Selective hydroaminomethylation of olefins using simple and efficient Rh–phosphinite complex catalyst

Hydroaminomethylation of various olefins with primary and secondary amines was carried out using a simple and efficient rhodium–phosphinite complex catalyst. The influence of various reaction parameters including the effects of temperature, pressure, catalyst loading, time and solvents has been investigated. The present protocol is general with wider substrate applicability for the synthesis of an important class of aliphatic amines and arylethylamines. High activity and selectivity for amines was achieved with a very good substrate/catalyst molar ratio (turnover number 2500) under mild reaction conditions. Copyright © 2013 John Wiley & Sons, Ltd.     

Novel Protonic Conductive Silicates Produced by the Sol-Gel Method

ABSTRACT

Materials which display ionic conductivity were produced by the sol-gel and microemulsion-gel methods. The charging and discharging characteristics were investigated and it was found that a single ionic species was responsible for the conduction, the ionic species being residual protons from the initial component mixture. The complex impedence of various samples was measured and the ionic conductivities ranged in value from 9 × 10^?8 to 1 × 10^?5 ohm^?1 cm^?1. An Arrhemius plot for a microemulsion-gel revealed that the energy of activation was 0.15 eV.     

Aktivierungsanalytische Bestimmung von Spurenelementen in Tomaten

Die Autoren machen mit aktivierungsanalytischen Untersuchungen am Reaktor der Technischen Universität Budapest bekannt. Der thermische Neutronenfluβ war 2·10¹¹ ncm^?28^?1, und es wurde ein Ge(Li)-Detektor mit 25 cm³ Volumen und einer Energieauflösung von 2 keV angewendet. Die untersuchten Tomatenproben enthielten durchschnittlich 85% Trockensubstanz. Es wurden folgende Konzentrationen an Spurenelementen ermittelt (in mg/kg): Br: 50,1; Mn: 10,2; Zn: 9,3; Cu: 6,6; As: 0,051; Sb:0,030; Au: 0,005.     

Eine einfache Mehrprobenrotationsanordnung zur Aktivierungsanalyse am Neutronengenerator

Es wird eine Anordnung beschrieben, die es gestattet, bis zu 7 Proben unter identischen Bedingungen rotationssymmetrisch zu aktivieren. Die Proben rotieren um zwei parallele Achsen. Es wird über Erprobungsmessungen durch Aktivierung von Cu-und N-haltigen Proben berichtet.     

Unique ion beam scattering technique on depth profile determination

Abstract

By combination of energy and time of flight detection in ERDA or NRA measurement, the particles' masses can be determined, additionally to the depth information. This leads to unique depth profile determination even for complex targets. Combination with th concept of Jacobi transformations results in extremely fast measurements. In this paper, a way is shown how this concept can be realized even for accelerators ofenergies as low as about 1 MeV.     

CuNaY分子筛的制备及其催化甲醇氧化羰基化

采用多种铜盐溶液与NaY分子筛离子交换制备了CuNaY催化剂,通过加入氨水提高溶液pH值以及高温活化,显著提高了该催化剂对甲醇氧化羰基化合成碳酸二甲酯的反应活性。不同的铜盐水溶液交换制备的CuNaY催化剂催化活性不同,添加氨水将溶液pH值调节为11后,离子交换制备的CuNaY催化剂的催化活性和DMC选择性明显升高且趋于一致。经元素分析、XRD、XPS和H₂-TPR表征可知,加入氨水可促进Cu²⁺离子交换的进行,提高CuNaY催化剂中Cu的交换量,催化剂中约75%的Cu²⁺定位于分子筛的超笼中。     

一个吡啶二甲酸镉配位聚合物的合成、晶体结构及荧光性质

通过水热方法,采用H3CAM(H3CAM=4-hydroxy-pyridine-2,6-dicarboxylic acid)与Cd(NO3)2.4H2O反应,合成了1个镉配位聚合物[Cd4(HCAM)4(H2O)8]n(1),并对其结构和荧光性质进行了研究。结构分析结果表明该配合物属于单斜晶系,C2/c空间群。四个HCAM2-配体桥联4个镉离子形成了1个四核镉单元。这些孤立的单元通过氢键作用形成了1个三维配位框架。研究表明,该配合物在室温下能发出兰色荧光。     

Binuclear ruthenium(II) pyridazine complex catalyzed transfer hydrogenation of ketones

A convenient and general method of synthesis of binuclear ruthenium(II) pyridazine complex was reported. The synthesized complex was characterized by analytical and spectral methods. The structure of the complex was confirmed by X-ray diffraction technique and was found to be an efficient catalyst for the transfer hydrogenation of ketones with excellent conversions in the presence of isopropanol/KOH at 82 °C. The effect of solvents, bases, and different catalyst/substrate ratio for the reaction was also investigated.     

The Determination of the Titre of Ascorbic Acid Standard Solutions

Abstract

A new method for the determination of the titre of ascorbic acid standard solutions employing potassium dichromate as a primary standard has been developed. In a pyrophosphate medium, the pyrophosphate complex of divalent manganese is oxidized by dichromate to the pyrophosphate complex of tervalent manganese; the latter oxidizes o-tolidine reversibly with formation of the corresponding quinonediimine, which is visually titrated by the ascorbic acid standard solution.