Evolution of the interfacial tension between polydisperse "immiscible" polymers in the absence and in the presence of a compatibilizer

The interfacial tension sigma between two polyisobutylenes (PIB) of dissimilar polydispersity and two polydisperse samples of poly(dimethylsiloxane) (PDMS) was measured as a function of time by means of a pendent drop apparatus at different temperatures ranging from 30 to 110 degreesC. In addition to three of the four possible binary blends, the time evolution of sigma was also determined for one ternary system, where the PIB phase contained 0.03 wt % of a diblock copolymer poly(isobutylene-b-dimethylsiloxane). The pronounced decrease of sigma with advancing time, observed in all cases, is attributed to the migration of the interfacially active lower molecular weight components of the homopolymers and of the compatibilizer into the interphase. Several days are normally required until a becomes constant. These time independent values are not considered as equilibrium data, but accredited to stationary states. A kinetic model is established for sigma(t), which enables a detailed investigation of the rates of transport of the different migrating species of average molar mass of M.

Mechanical and thermal properties of high-density polyethylene toughened with glass beads

Glass beads were used to improve the mechanical and thermal properties of high-density polyethylene (HDPE). HDPE/glass-bead blends were prepared in a Brabender-like apparatus, and this was followed by press molding. Static tensile measurements showed that the modulus of the HDPE/glass-bead blends increased considerably with increasing glass-bead content, whereas the yield stress remained roughly unchanged at first and then decreased slowly with increasing glass-bead content. Izod impact tests at room temperature revealed that the impact strength changed very slowly with increasing glass-bead content up to a critical value; thereafter, it increased sharply with increasing glass-bead content. That is, the lzod impact strength of the blends underwent a sharp transition with increasing glass-bead content. It was calculated that the critical interparticle distance for the HDPE/glass-bead blends at room temperature (25degreesC) was 2.5 mum. Scanning electron microscopy observations indicated that the high impact strength of the HDPE/glass-bead blends resulted from the deformation of the HDPE matrix. Dynamic mechanical analyses and thermogravimetric measurements implied that the heat resistance and heat stability of the blends tended to increase considerably with increasing glass-bead content.

Fabrication of integrated microelectrodes for electrochemical detection on electrophoresis microchip by electroless deposition and micromolding in capillary technique

A new method for the fabrication of an integrated microelectrode for electrochemical detection (ECD) on an electrophoresis microchip is described. The pattern of the microelectrode was directly made on the surface of a microscope slide through an electroless deposition procedure. The surface of the slide was first selectively coated with a thin layer of sodium silicate through a micromolding in capillary technique provided by a poly(dimethylsiloxane) (PDMS) microchannel; this left a rough patterned area for the anchoring of catalytic particles. A metal layer was deposited on the pattern guided by these catalytic particles and was used as the working electrode. Factors influencing the fabrication procedure were discussed. The whole chip was built by reversibly sealing the slide to another PDMS layer with electrophoresis microchannels at room temperature. This approach eliminates the need of clean room facilities and expensive apparatus such as for vacuum deposition or sputtering and makes it possible to produce patterned electrodes suitable for ECD on microchip under ordinary chemistry laboratory conditions. Also once the micropattern is ready, it allows the researchers to rebuild the electrode in a short period of time when an electrode failure occurs. Copper and gold microelectrodes were fabricated by this technique. Glucose, dopamine, and catechol as model analytes were tested.

Relationship between the continually expanded interlayer distance of layered silicates and excess intercalation of cationic surfactants

Excess intercalation of cationic surfactants into Na-montmorillonites (MMTs) was investigated in organically modified silicates (OMSs), synthesized with MMTs and octadecylammonium chloride (OAC) by systematically varying the surfactant loading level from 0.625 to 1, 1.25, 1.56, 2, and 2.5 with respect to the cation exchange capacity (CEC) of MMTs. Wide-angle X-ray diffraction and thermogravimetric analysis results indicated that the continuous increase of interlayer distances came from the entering of surfactants into the interlayer of MMTs. Excess surfactants were extracted with a Soxhlet apparatus, which showed two kinds of intercalation states of surfactants in the interlayer when the surfactant loading level was beyond the CEC. Fourier transform infrared spectroscopy and differential scanning calorimetry were used to explore the microstructures of OMSs. It was found that the surfactants arranged more orderly as the loading level increased and the excess surfactants piled up in the interlayer together with counterions, forming a sandwiched surfactant layer. On the basis of the results, the layer structures of OMSs and the mechanism by which the surfactants entered the interlayer were expounded: surfactant cations entered the interlayer through cation exchange reactions and were tightly attracted to the silicate platelet surfaces when the surfactant loading level was below the CEC;

Study of PVT behavior of biaxially oriented polypropylene resins in the melting state

The PVT data of five kinds of biaxially oriented polypropylene (BOPP) Resins was measured by the PVT-100 apparatus. Thermal expansion coefficients (alpha) and isothermal compressibility (beta) were evaluated from Tait equation in the melting state and then compared with those fitted with the value of experiment. The results showed that it was reasonable to calculate alpha and beta with Tait equation in the melting state. At the same time, it was found that thermal expansion coefficients, isothermal compressibility and the melting temperature (T-m) of one of BOPP melts (S28C) were lower than those of the others in the same test conditions, indicating that the volume deformation of S28C resin is' less so that it could be realized to avoid arising surface defects of the film (biaxially oriented polypropylene film) due to. contracting, thereby decrease damage to the film in the subsequence process. Accordingly superior processing properties of S28C resin are confirmed from PVT. speciality.

Identification of high-lying odd energy levels of uranium by resonant ionization mass spectrometry

Single-colour and two-colour multiphoton resonant ionization spectra of uranium atom were studied extensively with a Nd: YAG laser-pumped dye laser atomic beam apparatus time-of-flight mass spectrometer in our laboratory. The energy locations of high-lying odd-parity levels in the region 33 003-34 264 cm(-1),mearured by a two-colour three-step ionization technique, were reported here. The angular momentum quantum number J was uniquely assigned for these levels by using angular momentum selection rules.

The kinetics study in liquid-liquid systems with constant interfacial area cell with Laminar flow

A novel constant interfacial cell with laminar flow is proposed as an approach to obtain extraction kinetics data in liquid-liquid systems. Applications and theoretical fundamentals of the apparatus have been elaborated.. The equation which can express the mass transfer of liquid-liquid system run in the constant interfacial cell with laminar flow is deduced. Simulations from the equations indicate that diffusivity is a suitable factor to represent the characteristics of extraction kinetics rather than the extraction rate in the diffusion controlling step. The dependence of the aqueous phase concentration on time is recommended to determine the extraction regime. The diffusivities of the EuCl3-HDEHP extraction system obtained by different methods are compared to certify the hydrodynamic theory of the cell. The diffusivities of the ErCl3-HEH/EHP extraction system are determined, which show that this technique is a convenient method to obtain the diffusivities in the liquid-liquid system and to determine the extraction regime. (C) 1998 Elsevier Science Ltd. All rights reserved.

An amperometric detector with a tubular electrode deposited on the capillary for capillary liquid chromatography

A procedure is described for the preparation of a tubular electrode by chemical deposition of platinum at the end of a fused-silica capillary. The properties of the electrode were tested under liquid chromatographic conditions, demonstrating that both the static and the dynamic behaviour of the detection system satisfy the requirements of capillary chromatographic separations and compare well with a wall-jet amperometric system and with UV photometric detection. The detection system described is easy to prepare and does not require any time-consuming positioning of the electrode system as it is integrated into the separation part of the apparatus. (C) 1998 Elsevier Science B.V.

Synthesis, extraction and electronic structure of Ce@C-2n

In view of the growing interest in endohedral lanthanide fullerenes, Ce, as a typical +4 oxidation state lanthanide element, has been systematically studied. The synthesis, extraction and electronic structure of Ce@C-2n are investigated. Soot containing Ce@C-2n was synthesized in high yield by carbonizing CeO2-containing graphite rods and are back-burning the CeC2-enriched cathode deposit in a DC are plasma apparatus. Ce@C-2n, dominated by Ce@C-82, can be efficiently extracted from the insoluble part of the soot after toluene Soxhlet extraction by pyridine at high temperature and high pressure in a closed vessel. About 60% Ce@C-2n (2n = 82,80,78,76) and 35% Ce@C-82 can be enriched in the pyridine extract. This fact is identified by desorption electron impact mass spectrometry (DEI MS). The electronic structure of Ce@C-2n is analyzed by using X-ray photoemission spectroscopy (XPS) of pyridine-free film. It is suggested that the encapsulated Ce atom is in a charge state close to +3 and was effectively protected from reaction with water and oxygen by the enclosing fullerene cage. Unlike theoretical expectation, the electronic state of Ce@C-82 is formally described as Ce+3@C-82(3-). (C) 1997 Elsevier Science Ltd.

Application of digital image analysis to the study of banded spherulite during growing and melting process

A digital image analysis(DIA) technique can be applied directly to the image obtained by polarizing microscope. The time-resolved DIA apparatus including image collecting, showing and data analysis has been home-made. As an example, it has been used to study the banded spherulite in the blends of poly(epsilon-caprolactone) (PCL) and poly(styrene-ran-acrylonitrile) (SAN).

Study of the blends containing core-shell latex polymer

Polycarbonate (PC) and a core-shell latex polymer composed of poly(butyl acrylate) and poly(methyl methacrylate) (PBA-cs-PMMA) as core and shell, respectively, were mixed using a Brabender-like apparatus under different conditions. The mechanical properties, the morphology and the processability of the blends were investigated. Because of the good compatibility of PC and PMMA, even dispersion of PBA-cs-PMMA in PC matrix and good adhesion between the components have been achieved. PBA-cs-PMMA is thus a very good impact modifier for PC. The toughening mechanism is both cavitation and shear yielding, as indicated by SEM observation. (C) 1997 Elsevier Science Ltd.

Toughening of poly(butylene terephthalate) with epoxidized ethylene propylene diene rubber

In this paper, unepoxidized ethylene propylene diene rubber (uEPDM) was first epoxidized with formic acid and H2O2, and then the epoxidized ethylene propylene diene rubber (eEPDM) was melt-mixed with PET resin in a Brabender-like apparatus. Toughening of PET matrix was achieved by this method. The dispersion of rubber particles and phase structure of the blends were also observed by SEM. It has been suggested that the epoxy groups in the eEPDM could react with PET end groups to form a graft copolymer which could act as an interfacial compatibilizer between the PBT matrix and eEPDM rubber dispersed phase. This is beneficial to the improvement of the impact performance of PBT. (C) 1997 Elsevier Science Ltd.

Impedance spectrum measurement in liquid liquid interface electrochemistry .1. Analysis of various kinds of interfacial impedance in the four-electrode system

Applying impedance spectrum technique to liquid/liquid interfacial electrochemistry, we present the theoretical expression of the liquid/liquid interfacial impedance in the four - electrode electrolytic cell measured by alternating current impedance method. The influence of the electrolytic cell parameters and input passage parameters of the impedance apparatus on impedance spectrum curves are theoretically studied.

Mechanical properties and miscibility of polyethersulfone phenoxy blends

The blends of polyethersulfone and phenoxy were prepared by melt mixing in a Brabender-like apparatus. The specimens for measurements were made by compression molding and then were water-quenched at room temperature under pressure. The tensile strength, tensile modulus, elongation at break and yield, density, thermal analysis, and dynamic mechanical properties were each measured. The dependence of tensile strength, tensile modulus, elongation at break and yield, and density on composition was obtained. The relationship between tensile modulus and elongation at break and yield and speed of the crosshead at different weight ratios of the blends is shown. The effects of composition and miscibility on the mechanical properties are discussed. (C) 1996 John Wiley & Sons, Inc.

ELECTROCHEMICAL SCANNING-TUNNELING-MICROSCOPY

An ECSTM apparatus with an ideal tip using a homemade SSX-1A STM instrument has been constructed. STM and ECSTM tips were made by electrochemical etching and insulating with paraffin, silicon rubber or epoxy resin under an optical microscope. In situ imag