Efficient synthesis of p-bis-(chlorodifluoromethyl)benzene

Selective, high yield partial fluorination of p-bis-(trichloromethyl)benzene to p-bis-(chlorodifluoromethyl)benzene has been accomplished by warming a slurry of the p-bis-(trichloromethyl)benzene in anhydrous HF which also contains a small quantity of inert solvent, such as 1,2-dichloroethane.     

Electrowetting: a model for contact-angle saturation

 Electrowetting (EW) involves the application of an electric potential across a solid–liquid (SL) interface, which modifies the wetting properties of that interface by reducing the SL surface energy and induces a contact-angle change without altering either the bulk liquid or solid properties. Reversible contact angles are achieved at low potentials, while the application of high potentials results in contact-angle saturation and system instabilities. In the present work, an EW system consisting of a substrate (plate or rod) coated with a thin Au underlayer, a dielectric (parylene) layer of various thickness and a 100-nm layer of fluoropolymer (Teflon AF1600) is studied both theoretically and experimentally. A theoretical consideration of the EW effect, taking into account the detailed structure of the electrical double layer, and a model for the saturation of the contact angle observed at high applied potentials are presented. The theoretical treatment presented here confirms that the EW effect is, in the most part, due to polarization of the dielectric, as opposed to purely a rearrangement of the double layer, and explains why no dependence of the EW effect on the electrolyte concentration has been observed. The theory is only applicable over a limited potential range, and we have developed a model that predicts the potential at which this limit occurs. This is the potential at which the SL surface energy becomes zero. The limiting potential is dependent only on the bulk liquid and solid properties and is thus fixed for a given system. Experimentally, the limiting potential corresponds to the onset of contact-angle saturation, although variations in the exact angle of saturation are not uncommon due to the kinetic effects involved in a real system as opposed to a strict thermodynamic analysis. The model predicts that for an EW device in which an aqueous droplet can be forced to completely wet a hydrophobic surface, a surface with basically the same surface energy as the liquid is required. Received: 2 January 1998 Accepted: 21 March 1998     

Magnetically Enhanced 15 kHz Glow Discharge of Methane

This work deals with the luminous chemical vapour deposition (plasma polymerization) of hydrocarbon polymeric thin films in a magnetic field enhanced discharge of methane. The films were deposited on 4″ <111> single crystal silicon substrates. We investigated the influence of the different glow discharge parameters (e.g. pressure, flow rate, power input, etc.) on the deposition rate of methane and the refractive index of the resulting polymeric films, as well as the distribution of these parameters across the wafer. We used a Shinko Seiki Plasma Polymerization equipment with a bell jar reactor comprising two electrodes connected to a symmetric AC power supply of 15 kHz. Two magnetrons were formed by placing two circular shaped concentric magnetic poles behind each electrode. The substrates were attached on both sides of a rotating wheel held at a floating potential in the middle of the two electrodes. This equipment allowed us to vary a single parameter and keep the other parameters constant over the whole process. We measured the thickness and the refractive index and their distribution over the wafer. The effect of the system pressure, decoupled from the effect of flow rate, is explained by the characteristic nature of luminous gas phase and by the polymerization/deposition mechanism of luminous chemical vapour deposition.     

热拉伸和化学腐蚀相结合制备弯曲光纤探针

提出了原子力/光子扫描隧道显微镜(AF/PSTM)系统的关键部分——双功能弯曲光纤探针的制作方法.采用热拉伸与动态、静态两步化学腐蚀相结合的方法制作出AF/PSTM弯曲光纤探针，弯曲角度约为150°，尖端曲率半径优于100nm，锥角范围为60°—90°.将这种双功能弯曲光纤探针应用在新研制的AF/PSTM系统上，同时获得了样品的光学与形貌图像，实现了图像分解. 关键词： 原子力/光子扫描隧道显微镜 光纤探针 热拉伸 化学腐蚀     

Novel ring-cleaving reaction of 4-nitro-1,1,2,2,9,9,10,10-octafluoro[2.2]paracyclophane with nucleophiles

When 4-nitro-AF4 is treated with nucleophiles such as alkoxides and cyanide, a novel ring opening, cyclophane destroying reaction is observed whereby, via an S_NAr mechanism, the nucleophile attacks the bridgehead aryl carbon vicinal to the nitro group with subsequent aryl-CF₂ bond cleavage.     

Optimisation of ambient and high temperature asymmetric flow field-flow fractionation with dual/multi-angle light scattering and infrared/refractive index detection

Asymmetric flow field-flow fractionation (AF4) enables to analyse polymers with very high molar masses under mild conditions in comparison to size exclusion chromatography (SEC). Conventionally, membranes for AF4 are made from cellulose. Recently, a novel ceramic membrane has been developed which can withstand high temperatures above 130 °C and chlorinated organic solvents, thus making it possible to characterise semicrystalline polyolefins by HT-AF4. Two ceramic membranes and one cellulose membrane were compared with regard to their quality of molar mass separation and the loss of the polymer material through the pores. Separating polystyrene standards as model compounds at different cross-flow gradients the complex relationship between cross-flow velocity, separation efficiency, the molar mass and peak broadening could be elucidated in detail. Moreover, the dependence of signal quality and reproducibility on sample concentration and mass loading was investigated because the evaluation of the obtained fractograms substantially depends on the signal intensities. Finally, the performance of the whole system was tested at high temperature by separating PE reference materials of high molar mass.     

Review of near-field optical microscopy

This review has introduced a new near-field optical microscope (NOM)—atomic force microscope combined with photon scanning tunneling microscope (AF / PSTM). During scanning, AF/PSTM could get two optical images of refractive index image and transmissivity image, and two AFM images of topography image and phase image. A reflected near-field optical microscope (AF/RSNOM) has also been developed on AF/PSTM platform. The NOM has been reviewed in this paper and the comparison between AF/PSTM & RSNOM and the commercial A-SNOM & RNOM has also been discussed. The functions of AF/PSTM & RSNOM are much better than A-SNOM & RNOM.     

Liposomal structure: A comparative study on light scattering and chromatography techniques

Liposomes play an important role in medical and pharmaceutical science as, nanoscale drug carriers. One of the most important features is their size and size distribution, influencing both their bio-distribution and their targeting efficiency to tumors and also therapeutic activity of liposomal antitumor drugs. In this study, the effect of preparation method and molecular interaction on size and shape of liposome was studied. The size and shape characterization of liposomes was performed by asymmetrical flow field-flow fractionation coupled online with multi-angle light scattering (AF4-MALS). The size distributions obtained by AF4-MALS were compared to mean particle sizes and size distribution measured with other standard method such as Photon Correlation Spectroscopy (PCS). Furthermore, the effect of molecular interaction (hydrophilic and hydrophobic model drugs) on liposomal structure was assessed.     

Novel sponge-like molecularly imprinted mesoporous silica material for selective isolation of bisphenol A and its analogues from sediment extracts

Bisphenol A (BPA) imprinted sponge mesoporous silica was synthesized using a combination of semi-covalent molecular imprinting and simple self-assembly process. The molecularly imprinted sponge mesoporous silica (MISMS) material obtained was characterized by FT-IR, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption–desorption measurements. The results show that the MISMS possessed a large specific surface area (850.55 m² g⁻¹) and a highly interconnected 3-D porous network. As a result, the MISMS demonstrated a superior specific adsorption capacity of 169.22 μmol g⁻¹ and fast adsorption kinetics (reaching equilibrium within 3 min) for BPA. Good class selectivity for BPA and its analogues (bisphenol F, bisphenol B, bisphenol E and bisphenol AF) was also demonstrated by the sorption experiment. The MISMS as solid-phase extraction (SPE) material was then evaluated for isolation and clean-up of these bisphenols (BPs) from sediment samples. An accurate and sensitive analytical method based on the MISMS–SPE coupled with HPLC–DAD has been successfully established for simultaneous determination of five BPs in river sediments with detection limits of 0.43–0.71 ng g⁻¹ dry weight (dw). The recoveries of BPs for lyophilizated sediment samples at two spiking levels (50 and 500 ng g⁻¹ dw for each BP) were in the range of 75.5–105.5% with RSD values below 7.5%.     

非对称场流分离技术在蛋黄浆质低密度脂蛋白粒径表征中的应用

通过自组装的非对称场流分离系统(AF4)与紫外可见光检测器联用分离表征了笼养鸡蛋、柴鸡蛋、鹌鹑蛋和鸭蛋蛋黄浆质中的低密度脂蛋白(LDL)。在近似蛋黄浆质生理条件下,研究了进样量、交叉流流速、膜的类型对AF4蛋黄浆质中LDL分离表征的影响;考察了该方法的精密度。在优化的AF4分析条件下,检测出了笼养鸡蛋、柴鸡蛋、鹌鹑蛋和鸭蛋蛋黄浆质中LDL的水力学粒径分布。LDL的AF4洗脱峰高和峰面积的日内精密度分别为1.3%和1.9%(n=7),日间精密度分别为2.4%和2.3%(n=7)。研究结果表明,该方法可用于分离禽类蛋黄浆质中的LDL,同时能够得到LDL水力学粒径分布。