β沸石的铝化

β沸石自1988年结构被确定以来受到普遍重视,由干结构上的特殊性,G沸石既具有较强酸性又具有明显的碱性［‘,‘］．但q佛石的高硅铝比使其在化学组成上对碱性的贡献甚微,如果能降低其硅铝比,则有可能获得具有较强碱性的佛石分子筛．直接合成的o佛石,硅铝比一般在10以上．     

取代脂环烃物理化学性质的拓扑化学研究

为了探讨有机化合物的分子结构与理化性质的关系,作者在以前的工作基础上,基于一阶分子连通性拓扑指数构建了一个信息拓扑指数.将拓扑指数与取代脂环烃系列分子的气态标准生成热、气态标准熵、气态标准生成自由能、沸点、临界温度、临界压力、临界体积、汽化热、密度、热容及表面张力等十一种热力学性质及物理化学性质相关联,用一个通用公式对各类性质进行概括,然后用已有的实验数据与拓扑指数进行回归分析,得到一系列计算各性质的经验公式.回归结果发现,分子的理化性质与拓扑指数有较好的相关性,有5类性质的复相关系数大于0.99.用经验公式对各类性质进行重新计算,其结果与实验值比较符合,用实验值对计算值作图,发现各数据点紧靠对角线,说明误差较小.残差分布呈正态分布.     

甲基橙褪色动力学光度法测定槲皮素的研究

基于稀H2SO4介质中,槲皮素对KBrO3氧化甲基橙褪色反应的明显催化作用,建立了测定痕量槲皮素的动力学光度法。在选定的条件下,方法的线性范围为0~0.05 mg/L,表观摩尔吸光系数为4.52×106L.mol-1.cm-1,检出限为0.0012 mg/L。利用此法测定了银杏叶和中药制剂慢严舒柠中的槲皮素,加标回收率为95%~106.7%,相对标准偏差小于3.3%。     

N,C10-Überbrückte Morphinalkaloide, 5H-10,13-Iminoethano-phenanthro[4,5-bcd]furan, 2. Mitt.

Summary Following our concept of rather new structural variations in the nitrogen region of morphine alkaloids we describe the first synthesis of N/C-10-bridged tertiary bases.

     

Solid-state interactions and drug release of teicoplanin in binary combinations with peracetylated α-, β-, and γ-cyclodextrins

Triacetyl α-cyclodextrin, triacetyl β-cyclodextrin and triacetyl γ-cyclodextrin were tested as possible hydrophobic carriers to prolong the release of hydrophilic teicoplanin (TCP). Physical–chemical characterization of individual components, drug-carrier physical mixtures at 0.5, 0.67 and 0.75 mass fraction of carrier, and the respective interaction products by kneading or evaporative crystallization under microwave irradiation was carried out using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). In vitro drug release in pH 7.4 phosphate buffer at 37 °C was determined by intrinsic dissolution rate (IDR) measurements on non disintegrating compressed discs. Solid-state interactions of TCP with triacetyl α-cyclodextrin by evaporative crystallization and kneading and with triacetyl β-cyclodextrin by evaporative crystallization (probably resulting in carrier amorphization) were demonstrated. The role of carrier hydrophobicity, carrier mass fraction and preparation method of solid drug-carrier combinations on solid-state drug-carrier interactions and slowing down of TCP release was assessed. Modulation of drug release can be achieved using TCP-triacetyl γ-cyclodextrin combinations at 0.5 mass fraction of carrier.     

动力学分光光度法测定痕量硫氰酸根的研究

利用SCN~-对溴酸钾氧化罗丹明B反应的抑制作用。建立了动力学光度法测定痕量SCN~-的新方法。检出限为0.30ng SCN~-/ml,测定范围为0.30～8.3ngSCN~-/ml.应用于吸烟者与不吸烟者尿中SCN~-的测定。结果较为满意。     

痕量溴的阻抑动力学荧光法测定

基于在磷酸介质中溴对溴酸钾氧化丁基罗丹明B反应的抑制作用，建立了痕量溴的阻抑动力学荧光分析的新方法；应用单纯形最优化法确定了 实验条件，方法的检出限0.075μg/L，线性范围0.40-6.40μg/L；将该法应用于地下水、人发中溴的分析，获得满意结果，并对反应机理进行了初步探讨。     

Kinetic Spectrophotometric Determination of Trace Amounts of Nitrite by Catalytic Reaction between Methylthymol Blue and Bromate

A kinetic spectrophotometric method for determination of trace nitrite in two dynamic ranges (2–100 and 100–500 ng/mL) based on its catalytic effect on the reaction between methylthymol blue and potassium bromate in acidic (sulfuric acid) media is described. The reaction was monitored spectrophotometrically by measuring the decreasing color of methylthymol blue at 437 nm by the fixed‐time method of 4.0 min at 30°C. The detection limit is 0.6 ng/mL, and the relative standard deviations for 50.0 and 250.0 ng/mL nitrite are 1.6% and 1.3%, respectively. The method was used for the determination of nitrite in water samples.     

Chelatometric titration of tin in non-ferrous alloys with hedta

A new titrimetric method for determination of tin (4%) in aluminium alloys, tin- and lead-base alloys, solders, white bearing alloys, special bronzes and silver brazing alloys is proposed. HEDTA, Semi-Xylenol Orange and bismuth perchlorate are used as titrant, indicator and back-titrant respectively. Measures are taken to overcome the hydrolysis of Sn(IV). Monochloroacetic acid and ethylene glycol are added as auxiliary agents. The standard deviation of this method was found to be 0.2 mg and its coefficient of variation to vary from 0.25 to 2%, according to amount of tin. A novel method of sample decomposition and a modified method for separating Sn(IV) are also suggested.     

Synthesis on the basis of electrogenerated carbenes

A series ofS _N2 reactions with halomethanes as substrates and the corresponding anions as nucleophiles were studied by the semiempirical MNDO and AM1 methods, taking into account solvent effects. Analysis of the kinetics, structures of reagents, intermediates and products, and charge distribution in them allows one to draw the conclusion that the retardation ofS _N2 reactions is stronger in solvents than in the gas phase, and the rates of reactions involving anions with a lower number of halogen atoms are higher.For Part 8 see Ref. 1.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2148–2154, November, 1995.This work was partially financially supported by the International Science Foundation (Grant No. MHYOO).