Efficient Synthesis of Bis-Coumarins Using Silica-Supported Preyssler Nanoparticles

Reaction of aldehydes and 4-hydroxycoumarin in the presence of catalytic amount of silica-supported Preyssler nanoparticles led to synthesis of bis-coumarins in excellent yields.     

Photoactivated Nitrene Chemistry to Prepare Gold Nanoparticle Hybrids with Carbonaceous Materials

Photolysis of organic solvent soluble aryl azide‐modified gold nanoparticles (N₃‐AuNPs) with a core size of 4.6±1.6 nm results in the generation of interfacial reactive nitrene intermediates. The high reactivity of the nitrenes is utilized to tether the AuNP to the native surface of carbon nanotubes, and reduce graphene oxide and micro‐diamond powder, likely via addition to π‐conjugated carbon skeleton or insertion into the functionalities at the surface, to yield the desired hybrid material without the need for pretreatment of the surface. The AuNP‐covalent hybrid materials are robust in that they survive vigorous washing and sonication. In the absence of photolysis no attachment occurs with the same N₃‐AuNP. The nanohybrid AuNP‐nanohybrid materials are characterized using a combination of TEM, powder XRD, XPS and UV/Vis and IR spectroscopies. All of the characterization studies confirm the uniform incorporation of the AuNP on the irradiated substrates.     

Determination of non-steroidal anti-inflammatory drugs in water samples by solid-phase microextraction based sol–gel technique using poly(ethylene glycol) grafted multi-walled carbon nanotubes coated fiber

In this study, poly(ethylene glycol) (PEG) grafted multi-walled carbon nanotubes (PEG-g-MWCNTs) were synthesized by the covalent functionalization of MWCNTs with hydroxyl-terminated PEG chains. PEG-g-MWCNTs was used as a novel stationary phase to prepare the sol–gel solid-phase microextraction (SPME) fiber in combination with gas chromatography–flame ionization detector (GC–FID) for the determination of ibuprofen, naproxen and diclofenac in real water samples.     

Dispersive solid phase micro-extraction of dopamine from human serum using a nano-structured Ni-Al layered double hydroxide, and its direct determination by spectrofluorometry

We report on a simple method for dispersive solid-phase micro-extraction of dopamine (DA) from human serum. It is based on a layered double hydroxide (LDH) of nickel-aluminum, which acts as the extractant. DA is extracted at pH 8 using the LDH sol solution as a dispersed solid-phase extractor. The extracted DA is quantified by spectrofluorometry at 285?nm excitation and 315?nm emission wavelengths. A comparison of the fluorescence of DA in bulk solution and that of DA intercalated in the LDH revealed a nearly 5-fold improvement in intensity. Factors such as pH, concentration of LDH in the sol solution, and temperature were optimized. Under these conditions, the limit of detection is 0.015?μg?L^?1. The inter- and intra-day relative standard deviations for six replicate determinations of 1?μg?L^?1 DA were 1.7 and 1.1?%, respectively. The method was successfully applied to the determination of DA in human serum samples.

Feasibility study on reducing lead and cadmium absorption by spinach (Spinacia oleracea L.) in a contaminated soil using nanoporous activated carbon

Activated carbons (AC) have been long recognized as prominent absorbents in industries and feature numerous applications in preventing or absorbing the harmful gases and liquids and could be employed for filtration and remediation or even reutilization of chemicals. In order to investigate the capacity of AC in reducing the absorption of heavy metals (HM) including lead (Pb) and cadmium (Cd) and dual complex (Pb?×?Cd) by spinach, a factorial experiment in a completely randomized design with three replications on a pot trial was conducted. Three factors including five levels of AC 0, 5000, 10000, 15000, 20000?mg/kg soil, one concentration level of Pb 4,000?mg/kg soil and one concentration level of cadmium Cd 8?mg/kg soil were tested. The index of heavy metal concentration was calculated in leaf, stem and root and their corresponding dry weights. Results illustrated that in contaminated soils, plants with AC exhibited a superior reduction of absorption of HM vis-à-vis the plants without AC. The foremost result regarding the impact of AC on reducing the concentration of Pb and Cd was observed in 20,000 level of AC. This reveals that AC declined the soil contamination and lessened the accumulation of HM into the shoots and roots. Results suggest that the application of AC may be an eligible solution for decreasing the translocation of HM into the plants.     

Solvent influence upon complexation of N-phenylaza-15-crown-5 with UO2 2+ cation in binary mixed non-aqueous solvents

The complexation reaction of N-phenylaza-15-crown-5 (PhA15C5) with UO₂ ²⁺ cation was studied in acetonitrile–methanol (AN–MeOH), acetonitrile–butanol (AN–BuOH), acetonitrile–dimethylformamide (AN–DMF) and methanol–propylencarbonate (MeOH–PC) binary solutions, at different temperatures by conductometry method. The conductance data show that the stoichiometry of the complex formed between PhA15C5 with UO₂ ²⁺ cation in most cases is 1:1 [M:L], but in some solvent systems a 1:2 [M:L₂] complex is formed in solutions. The results revealed that, the stability constant of (PhA15C5·UO₂)²⁺ complex in the binary mixed solvents varies in the order: AN–BuOH>AN–MeOH>AN–DMF. In the case of the pure organic solvents, the sequence of the stability of the complex changes as: AN>PC>BuOH>DMF. A non-linear relationship was observed for changes of logK_f of (PhA15C5·UO₂)²⁺ complex versus the composition of the binary mixed solvents. The corresponding standard thermodynamic parameters (ΔH_c°, ΔS_c°) were obtained from temperature dependence of the stability constant. The results show that the values and also the sign of these parameters are influenced by the nature and composition of the mixed solvents.     

A Study on Transreactions of PET/PEN Reactive Blending in a Twin‐Screw Extruder Using an Axial Dispersion Model

Transreactions of PET and PEN melt‐mixed in a twin‐screw extruder are investigated. The extruder is modeled and characterized in the frame of a tubular system of closed type. The kinetic modeling is based on a modified second‐order reversible reaction equation, which allows the dispersion equation to be solved analytically. The analysis shows a good agreement between the model and experiment. The axial dispersion model is employed to predict the extent of transesterification reactions (X) and degree of randomness (RD). ¹H NMR measurements are performed to estimate X and RD. Theoretical and experimental data are in good agreement. The model can thus be exploited to describe the effects of processing parameters, mixing time, mixing temperature, and blend composition on X and RD.

     

以方沸石负载Ni(Ⅱ)催化剂修饰的电极电氧化甲醇(英文)

There is a high overvoltage in the oxidation of methanol in fuel cells,and so modified electrodes are used to decrease it.A modified electrode that used Ni(II) loaded analcime zeolite to catalyze the electrooxidation of methanol in alkaline solution was proposed.Analcime zeolite was synthesized by hydrothermal synthesis,and Ni(II) ions were incorporated into the analcime structure,which was then mixed with carbon paste to prepare modified electrode.The electrocatalytic oxidation of methanol on the surface of the modified electrode in alkaline solution was investigated by cyclic voltammetry and chronoamperometry.The effects of the scan rate of the potential,concentration of methanol,and amount of zeolite were investigated.The rate constant for the catalytic reaction of methanol was 6 × 103 cm3 mol-1 s-1 from measurements using chronoamperometry.The proposed electrode significantly improved the electron transfer rate and decreased the overpotential for methanol oxidation.     

Magnetically nano core–shell Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@Cu(OH)<Subscript>x</Subscript>: a highly efficient and reusable catalyst for rapid and green reduction of nitro compounds

Magnetically separable nano core–shell Fe₃O₄@Cu(OH)_x with 22 % Cu content was prepared by the addition of sodium hydroxide to a mixture of CuCl₂·2H₂O and nano Fe₃O₄ in water. Characterization of the impregnated copper hydroxide was carried out by X-ray fluorescence (XRF), X-ray diffraction (XRD) atomic absorption spectroscopy (AAS), scanning electron microscopy (SEM), value stream mapping (VSM) and Brunauer–Emmett–Teller (BET) analysis. The core–shell nanocatalyst exhibited the excellent catalytic activity toward reduction of various nitro compounds to the corresponding amines with NaBH₄. All reactions were carried out in H₂O (55–60 °C) within 3–15 min to afford amines in high to excellent yields. Reusability of core–shell Cu(OH)_x catalyst was examined 9 times without significant loss of its catalytic activity.     

New polypyrrole–carbon nanotubes–silicon dioxide solid‐phase microextraction fiber for the preconcentration and determination of benzene,toluene, ethylbenzene,and o‐xylene using gas liquid chromatography

For the first time, a polypyrrole–carbon nanotubes–silicon dioxide composite film coated on a steel wire was prepared by an electrochemical method. Scanning electron microscopy images showed that this composite film was even and porous. The prepared fiber was used as an absorbent for the headspace solid‐phase microextraction of benzene, toluene, ethylbenzene, and o‐xylene, followed by gas chromatographic analysis. This method presented an excellent performance, which was much better than that of a polypyrrole–carbon nanotube fiber. It was found that under the optimized conditions, the linear ranges were 0.01–200 ng/mL with correlation coefficients >0.9953, the detection limits were 0.005–0.020 ng/mL, the relative standard deviations were 3.9–6.4% for five successive measurements with a single fiber, and the reproducibility was 5.5–8.5% (n = 3). Finally, the developed method was successfully applied to real water samples, and the relative recoveries obtained for the spiked water samples were from 91.0 to 106.7%.