Liquid-liquid microextraction without phase separation in a multicommuted flow system for diltiazem determination in pharmaceuticals

Liquid-liquid microextraction without phase segmentation was implemented in a multicommuted flow system for determination of the anti-hypertensive diltiazem. The procedure was based on ion pair formation between the drug and the dye bromothymol blue at pH 3.5. The detection was performed without phase separation in a glass tube coupled to a fiber-optics spectrophotometer. The total volume of chloroform was reduced to 50 mu L in comparison with 10 mL consumed in batch. A linear response was observed between 9 and 120 mu mol L(-1), with a detection limit of 0.9 mu mol L(-1) (99.7% confidence level). The coefficient of variation (n = 10), sampling rate and extraction efficiency were estimated as 0.6%, 78 determinations per hour and 61%, respectively. About 30 mu g of bromothymol blue was consumed and the waste volume was 380 mu L per determination. The results for pharmaceutical samples agreed with those obtained by the reference procedure at the 95% confidence level. (C) 2011 Elsevier B.V. All rights reserved.

Investigating Giant (Gt) Repression in the Formation of Partially Overlapping Pair-Rule Stripes

Drosophila pair-rule genes are expressed in striped patterns with a precise order of overlap between stripes of different genes. We investigated the role of Giant (Gt) in the regulation of even-skipped, hairy, runt, and fushi tarazu stripes formed in the vicinity of Gt expression domains. In gt null embryos, specific stripes of eve, h, run, and ftz are disrupted. With an ectopic expression system, we verified that stripes affected in the mutant are also repressed. Simultaneously hybridizing gt misxpressing embryos with two pair-rule gene probes, we were able to distinguish differences in the repression of pairs of stripes that overlap extensively. Together, our results showed Gt repression roles in the regulation of two groups of partially overlapping stripes and that Gt morphogen activity is part of the mechanism responsible for the differential positioning of these stripes borders. We discuss the possibility that other factors regulate Gt stripe targets as well. Developmental Dynamics 239:2989-2999, 2010. (C) 2010 Wiley-Liss, Inc.

ECAP of Fe. Experiments and simulations of the in-elbow textures

The study of deformation properties of low carbon steels is of particular interest because of their many technological applications. Obtaining fine grained Fe based materials can be approached by one of the several available Severe Plastic Deformation (SPD) techniques. The current paper shows experimental data and simulations of the deformation process of iron samples by Equal Channel Angular Extrusion (ECAE). The samples were extruded in a 120 degrees channel die either by one or a few passes. The heterogeneity and local development of the deformation on the elbow of the channel has been studied by X-ray measuring and simulation of the texture evolution. The Self Consistent models used for simulation allowed the calculation of the spin of the main texture components which agreed pretty well with the experiments.

Characterization of nickel-niobium composite electrocoatings

The electrodeposition of nickel based composites is been performed in order to improve properties of nickel layers, such as hardness, wear resistance, lubrication, corrosion resistance and catalytic activity. In the present work Nb powders (20 mu m average size) and Ni were codeposited on 1020 carbon steel by galvanostatic electrolysis of Watts bath, using 10, 20 and 40 mA/cm(2) cathodic current density and 240, 400 and 550 rpm electrolyte stirring rate. The morphology and texture of the coatings, Nb incorporated volume fraction, microhardness, adhesion to the substrate and corrosion behavior were evaluated. The Ni-Nb composite layers presented a rough morphology with randomly oriented Ni grains, whereas pure Ni coatings were smooth and showed highly preferred orientation in the [110] or [100] direction. The volume fraction of Nb in the composites determined by image analysis ranged from 8.5 to 19%. The 400 rpm stirring rate led to the highest Nb content (16 to 19016) for all current densities investigated The microhardness of the composite layers was higher than that of pure Ni coatings due to refining of Ni grains induced by incoporation of Nb particles. The adhesion of the coatings estimated qualitatively by bend test was found satisfactory. The Ni-Nb composites presented lower corrosion rate than Ni coatings in both 3% NaCl and 20% H2SO4 solutions.

Compositional and textural properties of milkfat-soybean oil enzymatic interesterification

Milkfat-soybean oil blends were enzymatically interesterified (EIE) by Aspergillus niger lipase immobilized on SiO(2)-PVA hybrid composite in a solvent free system. An experimental mixture design was used to study the effects of binary blends of milkfat-soybean oil (MF:SBO) at different proportions (0:100; 25:75; 33:67; 50:50; 67:33; 75:25; 100:0) on the compositional and textural properties of the EIE products, considering, as response variables, the interesterification yield (IY), consistency and hardness. Lipase-catalysed interesterification reactions increased the relative proportion of TAGs` C(46)-C(52) and decreased the TAGs` C(40)-C(42) and C(54) concentrations. The highest IY was attained (10.8%) for EIE blend of MF:SBO 67:33 resulting in a more spreadable material at refrigerator temperature in comparison with butter, milkfat or non-interesterified (NIE) blend. In this case, consistency and hardness values were at least 32% lower than values measured for butter. Thus, using A. niger lipase immobilized on SiO(2)-PVA improves the textural properties of milkfat and has potential for development of a product incorporating unsaturated and essential fatty acids from soybean oil. (C) 2010 Elsevier Ltd. All rights reserved.

Magnetostriction of melt-spun Fe(85)Ga(15), Fe(78)Ni(7)Ga(15) and Fe(78)Co(7)Ga(15) stacked ribbon samples

A set of stacked ribbon samples with the compositions Fe(85)Ga(15), Fe(78)Ni(7)Ga(15) and Fe(78)Co(7)Ga(15) were prepared. XRD on these ribbons show that the binary Fe(85)Ga(15) ribbon exhibits the disordered A2 structure where as the addition of Co and Ni leads to the appearance of an additional ordered DO(3) structure. A comparison of the ratio of the XRD-line intensities gave strong evidence of a (100) texture perpendicular to the ribbon surface. The optical studied microstructure supports these results because it shows a columnar grain growth parallel to the solidification direction-which is parallel to ribbon thickness. The highest magnetostriction was found for Fe(78)Ni(7)Ga(15) (370 ppm), while the Fe(78)Co(7)Ga(15) a smaller magnetostriction of 270 ppm was found. The enhancement of the magnetostriction is attributed to the (100) texture in these ribbons. (C) 2009 Elsevier B.V. All rights reserved.

Microstructure and mechanical properties of laser-welded joints of TWIP and TRIP steels

With the aim of investigating a laser-welded dissimilar joint of TWIP and TRIP steel sheets, the microstructure was characterized by means of OM, SEM, and EBSD to differentiate the fusion zone, heat-affected zone, and the base material. OIM was used to differentiate between ferritic, bainitic, and martensitic structures. Compositions were measured by means of optical emission spectrometry and EDX to evaluate the effect of manganese segregation. Microhardness measurements and tensile tests were performed to evaluate the mechanical properties of the joint. Residual stresses and XRD phase quantification were used to characterize the weld. Grain coarsening and martensitic areas were found in the fusion zone, and they had significant effects on the mechanical properties of the weld. The heat-affected zone of the TRIP steel and the corresponding base material showed considerable differences in the microstructure and properties. (C) 2009 Elsevier B.V. All rights reserved.

HYBRID AND INCREMENTAL FUZZY LEARNING FOR HUMAN SKIN DETECTION

In this paper, a framework for detection of human skin in digital images is proposed. This framework is composed of a training phase and a detection phase. A skin class model is learned during the training phase by processing several training images in a hybrid and incremental fuzzy learning scheme. This scheme combines unsupervised-and supervised-learning: unsupervised, by fuzzy clustering, to obtain clusters of color groups from training images; and supervised to select groups that represent skin color. At the end of the training phase, aggregation operators are used to provide combinations of selected groups into a skin model. In the detection phase, the learned skin model is used to detect human skin in an efficient way. Experimental results show robust and accurate human skin detection performed by the proposed framework.

Assessment of the cavitation erosion resistance in high nitrogen austenitic stainless steels: study of the wear mechanisms

Specimens of a UNS S31803 steel were submitted to high temperature gas nitriding and then to vibratory pitting wear tests. Nitrided samples displayed fully austenitic microstructures and 0.9 wt. % nitrogen contents. Prior to pitting tests, sample texture was characterized by electron backscattering diffraction, EBSD. Later on, the samples were tested in a vibratory pit testing equipment using distilled water Pitting tests were periodically interrupted to evaluate mass loss and to characterize the surface wear by SEM observations. At earlier pit erosion, stages intense and highly heterogeneous plastic deformation inside individual grains was observed. Later on, after the incubation period, mass loss by debris detachment was observed. Initial debris micro fracturing was addressed to low cycle fatigue. Damage started at both sites, inside the grains and grain boundaries. The twin boundaries were the most prone to mass-loss incubation. Grains with (101) planes oriented near parallel to the sample surface displayed higher wear resistance than grains with other textures. This was attributed to lower resolved stresses for plastic deformation inside the grains with (101)

Mesoscale plasticity anisotropy at the earliest stages of cavitation-erosion damage of a high nitrogen austenitic stainless steel

A high nitrogen austenitic stainless steel (0.9wt% N) and an ordinary 304 austenitic stainless steel were submitted to cavitation-erosion tests in a vibratory apparatus operating at a frequency of 20 kHz. The high nitrogen stainless steel was obtained by high temperature gas nitriding a 1-mm thick strip of an UNS 31803 duplex stainless steel. The 304 austenitic stainless steel was used for comparison purposes. The specimens were characterized by scanning electron microscopy and Electron Back Scatter Diffraction. The surface of the cavitation damaged specimens was analyzed trying to find out the regions where cavitation damage occurred preferentially. The distribution of sites where cavitation inception occurred was extremely heterogeneous, concentrating basically at (i) slip lines inside some grains and (ii) Sigma-3 coincidence site lattice (CSL) boundaries (twin boundaries). Furthermore, it was observed that the CE damage spread faster inside those grains which were more susceptible to damage incubation. The damage heterogeneity was addressed to plasticity anisotropy. Grains in which the crystallographic orientation leads to high resolved shear stress show intense damage at slip lines. Grain boundaries between grains with large differences in resolved shear stress where also intensely damaged. The relationship between crystallite orientation distributions, plasticity anisotropy and CE damage mechanisms are discussed. (C) 2009 Elsevier B.V. All rights reserved.

Hysteresis loss subdivision

Assuming that different energy dissipation mechanisms are at work along hysteresis, a hysteresis loss subdivision procedure has been proposed, using the induction at maximum permeability ( around 0.8 T, in electrical steels) as the boundary between the ""low-induction`` and the ""high-induction`` regions. This paper reviews the most important results obtained in 10 years of investigation of the effect of microstructure on these components of the hysteresis loss. As maximum induction increases, the ""low-induction loss`` increases linearly up to 1.2 T, while the ""high-induction loss`` is zero up to 0.7 T and then increases as a power law with n = 5. Low-induction loss behavior is linearly related to H(c) between 0.4 and 1.2 T. Grain size has a larger influence on low-induction losses than on high-induction losses. Texture has a much stronger influence on high loss than on low-induction loss, and it is related to the average magnetocrystalline energy. 6.5%Si steel shows smaler hysteresis loss at 1.5 T than 3.5%Si steel only because of its smaler high-induction component. The abrupt increase in hysteresis loss due to very small plastic deformation is strongly related to the high-induction loss component. These results are discussed in terms of energy dissipation mechanisms such as domain wall movement, irreversible rotation and domain wall energy dissipation at domain nucleation and annihilation. (C) 2008 Elsevier B.V. All rights reserved.

On the Steinmetz hysteresis law

The behavior of the Steinmetz coefficient has been described for several different materials: steels with 3.2% Si and 6.5% Si, MnZn ferrite and Ni-Fe alloys. It is shown that, for steels, the Steinmetz law achieves R(2)> 0.999 only between 0.3 and 1.2 T, which is the interval where domain wall movement dominates. The anisotropy of Steinmetz coefficient for non-oriented (NO) steel is also discussed. It is shown that for a NO 3.2% Si steel with a strong Goss component in texture, the power law coefficient and remanence decreases monotonically with the direction of measurement going from rolling direction (RD) to transverse direction (TD), although coercive field increased. The remanence behavior can be related to the minimization of demagnetizing field at the surface grains. The data appear to indicate that the Steinmetz coefficient increases as magnetocrystalline anisotropy constant decreases. (c) 2008 Elsevier B.V. All rights reserved.

Effect of rolling on the residual stresses and magnetic properties of a 0.5% Si electrical steel

Cold-rolled (0-19% of reduction) 0.5% Si electrical steel sheets were studied in detail, including macro and micro residual stress measurements, crystallographic texture, dc-hysteresis curves and iron losses. Even for the smallest deformation, losses increase significantly, with large increase of the hysteresis losses, whereas the anomalous losses reduce slightly. The residual microstresses are similar to 150-350 MPa, whereas residual macrostresses are compressive, similar to 50 MPa. The large increase of the hysteresis losses is attributed to the residual microstresses. The dislocation density estimated by X-ray diffraction is in reasonable agreement with that predicted from the Sablik et al. model for effect of plastic deformation on hysteresis. The intensity of the texture fibers {1 1 1}< u v w > and < 110 >//RD (RD = rolling direction) increases with the reduction. (C) 2008 Elsevier B.V. All rights reserved.

Recognition of noisy images by PLL networks

We use networks composed of three phase-locked loops (PLLs), where one of them is the master, for recognizing noisy images. The values of the coupling weights among the PLLs control the noise level which does not affect the successful identification of the input image. Analytical results and numerical tests are presented concerning the scheme performance. (c) 2008 Elsevier B.V. All rights reserved.

Determining the effect of grain size and maximum induction upon coercive field of electrical steels

Although theoretical models have already been proposed, experimental data is still lacking to quantify the influence of grain size upon coercivity of electrical steels. Some authors consider a linear inverse proportionality, while others suggest a square root inverse proportionality. Results also differ with regard to the slope of the reciprocal of grain size-coercive field relation for a given material. This paper discusses two aspects of the problem: the maximum induction used for determining coercive force and the possible effect of lurking variables such as the grain size distribution breadth and crystallographic texture. Electrical steel sheets containing 0.7% Si, 0.3% Al and 24 ppm C were cold-rolled and annealed in order to produce different grain sizes (ranging from 20 to 150 mu m). Coercive field was measured along the rolling direction and found to depend linearly on reciprocal of grain size with a slope of approximately 0.9 (A/m)mm at 1.0 T induction. A general relation for coercive field as a function of grain size and maximum induction was established, yielding an average absolute error below 4%. Through measurement of B(50) and image analysis of micrographs, the effects of crystallographic texture and grain size distribution breadth were qualitatively discussed. (C) 2011 Elsevier B.V. All rights reserved.