两相滴定法研究2-乙基己基膦酸单2-乙基己基酯从盐酸介质中萃取钕(Ⅲ)的动力学

本文利用两相滴定法作为分析手段,用恒界面池搅拌法考察了多种因素对2-乙基己基膦酸单2-乙基己基酯(HEHEHP,HA)从盐酸介质中萃取Nd(Ⅲ)动力学的影响,从实验结果推论出萃取过程为界面化学反应控制型机理。     

邻硝基对甲基苯胺的极谱研究

用单扫示波极谱法，在生理盐水底液中，２５℃时邻硝基对甲基苯胺于－０．８２±０．０１伏（ＳＣ）处有一良好的二阶导数还原峰，浓度为２×１０（－８）－１×１０（－５）ｍｏｌ／Ｌ时，与峰电流呈良好的线性关系，可作分析测定，检测限为１×１０－８ｍｏｌ／Ｌ。许多无机离子不干扰测定。此外，还证明其电极过程为吸附过程，ｎ＝４，提出了电极反应机理。     

Gas Phase Catalysis by Metal Nanoparticles in Nanoporous Alumina Membranes

Nanoporous alumina membranes, loaded with palladium and ruthenium nanoparticles of various size, were used for gas phase hydrogenation of 1, 3‐butadiene and for oxidation of carbon monoxide, respectively. Those membranes contain 10⁹ ‐ 10¹¹ pores per cm², all running perpendicular to the surface. Membrane discs of 20 mm in diameter and only 60 μm thick, incorporated in a reactor in which the reactants can be pumped in a closed circuit through the pores, turned out to very actively catalyze hydrogenation of butadiene (Pd) and oxidation of CO (Ru). The activity of the Pd catalysts depends characteristically on the particles size, the gas flow, and of the educts ratio. As could be expected, larger particles are less active than smaller ones, whereas increasing gas flows in case of hydrogenation accelerates the reactions. Excessive hydrogen reduces selectivity with respect to the various butenes, but favours formation of butane.     

高效液相色谱指纹图谱应用于地黄的研究

利用高效液相色谱建立了地黄的色谱指纹图谱。采用反相C1 8柱 (5 μm ,1 5 0mm× 4.6mm) ,流动相甲醇∶水 (V V =5∶95 ) ,检测波长为 2 80nm ,流速 1 .0mL min进行实验。根据相对保留值和相对面积值对色谱指纹图谱进行分析对比研究 ,建立了控制地黄药材质量的新方法。该法为中药样品的鉴定提供了较全面的信息 ,并为HPLC在复杂组分的样品分析领域开拓了新的应用途径。     

红四氮唑作为电化学嵌合剂的核酸杂交生物传感器

提出了一种以红四氮唑 (TTC)作为嵌合剂 ,采用石墨修饰电极监测核酸杂交过程和测定特定 DNA片段的灵敏的电化学方法 . TTC具有背景电流低 ,电活性强和对双链 DNA(ds DNA)选择性好等一系列优点 ,可在石墨电极表面形成 ds DNA-TTC层 .在电化学测定中 ,TTC的还原电流与靶 DNA浓度具有良好的线性关系 ,对 DNA的检测限可低达 6× 1 0 - 1 1 mol/L .     

Three tetrahydroisoquinolinedione derivatives

N‐(2‐Chloro­benzyl)‐1,2,3,4‐tetra­hydro­iso­quinoline‐1,3‐dione, C₁₆H₁₂ClNO₂, crystallizes in P2₁/n with three crystallographically independent mol­ecules in the asymmetric unit, which differ slightly in conformation, N‐(2‐bromo‐4‐methyl­phenyl)‐1,2,3,4‐tetra­hydro­iso­quinoline‐1,3‐dione, C₁₆H₁₂BrNO₂, crystallizes in P2₁/n with one mol­ecule in the asymmetric unit andN‐(2,3‐di­chloro­phenyl)‐1,2,3,4‐tetra­hydro­iso­quinoline‐1,3‐dione, C₁₅H₉Cl₂NO₂, crystallizes in P2₁/c with one mol­ecule in the asymmetric unit. In all three structures, the heterocyclic rings adopt approximately planar conformations. The pyridine rings are orthogonal to the substituted phenyl rings. In all three structures, the crystal packing is stabilized by intermolecular C—H?O hydrogen bonds.     

Cover Picture: Highly Regioselective Sequential 1,1‐Dihydrosilylation of Terminal Aliphatic Alkynes with Primary Silanes (Chin. J. Chem. 5/2019)

The cover picture shows that sequential 1,1‐dihydrosilylation of terminal aliphatic alkynes with primary silanes enabled by one earth‐abundant cobalt catalyst has been developed. This protocol is operationally simple using readily available aliphatic alkynes, including simple acetylene and complex drug derivative, for efficient access to valuable gem‐bis(dihydrosilyl)alkanes in highly regioselective and atom‐economic manners. Corresponding asymmetric transformations are achieved with excellent enantioselectivities. More details are discussed in the article by Lu et al. on page 457–461.

     

NCO自由基与SO_2、CS_2反应的速率常数

利用波长为266nm的激光光解CHBr3产生CH自由基,其与NO反应作为NCO自由基的来源.在298K,总压2660Pa的条件下,采用激光诱导荧光的方法,研究了NCO自由基与SO2、CS2的反应.得到了NCO自由基与SO2、CS2双分子反应速率常数分别为(1.8±0.3)×10-11和(3.1±0.4)×10-12cm3·molecule-1·s-1.对这两个反应在B3LYP/6-31 G(d)的水平上进行理论研究的结果表明,NCO自由基与SO2、CS2的反应是加成反应,其机理是NCO自由基中的N原子攻击反应物的中心原子,得到加成产物.     

钇提高YT14硬质合金耐磨性的机制

研究了不同Ｙ添加量对ＹＴ１４硬质合金显微组织、结构和耐磨性的影响。结果表明，在ＹＴ１４硬质合金中添加微量Ｙ，可显著提高合金的耐磨性。Ｙ的主要作用是均匀细化碳化物相和Ｃｏ相；提高Ｃｏ粘结相中Ｗ、Ｔｉ元素的固溶量及αＣｏ相所占的体积分数，从而提高Ｃｏ粘结相的强韧性；Ｙ在合金中形成Ｙ２ＷＯ６，表明Ｙ还可还原和清除碳化钨表面氧化膜，增强Ｃｏ粘结相与硬质相之间的结合强度     

Indirect Determination of Captopril with Sodium Nitrate and Thiocyanate by Floatation Separation of Copper

A new method for indirect determination of captopril (CPT) with NaNO₃ and NH₄SCN by floatation and separation of copper has been studied. In the weak acid, a small amount of Cu(II) can be reduced to Cu(I) by CPT, then Cu(I) reacted with the SCN, which can float on the surface of the liquid phase with NaNO₃. A good linear relationship is observed between the floatation yield (E%) of Cu(II) and the amount of captopril. The linear range is 2?32 mg/L. On the ground, captopril can be indirectly determined by determining E(%) of Cu(II). The method is simple, rapid, reliable and has good selectivity. The developed method can be applied to indirect determination of captopril with satisfactory results.