Time-frequency and time-scale analysis of Barkhausen noise signals

Carrying out information about the microstructure and stress behaviour of ferromagnetic steels, magnetic Barkhausen noise (MBN) has been used as a basis for effective non-destructive testing methods, opening new areas in industrial applications. One of the factors that determines the quality and reliability of the MBN analysis is the way information is extracted from the signal. Commonly, simple scalar parameters are used to characterize the information content, such as amplitude maxima and signal root mean square. This paper presents a new approach based on the time-frequency analysis. The experimental test case relates the use of MBN signals to characterize hardness gradients in a AISI4140 steel. To that purpose different time-frequency (TFR) and time-scale (TSR) representations such as the spectrogram, the Wigner-Ville distribution, the Capongram, the ARgram obtained from an AutoRegressive model, the scalogram, and the Mellingram obtained from a Mellin transform are assessed. It is shown that, due to nonstationary characteristics of the MBN, TFRs can provide a rich and new panorama of these signals. Extraction techniques of some time-frequency parameters are used to allow a diagnostic process. Comparison with results obtained by the classical method highlights the improvement on the diagnosis provided by the method proposed.

Synthesis and Structural Analysis of New Palladium(II) Thiosaccharinates with Triphenylphosphane or Diphosphanes

A series of palladium(II) thiosaccharinates with triphenylphosphane (PPh(3)), bis(diphenylphosphanyl)methane (dppm), and bis(diphenylphosphanyl)ethane (dppe) have been prepared and characterized. From mixtures of thiosaccharin, Htsac, and palladium(II) acetylacetonate, Pd(acac)(2), the palladium(II) thiosaccharinate, Pd(tsac)(2) (tsac: thiosaccharinate anion) (1) was prepared. The reaction of I with PPh(3), dppm, and dppe leads to the mononuclear species Pd(tsac)(2)(PPh(3))(2)center dot MeCN (2), [Pd(tsac)(2)(dppm)] (3), Pd(tsac)(2)(dppm)(2) (4), and [Pd(tsac)(2)(dppe)]center dot MeCN (5). Compounds 2, 4, and 5 have been prepared also by the reaction of Pd(acac)(2) with the corresponding phosphane and Htsac. All the new complexes have been characterized by chemical analysis, UV/Vis, IR, and Raman spectroscopy. Some of them have been also characterized by NMR spectroscopy. The crystalline structures of complexes 3, and 5 have been studied by X-ray diffraction techniques. Complex 3 crystallizes in the monoclinic space group P2(1)/n with a = 16.3537(2), b = 13.3981(3), c = 35.2277(7) angstrom, beta = 91.284(1)degrees, and Z = 8 molecules per unit cell, and complex 5 in P2(1)/n with a = 10.6445(8), b = 26.412(3), c = 15.781(2) angstrom, beta = 107.996(7)degrees, and Z = 4. In compounds 3 and 5, the palladium ions are in a distorted square planar environment. They are closely related, having two sulfur atoms of two thiosaccharinate anions, and two phosphorus atoms of one molecule of dppm or dppe, respectively, bonded to the Pd(II) atom. The molecular structure of complex 3 is the first reported for a mononuclear Pd(II)-dppm-thionate system.

Synthesis and biocompatibility of an experimental glass ionomer cement prepared by a non-hydrolytic sol-gel method

The aims of this study were to demonstrate the synthesis of an experimental glass ionomer cement (GIC) by the non-hydrolytic sol-gel method and to evaluate its biocompatibility in comparison to a conventional glass ionomer cement (Vidrion R). Four polyethylene tubes containing the tested cements were implanted in the dorsal region of 15 rats, as follows: GI - experimental GIC and GII - conventional GIC. The external tube walls was considered the control group (CG). The rats were sacrificed 7, 21 and 42 days after implant placement for histopathological analysis. A four-point (I-IV) scoring system was used to graduate the inflammatory reaction. Regarding the experimental GIC sintherization, thermogravimetric and x-ray diffraction analysis demonstrated vitreous material formation at 110oC by the sol-gel method. For biocompatibility test, results showed a moderate chronic inflammatory reaction for GI (III), severe for GII (IV) and mild for CG (II) at 7 days. After 21 days, GI presented a mild reaction (II); GII, moderate (III) and CG, mild (II). At 42 days, GI showed a mild/absent inflammatory reaction (II to I), similar to GII (II to I). CG presented absence of chronic inflammatory reaction (I). It was concluded that the experimental GIC presented mild/absent tissue reaction after 42 days, being biocompatible when tested in the connective tissue of rats.

Regional scale analysis of landform configuration with base-level (isobase) maps

Base-level maps (or ""isobase maps"", as originally defined by Filosofov, 1960), express a relationship between valley order and topography. The base-level map can be seen as a ""simplified"" version of the original topographic surface, from which the ""noise"" of the low-order stream erosion was removed. This method is able to identify areas with possible tectonic influence even within lithologically uniform domains. Base-level maps have been recently applied in semi-detail scale (e.g., 1:50 000 or larger) morphotectonic analysis. In this paper, we present an evaluation of the method's applicability in regional-scale analysis (e.g., 1:250 000 or smaller). A test area was selected in northern Brazil, at the lower course of the Araguaia and Tocantins rivers. The drainage network extracted from SRTM30_PLUS DEMs with spatial resolution of approximately 900 m was visually compared with available topographic maps and considered to be compatible with a 1:1,000 000 scale. Regarding the interpretation of regional-scale morphostructures, the map constructed with 2nd and 3rd-order valleys was considered to present the best results. Some of the interpreted base-level anomalies correspond to important shear zones and geological contacts present in the 1:5 000 000 Geological Map of South America. Others have no correspondence with mapped Precambrian structures and are considered to represent younger, probably neotectonic, features. A strong E-W orientation of the base-level lines over the inflexion of the Araguaia and Tocantins rivers, suggest a major drainage capture. A N-S topographic swath profile over the Tocantins and Araguaia rivers reveals a topographic pattern which, allied with seismic data showing a roughly N-S direction of extension in the area, lead us to interpret this lineament as an E-W, southward-dipping normal fault. There is also a good visual correspondence between the base-level lineaments and geophysical anomalies. A NW-SE lineament in the southeast of the study area partially corresponds to the northern border of the Mosquito lava field, of Jurassic age, and a NW-SE lineament traced in the northeastern sector of the study area can be interpreted as the Picos-Santa Ines lineament, identifiable in geophysical maps but with little expression in hypsometric or topographic maps.

Novel benzofuroxan derivatives against multidrug-resistant Staphylococcus aureus strains: Design using Topliss` decision tree, synthesis and biological assay

The aim of this study was the design of a set of benzofuroxan derivatives as antimicrobial agents exploring the physicochemical properties of the related substituents. Topliss` decision tree approach was applied to select the substituent groups. Hierarchical cluster analysis was also performed to emphasize natural clusters and patterns. The compounds were obtained using two synthetic approaches for reducing the synthetic steps as well as improving the yield. The minimal inhibitory concentration method was employed to evaluate the activity against multidrug-resistant Staphylococcus aureus strains. The most active compound was 4-nitro-3-(trifluoromethyl)[N`-(benzofuroxan-5-yl) methylene] benzhydrazide (MIC range 12.7-11.4 mu g/mL), pointing out that the antimicrobial activity was indeed influenced by the hydrophobic and electron-withdrawing property of the substituent groups 3-CF(3) and 4-NO(2), respectively. (C) 2011 Elsevier Ltd. All rights reserved.

Synthesis and Study of the Photophysical Properties of a New Eu(3+) Complex with 3-Hydroxypicolinamide

This work reports on the synthesis and characterization of a new complex of Eu(3+) with the 3-hydroxypicolinamide ligand (Hhpa). Here we present an approach for obtaining bis[2-carbamoyl(kappa O)pyridin-3-olato(kappa O`)] lanthanide complexes, which were characterized through elemental analysis, thermal analysis, infrared and photoluminescence spectroscopies (emission, excitation, luminescence lifetimes, quantum efficiencies, Judd-Ofelt parameters and quantum yields). Although hpa can act as a bidentate ligand in different conformations, the results attest for the occurrence of a unique coordination site of low symmetry for the Eu(3+) ions, in which two anionic hpa ligands coordinate the cations through an O/O chelating system. The phosphorescence of the synthesized gadolinium complex provides the energy of the triplet state, which is determined to be at 20,830 cm(-1) over the ground state. This makes the Hhpa ligand very adequate for sensitizing the Eu(3+) luminescence, which leads to a very efficient antenna effect and opens a wide range of applications for the complex in light emitting organic-inorganic devices.

Synthesis and Characterization of Semi-Interpenetrating Networks Based on Poly(dimethylsiloxane) and Poly(vinyl alcohol)

Semi-interpenetrating networks (Semi-IPNs) with different compositions were prepared from poly(dimethylsiloxane) (PDMS), tetraethylorthosilicate (TEOS), and poly (vinyl alcohol) (PVA) by the sol-gel process in this study. The characterization of the PDMS/PVA semi-IPN was carried out using Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and swelling measurements. The presence of PVA domains dispersed in the PDMS network disrupted the network and allowed PDMS to crystallize, as observed by the crystallization and melting peaks in the DSC analyses. Because of the presence of hydrophilic (-OH) and hydrophobic (Si-(CH(3))(2)) domains, there was an appropriate hydrophylic/hydrophobic balance in the semi-IPNs prepared, which led to a maximum equilibrium water content of similar to 14 wt % without a loss in the ability to swell less polar solvents. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 115: 158-166, 2010

Synthesis and characterization of trans-[Ru(NO)Cl(L)(4)](PF(6))(2) (L = isonicotinamide; 4-acetylpyridine) and related species

The trans-[RUCl(2)(L)(4)], trans-[Ru(NO)Cl (L)(4)](PF(6))(2) (L = isonicotinamide and 4-acetylpyridine) and trans-[Ru(NO)(OH)(py)(4)]Cl(2) (py = pyridine) complexes have been prepared and characterized by elemental analysis, UV-visible, infrared, and (1)H NMR spectroscopies, and cyclic voltammetry. The MLCT band energies of trans-[RUCl(2)(L)(4) increase in the order 4-acpy < isn < py. The reduction potentials of trans-[RuCl(2)(L)(4)] and trans-[Ru(NO)Cl(L)(4)](2+) increase in the order py < isn < 4-acpy. The stretching band frequency. v(NO), of the nitrosyl complexes ranges from 1913 to 1852 cm(-1) indicating a nitrosonium character for the NO ligand. Due to the large pi-acceptor ability of the equatorial ligands, the coordinated water is much more acidic in the water soluble trans-[Ru(NO)(H(2)O)(py)(4)](3+) than in trans-[Ru(NO)(H(2)O)(NH(3))(4)](3+) (C) 2009 Elsevier B.V. All rights reserved.

The p.A2215D Thyroglobulin Gene Mutation Leads to Deficient Synthesis and Secretion of the Mutated Protein and Congenital Hypothyroidism with Wide Phenotype Variation

Context: Thyroglobulin (TG) is a large glycoprotein and functions as a matrix for thyroid hormone synthesis. TG gene mutations give rise to goitrous congenital hypothyroidism (CH) with considerable phenotype variation. Objectives: The aim of the study was to report the genetic screening of 15 patients with CH due to TG gene mutations and to perform functional analysis of the p. A2215D mutation. Design: Clinical evaluation and DNA sequencing of the TG gene were performed in all patients. TG expression was analyzed in the goitrous tissue of one patient. Human cells were transfected with expression vectors containing mutated and wild-type human TG cDNA. Results: All patients had an absent rise of serum TG after stimulation with recombinant human TSH. Sequence analysis revealed three previously described mutations (p. A2215D, p. R277X, and g. IVS30 + 1G > T), and two novel mutations (p. Q2142X and g. IVS46-1G > A). Two known (g. IVS30 + 1G/p. A2215D and p. A2215D/p. R277X) and one novel (p. R277X/g. IVS46-1G > A) compound heterozygous constellations were also identified. Functional analysis indicated deficiency in TG synthesis, reduction of TG secretion, and retention of the mutant TG within the cell, leading to an endoplasmic reticulum storage disease, whereas small amounts of mutant TG were still secreted within the cell system. Conclusion: All studied patients were either homozygous or heterozygous for TG gene mutations. Two novel mutations have been detected, and we show that TG mutation p. A2215D promotes the retention of TG within the endoplasmic reticulum and reduces TG synthesis and secretion, causing mild hypothyroidism. In the presence of sufficient iodine supply, some patients with TG mutations are able to compensate the impaired hormonogenesis and generate thyroid hormone. (J Clin Endocrinol Metab 94: 2938-2944, 2009)

Development of an Evaluation Scale for Sitting and Standing From the Ground for Children With Duchenne Muscular Dystrophy

The authors developed an evaluation scale for sit-stand from the ground for children with Duchenne muscular dystrophy (DMD) and tested its reliability. The construction occurred in stages: (a) the characterization of the movement in healthy children, (b) the characterization of the movement in children with DMD, (c) the elaboration of the 1st version of the scale and the manual, (d) the evaluation by experts and readjustments, and (e) the analysis of inter- and intraexaminer reliability and correlation with the Vignos Scale, age, and time for the execution of the activity. The scale comprehended 3 phases for sitting and 5 for the standing. A very good repeatability of the measures of sitting and standing (ICC = 0.89 and 0.84, respectively) and excellent reproducibility (ICC = 0.93 and 0.92, respectively) was demonstrated. The Kappa coefficient for the 8 phases in the interexaminer analysis varied from 0.77 to 1.00 (excellent reliability), and in the intraexaminer analysis varied from 0.80 to 1.00 (excellent reliability). Good correlation was found between the variables on the Vignos Scale (age: r = 0.58; stand: r = 0.56). The scale is a reliability instrument that allows evaluation of the activity of sitting and standing in children with DMD.

Deep crustal structure of the Parana Basin from receiver functions and Rayleigh-wave dispersion: Evidence for a fragmented cratonic root

The deep crustal structure of the Parana Basin of southern Brazil is investigated by analyzing P- and PP-wave receiver functions at 17 Brazilian Lithosphere Seismic Project stations within the basin. The study area can be described as a typical Paleozoic intracratonic basin that hosts one of the largest Large Igneous Province of the world and makes a unique setting for investigating models of basin subsidence and their interaction with mantle plumes. Our study consists of (1) an analysis of the Moho interaction phases in the receiver functions to obtain the thickness and bulk Vp/Vs ratio of the basin`s underlying crust and (2) a joint inversion with Rayleigh-wave dispersion velocities from an independent tomographic study to delineate the detailed S-wave velocity variation with depth. The results of our analysis reveal that Moho depths and bulk Vp/Vs ratios (including sediments) vary between 41 and 48 km and between 1.70 and 1.76, respectively, with the largest values roughly coinciding with the basin`s axis, and that S-wave velocities in the lower crust are generally below 3.8 km/s. Select sites within the basin, however, show lower crustal S-wave velocities slightly above 3.9 km/s suggestive of underplated mafic material. We show that these observations are consistent with a fragmented cratonic root under the Parana basin that defined a zone of weakness for the initial Paleozoic subsidence of the basin and which allowed localized mafic underplating of the crust along the suture zones by Cenozoic magmatism.

Synthesis and in vitro activity of limonene derivatives against Leishmania and Trypanosoma

The synthesis and in vitro activity of R(+)-Limonene derivatives against Leishmania and Trypanosoma cruzi strains are reported. Seven compounds have shown better in vitro activity against Leishmania (V.)braziliensis than the standard drug pentamidine. Additionally, we have identified two promising new anti-T. cruzi limonene derivatives. (C) 2010 Elsevier Masson SAS. All rights reserved.

A new scale-invariant ratio and finite-size scaling for the stochastic susceptible-infected-recovered model

The critical behavior of the stochastic susceptible-infected-recovered model on a square lattice is obtained by numerical simulations and finite-size scaling. The order parameter as well as the distribution in the number of recovered individuals is determined as a function of the infection rate for several values of the system size. The analysis around criticality is obtained by exploring the close relationship between the present model and standard percolation theory. The quantity UP, equal to the ratio U between the second moment and the squared first moment of the size distribution multiplied by the order parameter P, is shown to have, for a square system, a universal value 1.0167(1) that is the same for site and bond percolation, confirming further that the SIR model is also in the percolation class.

Synthesis and structural characterization of a new polymeric zinc(II) complex with thiophene-2-carboxylic acid

A new polymeric zinc(II) complex with thiophene-2-carboxylic acid (-tpc) of composition [Zn2(C20H12O8S4)]n was obtained and structurally characterized by X-ray diffraction, thermal analysis, nuclear magnetic resonance (NMR), and infrared spectroscopies. Upfield shift in the 1H-NMR spectrum is explained by the crystalline structure, which shows the thiophene rings overlapping each other in parallel pairs. The compound crystallizes in the monoclinic system, space group P21/c, with a = 9.7074(4) angstrom, b = 13.5227(3) angstrom, c = 18.9735(7) angstrom, = 95.797(10)degrees, and Z = 4. Three -tpc groups bridge between two Zn(II) ions through oxygens and the fourth one bridges between one of these ions and the third one, symmetry related by a twofold screw axis. This arrangement gives rise to infinite chains along the crystallographic a direction. The metal atoms display an approximate tetrahedral configuration. The complex is insoluble in water, ethanol, and acetone, but soluble in dimethyl sulfoxide.

Synthesis and Crystal Structures of Octahedral Sn(IV) Complexes Prepared from SnCl(2)center dot 2H(2)O and 2-Hydroxyacetophenone (S-benzydithiocarbazate) Ligand (H(2)L)

Two coordination octahedral Sn(IV) complexes [Sn(L)(2)] and cis-[SnCl(2)(L)(dmso)], where H(2)L is 2-hydroxyacetophenone (S-benzydithiocarbazate), were prepared and characterized by elemental analysis, IR, NMR ((1)H, (13)C), (119)Sn Mossbauer spectroscopies and X-ray diffraction techniques to investigate their structural properties. Both crystallize in the Monoclinic system, with parameters: a = 8.1905(3), b = 30.8811(15), c = 12.8959(7) angstrom, beta = 94.465(3)degrees and Z = 4 for [Sn(L)(2)] and a = 8.5247(2), b = 21.5445(7), c = 12.3706(3) angstrom, beta = 96.932(2)degrees and Z = 4 for cis-[SnCl(2)(L)(dmso)]. In both complexes, the Sn(IV) central atom is coordinated in a distorted octahedral geometry with the thiolate ligand (L(2-)) coordinated via O, N and S atoms. The (119)Sn Mossbauer spectroscopy of the complexes were studied and the results revealed that both complexes posses isomer shift (delta) and quadrupole splitting (Delta), which are almost the same.