Electrochemical Derivatization of Acetaminophen for Indirect Determination of Eflornithine Using β‐CD Modified Glassy Carbon Electrode

In the present work, the oxidation of acetaminophen in the absence and presence of eflornithine was electrochemically investigated by means of cyclic voltammetry at a glassy carbon electrode (GCE). Our results indicate that N‐acetyl‐p‐benzoquinone imine (NAPQI) produced from two‐electron electrochemical oxidation of acetaminophen participates in a Michael addition reaction with eflornithine via an ECE mechanism. This fact was used for the determination of eflornithine using differential pulse voltammetry (DPV) technique on the surface of β‐Cyclodextrin modified glassy carbon (β‐CD/GC) electrode. β‐CD/GC electrode was prepared through an electrodeposition procedure and characterized by Fourier‐transform infrared spectroscopy (FT‐IR), Cyclic Voltammetry (CV), Field Emission Scanning Electron Microscopy (FESEM) and Energy‐dispersive X‐ray spectroscopy (EDS) techniques. Under optimum conditions, the β‐CD/GC electrode showed a good linearity as a function of the eflornithine concentration over the range from 5 to 100 μM with detection limit and quantification limit of 1.94 and 5.8 μM, respectively. Finally, the proposed protocol was confirmed to be successful in determination of eflornithine in human urine samples with good recovery, ranging from 97.2 % to 104.8 %.     

Comprehensive DFT calculations on organic sulfuric acid derivatives to design of powerful neutral organic superacids

In order to examine the acidity of organic sulfuric acid derivatives in gas phase, comprehensive density functional theory (DFT) calculations at B3LYP/6-31++G(d,p) level have been undertaken. In the title compounds, one of the oxygen atoms is substituted by an 1,3-cyclopentadiene group. The focus of this paper is on DFT studies of two classes of sulfuric acid derivatives: dithionic and peroxydisulfuric acids. Tautomers of proposed organic sulfuric acids are also investigated. DFT calculations indicate that the acidity of the proposed acids without any electron withdrawing groups on the ring was more than sulfuric acid.

     

Electrospun EGNPs reinforced precursor carbon nanofibril composites by using RSM

Response surface methodology (RSM),based on five‐level, four variable Box‐Benkhen technique was investigated for modeling the average fiber diameter of electrospun polyacrylonitrile (PAN) nanofibers. The four important electrospinning parameters were studied including applied voltage (kV), Berry's number, deposition distance from nozzle to collector (cm), and spinning angle (? in degree). The measured fiber diameters were in a good agreement with the predicted results by using RSM technique. High‐regression coefficient between the variables and the response (R² = 87.74%) indicates excellent evaluation of experimental data by second‐order polynomial regression model. The optimum PAN average fiber diameters of 208 and 37‐nm standard deviation were collected at 19 kV, Berry's number = 10, 25^° spinning angle, and 16‐cm deposition distance. The PAN/N,N‐dimethylformamide (DMF) polymer solution with the optimum weight concentration (10 wt.%) was selected to study the effect of dispersing exfoliated graphite nanoplatelets (EGNPs) in PAN/DMF solution on the electrospun EGNP/PAN fibril composite diameter. Five different EGNPs weight concentrations (2, 4, 6, 8, and 10 wt.%) were dispersed in the optimized PAN/DMF polymer solution. Morphology of EGNPs/PAN fibril composites and its distribution were investigated by scanning electron microscopy (SEM) to show the minimum fiber diameter for the above‐mentioned 5 wt. % of EGNPs. A minimum fibril composite diameter of 182 nm was obtained at 10 wt.% of EGNPs. Morphological characteristics of electrospun fibers and their distribution were tested by Raman spectroscopy, SEM, differential light scattering, and high‐resolution transmission electron microscopy.     

A cost-effective form-stable PCM composite with modified paraffin and expanded perlite for thermal energy storage in concrete

Journal of Thermal Analysis and Calorimetry - High thermal conductivity in phase change materials (PCM) is preferred in thermal energy storage (TES) systems. Carbon additives are considered as...     

Isolation and antiproliferative activity of triterpenoids and fatty acids from the leaves and stem of Turraea vogelii Hook. f. ex benth

Chloroform extract from the leaves of Turraea vogelii Hook f. ex Benth demonstrated cytotoxic activity against a chronic myelogenous leukemia cell, K-562 with IC₅₀ of 14.27 μg/mL, while chloroform, ethyl acetate and methanol extracts from the stem of the plant inhibited K-562 cells growth with IC₅₀ of 19.50, 24.10 and 85.40 μg/mL respectively. Bioactive chloroform extract of Turraea vogelii leaves affords two triterpenoids: oleana-12,15,20-trien-3β-ol (1), and oleana-11,13-dien-3β,16α,28-triol (2), with six fatty esters, ethyl hexaeicos-5-enoate (3), 3-hydroxy-1,2,3-propanetriyltris(tetadecanoate) (4), 1,2,3-propanetriyl(7Z,7′Z,7′′Z)tris(-7-hexadecenoate) (5), 1,2,3-propanetriyl(5Z,5′Z,5′′Z)tris(-5-hexadecenoate) (6), 1,2,3-propanetriyltris(octadecanoate) (7), and 2β-hydroxymethyl tetraeicosanoate (8). Tetradecane (9), four fatty acids: hexadecanoic acid (10), tetradecanoic acid (11), (Z)-9-eicosenoic acid (12), and ethyl tetradec-7-enoate (13) were isolated from chloroform extract of Turraea vogelii stem. 1,2,3-propanetriyltris(heptadecanoate) (14), (Z)-9-octadecenoic acid (15) and (Z)-7-tetradecenoic acid (16) were isolated from ethyl acetate extract while (Z)-5-pentadecenoic acid (17) was obtained from methanol extract of the plant stem. Compounds 1, 2, 5, 6, 11, 12, 15, 16 and 17 exhibited pronounced antiproliferative activity against K-562 cell lines.     

Laser surface alloying of an electroless Ni–P coating with Al-356 substrate

Laser surface alloying of an electroless plating Ni–P coatings on an Al-356 aluminium alloy was carried out using a 1-kW pulsed Nd:YAG laser. The microstructure, chemical composition and phase identification of the alloyed layer were determined using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffractometry (XRD), respectively. It was shown that laser surface treatment produced a relatively smooth, crack-free and hard surface layer. The hardness of the surface significantly increased due to the formation of the uniformly distributed fine Ni–Al intermetallic phases. The corrosion behaviour of the surface alloyed specimens in 3.5% NaCl solution at 23 °C was also determined by electrochemical techniques. The laser-alloyed surface showed an improved corrosion and pitting potential compared to the substrate as well as the plated Ni–P coating.     

Capillarylike fluctuations at the interface of falling granular jets

We study the interface fluctuations of a granular jet falling under gravity and show that for small scales they are the analog of the thermally induced capillary waves. Experimental results from radial height and velocity fluctuations, static correlation functions and capillary ripple velocities allow us to estimate a granular surface tension. The ultralow interfacial tensions measured (of the order of 100 microN/m) can be rationalized using a simple model.     

Impact of laser produced X-rays on the surface of gold

In the paper an attempt has been made to use the laser-induced plasma as an X-ray source for the growth of nanostructures on the surface of gold. For this purpose, an Nd:YAG laser operated at second harmonics (λ = 532 nm, E = 400 mJ) is used to produce plasma from analytical grade 5N pure Al, Cu and W targets. An analytical grade (5N pure) gold substrate was irradiated by X-rays generated from Al, Cu and W plasma under the vacuum ∼10⁻⁴ Torr. The surface was analyzed by two techniques, XRD and AFM. The aberrations in the XRD peaks show that there are significant structural changes in the exposed gold, in terms of decreased reflection intensities, increased dislocation line density, changes in the d-spacing and disturbance in the periodicity of the planes. AFM used to explore the topography of the irradiated gold reveals that regardless of the source, nm sized hillocks have been produced on the gold surface. The roughness of the surface has increased due to the growth of these hillocks.     

Versatile vacuum chamber for in situ surface X‐ray scattering studies

A compact portable vacuum‐compatible chamber designed for surface X‐ray scattering measurements on beamline ID01 of the European Synchrotron Radiation Facility, Grenoble, is described. The chamber is versatile and can be used for in situ investigation of various systems, such as surfaces, nanostructures, thin films etc., using a variety of X‐ray‐based techniques such as reflectivity, grazing‐incidence small‐angle scattering and diffraction. It has been conceived for the study of morphology and structure of semiconductor surfaces during ion beam erosion, but it is also used for the study of surface oxidation or thin film growth under ultra‐high‐vacuum conditions. Coherent X‐ray beam experiments are also possible. The chamber is described in detail, and examples of its use are given.     

An efficient one‐pot procedure for the preparation of 1,3,4‐thiadiazoles in ionic liquid [bmim]BF4 as dual solvent and catalyst

The one‐pot three component condensation of hydrazine hydrate with substituted phenylisothiocyanates followed by the addition of substituted benzaldehydes in the presence of ionic liquid 1‐butyl‐3‐methylimidazolium tetrafluoroborate ([bmim]BF₄) and in the absence of any other catalyst under mild condition afforded 1,3,4‐thiadiazoles in excellent yields. The reaction workup is simple, and the ionic liquid was easily recovered from the reaction and reused. © 2008 Wiley Periodicals, Inc. Heteroatom Chem 19:320–324, 2008; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20432