Fabrication of NiO coated SiO2 and SiO2 coated NiO for the removal of Pb2＋ ions

We have prepared silica,SiO2coated NiO and NiO coated SiO2by sol-gel method.The physicochemical properties of the desired materials were investigated by surface charge properties,scanning electron microscopy（SEM）,energy dispersive X-ray（EDX） spectroscopy,surface area measurements and X-ray diffraction（XRD） analyses.The point of zero charge（PZC） of the solid was determined by the salt addition method.In coated materials,two PZC values were noted representing the surface charge of their counterparts.The SEM image of SiO2coated NiO displays a uniform coating of silica on the surface of NiO whereas in case of NiO coated SiO2,a honeycomb like appearance was observed with highly porous structures.In the diffractograms of NiO,the characteristic peaks were suppressed in NiO coated silica however,no diffraction peak could be seen in SiO2coated NiO.Batch adsorption technique was applied for the removal of Pb2＋ions from aqueous solution.The sorption trend for Pb2＋ions was observed in the order of NiO coated SiO2〉 SiO2coated NiO 〉 NiO 〉 SiO2.This trend confirms that the coated materials have more sorption capacities than their parent counterparts.     

One‐Pot Synthesis of Sulfonamides and Sulfonyl Azides from Thiols using Chloramine‐T

A convenient synthesis of sulfonamides and sulfonyl azides from thiols is described. In situ preparation of sulfonyl chlorides from thiols was accomplished by oxidation with chloramine‐T (=N‐chlorotosylamide=N‐chloro‐4‐methylbenzenesulfonamide), tetrabutylammonium chloride (Bu₄NCl), and H₂O. The sulfonyl chlorides were then further allowed to react with excess amine or NaN₃ in the same pot.     

Synthesis of α-Functionalized Allenes

It is known, since the work of Landor et al, that α-allenic alcohols can be specifically obtained by treating the monotetrahydropyranyl ether of a butyn-1,4-diol with lithium aluminium hydride (1). In this reaction, which can be also realized with another leaving group (halogen, ammonium) (2), the allenic linkage is formed by an S_N ^2′ process where the nucleophilic hydride is transferred from the initially formed alcoholate (scheme 1).     

Cobalt(I)-catalyzed cocyclotrimerization of acetylene with 2,6-dicyanopyridines

A procedure of general application to the synthesis of alkyl-substituted 2-cyano-6-(2-pyridyl)pyridines from alkylpyridines is outlined.     

NMR and INDO study of the Ni(II) complexes of maleic and succinic acids

A new approach to investigate the conformational properties of the Ni(II) complexes of maleic and succinic acids is reported. The use of C-13 and H-1 paramagnetic shifts and relaxation rates together with an INDO analysis on suitable radical models of the ligands proved a powerful tool in elucidating the conformation of the Ni(II) complex with the partially rigid maleic acid.     

The conductance of cyclic polyether-cation complexes

Precise conductance measurements are reported for sodium, potassium, and cesium salts in methanol and acetonitrile solutions containing cyclic polyethers dibenzo-18-crown-6 and dicyclohexyl-18-crown-6. Decreases in equivalent conductance caused by the addition of a cyclic polyether to solutions of constant ionic strength were analyzed by nonlinear least squares to give association constants and equivalent conductances of the cation-polyether complex. The selectivity observed for the complexing is a function not only of ionic size but also of solvent.     

C-13 magnetic relaxation rates and H-1 and C-13 paramagnetic shifts of Ni(II) complex of dopamine

The ¹H and ¹³C isotropic contact shifts and the ¹³C relaxation times of dopamine in aqueous solution have been measured in the presence of the Ni(II) ion. The pD dependence of the ¹H and ¹³C paramagnetic shifts was also investigated. From the analysis of the shifts at pD = 6.5 and from the INDO MO calculations on selected models of dopamine radicals, a dominant σ delocalization mechanism of the spin density is proposed. From the spin distribution on the ligand carbon atoms, the metal centered as well as the ligand centered dipolar contributions of the modified Solomon—Bloembergen equation were calculated and an estimate of the correlation time τ_c was given.     

Modification of the Electrode Surface by Ag Nanoparticles Decorated Nano Diamond‐graphite for Voltammetric Determination of Ceftizoxime

A modified glassy carbon electrode with a film of nano diamond? graphite nano mixture decorated with Ag nanoparticles (AgNPs? NDG/GCE) was constructed and used for sensitive voltammetric determination of ceftizoxime (CFX). Morphology of AgNPs? NDG/GCE has been examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Experimental variables such as deposited amount of the modifier suspension, pH of the supporting electrolyte and accumulation potential and time were optimized by monitoring of CV and LSV responses of CFX. The results illustrate that AgNPs? NDG/GCE exhibits an excellent electrocatalytic effect in the electro‐oxidation of CFX that leads to a considerable improvement in the corresponding anodic peak current. This also allows the development of a highly sensitive voltammetric sensor for the determination of CFX in pharmaceutical and clinical samples. Under the optimum conditions, the modified electrode showed a linear response to the concentration of CFX in the range of 0.02–7 µM with detection limit of 6 nM. The prepared modified electrode has some remarkable electrochemical properties such as simple preparation, high sensitivity, excellent repeatability and reproducibility and long‐term stability.