Thin layer chromatographic studies of anils II. Separation,identification and determination

Thin layer chromatographic behaviour of ten anils was studied on silica gel adsorbent mixed with starch binder with ten solvent systems. Simultaneous separation, identification and determination of ternary mixtures of isomers was stressed. TheR _F increasing order was found to be dependent on the solvent and independent of the degree of saturation of the chamber. The correlations ofR _F with _max and (C=O) of isomers were established and used in their identification. Six anils were separated in methanol—benzene (11).     

Single-phase and gram-scale routes toward nearly monodisperse Au and other noble metal nanocrystals

Single-phase approaches are introduced for the synthesis of nearly monodisperse Au and other noble metal nanocrystals. The new approaches possess all the advantages of the popular Brust method. With weak ligands or surfactants for the metal ions, the control of the size and size distribution of the nanocrystals in synthesis in the size range between 1 and 15 nm was achieved via maintaining balanced nucleation and growth by tuning the activities of the metal precursors and reducing reagents. Because only weak ligands are employed in the new synthetic schemes, surface modification and functionalization of the resulting nanocrystals can be readily carried out.     

Physically based molecular device model in a transient circuit simulator

Two efficient, physically based models for the real-time simulation of molecular device characteristics of single molecules are developed. These models assume that through-molecule tunnelling creates a steady-state Lorentzian distribution of excess electron density on the molecule and provides for smooth transitions for the electronic degrees of freedom between the tunnelling, molecular-excitation, and charge-hopping transport regimes. They are implemented in the fREEDA™ transient circuit simulator to allow for the full integration of nanoscopic molecular devices in standard packages that simulate entire devices including CMOS circuitry. Methods are presented to estimate the parameters used in the models via either direct experimental measurement or density-functional calculations. The models require 6–8 orders of magnitude less computer time than do full a priori simulations of the properties of molecular components. Consequently, molecular components can be efficiently implemented in circuit simulators. The molecular-component models are tested by comparison with experimental results reported for 1,4-benzenedithiol.     

Sensitive and selective ion exchange test for microgram detection and spectrophotometric determination of picric acid

The microgram detection and determination of picric acid with sodium hypochlorite solution is based on its oxidation in alkaline solution and chlorination with excess of chlorine present in hypochlorite solution. A characteristic orange color is obtained, which can be used as a specific test. The sensitivity of the picric acid was enhanced by performing the resin spot test. This color reaction was applied for the determination of picric acid spectrophotometrically.     

An investigation of the properties of poly(dimethylsiloxane)-bioinspired silica hybrids

Elastomers typically require the incorporation of reinforcing fillers in order to improve their mechanical properties. For commercial silicone systems silica and titania are typically used as fillers. Fumed and precipitated silica are made on an industrial scale for many applications; however, we have shown recently that biological and synthetic macromolecules can generate new silica structures using a bioinspired route. Herein we have incorporated bioinspired silica fillers into poly(dimethylsiloxane) (PDMS) elastomers and investigated their mechanical, morphological and thermal properties as a function of filler loading. The equilibrium stress-strain characteristics of the PDMS-bioinspired silica hybrids were determined as a function of bioinspired filler loading and the Mooney-Rivlin constants (2C₁ and 2C₂) were calculated. The thermal characteristics, in particular glass transition temperatures (T_g) and melting points (T_m), of the PDMS-bioinspired silica hybrids were characterized using differential scanning calorimetry (DSC). The thermal stability of these hybrid materials were investigated using thermogravimetric analysis (TGA). The morphology of the samples was characterized using scanning electron microscopy (SEM), and the filler dispersion was characterized using ultra small angle X-ray scattering (USAXS) and scanning electron microscopy (SEM). Although spherical silica particles were used here, we have demonstrated elsewhere that this bioinspired synthetic route also enables highly asymmetric silica structures to be prepared such as fibres and sheets. This methodology therefore offers the interesting possibility of preparing new hybrid systems where the properties are highly anisotropic.     

P(i-PrNCH2CH2)3N: An efficient nonionic catalyst for the regioselective Michael addition of a β,γ-unsaturated ester and a nitrile

Michael additions of a β,γ-unsaturated ester and a nitrile to a variety of α,β-unsaturated ketones can be effected with high regioselectivity and in good yields using P(i-PrNCH₂CH₂)₃N as a catalyst.     

Fourth-derivative spectrophotometric determination of fungicide ferbam (iron(III) dimethyldithiocarbamate) in a commercial sample and wheat grains using 2,2′-bipyridyl

A procedure has been developed for the direct fourth-derivative spectrophotometric determination of iron(III) dimethyldithiocarbamate by converting it into an iron(II) 2,2'-bipyridyl complex, which is then dissolved in Triton X-100. Beer's law is obeyed over the concentration range 0.5-20 microg mL(-1 )in the final solution. Various parameters such as the effect of pH and interference of large number of ions on the determination of ferbam have been studied in detail. The method is sensitive, highly selective and can be used for the determination of ferbam in a commercial sample and in mixtures with various dithiocarbamates (ziram, zineb, maneb, etc.) and from wheat grains.     

Remarkably mild and efficient catalytic Sakurai reaction of N-alkoxycarbonylamino sulfones with allyltrimethylsilane using indium(III) chloride

The Sakurai reaction of N-alkoxycarbonylamino sulfones with allyltrimethylsilane in the presence of a catalytic amount of indium(III) chloride at room temperature produces the corresponding protected homoallylic amines in high yields.     

Preparation and reactions of triphenylarsoranylideneketene

Preparation and some reactions of the first cumulated ylide of arsenic, viz. triphenylarsoranylideneketene are described.     

Dispersing nanotubes with surfactants: a microscopic statistical mechanical analysis

A first theoretical study of surfactant-stabilized carbon nanotube dispersions is presented. Density functional theory is used to compute potential of mean force between nanotubes in an aqueous solution of cationic surfactant n-decyltrimethylammonium chloride. In agreement with experimental results, it is found that stable dispersions can be prepared for surfactant bulk concentrations below the critical micelle concentration. Computed density profiles of head and tail segments indicate that surfactants adsorb on nanotube surfaces in a random fashion rather than form cylindrical micelles, which is also in agreement with recent small-angle neutron scattering measurements.