Synthesis of novel tetracyclic chromenes through carbanion chemistry of 4-methyl coumarins

Various substituents were introduced onto the methyl group in 4-methyl coumarins through lithiation, followed by reactions with a wide range of electrophiles. The presence of an alkoxy group on 6′-phenyl ring was found to be pivotal for the success of this reaction. This procedure provided a convenient synthetic pathway to elaborate the methyl group of 4-methylcoumarins. Application of this methodology was showcased with the synthesis of biologically important novel tetracyclic chromene ring systems (n = 1-3).     

同步荧光法同时测定苯甲酸和水杨酸的研究

根据苯甲酸与水杨酸在酸性条件下荧光光谱出现的差异，用同步荧光法同时测定其混合物中二组份。苯甲酸及水杨酸的检测限分别为０．２４μｇ／ｍＬ和０．２５μｇ／ｍＬ相对标准偏差分别为１．３％和１．２％。方法用于商品杀菌腐剂中苯甲酸与水杨酸的同时测定，结果满意。     

Single-Molecule single crystals of isotactic polystyrene

Single-molecule single crystals were grown from amorphous droplets of fractionated isotactic polystyrene. The crystals were analyzed by electron microscopy and electron diffraction. The molecular mass distribution could be matched with a statistical analysis of single-molecule particles (amorphous and crystals). Proof was brought that single molecules of isotactic polystyrene do not reach equilibrium dimensions on crystallization, rather assume the lamellar morphology with chain-folded macroconformation, also known from crystallization of polymolecular crystals. © 1994 John Wiley & Sons, Inc.

1 This article is a US Government work and, as such, is in the public domain in the United States of America. US Government contract No. DE-AC05-840R-21400.

     

化学蒸气沉积硅氧化合物调变HZSM－5沸石的研究

本文研究了正硅酸乙酯分别在无胺法和有胺法制得的ＨＺＳＭ－５沸石上的沉积过程，并用吸附，ＮＨ３－ＴＰＤ及异丙醇探针反应等手段表征了沉积后的样品，发现沉积仅在外表面上进行，可使孔口变小但不影响孔道内性质，显示有对于二甲苯分子的择形吸附能力，且在甲苯甲醇烷基化反应和二甲苯异构化反应中表现出良好的择形催化性能．     

Fused silica capillary deactivation with D4 in the presence of oxygen

A new, simple procedure to deactivate fused silica capillaries without hydrothermal treatment is proposed. Based on high temperature reactions of octamethylcyclotetrasiloxane (D₄) in the presence of oxygen, this procedure results, upon coating with dimethylsilicone (SE-30), in columns which give almost symmetric peaks for as little as 150 pg of critical compounds, such as decylamine, thereby demonstrating very high inertness. A mechanism of the deactivation procedure, which, in contrast to previously developed procedures, is based on thermal reactions under aerobic conditions, is proposed.     

SrZnO_2∶Eu~(3+),Li~+长波紫外激发红光荧光体的合成及发光性能研究

采用高温固相法合成了一种长波紫外激发的SrZnO2∶Eu3+,Li+发光材料,用X射线衍射谱、荧光光谱对样品进行了表征。结果表明,Eu3+离子在SrZnO2基质中主要占据Sr2+离子不对称性格位,发射来源于5D0→7F2612 nm为主的红光。加入电荷补偿剂Li+离子能显著提高发光强度,350~400 nm内的激发峰也有明显提高,同时观察到来自Eu3+离子高能级5D1→7FJ(J=0~2)的跃迁发射,并对其产生机制进行了初步探讨。实验结果表明,SrZnO2∶Eu3+,Li+是一种有发展前途的长波紫外激发红光荧光体。     

In-channel indirect amperometric detection of nonelectroactive anions for electrophoresis on a poly(dimethylsiloxane) microchip

In the present paper, we describe a microfluidics-based sensing system for nonelectroactive anions under negative separation electric field by mounting a single carbon fiber disk working electrode (WE) in the end part of a poly(dimethylsiloxane) microchannel. In contrast to work in a positive separation electric field described in our previous paper (Anal. Chem. 2004, 76, 6902-6907), here the electrochemical reduction reaction at the WE is not coupled with the separation high-voltage (HV) system, whereas the electrochemical oxidation reaction at the WE is coupled with the separation HV system. The electroactive indicator is the carbon fiber WE itself but not dissolved oxygen. This provides a convenient and sensitive means for the determination of nonelectroactive anions by amperometry. The influences of separation voltage, detection potential, and the distance between the WE and the separation channel outlet on the response of the detector have been investigated. The present detection mode is successfully used to electrochemically detect F-, Cl-, SO4(2-), CH3COO-, H2PO4-. Based on the preliminary results, a detection limit of 2 microM and a dynamic range up to three orders of magnitude for Cl- could be achieved.     

Tris(2,2''''-bipyridyl)ruthenium(Ⅱ) electrochemiluminescence (ECL) enhanced by rutin on platinum electrode

Ru(bpy)_(3~(2 )) electrochemiluminescence (ECL) was applied to determination of rutin. ECL intensity of Ru(bpy)_(3~(2 ))could be enhanced in the presence of rutin in basic solution on platinum electrode. At pH 9.9, light emission intensity was found to be linear with rutin in the range of 1-50 mmol/L.     

Study of urinary nucleosides as biological marker in cancer patients analyzed by micellar electrokinetic capillary chromatography

Thirteen normal and modified nucleosides, primarily degradation products of transfer ribonucleic acid (tRNA), were evaluated as potential tumor markers for cancer patients. Their urinary concentrations were determined by means of micellar electrokinetic capillary chromatography (MEKC) in the urine from 54 healthy adults and 70 cancer patients, then quantitatively expressed as a function of creatinine excretion. It was found that urinary nucleosides for cancer patients were on the average significantly higher than those for healthy controls, however, no significant differences were found between male and female or between different ages. Based on 13 urinary nucleoside concentrations, principal component analysis (PCA) could be used to classify 72% of cancer patients from the healthy controls. The present study shows that the precise measurement of urinary nucleosides by MEKC in combining with PCA technique may provide a clinically useful approach for diagnosis of cancer.