SEM imaging of liquid jets

We present a technique for the study of liquid jets in an environmental scanning electron microscope (ESEM). By using a two-fluid stream consisting of a water inner core and a co-flowing outer gas sheath, we are able to produce liquid streams of sufficiently low flow rate to be compatible with ESEM vacuum requirements. We have recorded ESEM images of water jets down to 700 nm diameter. Details of the jet structure, such as the point of jet breakup and size and shape of the jet cone, can be measured with ESEM to far greater accuracy than with optical microscopy. ESEM imaging of liquid jets offers a valuable research tool for the study of aerosol production, combustion processes, ink-jet generation, and many other attributes of micro- and nanojet systems.     

Levels of mineral nutrients in fresh- and frozen bulk hydrated biological specimens: A comparison of EDS data collected in the environmental SEM and a conventional cryo-SEM

Energy-dispersive X-ray microanalysis (EDS) was compared in fresh- and frozen bulk hydrated tissues using the Environmental SEM (ESEM) and conventional cryo-SEM, respectively. Analyses of globoid inclusions of Eucalyptus calophylla seed from two soil types demontsrated that higher levels of cations (K, Ca, Mg, Al, Fe, Mn, Cu, Zn) occurred in seeds from soils containing higher levels of Al, while EDS-detectable levels of S and P were dependent upon the techniques utilised. Cumulative changes in ESEM-EDS-detectable levels of S and P were characterised by collecting cumulative spectra from nutrient standards and compared with those for K. Progressive increases in K occurred and were consistent with an enriching effect. Levels of S and P increased during early analysis (40–60 sec live time) and decreased thereafter. The semi-conductive nature of biological samples, the loss of anions and gain of cations from the net negatively-charged electron interaction volume contributed to an electrochemical bias. These local modifications in fluid chemistry were reversible. Dehydration effects also occurred in stable, “wet‘ samples. These differences indicated that EDS in ESEM may be limited to cations rather than anions, and that changes in fluid electrochemistry and dehydration may affect the level and distribution of elements.     

The differences observed in NMR VOSY between live and dead mouse brain

The differences in water suppressed VOSY of the brain between a live and dead mouse have been observed in experiments. In the water suppressed VOSY of the dead mouse brain some spectral lines near the water signal have disappeared but these spectral lines do exist in the water suppressed VOSY of the live mouse brain. The approach used to obtain the water suppressed VOSY of the mouse brain is termed phase-shift presaturation, whose water suppression factor, tested by a phantom of an aqueous solution of ethanol, is greater than 1000.     

Common features in the microscopic dynamics of hydration water on organic and inorganic surfaces

The microscopic dynamics of hydration water exhibits some universal features that do not depend on the nature of the hydrated surface. We show that the hydration level dependence of the dynamic transition in the mean squared atomic displacements measured by means of elastic neutron scattering is qualitatively similar for hydration water in inorganic and organic hosts. The difference is that the former are 'rigid', whereas the dynamics of the latter can be enhanced by the motions of the hydration water. The overall hydration level appears to be the main parameter governing the magnitude of the mean squared atomic displacements in the hydration water, irrespective of the details of the hydrated host.     

Dynamics of water in molecular sieves by dielectric spectroscopy

We present recent dielectric data on the dynamics of water confined in molecular sieves with pore sizes 5 and 10 A. The dielectric measurements in the frequency and temperature ranges 10(-2)-10(6) Hz and 120-300 K show three relaxation processes for both samples. In the case of the 10 A pore the slowest process shows an Arrhenius temperature dependence at low temperatures (<220 K), while at high temperatures the relaxation appears to follow a more Vogel-Fulcher-Tammann (VFT) like behaviour. The relaxation time for this process is 100 s at about 170 K. The second slowest process is at low temperatures very similar to the main process of (bulk-like) water in a fully hydrated clay, but also this process seems to exhibit some kind of dynamical transition, in this case at T approximately 185 K. All the three processes in the 5 A pore exhibit Arrhenius temperature dependence, and two of them are considerably slower than the main relaxation in the hydrated clay. Thus, dynamics of bulk-like water is only observed in the 10 A molecular sieves, and most of the water molecules in both 5 and 10 A pores have considerably slower dielectric relaxation than has been observed for water confined in clay, most likely due to strong interactions with the considerably more hydrophilic inner surfaces of molecular sieves.     

Properties of short-living ball lightning produced in the laboratory

An experimental setup for highly reproducible generation of artificial ball lightnings is implemented. Thousands of floating glowing plasmoids 12–20 cm in diameter are produced. Research facilities for studying the plasmoids are developed. It is found that short-lived ball lightnings live for about 1 s and carry an electric charge. The lightnings are shown to have a complex structure: a central kernel containing a rich variety of hydrated ions and aerosol of decay products is surrounded by a thin negatively charged shell.     

Decay of dipolar order in diamagnetic and paramagnetic proteins and protein gels

Magnetic relaxation in solids may be complicated by the creation and loss of dipolar order at finite rates. In tissues the molecular and spin dynamics may be significantly different because of the relatively high concentration of water. We have applied a modified Jeneer-Broekaert pulse sequence to measure dipolar relaxation rates in both dry and hydrated protein systems that may serve as magnetic models for tissue. In lyophilized and dry serum albumin, the dipolar relaxation time, T(1D) is on the order of 1 ms and is consistent with earlier reports. When hydrated by deuterium oxide, the dipolar relaxation times measured were on the order of tens of microseconds. When paramagnetic centers are included in the protein, the Jeneer-Broekaert echo decay times became the order of the decay time for transverse magnetization, i.e., the order of 10 micros or less. In the hydrated or paramagnetic systems, the dipolar relaxation times are too short to require inclusion in the quantitative analysis of magnetization transfer experiments.     

Temperature effects on the diffusion of water and monovalent counterions in the hydrated montmorillonite

We investigate here the effect of temperature on the diffusion of water and cations in the Wyoming-type montmorillonite clay. The considered cations are monovalent compensating ions, such as Li⁺, Na⁺, K⁺, Rb⁺ and Cs⁺ in one-, two- and three-hydration states. For this purpose, molecular dynamics simulations have been performed to obtain the dynamic behaviour regarding the interlayer ions and water molecules under a temperature range between 260 and 400 K. The diffusion coefficient of water and cations in different hydrated clays increases with temperature. The influence of temperature on the diffusion of water is much greater than that of cations in one-, two- or three-hydrated clay. The degree of hydration plays an important role on the diffusion behaviour of water and counterions. We found that the effect of temperature is negligible in weakly hydrated clay, whereas it became significant in highly hydrated one. Besides, the size and mass of cations’ hydrate also affect the diffusion behaviour of water and cations in the interlayer space of hydrated clay.     

量子点的荧光特性在生物探针方面的应用

量子点具有传统有机荧光染料无可比拟的光学魅力,在生物医学及材料领域已引起广泛的兴趣,许多科学工作者在量子点用于生物学领域方面已经取得一定进展。目前,量子点最有前途的应用领域是在生物体系中作为荧光标记物。通过观察量子点标记分子与靶分子相互作用的部位,及其在活细胞内的运行轨迹,可能为信号传递的分子机制提供线索,从而为阐明细胞生长发育的调控及癌变规律提供直观依据。文章介绍了量子点研究生物大分子之间的相互作用、生物大分子荧光标记、细胞及生物组织的荧光标记与成像以及活体成像等方面的应用。并概述了纳米量子点作为生物荧光探针的应用前景以及亟待解决的问题。     

A history of scanning electron microscopy developments: towards "wet-STEM" imaging

A recently developed imaging mode called "wet-STEM" and new developments in environmental scanning electron microscopy (ESEM) allows the observation of nano-objects suspended in a liquid phase, with a few manometers resolution and a good signal to noise ratio. The idea behind this technique is simply to perform STEM-in-SEM, that is SEM in transmission mode, in an environmental SEM. The purpose of the present contribution is to highlight the main advances that contributed to development of the wet-STEM technique. Although simple in principle, the wet-STEM imaging mode would have been limited before high brightness electron sources became available, and needed some progresses and improvements in ESEM. This new technique extends the scope of SEM as a high-resolution microscope, relatively cheap and widely available imaging tool, for a wider variety of samples.     

Trehalose-protected lipid membranes for determining membrane protein structure and insertion

Trehalose preserves lipid bilayers during dehydration and rehydration by replacing water to form hydrogen bonds between its own OH groups and lipid headgroups. We compare the lipid conformation and dynamics between trehalose-protected lyophilized membranes and hydrated membranes, to assess the suitability of the trehalose-containing membrane as a matrix for membrane protein structure determination. (31)P spectra indicate that the lipid headgroup of trehalose-protected dry POPC membrane (TRE-POPC) have an effective phase transition temperature that is approximately 50K higher than that of the hydrated POPC membrane. In contrast, the acyl chains have similar transition temperatures in the two membranes. Intramolecular lipid (13)C'-(31)P distances are the same in TRE-POPC and crystalline POPC, indicating that the lipid headgroup and glycerol backbone conformation is unaffected by trehalose incorporation. Intermolecular (13)C-(31)P distances between a membrane peptide and the lipid headgroups are 10% longer in the hydrated membrane at 226 K than in the trehalose-protected dry membrane at 253 K. This is attributed to residual motions in the hydrated membrane, manifested by the reduced (31)P chemical shift anisotropy, even at the low temperature of 226 K. Thus, trehalose lyoprotection facilitates the study of membrane protein structure by allowing experiments to be conducted at higher temperatures than possible with the hydrated membranes.     

Proton NMR relaxation of adsorbed water in gelatin and collagen

The dependence of the water self-diffusion coefficients as well as of the proton spin-lattice and spin-spin relaxation rates on the concentration have been studied in the gelatin-water system and in hydrated native collagen. The bound and free water fractions and the corresponding spin-spin and spin-lattice relaxation rates have been determined within the multi-phase water proton exchange model. Various theoretical models for the water proton cross-relaxation to the biopolymer have been studied and the results compared with the observed Larmor frequency dependence of the water proton spin-lattice relaxation rate.     

Morphological Changes of Oxide Grains During Oxidation of Pure Iron in an Environmental Scanning Electron Microscope

For modeling particles-gas reactions in terms of the morphology of nascent solid reaction products, a technique using the environmental scanning electron microscope (ESEM) was developed to monitor the in situ oxidation of iron. Experimental conditions of the oxidation experiments were selected as the temperature range of 500–750°C and the oxygen partial pressure range 10^–4–45 Pa. The evolution of nucleation and growth of oxide whiskers or grains on the surface of iron specimens under the ESEM was recorded. The characteristics of some specimens were further examined after oxidation by post-analysis. Three sets of experimental results and other relative micrographs are shown. In the light of the surface morphology and textures of the oxide growths in the micrographs, their growth mechanism and reaction kinetics are discussed. Finally, a plausible physical model for oxidation of iron is suggested.     

Size and stability of liposomes: A possible role of hydration and osmotic forces

Dynamic light scattering and electrophoretic mobility measurements have been used to characterize the size, size distribution and zeta potentials (ζ-potentials) of egg yolk phosphatidylcholine (EYPC) liposomes in the presence of monovalent ions ( Na⁺ and K⁺). To study the stability of liposomes the Derjaguin-Landau-Verwey-Overbeek (DLVO) theory has been extended by introducing the hydrated radius of the adsorbed ions onto the liposome surfaces. The decrease of liposome size is explained on the basis of the membrane impermeability to some ions which generate osmotic forces, which leads to evacuate water from liposome inside.     

Using environmental scanning electron microscopy (ESEM) as a quantitative method to analyse the attachment of Giardia duodenalis to epithelial cells

Giardia duodenalis is a human parasite that colonises the small intestine. In some studies, it may be necessary to estimate the parasite-host adhesion index. When working in vitro, it is very difficult to determine the relative number of parasites adhered to intestinal cells because parasites might be removed from enterocytes during specimen preparation. We have encountered such difficulties with sample analyses when using light and conventional scanning electron microscopy, including the loss of adherent cells during the processing steps. In this study, we showed that environmental scanning electron microscopy (ESEM), which allows the examination of specimens at normal atmospheric pressure or in very low vacuum without any previous treatment, can be used effectively in quantitative studies of the parasite-host relationship.     

Temperature and hydration dependence of proton MAS NMR spectra in MCM-41: Model based on motion induced chemical shift averaging

The proton MAS NMR spectra in MCM-41 at low hydration levels (less than hydration amounting to one water molecule per surface hydroxyl group) show complex proton resonance peak structures, with hydroxyl proton resonances seen in dry MCM-41 disappearing as water is introduced into the pores and new peaks appearing, representing water and hydrated silanol groups. Surface hydroxyl group–water molecule chemical exchange and chemical shift averaging brought about by a water molecule visiting different surface hydrogen bonding sites have been proposed as possible causes for the observed spectral changes. In this report a simple model based on chemical shift averaging, due to the making and breaking of hydrogen bonds as water molecules move on the MCM-41 surface, is shown to fully reproduce the NMR spectra, both as a function of hydration and temperature. Surface proton–water proton chemical exchange is not required in this model at low hydration levels.     

Electron spin resonance and electron spin echo modulation studies of Fe-containing mesoporous MCM-48 molecular sieves

Through electron spin resonance (ESR) and electron spin echo modulation (ESEM) studies, three Fe(III) species are found in liquid ion-exchanged Fe-MCM-48 and synthesized FeMCM-48. Species A with ESR parameters g^A = 4.30 with a line width of 160 G is observed in hydrated samples. This species is accompanied by a shoulder atg = 7.60 and is assigned to distorted tetrahedral Fe(III) likely located at framework defect sites. Species B is a broad peak centered at g^B = 2.00 and is assigned to distorted octahedral Fe(III) located at extraframework sites. This species is also observed in dehydrated samples. Species C is a very narrow isotropic signal at g^C = 4.30 with a line width of 30 G and is only observed in synthesized mesophase materials. It is consistent with rhombic Fe(III) with zero field parametersD andE corresponding toD/E =1/3 and is assigned to tetrahedral Fe(III) located at framework sites. Framework Fe(III) in FeMCM-48 is less accessible to ND₃ than is extraframework Fe(III) in Fe-MCM-48. On the basis of deuterium ESEM data, framework Fe(III) in synthesized FeMCM-48 directly coordinates to two D₂O or CH₃OD molecules and interacts more weakly with two more molecules. However, no deuterium ESEM is observed for extraframework Fe(III) in ion-exchanged Fe-MCM-48 with adsorbed D₂O or CH₃OD. It is also found that Fe(III) is incorporated into the framework of FeMCM-48 at an early stage of the formation of the MCM-48 mesostructure.     

Microwave heating and non-thermal effects of sodium chloride aqueous solution

ABSTRACT

The dielectric thermal and non-thermal properties of sodium chloride aqueous solution under the microwave region have been estimated. The dielectric properties, hydrogen bonding, transport properties, energy distribution and local structure have been evaluated by classical molecular dynamics method. In the process of microwave energy distribution, the direct coupling of rotational motion, vibration and redirection is revealed. Microwave energy is converted into kinetic energy and interaction energy between two molecules. A mechanism for exploring the effects of microwaves on the non-thermal effects of brine systems over a longer simulation time and a wider microwave range is proposed. The increase in field intensity is usually accompanied by local damage to the water structure near the hydrated ions. More specifically, above the field threshold, the residence time of water molecules near the ions significantly decreases.

Highlights

1. Microwave energy is transferred to the kinetic energy and the energy between the molecules.

2. The increase in field intensity is usually accompanied by local damage to the water structure near the hydrated ions.

3. The larger electric field strength amplifies the effect of frequency.

4. The residence time of water molecules near the ions significantly decreases.

     

Understanding hydrated polymers: the perspective of NMR

This review examines the divergent views in the literature on the role of water in hydrated polymers, specifically the origin of non-freezable water. One approach, based largely on site-specific information furnished by NMR invokes binding sites in the host polymer matrix as a principal source of bound or non-freezable water; the second approach is based on the thermodynamics of metastable, non-equilibrium states in the hydrated polymer without the necessity of binding sites. There is merit in both approaches: and they are not mutually exclusive. The situation is further exacerbated with a proliferation of terminology that is both technique and temperature dependent. Despite these difficulties, the behaviour of water has several generic features that are common to a wide variety of hydrated polymeric and non-polymeric systems. The advantages of a multi-technique approach in unravelling the intricacies of polymer-water interactions cannot be over-emphasised.     

Mechanisms of structure formation in particulate gels of β-lactoglobulin formed near the isoelectric point

Particulate gels are known to be formed by bovine β-lactoglobulin near the isoelectric point when partial unfolding is allowed to occur under heating. The aggregation process of the protein has been investigated within the context of a nucleation and growth process by preparing gels under precisely controlled thermal histories. This was achieved using a Differential Scanning Calorimeter (DSC) to provide controlled heating rates, and known final temperatures and incubation times. The resulting particulate gels were characterized by their particle size and polydispersity using Environmental Scanning Electron Microscopy (ESEM), which permits hydrated samples to be observed. Particle size was found to decrease with increasing final temperature, with the aggregation taking longer to reach completion for lower temperatures. Particle size was also found to decrease with increasing heating rate. This system could be modelled as evolving via nucleation and growth by taking into account the fact that the concentration of the aggregating species was varying as a function of temperature as well as time. The intrinsic tryptophan fluorescence as a function of temperature was used as a guide to the fraction of unfolded protein in solution, thereby permitting successful comparisons between the model predictions and the particle sizes to be made.-1