Room-Temperature,Metal-Free,and One-Pot Preparation of 2H-Indazoles through a Mills Reaction and Cyclization Sequence

The Mills reaction and cyclization of readily available 2-aminobenzyl alcohols and nitrosobenzenes using thionyl bromide provided 2H-indazoles in up to 88 % yields. In the metal-free process, acetic acid played a crucial role for the both Mills reaction and cyclization. A brominated 2H-indazole could also be obtained through the one-pot sequence.     

Preparation of benzoylchitosans and their chiroptical properties in dilute solutions

Two benzoyl substituted chitosan derivatives, 3,6‐O‐dibenzoylchitosan (DBC) and 2‐N‐3,6‐O‐tribenzoylchitosan (TBC), were prepared, and their optical activities in organic solvent were investigated by circular dichroism (CD). For TBC, two splitting bands (a negative one at 288 nm and a positive one at 274 nm) corresponding to the ¹L_b transition of the benzoyl group were observed in chloroform and dichloromethane, while only a negative CD band was recorded in N, N‐dimethylformamide (DMF). These results indicated that the transition moments of benzoyl groups were orderly arranged along the helical polymer chain when TBC was dissolved in a solvent with low polarity, but the same ordered structure did not appear in a polar solvent of DMF. For DBC, only negative CD signals corresponding to the ¹L_b transition of the benzoyl group were observed, regardless of the solvent property, which indicated that the chromophores were not arranged in an ordered fashion with appropriate geometry to interact with one another to induce bi‐signate CD signals. Adding methanol or DMF to the solution of TBC/chloroform resulted in a progressive decrease of the intensity of the positive split band at 274 nm. The intensity of the positive band was weakened upon heating a solution of TBC/chloroform from 20 to 60 °C. The results suggested that the ordered arrangement of the chromophores in the TBC system was dependent on solvent and sensitive to temperature. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 42: 4107–4115, 2004     

Ultrahigh‐molecular‐weight‐polyethylene‐fiber surface treatment by electron‐beam‐irradiation‐induced graft polymerization and its effect on adhesion in a styrene–butadiene rubber matrix

Aiming to develop a high‐performance fiber‐reinforced rubber from styrene–butadiene rubber (SBR), we applied a special technique using electron‐beam (EB)‐irradiation‐induced graft polymerization to ultrahigh‐molecular‐weight‐polyethylene (UHMWPE) fibers. The molecular interaction between the grafted UHMWPE fibers and an SBR matrix was studied through the evaluation of the adhesive behavior of the fibers in the SBR matrix. Although UHMWPE was chemically inert, two monomers, styrene and N‐vinyl formamide (NVF), were examined for graft polymerization onto the UHMWPE fiber surface. Styrene was not effective, but NVF was graft‐polymerized onto the UHMWPE fibers with this special method. A methanol/water mixture and dioxane were used as solvents for NVF, and the effects of the solvents on the grafting percentage of NVF were also examined. The methanol/water mixture was more effective. A grafting percentage of 16.4% was the highest obtained. This improved the adhesive force threefold with respect to that of untreated UHMWPE fibers. These results demonstrated that EB irradiation enabled graft polymerization to occur even on the inert surface of UHMWPE fibers. However, the mechanical properties of the fibers could be compromised according to the dose of EB irradiation. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 42: 2595–2603, 2004     

Improved detectability with a polymer-based trapping device in rapid HPLC analysis for ultra-low levels of bisphenol A (BPA) in environmental samples.

A new high-performance liquid chromatography (HPLC) method has been developed to detect ultra-low concentrations of bisphenol-A (BPA) (below 1 ng/L (ppt)) using column switching electrochemical detection (ECD). The results were superior to those obtained from manual pretreatment procedure with membrane stationary phase. BPA is inherently ubiquitous in the environment, including tools and solvents used for its analysis; to obtain meaningful results, therefore, the concentration of the overall BPA contamination must be below the detection limit for BPA using the analytical system. Therefore, purified water for preparing the standard BPA solution must be filtered with a hydrophobic membrane to suppress BPA background levels of contamination. In addition, we investigated methods for effectively preserving environmental water containing BPA. The addition of a small amount of ethylenediaminetetraacetic acid (EDTA) provided good recovery even after overnight storage. By employing these precautionary measures and procedures to reduce BPA contamination from the analytical procedure, we could accurately determine l(-10) ppt of BPA in environmental water samples using a column switching HPLC system.     

Boundary position feedback control of Kirchhoff's non‐linear strings

This paper is concerned with global stabilization of an undamped non‐linear string in the case where any velocity feedback is not available. The linearized system has an infinite number of poles and zeros on the imaginary axis. In the case where any velocity feedback is not available, a parallel compensator is effective. The stabilizer is constructed for the augmented system which consists of the controlled system and a parallel compensator. It is proved that the string can be stabilized by linear boundary control. Copyright © 2003 John Wiley & Sons, Ltd.     

Low‐gain adaptive stabilization of semilinear second‐order hyperbolic systems

In this paper low‐gain adaptive stabilization of undamped semilinear second‐order hyperbolic systems is considered in the case where the input and output operators are collocated. The linearized systems have an infinite number of poles and zeros on the imaginary axis. The adaptive stabilizer is constructed by a low‐gain adaptive velocity feedback. The closed‐loop system is governed by a non‐linear evolution equation. First, the well‐posedness of the closed‐loop system is shown. Next, an energy‐like function and a multiplier function are introduced and the exponential stability of the closed‐loop system is analysed. Some examples are given to illustrate the theory. Copyright © 2004 John Wiley & Sons, Ltd.     

Linear and Nonlinear Optical Properties Of Racemic (±)2-(α-Methylbenzylamino)-5-Nitropyridine Single Crystals

Linear and nonlinear optical properties of racemic (±)2-(α-methylbenzylamino)-5-nitropyridine ((±)MBANP) single crystals have been comprehensively investigated and compared with those of the enantiomorph (–)2-(α-methylbenzylamino)-5-nitropyridine ((–)MBANP) crystals. (±)MBANP crystal exhibits very high chemical and physical stability, but relatively small nonlinear optical coefficients (d₃₁ = 6.8 pm/V, d₃₂ = 4.7 pm/V, d₃₃ = 0.84 pm/V). A comparison between the nonlinear optical coefficients of (±)MBANP and (–)MBANP demonstrates the validity of the oriented-gas model in molecular crystals that neglects all the contributions from intermolecular interaction.     

Precise chelatometric titrations of zinc, cadmium, and lead with molecular spectroscopy.

Spectral data during a chelatometric titration were utilized for determining an equivalence point of the titration. Three-dimensional titration data were analyzed by fitting to a theoretical equation that was derived from equilibrium equations among a metal ion, an indicator and EDTA. The equation with optimized parameters successfully explained the three-dimensional titration data. This method was applied to EDTA titration systems of zinc, cadmium and lead with xylenol orange (XO) as an indicator. These systems were analyzed while taking the formation of 1:1 and 2:1 metal-indicator complexes into account. By this method, an accurate equivalence point was determined as well as stability constants and molar absorption spectra of metal-indicator complexes in each titration system. Moreover, the comparability among the concentrations of the metal standard solutions prepared from pure metals (Zn, Pb, and Cd) was also confirmed by the proposed evaluation method.     

New Plasmon Waveguides Composed of Twin Metal Wedges with a Nano Gap

We have numerically shown the existence of coupled wedge plasmons (CWPs) which propagates along a nano gap of a twin metal wedge. The CWPs are formed by wedge plasmons which can interact with each other. The dispersion relations of the wavenumber, propagation distance, and beam area of CWPs, are described and show that the characteristics of CWPs are similar to those of wedge plasmons and of gap plasmons. We also propose a new plasmon waveguide composed of twin metal wedges with a nano gap.     

In situ observations of domain wall motion in Mn–Zn and Ni–Zn ferrites by Lorentz microscopy and electron holography

Domain wall motion in Mn–Zn and Ni–Zn ferrites with applied magnetic fields is investigated by in situ observations with Lorentz microscopy and electron holography. It is found that both Mn–Zn and Ni–Zn ferrites have a mean grain size of approximately 10 μm and several pores with sizes ranging from 0.2 to 1.1 μm. In situ observations by Lorentz microscopy with an applied magnetic field reveals that in Mn–Zn ferrite, the domain walls move easily across the grain boundary, while in Ni–Zn ferrite, the domain walls move along the grain boundary but are pinned at the grain boundary and pores. From in situ observations of Ni–Zn ferrite by electron holography, it is clarified that domain wall pinning at the grain boundary retards a sensitive increase in magnetic flux parallel to the applied field direction, which is considered to result in high hysteresis loss.