and charge state sensitivity using resonant coherent diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kluge, T., E-mail: t.kluge@hzdr.de; Bussmann, M.; Huang, L. G., E-mail: lingen.huang@hzdr.de

Here, we propose to exploit the low energy bandwidth, small wavelength, and penetration power of ultrashort pulses from XFELs for resonant Small Angle Scattering (SAXS) on plasma structures in laser excited plasmas. Small angle scattering allows to detect nanoscale density fluctuations in forward scattering direction. Typically, the SAXS signal from laser excited plasmas is expected to be dominated by the free electron distribution. We propose that the ionic scattering signal becomes visible when the X-ray energy is in resonance with an electron transition between two bound states (resonant coherent X-ray diffraction). In this case, the scattering cross-section dramatically increases somore » that the signal of X-ray scattering from ions silhouettes against the free electron scattering background which allows to measure the opacity and derived quantities with high spatial and temporal resolution, being fundamentally limited only by the X-ray wavelength and timing. Deriving quantities such as ion spatial distribution, charge state distribution, and plasma temperature with such high spatial and temporal resolution will make a vast number of processes in shortpulse laser-solid interaction accessible for direct experimental observation, e.g., hole-boring and shock propagation, filamentation and instability dynamics, electron transport, heating, and ultrafast ionization dynamics.« less

Generalized skew-symmetric interfacial probability distribution in reflectivity and small-angle scattering analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiang, Zhang; Chen, Wei

Generalized skew-symmetric probability density functions are proposed to model asymmetric interfacial density distributions for the parameterization of any arbitrary density profiles in the `effective-density model'. The penetration of the densities into adjacent layers can be selectively controlled and parameterized. A continuous density profile is generated and discretized into many independent slices of very thin thickness with constant density values and sharp interfaces. The discretized profile can be used to calculate reflectivities via Parratt's recursive formula, or small-angle scattering via the concentric onion model that is also developed in this work.

Generalized skew-symmetric interfacial probability distribution in reflectivity and small-angle scattering analysis

DOE PAGES

Jiang, Zhang; Chen, Wei

2017-11-03

Generalized skew-symmetric probability density functions are proposed to model asymmetric interfacial density distributions for the parameterization of any arbitrary density profiles in the `effective-density model'. The penetration of the densities into adjacent layers can be selectively controlled and parameterized. A continuous density profile is generated and discretized into many independent slices of very thin thickness with constant density values and sharp interfaces. The discretized profile can be used to calculate reflectivities via Parratt's recursive formula, or small-angle scattering via the concentric onion model that is also developed in this work.

In-situ small angle x-ray scattering investigation on nucleation and growth of silica colloids

NASA Astrophysics Data System (ADS)

Bahadur, J.; Tripathi, B. M.; Prakash, J.; Das, Avik; Sen, D.; Mazumder, S.

2018-04-01

The nucleation and growth of silica colloids has been studied using real time small-angle X-ray scattering measurements. The ammonium fluorosilicate was used as precursor and both weak (NH3) and strong base (NaOH) has been used as reducing agent for the precursor. It is observed that nucleation, growth and aggregation phenomenon occur simultaneously. The kinetics of the nucleation and growth of silica colloids depends on the strength of the reducing agent as well on its concentration. The kinetics is slow for NH3 but is very fast for higher concentration of NaOH.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raghuwanshi, Vikram Singh, E-mail: vikram.raghuwanshi@helmholtz-berlin.de; Harizanova, Ruzha; Tatchev, Dragomir

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 enrichedmore » 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.« less

Structural and magnetic properties of multi-core nanoparticles analysed using a generalised numerical inversion method

PubMed Central

Bender, P.; Bogart, L. K.; Posth, O.; Szczerba, W.; Rogers, S. E.; Castro, A.; Nilsson, L.; Zeng, L. J.; Sugunan, A.; Sommertune, J.; Fornara, A.; González-Alonso, D.; Barquín, L. Fernández; Johansson, C.

2017-01-01

The structural and magnetic properties of magnetic multi-core particles were determined by numerical inversion of small angle scattering and isothermal magnetisation data. The investigated particles consist of iron oxide nanoparticle cores (9 nm) embedded in poly(styrene) spheres (160 nm). A thorough physical characterisation of the particles included transmission electron microscopy, X-ray diffraction and asymmetrical flow field-flow fractionation. Their structure was ultimately disclosed by an indirect Fourier transform of static light scattering, small angle X-ray scattering and small angle neutron scattering data of the colloidal dispersion. The extracted pair distance distribution functions clearly indicated that the cores were mostly accumulated in the outer surface layers of the poly(styrene) spheres. To investigate the magnetic properties, the isothermal magnetisation curves of the multi-core particles (immobilised and dispersed in water) were analysed. The study stands out by applying the same numerical approach to extract the apparent moment distributions of the particles as for the indirect Fourier transform. It could be shown that the main peak of the apparent moment distributions correlated to the expected intrinsic moment distribution of the cores. Additional peaks were observed which signaled deviations of the isothermal magnetisation behavior from the non-interacting case, indicating weak dipolar interactions. PMID:28397851

Mineral crystal alignment in mineralized fracture callus determined by 3D small-angle X-ray scattering

NASA Astrophysics Data System (ADS)

Liu, Yifei; Manjubala, Inderchand; Roschger, Paul; Schell, Hanna; Duda, Georg N.; Fratzl, Peter

2010-10-01

Callus tissue formed during bone fracture healing is a mixture of different tissue types as revealed by histological analysis. But the structural characteristics of mineral crystals within the healing callus are not well known. Since two-dimensional (2D) scanning small-angle X-ray scattering (sSAXS) patterns showed that the size and orientation of callus crystals vary both spatially and temporally [1] and 2D electron microscopic analysis implies an anisotropic property of the callus morphology, the mineral crystals within the callus are also expected to vary in size and orientation in 3D. Three-dimensional small-angle X-ray scattering (3D SAXS), which combines 2D SAXS patterns collected at different angles of sample tilting, has been previously applied to investigate bone minerals in horse radius [2] and oim/oim mouse femur/tibia [3]. We implement a similar 3D SAXS method but with a different way of data analysis to gather information on the mineral alignment in fracture callus. With the proposed accurate yet fast assessment of 3D SAXS information, it was shown that the plate shaped mineral particles in the healing callus were aligned in groups with their predominant orientations occurring as a fiber texture.

Small-Angle Scatter Measurement.

NASA Astrophysics Data System (ADS)

Wein, Steven Jay

The design, analysis, and performance of a small -angle scatterometer are presented. The effects of the diffraction background, geometrical aberrations and system scatter at the small-angles are separated. Graphs are provided that quantify their contribution. The far-field irradiance distributions of weakly truncated and untruncated Gaussian beams are compared. The envelope of diffraction ringing is shown to decrease proportionately with the level of truncation in the pupil. Spherical aberration and defocus are shown to have little effect on the higher-order diffraction rings of Gaussian apertures and as such will have a negligible effect on most scatter measurements. A method is presented for determining the scattered irradiance level for a given BRDF in relation to the peak irradiance of the point spread function. A method of Gaussian apodization is presented and tested that allows the level of diffraction ringing to become a design parameter. Upon sufficient reduction of the diffraction background, the scattered light from the scatterometers' primary mirror is seen to be the limiting component of the small-angle instrument profile. The scatterometer described was able to make a meaningful measurement close enough to the specular direction at 0.6328mum in order to observe the characteristic height and width of the scatter function. This allowed the rms roughness and autocorrelation length of the surface to be determined from the scatter data at this wavelength. The inferred rms roughness agreed well with an independent optical profilometer measurement of the surface. The BRDF of the samples were also measured at 10.6mum. The rms roughness inferred from this scatter data did not agree with the other measurements. The BRDF did not scale in accordance with the scaler diffraction theory of microrough surfaces. The scattering in the visible was dominated by the effects of surface roughness whereas the scattering in the far-infrared was apparently dominated by the effects of contaminants and surface defects. The model for the surface statistics is investigated. A K_0 (modified Bessel function) autocorrelation function is shown to predict the scattered light distribution of these samples much better than the conventional negative -exponential function. Additionally, a sampling theory is developed that addresses the negative-exponentially correlated output of lock-in amplifiers, detectors, and electronic circuits in general. It is shown that the optimum sampling rate is approximately one sample per time constant and at this rate the improvement in SNR is sqrt {N/2} where N is the number of measurements.

Optical Interactions at Randomly Rough Surfaces

DTIC Science & Technology

2003-03-10

frequency range. The design of a random surface that acts as a Lambertian diffuser, especially in the infrared region of the optical spectrum, is...FTIR grazing angle microscopy. Recently, an experimental study was performed of the far-field scattering at small grazing angles, especially the enhanced...a specular component in the scattered light, in this frequency range. The design of a random surface that acts as a Lambertian diffuser, especially in

Absolute Intra-Molecular Distance Measurements with Ångström-Resolution using Anomalous Small-Angle X-ray Scattering

DOE PAGES

Zettl, Thomas; Mathew, Rebecca S.; Seifert, Sönke; ...

2016-05-31

Accurate determination of molecular distances is fundamental to understanding the structure, dynamics, and conformational ensembles of biological macromolecules. Here we present a method to determine the full,distance,distribution between small (~7 Å) gold labels attached to macromolecules with very high-precision(≤1 Å) and on an absolute distance scale. Our method uses anomalous small-angle X-ray scattering close to a gold absorption edge to separate the gold-gold interference pattern from other scattering contributions. Results for 10-30 bp DNA constructs achieve excellent signal-to-noise and are in good agreement with previous results obtained by single-energy,SAXS measurements without requiring the preparation and measurement of single labeled andmore » unlabeled samples. Finally, the use of small gold labels in combination with ASAXS read out provides an attractive approach to determining molecular distance distributions that will be applicable to a broad range of macromolecular systems.« less

Spin waves in full-polarized state of Dzyaloshinskii-Moriya helimagnets: Small-angle neutron scattering study

NASA Astrophysics Data System (ADS)

Grigoriev, S. V.; Sukhanov, A. S.; Altynbaev, E. V.; Siegfried, S.-A.; Heinemann, A.; Kizhe, P.; Maleyev, S. V.

2015-12-01

We develop the technique to study the spin-wave dynamics of the full-polarized state of the Dzyaloshinskii-Moriya helimagnets by polarized small-angle neutron scattering. We have experimentally proven that the spin-waves dispersion in this state has the anisotropic form. We show that the neutron scattering image displays a circle with a certain radius which is centered at the momentum transfer corresponding to the helix wave vector in helimagnetic phase ks, which is oriented along the applied magnetic field H . The radius of this circle is directly related to the spin-wave stiffness of this system. This scattering depends on the neutron polarization showing the one-handed nature of the spin waves in Dzyaloshinskii-Moriya helimagnets in the full-polarized phase. We show that the spin-wave stiffness A for MnSi helimagnet decreased twice as the temperature increases from zero to the critical temperature Tc.

Measurement system to determine the total and angle-resolved light scattering of optical components in the deep-ultraviolet and vacuum-ultraviolet spectral regions

NASA Astrophysics Data System (ADS)

Schröder, Sven; Gliech, Stefan; Duparré, Angela

2005-10-01

An instrumentation for total and angle-resolved scattering (ARS) at 193 and 157 nm has been developed at the Fraunhofer Institute in Jena to meet the severe requirements for scattering analysis of deep- and vacuum-ultraviolet optical components. Extremely low backscattering levels of 10^-6 for the total scattering measurements and more than 9 orders of magnitude dynamic range for ARS have been accomplished. Examples of application extend from the control of at-wavelength scattering losses of superpolished substrates with rms roughness as small as 0.1 nm to the detection of volume material scattering and the study into the scattering of multilayer coatings. In addition, software programs were developed to model the roughness-induced light scattering of substrates and thin-film coatings.

Multiple scattered radiation emerging from Rayleigh and continental haze layers. 1: Radiance, polarization, and neutral points.

PubMed

Kattawar, G W; Plass, G N; Hitzfelder, S J

1976-03-01

The complete radiation field including polarization is calculated by the matrix operator method for scattering layers of various optical thicknesses. Results obtained for Rayleigh scattering are compared with those for scattering from a continental haze. Radiances calculated using Stokes vectors show differences as large as 23% compared to the approximate scalar theory of radiative transfer, while the same differences are only of the order of 0.1% for a continental haze phase function. The polarization of the reflected and transmitted radiation is given for a wide range of optical thicknesses of the scattering layer, for various solar zenith angles, and various surface albedos. Two entirely different types of neutral points occur for aerosol phase functions. Rayleigh-like neutral points (RNP) arise from the zero polarization in single scattering that occurs for all phase functions at scattering angles of 0 degrees and 180 degrees . For Rayleigh phase functions, the position of the RNP varies appreciably with the optical thickness of the scattering layer. At low solar elevations there may be four RNP. For a continental haze phase function the position of the RNP in the reflected radiation shows only a small variation with the optical thickness, and the RNP exists in the transmitted radiation only for extremely small optical thicknesses. Another type of neutral point (NRNP) exists for aerosol phase functions. It is associated with the zeros of the single scattered polarization, which occur between the end points of the curve; these are called non-Rayleigh neutral points (NRNP). There may be from zero to four of these neutral points associated with each zero of the single scattering curve. They occur over a range of azimuthal angles, unlike the RNP that are in the principal plane only. The position of these neutral points is given as a function of solar angle and optical thickness.

Impact of asymmetrical flow field-flow fractionation on protein aggregates stability.

PubMed

Bria, Carmen R M; Williams, S Kim Ratanathanawongs

2016-09-23

The impact of asymmetrical flow field-flow fractionation (AF4) on protein aggregate species is investigated with the aid of multiangle light scattering (MALS) and dynamic light scattering (DLS). The experimental parameters probed in this study include aggregate stability in different carrier liquids, shear stress (related to sample injection), sample concentration (during AF4 focusing), and sample dilution (during separation). Two anti-streptavidin (anti-SA) IgG1 samples composed of low and high molar mass (M) aggregates are subjected to different AF4 conditions. Aggregates suspended and separated in phosphate buffer are observed to dissociate almost entirely to monomer. However, aggregates in citric acid buffer are partially stable with dissociation to 25% and 5% monomer for the low and high M samples, respectively. These results demonstrate that different carrier liquids change the aggregate stability and low M aggregates can behave differently than their larger counterparts. Increasing the duration of the AF4 focusing step showed no significant changes in the percent monomer, percent aggregates, or the average Ms in either sample. Syringe-induced shear related to sample injection resulted in an increase in hydrodynamic diameter (dh) as measured by batch mode DLS. Finally, calculations showed that dilution during AF4 separation is significantly lower than in size exclusion chromatography with dilution occurring mainly at the AF4 channel outlet and not during the separation. This has important ramifications when analyzing aggregates that rapidly dissociate (<∼2s) upon dilution as the size calculated by AF4 theory may be more accurate than that measured by online DLS. Experimentally, the dhs determined by online DLS generally agreed with AF4 theory except for the more well retained larger aggregates for which DLS showed smaller sizes. These results highlight the importance of using AF4 retention theory to understand the impacts of dilution on analytes. Copyright © 2016 Elsevier B.V. All rights reserved.

Grazing-incidence small-angle X-ray scattering (GISAXS) on small periodic targets using large beams

PubMed Central

Soltwisch, Victor; Probst, Jürgen; Scholze, Frank; Krumrey, Michael

2017-01-01

Grazing-incidence small-angle X-ray scattering (GISAXS) is often used as a versatile tool for the contactless and destruction-free investigation of nano­structured surfaces. However, due to the shallow incidence angles, the footprint of the X-ray beam is significantly elongated, limiting GISAXS to samples with typical target lengths of several millimetres. For many potential applications, the production of large target areas is impractical, and the targets are surrounded by structured areas. Because the beam footprint is larger than the targets, the surrounding structures contribute parasitic scattering, burying the target signal. In this paper, GISAXS measurements of isolated as well as surrounded grating targets in Si substrates with line lengths from 50 µm down to 4 µm are presented. For the isolated grating targets, the changes in the scattering patterns due to the reduced target length are explained. For the surrounded grating targets, the scattering signal of a 15 µm × 15 µm target grating structure is separated from the scattering signal of 100 µm × 100 µm nanostructured surroundings by producing the target with a different orientation with respect to the predominant direction of the surrounding structures. As virtually all litho­graphically produced nanostructures have a predominant direction, the described technique allows GISAXS to be applied in a range of applications, e.g. for characterization of metrology fields in the semiconductor industry, where up to now it has been considered impossible to use this method due to the large beam footprint. PMID:28875030

Grazing-incidence small-angle X-ray scattering (GISAXS) on small periodic targets using large beams.

PubMed

Pflüger, Mika; Soltwisch, Victor; Probst, Jürgen; Scholze, Frank; Krumrey, Michael

2017-07-01

Grazing-incidence small-angle X-ray scattering (GISAXS) is often used as a versatile tool for the contactless and destruction-free investigation of nano-structured surfaces. However, due to the shallow incidence angles, the footprint of the X-ray beam is significantly elongated, limiting GISAXS to samples with typical target lengths of several millimetres. For many potential applications, the production of large target areas is impractical, and the targets are surrounded by structured areas. Because the beam footprint is larger than the targets, the surrounding structures contribute parasitic scattering, burying the target signal. In this paper, GISAXS measurements of isolated as well as surrounded grating targets in Si substrates with line lengths from 50 µm down to 4 µm are presented. For the isolated grating targets, the changes in the scattering patterns due to the reduced target length are explained. For the surrounded grating targets, the scattering signal of a 15 µm × 15 µm target grating structure is separated from the scattering signal of 100 µm × 100 µm nanostructured surroundings by producing the target with a different orientation with respect to the predominant direction of the surrounding structures. As virtually all litho-graphically produced nanostructures have a predominant direction, the described technique allows GISAXS to be applied in a range of applications, e.g.  for characterization of metrology fields in the semiconductor industry, where up to now it has been considered impossible to use this method due to the large beam footprint.

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.

A Structural Study of CESA1 Catalytic Domain of Arabidopsis Cellulose Synthesis Complex: Evidence for CESA Trimers.

PubMed

Vandavasi, Venu Gopal; Putnam, Daniel K; Zhang, Qiu; Petridis, Loukas; Heller, William T; Nixon, B Tracy; Haigler, Candace H; Kalluri, Udaya; Coates, Leighton; Langan, Paul; Smith, Jeremy C; Meiler, Jens; O'Neill, Hugh

2016-01-01

A cellulose synthesis complex with a "rosette" shape is responsible for synthesis of cellulose chains and their assembly into microfibrils within the cell walls of land plants and their charophyte algal progenitors. The number of cellulose synthase proteins in this large multisubunit transmembrane protein complex and the number of cellulose chains in a microfibril have been debated for many years. This work reports a low resolution structure of the catalytic domain of CESA1 from Arabidopsis (Arabidopsis thaliana; AtCESA1CatD) determined by small-angle scattering techniques and provides the first experimental evidence for the self-assembly of CESA into a stable trimer in solution. The catalytic domain was overexpressed in Escherichia coli, and using a two-step procedure, it was possible to isolate monomeric and trimeric forms of AtCESA1CatD. The conformation of monomeric and trimeric AtCESA1CatD proteins were studied using small-angle neutron scattering and small-angle x-ray scattering. A series of AtCESA1CatD trimer computational models were compared with the small-angle x-ray scattering trimer profile to explore the possible arrangement of the monomers in the trimers. Several candidate trimers were identified with monomers oriented such that the newly synthesized cellulose chains project toward the cell membrane. In these models, the class-specific region is found at the periphery of the complex, and the plant-conserved region forms the base of the trimer. This study strongly supports the "hexamer of trimers" model for the rosette cellulose synthesis complex that synthesizes an 18-chain cellulose microfibril as its fundamental product. © 2016 American Society of Plant Biologists. All Rights Reserved.

A Structural Study of CESA1 Catalytic Domain of Arabidopsis Cellulose Synthesis Complex: Evidence for CESA Trimers1

PubMed Central

Zhang, Qiu; Petridis, Loukas; Nixon, B. Tracy; Haigler, Candace H.; Kalluri, Udaya; Coates, Leighton; Smith, Jeremy C.; Meiler, Jens

2016-01-01

A cellulose synthesis complex with a “rosette” shape is responsible for synthesis of cellulose chains and their assembly into microfibrils within the cell walls of land plants and their charophyte algal progenitors. The number of cellulose synthase proteins in this large multisubunit transmembrane protein complex and the number of cellulose chains in a microfibril have been debated for many years. This work reports a low resolution structure of the catalytic domain of CESA1 from Arabidopsis (Arabidopsis thaliana; AtCESA1CatD) determined by small-angle scattering techniques and provides the first experimental evidence for the self-assembly of CESA into a stable trimer in solution. The catalytic domain was overexpressed in Escherichia coli, and using a two-step procedure, it was possible to isolate monomeric and trimeric forms of AtCESA1CatD. The conformation of monomeric and trimeric AtCESA1CatD proteins were studied using small-angle neutron scattering and small-angle x-ray scattering. A series of AtCESA1CatD trimer computational models were compared with the small-angle x-ray scattering trimer profile to explore the possible arrangement of the monomers in the trimers. Several candidate trimers were identified with monomers oriented such that the newly synthesized cellulose chains project toward the cell membrane. In these models, the class-specific region is found at the periphery of the complex, and the plant-conserved region forms the base of the trimer. This study strongly supports the “hexamer of trimers” model for the rosette cellulose synthesis complex that synthesizes an 18-chain cellulose microfibril as its fundamental product. PMID:26556795

A Structural Study of CESA1 Catalytic Domain of Arabidopsis Cellulose Synthesis Complex: Evidence for CESA Trimers

DOE PAGES

Vandavasi, Venu Gopal; Putnam, Daniel K.; Zhang, Qiu; ...

2015-11-10

In a cellulose synthesis complex a "rosette" shape is responsible for the synthesis of cellulose chains and their assembly into microfibrils within the cell walls of land plants and their charophyte algal progenitors. The number of cellulose synthase proteins in this large multisubunit transmembrane protein complex and the number of cellulose chains in a microfibril have been debated for many years. Our work reports a low resolution structure of the catalytic domain of CESA1 from Arabidopsis (Arabidopsis thaliana; AtCESA1CatD) determined by small-angle scattering techniques and provides the first experimental evidence for the self-assembly of CESA into a stable trimer inmore » solution. The catalytic domain was overexpressed in Escherichia coli, and using a two-step procedure, it was possible to isolate monomeric and trimeric forms of AtCESA1CatD. Moreover, the conformation of monomeric and trimeric AtCESA1CatD proteins were studied using small-angle neutron scattering and small-angle x-ray scattering. A series of AtCESA1CatD trimer computational models were compared with the small-angle x-ray scattering trimer profile to explore the possible arrangement of the monomers in the trimers. Several candidate trimers were identified with monomers oriented such that the newly synthesized cellulose chains project toward the cell membrane. In these models, the class-specific region is found at the periphery of the complex, and the plant-conserved region forms the base of the trimer. Finally, this study strongly supports the "hexamer of trimers" model for the rosette cellulose synthesis complex that synthesizes an 18-chain cellulose microfibril as its fundamental product.« less

On the role of block copolymer additives for calcium carbonate crystallization: small angle neutron scattering investigation by applying contrast variation.

PubMed

Endo, Hitoshi; Schwahn, Dietmar; Cölfen, Helmut

2004-05-15

The role of the double-hydrophilic block copolymer poly(ethylen glycol)-block-poly(methacrylic acid) (PEG-b-PMAA) on the morphogenesis of calcium carbonate (CaCO3) was studied by applying the contrast variation small angle neutron scattering technique. The morphology and size of CaCO3 crystals is strongly affected by the addition of PEG-b-PMAA. In order to determine the partial scattering functions of the polymer and CaCO3 mineral, we developed both an experimental and theoretical approach with a sophisticated method of their determination from the scattering intensity. Partial scattering functions give detailed information for each component. In particular, the partial scattering function of the polymer, Spp, shows a monotonic slope with Q(-2 to -3) where the scattering vector Q is low (Q < 0.01 Angstrom(-1)), which is a clear evidence that the polymer within the CaCO3 mineral has a mass fractal dimension. The other partial scattering functions reflected the geometry of the CaCO3 particles or the "interaction" of polymer and CaCO3 on a microscopic scale, which leads to a coherent view with Spp.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Perkins, Stephen J.; Wright, David W.; Zhang, Hailiang

2016-10-14

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-artmore » 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 whichGenAppprovides the deployment infrastructure for running applications on both standard and high-performance computing hardware, andSASSIEprovides 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.GenAppproduces the accessible web-based front end termedSASSIE-web, andGenAppandSASSIEalso 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.« less

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.

Sodium deoxycholate mediated enhanced solubilization and stability of hydrophobic drug Clozapine in pluronic micelles

NASA Astrophysics Data System (ADS)

Singla, Pankaj; Singh, Onkar; Chabba, Shruti; Aswal, V. K.; Mahajan, Rakesh Kumar

2018-02-01

In this report, the solubilization behaviour of a hydrophobic drug Clozapine (CLZ) in micellar suspensions of pluronics having different hydrophilic lipophilic balance (HLB) ratios viz. P84, F127 and F108 in the absence and presence of bile salt sodium deoxycholate (SDC) has been studied. UV-Vis spectroscopy has been exploited to determine the solubilization capacity of the investigated micellar systems in terms of drug loading efficiency, average number of drug molecules solubilized per micelle (ns), partition coefficient (P) and standard free energy of solubilization (Δ G°). The morphological and structural changes taking place in pluronics in different concentration regimes of SDC and with the addition of drug CLZ has been explored using dynamic light scattering (DLS) and small angle neutron scattering (SANS) measurements. The SANS results revealed that aggregation behaviour of pluronic-SDC mixed micelles gets improved in the presence of drug. The micropolarity measurements have been performed to shed light on the locus of solubilization of the drug in pure and mixed micellar systems. The compatibility between CLZ and drug carriers (pluronics and SDC) was confirmed using powder X-ray diffraction (PXRD) and Fourier transform infrared spectroscopy (FTIR) techniques. Among the investigated systems, P84-SDC mixed system was found to be highly efficient for CLZ loading. The long term stability data indicated that CLZ loaded P84-SDC mixed micellar formulation remained stable for 3 months at room temperature. Further, it was revealed that the CLZ loaded P84-SDC mixed micelles are converted into CLZ loaded pure P84 micelles at 30-fold dilutions which remain stable up to 48-fold dilutions. The results from the present studies suggest that P84-SDC mixed micelles can serve as suitable delivery vehicles for hydrophobic drug CLZ.

SAXS and other spectroscopic analysis of 12S cruciferin isolated from the seeds of Brassica nigra

NASA Astrophysics Data System (ADS)

Khaliq, Binish; Falke, Sven; Negm, Amr; Buck, Friedrich; Munawar, Aisha; Saqib, Maria; Mahmood, Seema; Ahmad, Malik Shoaib; Betzel, Christian; Akrem, Ahmed

2017-06-01

Oilseeds of the plant family Brassicaceae are important for providing both lipid and protein contents to human nutrition. Cruciferins (12S globulins) are seed storage proteins, which are getting attention due to their allergenic and pathogenicity related nature. This study describes the purification and characterization of a trimeric (∼190 kDa) cruciferin protein from the seeds of Brassica nigra (L.). Cruciferin was first partially purified by ammonium sulfate precipitation (30% saturation constant) and further purified by size exclusion chromatography. The N-terminal amino-acid sequence analysis showed 82% sequence homology with cruciferin from Arabidopsis thaliana. The 50-55 kDa monomeric cruciferin produced multiple bands of two major molecular weight ranges (α-polypeptides of 28-32 kDa and β-polypeptides of 17-20 kDa) under reduced conditions of SDS-PAGE. The 2D gel electrophoretic analysis showed the further separation of the bands into their isoforms with major pI ranges between 5.7 and 8.0 (α-polypeptides) and 5.5-8.5 (β-polypeptides). The Dynamic Light Scattering (DLS) showed the monodisperse nature of the cruciferin with hydrodynamic radius of 5.8 ± 0.1 nm confirming the trimeric nature of the protein. The Circular Dichroism (CD) spectra showed both α-helices and β-sheets in the native conformation of the trimeric protein. The pure cruciferin protein (40 mg/ml) was successfully crystallized; however, the crystals diffracted only to low resolution data (8 Å). Small-angle x-ray scattering (SAXS) was applied to gain insights into the three-dimensional structure in solution. SAXS showed that the radius of gyration is 4.24 ± 0.25 nm and confirmed the nearly globular shape. The SAXS based ab initio dummy model of B. nigra cruciferin was compared with 11S globulins.

Preparation, characterization, and in vitro activity evaluation of triblock copolymer-based polymersomes for drugs delivery

NASA Astrophysics Data System (ADS)

Besada, Lucas N.; Peruzzo, Pablo; Cortizo, Ana M.; Cortizo, M. Susana

2018-03-01

Polymersomes are polymer-based vesicles that form upon hydration of amphiphilic block copolymers and display high stability and durability, due to their mechanical and physical properties. They have hydrophilic reservoirs as well as thick hydrophobic membranes; allowing to encapsulate both water-soluble bioactive agent and hydrophobic drugs. In this study, poly ethylene glycol (PEG3350 and PEG6000) were used as hydrophilic part and poly(vinyl benzoate) (PVBz) as hydrophobic block to synthesize amphiphilic triblock copolymers (PVBz- b-PEG- b-PVBz). Different proportions of hydrophilic/hydrophobic part were assayed in order to obtain polymersomes by solvent injection method. For the synthesis of the copolymers, the initial block of PEG was derived to obtain a macroinitiator through a xanthate functional group (PEGX3 or PEGX6) and the polymerization of vinyl benzoate was carried out through reversible addition-fragmentation chain transfer polymerization (RAFT). The structure of PEGX and copolymers was confirmed by Infrared, 1H-NMR and UV-Vis spectrometry, while the average molecular weight (Mw) and polydispersity index (PI) were determined by size exclusion chromatography (SEC). The structures adopted by the copolymers in aqueous solution by self-assembly were investigated using transmission electron microscopy (TEM), dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS). Both techniques confirm that polymersomes were obtained for a fraction of hydrophilic block ( f) ≈ 35 ± 10%, with a diameter of 38.3 ± 0.3 nm or 22.5 ± 0.7 nm, as determined by TEM and according to the M w of the precursor block copolymer. In addition, we analyzed the possible cytotoxicity in view of its potential application as biomedical nanocarrier. The results suggest that polymersomes seem not induce cytotoxicity during the periods of time tested.

Lanthanide Oleates: Chelation, Self-assembly, and Exemplification of Ordered Nanostructured Colloidal Contrast Agents for Medical Imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Guozhen; Conn, Charlotte E.; Drummond, Calum J.

2010-01-12

Eight lanthanide(III) oleates have been prepared and characterized. The chelation and self-assembly structures of these rare-earth oleates have been studied by elemental analysis, Fourier transfer infrared spectroscopy (FTIR), and X-ray powder diffraction (XRD) analysis. Elemental analysis and FTIR results indicate that three oleate anions are complexed with one lanthanide cation and, with the exception of anhydrous cerium(III) oleate, form either a mono- or a hemihydrate. The X-ray analysis showed that the neat lanthanide soaps have a lamellar bilayer structure at room temperature. The thermal behavior has been investigated by cross-polarized optical microscopy (POM), differential scanning calorimetry (DSC), and thermogravimetric analysismore » (TGA). POM scans showed that all the lanthanide oleates form a lamellar phase in the presence of excess water. Small-angle X-ray scattering (SAXS) and XRD were used to investigate the internal structure of the bulk lanthanide oleates in excess water, and these X-ray results confirmed that the lanthanide oleates do not swell in water. Select lanthanide oleates were dispersed in water to form nonswelling lamellar submicrometer particles, confirmed by dynamic light scattering (DLS) and synchrotron SAXS measurements. NMR results indicated that colloidal dispersions of lanthanide oleates containing paramagnetic ions, such as gadolinium(III), terbium(III), and dysprosium(III), have a significant effect on the longitudinal (T{sub 1}) and transverse (T{sub 2}) relaxation times of protons in water. Time-resolved fluorescence measurements have demonstrated that colloidal dispersions of europium(III) oleate exhibit strong luminescence. The rare earth metal soaps exemplify the potential of self-assembled chelating amphiphiles as contrast agents in medical imaging modalities such as magnetic resonance imaging (MRI) and fluorescence imaging.« less

Dynamic light scattering for the characterization and counting of extracellular vesicles: a powerful noninvasive tool

NASA Astrophysics Data System (ADS)

Palmieri, Valentina; Lucchetti, Donatella; Gatto, Ilaria; Maiorana, Alessandro; Marcantoni, Margherita; Maulucci, Giuseppe; Papi, Massimiliano; Pola, Roberto; De Spirito, Marco; Sgambato, Alessandro

2014-09-01

Extracellular vesicles (EVs) are cell-to-cell shuttles that have recently drawn interest both as drug delivery platforms and disease biomarkers. Despite the increasingly recognized relevance of these vesicles, their detection, and characterization still have several technical drawbacks. In this paper, we accurately assess the size distribution and concentration of EVs by using a high-throughput non-perturbative technique such as Dynamic Light Scattering (DLS). The vesicle radii distribution, as further confirmed by Atomic Force Microscopy experiments, ranges from 10 to 80 nm and appears very asymmetric towards larger radii with a main peak at roughly 30 nm. By combining DLS and Bradford assay, we also demonstrate the feasibility of recovering the concentration and its distribution of proteins contained inside vesicles. The sensitivity of our approach allows to detect protein concentrations as low as 0.01 mg/ml.

Online submicron particle sizing by dynamic light scattering using autodilution

NASA Technical Reports Server (NTRS)

Nicoli, David F.; Elings, V. B.

1989-01-01

Efficient production of a wide range of commercial products based on submicron colloidal dispersions would benefit from instrumentation for online particle sizing, permitting real time monitoring and control of the particle size distribution. Recent advances in the technology of dynamic light scattering (DLS), especially improvements in algorithms for inversion of the intensity autocorrelation function, have made it ideally suited to the measurement of simple particle size distributions in the difficult submicron region. Crucial to the success of an online DSL based instrument is a simple mechanism for automatically sampling and diluting the starting concentrated sample suspension, yielding a final concentration which is optimal for the light scattering measurement. A proprietary method and apparatus was developed for performing this function, designed to be used with a DLS based particle sizing instrument. A PC/AT computer is used as a smart controller for the valves in the sampler diluter, as well as an input-output communicator, video display and data storage device. Quantitative results are presented for a latex suspension and an oil-in-water emulsion.

Exact Rayleigh scattering calculations for use with the Nimbus-7 Coastal Zone Color Scanner.

PubMed

Gordon, H R; Brown, J W; Evans, R H

1988-03-01

For improved analysis of Coastal Zone Color Scanner (CZCS) imagery, the radiance reflected from a planeparallel atmosphere and flat sea surface in the absence of aerosols (Rayleigh radiance) has been computed with an exact multiple scattering code, i.e., including polarization. The results indicate that the single scattering approximation normally used to compute this radiance can cause errors of up to 5% for small and moderate solar zenith angles. At large solar zenith angles, such as encountered in the analysis of high-latitude imagery, the errors can become much larger, e.g.,>10% in the blue band. The single scattering error also varies along individual scan lines. Comparison with multiple scattering computations using scalar transfer theory, i.e., ignoring polarization, show that scalar theory can yield errors of approximately the same magnitude as single scattering when compared with exact computations at small to moderate values of the solar zenith angle. The exact computations can be easily incorporated into CZCS processing algorithms, and, for application to future instruments with higher radiometric sensitivity, a scheme is developed with which the effect of variations in the surface pressure could be easily and accurately included in the exact computation of the Rayleigh radiance. Direct application of these computations to CZCS imagery indicates that accurate atmospheric corrections can be made with solar zenith angles at least as large as 65 degrees and probably up to at least 70 degrees with a more sensitive instrument. This suggests that the new Rayleigh radiance algorithm should produce more consistent pigment retrievals, particularly at high latitudes.

Optical properties of randomly distributed soot: improved polarimetric and intensity scattering functions

NASA Astrophysics Data System (ADS)

Renard, Jean-Baptiste; Daugeron, Daniel; Personne, Pascal; Legros, Guillaume; Baillargeat, Jacques; Hadamcik, Edith; Worms, Jean-Claude

2005-02-01

Reference scattering curves for polarization and intensity produced by aggregates and agglomerates of ethylene and kerosene soot are obtained for scattering angles in the 10-170° range. The polarization measurements were obtained with the Propriétés Optiques des Grains Astronomiques et Atmosphèriques instrument for particles that levitate in microgravity during parabolic flights and on the ground by an air draught technique. The intensity measurements were obtained also on the ground with a Laboratoire de Metéorologie Physique nephelometer. The maximum polarization is of the order of 80% at a scattering angle of 80° at lambda = 632.8 nm and approximately 75% at an angle of 90° at lambda = 543.5 nm. The polarization increases by approximately 10% when the size of the agglomerate increases from 10 μm to a few hundred micrometers. The intensity curve exhibits a strong increase at small scattering angles. These reference curves will be used in the near future for the detection of stratospheric soot by remote-sensing measurement techniques.

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.

Clinical Detection of Pre-Cataractous Lens Protein Changes using Dynamic Light Scattering

PubMed Central

Datiles, Manuel B.; Ansari, Rafat R.; Suh, Kwang I.; Vitale, Susan; Reed, George F.; Zigler, J. Samuel; Ferris., Frederick L.

2008-01-01

Purpose To use Dynamic Light Scattering (DLS) to clinically assess early pre-cataractous lens protein changes. Methods We performed a cross sectional study in 380 eyes of 235 subjects aged 7–86 years with AREDS clinical lens nuclear grades ranging from 0–3.8. A DLS device was used to assess α-crystallin, a molecular chaperone protein shown to bind other damaged lens proteins, preventing their aggregation. The outcome measure was the α-crystallin index (ACI), a measure of unbound α-crystallin in each lens. The association of ACI with increasing nuclear opacity and aging was determined. Results There was a significant decrease in ACI associated with increasing grades of lens nuclear opacity (p<0.0001). There are significant losses of α-crystallin even in clinically clear lenses associated with aging (p<0.0001). The standard error of measurement was 3%. Conclusions DLS clinically detects loss of α-crystallin proteins even in clinically clear lenses. ACI measurements may be useful in identifying patients at high risk for developing cataract, and as an outcome variable in clinical lens studies. Clinical Relevance Our studies suggest that the ACI may be a useful measure of the protective α-crystallin molecular chaperone reserve present in a lens, analogous to creatinine clearance in estimating renal function reserve. PMID:19064850

Solitary waves and double layers in a dusty electronegative plasma.

PubMed

Mamun, A A; Shukla, P K; Eliasson, B

2009-10-01

A dusty electronegative plasma containing Boltzmann electrons, Boltzmann negative ions, cold mobile positive ions, and negatively charged stationary dust has been considered. The basic features of arbitrary amplitude solitary waves (SWs) and double layers (DLs), which have been found to exist in such a dusty electronegative plasma, have been investigated by the pseudopotential method. The small amplitude limit has also been considered in order to study the small amplitude SWs and DLs analytically. It has been shown that under certain conditions, DLs do not exist, which is in good agreement with the experimental observations of Ghim and Hershkowitz [Y. Ghim (Kim) and N. Hershkowitz, Appl. Phys. Lett. 94, 151503 (2009)].

Laboratory-Based BRDF Calibration of Radiometric Tarps

NASA Technical Reports Server (NTRS)

Georgiev, Georgi T.; Butler, James J.

2007-01-01

The current study provides the remote sensing community with important high accuracy laboratory-based BRDF calibration of radiometric tarps. The results illustrate the dependence of tarps' weft and warp threads orientation on BRDF. The study was done at incident angles of 0deg, 10deg, and 30deg; scatter zenith angles from 0deg to 60deg, and scatter azimuth angles of 0deg, 45deg, 90deg, 135deg, and 180deg. The wavelengths were 485nm, 550nm, 633nm and 800nm. The dependence is well defined at all measurement geometries and wavelengths. It can be as high as 8% at 0deg incident angle and 2% at 30deg incident angle. The fitted BRDF data show a very small discrepancy from the measured ones. New data on the forward and backscatter properties of radiometric tarps is reported. The backward scatter is well pronounced for the white samples. The black sample has well pronounced forward scatter. The BRDF characterization of radiometric tarps can be successfully extended to other structured surface fabric samples. The results are NIST traceable.

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.

Direct Observation Of Nanoparticle-Surfactant Interactions Using Small Angle Neutron Scattering

NASA Astrophysics Data System (ADS)

Kumar, Sugam; Aswal, V. K.

2010-12-01

Interactions of anionic silica nanoparticles with anionic, cationic and nonionic surfactants have directly been studied by contrast variation small angle neutron scattering (SANS). The measurements are performed on 1 wt% of both silica nanoparticles and surfactants of anionic sodium dodecyle sulphate (SDS), cationic dodecyltrimethyl ammonium bromide (DTAB) and non-ionic polyoxyethylene 10 lauryl ether (C12E10) in aqueous solution. We show that there is no direct interaction in the case of SDS with silica particles, whereas strong interaction for DTAB leads to the aggregation of silica particles. The interaction of C12E10 is found through the micelles adsorbed on the silica particles.

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

PubMed

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

2017-12-01

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

Small-angle neutron scattering study of recombinant yeast-derived human hepatitis B virus surface antigen vaccine particle

NASA Astrophysics Data System (ADS)

Sato, M.; Ito, Y.; Kameyama, K.; Imai, M.; Ishikawa, N.; Takagi, T.

1995-02-01

The overall and internal structure of recombinant yeast-derived human hepatitis B virus surface antigen vaccine particles was investigated by small-angle neutron scattering using the contrast variation method. The vaccine is a nearly spherical particle, and its contrast-matching point was determined to be at about 24% D 2O content, indicating that a large part of the vaccine particle is occupied by lipids and carbohydrates from the yeast. The Stuhrmann plot suggests that the surface antigens exist predominantly in the peripheral region of the particle, which is favorable to the induction of anti-virus antibodies.

Photoluminescence studies on Cd(1-x)Zn(x)S:Mn2+ nanocrystals.

PubMed

Sethi, Ruchi; Kumar, Lokendra; Pandey, A C

2009-09-01

Highly monodispersed, undoped and doped with Mn2+, binary and ternary (CdS, ZnS, Cd(1-x)Zn(x)S) compound semiconductor nanocrystals have been synthesized by co-precipitation method using citric acid as a stabilizer. As prepared sample are characterized by X-ray diffraction, Small angle X-ray scattering, Transmission electron microscope, Optical absorption and Photoluminescence spectroscopy, for their optical and structural properties. X-ray diffraction, Small angle X-ray scattering and Transmission electron microscope results confirm the preparation of monodispersed nanocrystals. Photoluminescence studies show a significant blue shift in the wavelength with an increasing concentration of Zn in alloy nanocrystals.

Use of Small Angle Neutron Scattering to Study Various Properties of Wool and Mohair Fibres

DOE Office of Scientific and Technical Information (OSTI.GOV)

Franklyn, C. B.; Toeroek, Gy.

2011-12-13

To maintain a competitive edge in the wool and mohair industry, a detailed knowledge and understanding of the properties of wool fibres is essential. Standard techniques are used to determine fibre diameter, length and strength; however, properties such as hydroscopicity, lustre and changes in fibre structure following chemical or mechanical treatment are not so well understood. The unique capabilities of small angle neutron scattering to study changes in the supermolecular structure of wool fibres, particularly at the level of the microfibril-matrix complex, have been used to provide previously unknown features of the fibres. The results of these studies are presented.

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)

Mean-field Ising crossover and the critical exponents γ, ν, and η for a polymer blend: d-PB/PS studied by small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Janssen, S.; Schwahn, D.; Springer, T.

1992-05-01

The critical behavior of the polymer blend d-PB/PS was investigated by small-angle neutron scattering experiments. 3D Ising behavior was clearly observed with the critical exponents γ=1.26+/-0.01, ν=0.59+/-0.01, and η=0.047+/-0.004. The crossover to mean-field behavior occurs at T*=Tc+5.4 K. This is compared with the results of other experiments and the Landau-Ginzburg criterion. The Q dependence of the structure factor S(Q) follows the Ornstein-Zernike form in both regimes.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Zhen; Chen, Xiaowei; Meng, Lingpu

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.more » 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.« less

Multiple image x-radiography for functional lung imaging

NASA Astrophysics Data System (ADS)

Aulakh, G. K.; Mann, A.; Belev, G.; Wiebe, S.; Kuebler, W. M.; Singh, B.; Chapman, D.

2018-01-01

Detection and visualization of lung tissue structures is impaired by predominance of air. However, by using synchrotron x-rays, refraction of x-rays at the interface of tissue and air can be utilized to generate contrast which may in turn enable quantification of lung optical properties. We utilized multiple image radiography, a variant of diffraction enhanced imaging, at the Canadian light source to quantify changes in unique x-ray optical properties of lungs, namely attenuation, refraction and ultra small-angle scatter (USAXS or width) contrast ratios as a function of lung orientation in free-breathing or respiratory-gated mice before and after intra-nasal bacterial endotoxin (lipopolysaccharide) instillation. The lung ultra small-angle scatter and attenuation contrast ratios were significantly higher 9 h post lipopolysaccharide instillation compared to saline treatment whereas the refraction contrast decreased in magnitude. In ventilated mice, end-expiratory pressures result in an increase in ultra small-angle scatter contrast ratio when compared to end-inspiratory pressures. There were no detectable changes in lung attenuation or refraction contrast ratio with change in lung pressure alone. In effect, multiple image radiography can be applied towards following optical properties of lung air-tissue barrier over time during pathologies such as acute lung injury.

Flow-through compression cell for small-angle and ultra-small-angle neutron scattering measurements

NASA Astrophysics Data System (ADS)

Hjelm, Rex P.; Taylor, Mark A.; Frash, Luke P.; Hawley, Marilyn E.; Ding, Mei; Xu, Hongwu; Barker, John; Olds, Daniel; Heath, Jason; Dewers, Thomas

2018-05-01

In situ measurements of geological materials under compression and with hydrostatic fluid pressure are important in understanding their behavior under field conditions, which in turn provides critical information for application-driven research. In particular, understanding the role of nano- to micro-scale porosity in the subsurface liquid and gas flow is critical for the high-fidelity characterization of the transport and more efficient extraction of the associated energy resources. In other applications, where parts are produced by the consolidation of powders by compression, the resulting porosity and crystallite orientation (texture) may affect its in-use characteristics. Small-angle neutron scattering (SANS) and ultra SANS are ideal probes for characterization of these porous structures over the nano to micro length scales. Here we show the design, realization, and performance of a novel neutron scattering sample environment, a specially designed compression cell, which provides compressive stress and hydrostatic pressures with effective stress up to 60 MPa, using the neutron beam to probe the effects of stress vectors parallel to the neutron beam. We demonstrate that the neutron optics is suitable for the experimental objectives and that the system is highly stable to the stress and pressure conditions of the measurements.

Surface areas of fractally rough particles studied by scattering

NASA Astrophysics Data System (ADS)

Hurd, Alan J.; Schaefer, Dale W.; Smith, Douglas M.; Ross, Steven B.; Le Méhauté, Alain; Spooner, Steven

1989-05-01

The small-angle scattering from fractally rough surfaces has the potential to give information on the surface area at a given resolution. By use of quantitative neutron and x-ray scattering, a direct comparison of surface areas of fractally rough powders was made between scattering and adsorption techniques. This study supports a recently proposed correction to the theory for scattering from fractal surfaces. In addition, the scattering data provide an independent calibration of molecular adsorbate areas.

Small angle x ray scattering studies of reverse micelles in supercritical fluids

NASA Astrophysics Data System (ADS)

Pfund, D. M.; Fulton, J. L.

1994-10-01

The nature of aggregates formed in a supercritical fluid determines its solvent power and selectivity. Small angle X ray scattering (SAXS) is a powerful tool for studying the properties of aggregates with sizes in the 10(angstrom) to 200(angstrom) range. It is also useful in studying those interparticle interactions which operate over a similar distance. The authors have used SAXS to examine the aggregates formed in pure fluids, in mixtures and in fluid/surfactant/water systems. The scattered intensity as a function of angle depends on the geometry, polydispersity, X ray contrast, and interaction strength of the particles as well as on the phase behavior of the system. In this paper the authors present the results of modeling the X-ray scattering from AOT/water reverse micelles in supercritical propane and in propane/carbon dioxide mixtures. They examine the effect of dilution with CO2 anti-solvent on the phase behavior of the system and on the strength of intermicellar attractions. A better understanding of these systems must be obtained before the applications of supercritical reverse micelle systems to extractions, reactions, and enhanced oil recovery can be fully developed.

Scattering of fast electrons by vapour-atoms and by solid-atoms - A comparison

DOE Office of Scientific and Technical Information (OSTI.GOV)

Joshipura, K.N.; Mohanan, S.

1988-08-01

A comparative theoretical study has been done on the scattering of fast electrons by free (vapour) atoms and bound (solid) atoms, in particular, the alkali atoms, Al and Cu. The Born differential cross-sections (DCS), calculated with the static plus polarization electron-atom potential, are found in general, to be larger for free atoms that for bound atoms, at least at small angles of scattering. For Rb and Cs the two DCS tend to merge at very large angles only. The sample incident energies chosen are 400 eV and above.

Early detection of cataract and response to pantethine therapy with non-invasive static and dynamic light scattering

NASA Astrophysics Data System (ADS)

Ansari, Rafat R.; King, James F.; Seeberger, Teri; Clark, John I.

2003-07-01

Cataractogenesis is a risk factor for space travelers. Here on earth, half of all blindness is due to cataracts. At this time, the only known treatment is surgical removal of the lens. In this paper, we present static and dynamic light scattering (DLS) measurements of early onset of cataract before it has any effect on vision and to test the effectiveness of pantethine as an anticataract agent in reversing cataracts. In this preliminary study, experiments were conducted on 12 rodents. Static measurements were performed by scanning the animal eye (cornea to retina) at a laser power of 80 microwatts to collect photons or scattered intensity in steps of 10 microns. The rodents studied were control, selenite injected, and selenite plus pantethine injected. Selenite was used to induce cataracts. Static and dynamic changes (increase in light scatter and crystalline size) in the lenses are quantitatively measured as early as 1 day post selenite injections. Scattering intensity and DLS measurements from lenses of animals administered pantethine resembled controls. These subtle molecular changes are not noticeable when the animals are examined with conventional ophthalmic instruments because their lenses remain transparent. Acknowledgements: Technical support from C.Ganders, University of Washington, Seattle, NEI research grant EY04542 (JIC) and support under a NASA-NEI/NIH interagency agreement (RRA) are greatly appreciated. JFK works for QSS Inc. at NASA GRC.

Structural studies of Neurospora crassa LPMO9D and redox partner CDHIIA using neutron crystallography and small-angle scattering.

PubMed

Bodenheimer, Annette M; O'Dell, William B; Stanley, Christopher B; Meilleur, Flora

2017-08-07

Sensitivity to hydrogen/deuterium and lack of observable radiation damage makes cold neutrons an ideal probe the structural studies of proteins with highly photosensitive groups such as the copper center of lytic polysaccharide monooxygenases (LPMOs) and flavin adenine dinucleotide (FAD) and heme redox cofactors of cellobiose dehydrogenases (CDHs). Here, neutron crystallography and small-angle neutron scattering are used to investigate Neurospora crassa LPMO9D (NcLPMO9D) and CDHIIA (NcCDHIIA), respectively. The presence of LPMO greatly enhances the efficiency of commercial glycoside hydrolase cocktails in the depolymerization of cellulose. LPMOs can receive electrons from CDHs to activate molecular dioxygen for the oxidation of cellulose resulting in chain cleavage and disruption of local crystallinity. Using neutron protein crystallography, the hydrogen/deuterium atoms of NcLPMO9D could be located throughout the structure. At the copper active site, the protonation states of the side chains of His1, His84, His157 and Tyr168, and the orientation of water molecules could be determined. Small-angle neutron scattering measurements provided low resolution models of NcCDHIIA with both the dehydrogenase and cytochrome domains in oxidized states that exhibited elongated conformations. This work demonstrates the suitability of neutron diffraction and scattering for characterizing enzymes critical to oxidative cellulose deconstruction. Copyright © 2017 Elsevier Ltd. All rights reserved.

X-ray studies of dynamic aging in an aluminum alloy subjected to severe plastic deformation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sitdikov, V.D., E-mail: svil@mail.rb.ru; Laboratory for Mechanics of Bulk Nanomaterials, Saint Petersburg State University, 28 Universitetsky pr., Saint Petersburg 198504; Chizhov, P.S.

In this work, X-ray scattering methods were applied for a quantitative characterization of the microstructure of an aluminum alloy of the Al–Mg–Si system during dynamic aging realized through the high pressure torsion technique. A qualitative and quantitative phase analysis of the alloy was performed, together with Al alloy lattice parameter determination. From the reflections broadening the effective size of the coherent scattering domains and the lattice microstrain were determined in the framework of the Halder–Wagner approach. Using the method of small-angle X-ray scattering, the quantitative characteristics of the size, shape and spatial distribution of the secondary phase particles formed inmore » the Al alloy during dynamic aging were established. In order to validate the obtained results, the method of small-angle X-ray scattering was preliminarily tested on similar samples after artificial aging and compared with the results from small-angle neutron diffraction widely known in literature. - Highlights: • Spherical fcc β-Mg2Si precipitates formed in Al 6201 alloy during dynamic aging in the course of severe plastic deformation. • The size, shape and distribution of the precipitates due to artificial and dynamic aging were revealed by SAXS method. • Monoclinic needle-like β' precipitates and Al5FeSi intermetallic phase were detected in 6201 alloy after T6 treatment.« less

Structural studies of Neurospora crassa LPMO9D and redox partner CDHIIA using neutron crystallography and small-angle scattering

DOE PAGES

Bodenheimer, Annette M.; O'Dell, William B.; Stanley, Christopher B.; ...

2017-03-04

Sensitivity to hydrogen/deuterium and lack of observable radiation damage makes cold neutrons an ideal probe the structural studies of proteins with highly photosensitive groups such as the copper center of lytic polysaccharide monooxygenases (LPMOs) and flavin adenine dinucleotide (FAD) and heme redox cofactors of cellobiose dehydrogenases (CDHs). In this paper, neutron crystallography and small-angle neutron scattering are used to investigate Neurospora crassa LPMO9D (NcLPMO9D) and CDHIIA (NcCDHIIA), respectively. The presence of LPMO greatly enhances the efficiency of commercial glycoside hydrolase cocktails in the depolymerization of cellulose. LPMOs can receive electrons from CDHs to activate molecular dioxygen for the oxidation ofmore » cellulose resulting in chain cleavage and disruption of local crystallinity. Using neutron protein crystallography, the hydrogen/deuterium atoms of NcLPMO9D could be located throughout the structure. At the copper active site, the protonation states of the side chains of His1, His84, His157 and Tyr168, and the orientation of water molecules could be determined. Small-angle neutron scattering measurements provided low resolution models of NcCDHIIA with both the dehydrogenase and cytochrome domains in oxidized states that exhibited elongated conformations. Finally, this work demonstrates the suitability of neutron diffraction and scattering for characterizing enzymes critical to oxidative cellulose deconstruction.« less

Structural studies of Neurospora crassa LPMO9D and redox partner CDHIIA using neutron crystallography and small-angle scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bodenheimer, Annette M.; O'Dell, William B.; Stanley, Christopher B.

Sensitivity to hydrogen/deuterium and lack of observable radiation damage makes cold neutrons an ideal probe the structural studies of proteins with highly photosensitive groups such as the copper center of lytic polysaccharide monooxygenases (LPMOs) and flavin adenine dinucleotide (FAD) and heme redox cofactors of cellobiose dehydrogenases (CDHs). In this paper, neutron crystallography and small-angle neutron scattering are used to investigate Neurospora crassa LPMO9D (NcLPMO9D) and CDHIIA (NcCDHIIA), respectively. The presence of LPMO greatly enhances the efficiency of commercial glycoside hydrolase cocktails in the depolymerization of cellulose. LPMOs can receive electrons from CDHs to activate molecular dioxygen for the oxidation ofmore » cellulose resulting in chain cleavage and disruption of local crystallinity. Using neutron protein crystallography, the hydrogen/deuterium atoms of NcLPMO9D could be located throughout the structure. At the copper active site, the protonation states of the side chains of His1, His84, His157 and Tyr168, and the orientation of water molecules could be determined. Small-angle neutron scattering measurements provided low resolution models of NcCDHIIA with both the dehydrogenase and cytochrome domains in oxidized states that exhibited elongated conformations. Finally, this work demonstrates the suitability of neutron diffraction and scattering for characterizing enzymes critical to oxidative cellulose deconstruction.« less

A new detector for low Pt physics

NASA Astrophysics Data System (ADS)

Da Via, C.; DeSalvo, R.; Lundin, M.; Mondardini, M. R.; Orear, J.; Shimizu, T.; Shinji, O.

1992-12-01

Elastic pp (or poverlinep) scattering at microradian angles provides a measurement of the total pp (or poverlinep) cross sectio elastic scattering cross section with t (the square of the momentum transfer) and the ratio of real to imaginary scattering amplitudes, as well as an absolute luminosity calibration. A detector is proposed which can measure elastic scattering and small angle processes which are usually missed by a typical 4π detector. The detector consists of a bundle of scintillating fibers. Images from these fibers are transported via glass fiber optics and intensified with two proximity focused image intensifiers. Images are then reduced via an image taper and read out with a charge coupled device (CCD).

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

NASA Astrophysics Data System (ADS)

Nepal, Prakash; Saldin, D. K.

2018-05-01

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

Changes in small angle X-ray scattering parameters observed upon ligand binding to rabbit muscle pyruvate kinase are not correlated with allosteric transitions†

PubMed Central

Fenton, Aron W.; Williams, Rachel; Trewhella, Jill

2010-01-01

Protein fluorescence and small-angle X-ray scattering (SAXS) have been used to monitor effector affinity and conformational changes previously associated with allosteric regulation in rabbit muscle pyruvate kinase (M1-PYK). In the absence of substrate (phosphoenolpyruvate; PEP), SAXS-monitored conformational changes in M1-PYK elicited by the binding of phenylalanine (an allosteric inhibitor that reduces the affinity of M1-PYK for PEP) are similar to those observed upon binding of alanine or 2-aminobutyric acid. Under the current assay conditions, these small amino acids bind to the protein, but elicit a minimal change in the affinity of the protein for PEP. Therefore, if changes in scattering signatures represent cleft closure via domain rotation as previously interpreted, it can be concluded that these motions are not sufficient to elicit allosteric inhibition. Additionally, although PEP has similar affinities for the free enzyme and the M1-PYK/small-amino-acid complexes (i.e. the small amino acids have minimal allosteric effects), PEP binding elicits different changes in the SAXS signature of the free enzyme vs. the M1-PYK/small-amino-acid complexes. PMID:20712377

NONLINEAR AND FIBER OPTICS: Stimulated scattering of electromagnetic radiation in thermodynamic-nonequilibrium media

NASA Astrophysics Data System (ADS)

Blinov, N. A.; Zolotkov, V. N.; Lezin, A. Yu; Cheburkin, N. V.

1990-04-01

An analysis is made of transient stimulated scattering in a vibrationally nonequilibrium gas excited by a non-self-sustained discharge. A stability theory approach is used to describe the behavior of perturbation wave packets, yielding asymptotic expressions for the maximal increments of an instability of stimulated small-angle scattering by entropic and acoustic modes.

Theory of Parabolic Arcs in Interstellar Scintillation Spectra

NASA Astrophysics Data System (ADS)

Cordes, James M.; Rickett, Barney J.; Stinebring, Daniel R.; Coles, William A.

2006-01-01

Interstellar scintillation (ISS), observed as time variation in the intensity of a compact radio source, is caused by small-scale structure in the electron density of the interstellar plasma. Dynamic spectra of ISS show modulation in radio frequency and time. Here we relate the (two-dimensional) power spectrum of the dynamic spectrum-the secondary spectrum-to the scattered image of the source. Recent work has identified remarkable parabolic arcs in secondary spectra. Each point in a secondary spectrum corresponds to interference between points in the scattered image with a certain Doppler shift and a certain delay. The parabolic arc corresponds to the quadratic relation between differential Doppler shift and delay through their common dependence on scattering angle. We show that arcs will occur in all media that scatter significant power at angles larger than the rms angle. Thus, effects such as source diameter, steep spectra, and dissipation scales, which truncate high angle scattering, also truncate arcs. Arcs are equally visible in simulations of nondispersive scattering. They are enhanced by anisotropic scattering when the spatial structure is elongated perpendicular to the velocity. In weak scattering the secondary spectrum is directly mapped from the scattered image, and this mapping can be inverted. We discuss additional observed phenomena including multiple arcs and reverse arclets oriented oppositely to the main arc. These phenomena persist for many refractive scattering times, suggesting that they are due to large-scale density structures, rather than low-frequency components of Kolmogorov turbulence.

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

PubMed

Chen, Sen; Luo, Sheng Nian

2018-03-01

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

Polyhydroxyalkanoate-based natural synthetic hybrid copolymer films: A small-angle neutron scattering study

NASA Astrophysics Data System (ADS)

Foster, L. John R.; Knott, Robert; Sanguanchaipaiwong, Vorapat; Holden, Peter J.

2006-11-01

Polyhydroxyalkanoates have attracted attention as biodegradable alternatives to conventional thermoplastics and as biomaterials. Through modification of their biosynthesis using Pseudomonas oleovorans, we have manipulated the material properties of these biopolyesters and produced a natural-synthetic hybrid copolymer of polyhydroxyoctanoate- block-diethylene glycol (PHO- b-DEG). A mixture of PHO and PHO-DEG were solvent cast from analytical grade chloroform and analysed using small-angle neutron scattering. A scattering pattern, easily distinguished above the background, was displayed by the films with a diffraction ring at q∼0.12 Å -1. This narrow ring of intensity is suggestive of a highly ordered system. Analysis of the diffraction pattern supported this concept and showed a d-spacing of approximately 50 Å. In addition, conformation of the hybrid polymer chains can be manipulated to support their self-assembly into ordered microporous films.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Sen; Luo, Sheng-Nian

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

Effect of calcium concentration on the structure of casein micelles in thin films.

PubMed

Müller-Buschbaum, P; Gebhardt, R; Roth, S V; Metwalli, E; Doster, W

2007-08-01

The structure of thin casein films prepared with spin-coating is investigated as a function of the calcium concentration. Grazing incidence small-angle x-ray scattering and atomic force microscopy are used to probe the micelle structure. For comparison, the corresponding casein solutions are investigated with dynamic light-scattering experiments. In the thin films with added calcium three types of casein structures, aggregates, micelles, and mini-micelles, are observed in coexistence with atomic force microscopy and grazing incidence small-angle x-ray scattering. With increasing calcium concentration, the size of the aggregates strongly increases, while the size of micelles slightly decreases and the size of the mini-micelles increases. This effect is explained in the framework of the particle-stabilizing properties of the hairy layer of kappa-casein surrounding the casein micelles.

Effect of Calcium Concentration on the Structure of Casein Micelles in Thin Films

PubMed Central

Müller-Buschbaum, P.; Gebhardt, R.; Roth, S. V.; Metwalli, E.; Doster, W.

2007-01-01

The structure of thin casein films prepared with spin-coating is investigated as a function of the calcium concentration. Grazing incidence small-angle x-ray scattering and atomic force microscopy are used to probe the micelle structure. For comparison, the corresponding casein solutions are investigated with dynamic light-scattering experiments. In the thin films with added calcium three types of casein structures, aggregates, micelles, and mini-micelles, are observed in coexistence with atomic force microscopy and grazing incidence small-angle x-ray scattering. With increasing calcium concentration, the size of the aggregates strongly increases, while the size of micelles slightly decreases and the size of the mini-micelles increases. This effect is explained in the framework of the particle-stabilizing properties of the hairy layer of κ-casein surrounding the casein micelles. PMID:17496032

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 ismore » 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.« less

Dynamic Light Scattering of Diabetic Vitreopathy

NASA Technical Reports Server (NTRS)

Sebag, J.; Ansari, Rafat R.; Dunker, Stephan; Suh, Kwang I.

1999-01-01

Diabetes induces pathology throughout the body via nonenzymatic glycation of proteins. Vitreous, which is replete with type 11 collagen, undergoes significant changes in diabetes. The resultant diabetic vitreopathy plays an important role in diabetic retinopathy. Detecting these molecular changes could provide insight into diabetic eye disease as well as molecular effects elsewhere in the body. Human eyes were obtained at autopsy and studied in the fresh, unfixed state. Sclera, choroid, and retina were dissected off the vitreous for dark-field slit microscopy and dynamic light scattering (DLS). For the former, the entire vitreous was exposed. For the latter, only a window at the equator was dissected in some specimens, and the anterior segment was removed leaving the posterior lens capsule intact in others. DLS was performed to determine particle sizes at multiple sites 0.5 mm apart, spanning the globe at the equator (window dissections) and along the antero-posterior axis. Dark-field slit microscopy in diabetic subjects detected findings typical of age-related vitreous degeneration, but at much younger ages than nondiabetic controls. Noninvasive DLS measurements found a greater heterogeneity and larger particle sizes in vitreous of subjects with diabetes as compared to age-matched controls. DLS can detect and quantify the early molecular effects that cause vitreous collagen fibrils to cross-link and aggregate. This could provide valuable insight into ocular and systemic effects of hyperglycemia, because the molecular changes in diabetic vitreopathy could serve as an index of such effects throughout the body. In addition to the diagnostic implications, this methodology could provide a rapid, reproducible way to monitor the response to therapy with novel agents intended to prevent the complications of diabetes on a molecular level.

Small Angle Neutron Scattering experiments on ``side-on fixed"" liquid crystal polyacrylates

NASA Astrophysics Data System (ADS)

Leroux, N.; Keller, P.; Achard, M. F.; Noirez, L.; Hardouin, F.

1993-08-01

Small Angle Neutron Scattering experiments were carried out on liquid crystalline “side-on fixed” polyacrylates : we observe that the polymer backbone adopts a prolate conformation in the nematic phase. Such anisotropy of the global backbone is larger for smaller spacer length. In every case we measure at low temperatures a large chain extension as previously described in polysiloxanes. Par diffusion des neutrons aux petits angles nous observons que la chaîne de polyacrylates “en haltère” adopte une conformation type prolate en phase nématique. Son anisotropie est d'autant plus grande que l'espaceur est plus court. Dans tous les cas, nous retrouvons à basse température la forte extension de la chaîne polymère qui fut d'abord révélée dans les polysiloxanes.

Angular distribution of diffuse reflectance from incoherent multiple scattering in turbid media.

PubMed

Gao, M; Huang, X; Yang, P; Kattawar, G W

2013-08-20

The angular distribution of diffuse reflection is elucidated with greater understanding by studying a homogeneous turbid medium. We modeled the medium as an infinite slab and studied the reflection dependence on the following three parameters: the incident direction, optical depth, and asymmetry factor. The diffuse reflection is produced by incoherent multiple scattering and is solved through radiative transfer theory. At large optical depths, the angular distribution of the diffuse reflection with small incident angles is similar to that of a Lambertian surface, but, with incident angles larger than 60°, the angular distributions have a prominent reflection peak around the specular reflection angle. These reflection peaks are found originating from the scattering within one transport mean free path in the top layer of the medium. The maximum reflection angles for different incident angles are analyzed and can characterize the structure of angular distributions for different asymmetry factors and optical depths. The properties of the angular distribution can be applied to more complex systems for a better understanding of diffuse reflection.

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 technique and, if they so choose, to apply it to provide new information in areas of their own particular research interests.

Experimental light scattering by positionally-controlled small particles — Implications for Planetary Science

NASA Astrophysics Data System (ADS)

Gritsevich, M.; Penttilä, A.; Maconi, G.; Kassamakov, I.; Martikainen, J.; Markkanen, J.; Vaisanen, T.; Helander, P.; Puranen, T.; Salmi, A.; Hæggström, E.; Muinonen, K.

2017-12-01

Electromagnetic scattering is a fundamental physical process that allows inferring characteristics of an object studied remotely. This possibility is enhanced by obtaining the light-scattering response at multiple wavelengths and viewing geometries, i.e., by considering a wider range of the phase angle (the angle between the incident light and the light reflected from the object) in the experiment. Within the ERC Advanced Grant project SAEMPL (http://cordis.europa.eu/project/rcn/107666_en.html) we have assembled an interdisciplinary group of scientists to develop a fully automated, 3D scatterometer that can measure scattered light at different wavelengths from small particulate samples. The setup comprises: (a) the PXI Express platform to synchronously record data from several photomultiplier tubes (PMTs); (b) a motorized rotation stage to precisely control the azimuthal angle of the PMTs around 360°; and (c) a versatile light source, whose wavelength, polarization, intensity, and beam shape can be precisely controlled. An acoustic levitator is used to hold the sample without touching it. The device is the first of its kind, since it measures controlled spectral angular scattering including all polarization effects, for an arbitrary object in the µm-cm size scale. It permits a nondestructive, disturbance-free measurement with control of the orientation and location of the scattering object. To demonstrate our approach we performed detailed measurements of light scattered by a Chelyabinsk LL5 chondrite particle, derived from the light-colored lithology sample of the meteorite. These measurements are cross-validated against the modeled light-scattering characteristics of the sample, i.e., the intensity and the degree of linear polarization of the reflected light, calculated with state-of-the-art electromagnetic techniques (see Muinonen et al., this meeting). We demonstrate a unique non-destructive approach to derive the optical properties of small grain samples which facilitates research on highly valuable planetary materials, such as samples returned from space missions or rare meteorites.

Element-selective investigation of domain structure in CoPd and FePd alloys using small-angle soft X-ray scattering

NASA Astrophysics Data System (ADS)

Weier, C.; Adam, R.; Frömter, R.; Bach, J.; Winkler, G.; Kobs, A.; Oepen, H. P.; Grychtol, P.; Kapteyn, H. C.; Murnane, M. M.; Schneider, C. M.

2014-03-01

Recent optical pump-probe experiments on magnetic multilayers and alloys identified perpendicular spin superdiffusion as one of possible mechanisms responsible for femtosecond magnetization dynamics. On the other hand, no strong evidence for the ultrafast lateral spin transport has been reported, so far. To address this question, we studied magnetic domain structure of CoPd and FePd thin films using small-angle scattering of soft X-rays. By tuning the synchrotron-generated X-rays to the absorption edges of Fe or Co we recorded Fourier images of the magnetic domain structure corresponding to a chosen element. Applying in - situ magnetic fields resulted in pronounced rearrangement of domain structure that was clearly observed in scattering images. Our analysis of both the stand-alone, as well as magnetically coupled CoPd/FePd layers provides insight into the formation of domains under small magnetic field perturbations and pave the way to better understanding of transient changes expected in magneto-dynamic measurements.

Intraocular light scatter, reflections, fluorescence and absorption: what we see in the slit lamp.

PubMed

van den Berg, Thomas J T P

2018-01-01

Much knowledge has been collected over the past 20 years about light scattering in the eye- in particular in the eye lens- and its visual effect, called straylight. It is the purpose of this review to discuss how these insights can be applied to understanding the slit lamp image. The slit lamp image mainly results from back scattering, whereas the effects on vision result mainly from forward scatter. Forward scatter originates from particles of about wavelength size distributed throughout the lens. Most of the slit lamp image originates from small particle scatter (Rayleigh scatter). For a population of middle aged lenses it will be shown that both these scatter components remove around 10% of the light from the direct beam. For slit lamp observation close to the reflection angles, zones of discontinuity (Wasserspalten) at anterior and posterior parts of the lens show up as rough surface reflections. All these light scatter effects increase with age, but the correlations with age, and also between the different components, are weak. For retro-illumination imaging it will be argued that the density or opacity seen in areas of cortical or posterior subcapsular cataract show up because of light scattering, not because of light loss. NOTES: (1) Light scatter must not be confused with aberrations. Light penetrating the eye is divided into two parts: a relatively small part is scattered, and removed from the direct beam. Most of the light is not scattered, but continues as the direct beam. This non-scattered part is the basis for functional imaging, but its quality is under the control of aberrations. Aberrations deflect light mainly over small angles (<1°), whereas light scatter is important because of the straylight effects over large angles (>1°), causing problems like glare and hazy vision. (2) The slit lamp image in older lenses and nuclear cataract is strongly influenced by absorption. However, this effect is greatly exaggerated by the light path lengths concerned. This obviates proper judgement of the functional importance of absorption, and hinders the appreciation of the Rayleigh nature of what is seen in the slit lamp image. © 2017 The Authors Ophthalmic & Physiological Optics © 2017 The College of Optometrists.

Light Scattering by Fractal Dust Aggregates. I. Angular Dependence of Scattering

NASA Astrophysics Data System (ADS)

Tazaki, Ryo; Tanaka, Hidekazu; Okuzumi, Satoshi; Kataoka, Akimasa; Nomura, Hideko

2016-06-01

In protoplanetary disks, micron-sized dust grains coagulate to form highly porous dust aggregates. Because the optical properties of these aggregates are not completely understood, it is important to investigate how porous dust aggregates scatter light. In this study, the light scattering properties of porous dust aggregates were calculated using a rigorous method, the T-matrix method, and the results were then compared with those obtained using the Rayleigh-Gans-Debye (RGD) theory and Mie theory with the effective medium approximation (EMT). The RGD theory is applicable to moderately large aggregates made of nearly transparent monomers. This study considered two types of porous dust aggregates—ballistic cluster-cluster agglomerates (BCCAs) and ballistic particle-cluster agglomerates. First, the angular dependence of the scattered intensity was shown to reflect the hierarchical structure of dust aggregates; the large-scale structure of the aggregates is responsible for the intensity at small scattering angles, and their small-scale structure determines the intensity at large scattering angles. Second, it was determined that the EMT underestimates the backward scattering intensity by multiple orders of magnitude, especially in BCCAs, because the EMT averages the structure within the size of the aggregates. It was concluded that the RGD theory is a very useful method for calculating the optical properties of BCCAs.

LIGHT SCATTERING BY FRACTAL DUST AGGREGATES. I. ANGULAR DEPENDENCE OF SCATTERING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tazaki, Ryo; Tanaka, Hidekazu; Okuzumi, Satoshi

2016-06-01

In protoplanetary disks, micron-sized dust grains coagulate to form highly porous dust aggregates. Because the optical properties of these aggregates are not completely understood, it is important to investigate how porous dust aggregates scatter light. In this study, the light scattering properties of porous dust aggregates were calculated using a rigorous method, the T -matrix method, and the results were then compared with those obtained using the Rayleigh–Gans–Debye (RGD) theory and Mie theory with the effective medium approximation (EMT). The RGD theory is applicable to moderately large aggregates made of nearly transparent monomers. This study considered two types of porousmore » dust aggregates—ballistic cluster–cluster agglomerates (BCCAs) and ballistic particle–cluster agglomerates. First, the angular dependence of the scattered intensity was shown to reflect the hierarchical structure of dust aggregates; the large-scale structure of the aggregates is responsible for the intensity at small scattering angles, and their small-scale structure determines the intensity at large scattering angles. Second, it was determined that the EMT underestimates the backward scattering intensity by multiple orders of magnitude, especially in BCCAs, because the EMT averages the structure within the size of the aggregates. It was concluded that the RGD theory is a very useful method for calculating the optical properties of BCCAs.« less

Understanding how the aggregation structure of starch affects its gastrointestinal digestion rate and extent.

PubMed

Chen, Pei; Wang, Kai; Kuang, Qirong; Zhou, Sumei; Wang, Dazheng; Liu, Xingxun

2016-06-01

Regulating the starch gastrointestinal digestion rate by control of its aggregation structure is an effective way, but the mechanism is still not clear. Multi-scale structure of waxy and normal wheat starches were studied by confocal laser scanning and scanning electron microscopes, as well as wide-angle and small-angle X-ray techniques in this study. In vitro digestion kinetics of those two starches and structure-digestion relationship were also discussed. Both waxy and normal starches show A-type diffraction pattern, but waxy variety shows a slightly higher crystallinity. Small-angle X-ray scattering results show that waxy wheat starch has higher scattering peak intensity (Imax) and a larger crystallinity lamellar repeat distance (Lp) compared with the normal wheat starch. We suggested that the higher digestion rate of waxy starch at initial stage is mainly due to more small-size particles, but the higher crystallinity and the larger crystalline lamellar size limit the digestion extent. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Ultra-small-angle neutron scattering with azimuthal asymmetry

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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

Fractal Structures on Fe3O4 Ferrofluid: A Small-Angle Neutron Scattering Study

NASA Astrophysics Data System (ADS)

Giri Rachman Putra, Edy; Seong, Baek Seok; Shin, Eunjoo; Ikram, Abarrul; Ani, Sistin Ari; Darminto

2010-10-01

A small-angle neutron scattering (SANS) which is a powerful technique to reveal the large scale structures was applied to investigate the fractal structures of water-based Fe3O4ferrofluid, magnetic fluid. The natural magnetite Fe3O4 from iron sand of several rivers in East Java Province of Indonesia was extracted and purified using magnetic separator. Four different ferrofluid concentrations, i.e. 0.5, 1.0, 2.0 and 3.0 Molar (M) were synthesized through a co-precipitation method and then dispersed in tetramethyl ammonium hydroxide (TMAH) as surfactant. The fractal aggregates in ferrofluid samples were observed from their SANS scattering distributions confirming the correlations to their concentrations. The mass fractal dimension changed from about 3 to 2 as ferrofluid concentration increased showing a deviation slope at intermediate scattering vector q range. The size of primary magnetic particle as a building block was determined by fitting the scattering profiles with a log-normal sphere model calculation. The mean average size of those magnetic particles is about 60 - 100 Å in diameter with a particle size distribution σ = 0.5.

Small Angle X-Ray Scattering from Lipid-Bound Myelin Basic Protein in Solution

PubMed Central

Haas, H.; Oliveira, C. L. P.; Torriani, I. L.; Polverini, E.; Fasano, A.; Carlone, G.; Cavatorta, P.; Riccio, P.

2004-01-01

The structure of myelin basic protein (MBP), purified from the myelin sheath in both lipid-free (LF-MBP) and lipid-bound (LB-MBP) forms, was investigated in solution by small angle x-ray scattering. The water-soluble LF-MBP, extracted at pH < 3.0 from defatted brain, is the classical preparation of MBP, commonly regarded as an intrinsically unfolded protein. LB-MBP is a lipoprotein-detergent complex extracted from myelin with its native lipidic environment at pH > 7.0. Under all conditions, the scattering from the two protein forms was different, indicating different molecular shapes. For the LB-MBP, well-defined scattering curves were obtained, suggesting that the protein had a unique, compact (but not globular) structure. Furthermore, these data were compatible with earlier results from molecular modeling calculations on the MBP structure which have been refined by us. In contrast, the LF-MBP data were in accordance with the expected open-coil conformation. The results represent the first direct structural information from x-ray scattering measurements on MBP in its native lipidic environment in solution. PMID:14695288

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

2017-02-28

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 effortmore » but results in greater structural resolution, showing a slightly lower packing of lipids in the outer bilayer leaflet of ~120 nm diameter palmitoyloleoyl phosphatidylcholine (POPC) vesicles, compared to the inner leaflet. Here, analysis of asymmetric dipalmitoyl phosphatidylcholine/POPC vesicles did not reveal evidence of transbilayer coupling between the inner and outer leaflets at 323 K, i.e.above the melting transition temperature of the two lipids.« less

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

PubMed

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

2000-12-01

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

Probing the anisotropic vortex lattice in the Fe-based superconductor KFe2As2 using small angle neutron scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Debeer-Schmitt, Lisa M; Dewhurst, Charles; Kikuchi, Hiroko

Using small angle neutron scattering, the anisotropy of the magnetic vortex lattice (VL), in the heavily hole-doped pnictide superconductor, KFe2As2, was studied. Well-ordered VL scattering patterns were measured with elds applied in directions between B k c and the basal plane, rotating either towards [100] or [110]. Slightly distorted hexagonal patterns were observed when B k c. However, the scattering pattern distorted strongly as the eld was rotated away from the c- axis. At low eld, the arrangement of vortices is strongly aected by the anisotropy of penetration depth in the plane perpendicular to the eld. By tting the distortionmore » with the anisotropic London model, we obtained an estimate of 3:4 for the anisotropy factor, , between the in-plane and c-axis penetration depths at the lowest temperature studied. The results further reveal VL phase transitions as a function of eld direction. We discuss these transitions using the "Hairy Ball" theorem.« less

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.

Impact of Interfacial Roughness on the Sorption Properties of Nanocast Polymers

DOE PAGES

Sridhar, Manasa; Gunugunuri, Krishna R.; Hu, Naiping; ...

2016-03-16

Nanocasting is an emerging method to prepare organic polymers with regular, nanometer pores using inorganic templates. This report assesses the impact of imperfect template replication on the sorption properties of such polymer castings. Existing X-ray diffraction data show that substantial diffuse scattering exists in the small-angle region even though TEM images show near perfect lattices of uniform pores. To assess the origin of the diffuse scattering, the morphology of the phenol - formaldehyde foams (PFF) was investigated by small-angle X-ray scattering (SAXS). The observed diffuse scattering is attributed to interfacial roughness due to fractal structures. Such roughness has a profoundmore » impact on the sorption properties. Conventional pore- filling models, for example, overestimate protein sorption capacity. A mathematical framework is presented to calculate sorption properties based on observed morphological parameters. The formalism uses the surface fractal dimension determined by SAXS in conjunction with nitrogen adsorption isotherms to predict lysozyme sorption. The results are consistent with measured lysozyme loading.« less

Quasielastic small-angle neutron scattering from heavy water solutions of cyclodextrins

NASA Astrophysics Data System (ADS)

Kusmin, André; Lechner, Ruep E.; Saenger, Wolfram

2011-01-01

We present a model for quasielastic neutron scattering (QENS) by an aqueous solution of compact and inflexible molecules. This model accounts for time-dependent spatial pair correlations between the atoms of the same as well as of distinct molecules and includes all coherent and incoherent neutron scattering contributions. The extension of the static theory of the excluded volume effect [A. K. Soper, J. Phys.: Condens. Matter 9, 2399 (1997)] to the time-dependent (dynamic) case allows us to obtain simplified model expressions for QENS spectra in the low Q region in the uniform fluid approximation. The resulting expressions describe the quasielastic small-angle neutron scattering (QESANS) spectra of D _2O solutions of native and methylated cyclodextrins well, yielding in particular translational and rotational diffusion coefficients of these compounds in aqueous solution. Finally, we discuss the full potential of the QESANS analysis (that is, beyond the uniform fluid approximation), in particular, the information on solute-solvent interactions (e.g., hydration shell properties) that such an analysis can provide, in principle.

Effect of the solvent on the size of clay nanoparticles in solution as determined using an ultraviolet-visible (UV-Vis) spectroscopy methodology.

PubMed

Alin, Jonas; Rubino, Maria; Auras, Rafael

2015-06-01

Ultraviolet-visible (UV-Vis) spectroscopy methodology was developed and utilized for the in situ nanoscale measurement of the size of mineral clay agglomerates in various liquid suspensions. The clays studied were organomodified and unmodified montmorillonite clays (I.44p, Cloisite 93a, and PGN). The methodology was compared and validated against dynamic light scattering (DLS) analysis. The method was able to measure clay agglomerates in solvents in situations where DLS analysis was unsuccessful due to the shapes, polydispersity, and high aspect ratios of the clay particles and the complexity of the aggregates, or dispersion medium. The measured clay agglomerates in suspension were found to be in the nanometer range in the more compatible solvents, and their sizes correlated with the Hansen solubility parameter space distance between the clay modifiers and the solvents. Mass detection limits for size determination were in the range from 1 to 9 mg/L. The methodology thus provides simple, rapid, and inexpensive characterization of clays or particles in the nano- or microsize range in low concentrations in various liquid media, including complex mixtures or highly viscous fluids that are difficult to analyze with DLS. In addition, by combining UV-VIS spectroscopy with DLS it was possible to discern flocculation behavior in liquids, which otherwise could result in false size measurements by DLS alone.

Characterisation of large scale structures in starch granules via small-angle neutron and X-ray scattering.

PubMed

Doutch, James; Gilbert, Elliot P

2013-01-02

Small angle scattering (SAS) techniques have a distinguished track record in illuminating the semi-crystalline lamellar structure of the starch granule. To date, there have been few attempts to use SAS techniques to characterise larger-scale structures reported from imaging techniques such as growth rings, blocklets or pores, nor how these structures would modulate the well-known scattering arising from the semi-crystalline lamellar structure. In this study, SAS data collected over an extended q range were gathered from dry and hydrated starch powders from varied botanical sources. The use of neutrons and X-rays, as well as comparing dry and hydrated granules, allowed different levels of contrast in scattering length density to be probed and therefore selected structural regions to be highlighted. The lowest q range, 0.002-0.04 Å(-1), was found to be dominated by scattering from the starch granules themselves, especially in the dry powders; however an inflection point from a low contrast structure was observed at 0.035 Å(-1). The associated scattering was interpreted within a unified scattering framework with the inflexion point correlating with a structure with radius of gyration ~90 Å - a size comparable to small blocklets or superhelices. In hydrated starches, it is observed that there is an inflection point between lamellar and q(-4) power-law scattering regions at approximately 0.004 Å(-1) which may correlate with growth rings and large blocklets. The implications of these findings on existing models of starch lamellar scattering are discussed. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

Modification of Classical SPM for Slightly Rough Surface Scattering with Low Grazing Angle Incidence

NASA Astrophysics Data System (ADS)

Guo, Li-Xin; Wei, Guo-Hui; Kim, Cheyoung; Wu, Zhen-Sen

2005-11-01

Based on the impedance/admittance rough boundaries, the reflection coefficients and the scattering cross section with low grazing angle incidence are obtained for both VV and HH polarizations. The error of the classical perturbation method at grazing angle is overcome for the vertical polarization at a rough Neumann boundary of infinite extent. The derivation of the formulae and the numerical results show that the backscattering cross section depends on the grazing angle to the fourth power for both Neumann and Dirichlet boundary conditions with low grazing angle incidence. Our results can reduce to that of the classical small perturbation method by neglecting the Neumann and Dirichlet boundary conditions. The project supported by National Natural Science Foundation of China under Grant No. 60101001 and the National Defense Foundation of China

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

PubMed

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

2013-09-10

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

Preliminary small-angle X-ray scattering and X-ray diffraction studies of the BTB domain of lola protein from Drosophila melanogaster

NASA Astrophysics Data System (ADS)

Boyko, K. M.; Nikolaeva, A. Yu.; Kachalova, G. S.; Bonchuk, A. N.; Dorovatovskii, P. V.; Popov, V. O.

2017-11-01

The Drosophila genome has several dozens of transcription factors (TTK group) containing BTB domains assembled into octamers. The LOLA protein belongs to this family. The purification, crystallization, and preliminary X-ray diffraction and small-angle X-ray scattering (SAXS) studies of the BTB domain of this protein are reported. The crystallization conditions were found by the vapor-diffusion technique. A very low diffraction resolution (8.7 Å resolution) of the crystals was insufficient for the determination of the threedimensional structure of the BTB domain. The SAXS study demonstrated that the BTB domain of the LOLA protein exists as an octamer in solution.

Vacuum System Upgrade for Extended Q-Range Small-Angle Neutron Scattering Diffractometer (EQ-SANS) at SNS

DOE PAGES

Stone, Christopher M.; Williams, Derrick C.; Price, Jeremy P.

2016-09-23

The Extended Q-Range Small-Angle Neutron Scattering Diffractometer (EQ-SANS) instrument at the Spallation Neutron Source (SNS), Oak Ridge, Tennessee, incorporates a 69m3 detector vessel with a vacuum system which required an upgrade with respect to performance, ease of operation, and maintenance. The upgrade focused on improving pumping performance as well as optimizing system design to minimize opportunity for operational error. This upgrade provided the following practical contributions: Reduced time required to evacuate from atmospheric pressure to 2mTorr from 500-1,000 minutes to 60-70 minutes Provided turn-key automated control with a multi-faceted interlock for personnel and machine safety.

Structure of disordered gold-polymer thin films using small angle x-ray scattering

NASA Astrophysics Data System (ADS)

Teixeira, F. S.; Salvadori, M. C.; Cattani, M.; Brown, I. G.

2010-11-01

We have investigated the structure of disordered gold-polymer thin films using small angle x-ray scattering and compared the results with the predictions of a theoretical model based on two approaches—a structure form factor approach and the generalized Porod law. The films are formed of polymer-embedded gold nanoclusters and were fabricated by very low energy gold ion implantation into polymethylmethacrylate (PMMA). The composite films span (with dose variation) the transition from electrically insulating to electrically conducting regimes, a range of interest fundamentally and technologically. We find excellent agreement with theory and show that the PMMA-Au films have monodispersive or polydispersive characteristics depending on the implanted ion dose.

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

Vacuum System Upgrade for Extended Q-Range Small-Angle Neutron Scattering Diffractometer (EQ-SANS) at SNS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stone, Christopher M.; Williams, Derrick C.; Price, Jeremy P.

The Extended Q-Range Small-Angle Neutron Scattering Diffractometer (EQ-SANS) instrument at the Spallation Neutron Source (SNS), Oak Ridge, Tennessee, incorporates a 69m3 detector vessel with a vacuum system which required an upgrade with respect to performance, ease of operation, and maintenance. The upgrade focused on improving pumping performance as well as optimizing system design to minimize opportunity for operational error. This upgrade provided the following practical contributions: Reduced time required to evacuate from atmospheric pressure to 2mTorr from 500-1,000 minutes to 60-70 minutes Provided turn-key automated control with a multi-faceted interlock for personnel and machine safety.

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

Small angle x-ray scattering study on the conformation of polystyrene in toluene during adding anti-solvent CO2

NASA Astrophysics Data System (ADS)

Liu, Yi; Chen, Dong-Feng; Wang, Hong-Li; Chen, Na; Li, Dan; Han, Bu-Xing; Rong, Li-Xia; Zhao, Hui; Wang, Jun; Dong, Bao-Zhong

2002-10-01

The conformation of polystyrene in the anti-solvent process of supercritical fluids (compressed CO2 + polystyrene + toluene) has been studied by small angle x-ray scattering with synchrotron radiation as an x-ray source. Coil-to-globule transformation of the polystyrene chain was observed with the increase of the anti-solvent CO2 pressure; i.e. polystyrene coiled at a pressure lower than the cloud point pressure (Pc) and turned into a globule with a uniform density at pressures higher than Pc. Fractal behaviour was also found in the chain contraction and the mass fractal dimension increased with increasing CO2 pressure.

Tea Derived Galloylated Polyphenols Cross-Link Purified Gastrointestinal Mucins

PubMed Central

Georgiades, Pantelis; Pudney, Paul D. A.; Rogers, Sarah; Thornton, David J.; Waigh, Thomas A.

2014-01-01

Polyphenols derived from tea are thought to be important for human health. We show using a combination of particle tracking microrheology and small-angle neutron scattering that polyphenols acts as cross-linkers for purified gastrointestinal mucin, derived from the stomach and the duodenum. Both naturally derived purified polyphenols, and green and black tea extracts are shown to act as cross-linkers. The main active cross-linking component is found to be the galloylated forms of catechins. The viscosity, elasticity and relaxation time of the mucin solutions experience an order of magnitude change in value upon addition of the polyphenol cross-linkers. Similarly small-angle neutron scattering experiments demonstrate a sol-gel transition with the addition of polyphenols, with a large increase in the scattering at low angles, which is attributed to the formation of large scale (>10 nm) heterogeneities during gelation. Cross-linking of mucins by polyphenols is thus expected to have an impact on the physicochemical environment of both the stomach and duodenum; polyphenols are expected to modulate the barrier properties of mucus, nutrient absorption through mucus and the viscoelastic microenvironments of intestinal bacteria. PMID:25162539

Laboratory-Based Bidirectional Reflectance Distribution Functions of Radiometric Tarps

NASA Technical Reports Server (NTRS)

Georgiev, Georgi T.; Butler, James J.

2008-01-01

Laboratory-based bidirectional reflectance distribution functions of radiometric tarp samples used in the vicarious calibration of Earth remote sensing satellite instruments are presented in this paper. The results illustrate the BRDF dependence on the orientation of the tarps weft and warp threads. The study was performed using the GSFC scatterometer at incident zenith angles of 0 deg, 10 deg, and 30 deg; scatter zenith angles from 0 deg. to 60 deg.; and scatter azimuth angles of 0 deg., 45 deg., 90 deg., 135 deg. and 180 deg. The wavelengths were 485nm, 550nm, 633nm and 800nm. The tarp's weft and warp dependence on BRDF is well defined at all measurement geometries and wavelengths. The BRDF difference can be as high as 8% at 0o incident angle and 12% at 30 deg. incident angle. The fitted BRDF data shows a very small discrepancy from the measured ones. New data on the forward and backscatter properties of radiometric tarps are reported. The backward scatter is well pronounced for the white samples. The black sample has well pronounced forward scatter. The provided BRDF characterization of radiometric tarps is an excellent reference for anyone interested in using tarps for radiometric calibrations. The results are NIST traceable.

Ultra-small and anionic starch nanospheres: formation and vitro thrombolytic behavior study.

PubMed

Huang, Yinjuan; Ding, Shenglong; Liu, Mingzhu; Gao, Chunmei; Yang, Jinlong; Zhang, Xinjie; Ding, Bin

2013-07-25

This paper is considered as the first report on the investigation of nattokinase (NK) release from anionic starch nanospheres. The ultra-small and anionic starch nanospheres were prepared by the method of reverse micro-emulsion crosslinking in this work. Starch nanospheres were characterized through Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and dynamic light scattering (DLS). Effects of preparation conditions on particle size were studied. The cytotoxicity, biodegradable and vitro thrombolytic behaviors of nattokinase (NK) loaded anionic starch nanospheres were also studied. The results showed that the anionic starch nanospheres are non-toxic, biocompatible and biodegradable. Moreover, the anionic starch nanospheres can protect NK from fast biodegradation hence prolongs the circulation in vivo and can reduce the risk of acute hemorrhage complication by decreasing the thrombolysis rate. Copyright © 2013 Elsevier Ltd. All rights reserved.

SAR Polarimetry

NASA Technical Reports Server (NTRS)

vanZyl, Jakob J.

2012-01-01

Radar Scattering includes: Surface Characteristics, Geometric Properties, Dielectric Properties, Rough Surface Scattering, Geometrical Optics and Small Perturbation Method Solutions, Integral Equation Method, Magellan Image of Pancake Domes on Venus, Dickinson Impact Crater on Venus (Magellan), Lakes on Titan (Cassini Radar, Longitudinal Dunes on Titan (Cassini Radar), Rough Surface Scattering: Effect of Dielectric Constant, Vegetation Scattering, Effect of Soil Moisture. Polarimetric Radar includes: Principles of Polarimetry: Field Descriptions, Wave Polarizations: Geometrical Representations, Definition of Ellipse Orientation Angles, Scatter as Polarization Transformer, Scattering Matrix, Coordinate Systems, Scattering Matrix, Covariance Matrix, Pauli Basis and Coherency Matrix, Polarization Synthesis, Polarimeter Implementation.

Small-angle light scattering symmetry breaking in polymer-dispersed liquid crystal films with inhomogeneous electrically controlled interface anchoring

DOE Office of Scientific and Technical Information (OSTI.GOV)

Loiko, V. A., E-mail: loiko@ifanbel.bas-net.by; Konkolovich, A. V.; Zyryanov, V. Ya.

2017-03-15

We have described the method of analyzing and reporting on the results of calculation of the small-angle structure of radiation scattered by a polymer-dispersed liquid crystal film with electrically controlled interfacial anchoring. The method is based on the interference approximation of the wave scattering theory and the hard disk model. Scattering from an individual liquid crystal droplet has been described using the anomalous diffraction approximation extended to the case of droplets with uniform and nonuniform interface anchoring at the droplet–polymer boundary. The director field structure in an individual droplet is determined from the solution of the problem of minimizing themore » volume density of the free energy. The electrooptical effect of symmetry breaking in the angular distribution of scattered radiation has been analyzed. This effect means that the intensities of radiation scattered within angles +θ{sub s} and–θ{sub s} relative to the direction of illumination in the scattering plane can be different. The effect is of the interference origin and is associated with asymmetry of the phase shift of the wavefront of an incident wave from individual parts of the droplet, which appears due to asymmetry of the director field structure in the droplet, caused by nonuniform anchoring of liquid crystal molecules with the polymer on its surface. This effect is analyzed in the case of normal illumination of the film depending on the interfacial anchoring at the liquid crystal–polymer interface, the orientation of the optical axes of droplets, their concentration, sizes, anisometry, and polydispersity.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Giudicotti, L., E-mail: leonardo.giudicotti@unipd.it; Department of Industrial Engineering, Padova University, Via Gradenigo 6/a, 35131 Padova; Pasqualotto, R.

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 spectralmore » 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.« less

Length scale dependence of the dynamic properties of hyaluronic acid solutions in the presence of salt.

PubMed

Horkay, Ferenc; Falus, Peter; Hecht, Anne-Marie; Geissler, Erik

2010-12-02

In solutions of the charged semirigid biopolymer hyaluronic acid in salt-free conditions, the diffusion coefficient D(NSE) measured at high transfer momentum q by neutron spin echo is more than an order of magnitude smaller than that determined by dynamic light scattering, D(DLS). This behavior contrasts with neutral polymer solutions. With increasing salt content, D(DLS) approaches D(NSE), which is independent of ionic strength. Contrary to theoretical expectation, the ion-polymer coupling, which dominates the low q dynamics of polyelectrolyte solutions, already breaks down at distance scales greater than the Debye-Hückel length.

Gold nanoparticle-based simple colorimetric and ultrasensitive dynamic light scattering assay for the selective detection of Pb(II) from paints, plastics, and water samples.

PubMed

Beqa, Lule; Singh, Anant Kumar; Khan, Sadia Afrin; Senapati, Dulal; Arumugam, Sri Ranjini; Ray, Paresh Chandra

2011-03-01

Pb (II) is a common water pollutant with high toxicity. According to the CDC, about 310,000 U.S. children of ages 1-5 have high levels of lead in their blood that it is due to the exposure to lead from plastic toys and other products. As a result, the development of ultrasensitive assays for the real-time detection of Pb(II) from plastic toys and paints is very important for water controlling, clinical toxicology and industrial processes. Driven by the need to detect trace amounts of Pb(II) from water samples, we report a label-free, highly selective and ultra sensitive glutathione modified gold nanoparticle based dynamic light scattering (DLS) probe for Pb(II) recognition in 100 ppt level from aqueous solution with excellent discrimination against other heavy metals. The sensitivity of our assay to detect Pb(II) level in water is almost 2 orders of magnitude higher than the EPA standard limit. We have also demonstrated that our DLS assay is capable of measuring the amount of Pb(II) in paint, plastic toys, and water from MS river. A possible mechanism and operating principles of our DLS assay have been discussed. Ultimately, this nanotechnology driven assay could have enormous potential applications in rapid, on-site monitoring of Pb(II) from day-to-day sample.

Superhydrophobic surfaces allow probing of exosome self organization using X-ray scattering

NASA Astrophysics Data System (ADS)

Accardo, Angelo; Tirinato, Luca; Altamura, Davide; Sibillano, Teresa; Giannini, Cinzia; Riekel, Christian; di Fabrizio, Enzo

2013-02-01

Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates.Drops of exosome dispersions from healthy epithelial colon cell line and colorectal cancer cells were dried on a superhydrophobic PMMA substrate. The residues were studied by small- and wide-angle X-ray scattering using both a synchrotron radiation micrometric beam and a high-flux table-top X-ray source. Structural differences between healthy and cancerous cells were detected in the lamellar lattices of the exosome macro-aggregates. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr34032e

Time resolved small angle X-ray scattering experiments performed on detonating explosives at the advanced photon source: Calculation of the time and distance between the detonation front and the x-ray beam

DOE PAGES

Gustavsen, Richard L.; Dattelbaum, Dana Mcgraw; Watkins, Erik Benjamin; ...

2017-03-10

Time resolved Small Angle X-ray Scattering (SAXS) experiments on detonating explosives have been conducted at Argonne National Laboratory's Advanced Photon Source Dynamic Compression Sector. The purpose of the experiments is to measure the SAXS patterns at tens of ns to a few μs behind the detonation front. Corresponding positions behind the detonation front are of order 0.1–10 mm. From the scattering patterns, properties of the explosive products relative to the time behind the detonation front can be inferred. Lastly, this report describes how the time and distance from the x-ray probe location to the detonation front is calculated, as wellmore » as the uncertainties and sources of uncertainty associated with the calculated times and distances.« less

Small-angle scattering study of Aspergillus awamori glycoprotein glucoamylase

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schmidt, A. E., E-mail: schmidt@omrb.pnpi.spb.ru; Shvetsov, A. V.; Kuklin, A. I.

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 substantialmore » 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.« less

The suite of small-angle neutron scattering instruments at Oak Ridge National Laboratory

DOE PAGES

Heller, William T.; Cuneo, Matthew J.; Debeer-Schmitt, Lisa M.; ...

2018-02-21

Oak Ridge National Laboratory is home to the High Flux Isotope Reactor (HFIR), a high-flux research reactor, and the Spallation Neutron Source (SNS), the world's most intense source of pulsed neutron beams. The unique co-localization of these two sources provided an opportunity to develop a suite of complementary small-angle neutron scattering instruments for studies of large-scale structures: the GP-SANS and Bio-SANS instruments at the HFIR and the EQ-SANS and TOF-USANS instruments at the SNS. This article provides an overview of the capabilities of the suite of instruments, with specific emphasis on how they complement each other. As a result, amore » description of the plans for future developments including greater integration of the suite into a single point of entry for neutron scattering studies of large-scale structures is also provided.« less

Feasibility and applications of the spin-echo modulation option for a small angle neutron scattering instrument at the European Spallation Source

NASA Astrophysics Data System (ADS)

Kusmin, A.; Bouwman, W. G.; van Well, A. A.; Pappas, C.

2017-06-01

We describe theoretical and practical aspects of spin-echo modulated small-angle neutron scattering (SEMSANS) as well as the potential combination with SANS. Based on the preliminary technical designs of SKADI (a SANS instrument proposed for the European Spallation Source) and a SEMSANS add-on, we assess the practicability, feasibility and scientific merit of a combined SANS and SEMSANS setup by calculating tentative SANS and SEMSANS results for soft matter, geology and advanced material samples that have been previously studied by scattering methods. We conclude that lengths from 1 nm up to 0.01 mm can be observed simultaneously in a single measurement. Thus, the combination of SANS and SEMSANS instrument is suited for the simultaneous observation of a wide range of length scales, e.g. for time-resolved studies of kinetic processes in complex multiscale systems.

The study of the structural properties of very low viscosity sodium alginate by small-angle neutron scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Badita, C. R., E-mail: ramona@tandem.nipne.ro; University of Bucharest, Faculty of Physics, Atomiştilor 405, CP MG - 11, RO – 077125, Bucharest-Magurele; Aranghel, D., E-mail: daranghe@nipne.ro

2016-03-25

Sodium alginate is a linear polymer extract from brown algae and it is used in the biomedical, food, cosmetics and pharmaceutical industries as solution property modifiers and gelling agents. But despite the extensive studies of the alginate gelation process, still some fundamental questions remain unresolved. The fractal behavior of very low viscosity sodium alginate solutions and their influence on the critical gelation of alginate induced by Ca{sup 2+} ions were investigated using Small-Angle Neutron Scattering (SANS) measurements. SANS data are interpreted using both standard linear plots and the Beaucage model. The scattering intensity is dependent by alginate concentration and Ca{supmore » 2+} concentration. From a critical concentration of 1.0 % w/w our polymer swelled forming spherical structures with rough surfaces. Also the addition of the salt induces the collapse and the appearance of the aggregation and clusters formation.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 σ 2(q) = [I(q) + const.]/(kq), whereI(q) is the scattering intensity as a function of the momentum transferq;kand const. are fitting parameters that are characteristic of the experimental setup. The model gives a concrete procedure for calculating realistic measurementmore » 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.« less

The suite of small-angle neutron scattering instruments at Oak Ridge National Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Heller, William T.; Cuneo, Matthew J.; Debeer-Schmitt, Lisa M.

Oak Ridge National Laboratory is home to the High Flux Isotope Reactor (HFIR), a high-flux research reactor, and the Spallation Neutron Source (SNS), the world's most intense source of pulsed neutron beams. The unique co-localization of these two sources provided an opportunity to develop a suite of complementary small-angle neutron scattering instruments for studies of large-scale structures: the GP-SANS and Bio-SANS instruments at the HFIR and the EQ-SANS and TOF-USANS instruments at the SNS. This article provides an overview of the capabilities of the suite of instruments, with specific emphasis on how they complement each other. As a result, amore » description of the plans for future developments including greater integration of the suite into a single point of entry for neutron scattering studies of large-scale structures is also provided.« less

The study of the structural properties of very low viscosity sodium alginate by small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Badita, C. R.; Aranghel, D.; Radulescu, A.; Anitas, E. M.

2016-03-01

Sodium alginate is a linear polymer extract from brown algae and it is used in the biomedical, food, cosmetics and pharmaceutical industries as solution property modifiers and gelling agents. But despite the extensive studies of the alginate gelation process, still some fundamental questions remain unresolved. The fractal behavior of very low viscosity sodium alginate solutions and their influence on the critical gelation of alginate induced by Ca2+ ions were investigated using Small-Angle Neutron Scattering (SANS) measurements. SANS data are interpreted using both standard linear plots and the Beaucage model. The scattering intensity is dependent by alginate concentration and Ca2+ concentration. From a critical concentration of 1.0 % w/w our polymer swelled forming spherical structures with rough surfaces. Also the addition of the salt induces the collapse and the appearance of the aggregation and clusters formation.

Time resolved small angle X-ray scattering experiments performed on detonating explosives at the advanced photon source: Calculation of the time and distance between the detonation front and the x-ray beam

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gustavsen, Richard L.; Dattelbaum, Dana Mcgraw; Watkins, Erik Benjamin

Time resolved Small Angle X-ray Scattering (SAXS) experiments on detonating explosives have been conducted at Argonne National Laboratory's Advanced Photon Source Dynamic Compression Sector. The purpose of the experiments is to measure the SAXS patterns at tens of ns to a few μs behind the detonation front. Corresponding positions behind the detonation front are of order 0.1–10 mm. From the scattering patterns, properties of the explosive products relative to the time behind the detonation front can be inferred. Lastly, this report describes how the time and distance from the x-ray probe location to the detonation front is calculated, as wellmore » as the uncertainties and sources of uncertainty associated with the calculated times and distances.« less

Insights into molecular architecture of terpenes using small angle neutron scattering

NASA Astrophysics Data System (ADS)

Rai, Durgesh K.; Annamraju, Aparna; Pingali, Sai Venkatesh; O'Neill, Hugh M.; Mewalal, Ritesh; Gunter, Lee E.; Tuskan, Gerald A.

Understanding macromolecular architectures is vital to engineering prospective terpene candidates for advanced biofuels. Eucalyptus plants store terpenes in specialized cavity-like structures in the leaves called oil glands, which comprises of volatile (VTs) and non-volatile (NVTs) terpenes. Using small-angle neutron scattering, we have investigated the structure and phase behavior of the supramolecular assembly formed by Geranyl beta-D-glucoside (GDG), a NVT and compare the results with that of beta-octyl glucoside (BOG). The formation of micellar structures was observed in the concentration range of 0.5-5 v/v% in water using small angle neutron scattering (SANS) where Schultz sphere model was used in quantifying structural parameters of micelles. SANS studies determine that GDG and BOG behave like amphiphiles forming micellar structures in aqueous solution. The micelles swell upon addition of alpha-Pinene (AP) indicating partition to the core region of the micelles. The general behavior of the micellar growth after partitioning of AP to form thermodynamically stable sizes varies with the NVT concentration. Our studies reveal that the presence of steric hindrance in the GDG via the unsaturated bonds could help stabilize VTs inside the oil glands. LDRD project LOIS ID 7428, SNS, CSMB, HFIR, ORNL, DOE Office of Science User Facilities.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yennawar, Hemant; Møller, Magda; University of Copenhagen, DK-2100 Copenhagen

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

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

Optical method and apparatus for detection of defects and microstructural changes in ceramics and ceramic coatings

DOEpatents

Ellingson, William A.; Todd, Judith A.; Sun, Jiangang

2001-01-01

Apparatus detects defects and microstructural changes in hard translucent materials such as ceramic bulk compositions and ceramic coatings such as after use under load conditions. The beam from a tunable laser is directed onto the sample under study and light reflected by the sample is directed to two detectors, with light scattered with a small scatter angle directed to a first detector and light scattered with a larger scatter angle directed to a second detector for monitoring the scattering surface. The sum and ratio of the two detector outputs respectively provide a gray-scale, or "sum" image, and an indication of the lateral spread of the subsurface scatter, or "ratio" image. This two detector system allows for very high speed crack detection for on-line, real-time inspection of damage in ceramic components. Statistical image processing using a digital image processing approach allows for the quantative discrimination of the presence and distribution of small flaws in a sample while improving detection reliability. The tunable laser allows for the penetration of the sample to detect defects from the sample's surface to the laser's maximum depth of penetration. A layered optical fiber directs the incoming laser beam to the sample and transmits each scattered signal to a respective one of the two detectors.

Metallated DNA Aptamers for Prostate Cancer Treatment. Revision

DTIC Science & Technology

2013-10-01

determined using Matlab software. Dynamic light scattering (DLS) was performed under ambient conditions using a Malvern Zetasizer nano series ZEN-1600... entangling porphyrins as suitable vessels for light-induced energy and electron transfer. J Mater Chem 2008;18:802-5. 57. Meenakshisundaram G, Eteshola

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

NASA Astrophysics Data System (ADS)

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

2011-01-01

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

On the definition of albedo and application to irregular particles

NASA Technical Reports Server (NTRS)

Hanner, M. S.; Giese, R. H.; Weiss, K.; Zerull, R.

1981-01-01

The various definitions of albedo used in planetary astronomy are reviewed. In particular, the Bond albedo, which refers only to the reflected and refracted components, is not applicable to small particles or highly irregular particles, where diffraction is not restricted to a well-defined lobe at small scattering angles. Measured scattering functions for irregular particles are presented in a normalized form and are applied to the case of zodiacal light.

Polyethylene glycol-covered ultra-small Gd2O3 nanoparticles for positive contrast at 1.5 T magnetic resonance clinical scanning

NASA Astrophysics Data System (ADS)

Fortin, Marc-André; Petoral, Rodrigo M., Jr.; Söderlind, Fredrik; Klasson, A.; Engström, Maria; Veres, Teodor; Käll, Per-Olof; Uvdal, Kajsa

2007-10-01

The size distribution and magnetic properties of ultra-small gadolinium oxide crystals (US-Gd2O3) were studied, and the impact of polyethylene glycol capping on the relaxivity constants (r1, r2) and signal intensity with this contrast agent was investigated. Size distribution and magnetic properties of US-Gd2O3 nanocrystals were measured with a TEM and PPMS magnetometer. For relaxation studies, diethylene glycol (DEG)-capped US-Gd2O3 nanocrystals were reacted with PEG-silane (MW 5000). Suspensions were adequately dialyzed in water to eliminate traces of Gd3+ and surfactants. The particle hydrodynamic radius was measured with dynamic light scattering (DLS) and the proton relaxation times were measured with a 1.5 T MRI scanner. Parallel studies were performed with DEG-Gd2O3 and PEG-silane-SPGO (Gd2O3,< 40 nm diameter). The small and narrow size distribution of US-Gd2O3 was confirmed with TEM (~3 nm) and DLS. PEG-silane-US-Gd2O3 relaxation parameters were twice as high as for Gd-DTPA and the r2/r1 ratio was 1.4. PEG-silane-SPGO gave low r1 relaxivities and high r2/r1 ratios, less compatible with positive contrast agent requirements. Higher r1 were obtained with PEG-silane in comparison to DEG-Gd2O3. Treatment of DEG-US-Gd2O3 with PEG-silane provides enhanced relaxivity while preventing aggregation of the oxide cores. This study confirms that PEG-covered Gd2O3 nanoparticles can be used for positively contrasted MR applications requiring stability, biocompatible coatings and nanocrystal functionalization.

Forward multiple scattering corrections as function of detector field of view

NASA Astrophysics Data System (ADS)

Zardecki, A.; Deepak, A.

1983-06-01

The theoretical formulations are given for an approximate method based on the solution of the radiative transfer equation in the small angle approximation. The method is approximate in the sense that an approximation is made in addition to the small angle approximation. Numerical results were obtained for multiple scattering effects as functions of the detector field of view, as well as the size of the detector's aperture for three different values of the optical depth tau (=1.0, 4.0 and 10.0). Three cases of aperture size were considered--namely, equal to or smaller or larger than the laser beam diameter. The contrast between the on-axis intensity and the received power for the last three cases is clearly evident.

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.

Modified interactions among globular proteins below isoelectric point in the presence of mono-, di- and tri-valent ions: A small angle neutron scattering study

NASA Astrophysics Data System (ADS)

Das, Kaushik; Kundu, Sarathi; Mehan, Sumit; Aswal, V. K.

2016-02-01

Both short range attraction and long range electrostatic repulsion exist among globular protein Bovine Serum Albumin in solution below its isoelectric point (pI ≈ 4.8). At pD ≈ 4.0, below pI, protein has a net positive surface charge although local charge inhomogeneity presents. Small angle neutron scattering study reveals that in the presence of both mono-(Na+) and di-(Ni2+) valent ions attractive interaction increases and repulsive interaction decreases with the increase of salt concentration. However, for tri-valent (Fe3+) ions, both attractive and repulsive interaction increases with increasing salt concentration but the relative strength of repulsion is more than the attraction.

Protein structure and interactions in the solid state studied by small-angle neutron scattering.

PubMed

Curtis, Joseph E; McAuley, Arnold; Nanda, Hirsh; Krueger, Susan

2012-01-01

Small-angle neutron scattering (SANS) is uniquely qualified to study the structure of proteins in liquid and solid phases that are relevant to food science and biotechnological applications. We have used SANS to study a model protein, lysozyme, in both the liquid and water ice phases to determine its gross-structure, interparticle interactions and other properties. These properties have been examined under a variety of solution conditions before, during, and after freezing. Results for lysozyme at concentrations of 50 mg mL(-1) and 100 mg mL(-1), with NaCl concentrations of 0.4 M and 0 M, respectively, both in the liquid and frozen states, are presented and implications for food science are discussed.

Interactions of amelogenin with phospholipids

DOE PAGES

Bekshe Lokappa, Sowmya; Chandrababu, Karthik Balakrishna; Dutta, Kaushik; ...

2014-11-22

Amelogenin protein has the potential to interact with other enamel matrix proteins, mineral, and cell surfaces. In this paper, we investigated the interactions of recombinant amelogenin rP172 with small unilamellar vesicles as model membranes, toward the goal of understanding the mechanisms of amelogenin–cell interactions during amelogenesis. Dynamic light scattering (DLS), fluorescence spectroscopy, circular dichroism (CD), and nuclear magnetic resonance (NMR) were used. In the presence of phospholipid vesicles, a blue shift in the Trp fluorescence emission maxima of rP172 was observed (~334 nm) and the Trp residues of rP172 were inaccessible to the aqueous quencher acrylamide. DLS studies indicated complexationmore » of rP172 and phospholipids, although the possibility of fusion of phospholipids following amelogenin addition cannot be ruled out. NMR and CD studies revealed a disorder–order transition of rP172 in a model membrane environment. Strong fluorescence resonance energy transfer from Trp in rP172 to DNS-bound-phospholipid was observed, and fluorescence polarization studies indicated that rP172 interacted with the hydrophobic core region of model membranes. Finally, our data suggest that amelogenin has ability to interact with phospholipids and that such interactions may play key roles in enamel biomineralization as well as reported amelogenin signaling activities.« less

Wave Turning and Flow Angle in the E-Region Ionosphere

NASA Astrophysics Data System (ADS)

Young, M.; Oppenheim, M. M.; Dimant, Y. S.

2016-12-01

This work presents results of particle-in-cell (PIC) simulations of Farley-Buneman (FB) turbulence at various altitudes in the high-latitude E-region ionosphere. In that region, the FB instability regularly produces meter-scale plasma irregularities. VHF radars observe coherent echoes via Bragg scatter from wave fronts parallel or anti-parallel to the radar line of sight (LoS) but do not necessarily measure the mean direction of wave propagation. Haldoupis (1984) conducted a study of diffuse radar aurora and found that the spectral width of back-scattered power depends critically on the angle between the radar LoS and the true flow direction, called the flow angle. Knowledge of the flow angle will allow researchers to better interpret observations of coherent back-scatter. Experiments designed to observe meter-scale irregularities in the E-region ionosphere created by the FB instability typically assume that the predominant flow direction is the E×B direction. However, linear theory of Dimant and Oppenheim (2004) showed that FB waves should turn away from E×B and particle-in-cell simulations by Oppenheim and Dimant (2013) support the theory. The present study comprises a quantitative analysis of the dependence of back-scattered power, flow velocity, and spectral width as functions of the flow angle. It also demonstrates that the mean direction of meter-scale wave propagation may differ from the E×B direction by tens of degrees. The analysis includes 2-D and 3-D simulations at a range of altitudes in the auroral ionosphere. Comparison between 2-D and 3-D simulations illustrates the relative importance to the irregularity spectrum of a small but finite component in the direction parallel to B. Previous work has shown this small parallel component to be important to turbulent electron heating and nonlinear transport.

Copolymers of poly-L-lysine with serine and tryptophan form stable DNA vectors: implications for receptor-mediated gene transfer.

PubMed

Gómez-Valadés, A G; Molas, M; Vidal-Alabró, A; Bermúdez, J; Bartrons, R; Perales, J C

2005-01-20

Inefficient gene transfer and poor stability in physiological medium are important shortcomings for receptor-mediated gene transfer vectors. Here, we evaluate vectors formulated with random copolymers of L-lysine/L-serine (3:1) and L-lysine/L-tryptophan (4:1), focusing on both their biophysical and functional characterization. By means of dynamic light scattering (DLS) and transmission electron microscopy (TEM), we demonstrate that poly-L-lysine (pK), poly-L-lysine-L-tryptophan (pKW) and poly-L-lysine-L-serine (pKS) are able to form compacted, small particles when mixed with plasmid DNA in the absence of salt. Upon dilution in physiological medium, copolymers of both lys/ser and lys/trp do not aggregate, in contrast with poly-L-lysine DNA complexes as determined by scattering, DLS and TEM measurements. Tight packing, as demonstrated by resistance to heparin, SDS and trypsin treatments, is also featured in tryptophan-containing complexes. Successful receptor-mediated endocytosis gene transfer using galactosylated copolymers into cells expressing the asiagloglycoprotein receptor correlated with lack of aggregation. Particles obtained using galactosylated poly-L-lysine-L-tryptophan (Gal-pKW) copolymer demonstrated specific receptor-mediated gene transfer since reporter gene activity dropped in the presence of an excess ligand in the culture medium during transfection. Although copolymers of galactosylated poly-L-lysine-L-serine (Gal-pKS) do not aggregate in the presence of salt, they are not able to internalize in a specific receptor-mediated endocytosis fashion. The introduction of bulky aromatic/hydrophobic (tryptophan) or hydrophillic (serine) moieties into the positively charged vectors allows the compacted particles to disperse into salt-containing medium avoiding salt-induced aggregation. Moreover, tryptophan-containing particles are able to mediate specific gene transfer via receptor-mediated endocytosis.

Non-Invasive Evaluation of Corneal Abnormalities Using Static and Dynamic Light Scattering

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Misra, Anup K.; Leung, Alfred B.; King, James F.; Datiles, Manuel B., III

2002-01-01

A preliminary study of corneal abnormalities in intact bovine eyes is presented. Twenty-one eyes were treated with chemicals, cotton swabs, and radial and photo-refractive surgeries. Dynamic and static light scattering was performed as a function of the penetration depth into the corneal tissue. Topographical maps of corneal refractive power from untreated and treated corneas were also obtained using videokeratoscopy and results compared. The ultimate aim is to develop the technique of dynamic light scattering (DLS) for clinical applications in early evaluation of corneal complications after laser-assisted in situ keratomileusis (LASIK) surgeries and other corneal abnormalities.

Noninvasive evaluation of corneal abnormalities using static and dynamic light scattering

NASA Astrophysics Data System (ADS)

Ansari, Rafat R.; Misra, Anup K.; Leung, Alfred B.; King, James F.; Datiles, Manuel B., III

2002-06-01

A preliminary study of corneal abnormalities in intact bovine eyes is presented. Twenty-one eyes were treated with chemicals, cotton swabs, and radial and photo-refractive surgeries. Dynamic and static light scattering was performed as a function of the penetration depth into the corneal tissue. Topographical maps of corneal refractive power from untreated and treated corneas were also obtained using videokeratoscopy and results compared. The ultimate aim is to develop the technique of dynamic light scattering (DLS) for clinical applications in early evaluation of corneal complications after laser-assisted in situ keratomileusis (LASIK) surgeries and other corneal abnormalities.

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

USGS Publications Warehouse

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

2003-01-01

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

TH-A-18C-04: Ultrafast Cone-Beam CT Scatter Correction with GPU-Based Monte Carlo Simulation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Y; Southern Medical University, Guangzhou; Bai, T

2014-06-15

Purpose: Scatter artifacts severely degrade image quality of cone-beam CT (CBCT). We present an ultrafast scatter correction framework by using GPU-based Monte Carlo (MC) simulation and prior patient CT image, aiming at automatically finish the whole process including both scatter correction and reconstructions within 30 seconds. Methods: The method consists of six steps: 1) FDK reconstruction using raw projection data; 2) Rigid Registration of planning CT to the FDK results; 3) MC scatter calculation at sparse view angles using the planning CT; 4) Interpolation of the calculated scatter signals to other angles; 5) Removal of scatter from the raw projections;more » 6) FDK reconstruction using the scatter-corrected projections. In addition to using GPU to accelerate MC photon simulations, we also use a small number of photons and a down-sampled CT image in simulation to further reduce computation time. A novel denoising algorithm is used to eliminate MC scatter noise caused by low photon numbers. The method is validated on head-and-neck cases with simulated and clinical data. Results: We have studied impacts of photo histories, volume down sampling factors on the accuracy of scatter estimation. The Fourier analysis was conducted to show that scatter images calculated at 31 angles are sufficient to restore those at all angles with <0.1% error. For the simulated case with a resolution of 512×512×100, we simulated 10M photons per angle. The total computation time is 23.77 seconds on a Nvidia GTX Titan GPU. The scatter-induced shading/cupping artifacts are substantially reduced, and the average HU error of a region-of-interest is reduced from 75.9 to 19.0 HU. Similar results were found for a real patient case. Conclusion: A practical ultrafast MC-based CBCT scatter correction scheme is developed. The whole process of scatter correction and reconstruction is accomplished within 30 seconds. This study is supported in part by NIH (1R01CA154747-01), The Core Technology Research in Strategic Emerging Industry, Guangdong, China (2011A081402003)« less

Geometrical-optics approximation of forward scattering by coated particles.

PubMed

Xu, Feng; Cai, Xiaoshu; Ren, Kuanfang

2004-03-20

By means of geometrical optics we present an approximation algorithm with which to accelerate the computation of scattering intensity distribution within a forward angular range (0 degrees-60 degrees) for coated particles illuminated by a collimated incident beam. Phases of emerging rays are exactly calculated to improve the approximation precision. This method proves effective for transparent and tiny absorbent particles with size parameters larger than 75 but fails to give good approximation results at scattering angles at which refractive rays are absent. When the absorption coefficient of a particle is greater than 0.01, the geometrical optics approximation is effective only for forward small angles, typically less than 10 degrees or so.

The conformation of Pluronic block copolymers adsorbed on carbon nanotubes and their interaction with water studied by small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Cohen, Yachin; Granite, Meirav; Pyckhout-Hintzen, Wim; Radulescu, Aurel

2010-03-01

Amphiphilic block copolymers are particularly useful in dispersing single-walled carbon nanotubes (SWCNT) in water. Small-angle neutron scattering measurements conducted at different D2O/H2O content of the dispersing medium provide quantitative information on the adsorption density and conformation of the polymer interacting with the nanotube surface. Data is presented on Pluronic F108 - (EO)132(PO)50(EO)132 and F127 (EO)100(PO)65(EO)100, where EO-ethylene oxide and PO-propylene oxide, well below the critical micellization temperature of the polymer. A dense coating of the PPO blocks on the nanotube surface is determined with the PEO chains extended from the cylindrical core-shell structure. The data from the two Pluronic systems show minimal scattering at about 70% D2O in the dispersing water, which exhibit a q -1 power law of the scattering vector (q ). This indicates near matching of the polymer chains at a surprisingly high scattering length density. The model fit required considerations of tight association of water molecules around PEO chains and slight isotopic selectivity.

Narrowly peaked forward light scattering on particulate media: II. Angular spreading of light scattered by polystyrene microspheres

NASA Astrophysics Data System (ADS)

Turcu, Ioan; Bratfalean, Radu; Neamtu, Silvia

2008-07-01

The adequacy of the effective phase function (EPF) used to describe the light scattered at small angles was tested on aqueous suspensions of polystyrene microspheres. Angular resolved light scattering measurements were performed on two types of latex suspension, which contained polystyrene spheres of 3 µm and 5 µm diameters, respectively. The experimental data were fitted with two EPF approximants. If the polystyrene spheres are at least 3 µm in diameter the quasi-ballistic light scattering process can be described relatively well by the EPF in a small angular range centered in the forward direction. The forward light scattering by macroscopic samples containing microspheres can be modeled relatively well if the true Mie single particle scattering phase function is replaced by a simpler Henyey-Greenstein dependence having the same width at half-height as the first scattering lobe.

Neutrons measure phase behavior in pores at Angstrom size

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bardoel, Agatha A; Melnichenko, Yuri B

Researchers have measured the phase behavior of green house gases in pores at the Angstrom-level, using small angle neutron scattering (SANS) at the Oak Ridge National Laboratory's High Flux Isotope Reactor. Yuri Melnichenko, an instrument scientist on the General Purpose Small Angle Neutron Scattering (GP SANS) Diffractometer at ORNL's High Flux Isotope Reactor, his postdoctoral associate Lilin He and collaborators Nidia Gallego and Cristian Contescu from the Material Sciences Division (ORNL) were engaged in the work. They were studying nanoporous carbons to assess their attractiveness as storage media for hydrogen, with a view to potential use for on-board hydrogen storagemore » for transportation applications. Nanoporous carbons can also serve as electrode material for supercapacitors and batteries. The researchers successfully determined that the most efficiently condensing pore size in a carbon nanoporous material for hydrogen storage is less than one nanometer. In a paper recently published by the Journal of the American Chemical Society, the collaborators used small angle neutron scattering to study how hydrogen condenses in small pores at ambient temperature. They discovered that the surface-molecule interactions create internal pressures in pores that may exceed the external gas pressure by a factor of up to 50. 'This is an exciting result,' Melnichenko said, 'as you achieve extreme densification in pores 'for free', i.e. without spending any energy. These results can be used to guide the development of new carbon adsorbents tailored to maximize hydrogen storage capacities.' Another important factor that defines the adsorption capacity of sub-nanometer pores is their shape. In order to get accurate structural information and maximize sorption capacity, it is important that pores are small and of approximately uniform size. In collaboration with Drexel University's Yury Gogotsi who supplied the samples, Melnichenko and his collaborators used the GP SANS instrument to study how the size and shape of pores in sub-nanometer porous carbons varies, depending on the manufacturing conditions. While small angle X-ray scattering (SAXS) can do the job too, Melnichenko says, the SANS method broke new ground in analyzing the shape and behavior of pores at subnanometer size, when subjected to varying synthesis temperature. 'We found that these very small pores are in fact spherical, and that when we change the synthesis conditions, they become elongated, even 'slit-like', and all of this on a subnanometer scale,' Melnichenko said.« less

Neutron Polarization Analysis for Biphasic Solvent Extraction Systems

DOE PAGES

Motokawa, Ryuhei; Endo, Hitoshi; Nagao, Michihiro; ...

2016-06-16

Here we performed neutron polarization analysis (NPA) of extracted organic phases containing complexes, comprised of Zr(NO 3) 4 and tri-n-butyl phosphate, which enabled decomposition of the intensity distribution of small-angle neutron scattering (SANS) into the coherent and incoherent scattering components. The coherent scattering intensity, containing structural information, and the incoherent scattering compete over a wide range of magnitude of scattering vector, q, specifically when q is larger than q* ≈ 1/R g, where R g is the radius of gyration of scatterer. Therefore, it is important to determine the incoherent scattering intensity exactly to perform an accurate structural analysis frommore » SANS data when R g is small, such as the aforementioned extracted coordination species. Although NPA is the best method for evaluating the incoherent scattering component for accurately determining the coherent scattering in SANS, this method is not used frequently in SANS data analysis because it is technically challenging. In this study, we successfully demonstrated that experimental determination of the incoherent scattering using NPA is suitable for sample systems containing a small scatterer with a weak coherent scattering intensity, such as extracted complexes in biphasic solvent extraction systems.« less

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.

Planar small-angle x-ray scattering imaging of phantoms and biological samples

NASA Astrophysics Data System (ADS)

Choi, M.; Badano, A.

2017-04-01

Coherent small-angle x-ray scattering (SAXS) provides molecular and nanometer-scale structural information. By capturing SAXS data at multiple locations across a sample, we obtained planar images and observed improved contrast given by the difference in the material scattering cross sections. We use phantoms made with 3D printing techniques, with tissue-mimicking plastic (PMMA), and with a highly scattering reference material (AgBe), which were chosen because of their well characterized scattering cross section to demonstrate and characterize the planar imaging of a laboratory SAXS system. We measure 1.07 and 2.14 nm-1 angular intensity maps for AgBe, 9.5 nm-1 for PMMA, and 12.3 nm-1 for Veroclear. The planar SAXS images show material discrimination based on their cross sectional features. The image signal-to-noise ratio (SNR) of each q image was dependent on exposure time and x-ray flux. We observed a lower SNR (91 ± 48) at q angles where no characteristic peaks for either material exist. To improve the visualization of the acquired data by utilizing all q-binned data, we describe a weighted-sum presentation method with a priori knowledge of relevant cross sections to improve the SNR (10 000 ± 6400) over the SNR from a single q-image at 1.07 nm-1 (1100 ± 620). In addition, we describe planar SAXS imaging of a mouse brain slice showing differentiation of tissue types as compared to a conventional absorption-based x-ray imaging technique.

Laboratory-based bidirectional reflectance distribution functions of radiometric tarps.

PubMed

Georgiev, Georgi T; Butler, James J

2008-06-20

Laboratory-based bidirectional reflectance distribution functions (BRDFs) of radiometric tarp samples used in the vicarious calibration of Earth remote sensing satellite instruments are presented in this paper. The results illustrate the BRDF dependence on the orientation of the tarps' weft and warp threads. The study was performed using the GSFC scatterometer at incident zenith angles of 0 degrees, 10 degrees, and 30 degrees; scatter zenith angles from 0 degrees to 60 degrees; and scatter azimuth angles of 0 degrees, 45 degrees, 90 degrees, 135 degrees, and 180 degrees. The wavelengths were 485 nm, 550 nm, 633 nm, and 800 nm. The tarp's weft and warp dependence on BRDF is well defined at all measurement geometries and wavelengths. The BRDF difference can be as high as 8% at 0 degrees incident angle and 12% at 30 degrees incident angle. The fitted BRDF data show a very small discrepancy from the measured ones. New data on the forward and backscatter properties of radiometric tarps are reported. The backward scatter is well pronounced for the white samples. The black sample has well-pronounced forward scatter. The provided BRDF characterization of radiometric tarps is an excellent reference for anyone interested in using tarps for radiometric calibrations. The results are NIST traceable.

Zeta-potential and particle size studies of silver sulphide nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Vikash, E-mail: vikash@csr.res.in; Tarachand,; Ganesan, V.

Silver sulfide (Ag{sub 2}S) nanoparticles (NPs) were prepared successfully for the first time using diethylene glycol (DEG) as a surfactant. X-ray diffraction (XRD) data revealed single phase nature of the compound and energy-dispersive X-ray (EDX) confirmed its nominal composition. Their sizes were 43 nm from XRD, 50 nm from atomic force microscopy (AFM) and 19 nm & 213 nm from dynamic light scattering (DLS); their differences have been discussed. Autotitration study of zeta potential of these NPs in deionized water by DLS at different pH values confirmed an isoelectric point at pH = 5.14 and their very unstable nature in deionized water.

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

Multiple scattering corrections to the Beer-Lambert law. 1: Open detector.

PubMed

Tam, W G; Zardecki, A

1982-07-01

Multiple scattering corrections to the Beer-Lambert law are analyzed by means of a rigorous small-angle solution to the radiative transfer equation. Transmission functions for predicting the received radiant power-a directly measured quantity in contrast to the spectral radiance in the Beer-Lambert law-are derived. Numerical algorithms and results relating to the multiple scattering effects for laser propagation in fog, cloud, and rain are presented.

Small Angle X-ray Scattering for Nanoparticle Research

DOE PAGES

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

2016-04-07

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 ångström 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,more » shape, and organization into hierarchal structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well the combination of SAXS with other X-ray and non-X ray characterization tools. Furthermore, we conclude with an examination of several key areas of research where X-rays scattering has played a pivotal role, including in situ nanoparticle synthesis, nanoparticle assembly, and in 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.« less

Small Angle X-ray Scattering for Nanoparticle Research

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 ångström 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,more » shape, and organization into hierarchal structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well the combination of SAXS with other X-ray and non-X ray characterization tools. Furthermore, we conclude with an examination of several key areas of research where X-rays scattering has played a pivotal role, including in situ nanoparticle synthesis, nanoparticle assembly, and in 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.« less

Airborne Polarized Lidar Detection of Scattering Layers in the Ocean

NASA Astrophysics Data System (ADS)

Vasilkov, Alexander P.; Goldin, Yury A.; Gureev, Boris A.; Hoge, Frank E.; Swift, Robert N.; Wright, C. Wayne

2001-08-01

A polarized lidar technique based on measurements of waveforms of the two orthogonal-polarized components of the backscattered light pulse is proposed to retrieve vertical profiles of the seawater scattering coefficient. The physical rationale for the polarized technique is that depolarization of backscattered light originating from a linearly polarized laser beam is caused largely by multiple small-angle scattering from particulate matter in seawater. The magnitude of the small-angle scattering is determined by the scattering coefficient. Therefore information on the vertical distribution of the scattering coefficient can be derived potentially from measurements of the timedepth dependence of depolarization in the backscattered laser pulse. The polarized technique was verified by field measurements conducted in the Middle Atlantic Bight of the western North Atlantic Ocean that were supported by in situ measurements of the beam attenuation coefficient. The airborne polarized lidar measured the timedepth dependence of the backscattered laser pulse in two orthogonal-polarized components. Vertical profiles of the scattering coefficient retrieved from the timedepth depolarization of the backscattered laser pulse were compared with measured profiles of the beam attenuation coefficient. The comparison showed that retrieved profiles of the scattering coefficient clearly reproduce the main features of the measured profiles of the beam attenuation coefficient. Underwater scattering layers were detected at depths of 2025 m in turbid coastal waters. The improvement in dynamic range afforded by the polarized lidar technique offers a strong potential benefit for airborne lidar bathymetric applications.

Nonlinear Coherent Structures, Microbursts and Turbulence

NASA Astrophysics Data System (ADS)

Lakhina, G. S.

2015-12-01

Nonlinear waves are found everywhere, in fluids, atmosphere, laboratory, space and astrophysical plasmas. The interplay of nonlinear effects, dispersion and dissipation in the medium can lead to a variety of nonlinear waves and turbulence. Two cases of coherent nonlinear waves: chorus and electrostatic solitary waves (ESWs) and their impact on modifying the plasma medium are discussed. Chorus is a right-hand, circularly-polarized electromagnetic plane wave. Dayside chorus is a bursty emission composed of rising frequency "elements" with duration of ~0.1 to 1.0 s. Each element is composed of coherent subelements with durations of ~1 to 100 ms or more. The cyclotron resonant interaction between energetic electrons and the coherent chorus waves is studied. An expression for the pitch angle transport due to this interaction is derived considering a Gaussian distribution for the time duration of the chorus elements. The rapid pitch scattering can provide an explanation for the ionospheric microbursts of ~0.1 to 0.5 s in bremsstrahlung x-rays formed by ~10-100 keV precipitating electrons. On the other hand, the ESWs are observed in the electric field component parallel to the background magnetic field, and are usually bipolar or tripolar. Generation of coherent ESWs has been explained in terms of nonlinear fluid models of ion- and electron-acoustic solitons and double layers (DLs) based on Sagdeev pseudopotential technique. Fast Fourier transform of electron- and ion-acoustic solitons/DLs produces broadband wave spectra which can explain the properties of the electrostatic turbulence observed in the magnetosheath and plasma sheet boundary layer, and in the solar wind, respectively.

Studies of electron-molecule collisions - Applications to e-H2O

NASA Technical Reports Server (NTRS)

Brescansin, L. M.; Lima, M. A. P.; Gibson, T. L.; Mckoy, V.; Huo, W. M.

1986-01-01

Elastic differential and momentum transfer cross sections for the elastic scattering of electrons by H2O are reported for collision energies from 2 to 20 eV. These fixed-nuclei static-exchange cross sections were obtained using the Schwinger variational approach. In these studies the exchange potential is directly evaluated and not approximated by local models. The calculated differential cross sections, obtained with a basis set expansion of the scattering wave function, agree well with available experimental data at intermediate and larger angles. As used here, the results cannot adequately describe the divergent cross sections at small angles. An interesting feature of the calculated cross sections, particularly at 15 and 20 eV, is their significant backward peaking. This peaking occurs in the experimentally inaccessible region beyond a scattering angle of 120 deg. The implication of this feature for the determination of momentum transfer cross sections is described.

Disordered porous solids : from chord distributions to small angle scattering

NASA Astrophysics Data System (ADS)

Levitz, P.; Tchoubar, D.

1992-06-01

Disordered biphasic porous solids are examples of complex interfacial media. Small angle scattering strongly depends on the geometrical properties of the internal surface partitioning a porous system. Properties of the second derivative of the bulk autocorrelation function quantitatively defines the level of connection between the small angle scattering and the statistical properties of this interface. A tractable expression of this second derivative, involving the pore and the mass chord distribution functions, was proposed by Mering and Tchoubar (MT). Based on the present possibility to make a quantitative connection between imaging techniques and the small angle scattering, this paper tries to complete and to extend the MT approach. We first discuss how chord distribution functions can be used as fingerprints of the structural disorder. An explicit relation between the small angle scattering and these chord distributions is then proposed. In a third part, the application to different types of disorder is critically discussed and predictions are compared to available experimental data. Using image processing, we will consider three types of disorder : the long-range Debye randomness, the “ correlated " disorder with a special emphasis on the structure of a porous glass (the vycor), and, finally, complex structures where length scale invariance properties can be observed. Les solides poreux biphasiques sont des exemples de milieux interfaciaux complexes. La diffusion aux petits angles (SAS) dépend fortement des propriétés géométriques de l'interface partitionant le milieu poreux. Les propriétés de la dérivée seconde de la fonction d'autocorrélation de densité définit quantitativement le niveau de connection entre la diffusion aux petits angles et les caractéristiques statistiques de cette interface. Une expression utilisable de cette seconde dérivée, impliquant les distributions de cordes associées à la phase massique et au réseau de pores, fut proposée par Mering et Tchoubar (MT). Mettant à profit la possibilité actuelle d'une comparaison quantitative entre les techniques d'imagerie et la diffusion aux petits angles, ce papier tente de compléter et d'étendre l'approche MT. Dans un premier temps, nous montrons en quoi la connaissance de ces distributions de cordes permet de distinguer certains types de désordres structuraux. Une relation explicite entre le spectre de diffusion aux petits angles et les distributions de cordes est alors proposée. Dans une troisième partie, l'application à différents types de désordre est discutée et les prédictions du modèle comparées aux résultats expérimentaux disponibles. Par utilisation du traitement d'images, nous nous intéressons à trois types de désordre : le milieu aléatoire de Debye, pour ses propriétés à grandes distances, le désordre “ corrélé " avec une attention particulière pour le cas d'un verre poreux (le Vycor) et enfin des organisations complexes où des propriétés d'invariance d'échelle de longueur peuvent être observées.

Small-angle neutron scattering study of micropore collapse in amorphous solid water.

PubMed

Mitterdorfer, Christian; Bauer, Marion; Youngs, Tristan G A; Bowron, Daniel T; Hill, Catherine R; Fraser, Helen J; Finney, John L; Loerting, Thomas

2014-08-14

Vapor-deposited amorphous solid water (ASW) is the most abundant solid molecular material in space, where it plays a direct role in both the formation of more complex chemical species and the aggregation of icy materials in the earliest stages of planet formation. Nevertheless, some of its low temperature physics such as the collapse of the micropore network upon heating are still far from being understood. Here we characterize the nature of the micropores and their collapse using neutron scattering of gram-quantities of D2O-ASW of internal surface areas up to 230 ± 10 m(2) g(-1) prepared at 77 K. The model-free interpretation of the small-angle scattering data suggests micropores, which remain stable up to 120-140 K and then experience a sudden collapse. The exact onset temperature to pore collapse depends on the type of flow conditions employed in the preparation of ASW and, thus, the specific surface area of the initial deposit, whereas the onset of crystallization to cubic ice is unaffected by the flow conditions. Analysis of the small-angle neutron scattering signal using the Guinier-Porod model suggests that a sudden transition from three-dimensional cylindrical pores with 15 Å radius of gyration to two-dimensional lamellae is the mechanism underlying the pore collapse. The rather high temperature of about 120-140 K of micropore collapse and the 3D-to-2D type of the transition unraveled in this study have implications for our understanding of the processing and evolution of ices in various astrophysical environments.

The Denaturation Transition of DNA in Mixed Solvents

PubMed Central

Hammouda, Boualem; Worcester, David

2006-01-01

The helix-to-coil denaturation transition in DNA has been investigated in mixed solvents at high concentration using ultraviolet light absorption spectroscopy and small-angle neutron scattering. Two solvents have been used: water and ethylene glycol. The “melting” transition temperature was found to be 94°C for 4% mass fraction DNA/d-water and 38°C for 4% mass fraction DNA/d-ethylene glycol. The DNA melting transition temperature was found to vary linearly with the solvent fraction in the mixed solvents case. Deuterated solvents (d-water and d-ethylene glycol) were used to enhance the small-angle neutron scattering signal and 0.1M NaCl (or 0.0058 g/g mass fraction) salt concentration was added to screen charge interactions in all cases. DNA structural information was obtained by small-angle neutron scattering, including a correlation length characteristic of the inter-distance between the hydrogen-containing (desoxyribose sugar-amine base) groups. This correlation length was found to increase from 8.5 to 12.3 Å across the melting transition. Ethylene glycol and water mixed solvents were found to mix randomly in the solvation region in the helix phase, but nonideal solvent mixing was found in the melted coil phase. In the coil phase, solvent mixtures are more effective solvating agents than either of the individual solvents. Once melted, DNA coils behave like swollen water-soluble synthetic polymer chains. PMID:16815902

Analysis of Self-Associating Proteins by Singular Value Decomposition of Solution Scattering Data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Williamson, Tim E.; Craig, Bruce A.; Kondrashkina, Elena

2008-07-08

We describe a method by which a single experiment can reveal both association model (pathway and constants) and low-resolution structures of a self-associating system. Small-angle scattering data are collected from solutions at a range of concentrations. These scattering data curves are mass-weighted linear combinations of the scattering from each oligomer. Singular value decomposition of the data yields a set of basis vectors from which the scattering curve for each oligomer is reconstructed using coefficients that depend on the association model. A search identifies the association pathway and constants that provide the best agreement between reconstructed and observed data. Using simulatedmore » data with realistic noise, our method finds the correct pathway and association constants. Depending on the simulation parameters, reconstructed curves for each oligomer differ from the ideal by 0.050.99% in median absolute relative deviation. The reconstructed scattering curves are fundamental to further analysis, including interatomic distance distribution calculation and low-resolution ab initio shape reconstruction of each oligomer in solution. This method can be applied to x-ray or neutron scattering data from small angles to moderate (or higher) resolution. Data can be taken under physiological conditions, or particular conditions (e.g., temperature) can be varied to extract fundamental association parameters ({Delta}H{sub ass}, S{sub ass}).« less

Periodic organosilica hollow nanospheres as anode materials for lithium ion rechargeable batteries

NASA Astrophysics Data System (ADS)

Sasidharan, Manickam; Nakashima, Kenichi; Gunawardhana, Nanda; Yokoi, Toshiyuki; Ito, Masanori; Inoue, Masamichi; Yusa, Shin-Ichi; Yoshio, Masaki; Tatsumi, Takashi

2011-11-01

Polymeric micelles with core-shell-corona architecture have been found to be the efficient colloidal templates for synthesis of periodic organosilica hollow nanospheres over a broad pH range from acidic to alkaline media. In alkaline medium, poly (styrene-b-[3-(methacryloylamino)propyl] trimethylammonium chloride-b-ethylene oxide) (PS-PMAPTAC-PEO) micelles yield benzene-silica hollow nanospheres with molecular scale periodicity of benzene groups in the shell domain of hollow particles. Whereas, an acidic medium (pH 4) produces diverse hollow particles with benzene, ethylene, and a mixture of ethylene and dipropyldisulfide bridging functionalities using poly(styrene-b-2-vinyl pyridine-b-ethylene oxide) (PS-PVP-PEO) micelles. These hollow particles were thoroughly characterized by powder X-ray diffraction (XRD), dynamic light scattering (DLS), thermogravimetric analysis (TG/DTA), Fourier transformation infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), magic angle spinning-nuclear magnetic resonance (29Si MAS NMR and 13CP-MAS NMR), Raman spectroscopy, and nitrogen adsorption/desorption analyses. The benzene-silica hollow nanospheres with molecular scale periodicity in the shell domain exhibit higher cycling performance of up to 300 cycles in lithium ion rechargeable batteries compared with micron-sized dense benzene-silica particles.Polymeric micelles with core-shell-corona architecture have been found to be the efficient colloidal templates for synthesis of periodic organosilica hollow nanospheres over a broad pH range from acidic to alkaline media. In alkaline medium, poly (styrene-b-[3-(methacryloylamino)propyl] trimethylammonium chloride-b-ethylene oxide) (PS-PMAPTAC-PEO) micelles yield benzene-silica hollow nanospheres with molecular scale periodicity of benzene groups in the shell domain of hollow particles. Whereas, an acidic medium (pH 4) produces diverse hollow particles with benzene, ethylene, and a mixture of ethylene and dipropyldisulfide bridging functionalities using poly(styrene-b-2-vinyl pyridine-b-ethylene oxide) (PS-PVP-PEO) micelles. These hollow particles were thoroughly characterized by powder X-ray diffraction (XRD), dynamic light scattering (DLS), thermogravimetric analysis (TG/DTA), Fourier transformation infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), magic angle spinning-nuclear magnetic resonance (29Si MAS NMR and 13CP-MAS NMR), Raman spectroscopy, and nitrogen adsorption/desorption analyses. The benzene-silica hollow nanospheres with molecular scale periodicity in the shell domain exhibit higher cycling performance of up to 300 cycles in lithium ion rechargeable batteries compared with micron-sized dense benzene-silica particles. Electronic supplementary information (ESI) available: FTIR, Raman spectral data, additional TEM pictures, N2 adsorption and physical characteristics of hollow particles data, and cycling performance of dense silica particles. See DOI: 10.1039/c1nr10804b

Extension and applications of switching model: Range theory, multiple scattering model of Goudsmit-Saunderson, and lateral spread treatment of Marwick-Sigmund

NASA Astrophysics Data System (ADS)

Ikegami, Seiji

2017-09-01

The switching model (PSM) developed in the previous paper is extended to obtain an ;extended switching model (ESM). In the ESM, the mixt electronic-and-nuclear energy-loss region, in addition to the electronic and nuclear energy-loss regions in PSM, is taken into account analytically and appropriately. This model is combined with a small-angle multiple scattering range theory considering both nuclear and electronic stopping effects developed by Marwick-Sigmund and Valdes-Arista to formulate a improved range theory. The ESM is also combined with the multiple scattering theory with non-small angle approximation by Goudsmit-Saunderson. Furthermore, we applied ESM to lateral spread model of Marwick-Sigmund. Numerical calculations of the entire distribution functions including one of the mixt region are roughly and approximately possible. However, exact numerical calculation may be impossible. Consequently, several preliminary numerical calculations of the electronic, mixt, and nuclear regions are performed to examine their underlying behavior with respect to the incident energy, the scattering angle, the outgoing projectile intensity, and the target thickness. We show the numerical results not only of PSM and but also of ESM. Both numerical results are shown in the present paper for the first time. Since the theoretical relations are constructed using reduced variables, the calculations are made only on the case of C colliding on C.

Large-viewing-angle electroholography by space projection

NASA Astrophysics Data System (ADS)

Sato, Koki; Obana, Kazuki; Okumura, Toshimichi; Kanaoka, Takumi; Nishikawa, Satoko; Takano, Kunihiko

2004-06-01

The specification of hologram image is the full parallax 3D image. In this case we can get more natural 3D image because focusing and convergence are coincident each other. We try to get practical electro-holography system because for conventional electro-holography the image viewing angle is very small. This is due to the limited display pixel size. Now we are developing new method for large viewing angle by space projection method. White color laser is irradiated to single DMD panel ( time shared CGH of RGB three colors ). 3D space screen constructed by very small water particle is used to reconstruct the 3D image with large viewing angle by scattering of water particle.

Compartmentalisation Strategies for Hydrocarbon-based Biota on Titan

NASA Astrophysics Data System (ADS)

Norman, L.; Fortes, A. D.; Skipper, N.; Crawford, I.

2013-05-01

The goal of our study is to determine the nature of compartimentalisation strategies for any organisms inhabiting the hydrocarbon lakes of Titan (the largest moon of Saturn). Since receiving huge amounts of data via the Cassini-Huygens mission to the Saturnian system astrobiologists have speculated that exotic biota might currently inhabit this environment. The biota have been theorized to consume acetylene and hydrogen whilst excreting methane (1,2) leading to an anomalous hydrogen depletion near the surface; and there has been evidence to suggest this depletion exists (3). Nevertheless, many questions still remain concerning the possible physiological traits of biota in these environments, including whether cell-like structures can form in low temperature, low molecular weight hydrocarbons. The backbone of terrestrial cell membranes are vesicular structures composed primarily of a phospholipid bilayer with the hydrophilic head groups arranged around the periphery and are thought to be akin to the first protocells that terrestrial life utilised (4). It my be possible that reverse vesicles composed of a bilayer with the hydrophilic head groups arranged internally and a nonpolar core may be ideal model cell membranes for hydrocarbon-based organisms inhabiting Titan's hydrocarbon lakes (5). A variety of different surfactants have been used to create reverse vesicles in nonpolar liquids to date including; non-ionic ethers (7) and esters (6, 8); catanionic surfactant mixtures (9); zwitterionic gemini surfactants (10); coblock polymer surfactants (11); and zwitterionic phospholipid surfactants (12). In order to discover whether certain phospholipids can exhibit vesicular behaviour within hydrocarbon liquids, and to analyse their structure, we have carried out experimental studies using environmental conditions that are increasing comparable to those found on the surface of Titan. Experimental methods that have been used to determine the presence of vesicles include the use of microscopy, the presence of the Tyndall scattering effect, transmission electron microscopy (TEM), dynamic light scattering (DLS) , small-angle neutron scattering (SANS) and small-angle x-ray scattering (SAXS). These studies are currently being anaylzed, however, some results have indcated the presence of reverse vesicles in certain systems. Compounds that are shown to form reverse vesicles in conditions comparable to those of Titan's lakes could be potential 'biomarkers' and searched for in future missions to Titan. References [1] Schulze-Makuch D et al. Orig Life Evol Biosph 36, 324 (2006). [2] McKay C P et al. Icarus 178, 274 (2005). [3] Strobel D F. Icarus 208, 878 (2010). [4]. Fiordemondo D et al. Chem. Bio. Chem. 8, 1965 (2007). [5] Norman L H et al. A&G 52, 39 (2011). [6] Mollee H et al. J Pharm Sci 89, 930 (2000). ). [7] Kunieda H et al. Langmuir 15, 3118 (1999). [8] Shrestha L K et al. Langmuir 22, 1449 (2006). [9] Li H G et al. Chem. Lett 36, 702 (2007). [10] Peresypkin A et al. Mendeleev Commun. 17, 82 (2007). [11] Rangelov S et al. J. Phys. Chem B 108, 7542 (2004). [12] Tung S H et al. J. Am. Chem. 130, 8813 (2008).

Crystallization in Micellar Cores: confinement effects and dynamics

NASA Astrophysics Data System (ADS)

Lund, Reidar; Zinn, Thomas; Willner, Lutz; Department of Chemistry, University of Oslo Team; Forschungszentrum Jülich Collaboration

It is well known that liquids confined to small nanoscopic pores and droplets exhibit thermal behavior very different from bulk samples. Here we demonstrate that n-alkanes forming 2-3 nm small micellar cores are considerably affected by confinement in analogue with hard confined systems. We study micelles form by self-assembly of a series of well-defined n-Alkyl-PEO polymers in aqueous solutions. By using small-angle X-ray scattering (SAXS), densiometry and differential scanning calorimetry (DSC), we show that n-alkane exhibit a first-order phase transition i.e. melting. Correlating the structural and thermodynamic data, we find that a melting depression can be accurately described by the Gibbs-Thomson equation. ∖f1 The effect of core crystallinity on the molecular exchange kinetics is investigated using time-resolved small-angle neutron scattering (TR-SANS). We show that there are considerable entropic and enthalpic contributions from the chain packing that affect the kinetic stability of micelles. ∖pard

Protein size resolution in human eye lenses by dynamic light scattering after in vivo measurements: first analysis of a clinical validation

NASA Astrophysics Data System (ADS)

Dierks, Karsten; Dieckmann, Matthias; Niederstrasser, Dirk; Schwartz, R.; Wegener, Alfred R.

1995-01-01

Laser light source powers of our instrument LEPOSIAR are minimized so that dynamic light scattering (DLS) measurements can be conducted with lowest intensity levels on human eye lenses (3.2 mW/cm2) within measurement times of 3 to 5 seconds. We describe an extension of DLS and an eye lens characterization along the optical axis (OA), revealing the molecular size ranges together with distributions found in lens regions parallel to the OA. The microstructures of various lens regions are separated by the analyzed radius distributions reflecting the visco-elastic properties of the eye lens. Detailed analysis and applied statistical categorization of results are described. The data obtained by DLS allow for an objective interpretation of opacity occurrences on molecular size range which are related to refraction anomalies. Apart from changes in color and fluorescence properties, the refractive anomalies can be assumed as the origin of the cataract. The bimodal radius distributions are characterized as a function of patient ages varying from 9 to 85 years. Our clinical study on 42 subjects proves a size decrease of the monomeric fraction with age, whereby their relative frequency of occurrence decreases. The larger polymeric radius fractions which are detected in lenses of all subjects increase with their age. An increase of protein polymer size is likely to be linked to the decrease of the (gamma) -crystallin fraction in old eye lens nuclei. Our preliminary analysis of clinical results is corresponding to the chemical gradients parallel to the OA of the lenses which are reported by O. Hockwin after examination on extracted eye lenses. The normalization of the lens densitometric data derived after Scheimpflug- photography against the protein size fraction analysis by DLS is performed. As a comparison mean between both techniques on identical eye lenses, an absorption corrected densitometry is conducted for the first time.

New Programs Utilizing Light Scattering and Flow Imaging Techniques for Macromolecular Crystal Growth and Fluid Dynamics Studies

NASA Technical Reports Server (NTRS)

2003-01-01

Dr. Phil Segre, a physicist by training, is a recent addition to the Biotech group, SD46, having joined NASA in August of 2000. Over the past two years he has been developing a laboratory for the study of macromolecular and protein crystal growth. The main apparatus for this work is a Dynamic Light Scattering apparatus, DLS, which is capable of making highly precise measurements of size distributions of both protein solutions and protein crystals. With Drs. Chernov and Thomas (USRA), he has begun a collaboration studying the affects of protein impurities on protein crystal growth and subsequent crystal quality. One of the hypotheses behind the differences between Earth and space grown protein crystals is that the absorption of harmful impurities is reduced in space due to the absence of convective flows. Using DLS measurements we are examining crystal growth with varying amounts of impurities and testing whether there is a strong physical basis behind this hypothesis. With Dr. Joe Ng of UAH he has been collaborating on a project to examine the folding/unfolding dynamics of large RNA complexes. A detailed understanding of this process is necessary for the handling of RNA in biotech applications, and the DLS instrument gives details and results beyond that of other instruments. With Prof. Jim McClymer of the University of Maine (summer faculty visitor to NASA in 2001, 2002), we have been studying the crystallization process in model colloidal suspensions whose behavior in some cases can mimic that of much smaller protein solutions. An understanding of the self-assembly of colloids is the first step in the process of engineering novel materials for photonic and light switching applications. Finally, he has begun an investigation into the physics of particle sedimentation. In addition to the DLS instrument he also has an instrument (called PIV) that can measure flow fields of fluids. The applications are to the dynamics of protein crystal motions both on earth and in low-gravity.

Casein micelles and their internal structure.

PubMed

de Kruif, Cornelis G; Huppertz, Thom; Urban, Volker S; Petukhov, Andrei V

2012-01-01

The internal structure of casein micelles was studied by calculating the small-angle neutron and X-ray scattering and static light scattering spectrum (SANS, SAXS, SLS) as a function of the scattering contrast and composition. We predicted experimental SANS, SAXS, SLS spectra self consistently using independently determined parameters for composition size, polydispersity, density and voluminosity. The internal structure of the casein micelles, i.e. how the various components are distributed within the casein micelle, was modeled according to three different models advocated in the literature; i.e. the classical sub-micelle model, the nanocluster model and the dual binding model. In this paper we present the essential features of these models and combine new and old experimental SANS, SAXS, SLS and DLS scattering data with new calculations that predict the spectra. Further evidence on micellar substructure was obtained by internally cross linking the casein micelles using transglutaminase, which led to casein nanogel particles. In contrast to native casein micelles, the nanogel particles were stable in 6M urea and after sequestering the calcium using trisodium citrate. The changed scattering properties were again predicted self consistently. An important result is that the radius of gyration is independent of contrast, indicating that the mass distribution within a casein micelle is homogeneous. Experimental contrast is predicted quite well leading to a match point at a D(2)O volume fraction of 0.41 ratio in SANS. Using SANS and SAXS model calculations it is concluded that only the nanocluster model is capable of accounting for the experimental scattering contrast variation data. All features and trends are predicted self consistently, among which the 'famous' shoulder at a wave vector value Q=0.35 nm(-1) In the nanocluster model, the casein micelle is considered as a (homogeneous) matrix of caseins in which the colloidal calcium phosphate (CCP) nanoclusters are dispersed as very small (about 2 nm) "cherry stones" at an average distance of 18.6 nm. Attached to the surface of the nanoclusters are the centers of phosphorylation (3-5 nearby phosphorylated amino acid residues) of the caseins. The tails of the caseins, much larger than the CCP clusters, then associate to form a protein matrix, which can be viewed as polymer mesh with density fluctuations at the 2 nm scale. The association of the tails is driven by a collection of weak interactions. We explicitly use weak interactions as a collective term for hydrophobic interactions, hydrogen bonding, ion bonding, weak electrostatic Van der Waals attraction and other factors (but not the strong calcium phosphate interaction) leading to self association. The association is highly cooperative and originates in the weak interactions. It is the cooperativety that leads to a stable casein micelle. Invariably, κ-casein is thought to limit the process of self association leading to stabilization of the native casein micelle. Copyright © 2012 Elsevier B.V. All rights reserved.

Casein micelles and their internal structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

De Kruif, Cornelis G; Huppertz, Thom; Urban, Volker S

2012-01-01

The internal structure of casein micelles was studied by calculating the small-angle neutron and X-ray scattering and static light scattering spectrum (SANS, SAXS, SLS) as a function of the scattering contrast and composition. We predicted experimental SANS, SAXS, SLS spectra self consistently using independently determined parameters for composition size, polydispersity, density and voluminosity. The internal structure of the casein micelles, i.e. how the various components are distributed within the casein micelle, was modeled according to three different models advocated in the literature; i.e. the classical sub-micelle model, the nanocluster model and the dual binding model. In this paper we presentmore » the essential features of these models and combine new and old experimental SANS, SAXS, SLS and DLS scattering data with new calculations that predict the spectra. Further evidence on micellar substructure was obtained by internally cross linking the casein micelles using transglutaminase, which led to casein nanogel particles. In contrast to native casein micelles, the nanogel particles were stable in 6 M urea and after sequestering the calcium using trisodium citrate. The changed scattering properties were again predicted self consistently. An important result is that the radius of gyration is independent of contrast, indicating that the mass distribution within a casein micelle is homogeneous. Experimental contrast is predicted quite well leading to a match point at a D{sub 2}O volume fraction of 0.41 ratio in SANS. Using SANS and SAXS model calculations it is concluded that only the nanocluster model is capable of accounting for the experimental scattering contrast variation data. All features and trends are predicted self consistently, among which the 'famous' shoulder at a wave vector value Q = 0.35 nm{sup -1}. In the nanocluster model, the casein micelle is considered as a (homogeneous) matrix of caseins in which the colloidal calcium phosphate (CCP) nanoclusters are dispersed as very small (about 2 nm) 'cherry stones' at an average distance of 18.6 nm. Attached to the surface of the nanoclusters are the centers of phosphorylation (3-5 nearby phosphorylated amino acid residues) of the caseins. The tails of the caseins, much larger than the CCP clusters, then associate to form a protein matrix, which can be viewed as polymer mesh with density fluctuations at the 2 nm scale. The association of the tails is driven by a collection of weak interactions. We explicitly use weak interactions as a collective term for hydrophobic interactions, hydrogen bonding, ion bonding, weak electrostatic Van der Waals attraction and other factors (but not the strong calcium phosphate interaction) leading to self association. The association is highly cooperative and originates in the weak interactions. It is the cooperativety that leads to a stable casein micelle. Invariably, K-casein is thought to limit the process of self association leading to stabilization of the native casein micelle.« less

Dispersed SiC nanoparticles in Ni observed by ultra-small-angle X-ray scattering

DOE PAGES

Xie, R.; Ilavsky, J.; Huang, H. F.; ...

2016-11-24

In this paper, a metal-ceramic composite, nickel reinforced with SiC nanoparticles, was synthesized and characterized for its potential application in next-generation molten salt nuclear reactors. Synchrotron ultra-small-angle X-ray scattering (USAXS) measurements were conducted on the composite. The size distribution and number density of the SiC nanoparticles in the material were obtained through data modelling. Scanning and transmission electron microscopy characterization were performed to substantiate the results of the USAXS measurements. Tensile tests were performed on the samples to measure the change in their yield strength after doping with the nanoparticles. Finally, the average interparticle distance was calculated from the USAXSmore » results and is related to the increased yield strength of the composite.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Egorov, V. V., E-mail: vlaegur@omrb.pnpi.spb.ru; Gorshkov, A. N.; Murugova, T. N.

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 ablemore » to influence the protein oligomerization are discussed.« less

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.

Small angle neutron scattering study on the structural variation of lysozyme in bioprotectants

NASA Astrophysics Data System (ADS)

Koda, Shota; Takayama, Haruki; Shibata, Tomohiko; Mori, Tatsuya; Kojima, Seiji; Park, In-Sung; Shin, Tae-Gyu

2015-05-01

The thermal denaturation and subsequent structural variation of lysozyme in various bioprotectant candidate solutions such as trehalose and choline acetate have been investigated by using small angle neutron scattering and differential scanning calorimetry. The gyration radius shows little change with the addition of additives in a native state at room temperature. On heating the lysozyme solution, a remarkable increase in the gyration radius is observed at temperatures above the denaturation temperature without any bioprotectants. Such an increase is suppressed by the additives owing to the intermolecular interactions between the lysozyme molecules and the bioprotectants of trehalose and choline acetate. The fractal dimension of lysozyme varies slightly with the addition of the bioprotectant solutions, and shows a remarkable drop in the vicinity of the denaturation temperature for all the solutions.

Robust, high-throughput solution structural analyses by small angle X-ray scattering (SAXS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hura, Greg L.; Menon, Angeli L.; Hammel, Michal

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 formore » 41 proteins. We believe that high-throughput SAXS is an enabling technology that may change the way that structural genomics research is done.« less

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

PubMed

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

2017-10-01

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

Effect of annealing conditions on the microstructure and magnetic properties of sintered Nd-Fe-B magnets as seen by magnetic small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Périgo, Élio A.; Titov, Ivan; Weber, Raoul; Mettus, Denis; Peral, Inma; Vallcorba, Oriol; Honecker, Dirk; Feoktystov, Artem; Michels, Andreas

2018-03-01

We have investigated the effect of the annealing conditions (heating rate and temperature) on the magnetic microstructure of sintered Nd-Fe-B magnets by means of magnetometry, scanning electron microscopy, high-energy synchrotron x-ray diffraction, and small-angle neutron scattering (SANS). While the temperature treatment has a strong effect on the coercivity (reduction by about 50% on annealing), the associated changes in the microstructure do surprisingly not show up (or at best only very weakly) in the neutron-scattering signal, which probes a mesoscopic real-space length scale ranging between about 1–300 nm. On the other hand, the x-ray data reveal microstructural changes in the Nd-rich phases, presumably due to modifications in grain-boundary regions. Moreover, we observe an unusual diamond-shaped angular anisotropy in the SANS cross section, which strongly points towards the existence of texture in the nuclear microstructure.

All-atom ensemble modeling to analyze small angle X-ray scattering of glycosylated proteins

PubMed Central

Guttman, Miklos; Weinkam, Patrick; Sali, Andrej; Lee, Kelly K.

2013-01-01

Summary The flexible and heterogeneous nature of carbohydrate chains often renders glycoproteins refractory to traditional structure determination methods. Small Angle X-ray scattering (SAXS) can be a useful tool for obtaining structural information of these systems. All-atom modeling of glycoproteins with flexible glycan chains was applied to interpret the solution SAXS data for a set of glycoproteins. For simpler systems (single glycan, with a well defined protein structure), all-atom modeling generates models in excellent agreement with the scattering pattern, and reveals the approximate spatial occupancy of the glycan chain in solution. For more complex systems (several glycan chains, or unknown protein substructure), the approach can still provide insightful models, though the orientations of glycans become poorly determined. Ab initio shape reconstructions appear to capture the global morphology of glycoproteins, but in most cases offer little information about glycan spatial occupancy. The all-atom modeling methodology is available as a webserver at http://modbase.compbio.ucsf.edu/allosmod-foxs. PMID:23473666

Infrastructure development for radioactive materials at the NSLS-II

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sprouster, D. J.; Weidner, R.; Ghose, S. K.

2018-02-01

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this article, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. We describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

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.

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

Infrastructure development for radioactive materials at the NSLS-II

DOE PAGES

Sprouster, David J.; Weidner, R.; Ghose, S. K.; ...

2017-11-04

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this paper, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilitiesmore » at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. Finally, we describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.« less

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

PubMed Central

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

2017-01-01

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takagi, H., E-mail: takagih@post.kek.jp; Igarashi, N.; Mori, T.

BL-6A has been operational since 2011 as a small angle X-ray scattering (SAXS) beamline at the Photon Factory (PF), and beginning in 2013 its old components and systems, which were mainly inside the experimental hutch, have been extensively updated. Both the vacuum-passes located between the sample stage and the detector and the fixed surface plate have been replaced by a new semi-automatic diffractometer. These upgrades allow simultaneous SAXS/WAXS experiments and grazing-incidence small angle X-ray scattering (GISAXS) measurements to be conducted. The hybrid pixel detector PILATUS3 1M is installed for SAXS, and PILATUS 100K is available as a WAXS detector. Additionally,more » a pinhole equipped with a micro-ion chamber is available to realize a lower-background and higher-resolution of low angles. Moreover, in a simultaneous SAXS/WAXS experiment, we developed a new beam stop with an embedded photodiode. Thus, BL-6A has evolved into a multipurpose beamline capable of dealing with various types of samples and experimental techniques.« less

Exact Rayleigh scattering calculations for use with the Nimbus-7 Coastal Zone Color Scanner

NASA Technical Reports Server (NTRS)

Gordon, Howard R.; Brown, James W.; Evans, Robert H.

1988-01-01

The radiance reflected from a plane-parallel atmosphere and flat sea surface in the absence of aerosols has been determined with an exact multiple scattering code to improve the analysis of Nimbus-7 CZCS imagery. It is shown that the single scattering approximation normally used to compute this radiance can result in errors of up to 5 percent for small and moderate solar zenith angles. A scheme to include the effect of variations in the surface pressure in the exact computation of the Rayleigh radiance is discussed. The results of an application of these computations to CZCS imagery suggest that accurate atmospheric corrections can be obtained for solar zenith angles at least as large as 65 deg.

Faraday effect on stimulated Raman scattering in the linear region

NASA Astrophysics Data System (ADS)

Liu, Z. J.; Li, B.; Xiang, J.; Cao, L. H.; Zheng, C. Y.; Hao, L.

2018-04-01

The paper presents the effect of Faraday rotation on stimulated Raman scattering (SRS). When light propagates along the magnetic field upon plasma, Faraday rotation occurs. The rotation angle can be expressed as {{d}}θ /{{d}}{s}=2.93× {10}-4B\\tfrac{{n}e/{n}c}{\\sqrt{1-{n}e/{n}c}} {cm}}-1 approximately, where θ is the rotation angle and s is distance, n e is the electron density, n c is the critical density and B is magnetic field in unit of Gauss. Both the incident light and Raman light have Faraday effects. The angle between the polarization directions of incident light and Raman light changes with position. The driven force of electron plasma wave also reduces, and then SRS scattering level is reduced. Faraday rotation effect can increase the laser intensity threshold of Raman scattering, even if the magnetic field strength is small. The circularly polarized light incident case is also compared with that of the linearly polarized light incident. The Raman scattering level of linearly polarized light is much smaller than that of circularly polarized light in the magnetized plasma. The difference between linearly and circularly polarized lights is also discussed.

Measurements of Euglena motion parameters by laser light scattering.

PubMed Central

Ascoli, C; Barbi, M; Frediani, C; Murè, A

1978-01-01

Measurements of Euglena gracilis motion parameters have been performed by the spectral analysis of the scattered laser light. Samples were oriented by a radiofrequency field to obtain easily interpretable spectra. Cell rotation frequency and flagellar beating frequency distributions were obtained from the homodyne spectra, whereas the Doppler lines obtained at small observation angles by heterodyne detection yielded the swimming speed distributions. We discuss the broadening of the heterodyne spectra at large angles of observation. An application of this method to the study of the photo-kinetic effect is also described. Images FIGURE 3 PMID:104747

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.

Dynamics of Single Chains of Suspended Ferrofluid Particles

NASA Technical Reports Server (NTRS)

Cutillas, S.; Liu, J.

1999-01-01

We present an experimental study of the dynamics of isolated chains made of super-paramagnetic particles under the influence of a magnetic field. The motivation of this work is to understand if the chain fluctuations exist and, if it does, how does the fluctuation affect chain aggregation. We find that single chains strongly fluctuate and that the characteristic frequency of their fluctuations is inversely proportional to the magnetic field strength. The higher the field the lower the characteristic frequency of the chain fluctuations. In the high magnetic field limit, chains behave like rigid rods without any internal motions. In this work, we used ferrofluid particles suspended in water. These particles do not have any intrinsic magnetization. Once a magnetic field is applied, a dipole moment is induced in each particle, proportional to the magnetic field. A dipolar magnetic interaction then occurs between particles. If dipole-dipole magnetic energy is higher than the thermal energy, the result is a structure change inside the dipolar fluid. The ratio of these two energies is expressed by a coupling constant lambda as: lambda = (pi(a(exp 3))(chi(exp 2))(mu(sub 0))(H(sub 0))(exp 2))/18kT Where a is the particle radius, mu(sub 0) is the vacuum magnetic permeability, H(sub 0) the applied magnetic field, k the Boltzmann constant and T the absolute temperature. If lambda > 1, magnetic particles form chains along the field direction. The lateral coalescence of several chains may form bigger aggregates especially if the particle volume fraction is high. While many studies and applications deal with the rheological properties and the structural changes of these dipolar fluids, this work focuses on the understanding of the chain dynamics. In order to probe the chain dynamics, we used dynamic light scattering (DLS) in self-beating mode as our experimental technique. The experimental geometry is such that the scattering plane is perpendicular to the magnetic field. Therefore, only motions in this plane are probed. A very dilute sample of a ferrofluid emulsion with a particle volume fraction of 10(exp -5) is used in this experiment. We chose such a low volume fraction to avoid multiple light scattering as well as lateral chain-chain aggregation. DLS measures the dynamic structure factor S(q,t) of the sample (q is the scattering wave vector, t is the time). In the absence of the magnetic field, identical particles of ferrofluid droplets are randomly distributed and S(q,t) reduces to exp(-q(exp 2)2D(sub 0)t). D(sub 0)=(kT/(6(pi)(eta)(a)) is the diffusion coefficient of Brownian particles (where Xi = (6(pi)(eta)(a)) is the Stokes frictional coefficient of a spherical particle in a fluid of viscosity eta). If interactions or polydispersity can not be ignored, an effective diffusion coefficient is introduced. Formally, D(sub eff) is defined as: D(sub eff) = - q(exp -2) partial derivative of (ln(S(q,t)) with respect to time, as t goes to 0. D(sub eff) reduces to D(sub 0) if no interactions and only a few particles size are present. Therefore, we can use DLS to measure particle size. The particle radius was found to be a=0.23 mu m with 7% of polydispersity. In this case, if we vary the scattering angle theta (and so q) we do not have any change in the measured diffusion coefficient: it is q-independent. When a magnetic field is applied, particles aggregate into chains if lambda > 1. We first studied the kinetics of the chain formation when lambda = 406. At a fixed scattering angle, we measured diffusion coefficient D(sub eff) as a function of time. Experimentally, we find that D(sub eff) decreases monotonously with time. Physically, this means that chains are becoming longer and longer. Since we are only sensitive to motions in the scattering plane and since chains have their main axis perpendicular to this plane, the measured diffusion coefficient is the trans-verse diffusion coefficient. We can relate D(sub eff) to the mean number of particles per chain N(t) at a given time and to the diffusion coefficient of an isolated particle D(sub 0) as D(sub eff)=f(N(t))D(sub 0). Since f(N) is known from other recent work, N can be expressed as a function of the time. We found a square root dependency: N(t) proportional to the square root of t. As expected for very low volume fraction, this behavior is characteristic of a diffusion-limited aggregation as suggested by several authors and by our previous work. In this study, we focus on the dependence of the effective diffusion coefficient on the scattering angle and the magnetic field strength. After the magnetic field is applied (lambda = 406) for a long time, typically 6 hours, kinetics of chain formation becomes very slow. Chain size does not vary much over the next hour period. Thus, we can perform different interesting experiments. First, at a fixed magnetic field, we measure the effective diffusion coefficient as a function of the scattering angle (from 5 to 130 deg). Our results show that the measured diffusion coefficient increases linearly with the scattering angle: D(sub eff) proportional to q. If we do the same experiment for different lambda values, D(sub eff) depends on lambda as D(sub eff) proportional to lambda(exp -1/2). We also find for different lambda values that the same asymptotic D(sub eff) value is obtained when q approaches zero. The angle dependency of D(sub eff) suggests that an additional motion exists besides chain drifting. Chain size is constant during experiment, which was verified by measuring the same diffusion coefficient at the beginning and at the end of the angle switching. If chains are rigid, D(sub eff) is independent of q. Therefore, we found that D(sub eff) not only measures the motion of the entire chain but also its internal fluctuations. These internal motions are the fluctuations of the particles in the chain. To understand the q dependency of D(sub eff), let us look at the probing length used. In our study, the characteristic length scale probed is l=2pi/q which is in the range of 0.9

Halo structure of 8B determined from intermediate energy proton elastic scattering in inverse kinematics

NASA Astrophysics Data System (ADS)

Korolev, G. A.; Dobrovolsky, A. V.; Inglessi, A. G.; Alkhazov, G. D.; Egelhof, P.; Estradé, A.; Dillmann, I.; Farinon, F.; Geissel, H.; Ilieva, S.; Ke, Y.; Khanzadeev, A. V.; Kiselev, O. A.; Kurcewicz, J.; Le, X. C.; Litvinov, Yu. A.; Petrov, G. E.; Prochazka, A.; Scheidenberger, C.; Sergeev, L. O.; Simon, H.; Takechi, M.; Tang, S.; Volkov, V.; Vorobyov, A. A.; Weick, H.; Yatsoura, V. I.

2018-05-01

The absolute differential cross section for small-angle proton elastic scattering on the proton-rich 8B nucleus has been measured in inverse kinematics for the first time. The experiment was performed using a secondary radioactive beam with an energy of 0.7 GeV/u at GSI, Darmstadt. The active target, namely hydrogen-filled time projection ionization chamber IKAR, was used to measure the energy, angle and vertex point of the recoil protons. The scattering angle of the projectiles was simultaneously determined by the tracking detectors. The measured differential cross section is analyzed on the basis of the Glauber multiple scattering theory using phenomenological nuclear-density distributions with two free parameters. The radial density distribution deduced for 8B exhibits a halo structure with the root-mean-square (rms) matter radius Rm = 2.58 (6) fm and the rms halo radius Rh = 4.24 (25) fm. The results on 8B are compared to those on the mirror nucleus 8Li investigated earlier by the same method. A comparison is also made with previous experimental results and theoretical predictions for both nuclei.

Power law relation between particle concentrations and their sizes in the blood plasma

NASA Astrophysics Data System (ADS)

Kirichenko, M. N.; Chaikov, L. L.; Zaritskii, A. R.

2016-08-01

This work is devoted to the investigation of sizes and concentrations of particles in blood plasma by dynamic light scattering (DLS). Blood plasma contains many different proteins and their aggregates, microparticles and vesicles. Their sizes, concentrations and shapes can give information about donor's health. Our DLS study of blood plasma reveals unexpected dependence: with increasing of the particle sizes r (from 1 nm up to 1 μm), their concentrations decrease as r-4 (almost by 12 orders). We found also that such dependence was repeated for model solution of fibrinogen and thrombin with power coefficient is -3,6. We believe that this relation is a fundamental law of nature that shows interaction of proteins (and other substances) in biological liquids.

Selective tuning of the self-assembly and gelation of a hydrophilic poloxamine by cyclodextrins.

PubMed

González-Gaitano, Gustavo; da Silva, Marcelo A; Radulescu, Aurel; Dreiss, Cécile A

2015-05-26

Complexes formed between cyclodextrins (CDs) and polymers - pseudopolyrotaxanes (PPRs) - are the starting point of a multitude of supramolecular structures, which are proposed for a wide range of biomedical and technological applications. In this work, we investigate the complexation of a range of cyclodextrins with Tetronic T1307, a four-arm block copolymer of poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) with a pH-responsive central ethylene diamine spacer, and its impact on micellization and the sol-gel transition. At low concentrations, small-angle neutron scattering (SANS) combined with dynamic light scattering (DLS) measurements show the presence of spherical micelles with a highly hydrated shell and a dehydrated core. Increasing the temperature leads to more compact micelles and larger aggregation numbers, whereas acidic conditions induce a shrinking of the micelles, with fewer unimers per micelle and a more hydrated corona. At high concentrations, T1307 undergoes a sol-gel transition, which is suppressed at pH below the pKa,1 (4.6). SANS data analysis reveals that the gels result from a random packing of the micelles, which have an increasing aggregation number and increasingly dehydrated shell and hydrated core with the temperature. Native CDs (α, β, γ-CD) can complex T1307, resulting in the precipitation of a PPR. Instead, modified CDs compete with micellization to an extent that is critically dependent on the nature of the substitution. (1)H and ROESY NMR combined with SANS demonstrate that dimethylated β-CD can thread onto the polymer, preferentially binding to the PO units, thus hindering self-aggregation by solubilizing the hydrophobic block. The various CDs are able to modulate the onset of gelation and the extent of the gel phase, and the effect correlates with the ability of the CDs to disrupt the micelles, with the exception of a sulfated sodium salt of β-CD, which, while not affecting the CMT, is able to fully suppress the gel phase.

Light scattering from normal and cervical cancer cells.

PubMed

Lin, Xiaogang; Wan, Nan; Weng, Lingdong; Zhou, Yong

2017-04-20

The light scattering characteristic plays a very important role in optic imaging and diagnostic applications. For optical detection of the cell, cell scattering characteristics have an extremely vital role. In this paper, we use the finite-difference time-domain (FDTD) algorithm to simulate the propagation and scattering of light in biological cells. The two-dimensional scattering cell models were set up based on the FDTD algorithm. The cell models of normal cells and cancerous cells were established, and the shapes of organelles, such as mitochondria, were elliptical. Based on these models, three aspects of the scattering characteristics were studied. First, the radar cross section (RCS) distribution curves of the corresponding cell models were calculated, then corresponding relationships between the size and the refractive index of the nucleus and light scattering information were analyzed in the three periods of cell canceration. The values of RCS increase positively with the increase of the nucleo-cytoplasmic ratio in the cancerous process when the scattering angle ranges from 0° to 20°. Second, the effect of organelles in the scattering was analyzed. The peak value of the RCS of cells with mitochondria is higher than the cells without mitochondria when the scattering angle ranges from 20° to 180°. Third, we demonstrated that the influence of cell shape is important, and the impact was revealed by the two typical ideal cells: round cells and oval cells. When the scattering angle ranges from 0° to 80°, the peak values and the frequencies of the appearance of the peaks from the two models are roughly similar. It can be concluded that: (1) the size of the nuclei and the change of the refractive index of cells have a certain impact on light scattering information of the whole cell; (2) mitochondria and other small organelles contribute to the cell light scattering characteristics in the larger scattering angle area; and (3) the change of the cell shape significantly influences the value of scattering peak and the deviation of scattering peak position. The results of the numerical simulation will guide subsequent experiments and early diagnosis of cervical cancer.

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.

Small-angle neutron scattering study of specific interaction and coordination structure formed by mono-acetyl-substituted dibenzo-20-crown-6-ether and cesium ions

DOE PAGES

Motokawa, Ryuhei; Kobayashi, Tohru; Endo, Hitoshi; ...

2015-10-26

This study uses small-angle neutron scattering (SANS) to elucidate the coordination structure of the complex of mono-acetyl-substituted dibenzo-20-crown-6-ether (ace-DB20C6) with cesium ions (Cs +). SANS profiles obtained for the complex of ace-DB20C6 and Cs + (ace-DB20C6/Cs) in deuterated dimethyl sulfoxide indicated that Cs + coordination resulted in a more compact structure than the free ace-DB20C6. The data were fitted well with SANS profiles calculated using Debye function for scattering on an absolute scattering intensity scale. For this theoretical calculation of the scattering profiles, the coordination structure proposed based on density functional theory calculation was used. Furthermore, we conclude that themore » SANS analysis experimentally supports the proposed coordination structure of ace-DB20C6/Cs and suggests the following: (1) the complex of ace-DB20C6 and Cs + is formed with an ace-DB20C6/Cs molar ratio of 1/1 and (2) the two benzene rings of ace-DB20C6 fold around Cs + above the center of the crown ether ring of ace-DB20C6.« less

Measurement of carbon condensates using small-angle x-ray scattering during detonation of high explosives

NASA Astrophysics Data System (ADS)

Willey, T. M.; Bagge-Hansen, M.; Lauderbach, L.; Hodgin, R.; Hansen, D.; May, C.; van Buuren, T.; Dattelbaum, D. M.; Gustavsen, R. L.; Watkins, E. B.; Firestone, M. A.; Jensen, B. J.; Graber, T.; Bastea, S.; Fried, L.

2017-01-01

The lack of experimental validation for processes occurring at sub-micron length scales on time scales ranging from nanoseconds to microseconds hinders detonation model development. Particularly, quantification of late-time energy release requires measurement of carbon condensation kinetics behind detonation fronts. A new small-angle x-ray scattering (SAXS) endstation has been developed for use at The Dynamic Compression Sector to observe carbon condensation during detonation. The endstation and beamline demonstrate unprecedented fidelity; SAXS profiles can be acquired from single x-ray pulses, which in 24-bunch mode are about 80 ps in duration and arrive every 153.4 ns. This paper presents both the current temporal capabilities of this beamline, and the ability to distinguish different carbon condensate morphologies as they form behind detonation fronts. To demonstrate temporal capabilities, three shots acquired during detonation of hexanitrostilbene (HNS) are interleaved to show the evolution of the SAXS in about 50 ns steps. To show fidelity of the SAXS, the scattering from carbon condensates at several hundred nanoseconds varies with explosive: scattering from HNS is consistent with a complex morphology that we assert is associated with sp2 carbon., while Comp B scattering is consistent with soots containing three-dimensional diamond nanoparticles.

Small-angle neutron scattering study of specific interaction and coordination structure formed by mono-acetyl-substituted dibenzo-20-crown-6-ether and cesium ions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Motokawa, Ryuhei; Kobayashi, Tohru; Endo, Hitoshi

This study uses small-angle neutron scattering (SANS) to elucidate the coordination structure of the complex of mono-acetyl-substituted dibenzo-20-crown-6-ether (ace-DB20C6) with cesium ions (Cs +). SANS profiles obtained for the complex of ace-DB20C6 and Cs + (ace-DB20C6/Cs) in deuterated dimethyl sulfoxide indicated that Cs + coordination resulted in a more compact structure than the free ace-DB20C6. The data were fitted well with SANS profiles calculated using Debye function for scattering on an absolute scattering intensity scale. For this theoretical calculation of the scattering profiles, the coordination structure proposed based on density functional theory calculation was used. Furthermore, we conclude that themore » SANS analysis experimentally supports the proposed coordination structure of ace-DB20C6/Cs and suggests the following: (1) the complex of ace-DB20C6 and Cs + is formed with an ace-DB20C6/Cs molar ratio of 1/1 and (2) the two benzene rings of ace-DB20C6 fold around Cs + above the center of the crown ether ring of ace-DB20C6.« less

A generalized quantitative interpretation of dark-field contrast for highly concentrated microsphere suspensions

PubMed Central

Gkoumas, Spyridon; Villanueva-Perez, Pablo; Wang, Zhentian; Romano, Lucia; Abis, Matteo; Stampanoni, Marco

2016-01-01

In X-ray grating interferometry, dark-field contrast arises due to partial extinction of the detected interference fringes. This is also called visibility reduction and is attributed to small-angle scattering from unresolved structures in the imaged object. In recent years, analytical quantitative frameworks of dark-field contrast have been developed for highly diluted monodisperse microsphere suspensions with maximum 6% volume fraction. These frameworks assume that scattering particles are separated by large enough distances, which make any interparticle scattering interference negligible. In this paper, we start from the small-angle scattering intensity equation and, by linking Fourier and real-space, we introduce the structure factor and thus extend the analytical and experimental quantitative interpretation of dark-field contrast, for a range of suspensions with volume fractions reaching 40%. The structure factor accounts for interparticle scattering interference. Without introducing any additional fitting parameters, we successfully predict the experimental values measured at the TOMCAT beamline, Swiss Light Source. Finally, we apply this theoretical framework to an experiment probing a range of system correlation lengths by acquiring dark-field images at different energies. This proposed method has the potential to be applied in single-shot-mode using a polychromatic X-ray tube setup and a single-photon-counting energy-resolving detector. PMID:27734931

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

PubMed

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

2018-01-01

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

EUV-angle resolved scatter (EUV-ARS): a new tool for the characterization of nanometre structures

NASA Astrophysics Data System (ADS)

Fernández Herrero, Analía.; Mentzel, Heiko; Soltwisch, Victor; Jaroslawzew, Sina; Laubis, Christian; Scholze, Frank

2018-03-01

The advance of the semiconductor industry requires new metrology methods, which can deal with smaller and more complex nanostructures. Particularly for inline metrology a rapid, sensitive and non destructive method is needed. Small angle X-ray scattering under grazing incidence has already been investigated for this application and delivers significant statistical information which tracks the profile parameters as well as their variations, i.e. roughness. However, it suffers from the elongated footprint at the sample. The advantage of EUV radiation, with its longer wavelengths, is that larger incidence angles can be used, resulting in a significant reduction of the beam footprint. Targets with field sizes of 100 μm and smaller are accessible with our experimental set-up. We present a new experimental tool for the measurement of small structures based on the capabilities of soft X-ray and EUV scatterometry at the PTB soft X-ray beamline at the electron storage ring BESSY II. PTB's soft X-ray radiometry beamline uses a plane grating monochromator, which covers the spectral range from 0.7 nm to 25 nm and was especially designed to provide highly collimated radiation. An area detector covers the scattered radiation from a grazing exit angle up to an angle of 30° above the sample horizon and the fluorescence emission can be detected with an energy dispersive X-ray silicon drift detector. In addition, the sample can be rotated and linearly moved in vacuum. This new set-up will be used to explore the capabilities of EUV-scatterometry for the characterization of nanometre-sized structures.

Detection of submicron-sized raft-like domains in membranes by small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Pencer, J.; Mills, T.; Anghel, V.; Krueger, S.; Epand, R. M.; Katsaras, J.

2005-12-01

Using coarse grained models of heterogeneous vesicles we demonstrate the potential for small-angle neutron scattering (SANS) to detect and distinguish between two different categories of lateral segregation: 1) unilamellar vesicles (ULV) containing a single domain and 2) the formation of several small domains or “clusters” (~10 nm in radius) on a ULV. Exploiting the unique sensitivity of neutron scattering to differences between hydrogen and deuterium, we show that the liquid ordered (lo) DPPC-rich phase can be selectively labeled using chain deuterated dipalymitoyl phosphatidylcholine (dDPPC), which greatly facilitates the use of SANS to detect membrane domains. SANS experiments are then performed in order to detect and characterize, on nanometer length scales, lateral heterogeneities, or so-called “rafts”, in ~30 nm radius low polydispersity ULV made up of ternary mixtures of phospholipids and cholesterol. For 1:1:1 DOPC:DPPC:cholesterol (DDC) ULV we find evidence for the formation of lateral heterogeneities on cooling below 30 °C. These heterogeneities do not appear when DOPC is replaced by SOPC. Fits to the experimental data using coarse grained models show that, at room temperature, DDC ULV each exhibit approximately 30 domains with average radii of ~10 nm.

Are Planetary Regolith Particles Back Scattering? Response to a Paper by M. Mishchenko

NASA Technical Reports Server (NTRS)

Hapke, Bruce

1996-01-01

In a recent paper Mishchenko asserts that soil particles are strongly forward scattering, whereas particles on the surfaces of objects in the solar system have been inferred to be back scattering. Mishchenko suggests that this apparent discrepancy is an artifact caused by using an approximate light scattering model to analyse the data, and that planetary regolith particles are actually strong forward scatterers. The purpose of the present paper is to point out the errors in Mishchenko's paper and to show from both theoretical arguments and experimental data that inhomogencous composite particles which are large compared to the wavelength of visible light, such as rock fragments and agglutinates, can be strongly back scattering and are the fundamental scatterers in media composed of them. Such particles appear to be abundant in planetary regoliths and can account for the back scattering character of the surfaces of many bodies in the solar system. If the range of phase angles covered by a data set is insufficient, serious errors in retrieving the particle scattering properties can result whether an exact or approximate scattering model is used. However, if the data set includes both large and small phase angles, approximate regolith scattering models can correctly retrieve the sign of the particle scattering asymmetry.

Effect of enzymatic hydrolysis on native starch granule structure.

PubMed

Blazek, Jaroslav; Gilbert, Elliot Paul

2010-12-13

Enzymatic digestion of six starches of different botanical origin was studied in real time by in situ time-resolved small-angle neutron scattering (SANS) and complemented by the analysis of native and digested material by X-ray diffraction, differential scanning calorimetry, small-angle X-ray scattering, and scanning electron microscopy with the aim of following changes in starch granule nanostructure during enzymatic digestion. This range of techniques enables coverage over five orders of length-scale, as is necessary for this hierarchically structured material. Starches studied varied in their digestibility and displayed structural differences in the course of enzymatic digestion. The use of time-resolved SANS showed that solvent-drying of digested residues does not induce any structural artifacts on the length scale followed by small-angle scattering. In the course of digestion, the lamellar peak intensity gradually decreased and low-q scattering increased. These trends were more substantial for A-type than for B-type starches. These observations were explained by preferential digestion of the amorphous growth rings. Hydrolysis of the semicrystalline growth rings was explained on the basis of a liquid-crystalline model for starch considering differences between A-type and B-type starches in the length and rigidity of amylopectin spacers and branches. As evidenced by differing morphologies of enzymatic attack among varieties, the existence of granular pores and channels and physical penetrability of the amorphous growth ring affect the accessibility of the enzyme to the substrate. The combined effects of the granule microstructure and the nanostructure of the growth rings influence the opportunity of the enzyme to access its substrate; as a consequence, these structures determine the enzymatic digestibility of granular starches more than the absolute physical densities of the amorphous growth rings and amorphous and crystalline regions of the semicrystalline growth rings.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Fan; Levine, Lyle E.; Allen, Andrew J.

The precipitate structure and precipitation kinetics in an Al-Cu-Mg alloy (AA2024) aged at 190 °C, 208 °C, and 226 °C have been studied using ex situ Transmission Electron Microscopy (TEM) and in situ synchrotron-based, combined ultra-small angle X-ray scattering, small angle X-ray scattering (SAXS), and wide angle X-ray scattering (WAXS) across a length scale from sub-Angstrom to several micrometers. TEM brings information concerning the nature, morphology, and size of the precipitates while SAXS and WAXS provide qualitative and quantitative information concerning the time-dependent size and volume fraction evolution of the precipitates at different stages of the precipitation sequence. Within themore » experimental time resolution, precipitation at these ageing temperatures involves dissolution of nanometer-sized small clusters and formation of the planar S phase precipitates. Using a three-parameter scattering model constructed on the basis of TEM results, we established the temperature-dependent kinetics for the cluster-dissolution and S-phase formation processes simultaneously. These two processes are shown to have different kinetic rates, with the cluster-dissolution rate approximately double the S-phase formation rate. We identified a dissolution activation energy at (149.5 ± 14.6) kJ mol-1, which translates to (1.55 ± 0.15) eV/atom, as well as an activation energy for the formation of S precipitates at (129.2 ± 5.4) kJ mol-1, i.e. (1.33 ± 0.06) eV/atom. Importantly, the SAXS/WAXS results show the absence of an intermediate Guinier-Preston Bagaryatsky 2 (GPB2)/S" phase in the samples under the experimental ageing conditions. These results are further validated by precipitation simulations that are based on Langer-Schwartz theory and a Kampmann-Wagner numerical method.« less

PARTITIONING OF PERFLUOROOCTANOATE INTO PHOSPHATIDYLCHOLINE BILAYERS IS CHAIN LENGTH-INDEPENDENT

PubMed Central

Xie, Wei; Bothun, Geoffrey D.; Lehmler, Hans-Joachim

2010-01-01

The chain length dependence of the interaction of PFOA, a persistent environmental contaminant, with dimyristoyl- (DMPC), dipalmitoyl- (DPPC) and distearoylphosphatidylcholine (DSPC) was investigated using steady-state fluorescence anisotropy spectroscopy, differential scanning calorimetry (DSC) and dynamic light scattering (DLS). PFOA caused a linear depression of the main phase transition temperature Tm while increasing the width of the phase transition of all three phosphatidylcholines. Although PFOA’s effect on the on Tm and the transition width decreased in the order DMPC > DPPC > DSPC, its relative effect on the phase behavior was largely independent of the phosphatidylcholine. PFOA caused swelling of DMPC but not DPPC and DSPC liposomes at 37°C in the DLS experiments, which suggests that PFOA partitions more readily into bilayers in the fluid phase. These findings suggest that PFOA’s effect on the phase behavior of phosphatidylcholines depends on the cooperativity and state (i.e., gel versus liquid phase) of the membrane. DLS experiments are also consistent with partial liposome solubilization at PFOA/lipid molar ratios > 1, which suggests the formation of mixed PFOA-lipid micelles. PMID:20096277

Dependence of the forward light scattering on the refractive index of particles

NASA Astrophysics Data System (ADS)

Guo, Lufang; Shen, Jianqi

2018-05-01

In particle sizing technique based on forward light scattering, the scattered light signal (SLS) is closely related to the relative refractive index (RRI) of the particles to the surrounding, especially when the particles are transparent (or weakly absorbent) and the particles are small in size. The interference between the diffraction (Diff) and the multiple internal reflections (MIR) of scattered light can lead to the oscillation of the SLS on RRI and the abnormal intervals, especially for narrowly-distributed small particle systems. This makes the inverse problem more difficult. In order to improve the inverse results, Tikhonov regularization algorithm with B-spline functions is proposed, in which the matrix element is calculated for a range of particle sizes instead using the mean particle diameter of size fractions. In this way, the influence of abnormal intervals on the inverse results can be eliminated. In addition, for measurements on narrowly distributed small particles, it is suggested to detect the SLS in a wider scattering angle to include more information.

Estimation and modeling of coal pore accessibility using small angle neutron scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Rui; Liu, Shimin; Bahadur, Jitendra

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 (CD 4) at lowmore » 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 CD 4 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

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 (CD 4) at lowmore » 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 CD 4 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

Magnetic small-angle neutron scattering on bulk metallic glasses: A feasibility study for imaging displacement fields

NASA Astrophysics Data System (ADS)

Mettus, Denis; Deckarm, Michael; Leibner, Andreas; Birringer, Rainer; Stolpe, Moritz; Busch, Ralf; Honecker, Dirk; Kohlbrecher, Joachim; Hautle, Patrick; Niketic, Nemanja; Fernández, Jesús Rodríguez; Barquín, Luis Fernández; Michels, Andreas

2017-12-01

Magnetic-field-dependent small-angle neutron scattering (SANS) has been utilized to study the magnetic microstructure of bulk metallic glasses (BMGs). In particular, the magnetic scattering from soft magnetic Fe70Mo5Ni5P12.5B2.5C5 and hard magnetic (Nd60Fe30Al10) 92Ni8 alloys in the as-prepared, aged, and mechanically deformed state is compared. While the soft magnetic BMGs exhibit a large field-dependent SANS response with perturbations originating predominantly from spatially varying magnetic anisotropy fields, the SANS cross sections of the hard magnetic BMGs are only weakly dependent on the field, and their angular anisotropy indicates the presence of scattering contributions due to spatially dependent saturation magnetization. Moreover, we observe an unusual increase in the magnetization of the rare-earth-based alloy after deformation. Analysis of the SANS cross sections in terms of the correlation function of the spin misalignment reveals the existence of field-dependent anisotropic long-wavelength magnetization fluctuations on a scale of a few tens of nanometers. We also give a detailed account of how the SANS technique relates to unraveling displacement fields on a mesoscopic length scale in disordered magnetic materials.

Angular distribution of elastic scattering induced by 17F on medium-mass target nuclei at energies near the Coulomb barrier

NASA Astrophysics Data System (ADS)

Zhang, G. L.; Zhang, G. X.; Lin, C. J.; Lubian, J.; Rangel, J.; Paes, B.; Ferreira, J. L.; Zhang, H. Q.; Qu, W. W.; Jia, H. M.; Yang, L.; Ma, N. R.; Sun, L. J.; Wang, D. X.; Zheng, L.; Liu, X. X.; Chu, X. T.; Yang, J. C.; Wang, J. S.; Xu, S. W.; Ma, P.; Ma, J. B.; Jin, S. L.; Bai, Z.; Huang, M. R.; Zang, H. L.; Yang, B.; Liu, Y.

2018-04-01

The elastic scattering angular distributions were measured for 50- and 59-MeV 17F radioactive ion beam on a 89Y target. The aim of this work is to study the effect of the breakup of the proton halo projectile on the elastic scattering angular distribution. The experimental data were analyzed by means of the optical model with the double-folding São Paulo potential for both real and imaginary parts. The theoretical calculations reproduced the experimental data reasonably well. It is shown that the method of the data analysis is correct. In order to clarify the difference observed at large angles for the 59-MeV incident energy data, Continuum-Discretized Coupled-Channels (CDCC) calculations were performed to consider the breakup coupling effect. It is found that the experimental data show the Coulomb rainbow peak and that the effect of the coupling to the continuum states is not very significant, producing only a small hindrance of the Coulomb rainbow peak and a very small enhancement of the elastic scattering angular distribution at backward angles, suggesting that the multipole response of the neutron halo projectiles is stronger than that of the proton halo systems.

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.

Structural hierarchy of chromatin in chicken erythrocyte nuclei based on small-angle neutron scattering: Fractal nature of the large-scale chromatin organization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lebedev, D. V., E-mail: isaev@omrb.pnpi.spb.ru; Filatov, M. V.; Kuklin, A. I.

The chromatin organization in chicken erythrocyte nuclei was studied by small-angle neutron scattering in the scattering-vector range from 1.5 x 10{sup -1} to 10{sup -4} A{sup -1} with the use of the contrast-variation technique. This scattering-vector range corresponds to linear dimensions from 4 nm to 6 {mu}m and covers the whole hierarchy of chromatin structures, from the nucleosomal structure to the entire nucleus. The results of the present study allowed the following conclusions to be drawn: (1) both the chromatin-protein structure and the structure of the nucleic acid component in chicken erythrocyte nuclei have mass-fractal properties, (2) the structure ofmore » the protein component of chromatin exhibits a fractal behavior on scales extending over two orders of magnitude, from the nucleosomal size to the size of an entire nucleus, and (3) the structure of the nucleic acid component of chromatin in chicken erythrocyte nuclei is likewise of a fractal nature and has two levels of organization or two phases with the crossover point at about 300-400 nm.« less

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.

Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

PubMed Central

Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole

2016-01-01

The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles. PMID:26917133

The loss rates of O+ in the inner magnetosphere caused by both magnetic field line curvature scattering and charge exchange reactions

NASA Astrophysics Data System (ADS)

Ji, Y.; Shen, C.

2014-03-01

With consideration of magnetic field line curvature (FLC) pitch angle scattering and charge exchange reactions, the O+ (>300 keV) in the inner magnetosphere loss rates are investigated by using an eigenfunction analysis. The FLC scattering provides a mechanism for the ring current O+ to enter the loss cone and influence the loss rates caused by charge exchange reactions. Assuming that the pitch angle change is small for each scattering event, the diffusion equation including a charge exchange term is constructed and solved; the eigenvalues of the equation are identified. The resultant loss rates of O+ are approximately equal to the linear superposition of the loss rate without considering the charge exchange reactions and the loss rate associated with charge exchange reactions alone. The loss time is consistent with the observations from the early recovery phases of magnetic storms.

Emission-angle and polarization-rotation effects in the lensed CMB

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lewis, Antony; Hall, Alex; Challinor, Anthony, E-mail: antony@cosmologist.info, E-mail: ahall@roe.ac.uk, E-mail: a.d.challinor@ast.cam.ac.uk

Lensing of the CMB is an important effect, and is usually modelled by remapping the unlensed CMB fields by a lensing deflection. However the lensing deflections also change the photon path so that the emission angle is no longer orthogonal to the background last-scattering surface. We give the first calculation of the emission-angle corrections to the standard lensing approximation from dipole (Doppler) sources for temperature and quadrupole sources for temperature and polarization. We show that while the corrections are negligible for the temperature and E-mode polarization, additional large-scale B-modes are produced with a white spectrum that dominates those from post-Bornmore » field rotation (curl lensing). On large scales about one percent of the total lensing-induced B-mode amplitude is expected to be due to this effect. However, the photon emission angle does remain orthogonal to the perturbed last-scattering surface due to time delay, and half of the large-scale emission-angle B modes cancel with B modes from time delay to give a total contribution of about half a percent. While not important for planned observations, the signal could ultimately limit the ability of delensing to reveal low amplitudes of primordial gravitational waves. We also derive the rotation of polarization due to multiple deflections between emission and observation. The rotation angle is of quadratic order in the deflection angle, and hence negligibly small: polarization typically rotates by less than an arcsecond, orders of magnitude less than a small-scale image rotates due to post-Born field rotation (which is quadratic in the shear). The field-rotation B modes dominate the other effects on small scales.« less

Diffraction evidence for the structure of cellulose microfibrils in bamboo, a model for grass and cereal celluloses.

PubMed

Thomas, Lynne H; Forsyth, V Trevor; Martel, Anne; Grillo, Isabelle; Altaner, Clemens M; Jarvis, Michael C

2015-06-23

Cellulose from grasses and cereals makes up much of the potential raw material for biofuel production. It is not clear if cellulose microfibrils from grasses and cereals differ in structure from those of other plants. The structures of the highly oriented cellulose microfibrils in the cell walls of the internodes of the bamboo Pseudosasa amabilis are reported. Strong orientation facilitated the use of a range of scattering techniques. Small-angle neutron scattering provided evidence of extensive aggregation by hydrogen bonding through the hydrophilic edges of the sheets of chains. The microfibrils had a mean centre-to-centre distance of 3.0 nm in the dry state, expanding on hydration. The expansion on hydration suggests that this distance between centres was through the hydrophilic faces of adjacent microfibrils. However in the other direction, perpendicular to the sheets of chains, the mean, disorder-corrected Scherrer dimension from wide-angle X-ray scattering was 3.8 nm. It is possible that this dimension is increased by twinning (crystallographic coalescence) of thinner microfibrils over part of their length, through the hydrophobic faces. The wide-angle scattering data also showed that the microfibrils had a relatively large intersheet d-spacing and small monoclinic angle, features normally considered characteristic of primary-wall cellulose. Bamboo microfibrils have features found in both primary-wall and secondary-wall cellulose, but are crystallographically coalescent to a greater extent than is common in celluloses from other plants. The extensive aggregation and local coalescence of the microfibrils are likely to have parallels in other grass and cereal species and to influence the accessibility of cellulose to degradative enzymes during conversion to liquid biofuels.

Determination of line profiles on nano-structured surfaces using EUV and x-ray scattering

NASA Astrophysics Data System (ADS)

Soltwisch, Victor; Wernecke, Jan; Haase, Anton; Probst, Jürgen; Schoengen, Max; Krumrey, Michael; Scholze, Frank; Pomplun, Jan; Burger, Sven

2014-09-01

Non-imaging techniques like X-ray scattering are supposed to play an important role in the further development of CD metrology for the semiconductor industry. Grazing Incidence Small Angle X-ray Scattering (GISAXS) provides directly assessable information on structure roughness and long-range periodic perturbations. The disadvantage of the method is the large footprint of the X-ray beam on the sample due to the extremely shallow angle of incidence. This can be overcome by using wavelengths in the extreme ultraviolet (EUV) spectral range, EUV small angle scattering (EUVSAS), which allows for much steeper angles of incidence but preserves the range of momentum transfer that can be observed. Generally, the potentially higher momentum transfer at shorter wavelengths is counterbalanced by decreasing diffraction efficiency. This results in a practical limit of about 10 nm pitch for which it is possible to observe at least the +/- 1st diffraction orders with reasonable efficiency. At the Physikalisch-Technische Bundesanstalt (PTB), the available photon energy range extends from 50 eV up to 10 keV at two adjacent beamlines. PTB commissioned a new versatile Ellipso-Scatterometer which is capable of measuring 6" square substrates in a clean, hydrocarbon-free environment with full flexibility regarding the direction of the incident light polarization. The reconstruction of line profiles using a geometrical model with six free parameters, based on a finite element method (FEM) Maxwell solver and a particle swarm based least-squares optimization yielded consistent results for EUV-SAS and GISAXS. In this contribution we present scatterometry data for line gratings and consistent reconstruction results of the line geometry for EUV-SAS and GISAXS.

Characterization of the shape and line-edge roughness of polymer gratings with grazing incidence small-angle X-ray scattering and atomic force microscopy

DOE PAGES

Suh, Hyo Seon; Chen, Xuanxuan; Rincon-Delgadillo, Paulina A.; ...

2016-04-22

Grazing-incidence small-angle X-ray scattering (GISAXS) is increasingly used for the metrology of substrate-supported nanoscale features and nanostructured films. In the case of line gratings, where long objects are arranged with a nanoscale periodicity perpendicular to the beam, a series of characteristic spots of high-intensity (grating truncation rods, GTRs) are recorded on a two-dimensional detector. The intensity of the GTRs is modulated by the three-dimensional shape and arrangement of the lines. Previous studies aimed to extract an average cross-sectional profile of the gratings, attributing intensity loss at GTRs to sample imperfections. Such imperfections are just as important as the average shapemore » when employing soft polymer gratings which display significant line-edge roughness. Herein are reported a series of GISAXS measurements of polymer line gratings over a range of incident angles. Both an average shape and fluctuations contributing to the intensity in between the GTRs are extracted. Lastly, the results are critically compared with atomic force microscopy (AFM) measurements, and it is found that the two methods are in good agreement if appropriate corrections for scattering from the substrate (GISAXS) and contributions from the probe shape (AFM) are accounted for.« less

Carbon Condensation during High Explosive Detonation with Time Resolved Small Angle X-ray Scattering

NASA Astrophysics Data System (ADS)

Hammons, Joshua; Bagge-Hansen, Michael; Nielsen, Michael; Lauderbach, Lisa; Hodgin, Ralph; Bastea, Sorin; Fried, Larry; May, Chadd; Sinclair, Nicholas; Jensen, Brian; Gustavsen, Rick; Dattelbaum, Dana; Watkins, Erik; Firestone, Millicent; Ilavsky, Jan; van Buuren, Tony; Willey, Trevor; Lawrence Livermore National Lab Collaboration; Los Alamos National Laboratory Collaboration; Washington State University/Advanced Photon Source Team

Carbon condensation during high-energy detonations occurs under extreme conditions and on very short time scales. Understanding and manipulating soot formation, particularly detonation nanodiamond, has attracted the attention of military, academic and industrial research. An in-situ characterization of these nanoscale phases, during detonation, is highly sought after and presents a formidable challenge even with today's instruments. Using the high flux available with synchrotron X-rays, pink beam small angle X-ray scattering is able to observe the carbon phases during detonation. This experimental approach, though powerful, requires careful consideration and support from other techniques, such as post-mortem TEM, EELS and USAXS. We present a comparative survey of carbon condensation from different CHNO high explosives. This work was performed under the auspices of the US DOE by LLNL under Contract DE-AC52-07NA27344.

Agglomeration dynamics of germanium islands on a silicon oxide substrate: A grazing incidence small-angle x-ray scattering study

NASA Astrophysics Data System (ADS)

Cheynis, F.; Leroy, F.; Passanante, T.; Müller, P.

2013-04-01

Grazing-incidence small-angle X-ray scattering (GISAXS) and grazing-incidence X-ray diffraction techniques are used to characterise the thermally induced solid-state dewetting of Ge(001) thin films leading to the formation of 3D Ge islands. A quantitative analysis based on the Kolmogorov-Johnson-Mehl-Avrami model is derived. The main physical parameters controlling the dewetting (activation energy and kinetic pre-factors) are determined. Assuming that the dewetting is driven by surface/interface minimisation and limited by surface diffusion, the Ge surface self-diffusion reads as Ds ,0c0 e-Ea/(kBT) ˜3×1018 e-2.6±0.3eV/(kBT) nm2/s. GISAXS technique enables to reconstruct the mean Ge-island shape, including facets.

Mapping the structural order of laser-induced periodic surface structures in thin polymer films by microfocus beam grazing incidence small-angle X-ray scattering.

PubMed

Martín-Fabiani, Ignacio; Rebollar, Esther; García-Gutiérrez, Mari Cruz; Rueda, Daniel R; Castillejo, Marta; Ezquerra, Tiberio A

2015-02-11

In this work we present an accurate mapping of the structural order of laser-induced periodic surface structures (LIPSS) in spin-coated thin polymer films, via a microfocus beam grazing incidence small-angle X-ray scattering (μGISAXS) scan, GISAXS modeling, and atomic force microscopy imaging all along the scanned area. This combined study has allowed the evaluation of the effects on LIPSS formation due to nonhomogeneous spatial distribution of the laser pulse energy, mapping with micrometric resolution the evolution of the period and degree of structural order of LIPSS across the laser beam diameter in a direction perpendicular to the polarization vector. The experiments presented go one step further toward controlling nanostructure formation in LIPSS through a deep understanding of the parameters that influence this process.

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

PubMed

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

2014-11-01

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

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

Supramolecular structure of methyl cellulose and lambda- and kappa-carrageenan in water: SAXS study using the string-of-beads model.

PubMed

Dogsa, Iztok; Cerar, Jure; Jamnik, Andrej; Tomšič, Matija

2017-09-15

A detailed data analysis utilizing the string-of-beads model was performed on experimental small-angle X-ray scattering (SAXS) curves in a targeted structural study of three, very important, industrial polysaccharides. The results demonstrate the quality of performance for this model on three polymers with quite different thermal structural behavior. Furthermore, they show the advantages of the model used by way of excellent fits in the ranges where the classic approach to the small-angle scattering data interpretation fails and an additional 3D visualization of the model's molecular conformations and anticipated polysaccharide supramolecular structure. The importance of this study is twofold: firstly, the methodology used and, secondly, the structural details of important biopolymers that are widely applicable in practice. Copyright © 2017 Elsevier Ltd. All rights reserved.

Pressure-jump small-angle x-ray scattering detected kinetics of staphylococcal nuclease folding.

PubMed Central

Woenckhaus, J; Köhling, R; Thiyagarajan, P; Littrell, K C; Seifert, S; Royer, C A; Winter, R

2001-01-01

The kinetics of chain disruption and collapse of staphylococcal nuclease after positive or negative pressure jumps was monitored by real-time small-angle x-ray scattering under pressure. We used this method to probe the overall conformation of the protein by measuring its radius of gyration and pair-distance-distribution function p(r) which are sensitive to the spatial extent and shape of the particle. At all pressures and temperatures tested, the relaxation profiles were well described by a single exponential function. No fast collapse was observed, indicating that the rate limiting step for chain collapse is the same as that for secondary and tertiary structure formation. Whereas refolding at low pressures occurred in a few seconds, at high pressures the relaxation was quite slow, approximately 1 h, due to a large positive activation volume for the rate-limiting step for chain collapse. A large increase in the system volume upon folding implies significant dehydration of the transition state and a high degree of similarity in terms of the packing density between the native and transition states in this system. This study of the time-dependence of the tertiary structure in pressure-induced folding/unfolding reactions demonstrates that novel information about the nature of protein folding transitions and transition states can be obtained from a combination of small-angle x-ray scattering using high intensity synchrotron radiation with the high pressure perturbation technique. PMID:11222312

Free–free experiments: the search for dressed atom effects

NASA Astrophysics Data System (ADS)

Martin, N. L. S.; Weaver, C. M.; Kim, B. N.; deHarak, B. A.

2018-07-01

Experiments on free–free electron scattering, specifically the absorption or emission of 1.17 eV photons from a Nd:YAG laser field by an unbound electron when it is scattered by an atom or molecule, are reviewed. For large scattering angles such experiments are well described by a simple analytical theory that is independent of the properties of the target. At small scattering angles this theory breaks down for targets with a high dipole polarizability α, and an additional term needs to be incorporated in the scattering amplitude. This term is proportional to the dipole polarizability, and hence introduces the properties of the target into the free–free cross section—i.e., the laser field ‘dresses’ the atom. A progress report is given of free–free experiments designed to look for such ‘dressed atom’ effects during the electron-impact excitation of argon in the presence of a laser field; the lowest excited states of argon have α ≈ 300 atomic units.

Conformations of gelatin in trivalent chromium salt solutions: Viscosity and dynamic light scattering study

NASA Astrophysics Data System (ADS)

Qiao, Congde; Zhang, Jianlong; Kong, Aiqun

2017-02-01

An investigation of the influences of pH, salt type, and salt concentration on the conformations of gelatin molecules in trivalent chromium salt solutions was performed by viscosity and dynamic light scattering (DLS) techniques. It was found that the viscosity behaviors as polyelectrolytes or polyampholytes depended on the charge distribution on the gelatin chains, which can be tuned by the value of pH of the gelatin solution. The intrinsic viscosity of gelatin in basic chromium sulfate aqueous solution at pH = 2.0 first decreased and then increased with increasing Cr(OH)SO4 concentration, while a monotonic decrease of the intrinsic viscosity of gelatin was observed in CrCl3 solution. However, the intrinsic viscosity of gelatin at pH = 5.0 was found to be increased first and then decreased with an increase in salt concentration in Cr(OH)SO4 solution, as well as in CrCl3 solution. We suggested that the observed viscosity behavior of gelatin in trivalent chromium salt solutions was attributed to the comprehensive effects of shielding, overcharging, and crosslinking (complexation) caused by the introduction of the different counterions. In addition, the average hydrodynamic radius ( R h ) of gelatin molecules in various salt solutions was determined by DLS. It was found that the change trend of R h with salt concentration was the same as the change of intrinsic viscosity. Based on the results of the viscosity and DLS, a possible mechanism for the conformational transition of gelatin chains with external conditions including pH, salt concentration, and salt type is proposed.

Fast, quantitative, and nondestructive evaluation of hydrided LWR fuel cladding by small angle incoherent neutron scattering of hydrogen

DOE PAGES

Yan, Y.; Qian, S.; Littrell, K.; ...

2015-02-13

A non-destructive neutron scattering method to precisely measure the uptake of hydrogen and the distribution of hydride precipitates in light water reactor (LWR) fuel cladding was developed. Zircaloy-4 cladding used in commercial LWRs was used to produce hydrided specimens. The hydriding apparatus consists of a closed stainless steel vessel that contains Zr alloy specimens and hydrogen gas. Following hydrogen charging, the hydrogen content of the hydrided specimens was measured using the vacuum hot extraction method, by which the samples with desired hydrogen concentration were selected for the neutron study. Optical microscopy shows that our hydriding procedure results in uniform distributionmore » of circumferential hydrides across the wall. Small angle neutron incoherent scattering was performed in the High Flux Isotope Reactor at Oak Ridge National Laboratory. This study demonstrates that the hydrogen in commercial Zircaloy-4 cladding can be measured very accurately in minutes by this nondestructive method over a wide range of hydrogen concentrations from a very small amount ( 20 ppm) to over 1000 ppm. The hydrogen distribution in a tube sample was obtained by scaling the neutron scattering rate with a factor determined by a calibration process using standard, destructive direct chemical analysis methods on the specimens. This scale factor will be used in future tests with unknown hydrogen concentrations, thus providing a nondestructive method for absolute hydrogen concentration determination.« less

Dynamics of microemulsions bridged with hydrophobically end-capped star polymers studied by neutron spin-echo

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoffmann, I., E-mail: ingo.hoffmann@tu-berlin.de; Institut Max von Laue-Paul Langevin; Malo de Molina, Paula

2014-01-21

The mesoscopic dynamical properties of oil-in-water microemulsions (MEs) bridged with telechelic polymers of different number of arms and with different lengths of hydrophobic stickers were studied with neutron spin-echo (NSE) probing the dynamics in the size range of individual ME droplets. These results then were compared to those of dynamicic light scattering (DLS) which allow to investigate the dynamics on a much larger length scale. Studies were performed as a function of the polymer concentration, number of polymer arms, and length of the hydrophobic end-group. In general it is observed that the polymer bridging has a rather small influence onmore » the local dynamics, despite the fact that the polymer addition leads to an increase of viscosity by several orders of magnitude. In contrast to results from rheology and DLS, where the dynamics on much larger length and time scales are observed, NSE shows that the linear polymer is more efficient in arresting the motion of individual ME droplets. This finding can be explained by a simple simulation, merely by the fact that the interconnection of droplets becomes more efficient with a decreasing number of arms. This means that the dynamics observed on the short and on the longer length scale depend in an opposite way on the number of arms and hydrophobic stickers.« less

Structural, chemical and optical properties of SnO2 NPs obtained by three different synthesis routes

NASA Astrophysics Data System (ADS)

Drzymała, Elżbieta; Gruzeł, Grzegorz; Depciuch, Joanna; Budziak, Andrzej; Kowal, Andrzej; Parlinska-Wojtan, Magdalena

2017-08-01

Polyol (P), chemical precipitation (C) and microwave-assisted (M) syntheses were chosen to produce SnO2 nanoparticles with uniform size and minimum agglomeration. Their structural, chemical and optical properties were investigated using dynamic light scattering (DLS), scanning transmission electron microscopy (STEM), Raman, Fourier Transform Infrared (FTIR) using the Attenuated Total Reflectance (ATR) technique and Ultraviolet-Visible (UV-Vis) spectroscopies. STEM observations showed that the SnO2(P) and SnO2(C) nanoparticles (NPs) are combined into larger agglomerates with heterogeneous thickness, while the microwave-assisted NPs form a uniform thin layer across the TEM grid. The strongest agglomeration of the SnO2(C) NPs, observed by DLS, STEM and UV-Vis is explained by the very moderate amount of water present on the surface of the NPs identified by FTIR spectroscopy. High resolution STEM combined with SAED and X-ray diffraction (XRD) patterns confirmed the crystalline character of the NPs. In the nanoparticles from polyol synthesis, chlorine from the remains of metal precursors during reduction was detected by energy dispersive spectroscopy (EDS), contrary to the NPs obtained by the chemical precipitation and microwave-assisted methods. All three syntheses routes lead to small, 2-10 nm SnO2 NPs, which were the result of the low concentration of Cl ions in the solutions.

Development of Multi-Field of view-Multiple-Scattering-Polarization Lidar ： analysis of angular resolved backscattered signals

NASA Astrophysics Data System (ADS)

Makino, T.; Okamoto, H.; Sato, K.; Tanaka, K.; Nishizawa, T.; Sugimoto, N.; Matsui, I.; Jin, Y.; Uchiyama, A.; Kudo, R.

2014-12-01

We have developed a new type of ground-based lidar, Multi-Field of view-Multiple-Scattering-Polarization Lidar (MFMSPL), to analyze multiple scattering contribution due to low-level clouds. One issue of the ground based lidar is the limitation of optical thickness of about 3 due to the strong attenuation in the lidar signals so that only the cloud bottom part can be observed. In order to overcome the problem, we have proposed the MFMSPL that has been designed to observe similar degree of multiple scattering contribution expected from space-borne lidar CALIOP on CALIPSO satellite. The system consists of eight detectors; four telescopes for parallel channels and four for perpendicular channels. The four pairs of telescope have been mounted with four different off-beam angles, ranging from -5 to 35mrad, where the angle is defined as the one between the direction of laser beam and the direction of telescope. Consequently, similar large foot print (100m) as CALIOP can be achieved in the MFMSPL observations when the altitude of clouds is located at about 1km. The use of multi-field of views enables to measure depolarization ratio from optically thick clouds. The outer receivers attached with larger angles generally detect backscattered signals from clouds located at upper altitudes due to the enhanced multiple scattering compared with the inner receiver that detects signals only from cloud bottom portions. Therefore the information of cloud microphysics from optically thicker regions is expected by the MFMSPL observations compared with the conventional lidar with small FOV. The MFMSPL have been continuously operated in Tsukuba, Japan since June 2014.Initial analyses have indicated expected performances from the theoretical estimation by backward Monte-Carlo simulations. The depolarization ratio from deeper part of the clouds detected by the receiver with large off-beam angle showed much larger values than those from the one with small angle. The calibration procedures and summary of initial observations will be presented. The observed data obtained by the MFMSPL will be used to develop and evaluate the retrieval algorithms for cloud microphysics applied to the CALIOP data.

Multiple scattering in particulate planetary surfaces

NASA Astrophysics Data System (ADS)

Muinonen, Karri; Peltoniemi, Jouni; Markkanen, Johannes; Penttilä, Antti; Videen, Gorden

2015-08-01

There are two ubiquitous phenomena observed at small solar phase angles (the Sun-Object-Observer angle) from, for example, asteroids and transneptunian objects. First, a nonlinear increase of brightness is observed toward the zero phase angle in the magnitude scale that is commonly called the opposition effect. Second, the scattered light is observed to be partially linearly polarized parallel to the Sun-Object-Observer plane that iscommonly called the negative polarization surge.The observations can be interpreted using a radiative-transfer coherent-backscattering Monte Carlo method (RT-CB, Muinonen 2004) that makes use of a so-called phenomenological fundamental single scatterer (Muinonen and Videen 2012). For the validity of RT-CB, see Muinonen et al. (2012). The method can allow us to put constraints on the size, shape, and refractive index of the fundamental scatterers.In the present work, we extend the RT-CB method for the specific case of a macroscopic medium of electric dipole scatterers. For the computation of the interactions, the far-field approximation inherent in the RT-CB method is replaced by an exact treatment, allowing us to account for, e.g., the so-called near-field effects. The present method constitutes the first milestone in the development of a multiple-scattering method, where the so-called ladder and maximally crossed cyclical diagrams of the multiple electromagnetic interactions are rigorously computed. We expect to utilize the new methods in the spectroscopic, photometric, and polarimetric studies of asteroids, as well as in the interpretation of radar echoes from small Solar System bodies.Acknowledgments. The research is funded by the ERC Advanced Grant No 320773 entitled Scattering and Absorption of Electromagnetic Waves in Particulate Media (SAEMPL).K. Muinonen, Waves in Random Media 14, 365 (2004).K. Muinonen, K., and G. Videen, JQSRT 113, 2385 (2012).K. Muinonen, M. I. Mishchenko, J. M. Dlugach, E. Zubko, A. Penttilä,and G. Videen, ApJ 760, 118 (2012).

2D pair distribution function analysis of anisotropic small-angle scattering patterns from elongated nano-composite hydrogels.

PubMed

Nishi, Kengo; Shibayama, Mitsuhiro

2017-05-03

Small angle scattering (SAS) on polymer nanocomposites under elongation or shear flow is an important experimental method to investigate the reinforcement effects of the mechanical properties by fillers. However, the anisotropic scattering patterns that appear in SAS are very complicated and difficult to interpret. A representative example is a four-spot scattering pattern observed in the case of polymer materials containing silica nanoparticles, the origin of which is still in debate because of the lack of quantitative analysis. The difficulties in the interpretation of anisotropic scattering patterns mainly arise from the abstract nature of the reciprocal space. Here, we focus on the 2D pair distribution function (PDF) directly evaluated from anisotropic scattering patterns. We applied this method to elongated poly(N,N-dimethylacrylamide) gels containing silica nanoparticles (PDAM-NP gel), which show a four-spot scattering pattern under elongation. From 2D PDFs, we obtained detailed and concrete structural information about the elongated PDAM-NP gel, such as affine and non-affine displacements of directly attached and homogeneously dispersed silica nanoparticles, respectively. We proposed that nanoparticles homogeneously dispersed in the perpendicular direction are not displaced due to the collision of the adsorbed polymer layer during elongation, while those in the parallel direction are displaced in an affine way. We assumed that this suppression of the lateral compression is the origin of the four-spot pattern in this study. These results strongly indicate that our 2D PDF analysis will provide deep insight into the internal structure of polymer nanocomposites hidden in the anisotropic scattering patterns.

Interior tomographic imaging for x-ray coherent scattering (Conference Presentation)

NASA Astrophysics Data System (ADS)

Pang, Sean; Zhu, Zheyuan

2017-05-01

Conventional computed tomography reconstructs the attenuation only high-dimensional images. Coherent scatter computed tomography, which reconstructs the angular dependent scattering profiles of 3D objects, can provide molecular signatures that improves the accuracy of material identification and classification. Coherent scatter tomography are traditionally acquired by setups similar to x-ray powder diffraction machine; a collimated source in combination with 2D or 1D detector collimation in order to localize the scattering point. In addition, the coherent scatter cross-section is often 3 orders of magnitude lower than that of the absorption cross-section for the same material. Coded aperture and structured illumination approaches has been shown to greatly improve the collection efficiency. In many applications, especially in security imaging and medical diagnosis, fast and accurate identification of the material composition of a small volume within the whole object would lead to an accelerated imaging procedure and reduced radiation dose. Here, we report an imaging method to reconstruct the material coherent scatter profile within a small volume. The reconstruction along one radial direction can reconstruct a scalar coherent scattering tomographic image. Our methods takes advantage of the finite support of the scattering profile in small angle regime. Our system uses a pencil beam setup without using any detector side collimation. Coherent scatter profile of a 10 mm scattering sample embedded in a 30 mm diameter phantom was reconstructed. The setup has small form factor and is suitable for various portable non-destructive detection applications.

Effect of benzocaine and propranolol on phospholipid-based bilayers.

PubMed

Mangiapia, G; Gvaramia, M; Kuhrts, L; Teixeira, J; Koutsioubas, A; Soltwedel, O; Frielinghaus, H

2017-12-06

Cell membranes play a fundamental role in protecting the cell from its surroundings, in addition to hosting many proteins with fundamental biological tasks. A study of drug/lipid interactions is a necessary and important step in fully clarifying the role and action mechanism of active ingredients, and shedding light on possible complications caused by drug overdosage. In this paper, the influence of benzocaine and propranolol drugs on the structure of l-α-phosphatidylcholine-based membranes has been investigated by means of neutron reflectivity, grazing incidence small angle neutron scattering, and small/ultra-small angle neutron scattering. Investigations allowed discovering a stiffening of the membranes and the formation of stalks, caused by the presence of benzocaine. On the other hand, disordered bilayers (lamellar powders) and highly curved structures were found in the presence of propranolol. The results obtained may be rationalized in terms of the molecular structures of drugs and may serve as a starting point for explaining the toxic behavior in long-term and overdosage scenarios.

Accounting for observed small angle X-ray scattering profile in the protein-protein docking server ClusPro.

PubMed

Xia, Bing; Mamonov, Artem; Leysen, Seppe; Allen, Karen N; Strelkov, Sergei V; Paschalidis, Ioannis Ch; Vajda, Sandor; Kozakov, Dima

2015-07-30

The protein-protein docking server ClusPro is used by thousands of laboratories, and models built by the server have been reported in over 300 publications. Although the structures generated by the docking include near-native ones for many proteins, selecting the best model is difficult due to the uncertainty in scoring. Small angle X-ray scattering (SAXS) is an experimental technique for obtaining low resolution structural information in solution. While not sufficient on its own to uniquely predict complex structures, accounting for SAXS data improves the ranking of models and facilitates the identification of the most accurate structure. Although SAXS profiles are currently available only for a small number of complexes, due to its simplicity the method is becoming increasingly popular. Since combining docking with SAXS experiments will provide a viable strategy for fairly high-throughput determination of protein complex structures, the option of using SAXS restraints is added to the ClusPro server. © 2015 Wiley Periodicals, Inc. © 2015 Wiley Periodicals, Inc.

High-energy synchrotron study of in-pile-irradiated U–Mo fuels

DOE PAGES

Miao, Yinbin; Mo, Kun; Ye, Bei; ...

2015-12-30

We report synchrotron scattering analysis results on U-7wt%Mo fuel samples irradiated in the Advanced Test Reactor to three different burnup levels. Mature fission gas bubble superlattice was observed to form at intermediate burnup. The superlattice constant was determined to be 11.7 nm and 12.1 nm by wide-angle and small-angle scattering respectively. Grain sub-division takes place throughout the irradiation and causes the collapse of the superlattice at high burnup. The bubble superlattice expands the lattice constant and acts as strong sinks of radiation induced defects. The evolution of dislocation loops was therefore suppressed until the bubble superlattice collapses.

Measurements of droplet size in shear-driven atomization using ultra-small angle x-ray scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kastengren, A.; Ilavsky, J.; Viera, Juan Pablo

Measurements of droplet size in optically-thick, non-evaporating, shear-driven sprays have been made using ultra-small angle x-ray scattering (USAXS). The sprays are produced by orifice-type nozzles coupled to diesel injectors, with measurements conducted from 1 – 24 mm from the orifice, spanning from the optically-dense near-nozzle region to more dilute regions where optical diagnostics are feasible. The influence of nozzle diameter, liquid injection pressure, and ambient density were examined. The USAXS measurements reveal few if any nanoscale droplets, in conflict with a popular computational model of diesel spray breakup. The average droplet diameter rapidly decreases with downstream distance from the nozzlemore » until a plateau value is reached, after which only small changes are seen in droplet diameter. This plateau droplet size is consistent with the droplets being small enough to be stable with respect to further breakup. As a result, liquid injection pressure and nozzle diameter have the biggest impact on droplet size, while ambient density has a smaller effect.« less

Measurements of droplet size in shear-driven atomization using ultra-small angle x-ray scattering

DOE PAGES

Kastengren, A.; Ilavsky, J.; Viera, Juan Pablo; ...

2017-03-16

Measurements of droplet size in optically-thick, non-evaporating, shear-driven sprays have been made using ultra-small angle x-ray scattering (USAXS). The sprays are produced by orifice-type nozzles coupled to diesel injectors, with measurements conducted from 1 – 24 mm from the orifice, spanning from the optically-dense near-nozzle region to more dilute regions where optical diagnostics are feasible. The influence of nozzle diameter, liquid injection pressure, and ambient density were examined. The USAXS measurements reveal few if any nanoscale droplets, in conflict with a popular computational model of diesel spray breakup. The average droplet diameter rapidly decreases with downstream distance from the nozzlemore » until a plateau value is reached, after which only small changes are seen in droplet diameter. This plateau droplet size is consistent with the droplets being small enough to be stable with respect to further breakup. As a result, liquid injection pressure and nozzle diameter have the biggest impact on droplet size, while ambient density has a smaller effect.« less

Measurement of elastic light scattering from two optically trapped microspheres and red blood cells in a transparent medium.

PubMed

Kinnunen, Matti; Kauppila, Antti; Karmenyan, Artashes; Myllylä, Risto

2011-09-15

Optical tweezers can be used to manipulate small objects and cells. A trap can be used to fix the position of a particle during light scattering measurements. The places of two separately trapped particles can also be changed. In this Letter we present elastic light scattering measurements as a function of scattering angle when two trapped spheres are illuminated with a He-Ne laser. This setup is suitable for trapping noncharged homogeneous spheres. We also demonstrate measurement of light scattering patterns from two separately trapped red blood cells. Two different illumination schemes are used for both samples.

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

NASA Astrophysics Data System (ADS)

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

2014-11-01

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

Confinement-Driven Phase Separation of Quantum Liquid Mixtures

NASA Astrophysics Data System (ADS)

Prisk, T. R.; Pantalei, C.; Kaiser, H.; Sokol, P. E.

2012-08-01

We report small-angle neutron scattering studies of liquid helium mixtures confined in Mobil Crystalline Material-41 (MCM-41), a porous silica glass with narrow cylindrical nanopores (d=3.4nm). MCM-41 is an ideal model adsorbent for fundamental studies of gas sorption in porous media because its monodisperse pores are arranged in a 2D triangular lattice. The small-angle scattering consists of a series of diffraction peaks whose intensities are determined by how the imbibed liquid fills the pores. Pure He4 adsorbed in the pores show classic, layer-by-layer film growth as a function of pore filling, leaving the long range symmetry of the system intact. In contrast, the adsorption of He3-He4 mixtures produces a structure incommensurate with the pore lattice. Neither capillary condensation nor preferential adsorption of one helium isotope to the pore walls can provide the symmetry-breaking mechanism. The scattering is consistent with the formation of randomly distributed liquid-liquid microdomains ˜2.3nm in size, providing evidence that confinement in a nanometer scale capillary can drive local phase separation in quantum liquid mixtures.

Characterization of surface modified carbon fibers and their epoxy composites by small angle x-ray scattering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stoll, B.; Fellers, J.F.; Lin, J.S.

1986-01-01

This paper correlated the interlaminar shear strength of 7 different carbon fiber/epoxy composites with structural characteristics determined by Small Angle X-ray Scattering (SAXS) measurements. The carbon fibers were all of the same type but had different surface treatments. The SAXS patterns of the fibers and of the composites showed a highly nonlinear Guinier region which could not be approximated by traditional linear regression. A new approach to the Guinier approximation was developed to treat this nonlinear curve using a polynomial of second order. The radius of gyration (RG) of the fibers, as determined by this new method, correlated clearly withmore » both the extent of the surface treatment and the interlaminar shear strength of the composite. Also the difference in scattering between a dry fiber and a glycerine soaked fiber provides a way to characterize the changes obtained by surface treatments. These methods provide new ways to estimate the efficiency of a surface treatment and its effect on the interlaminar shear strength by analyzing the SAXS patterns of the fibers.« less

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

PubMed

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

2017-01-01

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

The Effect of Different Coupling Agents on Nano-ZnO Materials Obtained via the Sol-Gel Process.

PubMed

Purcar, Violeta; Şomoghi, Raluca; Niţu, Sabina Georgiana; Nicolae, Cristian-Andi; Alexandrescu, Elvira; Gîfu, Ioana Cătălina; Gabor, Augusta Raluca; Stroescu, Hermine; Ianchiş, Raluca; Căprărescu, Simona; Cinteză, Ludmila Otilia

2017-12-12

Hybrid nanomaterials based on zinc oxide were synthesized via the sol-gel method, using different silane coupling agents: (3-glycidyloxypropyl)trimethoxysilane (GPTMS), phenyltriethoxysilane (PhTES), octyltriethoxysilane (OTES), and octadecyltriethoxysilane (ODTES). Morphological properties and the silane precursor type effect on the particle size were investigated using dynamic light scattering (DLS), environmental scanning electron microscopy (ESEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and X-ray diffraction (XRD). The bonding characteristics of modified ZnO materials were investigated using Fourier transform infrared spectroscopy (FTIR). The final solutions were deposited on metallic substrate (aluminum) in order to realize coatings with various wettability and roughness. The morphological studies, obtained by ESEM and TEM analysis, showed that the sizes of the ZnO nanoparticles are changed as function of silane precursor used in synthesis. The thermal stability of modified ZnO materials showed that the degradation of the alkyl groups takes place in the 300-500 °C range. Water wettability study revealed a contact angle of 142 ± 5° for the surface covered with ZnO material modified with ODTES and showed that the water contact angle increases as the alkyl chain from the silica precursor increases. These modified ZnO materials, therefore, can be easily incorporated in coatings for various applications such as anti-corrosion and anti-icing.

The influence of physical wedges on penumbra and in-field dose uniformity in ocular proton beams.

PubMed

Baker, Colin; Kacperek, Andrzej

2016-04-01

A physical wedge may be partially introduced into a proton beam when treating ocular tumours in order to improve dose conformity to the distal border of the tumour and spare the optic nerve. Two unwanted effects of this are observed: a predictable broadening of the beam penumbra on the wedged side of the field and, less predictably, an increase in dose within the field along a relatively narrow volume beneath the edge (toe) of the wedge, as a result of small-angle proton scatter. Monte Carlo simulations using MCNPX and direct measurements with radiochromic (GAFCHROMIC(®) EBT2) film were performed to quantify these effects for aluminium wedges in a 60 MeV proton beam as a function of wedge angle and position of the wedge relative to the patient. For extreme wedge angles (60° in eye tissue) and large wedge-to-patient distances (70 mm in this context), the 90-10% beam penumbra increased from 1.9 mm to 9.1 mm. In-field dose increases from small-angle proton scatter were found to contribute up to 21% additional dose, persisting along almost the full depth of the spread-out-Bragg peak. Profile broadening and in-field dose enhancement are both minimised by placing the wedge as close as possible to the patient. Use of lower atomic number wedge materials such as PMMA reduce the magnitude of both effects as a result of a reduced mean scattering angle per unit energy loss; however, their larger physical size and greater variation in density are undesirable. Copyright © 2016 Associazione Italiana di Fisica Medica. Published by Elsevier Ltd. All rights reserved.

Polar nephelometer for atmospheric particulate studies

NASA Technical Reports Server (NTRS)

Hansen, M. Z.; Evans, W. H.

1980-01-01

A polar nephelometer for use in studying atmospheric aerosols was developed. The nephelometer detects molecular scatter from air and measures scattering from very clean air using pure molecular scattering for calibration. A compact system using a folded light path with an air cooled argon laser for the light source was designed. A small, sensitive detector unit permits easy angular rotation for changing the scattering angle. A narrow detector field of view of + or - 1/4 degree of scattering along with a single wavelength of incident light is used to minimize uncertainties in the scattering theory. The system is automated for data acquisition of the scattering matrix elements over an angular range from 2 degrees to 178 degrees of scattering. Both laser output and detector sensitivity are monitored to normalize the measured light scattering.

Errors induced by the neglect of polarization in radiance calculations for Rayleigh-scattering atmospheres

NASA Technical Reports Server (NTRS)

Mishchenko, M. I.; Lacis, A. A.; Travis, L. D.

1994-01-01

Although neglecting polarization and replacing the rigorous vector radiative transfer equation by its approximate scalar counterpart has no physical background, it is a widely used simplification when the incident light is unpolarized and only the intensity of the reflected light is to be computed. We employ accurate vector and scalar multiple-scattering calculations to perform a systematic study of the errors induced by the neglect of polarization in radiance calculations for a homogeneous, plane-parallel Rayleigh-scattering atmosphere (with and without depolarization) above a Lambertian surface. Specifically, we calculate percent errors in the reflected intensity for various directions of light incidence and reflection, optical thicknesses of the atmosphere, single-scattering albedos, depolarization factors, and surface albedos. The numerical data displayed can be used to decide whether or not the scalar approximation may be employed depending on the parameters of the problem. We show that the errors decrease with increasing depolarization factor and/or increasing surface albedo. For conservative or nearly conservative scattering and small surface albedos, the errors are maximum at optical thicknesses of about 1. The calculated errors may be too large for some practical applications, and, therefore, rigorous vector calculations should be employed whenever possible. However, if approximate scalar calculations are used, we recommend to avoid geometries involving phase angles equal or close to 0 deg and 90 deg, where the errors are especially significant. We propose a theoretical explanation of the large vector/scalar differences in the case of Rayleigh scattering. According to this explanation, the differences are caused by the particular structure of the Rayleigh scattering matrix and come from lower-order (except first-order) light scattering paths involving right scattering angles and right-angle rotations of the scattering plane.

Modular structure of the full-length DNA gyrase B subunit revealed by small-angle X-ray scattering.

PubMed

Costenaro, Lionel; Grossmann, J Günter; Ebel, Christine; Maxwell, Anthony

2007-03-01

DNA gyrase, the only topoisomerase able to introduce negative supercoils into DNA, is essential for bacterial transcription and replication; absent from humans, it is a successful target for antibacterials. From biophysical experiments in solution, we report a structural model at approximately 12-15 A resolution of the full-length B subunit (GyrB). Analytical ultracentrifugation shows that GyrB is mainly a nonglobular monomer. Ab initio modeling of small-angle X-ray scattering data for GyrB consistently yields a "tadpole"-like envelope. It allows us to propose an organization of GyrB into three domains-ATPase, Toprim, and Tail-based on their crystallographic and modeled structures. Our study reveals the modular organization of GyrB and points out its potential flexibility, needed during the gyrase catalytic cycle. It provides important insights into the supercoiling mechanism by gyrase and suggests new lines of research.

In Situ μGISAXS: II. Thaumatin Crystal Growth Kinetic

PubMed Central

Gebhardt, Ronald; Pechkova, Eugenia; Riekel, Christian; Nicolini, Claudio

2010-01-01

The formation of thaumatin crystals by Langmuir-Blodgett (LB) film nanotemplates was studied by the hanging-drop technique in a flow-through cell by synchrotron radiation micrograzing-incidence small-angle x-ray scattering. The kinetics of crystallization was measured directly on the interface of the LB film crystallization nanotemplate. The evolution of the micrograzing-incidence small-angle x-ray scattering patterns suggests that the increase in intensity in the Yoneda region is due to protein incorporation into the LB film. The intensity variation suggests several steps, which were modeled by system dynamics based on first-order differential equations. The kinetic data can be described by two processes that take place on the LB film, a first, fast, process, attributed to the crystal growth and its detachment from the LB film, and a second, slower process, attributed to an unordered association and conversion of protein on the LB film. PMID:20713011

Using small angle x-ray scattering to measure the homogeneous nucleation rates of n-propanol, n-butanol, and n-pentanol in supersonic nozzle expansions

NASA Astrophysics Data System (ADS)

Ghosh, David; Manka, Alexandra; Strey, Reinhard; Seifert, Soenke; Winans, Randall E.; Wyslouzil, Barbara E.

2008-09-01

In our earlier publication [M. Gharibeh et al., J. Chem. Phys. 122, 094512 (2005)] we determined the temperatures and partial pressures corresponding to the maximum nucleation rate for a series n-alcohols (CiH2i+lOH; i =3-5) during condensation in a supersonic nozzle. Although we were able to determine the characteristic time ΔtJmax corresponding to the peak nucleation rate, we were unable to measure the number density of the aerosol and, thus, unable to directly quantify the nucleation rate J. In this paper we report the results of our pioneering small angle x-ray scattering (SAXS) experiments of n-alcohol droplets formed in a supersonic nozzle together with a new series of complementary pressure trace measurements. By combining the SAXS and pressure trace measurement data we determine the nucleation rates as a function of temperature and supersaturation.

An investigation of the effect of processing conditions on the lamellar and spherulitic morphology of polyhydroxyalkanoates

NASA Astrophysics Data System (ADS)

Xie, Yuping; Akpalu, Yvonne A.

2007-03-01

Polyhydroxyalkanoates (PHAs) have recently attracted much interest because of their biodegradability and biocompatibility. Since the ultimate properties of polymers can be controlled by processing conditions, particularly cooling rates, the systematic and thorough understanding of the effects of cooling rates on the final morphology and the resulting mechanical properties of PHAs is necessary and important. In this presentation, the lamellar (tens of nanometers), fibrillar (several hundred nanometers) and spherulitic (˜μm) morphologies of poly (3-hydroxybutyric acid) (PHB) and the copolymer poly (3-hydroxybutyric acid-co-3-hydroxyvaleric acid) (PHBV) crystallized under different cooling rates were studied using small angle X-ray scattering, ultra small angle X-ray scattering, and polarized optical microscopy, respectively. The morphology was observed to depend strongly on cooling rate. The influence of cooling rate on the morphology and mechanical properties such as toughness, tensile strength and overall stress-strain behavior will be discussed.

Modeling the Hydration Layer around Proteins: Applications to Small- and Wide-Angle X-Ray Scattering

PubMed Central

Virtanen, Jouko Juhani; Makowski, Lee; Sosnick, Tobin R.; Freed, Karl F.

2011-01-01

Small-/wide-angle x-ray scattering (SWAXS) experiments can aid in determining the structures of proteins and protein complexes, but success requires accurate computational treatment of solvation. We compare two methods by which to calculate SWAXS patterns. The first approach uses all-atom explicit-solvent molecular dynamics (MD) simulations. The second, far less computationally expensive method involves prediction of the hydration density around a protein using our new HyPred solvation model, which is applied without the need for additional MD simulations. The SWAXS patterns obtained from the HyPred model compare well to both experimental data and the patterns predicted by the MD simulations. Both approaches exhibit advantages over existing methods for analyzing SWAXS data. The close correspondence between calculated and observed SWAXS patterns provides strong experimental support for the description of hydration implicit in the HyPred model. PMID:22004761

Determination of the size and phase composition of silver nanoparticles in a gel film of bacterial cellulose by small-angle X-ray scattering, electron diffraction, and electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Volkov, V. V.; Klechkovskaya, V. V., E-mail: klechvv@ns.crys.ras.ru; Shtykova, E. V.

2009-03-15

The nanoscale structural features in a composite (gel film of Acetobacter Xylinum cellulose with adsorbed silver nanoparticles, stabilized by N-polyvinylpyrrolidone) have been investigated by small-angle X-ray scattering. The size distributions of inhomogeneities in the porous structure of the cellulose matrix and the size distributions of silver nanoparticles in the composite have been determined. It is shown that the sizes of synthesized nanoparticles correlate with the sizes of inhomogeneities in the gel film. Particles of larger size (with radii up to 100 nm) have also been found. Electron microscopy of thin cross sections of a dried composite layer showed that largemore » particles are located on the cellulose layer surface. Electron diffraction revealed a crystal structure of silver nanoparticles in the composite.« less

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)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rawolle, M.; Koerstgens, V.; Ruderer, M. A.

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 scatteredmore » intensity. Therefore, the acquisition time in GISAXS geometry is reduced significantly at beamline P03.« less

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

PubMed

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

2017-11-01

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

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

Spin-wave dynamics in the helimagnet FeGe studied by small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Siegfried, S.-A.; Sukhanov, A. S.; Altynbaev, E. V.; Honecker, D.; Heinemann, A.; Tsvyashchenko, A. V.; Grigoriev, S. V.

2017-04-01

We have studied the spin-wave stiffness of the Dzyaloshinskii-Moriya helimagnet FeGe in a temperature range from 225 K up to TC≈278.7 K by small-angle neutron scattering. The method we have used is based on [Grigoriev et al., Phys. Rev. B 92, 220415(R) (2015), 10.1103/PhysRevB.92.220415] and was extended here for the application in polycrystalline samples. We confirm the validity of the anisotropic spin-wave dispersion for FeGe caused by the Dzyaloshinskii-Moriya interaction. We have shown that the spin-wave stiffness A for the FeGe helimagnet decreases with a temperature as A (T ) =194 [1 -0.7 (T/TC) 4.2] meVÅ 2 . The finite value of the spin-wave stiffness A =58 meVÅ 2 at TC classifies the order-disorder phase transition in FeGe as being the first-order one.

Quantitative 3D determination of self-assembled structures on nanoparticles using small angle neutron scattering.

PubMed

Luo, Zhi; Marson, Domenico; Ong, Quy K; Loiudice, Anna; Kohlbrecher, Joachim; Radulescu, Aurel; Krause-Heuer, Anwen; Darwish, Tamim; Balog, Sandor; Buonsanti, Raffaella; Svergun, Dmitri I; Posocco, Paola; Stellacci, Francesco

2018-04-09

The ligand shell (LS) determines a number of nanoparticles' properties. Nanoparticles' cores can be accurately characterized; yet the structure of the LS, when composed of mixture of molecules, can be described only qualitatively (e.g., patchy, Janus, and random). Here we show that quantitative description of the LS' morphology of monodisperse nanoparticles can be obtained using small-angle neutron scattering (SANS), measured at multiple contrasts, achieved by either ligand or solvent deuteration. Three-dimensional models of the nanoparticles' core and LS are generated using an ab initio reconstruction method. Characteristic length scales extracted from the models are compared with simulations. We also characterize the evolution of the LS upon thermal annealing, and investigate the LS morphology of mixed-ligand copper and silver nanoparticles as well as gold nanoparticles coated with ternary mixtures. Our results suggest that SANS combined with multiphase modeling is a versatile approach for the characterization of nanoparticles' LS.

Small angle neutron scattering analyses and high temperature mechanical properties of nano-structured oxide dispersion strengthened steels produced via cryomilling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Jeoung Han; Byun, Thak Sang; Shin, Eunjoo

2015-08-17

Three oxide dispersion-strengthened (ODS) steels are produced in order to investigate the effect of the mechanical alloying (MA) temperature on the microstructural evolution and high temperature mechanical properties. The microstructural evolution with different MA conditions is examined using small angle neutron scattering. As the MA temperature decreases, the density of the nanoclusters below 10 nm increases and their mean diameter decreases. A low temperature during MA leads to a high strength in the compression tests performed at 500 *C; however, this effect disappears in testing at 900 *C. The milling process at *70 *C exhibits excellent high fracture toughness, whichmore » is better than the benchmark material 14YWT-SM10. However, the *150 *C milling process results in significantly worse fracture toughness properties. The reasons for this strong temperature dependency are discussed.« less