Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

An analytical methodology based on headspace solid phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography—time-of-flight mass spectrometry (GC × GC–ToFMS) was developed for the identification and quantification of the toxic contaminant ethyl carbamate (EC) directly in fortified wines. The method performance was assessed for dry/medium dry and sweet/medium sweet model wines, and for quantification purposes, calibration plots were performed for both matrices using the ion extraction chromatography (IEC) mode (m/z 62). Good linearity was obtained with a regression coefficient (r2) higher than 0.981. A good precision was attained (R.S.D. <20%) and low detection limits (LOD) were achieved for dry (4.31 μg/L) and sweet (2.75 μg/L) model wines. The quantification limits (LOQ) and recovery for dry wines were 14.38 μg/L and 88.6%, whereas for sweet wines were 9.16 μg/L and 99.4%, respectively. The higher performance was attainted with sweet model wine, as increasing of glucose content improves the volatile compound in headspace, and a better linearity, recovery and precision were achieved. The analytical methodology was applied to analyse 20 fortified Madeira wines including different types of wine (dry, medium dry, sweet, and medium sweet) obtained from several harvests in Madeira Island (Portugal). The EC levels ranged from 54.1 μg/L (medium dry) to 162.5 μg/L (medium sweet).

In-depth search focused on furans, lactones, volatile phenols, and acetals as potential age markers of Madeira wines by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction

The establishment of potential age markers of Madeira wine is of paramount significance as it may contribute to detect frauds and to ensure the authenticity of wine. Considering the chemical groups of furans, lactones, volatile phenols, and acetals, 103 volatile compounds were tentatively identified; among these, 71 have been reported for the first time in Madeira wines. The chemical groups that could be used as potential age markers were predominantly acetals, namely, diethoxymethane, 1,1-diethoxyethane, 1,1-diethoxy-2-methyl-propane, 1-(1-ethoxyethoxy)-pentane, trans-dioxane and 2-propyl-1,3-dioxolane, and from the other chemical groups, 5-methylfurfural and cis-oak-lactone, independently of the variety and the type of wine. GC × GC-ToFMS system offers a more useful approach to identify these compounds compared to previous studies using GC−qMS, due to the orthogonal systems, that reduce coelution, increase peak capacity and mass selectivity, contributing to the establishment of new potential Madeira wine age markers. Remarkable results were also obtained in terms of compound identification based on the organized structure of the peaks of structurally related compounds in the GC × GC peak apex plots. This information represents a valuable approach for future studies, as the ordered-structure principle can considerably help the establishment of the composition of samples. This new approach provides data that can be extended to determine age markers of other types of wines.

Lipid and energy contents in the bodies of queens of Atta sexdens rubropilosa Forel (Hymenoptera, Formicidae): pre-and post-nuptial flight

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Performance of aerodynamic baffles in cylindrical grinding analyzed on the basis of air layer pressure and speed

Over the years, grinding has been considered one of the most important manufacturing processes. Grinding is a high precision process, and the loss of a single workpiece in this stage of the production is unacceptable, fir the value added to the material is very high due to many processes it has already undergone prior to grinding. This study aims to contribute toward the development of an experimental methodology whereby the pressure and speed of the air layer produced by the high rotation of the grinding wheel is evaluated with and without baffles, i.e., in an optimized grinding operation and in a traditional one. Tests were also carried out with steel samples to check the difference in grinding wheel wear with and without the use of baffles.

Influence of the grinding wheel's dive speed on the damage of rectified hardened steels

The world tendency is the increase of the productivity and the production of pieces more and more sophisticated, with high degree of geometric and dimensional tolerances, with good surface finish and low cost. Rectification is responsible for the final finish in the machining process of a material. However, damages generated in this production phase affect all the resources used in the previous processes. Great part of the problems happennig in the rectification process is due to the enormous temperature generated in this activity because of the machining conditions. The dive speed, which is directly related to the productivity, is considered responsible for the damages that occur during rectification, limiting its values to those that do not cause such damages. In this work, through the variation of the dive speed in the process of cylindrical grinding of type ABNT D6 steel, rationalizing the application of two cutting fluids and using a CBN (cubic boron nitrate) abrasive wheel with vitrified blond, the influence of the dive speed on the surface damages of hardened steels was evaluated. The results allowed to say that the dive speed, associated to an efficient cooling and lubrication, didn't provoke thermal damages (including heated zones, cracks and tension stresses) to the material. Residual stresses and the roughness of rectified materials presented a correlation with the machining conditions. The work concluded that it is possible to increase the productivity without provoking damages in the rectified components.

Influence of belt speed, grit sizes and pressure on the sanding of Eucalyptus grandis wood

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

Power performance evaluation of an electric home fan with triac-based automatic speed control system

In order to provide a low cost system of thermal comfort, a common model of home fan, 40 cm diameter size, had its manual four-button control system replaced by an automatic speed control. The new control system has a temperature sensor feeding a microcontroller that, by using an optic coupling, DIAC or TRIAC-based circuit, varies the RMS value of the fan motor input voltage and its speed, according to the room temperature. Over a wide range of velocity, the fan net power and the motor fan input power were measured working under both control system. The temperature of the motor stator and the voltage waveforms were observed too. Measured values analysis showed that the TRIAC-based control system makes the fan motor work at a very low power factor and efficiency values. The worst case is at low velocity range where the higher fan motor stator temperatures were registered. The poor power factor and efficiency and the harmonics signals inserted in the motor input voltage wave by the TRIAC commutation procedure are correlated.

Positive leader characteristics from high-speed video observations

Based on analyses of high-speed video recordings of cloud-to-ground lightning in Brazil and the USA, the characteristics of positive cloud-to-ground (+CG) leaders are presented. The high frame rates permitted the average, 2-dimensional speeds of development along the paths of the channels to be resolved with good accuracy. The values range from 0.3 to 6.0 x 10(5) ms(-1) with a mean of 2.7 x 10(5) ms(-1). Contrary to what is usually assumed, downward +CG leader speeds are similar to downward -CG leader speeds. Our observations also show that the speeds tend to increase by a factor of 1.1 to 6.5 as they approach the ground. The presence of short duration, recoil leaders (RLs) during the development of positive leaders reveal a highly branched structure that is not usually recorded when using conventional photographic and video cameras. The existence of the RLs may help to explain observations of UHF-VHF radiation during the development of +CG flashes.

Considerations on corrosion and weld repair effects on the fatigue strength of a steel structure critical to the flight-safety

The aim of this study is to analyze the effects of corrosion and successive tungsten inert gas (TIC) welding repairs on the reverse bending fatigue strength of AISI 4130 steel used in components critical to the flight-safety. The tests were performed on hot-rolled steel plate specimens, 1.10 mm and 1.60 mm thick, by means of a SCHENK PWS equipment, with load ratio R = -1, constant amplitude, 30 Hz frequency and room temperature. It was observed that the reverse bending fatigue strength of AISI 4130 steel decreases due to the corrosion and the TIC welding and re-welding processes. (C) 2010 Elsevier Ltd. All rights reserved.

Repair Welding Effects on the Bending Fatigue Strength of AISI 4130 Aeronautical Steel used in a Critical to the Flight-Safety Structure

The aim of this study was to analyze the effect of successive TIG (tungsten inert gas) welding repairs on the reverse bending fatigue strength of AISI 4130 steel, which is widely used in components critical to the flight-safety. In order to simulate the abrupt maneuvers, wind bursts, motor vibration and helixes efforts, which generate cyclic bending loadings at the welded joints of a specific aircraft component called motor cradle, experimental reverse bending fatigue tests were carried out on specimens made from hot-rolled steel plate, 1.10 mm (0.043 in) thick, by mean of a SCHENK PWS equipment, with load ratio R = -1, under constant amplitude, at 30 Hz frequency and room temperature. It was observed that the bending fatigue strength decreases after the TIG (Tungsten Inert Gas) welding process application on AISI 4130 steel, with subsequent decrease due to re-welding sequence as well. Microstructural analyses and microhardness measurements on the base material, heat-affected zone (HAZ) and weld metal, as well as the effects of the weld bead geometry on the obtained results, have complemented this study.

Considerations about the welding repair effects on the structural integrity of an airframe critical to the flight-safety

Structures critical to the flight-safety are commonly submitted to several maintenance repairs at the welded joints in order to prolong the in-service life of aircrafts. The aim of this study is to analyze the effects of Tungsten Inert Gas (TIG) welding repair on the structural integrity of the AISI 4130 aeronautical steel by means of experimental fatigue crack growth tests in base-material, heat-affected zone (HAZ) and weld metal. The tests were performed on hot-rolled steel plate specimens, 0.89 mm thick, with load ratio R = 0.1, constant amplitude, at 10 Hz frequency and room temperature. Increase of the fracture resistance was observed in the weld metal but decreasing in the HAZ after repair. The results were associated to microhardness and microstructural changes with the welding sequence. (C) 2010 Published by Elsevier Ltd.

A novel HPF voltage source rectifier for variable speed refrigeration systems

A novel single-phase voltage source rectifier capable to achieve High-Power-Factor (HPF) for variable speed refrigeration system application, is proposed in this paper. The proposed system is composed by a single-phase high-power-factor boost rectifier, with two cells in interleave connection, operating in critical conduction mode, and employing a soft-switching technique, controlled by a Field Programmable Gate Array (FPGA), associated with a conventional three-phase IGBT bridge inverter (VSI - Voltage Source Inverter), controlled by a Digital Signal Processor (DSP). The soft-switching technique for the input stage is based on zero-current-switching (ZCS) cells. The rectifier's features include the reduction in the input current ripple, the reduction in the output voltage ripple, the use of low stress devices, low volume for the EMI input filter, high input power factor (PF), and low total harmonic distortion (THD) in the input current, in compliance with the EEC61000-3-2 standards. The digital controller for the output stage has been developed using a conventional voltage-frequency control (scalar V/f control), and a simplified stator oriented Vector control, in order to verify the feasibility and performance of the proposed digital controls for continuous temperature control applied at a refrigerator prototype.

On the dynamic behaviour of the "click" mechanism in dipteran flight

In this paper, the dynamic behaviour of the "click" mechanism is analysed. A more accurate model is used than in the past, in which the limits of movement due to the geometry of the flight mechanism are imposed. Moreover, the effects of different damping models are investigated. In previous work, the damping model was assumed to be of the linear viscous type for simplicity, but it is likely that the damping due to drag forces is nonlinear. Accordingly, a model of damping in which the damping force is proportional to the square of the velocity is used, and the results are compared with the simpler model of linear viscous damping. Because of the complexity of the model an analytical approach is not possible so the problem has been cast in terms of non-dimensional variables and solved numerically. The peak kinetic energy of the wing root per energy input in one cycle is chosen to study the effectiveness of the "click" mechanism compared with a linear resonant mechanism. It is shown that, the "click" mechanism has distinct advantages when it is driven below its resonant frequency. When the damping is quadratic, there are some further advantages compared to when the damping is linear and viscous, provided that the amplitude of the excitation force is large enough to avoid the erratic behaviour of the mechanism that occurs for small forces. (C) 2011 Elsevier Ltd. All rights reserved.

Comparative Histopathological Analysis of Human Pulps after Class I Cavity Preparation with a High-Speed Air-Turbine Handpiece or Er:YAG Laser

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Application of preparative high-speed counter-current chromatography for the separation of flavonoids from the leaves of Byrsonima crassa Niedenzu (IK)

The methanolic extract of the leaves of the medicinal plant Byrsonima crassa (Malpighiaceae) contain flavonoids with antioxidant activity. They were separated in a preparative scale using high-speed counter-current chromatography. The optimum solvent system used was composed of a mixture of ethyl acetate-n-propanol-water (140:8:80 (v/v/v)) and led to a successful separation between monoglucosilated flavonoids (quercetin-3-O-alpha-L-arabinoside, quercetin-3-O-beta-D-galactoside) and the biflavonoid amentoflavone in only 3.5 h. The purities of quercetin-3-O-alpha-L-arabinoside (95 mg), quercetin-3-O-beta-D-galactoside (16 mg) and the biflavonoid amentoflavone (114 mg) were all isolated at purity over 95%. Identification was performed by H-1 NMR, C-13 NMR and UV analyses. (C) 2004 Published by Elsevier B.V.