Magnetic solid-phase extraction using Schiff base ligand supported on magnetic nanoparticles as sorbent combined with dispersive liquid-liquid microextraction for the extraction of phenols from water samples

ABSTRACT

In this work, the magnetic sorbent was developed by covalent binding of a Schiff base ligand, N,N’-bis(3-salicyliden aminopropyl)amine (salpr), on the surface of silica coated magnetic nanoparticles (Salpr@SCMNPs). The core-shell nanoparticle was applied for the magnetic solid-phase extraction (MSPE) combined with dispersive liquid-liquid microextraction (DLLME) of phenolic compounds from water samples prior to gas chromatography-flame ionisation detector (GC?FID). Characterisation of the Salpr@SCMNPs was performed with different physicochemical methods such as Fourier transform infrared (FT-IR), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). Variables affecting the performance of both extraction steps such as pH of the water sample, the sorbent amount, the desorption conditions, the extraction time; and extraction solvent were studied. Under the optimised conditions, the analytical performances were determined with a linear range of 0.01–100 ng mL^?1 and a limit of detection at 0.003–0.02 ng mL^?1 for all of the analytes studied. The intra-day (n = 5) and inter-day (n = 3) relative standard deviations (RSD%) of three replicates were each demonstrated in the range of 6.9–8.9% and 7.3–10.1%, respectively. The proposed method was executed for the analysis of real water samples, whereby recoveries in the range of 92.9–99.0% and RSD% lower than 6.1% were attained.     

Reaction between triphenylphosphine and aromatic amines in the presence of diethyl azodicarboxylate: an efficient synthesis of aryliminophosphoranes under neutral and mild conditions

An efficient synthesis of aryliminophosphoranes is described. A mixture of an aromatic amine, diethyl azodicarboxylate and triphenylphosphine undergo a Mitsonobu type reaction at ambient temperature in dry dichloromethane to afford aryliminophosphoranes in excellent yields.     

Magnetic properties and microwave absorption in Ni-Zn and Mn-Zn ferrite nanoparticles synthesized by low-temperature solid-state reaction

In this work, Mn_0.7Zn_0.3Fe₂O₄ and Ni_0.7Zn_0.3Fe₂O₄ nanoparticles with super-paramagnetic properties and size distribution from 10 to 52 nm were investigated. These particles were produced by a low-temperature solid-state reaction method without the ball-milling process. The size and morphology of the nanocrystallites were determined by X-ray diffraction, transmission electron microscopy and scanning tunneling microscopy methods. Magnetic measurements such as alternating gradient field magnetometers were used to justify the super-paramagnetic properties of these nanoparticles. Their microwave absorption in the range of 8-18 GHz was studied by a vector network analyzer. Responses of the device under tests were studied. Also, the percentage of the resin, the size and thickness of the mount were determined. The band width of 2.3 GHz was obtained with reflection-loss/written-loss of −16 dB around 10.4 GHz.     

Integrated photonic crystal spectrometers for sensing applications

A combination of negative refraction and diffraction compensation in a superprism-based photonic crystal structure is used to demonstrate a compact on-chip photonic crystal spectrometer. This structure provides strong dispersion and signal isolation, which are essential for forming an efficient and compact spectrometer. Performance of these spectrometers as spectral pattern detectors is discussed. The experimental results show that a PC structure with 80 μm × 220 μm dimension can locate a single spectral feature with better than 10 pm accuracy over a bandwidth of 50 nm around 1550 nm center wavelength at an output signal-to-noise ratio of 13 dB.     

FDTD Simulation of Electromagnetic Pulse Interaction with a Switched Plasma Slab

This paper deals with the Finite Difference Time Domain (FDTD) simulation of interaction of an electromagnetic wave with a switched plasma slab. In formulating the simulation the well-known concepts of (a) total-field/scattered-field formulation (b) and PML lattice truncation are adapted to suit the simulation under consideration.FDTD is particularly well suited to handle the switched (time-varying) medium (including sudden switching) since the time varying parameters of the medium can be easily interpreted in the algorithm. The technique is applied to the difficult problem of interaction of an electromagnetic pulse source wave of frequency ₀ and a gaussian envelope with a newly created plasma slab of time-varying and space varying electron density profile. The creation of a pulse of Wiggler magnetic field in the slab is illustrated.     

Conceptual linearization of Euler governing equations to solve high speed compressible flow using a pressure‐based method

The main objective of the current work is to introduce a new conceptual linearization strategy to improve the performance of a primitive shock‐capturing pressure‐based finite‐volume method. To avoid a spurious oscillatory solution in the chosen collocated grids, both the primitive and extended methods utilize two convecting and convected momentum expressions at each cell face. The expressions are obtained via a physical‐based discretization of two inclusive statements, which are constructed via a novel incorporation of the continuity and momentum governing equations. These two expressions in turn provide a strong coupling among the Euler conservative statements. Contrary to the primitive work, the linearization in the current work respects the definitions and essence of physics behind deriving the Euler governing equations. The accuracy and efficiency of the new formulation are then investigated by solving the shock tube as a problem with moving normal and expansion waves and the converging‐diverging nozzle as a problem with strong stationary normal shock. The results show that there is good improvement in performance of the primitive pressure‐based shock‐capturing method while its superior accuracy is not deteriorated at all. © 2007 Wiley Periodicals, Inc. Numer Methods Partial Differential Eq, 2008     

On hydraulic permeability of random packs of monodisperse spheres: Direct flow simulations versus correlations

Hydraulic permeability is studied in porous media consisting of randomly distributed monodisperse spheres by means of computational fluid dynamics (CFD) simulations. The packing of spheres is generated by inserting a certain number of nonoverlapping spherical particles inside a cubic box at both low and high packing fractions using proper algorithms. Fluid flow simulations are performed within the interparticulate porous space by solving Navier-Stokes equations in a low-Reynolds laminar flow regime. The hydraulic permeability is calculated from the Darcy equation once the mean values of velocity and pressure gradient are calculated across the particle packing. The simulation results for the pressure drop across the packing are verified by the Ergun equation for the lower range of porosities (<0.75), and the Stokes equation for higher porosities (∼1). Using the results of simulations, the effects of porosity and particle diameters on the hydraulic permeability are investigated. Simulations precisely specified the range of applicability of empirical or semi-empirical correlations for hydraulic permeability, namely the Carman-Kozeny, Rumpf-Gupte, and Howells-Hinch formulas. The number of spheres in the model is gradually decreased from 2000 to 20 to discover the finite-size effect of pores on the hydraulic permeability of spherical packing, which has not been clearly addressed in the literature. In addition, the scale dependence of hydraulic permeability is studied via simulations of the packing of spheres shrunk to lower scales. The results of this work not only reveal the validity range of the aforementioned correlations, but also show the finite-size effect of pores and the scale-independence of direct CFD simulations for hydraulic permeability.     

A green and highly efficient alkylation of thiols in water

An environmentally benign and efficient process for the preparation of thioethers was developed by simple and practical reactions of alkyl halides and thiols in water in the presence of K₂CO₃ or Et₃N in very high yields. The reaction of aryl, alkyl, aliphatic and hindered thiols with various alkyl halides gave the corresponding products with significant advantages such as high conversions, short reaction time, mild reaction conditions, and low cost, simple workup with good to quantitative yields.     

KF‐Melamine Formaldehyde Resin (KF‐MFR) as a Versatile and Efficient Heterogeneous Reagent for Aldol Condensation of Aldehydes and Ketones under Microwave Irradiation

KF‐Melamine formaldehyde resin (KF‐MFR) was demonstrated to be a highly efficient heterogenious catalyst for cross‐aldol condensation under microwave irradiation. In this synthesis, various aldehydes and ketones were condensed together in the presence of supported KF on melamine‐formaldehyde resin to afford different chalcone derivatives in good to excellent yields. KF‐MFR proved to have unique termal and chemical resistance and can be reused for many consecutive runs without remarkable loss in catalytic activity.