Preparation of a fast-flow agarose-based chelating adsorbent with a novel dioxime derivative for selective column preconcentration of copper.

Fast-flow spherical homogeneous agarose beads were prepared by an emulsification method, and were cross-linked and activated by repeated treatment with allylbromide and bromine/water, followed by alkali. Bis(2-aminopyridyl)dioxime (APD) was synthesized by the reaction of 2-aminopyridine, and dichloroglyoxime and characterized by melting-point as well as IR, 1HNMR, 13CNMR and MS spectroscopies. APD was chemically linked to activated agarose beads to be employed for the column preconcentration of metal ions. Capacity measurements for eight metal ions indicated a high selectivity of the adsorbent towards Cu2+ with a capacity of 25.7 micromol per ml packed adsorbent. A factorial design was used for optimization of the effects of 5 different variables on the recovery of Cu2+. Under the optimized conditions, Cu2+ was quantitatively accumulated on a 0.25 ml packed column of the adsorbent in the pH range of 4 to 6, and simply eluted with 2 ml of a 1 mol 1(-1) hydrochloric acid solution. The column could tolerate salt concentrations up to 0.5 mol 1(-1), sample flow rates up to 15 ml min(-1), and sample volumes beyond 1000 ml. Matrix ions of Na+, Mg2+ and Ca2+ and potentially interfering ions of Ni2+, Cd2+, Zn2+, Fe3+ and Co2+ with relatively high concentrations did not show any significant effect on the analyte's signal. Preconcentration factors up to 500 and a detection limit of 0.16 microg 1(-1) were obtained for the determination of the analyte by flame AAS. Application of the method to the determination of natural and spiked copper in river water and seawater samples resulted in quantitative recoveries.     

Eutectic salts promote green synthesis of bis(indolyl) methanes

A convenient and rapid method for the electrophilic substitution reaction of indoles with carbonyl compounds has been developed by using deep eutectic solvent as green and reusable catalysts to afford the corresponding bis(indolyl) methanes in excellent yields at room temperature under mild reaction conditions.     

Constraints on the universe as a numerical simulation

The level scheme above the proton threshold in ²⁶Si is crucial for evaluating the ²⁵Al(p, γ)²⁶Si stellar reaction, which is important for understanding the astrophysical origin of the long-lived cosmic radioactivity ²⁶Al(T _1/2 = 7.17 × 10⁵ y) in the Galaxy. The excited states in ²⁶Si have been studied using an in-beam γ-ray spectroscopy technique with the ²⁴Mg(³He, nγ)²⁶Si reaction. γ-rays with energies up to 4.6 MeV emitted from excited states in ²⁶Si have been measured using large volume HPGe detectors. The spin-parity of one of the most important states reported recently at 5890.0keV has been assigned as 0⁺ by γ-γ angular correlation measurements in this work.     

Magnetically assisted solid phase extraction using Fe3O4 nanoparticles combined with enhanced spectrofluorimetric detection for aflatoxin M1 determination in milk samples

A novel, facile and inexpensive solid phase extraction (SPE) method using ethylene glycol bis-mercaptoacetate modified 3-(trimethoxysilyl)-1-propanethiol grafted Fe₃O₄ nanoparticles coupled with spectrofluorimetric detection was proposed for determination of aflatoxin M1 (AFM1) in liquid milk samples. The method uses the advantage fluorescence enhancement by β-cyclodexterin complexation of AFM1 in 12% (v/v) acetonitrile–water and the remarkable properties of Fe₃O₄ nanoparticles namely high surface area and strong magnetization were utilized to achieve high enrichment factor (57) and satisfactory extraction recoveries (91–102%) using only 100 mg of magnetic adsorbent. Furthermore, fast separation time of about 15 min avoids many time-consuming column-passing procedures of conventional SPE. The main factors affecting extraction efficiency including pH value, desorption conditions, extraction/desorption time, sample volume, and adsorbent amount were evaluated and optimized. Under the optimal conditions, a wide linear range of 0.04–8 ng mL⁻¹ with a low detection limit of 0.015 ng mL⁻¹ was obtained. The developed method was applied for extraction and preconcentration of AFM1 in three commercially available milk samples and the results were compared with the official AOAC method.     

Arene diazonium saccharin intermediates: a greener and cost-effective alternative method for the preparation of aryl iodide

In the current protocol, the arene diazonium saccharin derivatives were initially produced from various substituted aromatic amines; subsequently, these intermediates were treated with a greener organic iodide for the preparation of the aryl iodide. We tried to choose low-cost, commercially available, biodegradable, recoverable, ecofriendly, and safe reagents and solvents. The arene diazonium saccharin intermediates could be stored in the liquid phase into a refrigerator for a long time with no significant loss activity. The outstanding merits of the current protocol (a) included the partial recovering of saccharin and tetraethylammonium salt, (b) reduce the use of solvents and the reaction steps due to eliminating separation and purification of intermediates, (c) good yield of the sterically hindered substrates, and (d) avoid the generation of heavy metal or corrosive waste.     

Simple optical determination of silver ion in aqueous solutions using benzo crown-ether modified gold nanoparticles

We describe a method for the modification of gold nanoparticles (Au-NPs) with benzo-15-crown-5 that led to the development of a colorimetric assay for Ag(I) ion. The brown color of a solution of the modified Au-NPs turns to purple on addition of Ag(I) ion. The ratio of the UV–vis absorption at 600 nm and 525 nm is proportional to the concentration of Ag(I) ions in the range from 20 to 950 nM, and the detection limit is 12.5 nM. Other metal ions do not interfere if present in up to millimolar concentrations. The method enables a rapid determination of Ag(I) in lake and drinking water and is amenable to bare-eye readout.

Adhesion and interfacial interactions of BaO–SiO<Subscript>2</Subscript>–B<Subscript>2</Subscript>O<Subscript>3</Subscript>-based glass-ceramic seals and AISI430 interconnect for solid oxide fuel cell applications

In the present work, adhesion, leak rate, and chemical compatibility of a series of borosilicate-based glasses, belonging to the ternary BaO–SiO₂–B₂O₃ system, with AISI 430 alloys as interconnect were investigated for solid oxide fuel cell applications. Wetting angle and deformation behavior of the selected glasses with temperature and time were initially characterized with the hot-stage microscope. It was observed that the temperature ranges of wetting for all combinations were greater than 1000 °C. Significant deformation did not appear in the samples over soaking time at sealing temperature. In the next step, the leakage tests of AISI430/glass-ceramic couples were performed. The sample containing 32 % molar BaO (Ba32) had no gas leakage; a low leak rate of 10^?7to 10^?8 Pam³ s^?1 was obtained for the glass with 37 % molar BaO (Ba37) and big leak of the system (10^?3to 10^?4 Pam³ s^?1) for Ba42. Possible interfacial reactions between the as-received glass and cell ingredients and aging up to 100 h were studied by scanning electron microscopy in conjunction with energy-dispersive X-ray spectroscopy and X-ray dot mapping. The results showed that the Ba32 and Ba37 glasses coupled with AISI had fine adhesion, which remained stable under these conditions and were compatible with the interconnect. So, the use of these glass-ceramics will probably be successful in joining the ceramic electrolytes to the metallic interconnect.     

Dioxidomolybdenum(VI) complexes of allyl N'-2-hydroxy-3-methoxybenzylidenecarbamohydrazonothioate: synthesis,spectral, and theoretical investigations

The new dibasic NNO ligand H₂L (H₂L = allyl N′-2-hydroxy-3-methoxybenzylidenecarbamohydrazonothioate) was synthesized by condensation of 2-hydroxy-3-methoxybenzaldehyde with the product resulting from the reaction of thiosemicarbazide with allyl bromide. Four dioxidomolybdenum(VI) complexes with the general formula [MoO₂L(S)] (S=MeOH, EtOH, DMSO, and 1-methylimidazole) were synthesized and characterized by elemental analysis, FT-IR, EI-MS and UV-Vis spectroscopy, and by X-ray crystallography. Spectroscopic evidence indicates that the cis-MoO₂ chelates have octahedral geometry in which H₂L coordinates via the phenolate oxygen, azomethine nitrogen and deprotonated thioamide nitrogen. The other sites are occupied by two oxido and an additional ligand (S). Density functional theory calculations of spectral parameters were also carried out for these systems.     

Simultaneous voltammetric determination of uric acid and ascorbic acid using carbon paste/cobalt Schiff base composite electrode

Differential pulse and cyclic voltammetry were applied for the oxidation of mixture of uric acid and ascorbic acid at the surface of carbon paste/cobalt Schiff base composite electrode. The electrooxidation of these compounds at bare electrode is sluggish, and there is no suitable peak separation between them. However, using cobalt methyl salophen as modifier, two well-defined anodic waves with a considerable enhancement in the peak current and a remarkable peak potential separation near 315 mV are obtained. It can improve the kinetics of electron transfer for both compounds remarkably. All these improvements are created because of the electrocatalytic property of cobalt Schiff base complex. The effect of some parameters such as pH and scan rates were studied. All the anodic peak currents for the oxidation of ascorbic acid and uric acid shifted toward more negative potential with an increase in pH, revealing that protons have taken part in their electrode reaction processes. The best peak separation with appropriate current was obtained for pH 4.0. A linear range of 5.0?×?10^?4 to 1.0?×?10^?8 and 1.0?×?10^?3 to 1.0?×?10^?8 M with detection limit of 8.0?×?10^?9 and 8.0?×?10^?9 M was obtained for ascorbic acid and uric acid using differential pulse voltammetry at the surface of modified electrode, respectively. Analytical utility of the modified electrode has been examined successfully using human urine samples and vitamin C commercial tablets.     

Small signal gain and saturation intensity of a Yb:Silica fiber MOPA system

In this work, the small signal gain (γ₀) and signal saturation power (P_sat) of a continuous wave (CW) single-frequency ytterbium-doped (YD) double-clad (DC) fiber master oscillator power amplifier (MOPA) array has been determined in the optimum length. At first, we have obtained output versus input signal powers in the amplifier, using the coupled steady-state rate equations for the various end diode pumping such as co/counter propagation and bidirectional modes. On the other hand, the steady-state amplification relation was employed at a presumed γ₀ and P_sat as initial guess, to generate output signals. Then, using the least square method (LSM), those input/output signal powers were fitted by the best regression curve obtained from the amplification relation to determine the converged γ₀ and P_sat values. The analytical formulae for γ₀ and P_sat were derived using the rate equations as well.