Small angle neutron scattering from micellar solutions of triton X-100

Micellar solutions of non-ionic surfactant triton X-100 (8% by weight) show phase separation at cloud pointT _cp ～ 335 K. This paper reports results of small angle neutron scattering (SANS) experiments from this solution as a function of temperature between 298 and 332 K. The range of wave-vector transferQ, covered in these experiments is from 0.02 to 0.15 Å^?1. It is seen that as one approachesT _cp, the neutron scattering cross section diverges in the region of lowQ (<0.06 Å^?1) while it is independent of temperature in region of largeQ(>0.06 Å^?1). We believe that the divergence of scattering at lowQ with an increase in temperature is because of changes in the structure factorS(Q) of the solution. The measured distributions have been analyzed using four different models for inter-micellar potential. The models used to calculate the structure factorS(Q) are (1) mean spherical approximation (MSA) with Yukawa tail for attractive potential, (2) MSA with an attractive square well potential, (3) random phase approximation (RPA) with an attractive square-well potential and (4) Sticky hard sphere model (attractive square-well potential with Percus-Yevick approximation). The strengths of the attractive potential required to fit the SANS data are (?6.6 to ? 14.4)/kt for model (1), (? 6.6 to ? 15.0)/kt for model (2), (? 3.8 to ? 7.3)/k _B T for model (3) and (?2 to ?2.7)/kt for model (4). On the basis of reasonableness of the derived strength of the potential near the phase separation temperature and its relative temperature dependence, it is concluded that present data favour the Sticky hard sphere model.     

Small angle neutron scattering study of two nonionic surfactants in water micellar solutions

Two classic nonionic surfactants — C₁₄E₇ (heptaethylene glycol monotetradecyl ether) and C₁₀E₇ (heptaethylene glycol monodecyl ether) were investigated in heavy water solution for concentration c = 0.17% (dilute regime) at different temperatures in the range t = 10–35°C by small angle neutron scattering (SANS) method. In the case of C₁₄E₇ surfactant — for all temperatures at c = 0.17% there are two axial ellipsoidal micelles with longer axis 15 nm at 10°C and 49.5 nm at 35°C in investigated solutions. For C₁₀E₇ surfactant at the same concentration of solution and temperature — two axial ellipsoidal micelles were observed, too. The longer axis is equal to 7.5 nm at 10°C, 9 nm at 20°C and at 35°C this axis is equal to 12 nm. Micelles of C₁₀E₇ nonionic surfactant are smaller than those of C₁₄E₇ surfactant in the same experimental conditions.      

Small angle neutron scattering study of temperature-independent formulation of mixed micellar structures

SANS measurements have been performed on mixed systems of ionic surfactant sodium dodecyl sulphate (SDS) and nonionic surfactant polyoxyethylene 10 lauryl ether (C12E10). The total concentration of the mixed system was kept fixed (10 wt%) and the ionic to nonionic surfactant ratio varied in the range 0 to 1. The temperature effect on the structures of mixed micelles has been studied for temperatures between 30 and 75°C. Micelles of pure ionic and nonionic surfactants show opposite trends when the temperature is increased. Sizes of pure ionic micelles decrease and those of nonionic micelles increase with increase in temperature. We show a formulation balancing these two effects which is temperature-independent and consists of about 25% of ionic surfactants in the mixed system. Contrast variation SANS measurements by contrast matching one of the surfactant components to the solvent suggest homogeneous single mixed micelles of the two components in the mixed systems.      

Small-angle neutron scattering from micellar solutions

Micellar solutions are the suspension of the colloidal aggregates of the sur-factant molecules in aqueous solutions. The structure (shape and size) and the interaction of these aggregates, referred to as micelles, depend on the molecular architecture of the surfactant molecule, presence of additives and the solution conditions such as temperature, concentration etc. This paper gives the usefulness of small-angle neutron scattering to the study of micellar solutions with some of our recent results.     

Small angle neutron scattering study of mixed micelles of oppositely charged surfactants

Structures of mixed micelles of oppositely charged surfactants dodecyltrimethylammonium bromide (DTAB) and sodium dodecyl sulphate (SDS) have been studied using small angle neutron scattering. The concentration of one of the components was kept fixed (0.3 M) and that of another varied in the range 0 to 0.1 M. The aggregation number and micellar size increase and fractional charge decreases dramatically with the addition of small amount of oppositely charged surfactant. The effect of addition of SDS on DTAB is significantly different from that of the addition of DTAB on SDS. The contrast variation SANS experiments using deuterated surfactant suggests the homogeneous mixing of two components in mixed micellar system.      

Small angle neutron scattering and structural properties in electrolytic solutions

A new direct indication concerning the structural properties of liquid systems is obtained for the first time. Small angle neutron scattering (SANS) measurements have been performed on solutions of ZnCl₂, NiCl₂, CuBr₂ in D₂O and in non aqueous solvent (EtOAc). The spectra, taken at room temperature, as a function of concentration, in the range $\text{0.019 ? K ? 0.25 (}\text{A}\text{?}{}^{\mathrm{?1}}\text{)}$ show in aqueous solvent an “abnormal” k-dependent small angle coherent cross section. This anomalous contribution clearly indicates the existence in the systems of correlated regions (～ 30 Å) perhaps connected through a preferred distance of ～ 50 Å. Also in pure water the results seem to indicate the existence of correlated regions of finite size.     

Small angle neutron scattering from oxygen precipitates in silicon

The formation of silicon oxide precipitates from Czochralski grown silicon depends on the time and temperature of the heat treatment as well as on the initial content of interstitially dissolved oxygen. Samples containing between 5×10¹⁷ O_i/cm³ and 13×10¹⁷ O_i/cm³ have been heated at 750° C for 96 h. SiO₂ precipitates of various shape and size have been obtained and investigated by means of small angle neutron scattering (SANS) in the Q-range 0.05 Å^–1<Q<0.2 Å^–1. The obtained SANS patterns reveal a typical anisotropy of their intensity distribution, which splits into a central peak at Q<0.1 Å^–1 due to the shape of the individual particles and a number of weak intensities for large Q-values, originating from a correlation between defects, possibly between the precipitates. While these correlation peaks in the SANS patterns are seen best for rather low values of about (5–7)×10¹⁷ O_i/cm³ oxygen content, the central peak anisotropy is most pronounced for higher values of ca 10×10¹⁷ O_i/cm³. The integrated intensity of the central peak increases with increasing initial oxygen content. For comparison, untreated samples of the same initial oxygen content do not reveal any anisotropic SAN scattering or a broadened central peak beam.     

Absence of voids in fast neutron irradiated zirconium by small angle neutron scattering

Abstract

The aim of this research was to resolve a difference of opinion in the literature on the presence of voids in fast neutron irradiated zirconium. There is a great interest in the study of zirconium, since zirconium and its alloys are used extensively in modern power reactors, for example in the fuel rods as a containment material for enriched uranium. A polycrystalline sample of zirconium was irradiated in the HERALD reactor at 40°C with 10²⁰ fast neutrons per cm^?2. The neutron scattering from irradiated and unirradiated standard samples was studied over a wide Q range from 0.001 to 1.12 Å^?1 on a D11 Spectrometer at the ILL (France). The defect cross-section (the difference between the scattering of the standard zirconium crystal and irradiated crystal) was nearly flat as a function of Q (momentum transfer vector) with an average value of 8.5 mb/Str/atom. This indicates a point defect concentration of about 1.8%. Thus the absence of any small angle (Q dependent) defect scattering indicates that large damage regions (e.g. voids) are not produced in zirconium by fast neutron irradiation.     

Salt-free aqueous solutions of polyelectrolytes: Small angle X-ray and neutron scattering characterization

We give an introduction to the application of small angle X-ray and neutron scattering techniques to the study of the structure of polyelectrolyte solutions. The goal is not to be exhaustive and to describe the latest progress in the field of polyelectrolytes but rather to present the potential of the technique. We aim to give an overview on the main features of the scattering curves, and discuss the structural information that can be drawn. We will first give the basics of small angle scattering and highlight the role played by neutron scattering and isotopic labeling. Thus, we will discuss the significance of the monomer and counterion partial scattering functions according to the scattering length densities of both components, and will emphasize the unique possibility to separate out the intra- and intermolecular correlations. Then, some examples will show how the dispersion state and the average conformation of macroions can be addressed. We will however focus on salt-free aqueous solutions of linear flexible hydrophilic polyelectrolytes in the semidilute regime.     

Small angle neutron scattering study on the aggregation behaviour of PEO-PPO-PEO copolymers in the presence of a hydrophobic diol

Small angle neutron scattering (SANS) measurements on aqueous solutions of four polyethylene oxide-polypropylene oxide-polyethylene oxide block copolymers (commercially known as Pluronic®)F88, P85, F127 and P123 in the presence of hydrophobic C14Diol (also known as Surfynol® 104) reveal information on micellization, micellar size and micellar transitions. While most hydrophilic F88 (with least PPO/PEO ratio) remained unimers in water at 30°C, other copolymers formed micellar solutions. Surfynol® 104 is sparingly soluble in water to only about ～0.1 wt%, but on addition to pluronic solution, it gets incorporated in the micellar region of block copolymer which leads to increase in aggregation number and transformation of spherical to ellipsoidal micelles. The added diol-induced micellization in F88, though hydrophilic copolymers F88 and F127 did not show any appreciable micellar growth or shape changes as observed for P85 and P123 (which are comparatively more hydrophobic). The SANS results on copolymer pairs with same molecular weight PPO but different % PEO (viz. F88 and P85, F127 and P123) and with same molecular weight PEO but different PPO (F88 and F127) reveal that the copolymer with large PPO/PEO ratio facilitate micellar transition in the presence of diol. An increase in temperature and presence of added electrolyte (sodium chloride) in the solution further enhances these effects. The micellar parameters for these systems were found out using available software and are reported.     

Small angle neutron scattering and small angle X-ray scattering studies of platinum-loaded carbon foams

The morphology of carbon nanofoam samples comprising platinum nanoparticles dispersed in the matrix was characterized by small angle neutron scattering (SANS) and small angle X-ray scattering (SAXS) techniques. Results show that the structure of pores of carbon matrix exhibits a mass (pore) fractal nature and the average radius of the platinum particles is about 2.5 nm. The fractal dimension as well as the size distribution parameters of platinum particles varies markedly with the platinum content and annealing temperature. Transmission electron micrographs of the samples corroborate the SANS and SAXS results.      

Small angle neutron scattering and spin labeling of human ceruloplasmin

Small angle neutron scattering evidence of intermolecular correlations between cerulo plasmin units in anaqueous medium is provided. By the same technique, the radius of gyration of the globular biomolecule has been calculated to be 33 ± 3 Å. This value was found to agree very well with that measured by the authors with a spin labeling approach.     

Small angle neutron scattering study of pore microstructure in ceria compacts

Ceria powders were prepared by gel combustion process using cerium nitrate and hitherto unexplored amino acids such as aspartic acid, arginine and valine as fuels. The powders have been characterized by X-ray and laser diffraction. Cold pressed compacts of these powders have been sintered at 1250°C for 2 h. Internal pore microstructure of the sintered compacts has been investigated by small angle neutron scattering (SANS) over a scattering wave vector q range of 0.003–0.17 nm⁻¹. The SANS profiles indicate surface fractal morphology of the pore space with fractal dimensionality lying between 2.70 and 2.76.      

A small angle neutron scattering (SANS) experiment using very cold neutrons (VCN)

This paper describes the results of SANS measurements of small samples using the very cold neutron (VCN) beam of the PF2 instrument at the Institut Laue Langevin (ILL), France. In addition to a classical SANS pinhole collimation, the experiment used a polarizing supermirror as a monochromator and a magnetic sextupole lens to focus the neutron beam in order to gain intensity and avoid any material in the neutron beam besides the sample.     

Small angle neutron scattering study of disordered and crystalline iron nanoparticle assemblies

Monodisperse surfactant-coated iron nanoparticles are used to form both disordered nanoparticle assemblies and ordered face-centered cubic nanoparticle crystals. The structural order is probed by small angle X-ray scattering, and the magnetic scattering is studied using small angle neutron scattering. The magnetic scattering corresponding to different length scales is interpreted in terms of collective correlations among the particles within the assemblies.     

Small angle neutron scattering studies on protein denaturation induced by different methods

Small angle neutron scattering (SANS) has been used to study conformational changes in protein bovine serum albumin (BSA) as induced by varying temperature and in the presence of protein denaturating agents urea and surfactant. BSA has prolate ellipsoidal shape and is found to be stable up to 60°C above which it denaturates and subsequently leads to aggregation. The protein solution exhibits a fractal structure at temperatures above 64°C, with fractal dimension increasing with temperature. BSA protein is found to unfold in the presence of urea at concentrations greater than 4 M and acquires a random coil Gaussian chain conformation. The conformation of the unfolded protein in the presence of surfactant has been determined directly using contrast variation SANS measurements by contrast matching surfactant molecules. The protein acquires a random coil Gaussian conformation on unfolding with its radius of gyration increasing with increase in surfactant concentration      

Small angle neutron scattering setup for high pressure measurements at IBR-2

Abstract

The experiments which were carried out showed the possibility of using a titanium-zirconium high pressure cell for small angle neutron scattering. We report on some curves measured by SANS with the help of this setup to illustrate the capabilities of the method.     

Small angle x-ray and neutron scattering studies of plasma-deposited amorphous silicon-hydrogen films

Small-angle scattering measurements using both neutrons and X-rays have been made on a series of plasma-deposited a-Si : H films. One class of sample exhibits strong anisotropic scattering indicating rod-like microstructure normal to the film surface with a dominant rod diameter of ~ 60 Å. Other samples show isotropic scattering with a similar dimension or no scattering at all within the resolution of the experiment.     

Laser light scattering in micellar solutions

Summary The laser light scattering apparatus used for both total intensity and quasi-elastic light scattering experiments on micellar solutions is described in detail. The absolute calibration of the scattered intensity is obtained by exploiting the existence of a lower critical consolution point in a low-concentration aqueous solution of a nonionic amphiphile (C₁₂E₈). The obtained results suggest that micellar solutions may represent a very convenient light scattering standard for both static and dynamic experiments. Paper presented at the “Meeting on Lyotropics and Related Fields”, held in Rende, Cosenza, September 13—18, 1982.     

Small angle neutron scattering study of doxorubicin-surfactant complexes encapsulated in block copolymer micelles

Self-assembling behaviour of block copolymers and their ability to evade the immune system through polyethylene oxide stealth makes it an attractive candidate for drug encapsulation. Micelles formed by polyethylene oxide-polypropylene oxide- polyethylene oxide triblock copolymers (PEO-PPO-PEO), pluronic P123, have been employed for encapsulating the anti-cancer drug doxorubicin hydrochloride. The binding affinity of doxorubicin within the micelle carrier is enhanced through complex formation of drug and anionic surfactant, aerosol OT (AOT). Electrostatic binding of doxorubicin with negatively charged surfactants leads to the formation of hydrophobic drug-surfactant complexes. Surfactant-induced partitioning of the anti-cancer drug into nonpolar solvents such as chloroform is investigated. SANS measurements were performed on pluronic P123 micelles in the presence of drug-surfactant complex. No significant changes in the structure of the micelles are observed upon drug encapsulation. This demonstrates that surfactant- drug complexes can be encapsulated in block copolymer micelles without disrupting the structure of aggregates.