Polyhydroxyquinoline-carbon nanotube chelating resin for selective adsorption of lead ions: multivariate optimization,isothermic, and thermodynamic study

In this work a facile hydrothermal route has been employed to prepare a multiwall carbon nanotube wrapped in a chelating resin. 8-Hydroxyquinoline and p-formaldehyde were used as monomer and linker for polymer synthesis. The prepared composite was employed as an efficient adsorbent for lead adsorption and preconcentration from various matrices. Effective parameters on lead adsorption have been optimized by central composite design. Results showed that equilibrium adsorption was obtained at pH = 4, with a shacking time of 15 min and adsorbent dosage of 15 mg. Isotherm study showed that the sorbent has adsorbent capacity of 250 mg g^?1; moreover, the process followed a Langmuir isotherm model. Thermodynamic investigation confirmed that lead adsorption is spontaneous, as well as follows endothermic path.     

Chemical transformations of tetracyclo[3.3.1.1<Superscript>3,7</Superscript>.0<Superscript>1,3</Superscript>]decane (1,3-dehydroadamantane): II. Reaction of 1,3-dehydroadamantane with <Emphasis Type="Italic">N,N</Emphasis>-dialkylcarboxamides

Alkylation of N,N-dialkylcarboxamides with 1,3-dehydroadamantane has been accomplished for the first time. The reaction involves the C–H bond in the α-position with respect to the carbonyl group and provides a convenient one-step preparation of substituted carboxylic acid amides containing an 1-adamantyl substituent and a pharmacophoric group in the amide moiety.     

A thermomechanical analysis of interfaces between the mating parts in ultrasonic wire bonding

Ultrasonic welding (USW) is an alternative solution for the bonding process especially in automotive industry. Ultrasonic welding of metals is a joining technique as a combination of applying pressure and frictional vibrations within the range of ultrasonic frequencies. In automotive industry, ultrasonic welding is often used for wired connections. As an alternative for crimping technology of multi-strand aluminum cables in wire bonding, ultrasonic welding is used. This work presents a thermomechanical analysis of the interface between two mating parts in USW. For this reason, the temperature distribution at bonding locations inside a wire bundle due to frictional vibrations and pressure is investigated using the finite element method (FEM). The obvious difference in microsections from different welding samples, which originates from different local temperature rises, was the motivation for this study to further investigate the thermomechanical aspects of the USW by use of finite element simulations. (© 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim)     

Fluid flow and heat transfer around circular cylinder – flat and curved plates combinations

Experimental studies were carried out to investigate the fluid flow and heat transfer around a heated circular cylinder which was placed at various distances of a wall boundary with different geometries (flat or curved plate) with subcritical Reynolds number ranging from 3.5×10³ to 10⁴. The effects of plate geometry (aspect ratio: W|H=1.0,1.5 and 2.0, and rim angle, φ=0°,60°,90°, and 120°) and gap ratio, (G|D=0.0,0.86,2.0,7.0,10.0) on the fluid flow and heat transfer characteristics (static pressure around cylinder surface, wake width, base pressure, pressure drag coefficients, velocity distribution, and both local and mean Nusselt numbers) were presented. Also flow visualization was carried out to illustrate the flow patterns around the cylinder at various gap ratios (G|D). It was found that the heat transfer and fluid flow characteristics are dependent on the plate geometry at all tested gap ratios, except for G|D=7.0 and 10.0, they are independent of the plate geometry.     

Preparation and characterization of nanocomposites in system as: SnO<Subscript>2</Subscript>–xTiO<Subscript>2</Subscript> (where <Emphasis Type="Italic">x</Emphasis> = 25, 50 and 75 mol%)

Nanocomposite samples containing various molar compositions of tin and titanium oxides were synthesized by a sol–gel method using octadecylamine as controlling template agent. The structural and the crystalline features of the samples were investigated with Fourier Transformer Infra-red, X-ray diffraction, Transmission electron microscope (TEM) where the surface area was estimated by BET analysis. The crystalline parameters and the particle size were estimated by Rietveld quantitative phase analysis. It is interesting to mention that a reduction in the lattice parameters was detected upon introduction of various molar compositions of titanium oxide revealing that a part of titania is incorporated into the SnO₂ lattice forming Ti_1−xSn_xO₂ solid solution. The quantitative analysis claims that part of titanium oxide is incorporated substitutionally in the crystal lattice of SnO₂, forming a solid solution and other parts are either segregated as separate rutile titania phase or dispersed as amorphous phase on the grain boundary of SnO₂. The results show a remarkable reduction in particle size from 42 to 5 nm and increasing in the specific surface area up to 176 m²/g upon introduction of various content of titania implying the role of titania particles in preventing SnO₂ crystallites from further growing up during the progress of calcination. TEM images show that pure tin oxide particles arranged in large aggregation in wormhole like structure, while the existence of titanium oxide are successfully creates spherical nanoparticles system organized in a definite structure. The optical absorbance spectra indicate a red shift and band gap narrowing upon introduction of titania which increase with increasing in titania contents.     

Synthesis and anticancer activity of some new s-glycosyl and s-alkyl 1,2,4-triazinone derivatives

A series of S-glycosyl and S-alkyl derivatives of 4-amino-3-mercapto-6-(2-(2-thienyl)vinyl)-1,2,4-triazin-5(4H)-one (1) were synthesized using different halo compounds such as preacetylated sugar bromide, 4-bromobutylacetate, 2-acetoxyethoxy-methyl bromide, 3-chloropropanol, 1,3-dichloro-2-propanol, epichlorohydrin, allyl bromide, propargyl bromide, phthalic and succinic acids in POCl3. The structures of the synthesized compounds have been deduced from their elemental analysis and spectral (IR, 1H-NMR, and 13C-NMR) data. Some of the synthesized compounds were screened as anticancer agents. Significant anticancer activities were observed in vitro for some members of the series, and compounds 4-Amino-3-(3-hydroxypropylthio)-6-(2-(2-thienyl)vinyl)-1,2,4-triazin-5(4H)-one (12) and 3-(4-Oxo-3-(2-(2-thienyl)vinyl)-4H-[1,3,4]thiadiazolo-[2,3-c][1,2,4]tr-iazin-7-yl)propanoic acid (18) are active cytotoxic agents against different cancer cell lines.     

Floating and sustained-release characteristics of effervescent tablets prepared with a mixed matrix of Eudragit L-100-55 and Eudragit E PO

The aim of this study was to evaluate the influence of Na-bicarbonate as an effervescent agent on the floating and sustained-release characteristics in 0.1 M HCl of tablets made of Eudragit E PO (EE) and/or Eudragit L-100-55 (EL) as matrix formers at different EE:EL weight ratios: 0:100, 25:75, 50:50, 75:25, and 100:0. The tablets were made by direct compression utilizing metronidazole as a model drug. Effervescent tablets with 50EE/50EL (w/w) showed the best floating and sustained drug release properties in the dissolution medium. The corresponding noneffervescent tablets were nonfloating and showed significantly faster drug release. Effervescent tablets with single polymers showed an immediate drug release pattern. These results were explained by Fourier-transform infrared spectroscopy and elemental analysis, which showed strong evidence of interpolyelectrolyte complexation between EE and EL when they were exposed to 0.1 M HCl as an effervescent hybrid matrix, but not as a noneffervescent hybrid matrix. The role of Na-bicarbonate in allowing EE-EL complexation during dissolution was explained as due to raising the pH around EL particles for sufficient polymer ionization and ionic-interaction with the ionized EE.     

Hydrazone-based ligands for micro-solid phase extraction-high performance liquid chromatographic determination of biogenic amines in orange juice

Eight hydrazone-based ligands were synthesized, trapped in a silica sol-gel matrix, and were subsequently used in the micro-solid phase extraction (μ-SPE) of biogenic amines (BAs). The BAs investigated were tryptamine, phenylethylamine, putrescine, histamine, tyramine and spermidine. Prior to the extraction, dansyl chloride was added to the samples which were heated to 70°C for 10 min. The samples were extracted with μ-SPE, after which analytes were desorbed using acetonitrile via ultrasonication. The extracts were analysed by high performance liquid chromatography (HPLC) with ultraviolet detection. Of the eight ligands investigated as sorbents, benzophenone 2,4-dinitrophenylhydrazone was found to be the most promising. The enhanced π-π interaction between the analytes and the ligand facilitated the adsorption process. Under the most suitable extraction conditions, the method demonstrated good linearity with correlation coefficient of more than 0.985 over a concentration range of 1-50 μg L(-1). Satisfactory repeatability with relative standard deviations of 7.43-11.30% (n=3) were obtained. Detection limits ranged from 3.8 to 31.3 ng L(-1). The μ-SPE method exhibited lower recoveries (71.5-87.4%) when compared to the solid phase extraction technique (79.7-95.0%), but enrichment factors of 94-460 were obtained. The proposed μ-SPE-HPLC method was applied to the determination of BAs in orange juice purchased from local supermarkets, with satisfactory results. The orange juices were characterized by the presence of relatively high levels of putrescine (range, 550-2210 μg L(-1)) but tryptamine and phenylethylamine were not detected in any of the tested samples.     

Syntheses, crystal structures, transport properties and first-principles electronic structure study of the (tTTF)2X (X=Br, I) low-dimensional antiferromagnets

An efficient synthetic procedure for the preparation of unsymmetrically substituted tetrathiafulvalene (TTF) donors has been used to obtain the trimethylene-tetrathiafulvalene (tTTF) donor with high purity. Good quality crystals of the two (tTTF)(2)X (X = Br, I) salts have been obtained by electrocrystallization. The two salts are isomorphous and contain tTTF layers which are built from (tTTF)(2) dimeric units. Both systems are low-dimensional antiferromagnets with the highest Ne?el temperatures for TTF based radical cation salts: ≈ 35 K (Br salt) and ≈43 K (I salt). The resistivity is found to substantially decrease with pressure although both salts still have activated conductivity at 25 kbar. First-principles Density Functional Theory (DFT) calculations have been used to investigate the relative strength of the three different types of magnetic interactions in the tTTF layers as well as the potential magnetic ground states. These calculations successfully predict the nature of the ground state and suggest a possible correlation between structural details and Ne?el temperatures for the bromine and iodine salts. Remarkably, the calculated antiferromagnetic ground state can be predicted from the nesting properties of the Fermi surface for the hypothetical Pauli paramagnetic metallic state.