Efficient synthesis of mono- and disubstituted 2,3-dihydroquinazolin-4(1H)-ones using KAl(SO4)2·12H2O as a reusable catalyst in water and ethanol

KAl(SO₄)₂·12H₂O was found to catalyze efficiently a one-pot three-component cyclocondensation of isatoic anhydride and primary amines or ammonia sources such as (NH₄)₂CO₃, NH₄OAc and NH₄Cl with aromatic aldehydes under mild conditions to afford the corresponding mono- and disubstituted 2,3-dihydroquinazolin-4(1H)-ones in good yields.     

Thermal modified Kaolinite as useful material for separation and preconcentration of trace amounts of manganese ions

This work assesses for the first time the potential of natural Kaolinite as adsorptive material for preconcentration of metal traces. Manganese is quantitatively retained by 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) on thermal modified Kaolinite by column method in pH range of 8.5-10.0 at flow rate of 2 ml min⁻¹. Manganese was removed from column with 5.0 ml of H₂SO₄ 4 mol l⁻¹ and determined by flame atomic absorption spectrometric at 279.5 nm. In this case, 0.l μg of manganese can be concentrated from 800 ml of aqueous sample (where concentration is as low as 0.125 μg l⁻¹). Detection limit is 4.3 μg l⁻¹ (3 δ_bl m⁻¹) and analytical curve is linear in the 0.02-10 mg l⁻¹ in final solution with correlation coefficient 0.9997 and relative standard deviation for eight replicate determination of 5 μg of manganese in final solution is 0.71%. The interference of a large number of anions and cations has been studied in detail to optimize the conditions and method was successfully applied for determination of manganese in complex materials.     

Pyrrole-based conductive polymer as the solid-phase extraction medium for the preconcentration of environmental pollutants in water samples followed by gas chromatography with flame ionization and mass spectrometry detection

A pyrrole-based polymer was synthesized and applied as a new sorbent for solid-phase extraction (SPE) of some environmental pollutants from water samples. Polypyrrole (PPy) was synthesized by chemical oxidation of the monomer in nonaqueous solution. SPE of selected phenols, pesticides, and polyaromatic hydrocarbons (PAHs) from aqueous samples were performed using 200 mg PPy. The determination was subsequently carried out by gas chromatography-flame ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC-MS). The polymer showed much higher recoveries for aromatic compounds than aliphatics. Preconcentration of sample volumes up 11 led to acceptable recoveries for aromatic and other tested polar compounds. The R.S.D. for a river water sample spiked with phenols, pesticides and PAHs at sub-ppb level was lower than 10% (n = 3) and limits of detection for these compounds were between 15 and 120 ng l(-1).     

Quasicontinuum multiscale modeling of the effect of rough surface on nanoindentation behavior

Roughness of surface has as an important influence on identifying the mechanical behavior and performance of crystalline metals. In this study, nanoindentation simulations are conducted by the two dimensional quasicontinuum method to determine the load–penetration response and the critical load associated with the onset of plasticity in rough surfaces of a face-centered cubic single crystal copper. The arithmetic roughness index, ranging between 2 and 13 Å, is used to specify the roughness of surface. Results of indentation with different roughnesses are in good agreement with previous studies for the indenter size of 10–140 Å. The resultant load–penetration scattering, which stems from the roughness, indicates different dislocation nucleation steps, different subsequent dislocations intervals and varying stiffness values of samples. It can be concluded that the surface roughness has a significant effect on the first dislocation emission because of the indenter position and surface interactions beneath it. Moreover, the critical penetration depth for the first dislocation emission increases by the increase of the contact area between the indenter and surface.

     

Some new Schiff base ligands giving a NNOS coordination sphere and their nickel(II) complexes: Synthesis,characterization and complex formation

Some new tetradentate ligands with a NNOS coordination sphere were prepared and their corresponding nickel(II) complexes were synthesized and characterized by elemental analysis, IR, ¹H NMR, UV–Vis and mass spectrophotometry. The thermodynamic formation constants of the complexes were measured spectrophotometrically, at a constant ionic strength of 0.1 M (NaClO₄) at 25 °C in DMF solvent. The trend of the complex formation for nickel is as follows:     

Cubic spline solution of singularly perturbed boundary value problems with significant first derivatives

We develop a numerical technique for a class of singularly perturbed two-point singular boundary value problems on an uniform mesh using polynomial cubic spline. The scheme derived in this paper is second-order accurate. The resulting linear system of equations has been solved by using a tri-diagonal solver. Numerical results are provided to illustrate the proposed method and to compared with the methods in [R.K. Mohanty, Urvashi Arora, A family of non-uniform mesh tension spline methods for singularly perturbed two-point singular boundary value problems with significant first derivatives, Appl. Math. Comput., 172 (2006) 531–544; M.K. Kadalbajoo, V.K. Aggarwal, Fitted mesh B-spline method for solving a class of singular singularly perturbed boundary value problems, Int. J. Comput. Math. 82 (2005) 67–76].     

Using empirical Eigenfunctions and Galerkin method to two‐phase transport models

In this article, we consider a nonlinear partial differential system describing two‐phase transports and try to recover the source term and the nonlinear diffusion term when the state variable is known at different profile times. To this end, we use a POD‐Galerkin procedure in which the proper orthogonal decomposition technique is applied to the ensemble of solutions to derive empirical eigenfunctions. These empirical eigenfunctions are then used as basis functions within a Galerkin method to transform the partial differential equation into a set of ordinary differential equations. Finally, the validation of the used method has been evaluated by some numerical examples. © 2006 Wiley Periodicals, Inc. Numer Methods Partial Differential Eq 23: 456–474, 2007     

Wire-coated silver(I) ion-selective electrode based on 2-mercaptobenzothiazole (MBT) ionophore: application to the determination of silver in real samples.

A new wire-coated silver ion-selective electrode with a wider concentration range (10(-7) M - 10(-1) M) was developed using 2-mercaptobenzothiazole (MBT) as a neutral ionophore. An optimum mixture of PVC, ionophore, dioctylphtalate (DOP) as a plasticizer and sodium tetraphenylborate (NaTPB) as an ion-pairing agent was used in preparing the coatings. The effect of various parameters, such as the electrode bed nature, coating composition and solution pH, on the efficiency of the electrode is described. It has been shown that platinum acts as a more suitable bed for electrode preparation, and exhibits a slope of 59.5 +/- 1 mV over the whole range of studied concentrations. The selectivity coefficient of the electrode towards various interfering cations as well as its reproducibility, response time and lifetime of the electrode were estimated. The developed electrode was successfully used for the determination of trace amounts of silver in human hair and photographic waste as real samples and in the potentiometric titration of halides as an indicator electrode.     

Resolving the profile of metabolites generated during oxidation of dibenzofuran and chlorodibenzofurans by the biphenyl catabolic pathway enzymes

Although the metabolism of dibenzofuran by the biphenyl catabolic enzymes had been inferred in previous reports, the metabolic pattern has never been determined unambiguously. In this work, we describe the evolved biphenyl dioxygenase (BPDO) RR41 that exhibits a higher turnover rate of metabolism toward dibenzofuran and chlorodibenzofurans than the parental Burkholderia xenovorans LB400 BPDO. We used RR41 BPDO to identify unambiguously the metabolites produced from the oxygenation of dibenzofuran by LB400 BPDO, and we evaluated their further metabolism by the biphenyl catabolic pathway enzymes of strain LB400. RR41 BPDO was obtained by saturation mutagenesis of targeted amino acid residues. I335F336N338I341L409 of LB400 BphA were replaced by A335M336Q338V341F409 in RR41 BphA. Data confirm the critical role played by these amino acid residues for substrate specificity and regiospecificity.     

A novel one-pot,four component synthesis of some densely functionalized pyrroles

A new one-pot four component procedure for synthesis of densely functionalized pyrroles using commercially available ninhydrin with phosphorane intermediates produced in the reaction between triphenylphosphine, ammonium thiocyanate (or ammonium acetate) and various dialkyl acetylenedicarboxylates was developed.