Determination of some trace metal ions in various samples by FAAS after separation/preconcentration by copper(II)-BPHA coprecipitation method

A separation/preconcentration procedure based on the coprecipitation of Pb(II), Fe(III), Co(II), Cr(III) and Zn(II) ions with copper(II)-N-benzoyl-N-phenyl-hydroxylamine complex (Cu-BPHA) has been developed. The analytical variables including pH, amount of BPHA, amount of copper(II) as carrier element, and sample volume were investigated for the quantitative recoveries of the elements. No interfering effects were observed from the concomitant ions when present in real samples. The recoveries of the analyte ions were in the range of 95–100%. The detection limits (3 s) for Pb(II), Co(II), Fe(III), Cr(III) and Zn(II) ions were found to be 2.3, 0.7, 0.7, 0.3 and 0.4 µg L^?1, respectively. The validation of the procedure was performed by the analysis of CRM (SRM NIST-1547 peach leaves and LGC6019 river water) standard reference materials. The method was applied to the determination of the analytes in real samples including natural waters, hair, urine, soil, sediment and peritoneal fluids samples etc., and good results were obtained (relative standard deviations <4%, recoveries >95%).     

Electrical and interface state density properties of polyaniline–poly-3-methyl thiophene blend/p-Si Schottky barrier diode

We have formed conjugated polymeric aniline–thiophene organic material on p-Si substrate by adding polyaniline–poly-3-methyl thiophene blend solution in acetonitrile on top of a p-Si substrate and then evaporating the solvent. It has been seen that the forward bias current–voltage (I–V) characteristics of polyaniline–poly-3-methyl thiophene blend/p-Si/Al with a barrier height value of 0.60 eV and an ideality factor value of 3.37 showed rectifying behaviour at room temperature. The polyaniline–poly-3-methyl thiophene blend/p-Si/Al Schottky barrier diode showed non-ideal I–V behaviour with the value of ideality factor greater than unity that could be ascribed to the interfacial layer, interface states and series resistance. Furthermore, Cheung's functions and modified Norde's function were used to extract the diode parameters including ideality factor, barrier height and series resistance. It has been seen that there is a good agreement between the barrier height values from all methods. However, the values of series resistance obtained from Cheung's functions is higher than the values obtained from Norde's functions. The energy distribution of interface states density, determined from forward bias current–voltage (I–V) characteristic technique at room temperature, increases exponentially with bias from 2.81 × 10¹⁶ cm^?2 eV^?1 in (0.73–E_v) eV to 1.14 × 10¹⁷ cm^?2 eV^?1 in (0.48–E_v) eV.     

Protein–Inorganic Array Construction: Design and Synthesis of the Building Blocks

Herein we describe the design and synthesis of the first series of di‐functional ligands for the directed construction of inorganic‐protein frameworks. The synthesized ligands are composed of a metal‐ion binding moiety (terpyridine‐based) conjugated to an epoxysuccinyl peptide, known to covalently bind active cysteine proteases through the active‐site cysteine. We explore and optimize two different conjugation chemistries between the di‐functionalized metal‐ion ligand and the epoxysuccinyl‐containing peptide moiety: peptide‐bond formation (with limited success) and Cu^I‐catalysed click chemistry (with good results). Further, the complexation of the synthesized ligands with Fe^II and Ni^II ions is investigated: the di‐functional ligands are confirmed to behave similarly to the parent terpyridine. As designed, the peptidic moiety does not interfere with the complexation reaction, in spite of the presence of two triazole rings that result from the click reaction. ES‐MS together with NMR and UV/Vis studies establish the structure, the stoichiometry of the complexation reactions, as well as the conditions under which chemically sensitive peptide‐containing polypyridine ligands can undergo the self‐assembly process. These results establish the versatility of our approach and open the way to the synthesis of di‐functional ligands containing more elaborated polypyridine ligands as well as affinity labels for different enzyme families. As such, this paper is the first step towards the construction of robust supramolecular species that cover a size‐regime and organization level previously unexplored.     

Comparison of pre-irradiation and mutual grafting of 2-chloroacrylonitrile on cellulose by gamma-irradiation

Radiation-induced graft polymerization is one of the best methods for obtaining materials with new properties. In this work, radiation grafting of 2-chloroacrylonitrile to cellulose by mutual and pre-irradiation grafting methods was investigated. The grafting yield was enhanced by applying the emulsion grafting method. The grafting yield determined in the above systems was observed as 27% at highest and 6% at lowest. The effects of concentration of monomer, reaction time and reaction temperature on grafting yield were studied. Evidence of grafting has been based on the comparative studies of cellulose and grafted cellulose by infrared spectroscopy, thermal analysis and contact angle measurement. Grafting enhances thermal stability of cellulose backbone.     

Thermal desorption/gas chromatography/mass spectrometry approach for characterization of the volatile fraction from amber specimens: A possibility of tracking geological origins

Research on the chemical composition of fossil resins has evolved during the last decades as a multidisciplinary field and is strongly oriented toward the correlation with their geological and botanical origin. Various extraction procedures and chromatographic techniques have been used together for identifying the volatile compounds contained in the fossil resin matrix. Hyphenation between thermal desorption (TD), gas chromatography (GC) and mass spectrometry detection (MS) has been chosen to investigate the volatile compounds fraction from ambers with a focus on Romanite (Romanian amber) and Baltic amber species. A data analysis procedure was developed for the main purpose of fingerprinting ambers based on the MS identity of the peaks generated by the volatile fraction, together with their relative percentual area within the chromatogram. Chromatographic data analysis was based entirely on Automated Mass Spectral Deconvolution & Identification System (AMDIS) software to produce deconvoluted mass spectra which were used to build-up a mixed mass spectra and relative retention scale library. Multivariate data analysis was further applied on AMDIS results with successful discrimination between Romanite and Baltic ambers. A special trial was conducted to generate pyrolysis “like” macromolecular structure breakdown to volatile compounds by gamma irradiation with a high absorbed dose of 500 kGy. Contrary to our expectations the volatile fraction fingerprints were not modified after irradiation experiments. A complementary non-destructive new approach by ESR spectroscopy was also proposed for discriminating between Romanite and Baltic ambers.     

Asymptotic properties of a new Sturm–Liouville problem with retarded argument

In this work, we study the asymptotic properties of a new Sturm–Liouville problem with retarded argument. Contrary to previous works, differential equation includes eigenparameter as a quadratic function. In the considered problem arise new difficulties. Copyright © 2013 John Wiley & Sons, Ltd.     

On the Eigenvalues and Eigenvectors of a Lorentzian Rotation Matrix by Using Split Quaternions

In this paper, we examine eigenvalue problem of a rotation matrix in Minkowski 3 space by using split quaternions. We express the eigenvalues and the eigenvectors of a rotation matrix in term of the coefficients of the corresponding unit timelike split quaternion. We give the characterizations of eigenvalues (complex or real) of a rotation matrix in Minkowski 3 space according to only first component of the corresponding quaternion. Moreover, we find that the casual characters of rotation axis depend only on first component of the corresponding quaternion. Finally, we give the way to generate an orthogonal basis for ${\mathbb{E}^{3}_{1}}$ by using eigenvectors of a rotation matrix.     

Family constraining of iterative algorithms

In constraining iterative processes, the algorithmic operator of the iterative process is pre-multiplied by a constraining operator at each iterative step. This enables the constrained algorithm, besides solving the original problem, also to find a solution that incorporates some prior knowledge about the solution. This approach has been useful in image restoration and other image processing situations when a single constraining operator was used. In the field of image reconstruction from projections a priori information about the original image, such as smoothness or that it belongs to a certain closed convex set, may be used to improve the reconstruction quality. We study here constraining of iterative processes by a family of operators rather than by a single operator.     

Commutators of sublinear operators generated by Calderón-Zygmund operator on generalized weighted Morrey spaces

In this paper, the boundedness of a large class of sublinear commutator operators T _b generated by a Calderón-Zygmund type operator on a generalized weighted Morrey spaces \({M_{p,\varphi }}(w)\) with the weight function w belonging to Muckenhoupt’s class A _p is studied. When 1 < p < ∞ and b ∈ BMO, sufficient conditions on the pair (φ ₁, φ ₂) which ensure the boundedness of the operator T _b from \({M_{p,\varphi 1}}(w)\) to \({M_{p,\varphi 2}}(w)\) are found. In all cases the conditions for the boundedness of T _b are given in terms of Zygmund-type integral inequalities on (φ ₁, φ ₂), which do not require any assumption on monotonicity of φ ₁(x, r), φ ₂(x, r) in r. Then these results are applied to several particular operators such as the pseudo-differential operators, Littlewood-Paley operator, Marcinkiewicz operator and Bochner-Riesz operator.     

A collocation method based on the Bessel functions of the first kind for singular perturbated differential equations and residual correction

In this paper, a collocation method is given to solve singularly perturbated two‐point boundary value problems. By using the collocation points, matrix operations and the matrix relations of the Bessel functions of the first kind and their derivatives, the boundary value problem is converted to a system of the matrix equations. By solving this system, the approximate solution is obtained. Also, an error problem is constructed by the residual function, and it is solved by the presented method. Thus, the error function is estimated, and the approximate solutions are improved. Finally, numerical examples are given to show the applicability of the method, and also, our results are compared by existing results. Copyright © 2014 JohnWiley & Sons, Ltd.