Ethylene–propylene copolymerization with bis(β‐enaminoketonato) titanium complexes activated with modified methylaluminoxane

Ethylene–propylene copolymerization, using [(Ph)NC(R₂)CHC(R₁)O]₂TiCl₂ (R₁ = CF₃, Ph, or t‐Bu; R₂ = CH₃ or CF₃) titanium complexes activated with modified methylaluminoxane as a cocatalyst, was investigated. High‐molecular‐weight ethylene–propylene copolymers with relatively narrow molecular weight distributions and a broad range of chemical compositions were obtained. Substituents R₁ and R₂ influenced the copolymerization behavior, including the copolymerization activity, methylene sequence distribution, molecular weight, and polydispersity. With small steric hindrance at R₁ and R₂, one complex (R₁ = CF₃; R₂ = CH₃) displayed high catalytic activity and produced copolymers with high propylene incorporation but low molecular weight. The microstructures of the copolymers were analyzed with ¹³C NMR to determine the methylene sequence distribution and number‐average sequence lengths of uninterrupted methylene carbons. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 5846–5854, 2006     

Synthesis and light emitting properties of polyacetylenes having pendent fluorene groups

Five novel fluorene‐containing polymers, poly[(9,9‐dimethylfluoren‐2‐yl)acetylene] ( PFA1 ), poly[(1‐pentyl‐2‐(9,9‐dimethylfluoren‐2‐yl)acetylene) ( PFA2 ), poly[1‐decyl‐2‐(9,9‐dimethylfluoren‐2‐yl)acetylene] ( PFA3 ), poly[1‐phenyl‐2‐(9,9‐dimethylfluoren‐2‐yl)acetylene] ( PFA4 ), and poly[1‐(3,4‐difluorophenyl)‐2‐(9,9‐dimethylfluoren‐2‐yl)acetylene] ( PFA5 ) were synthesized by the polymerization of the corresponding fluorene‐substituted acetylenic monomers ( M1–M5), using WCl₆, MoCl_5, and TaCl₅ as catalysts and n‐Bu₄Sn as a cocatalyst. The synthesized polymers were thermally stable and readily soluble in common organic solvents. The degradation temperatures for a 5% weight loss of the polymers were ∼352–503 °C under nitrogen. PFA1–PFA5 show emission peaks from 402 to 590 nm. Besides, their electroluminescent properties were studied in heterostructure light‐emitting diodes (LEDs), using PFA2–PFA5 as an emitting layer. The PFA5 device revealed an orange‐red emission peak at 602 nm with a maximum luminescence of 923 cd/m² at 8 V. A device with the ITO/PEDOT/ a mixture of PFA2 (98 wt %) and PFA5 (2 wt %)/Ca/Al showed near white emission. Its maximum luminance and current efficiency are 450 cd/m² at 15 V and 1.3 cd/A, respectively. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 519–531, 2006     

Chemically modified proton‐conducting membranes based on sulfonated polyimides: Improved water stability and fuel‐cell performance

A series of branched/crosslinked sulfonated polyimide (B/C‐SPI) membranes were prepared and evaluated as proton‐conducting ionomers based on the new concept of in situ crosslinking from sulfonated polyimide (SPI) oligomers and triamine monomers. Chemical branching and crosslinking in SPI oligomers with 1,3,5‐tris(4‐aminophenoxy)benzene as a crosslinker gave the polymer membranes very good water stability and mechanical properties under an accelerated aging treatment in water at 130 °C, despite their high ion‐exchange capacity (2.2–2.6 mequiv g^?1). The resulting polymer electrolytes displayed high proton conductivities of 0.2–0.3 S cm^?1 at 120 °C in water and reasonably high conductivities of 0.02–0.03 S cm^?1 at 50% relative humidity. In a single H₂/O₂ fuel‐cell system at 90 °C, they exhibited high fuel‐cell performances comparable to those of Nafion 112. The B/C‐SPI membranes also displayed good performances in a direct methanol fuel cell with methanol concentrations as high as 50 wt % that were superior to those of Nafion 112. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 3751–3762, 2006     

Preparation and characterization of rigid poly(vinyl chloride)/MMT nanocomposites. II. XRD,morphological and mechanical characteristics

A Haake torque rheometer equipped with an internal mixer is used to study the influence of the amount of sodium montmorillonite (Na⁺‐MMT) and organically modified MMT (O‐MMT) on X‐ray diffraction (XRD), morphology, and mechanical characteristics of rigid poly (vinyl chloride) (PVC)/Na⁺‐MMT and PVC/O‐MMT nanocomposites, respectively. Results of XRD and transmission electron microscopy (TEM) indicate that MMT is partially encapsulated and intercalated in the rigid PVC/Na⁺‐MMT nanocomposites. However, results of XRD and TEM show MMT is partially intercalated and exfoliated in the rigid PVC/O‐MMT nanocomposites. Tensile strength, yield strength, and elongation at break of the rigid PVC/MMT nanocomposites were improved simultaneously with adding 1–3 wt % Na⁺‐MMT or O‐MMT with respect to that of pristine PVC. However, the addition of Na⁺‐MMT or O‐MMT should be kept as not more than 3 wt % to optimize the mechanical properties and the processing stability of the rigid PVC/MMT nanocomposites. SEM micrographs of the fractured surfaces of the rigid PVC/Na⁺‐MMT and PVC/O‐MMT nanocomposites both before and after tensile tests were also illustrated and compared. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 2145–2154, 2006     

Automated method, based on micro-sequential injection, for the study of enzyme kinetics and inhibition.

A micro-reactor system with continual spectrophotometric detection has been operated in Sequential Injection lab-on-valve (SI-LOV) mode and applied to enzyme kinetics and inhibition studies, using acetylcholinesterase (AChE) and angiotensin-converting enzyme (ACE) as model systems. With the advantages of automation, real-time kinetic measurement, and thorough mixing, the SI-LOV micro-reactor system allows for the monitoring of initial reaction rates and determination of reactant concentrations in the reaction mixture, both of which are essential for the determination of kinetic constants for enzymes and inhibitors. Enzyme, substrate, and inhibitor are precisely metered by the syringe pump and delivered to a stirred micro-reactor, followed by a reference scan that establishes the baseline for the following reaction rate measurement. Michaelis constants (Km) for AChE and ACE were determined to be 0.16 mM and 0.30 mM, respectively, which are consistent with literature values. The type of inhibition (competitive, uncompetitive, or mixed), the dissociation constants for the inhibitors, and the inhibitor dose-response curves were also determined.     

Chiral separation of synthetic vicinal diol compounds by capillary zone electrophoresis with borate buffer and beta-cyclodextrin as buffer additive.

The investigation on capillary electrophoretic enantioseparation of six synthetic compounds containing vicinal diol groups has been undertaken to acquire the optimum conditions using native beta-cyclodextrin (beta-CD) as chiral selector and borate as a background electrolyte. The separation was carried out in an uncoated capillary (58.5 cm x 75 microm i.d., effective length 48.5 cm) and the effects of several important factors were investigated in detail. The results showed that beta-CD as a chiral selector exhibited good enantioselectivity and that the enantioseparation was greatly influenced by the structure of the diols, the borate concentration and the buffer pH. The optimum performance was obtained for the chiral vicinal diols under the conditions of 200 mM borate buffer of pH 9.8 containing 1.7% beta-CD at an applied voltage of 15 kV and a capillary temperature of 20 degrees C. Under the conditions, four diols were baseline separated with fast analysis time and the good theoretical plate numbers (above 10 x 10(4)) and favorable migration-time reproducibilities (RSDs below 3.0%) were obtained. The separation results were satisfactory.     

A highly sensitive and rapid assay for protein determination in human urine and penicillin using a Rayleigh light-scattering technique with benzeneazo-8-acetylamino-1-naphthol-3,6-disulfonic acid sodium salt.

A simple and sensitive method was conducted for the determination of trace amounts of proteins with benzeneazo-8-acetylamino-1-naphthol-3,6-disulfonic acid sodium salt (azophloxine, AP) using a Rayleigh light-scattering (RLS) technique. At pH 2.60 and in the presence of an emulsifier OP microemulsion, the RLS of AP can be greatly enhanced by proteins, owing to the interaction between AP and protein. The enhanced intensity is proportional to the concentration of proteins. Four proteins, including bovine serum albumin (BSA), human serum albumin (HSA), lysozyme (Lys) and gamma globulin (gamma-G) have been tested. For example, the linear range of BSA was 0 - 0.06 microg mL(-1) with detection limits of 2.38 ng mL(-1). The method was applied to the analysis of protein in human urine and penicillin samples with satisfactory results. The relative standard deviation was in all instances less than 4.0%, and the recovery was in the range of 97.5 - 104%.     

Effects of microstructure on the temperature dependence of relative initial permeability of NiCuZn ferrites

In the present work, ferrites with compositions of (Ni_0.27Zn_0.64Cu_x)Fe_1.98O₄ (x=0.1, 0.2) were prepared by conventional ceramic methods. The relationship between the microstructure and the temperature dependence of relative initial permeability was investigated. It was found that intergranular pores in the ferrites generate large demagnetizing fields, reducing the temperature dependence of the effective anisotropy field H_eff, and decreasing the temperature dependence of the relative initial permeability accordingly. However, intragranular pores pin the movement of domain walls. Compared with the permeability induced by domain wall motion, the permeability that resulted from the spin rotation is more sensitive to temperature. As a result, the relative initial permeability of ferrites becomes more sensitive to temperature with increasing micropores within grains.     

Retracted: Determination of scutellarin isomer,a predominant metabolite of scutellarin,in human plasma by HPLC/tandem mass spectrometry and its application to a pharmacokinetic study in Chinese healthy volunteers

Retraction: The following article from Biomedical Chromatography, “Determination of scutellarin isomer, a predominant metabolite of scutellarin, in human plasma by HPLC/tandem mass spectrometry and its application to the pharmacokinetic study in Chinese healthy volunteers” by Chun‐hua Xia, Yu‐qing Xiong, and Guang‐ji Wang, published online on 21 June 2007 in Wiley Interscience (www.interscience.wiley.com/journal/bmc), has been retracted at the authors' request.     

LIMITING BEHAVIOR OF UNIFORM RECURSIVE TREES

The authors consider the limiting behavior of various branches in a uniform recursive tree with size growing to infinity.The limiting distribution ofζ_(n,m),the number of branches with size m in a uniform recursive tree of order n,converges weakly to a Poisson distribution with parameter 1/m with convergence of all moments.The size of any large branch tends to infinity almost surely.