Fabrication of Nano Flower‐shaped Platinum on Glassy Carbon Electrode as a Sensitive Sensor for Lead Electrochemical Analysis

Platinum nanoflowers modified glassy carbon electrodes (PtNFs/GCE) was fabricated simply for lead determination in water samples. The modified electrodes were prepared by electrodeposition in hexachloroplatinic acid solution at constant potential. The influence of deposition time and potential on surface morphology, chemical composition, electrochemical properties of electrode were investigated. At ?0.2 V of potential and 150 s of deposition duration, platinum developed as nanoflower shape and scattered densely all over the glassy carbon surface, producing the largest electrochemically active surface areas. The highest differential pulse stripping voltammetry (DPSV) signal of lead was obtained by using the prepared electrode. Under optimized experimental condition of electrolyte, accumulation potential and time, the peak current was found to be linear proportion to lead concentration in range of 1 to 100 μg L^?1 (slope=0.371) with a limit of detection of 0.398 μg L^?1. The method has good repeatability and reproducibility with relative standard deviations of 1.47 % and 4.83 %, respectively. The modified PtNFs/GCE also demonstrated an excellent long‐term stability with only 9 % decrease in Pb peak current over 30 days. Moreover, the performance of the modified PtNFs/GCE in determination of Pb(II) in two industrial wastewaters was good agreement with data obtained by a graphite furnace atomic absorption spectrometry (GFAAS) method.     

Site‐specific reversible immobilization and purification of His‐tagged protein on poly(2‐acetamidoacrylic acid) hydrogel beads

Ni²⁺‐complexed poly(2‐acetamidoacrylic acid) (PAAA) hydrogel beads were developed for the site‐specific reversible immobilization and purification of the histidine‐tagged green fluorescent protein (His‐tagged GFP). PAAA hydrogel beads were prepared by photopolymerization, and significantly improved mechanical properties of PAAA hydrogel beads were observed in comparison with PAAA hydrogel from our previous study. Confocal laser scanning microscopy was used to determine the binding of His‐tagged GFP to the hydrogel beads in three‐dimensional space. Photoluminescence spectroscopy revealed 89% of binding efficiency of His‐tagged GFP to the Ni²⁺‐PAAA hydrogel beads, 51% of yielding recovery. The maximum binding capacity of His‐tagged GFP was estimated to be 0.45 µg/mg of Ni²⁺‐PAAA hydrogel beads. The recombinant His‐tagged GFP from the soluble fraction of E. coli BL21(DE3) cell lysates was purified with Ni²⁺‐PAAA hydrogel beads. The major advantage of the Ni²⁺‐PAAA hydrogel beads system was simple preparation procedures of producing the matrix, because PAAA hydrogel beads had relatively enhanced mechanical strength than soft hydrogels. Copyright © 2012 John Wiley & Sons, Ltd.     

Stereocontrolled Iodolactonization of Acyclic Olefinic Amides

Acyclic olefinic amides were iodolactonized in the mixed solvent of CH₃CN and H₂O (90:10₂ v/v) under reflux to give products with trans configuration of the newly formed iodomethyl to the inherent alkyl group in high yield.     

Direct Oxidation of N‐Benzylamides to Aldehydes or Ketones by N‐Bromosuccinimide

A simple and efficient approach for the one‐pot transformation of N‐benzylamides to aldehydes or ketones under mild conditions was reported. All the 20 substrates gave moderate to excellent oxidative yields under the optimized conditions. Our study may provide a new approach for the one‐pot synthesis of aldehydes or ketones from the corresponding amides.     

Heterocyclic benzothiazole-based liquid crystals: synthesis and mesomorphic properties

Two homologous series of 2-(4-alkanoyloxybenzylidenamino)benzothiazoles and 2-(2-hydroxy-4-alkanoyloxybenzylidenamino)benzothiazoles were synthesised and characterised. Their molecular structures differed wherein the latter comprised a lateral hydroxyl group, unlike the former. Spectroscopic techniques such as FT-IR, ¹H & ¹³C NMR and mass spectrometry together with elemental analysis were employed to elucidate the molecular structures. The transition temperatures and their mesophases were determined by differential scanning calorimetry, optical polarising microscopy and X-ray diffraction techniques. Members with decanoyloxy till hexadecanoloxy chain in the series without the lateral hydroxyl group each exhibited a smectic A phase, while those in the series with the lateral hydroxyl group were non-mesogenic. The mesomorphic properties of the present series were compared with other structurally related series to establish the chemical structure–mesomorphic properties relationship.     

Optical properties of a mesogen by image analysis

An image analysis technique in conjunction with polarising optical microscopy (POM) is proposed for assessment of the thermo-optical properties of homogeneously aligned chiral ester liquid crystals of the type ((S)-(-)-2-methylbutyl 4′-(4″-n-alkanoyloxybenzoyloxy) biphenyl-4-carboxylates, where n?=?16 or 18. Chiral ester textures are recorded as a function of temperature using POM provided with a hot-stage and a high-resolution colour camera. Temperature-dependent optical parameters, or thermo-optical properties such as optical transmission, degree of polarisation, absorption coefficient and birefringence are computed for chiral esters by analysing the texture of samples using MATLAB software. This is a simple experimental technique for observing how the optical parameters of liquid crystals change with temperature.     

Reaction of 2-Methylsulfonyl-4H-4-chromenones with Nucleophiles

For the synthesis of 2-substituted 4H-4-chromenones, 2-methylsulfonyl-4H-4-chromenones as common intermediate were reacted with nucleophiles such as amines and thiophenol to afford the corresponding 2-substituted adducts in very high yields.     

In situ Fe K-edge X-ray absorption fine structure of a nitrosyl adduct of iron phthalocyanine irreversibly adsorbed on a high area carbon electrode in an acidic electrolyte

Key aspects of the microenvironment surrounding the Fe center in the nitrosyl adduct of iron phthalocyanine, [Fe(Pc)(NO)], have been elucidated from the analysis of the Fe K-edge extended X-ray absorption fine structure (EXAFS) of the material adsorbed on the surface of a high area carbon electrode recorded in situ, in 0.5 M H(2)SO(4). Statistical best fits to the EXAFS data place the Fe center in a five-coordinated square pyramidal configuration shifted away from the Pc plane toward the axially bound NO bent at an angle of ca. 40 degrees with respect to the normal to the Pc plane. This environment is analogous to that of Fe in the nitrosyl adduct of crystalline [Fe(TPP)], where TPP = meso-tetraphenylporphyrinato(2-), determined from X-ray diffraction.