Quantitative kinetic determination of Sb(V) and Sb(III) by spectrophotometric H-point standard addition method

The H-point standard addition method (HPSAM) was applied to kinetic data for simultaneous determination of Sb(V) and Sb(III) and also selectively determines Sb(V) in the presence of Sb(III). The method is based on the differences between rate of complexation of pyrogallol red with Sb(V) and Sb(III) at pH=2. Sb(V) can be determined in the range of 0.3-2.0 μg ml⁻¹ with satisfactory accuracy and precision in the presence of excess Sb(III). Good selectivity was obtained over the variety of metal ions. The proposed method was used for determination of Sb(V) and Sb(III) in river and spring water samples.     

A novel four-component reaction of diethylamine, an aromatic aldehyde and an alkyl isocyanide with dialkyl acetylenedicarboxylates in the presence of silica gel: an efficient route for the regio- and stereoselective synthesis of sterically congested alkenes

The 1:1 intermediate generated by the addition of an isocyanide to a dialkyl acetylenedicarboxylate is trapped by the iminium ion intermediate that forms from the reaction between an aromatic aldehyde and diethylamine. The reactions were completed in the presence of silica gel powder. The product dialkyl 2-[(alkylamino)carbonyl]-3-[(Z)-1-(diethylamino)-1-arylmethylidene]succinates, were produced in acceptable yields. The reactions are completely regio- and stereoselective.     

Effects of different parameters on supercritical fluid extraction of steroid drugs, from spiked matrices and tablets

Feasibility of supercritical CO(2) extractions of two steroid drugs, medroxyprogesterone acetate (med) and cyproterone acetate (cyp), were evaluated. The effects of temperature (308-348 K), pressure (100-300 bar), static extraction time (5-15 min), dynamic extraction time (10-30 min) and percent methanol modifier (1-10% v/v) on the SFE recoveries of these drugs from spiked matrices (glass) and pharmaceutical dosages (tablets) were investigated. The results showed that minor structural differences between related compounds might lead to dramatically differences in extraction behaviors under the same conditions. The optimum SFE conditions to extract the drugs from spiked glass were 10 min static, 30 min dynamic, 300 bar, 348 K and 5% modifier in the case of med acetate and 10 min static, 30 min dynamic, 100 bar, 308 K, and 10% modifier in the case of cyp. Under these conditions above 90% of the total recovery was obtained for both drugs. Extractions from pharmaceutical dosages were less efficient compared to glass beads under the same conditions. Quantitative recovery of solutes from tablets were obtained upon changing extraction conditions to: 15 min static, 45 min dynamic, P=300 bar, 20% modifier (for med) and 10% (for cyp).     

Synthesis and Dynamic NMR Spectroscopic Study of Dialkyl 4-Ethoxy-1-(1-naphthyl)-5-oxo-4,5-dihydro-1<Emphasis Type="Italic">H</Emphasis>-pyrrole-2,3-dicarboxylates

Summary. Protonation of the reactive 1:1 intermediate produced in the reaction between triphenylphosphine and dialkyl acetylenedicarboxylates with ethyl 2-(1-naphthylamino)-2-oxoacetate, leads to a vinylphosphonium salt, which undergoes intramolecular Wittig reaction to produce dialkyl 4-ethoxy-1-(1-naphthyl)-5-oxo-4,5-dihydro-1H-pyrrole-2,3-dicarboxylates in excellent yields. A dynamic NMR effect is observed in the ¹H NMR spectra of the title compounds as a result of restricted rotation around the single bond linking the naphthalene moiety and the heterocyclic system, which is attributed to the peri interaction between the pyrrole residue and the peri CH group. The free energy of activation (G ) for this process is 58±2kJmol^–1.Received December 6, 2002; accepted December 11, 2002 Published online June 12, 2003     

Investigation of Cu Doping,Morphology and Annealing Effects on Structural and Optical Properties of ZnO:Dy Nanostructures

Dysprosium (Dy) doped ZnO nanosheets and nanorods were synthesized by hydrothermal method. Effects of Cu doping, morphology and annealing in Oxygen ambient on structural and optical properties of ZnO nanostructures were investigated using X–ray diffraction (XRD), scanning electron microscopy (SEM), diffuse reflectance spectra (DRS) and photoluminescence (PL) spectroscopy. This study recommends that both of intrinsic and extrinsic defects facilitate energy transfer (ET) from the ZnO host to Dy³⁺ ions and consequently have an effective role on producing intense Dy emissions at indirect excitation. The results also revealed that annealing process improved the crystal structure of ZnO nanorods due to decrease of surface; however decreased ET and Dy emissions because of diminishing in oxygen vacancy. In addition, as a result of increasing of surface area in nanorods compared to nanosheets, the oxygen vacancies and ET were enhanced. Moreover the results exhibited that electrical and optical properties of ZnO:Dy can be tuned by various amount of Dy concentrations and also Cu doping.     

Using generating functions to convert an implicit (3,3) finite difference method to an explicit form on diffusion equation with different boundary conditions

In this article, our main goal is to develop an idea to convert an implicit (3,3) ??-scheme finite difference method to an explicit form for both linear and nonlinear diffusion equations and also for nonlinear advection-diffusion equation with different boundary conditions. Accordingly, we assist power series generating functions which are a routine method in discrete mathematics. Also, the stability analysis of ??–scheme to implement in nonlinear advection–diffusion equation has been investigated. Finally, the new approach has been implemented for Fisher, reaction–diffusion, Burgers and coupled Burgers equations as test problems to verify the ability and efficiency of the method proposed in this paper.     

A posteriori analysis: error estimation for the eighth order boundary value problems in reproducing Kernel space

In the previous work (Akram and Rehman Numer. Algor. 62 527–540 2013), Akram and Rehman presented the reproducing kernel method (RKM) for solving various eighth order boundary value problems. However, an effective error estimation for this method has not yet been discussed. This work is devoted to deal with this problem. Some other aspects of the RKM will be considered such as convergence analysis and numerical implementations.     

Optimization of ilmenite flotation process in the presence of microwave irradiation

In the present study, the effect of parameters, including microwave irradiation power, pH, dosage of chemical reagents (collector, depressant and activator) were studied by microflotation (in Hallimond tube) process. The mechanical flotation tests were carried out on optimum parameters obtained from microflotation tests. The software based on experimental design method (DX7) with the two-level full factorial design was applied to determine the parameter effects and to optimize the microflotation recovery. The optimum conditions were determined by analysis of variance (ANOVA), indicating that the irradiation power was the most effective parameter. The optimum values of parameters in the microflotation process are as follows: power of microwave (1000 W), pH (6.3), dosage of chemical reagents (sodium oleate 3.65 × 10^-4 M as a collector, acidified sodium silicate 2 g L^–1 as a depressant, and lead(II) nitrate 2.1 × 10^–5 M as an activator). By applying these optimized parameters, a product with ilmenite recovery of 83.26% was predicted by the software. The results of microflotation tests indicated that an ilmenite recovery of 82.35% was achieved being very close to the predicted value. The results of mechanical flotation based on optimized condition showed that the recovery and separation efficiency of irradiated ilmenite were improved up to 86.03% and 48.61%, respectively, indicating the positive effect of irradiation on ilmenite floatability.     

Experimental and theoretical study of some <Emphasis Type="Italic">N</Emphasis>-pyridinium salt derivatives as corrosion inhibitors for mild-steel in acidic media

N-pyridinium salt derivatives (1–5) were prepared and investigated as corrosion inhibitors for mild steel in 1 M H₂SO₄ solution at 30°C for 24 h. The corrosion inhibiting action was studied using weight loss measurements. The results demonstrated that the corrosion rate decreases, inhibition efficiencies increase, and surface coverage degree increases with increasing inhibitor concentration. Inhibition efficiencies for prepared N-pyridinium salt derivatives have highest inhibiting efficiency for even low concentration. The values of ΔG_ads^° showed physisorption effect for all prepared compounds. Molecular modeling systems were achieved for suggested inhibitors 1–5. Theoretical calculations could be used as a useful tool to obtain information for explaining the mechanism and nature of interaction between the metal surface and the organic molecule as a corrosion inhibitor.     

Preparation,Characterization and Electrochemical Application of ZnS/ZnAl2S4 Nanocomposite for Voltammetric Determination of Methionine and Tryptophan Using Modified Carbon Paste Electrode

ZnS/ZnAl₂S₄ nanocomposite and 2‐chlorobenzoyl ferrocene, were synthesized and used to construct a modified carbon paste electrode. The electrooxidation of methionine at the surface of the modified electrode was studied. Under the optimized conditions, the square wave voltammetric (SWV) peak current of methionine increased linearly with methionine concentration in the range of 5.0×10^?8 to 8.0×10^?4 M and detection limit of 10.0 nM was obtained for methionine. The prepared modified electrode exhibits a very good resolution between the voltammetric peaks of methionine and tryptophan which makes it suitable for the detection of methionine in the presence of tryptophan in real samples.