高效液相色谱-质谱联用法测定饮料中的苯甲酸含量

建立了高效液相色谱-质谱联用法检测饮料中的苯甲酸.选用ZORBAX XDB-C18柱(50mm×2.1mm,3.5μm)为分析柱,流动相为乙腈-水,梯度洗脱,流速为200μL·min-1;质谱条件选用气动辅助电喷雾离子源(ESI),检测方式为负离子多离子反应检测(MRM);苯甲酸校准曲线线性范围为1-500μg/L;方...     

Heterogeneous partial oxidation catalysis on metal oxides

This review paper presents an overview of heterogeneous selective ammoxidation and oxidative dehydrogenation (ODH) of light alkanes, particularly of ethane. The conversion of ethane to ethene is in great demand in the domestic and worldwide chemical industry. The review has been voluntarily restricted to metal oxide-type catalysts, as it is devoted to the special issue honouring Edmond Payen and is based on 30 years of experience and discussions with pioneering scientists in the field. The main key factors, designated by Grasselli as the “7 pillars”, have been emphasised: isolation of active sites, M–O bond strength, crystalline structure, redox features, phase cooperation, multifunctionality and the nature of the surface oxygen species. The main features and physical and chemical properties of solid catalysts for selective oxidation compared to total oxidation have also been emphasised. Several case studies have been presented to illustrate the concept and importance of the key factors of catalyst preparation and activation and of the catalytic atmosphere. Based on such analysis and recent discoveries and process developments perspective views are also given.     

2-Aryl-3,4-dihydropyrans as building blocks for organic synthesis: ring-opening reactions with nucleophiles

An electrophilic ring-opening reaction of 2-aryl-3,4-dihydropyran with many nucleophiles, such as thiophenols, thiols, benzenesulfinic acid, resorcin, 2-methylfuran, benzamide and allyltrimethylsilane, was developed. In the presence of an appropriate catalyst, a product that contains not only a moiety of the nucleophile but also a fragment of 1,3-dicarbonyl compound was obtained.     

Inhibition Effect of Hydantoin Compounds on the Corrosion of Iron in Nitric and Sulfuric Acid Solutions

Summary.  The inhibition of corrosion of iron in 2 M nitric acid and 2 M sulfuric acid solutions by substituted phenylhydantoin, thiohydantoin, and dithiohydantoin compounds was measured using thermometric, weight loss, and polarization methods. The three methods gave consistent results. The polarization curves indicated that the hydantoin compounds act as mixed-type inhibitors. The adsorption of the inhibitors were found to obey the Temkin adsorption isotherm. The higher inhibition efficiency of the additives in nitric with respect to sulfuric acid solution may be attributed to the reduced formation of soluble quaternary nitrogen salts in nitric acid medium, favouring adsorption of the parent additive on the metal surface. The obtained results indicate that the corrosion rate of iron in both acids increases with increasing temperature, both in absence and presence of the tested inhibitors. Kinetic-thermodynamic model functions and Temkin isotherm data are compared and discussed. The synergistic effect of halide anions on the inhibition efficiency of the hydantoin compounds was also investigated. Received June 5, 2000. Accepted (revised) September 13, 2000     

Calcium Bis[bis(trimethylsilyl)amino‐triethylgallate] — A Molecule with Ca‐C‐Ga Three‐Center Bonds

The reaction of calcium‐bis[bis(trimethylsilyl)amide] with two equivalents triethylgallium yields nearly quantitatively the addition product. In the solid state the calcium atoms are coordinated by two nitrogen atoms and two ethyl groups, whereas in solution all ethyl substituents are magnetically equivalent even at low temperatures. The Ca‐C‐Ga two‐electron three‐center bonds show mean Ca‐N and Ca‐C distances of 243 and 268 pm, respectively.     

钒(Ⅴ)-7-碘-8-羟基喹啉-5-磺酸显色体系测定钢样中的钒

研究了7-碘-8-羟基喹啉-5-磺酸（H2QSI）在乙醇存在下分光光度法测定钡（Ⅴ）的最佳条件。在乙醇存在下pH4的硫酸介质中,（H2QSI）与V（Ⅴ）形成了红棕色配合物,最大吸收位于506nm处,表观摩尔吸光系数εmax＝2.9×103L·mol-1·cm-1,有色配合物组成为V（Ⅴ）:（H2QSI）＝1:3。钒（Ⅴ）在0-14μg／25mL符合比耳定律、本法用于钢样中的测定,结果满意。H2QSI是光度分析中的一种显色剂,近年来,8-羟基喹啉类试剂用于钒（Ⅴ）的测定已有报道[1]:,H2QSI曾见用于稀土元素的光度测定[2],但用于钒（Ⅴ）的测定尚未见报道。本文研究了V（Ⅴ）与H2QSI的显色反应条件及组成,在pH4的乙醇介质中,V（Ⅴ）与H2QSI生成红棕色配合物ε506nm＝2.9×103L·mol-1·cm-1。本方法用于低碳合金钢中钒的测定,结果满意。     

A new method for introduction w-side chain of prostanoid using Barton radical reaction

A new method for introduction w-side chain of prostanoid was described in this note. Starting from acid chloride (3), via Barton radical reaction, a trans α,β-unsaturated ketone sython was introduced.     

抗坏血酸基体改进剂平台石墨炉原子吸收光谱法测定蚝油中的铅

本实验建立了以抗坏血酸为基体改进剂测定蚝油中铅的方法。研究了多种基体改进剂消除蚝油基体对测铅的干扰，方法的相对标准偏差为４．９％，回收率为９４％－９６％，检出限为１．５ｎｇ／ｍＬ。本方法可用于蚝油、贻贝油等调味品中铅含量的测定。     

量化计算在二芳基二硫代膦酸结构和光谱分析中的应用

在拉曼和红外光谱分析中，谱峰的归属直接关系到对分子结构的判定。本工作以量子化学理论计算为基础，探索对二芳基二硫代磷酸实验拉曼谱图进行谱峰归属的可行性。结果表明：二芳基二硫代膦酸理论计算谱图与实验谱图具有相关性，理论计算谱图可以指导实验谱图谱峰的归属分析。