Optimization of analytical procedures for the simultaneous voltammetric determination of total Hg(II) in presence of Cu(II) in environmental matrices

The present work reports the critical comparison about the employment of three different supporting electrolytes (0.1 mol L⁻¹ HClO₄, 0.01 mol L⁻¹ EDTA-Na² + 0.06 mol L⁻¹ NaCl + 2.0 mol L⁻¹ HClO₄ and 0.1 mol L⁻¹ KSCN + 0.001 mol L⁻¹ HClO₄) and their instrumental and chemical optimisation for the simultaneous voltammetric determination of total mercury(II) and copper(II) in sediments and sea water at gold electrode, especially discussing the reciprocal interference problems.     

Further bounds for hardy type differences

In this paper we define a functional as a difference between the right-hand side and left-hand side of the refined Boas type inequality using the notation of superquadratic and subquadratic functions and study its properties, such as exponential and logarithmic convexity. We also, state and prove improvements and reverses of new weighted Boas type inequalities. As a special case of our result we obtain improvements and reverses of the Hardy inequality and its dual inequality. We introduce new Cauchy type mean and prove monotonicity property of this mean.     

Comparison of arsenate, chromate and molybdate binding on schwertmannite: Surface adsorption vs anion-exchange

We have synthesized a series of nanocatalysts with different sizes (50-200 nm) for polymerization of 1,3-butadiene (Bd) by immobilizing salicylaldimine cobalt complexes on the mesoporous silica nanoparticles (MSNs). The prepared catalysts have been characterized by infrared (IR) spectra, thermal gravimetric analyses (TGAs), chemical composition analysis, nitrogen adsorption-desorption, scanning electron microscope (SEM), and transmission electron microscope (TEM). The nanocatalysts in combination with methylaluminoxane (MAO) show excellent catalytic efficiency in polymerization of 1,3-butadiene. The results reveal that these nanocatalysts also show higher activity than the homogeneous analog of cobalt complex and the same catalyst on bulky mesoporous silica supporting materials. The yield and the molecular weight of the poly-butadiene product depend on the particle size of the catalyst support. This catalysis process is also a facile way to directly synthesize the polymer/silica composite materials.     

Behaviour of phospholipids in analytical reactive pyrolysis

Checking for the presence of egg in a painting layer allows to decide whether or not it is a tempera. Several already assessed analytical techniques may be used to perform the chemical analysis for the detection of egg in paintings. As an advantageous and alternative methodology for the determination of egg, a new application of analytical pyrolysis, hyphenated with gas chromatography–mass spectrometry (GC–MS) system, in presence of hexamethyldisilazane (HMDS) and tetramethylammonium-hydroxide (TMAH), is reported here. The innovation lays mainly in the choice of new markers for the presence of egg. It is here demonstrated that in art diagnostic tris-TMS-ester and methyl ester of phosphoric acid, generated by the pyrolysis of standard phospholipids and synthetic painting layers containing egg as binding medium, may be used as new markers for identification of egg in tempera layers. The adoption of these new markers in analytical pyrolysis allows to obtain higher analytical performance with respect to classical markers (fatty acids), especially in terms of yield and, as a consequence, in terms of limit of detection.     

Ultra-sensitive voltammetric sensor for trace analysis of carbamazepine

A multi-walled carbon nanotubes (MWCNTs) film-coated glassy carbon electrode (GCE) was used for the voltammetric determination of carbamazepine (CBZ). The results showed that this simple modified electrode exhibited excellent electrocatalytic activity towards the oxidation of CBZ. The voltammetric response of CBZ at this film-modified electrode increased significantly when compared with that at a bare glassy carbon electrode and the sensor response was reproducible. The proposed method was applied to the quantification of CBZ in wastewater samples, collected in a municipal wastewater treatment plant, and in pharmaceutical formulations. The developed methodology yields results in accord with those obtained by chromatographic techniques commonly used in the quantification of pharmaceutical compounds in real samples. Good recoveries have been obtained and the limits of detection and quantification (40 and 140 nM, respectively) are among the lowest that have been reported to date for this pharmaceutical compound using voltammetric techniques.     

Dispersion-flattened polarization-maintaining photonic crystal fiber for nonlinear applications

In this paper, we propose a novel photonic crystal fiber design to achieve high birefringence, high nonlinearity with a flattened dispersion profile. The air holes which are embedded in silica are arranged in triangular lattice configuration. In the core region, an air hole is introduced as the central defect to flatten the dispersion curve. The shape of the defect air hole is deliberately designed elliptical so that high birefringence in the PCF is obtained for polarization-maintaining purpose. The structural parameters are carefully selected to optimize the optical properties.     

Photonic crystal fiber tip interferometer for refractive index sensing

In this paper we present an interferometer based on photonic crystal fiber (PCF) tip ended with a solid silica-sphere for refractive index sensing. The sensor is fabricated by splicing one end of the holey PCF to a single mode fiber (SMF) and applying arc at the other end to form a solid sphere. The sensor has been experimentally tested for refractive index and temperature sensing by monitoring its wavelength shift. Measurement results show that the sensor has the resolution of the order of 8.7×10(-4) over the refractive index range of 1.33-1.40, and temperature sensitivity of the order of 10 pm/°C in the range of 20-100 °C.     

Three-dimensional FDTD method for optical pulse propagation analysis in microstructured optical fibers

We propose a three-dimensional (3D) finite-difference time-domain (FDTD) method to analyze the pulse propagation characteristics in microstructured optical fibers (MOFs). The computation domain size is greatly reduced by adopting the technique of moving problem space. The propagating pulse is virtually held in the buffer cell of the problem space as simulation continues. This method is capable to investigate the temporal evolution of the propagating pulse. Spectral information can be obtained by Fourier analysis. As an example, the influence of the kerr nonlinearity on the optical pulse propagation in a Lorentz dispersive MOF is demonstrated. The model is also used to simulate the nonlinear interactions between the pump spectral broadening and third harmonic generations in a highly nonlinear fused silica nanowire with good agreement with the generalized nonlinear envelop equation (GNEE) model.     

Pigment analysis of Portuguese portrait miniatures of 17th and 18th centuries by Raman Microscopy and SEM‐EDS

Seventeen Portuguese miniature portraits on copper support from the Évora Museum collection (Portugal) were analyzed in situ and nondestructively by Raman microscopy (RM), SEM‐EDS, and stereomicroscopy. This work constitutes a great breakthrough in the study of miniature paintings from the 17^th and 18^th centuries, since the chemical information known about this unique kind of paintings are still scarce, and in particular, this exclusive collection was never been subjected to any physicochemical study. In this work, each portrait was examined in detail in order to characterize the pigments palette used by the miniaturists. The μ‐Raman analysis, in particular, guaranteed an exceptional visualization and good individual identification of small grains of pigments and other constituents of the pictorial layer. Using this technique, 19 compounds were identified, including bluish black covellite, a pigment rarely found in oil paintings. SEM‐EDS was used as an important complementary technique to confirm the chemical nature of some pigments and to identify shell gold (gold dust) in some portraits. Overall, the pigments identified in this large set of old paintings are broadly consistent with those mentioned in the painting treatises of that time or reported in other more modern bibliographic sources. Copyright © 2014 John Wiley & Sons, Ltd.