A potentiometric study on the complex equilibria between nickel(II) and 2-mercapto-2-phenylacetic acid

Complex formation between nickel(II) and 2-mercapto-2-phenylacetic acid (H₂MPA) has been studied at 25°C and 1 mol dm^?3 ClO₄^? in     

Spectrophotometric and potentiometric determination of the protonation constants of dithiocarbazates and studies on some of their metallic chelates

The protonation constants of 2-methyldithiocarbazate, 3,3-dimethyldithiocarbazate and 3-methyl-3-phenyldithiocarbazate, have been determined potentiometrically (I = 1.00M) and spectrophotometrically (I = 0.01M) at 25 degrees in aqueous solution. The analytical properties of the reagents have been studied, and also the compositions of some of their insoluble metallic chelates.     

The nitrosation of Amino Acids

With a view to clarifying analogies and differences between the mechanisms involved in the nitrosation of amino acids and secondary amines, we studied the kinetics of the nitrosation of five imino acids (azetidine-2-carboxylic acid, pyrrolidine-2-carboxylic acid, piperidine-2-carboxylic acid, piperidine-3-carboxylic acid, and piperidine-4-carboxylic acid) and of the ethyl esters of three of them. Reaction kinetics were determined by the initial rate method, by spectrophotometric monitoring of the concentration of nitroso amino acid formed. The presence of the ? COO^? group in the amino acids opens a new mechanistic route for the nitrosation of the secondary amino group: a nitrosyl carboxylate formed initially acts as an internal nitrosating agent, resulting in intramolecular migration of ? N ? O from the carboxylate group to the secondary amino group. The observed order of the α?, β?, and γ-amino acids as regards the ease of N-nitrosation by this route is explained in terms of the relative energies of (a) the equatorial and axial orientations of the C_ring? C_carboxyl bond, and (b) the chair and boat forms of the piperidine ring. © 1994 John Wiley & Sons, Inc.     

Incidence of element distribution on the ultrasonic field of segmented annular arrays

Segmented annular arrays are sometimes used for 3D ultrasonic imaging. However, owing to their geometrical complexity, the acoustic field generated by this type of aperture has not been adequately described. In this work, a method based on the array factor approach is used to describe the field radiated by sector annular arrays. This approach allows one to analyse the influence on the field of several aperture parameters, such as the number of elements per annulus, size and spatial distribution of elements, etc. In addition, strategies to reduce grating lobes are presented.     

Porosity estimation of concrete by ultrasonic NDE

The increasing number of concrete structures with symptoms of premature deterioration due to environmental action demands procedures to estimate the durability of this type of component. Concrete durability is related to porosity, which determines the intensity of interactions of the material with aggressive agents. The pores and capillaries inside the structure facilitate the destructive processes that generally begin in the surface. In this work, an ultrasonic NDE technique to estimate the porosity of concrete is developed. The method is based on the analysis of the mechanical behaviour of mortar probes built with calibrated sand, in which the concentration of water-cement mixture has been varied. In this sense, data of sound velocity are correlated with data of porosity, which have been previously measured by destructive measurements.     

Signal-to-noise ratio enhancement based on the whitening transformation of colored structural noise

In the ultrasonic testing and evaluation of highly scattering materials (i.e. non-homogeneous media such as composites, layered and clad materials) structural noise is an important limitation to the visibility of flaw echoes. This noise cannot be reduced by conventional linear filtering or by time-averaging techniques. In order to enhance the defect-to-background noise ratio (SNR), many different algorithms have been developed over the years. This work analyzes three new strategies for SNR enhancement based on the whitening transformation of the colored structural noise. By using this transformation, the small spectral differences between noise and flaw echoes are exploited, thereby allowing an improvement in the visibility of the flaw.     

Time‐resolved photoelectron spectroscopy using synchrotron radiation time structure

Synchrotron radiation time structure is becoming a common tool for studying dynamic properties of materials. The main limitation is often the wide time domain the user would like to access with pump–probe experiments. In order to perform photoelectron spectroscopy experiments over time scales from milliseconds to picoseconds it is mandatory to measure the time at which each measured photoelectron was created. For this reason the usual CCD camera‐based two‐dimensional detection of electron energy analyzers has been replaced by a new delay‐line detector adapted to the time structure of the SOLEIL synchrotron radiation source. The new two‐dimensional delay‐line detector has a time resolution of 5 ns and was installed on a Scienta SES 2002 electron energy analyzer. The first application has been to characterize the time of flight of the photoemitted electrons as a function of their kinetic energy and the selected pass energy. By repeating the experiment as a function of the available pass energy and of the kinetic energy, a complete characterization of the analyzer behaviour in the time domain has been obtained. Even for kinetic energies as low as 10 eV at 2 eV pass energy, the time spread of the detected electrons is lower than 140 ns. These results and the time structure of the SOLEIL filling modes assure the possibility of performing pump–probe photoelectron spectroscopy experiments with the time resolution given by the SOLEIL pulse width, the best performance of the beamline and of the experimental station.     

Silicon-based rectangular hollow integrated waveguides

This paper describes the simulation, fabrication and characterization of silicon-based rectangular hollow waveguides. Numerical evaluation of such structures has been done using both modal propagation and ray tracing, low total losses and multimodal behavior, even for small core sizes, are predicted. Since light propagation in rectangular hollow waveguides strongly depends on the Fresnel coefficients at the facets, the technological processes have been optimized to obtain wall angles close to 89° and wall and base average roughness of 57 nm and <5 nm, respectively. Hence, roughness is negligible to the working wavelength (678 nm). Measured waveguides show total losses close to 6.0 dB for 3.0 cm length. The non-lineal response due to mode filtering in hollow waveguides has also been experimentally observed. Finally, loss simulations and measurements are in agreement, especially for the widest waveguides. For thinner structures, the reduction of the depth due to the DRIE process, together with the blundering of the vertices, causes a dramatic attenuation increase. All these effects should be taken into consideration when defining hollow structures.     

Raman spectroscopy in the diagnosis of the wall painting History of Concepción,Chile

Pigments and fresco‐related materials from the wall painting Historia de Concepción by Gregorio De La Fuente in Concepción, Chile were identified by Raman microscopy. The pigments were compared with those obtained from the artist's studio, and results allowed inference about subsequent interventions. Materials coming from processes such as salt efflorescence were also studied. The results contribute to the diagnosis of the current conservation state of the wall painting for its future restoration. Copyright © 2011 John Wiley & Sons, Ltd.