Screening and confirmation of PAHs in vegetable oil samples by use of supercritical fluid extraction in conjunction with liquid chromatography and fluorimetric detection

A fast, simple, non-destructive method for the direct screening of polycyclic aromatic hydrocarbons (PAHs) in vegetable oil samples is proposed. The method uses a supercritical fluid extraction (SFE) system coupled on-line with a fluorimetric detector to determine PAHs. This special assembly avoids the main problems encountered in the determination of PAHs in complex matrices such as vegetable oils. PAHs are selectively extracted by using silica gel in the thimble and cleaned up by passage through a C18 column. Interferences are preferentially retained by the silica gel during the SFE process while PAHs are adsorbed in the C18 column and the remainder of the matrix is sent to waste. Finally, the C18 column is purged to remove residual CO2 gas and adsorbed PAHs are recovered by desorption with a solvent. The extracts from positive samples are subsequently analyzed by liquid chromatography (LC) with fluorescence detection. The proposed method allows the confirmation of vegetable oil safety and hence provides a new tool for consumer protection. (C) 2004 Elsevier B.V. All rights reserved.

Composting of urban solid residues (USR) by different dispositions - Kinetics of thermal decomposition

The thermal behavior and non-isothermal kinetics of thermal decomposition of three different kinds of composting of the USR like: stack with drilled PVC tubes (ST), revolved stack (SR) and stack with material of structure (SM), from the usine of composing of Araraquara city, São Paulo state, Brazil, within a period of 132 days of composting were studied.Results from TG, DTG and DSC curves obtained on inert atmosphere indicated that the cellulosic fraction present, despite the slow degradation during the composting process, is thermally less stable than other substances originated from that process. Due to that behavior, the cellulosic fraction decomposition could be kinetically evaluated through non-isothermal methods of analysis.The values obtained were: average activation energy, E-a=248, 257 and 259 kJ mol(-1) and pre-exponential factor, logA=21.4, 22.5, 22.7 min(-1), to the ST, SR and SM, respectively.From E-a and logA values and DSC curves, Malek procedure could be applied, suggesting that the SB (Sestak-Berggren) kinetic model is the appropriated one to the first thermal decomposition step.

The investigation of alpha -> beta phase transition in poly(vinylidene fluoride) (PVDF)

The phase transition from the non-polar a-phase to the polar beta-phase of poly(vinylidene fluoride) (PVDF) has been investigated using micro-Raman spectroscopy, which is advantageous for being a non-destructive technique. Films of alpha-PVDF were subjected to stretching under controlled rates and at 80 degrees C, the transition to beta-PVDF being monitored by the decrease in the Raman band at 794 cm(-1) characteristic of the a-phase, with the concomitant increase in the 839 cm(-1) band characteristic of the beta-phase. Poling with negative corona discharge was found to affect the alpha-PVDF morphology improving the Raman bands related to this crystalline phase. This effect is minimized for films stretched to higher ratios. Significantly, corona-induced effects could not be observed with the other experimental techniques, viz. X-ray diffraction and infrared spectroscopy.

Kinetic of thermal decomposition of residues from different kinds of composting

Non-isothermal kinetic parameters regarding to the thermal decomposition of the ligninocellulosic fraction present in compost from urban solid residues (USR) obtained through stack covered (SC) with composted material, comes from the usine in composing of Araraquara city, São Paulo state, Brazil, and from stack containing academic restaurant organic solid residues (SAR). The samples were periodically revolved round 132 days of composting.Results from TG, DTG and DSC curves obtained on inert atmosphere indicated that the lignocellulosic fraction present, despite the slow degradation during the composting process, is thermally less stable than other substances originated during that process. The lignocellulosic fraction decomposition, between 200 and 400degreesC, were kinetically evaluated through non-isothermal methods of analysis.By using the Flynn-Wall and Ozawa isoconversional method, the medium activation energy, E-a, and pre-exponential factor, IgA, were 283.0+/-4.6, 257.6+/-1.3 U mol(-1) and 25.4+/-0.8, 23.2+/-0.2 min(-1),to the SC and SAR, respectively, at 95% confidence level.From E-a, and IgA values and DSC curves, Malek procedure could be applied, Suggesting that the SB (Sestik-Berggren) kinetic model is suitable for the first thermal decomposition step.

Electrochemical noise analysis of bioleaching of bornite (Cu5FeS4) by Acidithiobacillus ferrooxidans

Electrochemical noise (EN) is a generic term describing the phenomenon of spontaneous fluctuations of potential or current noise of electrochemical systems. Since this technique provides a non-destructive condition for investigating corrosion processes, it can be useful to study the electrochemical oxidation of mineral sulfides by microorganisms, a process known as bacterial leaching of metals. This technique was utilized to investigate the dissolution of a bornite electrode in the absence (first 79 h) and after the addition of Acidithiobacillus ferrooxidans (next 113 h) in salts mineral medium at pH 1.8, without addition of the energy source (Fe2+ ions) for this chemolithotrophic bacterium. Potential and current noise data have been determined simultaneously with two identical working bornite electrodes which were linked by a zero resistance ammeter (ZRA). The mean potential, E-coup, coupling current, I-coup, standard deviations of potential and current noise fluctuations and noise resistance, R-n, have been obtained for coupled bornite electrodes. Noise measurements were recorded twice a day in an unstirred solution at 30 degrees C. Significant changes in these parameters were observed when the A. ferrooxidans suspension was added, related with bacterial activity on reduced species present in the sulfide moisture (Fe2+, S2-). ENA was a suitable tool for monitoring the changes of the corrosion behavior of bornite due to the presence of bacterium. (C) 2006 Elsevier B.V. All rights reserved.

Advances in phase-stepping real-time holography using photorefractive sillenite crystals

This work presents a review of recent developments in phase-stepping real-time holographic interferometry with photorefractive sillenite crystals. Quantitative results are shown in micro-rotation, micro-displacement, and micro-deformation measurements, and in wave-optics and surface analysis as well. The phase stepping was carried out in a four-frame process and the resulting phase map was unwrapped by applying a sin/cos filter. The experimental results are in good agreement with the ones obtained through other means, showing the promising potentialities of phase-stepping real-time holographic interferometry for in situ visualisation, monitoring and analysis in non-destructive testing.

Application of impedance spectroscopy to evaluate the effect of different setting accelerators on the developed microstructures of calcium phosphate cements

The main goal of the present study was to evaluate the effect of different setting accelerator agents on the developed microstructures of calcium phosphate cements (CPCs) by employing the impedance spectroscopy (IS) technique. Six compositions of CPCs were prepared from mixtures of commercial dicalcium phosphate anhydrous (DCPA) and synthesized tetracalcium phosphate (TTCP) as the solid phases. Two TTCP/DCPA molar ratios (1/1 and 1/2) and three liquid phases (aqueous solutions of Na(2)HPO(4), tartaric acid (TA) and oxalic acid (OA), 5% volume fraction) were employed. Initial (I) and final (F) setting times of the cement pastes were determined with Gillmore needles (ASTM standard C266-99). The hardened samples were characterized by X-ray powder diffraction (XRD), Fourier transformed infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and apparent density measurements. The IS technique was employed as a non-destructive tool to obtain information related to porosity, tortuosity and homogeneity of the cement microstructures. The formulation prepared from a TTCP/DCPA equimolar mixture and OA as the liquid phase presented the shortest I and F (12 and 20 min, respectively) in comparison to the other studied systems. XRD analyses revealed the formation of low-crystallinity hydroxyapatite (HA) (as the main phase) as well as the presence of little amounts of unreacted DCPA and TTCP after 24 h hardening in 100% relative humidity. This was related to the proposed mechanisms of dissolution of the reactants. The bands observed by FTIR allowed identifying the presence of calcium tartrate and calcium oxalate in the samples prepared from TA and OA, in addition to the characteristic bands of HA. High degree of entanglement of the formed crystals was observed by SEM in samples containing OA. SEM images were also correlated to the apparent densities of the hardened cements. Changes in porosity, tortuosity and microstructural homogeneity were determined in all samples, from IS results, when the TTCP/DCPA ratio was changed from 1/1 to 1/2. The cement formulated from an equimolar mixture of TTCP/DCPA and OA as the liquid phase presented setting times, degree of conversion to low-crystallinity HA and microstructural features suitable to be used as potential bone cement in clinical applications. The IS technique was shown to be a very sensitive and non-destructive tool to relate the paste composition to the developed microstructures. This approach could be very useful to develop calcium phosphate bone cements for specific clinical demands.

Confinement, solitons and the equivalence between the sine-Gordon and massive Thirring models

We consider a two-dimensional integrable and conformally invariant field theory possessing two Dirac spinors and three scalar fields. The interaction couples bilinear terms in the spinors to exponentials of the scalars. Its integrability properties are based on the sl(2) affine Kac-Moody algebra, and it is a simple example of the so-called conformal affine Toda theories coupled to matter fields. We show, using bosonization techniques, that the classical equivalence between a U(1) Noether current and the topological current holds true at the quantum level, and then leads to a bag model like mechanism for the confinement of the spinor fields inside the solitons. By bosonizing the spinors we show that the theory decouples into a sine-Gordon model and free scalars. We construct the two-soliton solutions and show that their interactions lead to the same time delays as those for the sine-Gordon solitons. The model provides a good laboratory to test duality ideas in the context of the equivalence between the sine-Gordon and Thirring theories. © 2000 Elsevier Science B.V. All rights reserved.

Anatomical and biochemical characterization of the calcium effect on eucalyptus urophylla callus morphogenesis in vitro

Calcium chloride concentrations from 0.0 to 12.12 mM were added to the culture medium and calcium content in calluses were determined directly by X-ray fluorescence spectrometry, a non-destructive method, allowing the processing of the same tissue for histological analysis. A multivariate statistical analysis (PCA - Principal Components Analysis) grouped the treatments into 5 blocks and indicated the most responsive group. Lack of calcium supply caused a complete absence of a morphogenic process and tissue collapse. An increase in calcium concentration gave higher total protein and sugar contents, an increase in peroxidase specific activity and changes in the histological characteristics. It was possible to verify that calcium stimulated globular somatic embryo formation at concentration of 6.62 mM.

Steel bars identification in reinforced concrete structures by using ANN and magnetic fields

This work proposes a methodology for non destructive testing (NDT) of reinforced concrete structures, using superficial magnetic fields and artificial neural networks, in order to identify the size and position of steel bars, embedded into the concrete. For the purposes of this paper, magnetic induction curves were obtained by using a finite element program. Perceptron Multilayered (PML) ANNs, with Levemberg-Marquardt training algorithm were used. The results presented very good agreement with the expect ones, encouraging the development of real systems based upon the proposed methodology.

The investigation of α→β phase transition in poly(vinylidene fluoride) (PVDF)

The phase transition from the non-polar α-phase to the polar β-phase of poly(vinylidene fluoride) (PVDF) has been investigated using micro-Raman spectroscopy, which is advantageous for being a non-destructive technique. Films of α-PVDF were subjected to stretching under controlled rates and at 80°C, the transition to β-PVDF being monitored by the decrease in the Raman band at 794 cm-1 characteristic of the α-phase, with the concomitant increase in the 839 cm-1 band characteristic of the β-phase. Poling with negative corona discharge was found to affect the a-PVDF morphology improving the Raman bands related to this crystalline phase. This effect is minimized for films stretched to higher ratios. Significantly, corona-induced effects could not be observed with the other experimental techniques, viz. X-ray diffraction and infrared spectroscopy.

A simple protocol for a low invasive DNA accessing in Stenella longirostris (Cetacea: Delphinidae)

The most significant studies about the spinner dolphin (Stenella longirostris) in the Southwestern Atlantic Ocean were conducted in Fernando de Noronha Archipelago, off Northeastern Brazil. The continuity of these studies depends upon the development of non-invasive methods. In this work, we present results from the skin swabbing sampling procedure for this species. We tested the performance of this method for nuclear and mitochondrial DNA analysis, unknown for this population. A total of skin 161 samples were collected during two expeditions. After the contacts the most of the dolphins remained close to the boat. Microsatellites markers and cytochrome b region primers were evaluated and the respective fragments were successfully amplified. Thus, skin swabbing may be considered an efficient strategy to obtain tissue samples for spinner dolphin genetic analysis in Fernando de Noronha Archipelago.

Piezoelectric composite film for acoustic emission detection

The continuous technological advances require materials with properties that conventional material cannot display. Material property combinations are being the focus to the development of composite materials, which are considered a multiphase material that exhibits properties of the constituent phases. One interesting material to be studied as sensing material is the composite made of ferroelectric ceramic and polymeric matrix as a two-phases composite material. In that case, the combinations properties intended are the high piezo and pyroelectric activities of the dense ceramic with the impact resistance, flexibility, formability and low densities of the polymer. Using the piezoelectric property of the composite film, it can be used to detect acoustic emission (AE), which is a transient elastic wave generated by sudden deformation in materials under stress. AE can be applied for evaluating the health of structures in a nondestructive way and without any lapse of time. The preliminary result indicates that the composite Pz34/PEEK can be used as sensing material for nondestructive evaluation. ©2009 IEEE.

Digital radiography for the inspection of weld seams of pipelines - better sensitivity

Conventional radiography, using industrial radiographic films, has its days numbered. Digital radiography, recently, has taken its place in various segments of products and services, such as medicine, aerospace, security, automotive, etc. As well as the technological trend, the digital technique has brought proven benefits in terms of productivity, sensitivity, the environment, tools for image treatment, cost reductions, etc. If the weld to be inspected is on a serried product, such as, for example, a pipe, the best option for the use of digital radiography is the plane detector, since its use can reduce the length of the inspection cycle due to its high degree of automation. This work tested welded joints produced with the submerged arc process, which were specially prepared in such a way that it shows small artificial cracks, which served as the basis forcomparing the sensitivity levels of the techniques involved. After carrying out the various experiments, the digital meth odshowed the highest sensitivity for the image quality indicator (IQI) of the wire and also in terms of detecting small discontinuities, indicating that the use of digital radiography using the plane detector had advantages over the conventional technique (Moreira et al. Digital radiography, the use of plane detectors for the inspection of welds in oil pipes and gas pipes.9th COTEQ and XXV National Testing Congress for Non Destructive Testing and Inspection; Salvador, Bahia, Brazil and Bavendiek et al. New digital radiography procedure exceeds film sensitivity considerably in aerospace applications. ECNDT; 2006; Berlin). The works were carried out on the basis of the specifications for oil and gas pipelines, API 5L 2004 edition (American Petroleum Institute. API 5L: specification for line pipe. 4th ed. p. 155; 2004) and ISO 3183 2007 edition (International Organization for Standardization, ISO 3183. Petroleum and gas industries - steel pipes for pi pelines transportation systems. p. 143; 2007). © 2010 Taylor & Francis.

Identification of steel bars immersed in reinforced concrete based on experimental results of eddy current testing and artificial neural network analysis

This paper presents an experimental research on the use of eddy current testing (ECT) and artificial neural networks (ANNs) in order to identify the gauge and position of steel bars immersed in concrete structures. The paper presents details of the ECT probe and concrete specimens constructed for the tests, and a study about the influence of the concrete on the values of measured voltages. After this, new measurements were done with a greater number of specimens, simulating a field condition and the results were used to generate training and validation vectors for multilayer perceptron ANNs. The results show a high percentage of correct identification with respect to both, the gauge of the bar and of the thickness of the concrete cover. © 2013 Copyright Taylor and Francis Group, LLC.