Amperometric differential determination of ascorbic acid in beverages and vitamin C tablets using a flow cell containing an array of gold microelectrodes modified with palladium

A simple and attractive method for quantification of ascorbic acid (AA) in beers, soda, natural juices and commercial vitamin C tablets was achieved by combining Bow injection analysis and amperometric detection. An array of gold microelectrodes electrochemically modified by deposition of palladium was employed as working electrode which was almost unaffected by fouling effects. Ascorbic acid was quantified in beverages and vitamin tablets using amperometric differential measurements. This method is based on three steps involving the flow injection of: 1) the sample plus a standard addition of AA, 2) the pure sample, and 3) the enzymatically-treated sample. The enzymatic treatment was carried out with Cucumis sativus tissue, which is a rich source of ascorbate oxidase, at pH 7. The calibration plots for freshly prepared ascorbic acid standards were very linear in the concentration range of 0.18-1.8 mg L-1 with a relative standard deviation (RSD) < 1%, while for real samples the deviations were between 2.7% to 8.9%.

Laminar forced convection to a pseudoplastic fluid food in circular and annular ducts

In this manuscript we investigated experimentally the steady-state heat transfer to an important pseudoplastic fluid food, the soursop juice, flowing in laminar regime through circular and concentric annular ducts. The mean convection heat transfer coefficients, determined by measuring the bulk temperatures before and after the heating sections with constant temperatures of the tube walls, were used to correlate simple new empiric expressions to estimate the average Nusselt number in the thermal entrance of the considered geometries. In addition, the thermophysical properties of the tested fluid food, as well as the rheological behavior, being essential for the heat transfer analyses, were experimentally determined. (c) 2006 Elsevier Ltd. All rights reserved.

Validation of an immunoassay method for the determination of traces of carbaryl in vegetable and fruit extracts by liquid chromatography with photodiode array and mass spectrometric detection

A competitive enzyme-linked immunosorbent assay (ELISA) method for carbaryl quantitation in crop extracts was validated by liquid chromatography (LC) with diode array detection (DAD). For this purpose, six crops (banana, carrot, green bean, orange, peach and potato) were chosen for recovery and reproducibility studies. The general sample preparation included extraction with methanol followed by liquid-liquid partitioning and clean-up on Celite-charcoal adsorbent column of the vegetable extracts. ELISA samples consisted of a diluted LC extract in assay phosphate buffer (pH 7.5). The potential effect of methanol in these samples was evaluated. It was observed that a maximum content of 10% methanol present in the assay buffer could be tolerated without expressive losses in the ELISA performance. Under these conditions, a IC50 similar to 1.48 mu g l(-1) was obtained. A minimum matrix effect with a 1:50 dilution of the methanolic extracts in assay buffer was noticed, except for green bean samples that inhibited completely the assay. For the vegetable extracts, the ELISA sensitivities varied from 3.9 to 5.7 mu g l(-1), and good recoveries (82-96%) with R.S.D.s ranging from 5.7 to 12.1% were found. An excellent correlation between the LC-DAD and ELISA techniques was obtained. The confirmation of the carbaryl in less concentrated samples was achieved by LC-mass spectrometry interfaced with atmospheric pressure chemical ionisation. The [M + H](+)= 202 and [M + H-57](+)=145 ions, equivalent to the protonated molecular and l-naphthol ions, respectively, were used to carbaryl identification in these samples. (C) 1998 Elsevier B.V. B.V. All rights reserved.

Flow-through cell based on an array of gold microelectrodes obtained from modified integrated circuit chips

The construction of a flow-through cell incorporating an array of gold microelectrodes is described and its application to flow injection analysis with amperometric detection is presented, Simple modification of almost any conventional integrated circuit chip, used as an inexpensive source of pre-assembled gold micro-wires, leads to the rapid and successful preparation of arrays of 8-48 elements, the polymeric encapsulation material from the top face of the chip is removed by abrasion until the gold micro-mires (used to interconnect the silicon circuit to the external contact pins of the chip) are disrupted and their transversal (elliptical) sections become exposed. Once polished, the flat and smooth top surface of the gold microelectrode-array chip (MEAC) is provided with a spacer and fitted under pressure against an acrylic block with the reference and auxiliary electrodes, to form the electrochemical (thin-layer) flow cell, while the contact pins are plugged into a standard IC socket, This design ensures autonomous electric contact with each electrode and allows fast dismantling for polishing or substitution, the performance of flow cells with MEACs was investigated utilizing the technique of reverse pulse amperometry without oxygen removal, A method was established for the determination of the copper concentration in sugar cane spirit, regulated by law for beverages, Samples from industrial producers and small-scale (alembic) brewers were compared, With a 24 MEAC, a detection limit of 30 mu g I-l of copper (4.7 x 10(-7) mol l(-1) of Cu-II for 100 mu l injections) was calculated, Routine operation was established at a frequency of 60-90 determinations per hour, Intercomparison with atomic absorption spectrometric determinations resulted in excellent agreement.

Determination of rice herbicides, their transformation products and clofibric acid using on-line solid-phase extraction followed by liquid chromatography with diode array and atmospheric pressure chemical ionization mass spectrometric detection

A simultaneous method for the trace determination of acidic, neutral herbicides and their transformation products in estuarine waters has been developed through an on-line solid-phase extraction method followed by liquid chromatography with diode array and mass spectrometric detection. An atmospheric pressure chemical ionization (APCI) interface was used in the negative ionization mode after optimization of the main APCI parameters. Limits of detection ranged from 0.1 to 0.02 ng/ml for 50 mi of acidified estuarine waters preconcentrated into polymeric precolumns and using time-scheduled selected ion monitoring mode. Two degradation products of the acidic herbicides (4-chloro-2-methylphenol and 2,4-dichlorophenol) did not show good signal response using APCI-MS at the concentration studied due to the higher fragmentor voltage needed for their determination For molinate and the major degradation product of propanil, 3,4-dichloroaniline, positive ion mode was needed for APCI-MS detection. The proposed method was applied to the determination of herbicides in drainage waters from rice fields of the Delta del Ebro (Spain). During the S-month monitoring of the herbicides, 8-hydroxybentazone and 4-chloro-2-methylphenoxyacetic acid were successively found in those samples. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Fluctuations of doublet splittings using the annular billiard

We study the statistical distribution of quantum energy splittings due to a dynamical tunneling. The system. The annular billiard, has whispering quasimodes due to a discrete symmetry that exists even when chaos is present in the underlying classical dynamics. Symmetric and antisymmetric combinations of these quasimodes correspond to quantum doublet states whose degeneracies decrease as the circles become more eccentric. We construct numerical ensembles composed of splittings for two distinct regimes, one which we call semiclassical for high quantum numbers and high energies where the whispering regions are connected by chaos, and other which we call quantal for low quantum numbers, low energies, and near integrable where dynamical tunneling is not a dominant mechanism. In both cases we observe a variation on the fluctuation amplitudes, but their mean behaviors follow the formula of Leyvraz and Ullmo [J. Phys. A 29, 2529 (1996)]. A description of a three-level collision involving a doublet and a singlet is also provided through a numerical example.

Damage Characterization Using Guided-Wave Linear Arrays and Image Compounding Techniques

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Dinuclear Azide-Bridged Copper(II) Complex as Building Block for the Assembly of a 2D-Supramolecular Array

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Controlled growth of anodic aluminium oxide films with hexagonal array of nanometer-sized pores filled with textured copper nanowires

Anodic aluminium oxide (AAO) films exhibiting a homogeneous morphology of parallel pores perpendicular to the surface were prepared in a two-step anodization process and filled with copper by electrochemical deposition. The optimum growth conditions for the formation of freestanding AAO films with hexagonal compact array of cylindrical pores were studied by field emission scanning electron microscopy and small angle X-ray scattering. The results show well-defined periodic structures with uniform pores size distribution for films with pore diameters between 40 and 70 nm prepared using different voltages and temperatures during the second anodization step. X-ray photoelectron spectroscopy and X-ray diffraction analysis of AAO films filled with copper show the formation of nanowires with high structural order, exhibiting a preferential crystalline orientation along the (2 2 0) axis and only small fraction of copper oxides. The best results for textured Cu nanowires were obtained at a reduction potential of -300 mV. (C) 2009 Elsevier Ltd. All rights reserved.

Array of Bose-Einstein condensates under time-periodic Feshbach-resonance management

The investigation of the dynamics of a discrete soliton in an array of Bose-Einstein condensates under the action of a periodically time-modulated atomic scattering length [Feshbach-resonance management (FRM)] was discussed. The slow and rapid modulations, in comparison with the tunneling frequency were considered. An averaged equation, which was a generalized discrete nonlinear Schrödinger equation, including higher-order effective nonlinearities and intersite nonlinear interactions was derived in the case of the rapid modulation. It was demonstrated that the modulations of sufficient strength results in splitting of the soliton by direct simulations.

Macromolecular array patterns of silk gland secretion in social Hymenoptera larvae

The cocoon, produced by most holometabolous insects, is built with silk that is usually produced by the larval salivary gland. Although this silk has been widely studied in the Lepidoptera, its composition and macromolecular arrangement remains unknown in the Hymenoptera. The macromolecular array patterns of the silk in the larval salivary gland of some meliponids, wasps, and ants were analyzed with polarized-light microscopy, and they were compared with those of Bombyx mori (Lepidoptera). There is a birefringent secretion in the glandular lumen of all larvae, due to filamentous structural proteins that display anisotropy. The silk in the distal, middle and proximal regions of the secretory portion of Formicidae and Vespidae glands presented a lattice optical pattern. We found a different pattern in the middle secretory portion of the Meliponini, with a zigzag rather than a lattice pattern. This indicates that the biopolymer fibers begin their macromolecular reorganization at this glandular region, different from the Formicidae and the Vespidae, in which the zigzag optical pattern was only found at the lateral duct. Probably, the mechanism of silk production in the Hymenoptera is a characteristic inherited from a common ancestor of Vespoidea and Sphecoidea; the alterations in the pattern observed in the Meliponini could be a derived characteristic in the Hymenoptera. We found no similarity in the macromolecular reorganization patterns of the silk between the Hymenoptera species and the silkworm.

Technique to combine images produced by different propagation modes of guided waves for damage detection and contrast improvement in plate-like structures

This paper describes an image compounding technique based on the use of different apodization functions, the evaluation of the signals phases and information from the interaction of different propagation modes of Lamb waves with defects for enhanced damage detection, resolution and contrast. A 16 elements linear array is attached to a 1 mm thickness isotropic aluminum plate with artificial defects. The array can excite the fundamental A0 and S0 modes at the frequencies of 100 kHz and 360 kHz, respectively. For each mode two synthetic aperture (SA) images with uniform and Blackman apodization and one image of Coherence Factor Map (CFM) are obtained. The specific interaction between each propagation mode and the defects and the characteristics of acoustic radiation patterns due to different apodization functions result in images with different resolution and contrast. From the phase information one of the SA images is selected at each pixel to compound the final image. The SA images are multiplied by the CFM image to improve contrast and for the dispersive A0 mode it is used a technique for dispersion compensation. There is a contrast improvement of 47.5 dB, reducing the dead zone and improving resolution and damage detection. © 2012 IEEE.

Sparse arrays and image compounding techniques for non-destructive testing using guided acoustic waves

Piezoelectric array transducers applications are becoming usual in the ultrasonic non-destructive testing area. However, the number of elements can increase the system complexity, due to the necessity of multichannel circuitry and to the large amount of data to be processed. Synthetic aperture techniques, where one or few transmission and reception channels are necessary, and the data are post-processed, can be used to reduce the system complexity. Another possibility is to use sparse arrays instead of a full-populated array. In sparse arrays, there is a smaller number of elements and the interelement spacing is larger than half wavelength. In this work, results of ultrasonic inspection of an aluminum plate with artificial defects using guided acoustic waves and sparse arrays are presented. Synthetic aperture techniques are used to obtain a set of images that are then processed with an image compounding technique, which was previously evaluated only with full-populated arrays, in order to increase the resolution and contrast of the images. The results with sparse arrays are equivalent to the ones obtained with full-populated arrays in terms of resolution. Although there is an 8 dB contrast reduction when using sparse arrays, defect detection is preserved and there is the advantage of a reduction in the number of transducer elements and data volume. © 2013 Brazilian Society for Automatics - SBA.

Genes candidatos a marcadores tumorais na progressão do adenocarcinoma de próstata indentificados por análise de HR-CGH e CGH-ARRAY

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Instantaneous Phase Threshold for Reflector Detection in Ultrasonic Images

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)