The cyclodimerisation of 3-methyl-2-butenenitrile

3-Methyl-2-butenenitrile (1) cyclodimerised on treatment with lithium diisopropylamide in dimethoxyethane at temperatures between ?78°C and 0°C to 3-amino-4-cyano-1,5,5-trimethyl-1,3-cyclohexadiene (2) the structure of which was established by acid hydrolysis to the known 4-cyano-1,5,5-trimethyl-1-cyclohexene-3-one (3).     

Spreading of liquid drops over saturated porous layers

Spreading of small liquid drops over thin porous layers saturated with the same liquid is investigated from both theoretical and experimental points of view. A theory is presented that shows that spreading is governed by the same power law as in the case of spreading over a dry solid substrate. The Brinkman's equations are used to model the liquid flow inside the porous substrate. An equation of the drop spreading is deduced, which shows that both an effective lubrication and the liquid exchange between the drop and the porous substrates are equally important. The presence of these two phenomena removes the well-known singularity at the moving three-phase contact line. Matching of the drop profile in the vicinity of the three-phase contact line with the main spherical part of the drop gives the possibility to calculate the pre-exponential factor in the spreading law via permeability and effective viscosity of the liquid in the porous layer. Unfortunately, the latter dependency turns out to be very weak. Spreading of silicone oils over different microfiltration membranes is carried out. Radii of spreading on time experimental dependencies confirm the theory predictions. Experimentally found coefficients agree with theoretical estimations.     

Preparation and characterization of PLGA particles for subcutaneous controlled drug release by membrane emulsification

Uniformly sized microparticles of poly(d,l-lactic-co-glycolic) (PLGA) acid, with controllable median diameters within the size range 40–140 μm, were successfully prepared by membrane emulsification of an oil phase injected into an aqueous phase, followed by solvent removal. Initially, simple particles were produced as an oil in water emulsion, where dichloromethane (DCM) and PLGA were the oil phase and water with stabiliser was the continuous phase. The oil was injected into the aqueous phase through an array type microporous membrane, which has very regular pores equally spaced apart, and two different pore sizes were used: 20 and 40 μm in diameter. Shear was provided at the membrane surface, causing the drops to detach, by a simple paddle stirrer rotating above the membrane. Further tests involved the production of a primary water in oil emulsion, using a mechanical homogeniser, which was then subsequently injected into a water phase through the microporous membrane to form a water in oil in water emulsion. These tests used a water-soluble model drug (blue dextran) and encapsulation efficiencies of up to 100% were obtained for concentrations of 15% PLGA dissolved in the DCM and injected through a 40 μm membrane.

Solidification of the PLGA particles was followed by removal of the DCM through the surrounding aqueous continuous phase. Different PLGA concentrations, particle size and osmotic pressures were considered in order to find their effect on encapsulation efficiency. Osmotic pressure was varied by changing the salt concentration in the external aqueous phase whilst maintaining a constant internal aqueous phase salt concentration. Osmotic pressure was found to be a significant factor on the resulting particle structure, for the tests conducted at lower PLGA concentrations (10% and 5% PLGA). The PLGA concentration and particle size distribution influence the time to complete the solidification stage and a slow solidification, formed by stirring gently overnight, provided the most monosized particles and highest encapsulation efficiency.     

Conical parametric scattering of a single extraordinary beam in BaTiO3 crystal

In this paper, the parametric scattering of a single extraordinary polarized beam of laser in BaTiO₃ photorefractive crystal has been investigated experimentally and theoretically. The resulting pattern consists of beam fanning, isotropic ring, and anisotropic one. Among all parts of scattering pattern, isotropic ring has not been studied as much as beam fanning and anisotropic ring, and there still are some differences in reports about it. Therefore, the study has mainly focused on this part. In this experimental configuration, isotropic ring is just visible in positive angles although the other parts of parametric scattering pattern can be visible from behind and in front of the crystal. In addition to steady state pattern in forward and backward directions, its transient behavior with the rotation of crystal has been studied. The results of experiments have been analyzed carefully, and their theoretical explanations have been presented based on the standard theory of parametric scattering in photorefractive crystals. It has been shown that this configuration corresponds to the so called parametric B-process scattering.     

PLGA particle production for water-soluble drug encapsulation: Degradation and release behaviour

Particles for subcutaneous depot use encapsulating a model water-soluble drug have been produced from poly(lactic–glycolic acid) (PLGA) using a membrane emulsification—solvent evaporation technique. The release behaviour, mainly the change in size and inner morphology are reported. During release, the particles initially swelled in size, then reduced. A diffusion based model, taking in to account the change in particle size, is presented. Surface erosion is evident from the particle size and image evidence, and the diffusion model provides a fit to the data even during the surface erosion period, suggesting that the model drug diffuses before the particle degrades.     

Self-chemical ionization of diethylzinc

The self-chemical ionization of diethylzinc is examined by Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometry and semiempirical molecular orbital calculations. Electron impact of diethylzinc neutral produces the radical cation, C(4)H(15)Zn(+) (m/z x 122), which reacts further with the neutral (C(2)H(5))(2)Zn to give the following product ions: Zn(+) (m/z x 64), C(2)H(5)Zn(+) (m/z x 93), C(4)H(9)Zn(+) (m/z x 121), C(4)H(11)Zn(2)(+) (m/z x 187), and C(6)H(15)Zn(2)(+) (m/z x 215). To determine the structure and pathways for production of these ions, monoisotopic (12)C(4)H(15)(64)Zn(+), (64)Zn(+) and (12)C(2)H(5)(64)Zn(+) were individually isolated and reacted with the neutral background. We also performed semiempirical molecular orbital calculations (ZINDO/1). The molecular orbital calculations and experimental data are consistent in predicting that the ethyl group on the diethylzinc cation carries the positive charge. Copyright 1999 John Wiley & Sons, Ltd.     

Sieve mechanism of microfiltration separation

A theoretical model of dead-end microfiltration (MF) of dilute suspensions is proposed. The model is based on a sieve mechanism of MF and takes into account the probability of membrane pore blocking during MF of dilute colloidal suspensions. An integro-differential equation (IDE) that includes both the membrane pore size and the particle size distributions is deduced. According to the suggested model a similarity property is applicable, which allows one to predict the flux through the membrane as a function of time for any pressure, and dilute concentration, based on one experiment at a single pressure and concentration. The suggested model includes only one fitting parameter, β>1, which takes into account the range of the hydrodynamic influence of a single pore. For a narrow pore size distribution in which one pore diameter predominates (track-etched membranes), the IDE is solved analytically and the derived equation is in good agreement with the measurements on different track-etched membranes. A simple approximate solution of the IDE is derived and that approximate solution, as well as the similarity principal of MF processes, is in good agreement with measurements using a commercial Teflon microfiltration membrane. The theory was further developed to take into account the presence of multiple pores (double, triple and so on pores) on a track-etched membrane surface.

A series of new dead-end filtration experiments are compared with the proposed initial and modified pore blocking models. The challenge suspension used was nearly monodispersed suspension of latex particles of 0.45 μm filtered on a track-etched membrane with similar sized pores 0.4 μm. The filtered suspension concentration ranged from 0.00006 to 0.01% (w/w) and the cross-membrane pressures varied from 1000 to 20,000 Pa. Three stages of microfiltration have been observed. The initial stage is well described by the proposed pore blocking model. The model required only a single parameter that was found to fit all the data under different experimental operational conditions. The second stage corresponds to the transition from the blocking mechanism to the third stage, which is cake filtration. The latter stage occurred after approximately 10–12 particle layers were deposited (mass = 0.006 g) on the surface of the microfiltration membrane.     

Controlled production of oil-in-water emulsions containing unrefined pumpkin seed oil using stirred cell membrane emulsification

Membrane emulsification of unrefined pumpkin seed oil was performed using microengineered flat disc membranes on top of which a paddle blade stirrer was operated to induce surface shear. The membranes used were fabricated by galvanic deposition of nickel onto a photolithographic template and contained hexagonal arrays of uniform cylindrical pores with a diameter of 19 or 40 μm and a pore spacing of 140 μm. The uniformly sized pumpkin seed oil drops with span values less than 0.4 were obtained at oil fluxes up to 640 L m⁻² h⁻¹ using 2 wt.% Tween 20 (polyoxyethylene sorbitan monolaurate) or 2–10 wt.% Pluronic F-68 (polyoxyethylene–polyoxypropylen copolymer) as an aqueous surfactant solution. Pumpkin seed oil is rich in surface active ingredients that can be adsorbed on the membrane surface, such as free fatty acids, phospholipids, and chlorophyll. The adsorption of these components on the membrane surface gradually led to membrane wetting by the oil phase and the formation of uniform drops was achieved only for dispersed phase contents less than 10 vol.%. At high oil fluxes, Pluronic F-68 molecules present at a concentration of 2 wt.% could not adsorb fast enough, on the newly formed oil drops, to stabilise the expanding interface.     

怀孕期头发中一些元素含量的变化趋势

用同步辐射激发X射线荧光分析,对11个产妇怀孕期间头发内一些元素含量的变化趋势进行了测量,在各自对比的基础上,得到了一些结果。