Small-angle X-ray scattering (SAXS) and elastic and quasi-elastic neutron scattering techniques were used to investigate the high-pressure-induced changes on interactions, the low-resolution structure and the dynamics of lysozyme in solution. SAXS data, analysed using a global-fit procedure based on a new approach for hydrated protein form factor description, indicate that lysozyme completely maintains its globular structure up to 1500 bar, but significant modifications in the protein -protein interaction potential occur at approximately 600-1000 bar. Moreover, the mass density of the protein hydration water shows a clear discontinuity within this pressure range. Neutron scattering experiments indicate that the global and the local lysozyme dynamics change at a similar threshold pressure. A clear evolution of the internal protein dynamics from diffusing to more localized motions has also been probed. Protein structure and dynamics results have then been discussed in the context of protein -water interface and hydration water dynamics. According to SAXS results, the new configuration of water in the first hydration layer induced by pressure is suggested to be at the origin of the observed local mobility changes.
Synchrotron small-angle X-ray scattering (SAXS) was applied for studying the effects of hydrostatic pressure and temperature on the structural behavior of fully hydrated tetradecane (TC)-loaded monoolein (MO) systems. Our main attention focused on investigating the impact of isobaric and isothermal changes on the stability of the inverted type discontinuous Fd3m cubic phase as compared to the inverted type hexagonal (H(2)) liquid crystalline phase. The present results show that compressing the TC-loaded Fd3m phase under isothermal conditions induces a significant increase of its lattice parameter: it approximately increases by 1 A per 75 bar. Further, the Fd3m phase is more pressure-sensitive as compared to the Pn3m and the H(2) phases. At ambient temperatures, we observed the following structural transitions as pressure increases: Fd3m --> H(2) --> Pn3m. Our findings under isobaric conditions reveal more complicated structural transitions. At high pressures, we recorded the interesting temperature-induced structural transition of (Pn3m + L(alpha)) --> (Pn3m + L(alpha) + H(2)) --> (L(alpha) + H(2)) --> H(2) --> Fd3m --> traces of Fd3m coexisting with L(2). At high pressures and low temperatures, the TC molecules partially crystallize as indicated by the appearance of an additional diffraction peak at q = 3.46 nm(-1). This crystallite disappears at high temperatures and also as the system gets decompressed. The appearance of the Pn3m and the L(alpha) phases during compressing the fully hydrated MO/TC samples at high pressures and low temperatures is generally related to a growing hydrocarbon chain condensation, which leads to membrane leaflets with less negative interfacial curvatures (decreasing the spontaneous curvatures |H(0)|). Both the effects of pressure and temperature are discussed in detail for all nonlamellar phases on the basis of molecular shape and packing concepts.
Polymer nanocomposites of epoxies with a novel filler, amino-functional butyltin oxide cage (stannoxane), were prepared and characterized. The nanofiller displays a promising antioxidizing effect, besides mechanical matrix reinforcement. The reinforcement can be assigned to physical interactions among the polymer bonded nanofiller. Moreover, the stannoxane cage undergoes a rearrangement to larger poly amino-functional nano-objects at higher temperatures, which highly reduces its extractability: it is practically not extractable from the nanocomposites in most cases. This, together with the fact that only a few weight percent are needed to achieve an optimal effect, makes it attractive as an antioxidative stabilizer. Epoxy–stannoxane nanocomposite synthesis, stannoxane reactivity and dispersion (morphology via TEM and SAXS), as well as the nanofiller effect on mechanical properties (DMTA) and on thermal stability are discussed. A brief comparison is drawn between the stannoxanes and the previously investigated POSS nanofiller.
A compact high pressure cell and its control environment designed for small-and wide-angle x-ray scattering experiments under hydrostatic pressure up to 3000 bar and temperatures between Ϫ20°C and ϩ80°C are described. With this system x-ray scattering experiments can be performed at constant pressure and temperature with a conventional laboratory x-ray source and it can be easily modified to carry out time resolved pressure jump studies at synchrotron radiation sources. The computer-aided pressure adjustment has a calibrated accuracy of Ϯ0.5%, and temperature is computer-controlled to a precision of Ϯ0.05°C. The instrument has been designed to investigate systems of biological interest, especially lipid-water dispersions, but it is equally possible to measure highly viscous or solid samples. The performance is illustrated by a pressure dependent small-and wide-angle x-ray scattering study of a phospholipid-water dispersion at constant temperature.
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