(Z)-1-[2-(Triarylstannyl)vinyl]-1-cycloheptanols: Synthesis, characterization, halodemetallation and crystal structures

The synthesis and characterization by ¹H, ¹³C, ¹¹⁹Sn NMR and ¹¹⁹Sn Mössbauer spectroscopy of (Z)-1-[2-(triphenylstannyl)vinyl]-1-cycloheptanol,

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(1), and (Z)-1-[2-tri-p-tolylstannyl)vinyl-1-cycloheptanol,

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(2), are described, together with their halodemetallation by I₂, Br₂ and ICIl to yield derivatives of the types

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(Ar = phenyl or p-tolyl, N = 1, 2; X = I, Br, Cl, respectively). The solid-state structures of four compounds have been determined by X-ray diffraction analysis. In the crystals of

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(1) and

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(2) the Sn atom has a tetrahedral geometry distorted towards trigonal bipyramid as a consequence of a close intramolecular contact with the hydroxyl O(1) atom of 2.742(3) Å and 2.768(3) Å, respectively. A trigonal bipyramidal geometry is found in

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(12) and

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(4), in which significant Sn---O(1) interactions are noted [2.437(8) Å and 2.407(8) Å, respectively].     

Carbon nanofibers extracted from soot as a sorbent for the determination of aromatic amines from wastewater effluent samples

The isolation and characterization of carbon nanofibers from soot obtained by burning natural oil is reported. The fibers were extracted from the soot with tetrahydrofuran followed by sonication. The carbon nanofibers were mixed with poly(vinyl alcohol) and electrospun to get the nanofiber mat. The extraction ability of electrospun nanofibers for the separation and preconcentration of aromatic compounds such as 3-nitroaniline, 4-chloroaniline, 4-bromoaniline and 3,4-dichloroaniline were tested and efficiently evaluated using high performance liquid chromatography. Under optimized conditions, the method showed good linearity in a range of 0.5–50 μg L⁻¹ with correlation coefficient ranging from 0.989 to 0.998. High precision of the extraction with RSD values of 4.5–5.8% and low LOD value in a range of 0.009–0.081 μg L⁻¹ for all aniline compounds were achieved. The proposed microextraction method offers advantages such as easy operation, high recovery, fast extraction, minimal use of organic solvent and elimination of tedious solvent evaporation and reconstitution steps.     

Voltammetric study of copper(I) thioacetamide complexes

Summary The composition and stability of copper(I) complexes with thioacetamide (TAA) have been evaluated with the help of square-wave voltammetry using the fast pulse technique. Two species, namely Cu(I) (TAA) and Cu(I) (TAA)₂, have been identified having the formation constants log ₁=16.85; log ₂=18.03. The complex is stable in highly acidic medium (pH1). The application for the determination of copper is pointed out.     

Enhanced thermal properties and flame retardancy from a thermosetting blend of a phosphorus‐containing bismaleimide and epoxy resins

Epoxy resins modified by an organosoluble phosphorus‐containing bismaleimide (3,3′‐bis(maleimidophenyl) ­phenylphosphine oxide; BMPPPO) were prepared by simultaneously curing epoxy/diaminodiphenylmethane (DDM), and BMPPPO. The resulted epoxy resins were found to exhibit glass transition temperatures as high as 212 °C, thermal stability at temperatures over 350 °C, and excellent flame retardancy with Limited oxygen index (LOI) values around 40. Incorporation of BMPPPO into epoxy resins via the thermosetting blend was demonstrated to be an effective way to enhance the thermal properties and flame retardancy simultaneously. Copyright © 2003 John Wiley & Sons, Ltd.     

Review of nanofluids for heat transfer applications

Research on nanofluids has progressed rapidly since its enhanced thermal conductivity was first repotted about a decade ago,though much controversy and inconsistency have been reported,and insufficient understanding of the formulation and mechanism of nanofluids further limits their applications.This work presents a critical review of research on heat transfer applications of nanofluids with the aim of identifying the limiting factors so as to push forward their further development.     

Preparation and Application of Cholesteryl‐Benzo‐15‐Crown‐5/Cholesteryl Mixed Liquid Crystals

Various mixed liquid crystals containing crown ether‐cholesteryl liquid crystal, benzo‐15‐crown‐5‐COO‐C₂₇H₄₅ (B15C5‐COOCh), with various common cholesteric liquid crystals, e.g., cholesteryl chloride, cholesteryl benzoate and cholesteryl palmitate, were prepared and studied using polarizing microscopy and differential scanning calorimetry. Investigating the concentration effect of B15C5‐COOCh in mixed liquid crystals revealed that the addition of B15C5‐COOCh resulted in wider phase transition temperature ranges of these cholesteryl liquid crystals. The stability of these B15C5‐COOCh/cholesteryl mixed liquid crystals was studied using comprehensive graphic molecular modeling computer programs (Insight II and Discover) to calculate their molecular energy and stability energy. The effect of salts, e.g. Na⁺, Co³⁺, Y³⁺ and La³⁺, on the transition temperature range of the mixed liquid crystals was also investigated. The crown ether cholesteric liquid crystal B15C5‐COOCh was applied both as a surfactant and an ion transport carrier to transport metal ions through liquid membranes. Cholesteryl benzo‐15‐crown‐5 exhibited distinctive characteristics of a surfactant and the critical micellar concentration (CMC) of the surfactant was investigated by the pyrene fluorescence probe method. Cholesteryl benzo‐15‐crown‐5 was successfully applied as a good ion transport carrier (Ionophore) to transport various metal ions, e.g. Li⁺, Na⁺, La³⁺, Fe³⁺ and Co³⁺, through organic liquid membranes. The transport ability of the cholesteryl benzo‐15‐crown‐5 surfactant for these metal ions was in the order: Co³⁺ ≥ Li⁺ > Fe³⁺ > Na⁺ > La³⁺.     

联二炔囊泡的光致聚合、热致变色及应用

物理化学实验为各大高校本科化学教学的主干实验课程之一。虽然各高校的物理化学实验内容已十分丰富,但仍然缺乏将不同章节知识点融会贯通以及与学科前沿密切联系的综合型实验内容。我们根据南开大学郭东升教授课题组发表的一篇有关联二炔程序性响应检测胆碱酯酶的工作设计了"联二炔囊泡的光致聚合、热致变色及应用"的物理化学实验,涉及到联二炔缔合胶体的制备、联二炔的紫外光致聚合反应和聚联二炔的热致变色,进而显示其在防伪领域的潜在应用价值。希望通过此实验,使学生对物理化学中的缔合胶体、光化学、热力学、动力学等章节有更深一步的贯通性掌握,并了解自组装、光聚合、变色材料和防伪等相关研究领域的前沿动态。     

随机静态存储器低能中子单粒子翻转效应

建立了中子单粒子翻转可视化分析方法,对不同特征尺寸（0.13~1.50 μm）CMOS工艺商用随机静态存储器(SRAM)器件开展了反应堆中子单粒子翻转效应的实验研究,获得了SRAM器件的裂变谱中子单粒子翻转截面随特征尺寸变化的变化趋势。研究结果表明:SRAM器件的特征尺寸越小,其对低能中子导致的单粒子翻转的敏感性越高。     

超临界流体萃取-胶束电动毛细管色谱法分离测定大黄中蒽醌类组分的含量

采用ＳＴＥ－ＭＥＣＣ法分离测定大黄中的芦荟大黄素，大黄素和大黄酸。萃取条件为压 力４１．４ＭＰａ，温度５０℃，改性剂量０．４ｍＬ。被测组分在１０ｍｉｎ得到全部分离。本法准确、简 便、快速、结果令人满意。     

进行子阵加权波束形成的波达方向估计

针对水声信道的多径效应以及海底散射信号信噪比低导致方位估计性能较差的问题,提出了一种基于子阵加权波束形成的UESPRIT算法(Weighted Beamspace UESPRIT Based on Subarrays,BS-BUESPRIT)。首先利用密集波束域转换矩阵估计回波信号的方位谱,进而估计同一时刻到达阵列的回波数目;之后将均匀线阵分为多个尺寸相同、相互重叠的子阵,利用加权波束形成对各子阵接收信号做指定方向的空域滤波;最后基于各子阵波束形成后的输出结果,利用UESPRIT算法实现回波方向的估计。仿真和湖试、海试试验结果表明,与UESPRIT算法相比,BS-BUESPRIT算法提高了信号波达方向估计性能,在多径和较低信噪比条件下有着更高的估计精度,应用于高分辨率测深侧扫声呐时有效地提高了声呐的测深性能。