Preparation of Silver Nanoparticles‐Based Sensors for the Electrochemical Detection of Thiourea in Leaching Solutions of Waste Electrical and Electronic Equipment

Waste of electrical and electronic equipment is an interesting secondary resource of base and precious metals. Particularly the use of thiourea‐leaching in acidic medium was proposed for noble metals recovery. In this work, a novel and easy‐to‐use electrochemical sensor was developed, aimed to test thiourea from leaching solutions containing significant thiourea and copper amounts. The sensor was constructed using silver nanoparticles (AgNPs) deposited on screen‐printed electrodes. Its performance was studied in a synthetic leaching solution; changes in the overall surface charge of AgNPs resulting in changes in the charge‐transfer resistance for the copper ions were evaluated by electrochemical impedance spectroscopy.     

Determination of mazindol in human oral fluid by high performance liquid chromatography–electrospray ionization mass spectrometry

Brazil is one of the countries most affected by abuse of stimulant medications by professional drivers, especially fenproporex, amfepramone and mazindol. Even though their sale is banned, they can be found in illegal markets, such as those located on the country's borders. The use of oral fluid to monitor drug levels has many advantages over plasma and urine because it is noninvasive, easier to collect and more difficult to adulterate. The aim of this study was to develop and validate a sensitive and specific method to quantify mazindol in human oral fluid by liquid chromatography–mass spectrometry (LC‐MS). The LC system consisted of an LC‐MS system operated in selected ion monitoring mode. The mobile phase was composed of water at pH 4.0, acetonitrile and methanol (60:15:25 v/v/v) at a flow rate of 1.0 mL/min and propranolol was used as internal standard. Total running time was 10 min. The lower limit of quantification was 0.2 ng/mL and the method exhibited good linearity within the 0.2–20 ng/mL range (r = 0.9987). A rapid, specific, sensitive, linear, precise and accurate method was developed for determination of mazindol in human oral fluid according to European Medicines Agency guidelines, and is suitable for monitoring mazindol levels in oral fluid of professional drivers. Copyright © 2014 John Wiley & Sons, Ltd.     

Human Y‐chromosome SNP characterization by multiplex amplified product‐length polymorphism analysis

We designed an allele‐specific amplification protocol to optimize Y‐chromosome SNP typing, which is an unavoidable step for defining the phylogenetic status of paternal lineages. It allows the simultaneous highly specific definition of up to six mutations in a single reaction by amplification fragment length polymorphism (AFLP) without the need of specialized equipment, at a considerably lower cost than that based on single‐base primer extension (SNaPshot?) technology or PCR‐RFLP systems, requiring as little as 0.5 ng DNA and compatible with the small fragments characteristic of low‐quality DNA. By designation of two primers recognizing the derived and ancestral state for each SNP, which can be differentiated by size by the addition of a noncomplementary nucleotide tail, we could define major Y clades E, F, K, R, Q, and subhaplogroups R1, R1a, R1b, R1b1b, R1b1c, J1, J2, G1, G2, I1, Q1a3, and Q1a3a1 through amplification fragments that ranged between 60 and 158bp.     

Support functions and integral formulas in the Lorentzian plane

In the Lorentzian plane, the support function of a closed convex curve is not a periodic one. We redefine this concept and the envelope of a families of lines. Using these, we prove integral formulas in the Crofton's style for convex sets in the Lorentzian plane. Received 10 February 2000.     

Some insight into characterizations of minimally nonideal matrices

Lehman (Polyhedral combinatorics 1 of DIMACS series in discrete math. and theoretical computer science, pp 101–105, 1990) described some conditions regular minimally nonideal (mni) matrices must satisfy. Although, there are few results on sufficient conditions for mni matrices. In most of these results, the covering polyhedron must have a unique fractional extreme point. This condition corresponds to ask the matrix to be the blocker of a near-ideal matrix, defined by the authors in a previous work (2006). In this paper we prove that, having the blocker of a near-ideal matrix, only a few very easy conditions have to be checked in order to decide if the matrix is regular mni. In doing so, we define the class of quasi mni matrices, containing regular mni matrices, and we find a generalization on the number of integer extreme points adjacent to the fractional extreme point in the covering polyhedron. We also give a relationship between the covering and stability number of regular mni matrices which allows to prove when a regular mni matrix can be a proper minor of a quasi mni. Partially supported by CONICET Grant PIP 2807/2000 (Argentina) and by CNPq/PROSUL Grant 490333/2004-4 (Brasil).     

Lead Sensor Using Gold Nanostructured Screen‐Printed Carbon Electrodes as Transducers

Gold nanostructured screen‐printed carbon electrodes are demonstrated to be suitable transducers for the determination of lead using square‐wave voltammetry. Reproducible gold nanostructures have been obtained by direct electrochemical deposition. A calibration plot from 2.5 to 250 μg/L was obtained in acidic solutions of Pb(II) with a reproducibility of 4% (n=10). The detection limit was 0.09 μg/L of lead. The method is then applied to perform a blood lead analysis by adjusting square‐wave parameters in capillary or venous blood with a minimum sample pretreatment and excellent accuracy and reproducibility.     

1,6‐ and 1,7‐naphthyridines III. 13C‐NMR analysis of some hydroxy derivatives

The ¹³C‐NMR spectra of some 1,6‐naphthyridines 2 and 1,7‐naphthyridines 3 , as well as those of N‐methyl derivatives 4 and 5 , were recorded and analyzed. Results in dimethyl‐d₆ sulfoxide and deuteriochlo‐roform provide useful data on intra and intermolecular hydrogen bonds.     

Shifting the Superparamagnetic Limit of Nanosized Copper Iron Spinel

In this paper we analyze trend of EFG values measured at Cd impurity in a group of semiconducting delafossites with chemical formula CuBO₂ (B = Al, Fe, Cr, Nd). We conclude that this trend reveals one of the most subtle details in electronic spectrum of the compounds: if impurity states are formed within or out of the band gap. In CuAlO₂ and CuFeO₂ the Cd EFG exhibits larger value than in CuCrO₂ and CuNdO₂, when Cd substitutes the Cu atom. This occurs because in the first two compounds the Cd forms shallow band within the gap, and in the second two compounds does not. When Cd occupies the B position it exhibits almost the same EFG in all delafossites. In this case, Cd does not form its states within the gap in none of the compounds. To arrive to these conclusions we analyzed and calculated various systems (Cd-doped CuAlO₂ and CuCrO₂ compounds, fictitious molecules), using the FP-LAPW method.     

Elucidating a particulate matter deposition episode by combining scanning electron microscopy and X-ray fluorescence spectrometry.

Multielemental composition and morphology of particulate matter samples were examined to detect the presence of two potential responsible pollutant emitters at four sites impacted during a pollution episode in the City of Campana, Argentina. Coke and smoke black are the main constituents associated to the industrial plants that were considered, a priori, as responsible pollutant emitters. Wavelength dispersive X-ray fluorescence (WDXRF) was employed for the analysis of metals in samples coming from both, suspected sources and four sites. On the basis of multielemental composition profiles, a screening analysis was undertaken for exploring similarities among sources and sample sites adopting the average concentration profile of the crustal rock as soil surrogate. Particle morphology was studied by scanning electron microscopy (SEM) in source samples and in those environmental samples selected through the screening analysis. Two types of collected samples were analyzed: 1) those with composition profiles closer to the potential sources and 2) those closer to the cluster rock. This strategy was adequate to identify the responsible source of the contamination episode.