Study of phase transition in (Pb,Ba)TiO(3) thin films

Dielectric and Raman scattering experiments were performed on polycrystalline Pb(1-x)Ba(x)TiO(3) thin films (x=0.40 and 0.60) as a function of temperature. The dielectric study on single phase compositions revealed that a diffuse-type phase transition occurred upon transformation of the cubic paraelectric to the tetragonal ferroelectric phase in all thin films, which showed a broadening of the dielectric peak. Diffusivity was found to increase with increasing barium contents in the composition range under study. In addition, the temperature dependence of Raman scattering spectra was investigated through the ferroelectric phase transition. The temperature dependence of the phonon frequencies was used to characterize the phase transitions. Raman modes persisted above the tetragonal to cubic phase transition temperature, although all optical modes should be Raman inactive. The origin of these modes was interpreted as a breakdown of the local cubic symmetry by chemical disorder. The lack of a well-defined transition temperature and the presence of broadbands in some temperature intervals above the paraferroelectric phase transition temperature suggest a diffuse-type phase transition. (C) 2008 American Institute of Physics.

Redetermination of 3-methylbenzoic acid

The asymmetric unit of the title compound, C(8)H(8)O(2), contains two crystallographically independent molecules, which form dimers linked by O center dot center dot center dot H-O hydrogen bonds. The benzene rings in the dimers are inclined at a dihedral angle of 7.30 (8)degrees and both methyl groups display rotational disorder. This redetermination results in a crystal structure with significantly higher precision than the original determination [Ellas & Garcia-Blanco (1963). Acta Cryst. 16, 434], in which the authors reported only the unit-cell parameters and space group, without any detailed information on the atomic arrangement. In the crystal, dimers are connected by weak C-H center dot center dot center dot O interactions, forming R(2)(2)(10) and R(4)(4)(18) rings along [110] and an infinite zigzag chain of dimers along the [001] direction also occurs.

2-(2-Nitroanilino)-5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophene-3-carbonitrile

The title compound, C(16)H(15)N(3)O(2)S, was synthesized by the reaction of 2-amino-5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophene-3-carbonitrile and o-fluoronitrobenzene. The thiophene and nitrophenyl rings and amino and carbonitrile groups are coplanar with a maximum deviation of 0.046 (2) angstrom and a dihedral angle of 0.92 (6)degrees between the rings. The cyclohepta ring adopts a chair conformation. Intramolecular N-H center dot center dot center dot O and C-H center dot center dot center dot S interactions occur. In the crystal, the molecules form layers that are linked by pi-pi stacking interactions between the thiophene and benzene rings [centroid-centroid distances = 3.7089 (12) and 3.6170 (12) angstrom].

Cadmium telluride nanocrystals as luminescent sensitizers in flow analysis

A fully automated multipumping flow system (MPFS) using water-soluble CdTe quantum dots (QD) as sensitizers is proposed for the chemiluminometric determination of the anti-diabetic drugs gliclazide and glipizide in pharmaceutical formulations. The nanocrystals acted as enhancers of the weak CL emission produced upon oxidation of sulphite by Ce(IV) in acidic medium, thus improving sensitivity and expanding the dynamical analytical concentration range. By interacting with the QD, the two analytes prevented their sensitizing effect yielding a chemiluminescence quenching of the Ce(IV)-SO(3)(2-)CdTe QD system. The pulsed flow inherent to MPFS assured a fast and efficient mixing of all solutions inside the flow cell, circumventing the need for a reaction coil and facilitating the monitoring of the short-lived generated chemiluminescent species. QD crystal size, concentration and spectral region for measurement were investigated. (C) 2011 Elsevier B.V. All rights reserved.

Relevance of leaf surface contamination for assessing chemical composition of bromeliads in a restinga forest

Resuspended soil and other airborne particles adhered to the leaf surface affect the chemical composition of the plant. A well-defined cleaning procedure is necessary to avoid this problem, providing a correct assessment of the inherent chemical composition of bromeliads. To evaluate the influence of a washing procedure, INAA was applied for determining chemical elements in the leaves of bromeliads from Vriesea carinata species, both non-washed and washed with Alconox, EDTA and bi-distilled water. Br, Ce, Hg, La, Sc, Se, Sm and Th showed higher mass fractions in non-washed leaves. The washing procedure removed the exogenous material without leaching chemical elements from inside the tissues.

PRODUCTION OF (15)N-ENRICHED NITRIC ACID (H(15)NO(3))

Techniques that employ (15)N have proved to be an important tool in many areas of the agronomic and biomedical sciences. Nevertheless, their use is limited by methodological difficulties and by the price of compounds in the international market. Nitric compounds ((15)NO(3)(-)) have attracted the interest of researchers. However, these compounds are not currently produced in Brazil. Thus, in the present work H(15)NO(3) was obtained from the oxidation of anhydrous (15)NH(3). The method we used differs from the industrial process in that the absorption tower is replaced with a polytetrafluoroethylene-lined, stainless-steel hydration reactor. The process output was evaluated based on the following parameters: reaction temperature; ratio of reagents; pressure and flow of (15)NH(3(g)) through the catalyst (Pt/Rh). The results showed that, at the best conditions (500 degrees C; 50% excess O(2); 0.4 MPa; and 3.39 g. min(-1) of (15)NH(3)), a conversion percentage (N-(15)NH(3) to N-(15)NO(3)(-)) of 62.2%, an overall nitrogen balance (N-(15)NH(3) + N-(15)NO(3)(-)) of 86.8%, and purity higher than 99% could be obtained.

Glypican-3 reexpression regulates apoptosis in murine adenocarcinoma mammary cells modulating PI3K/Akt and p38MAPK signaling pathways

Glypican-3 (GPC3) is a proteoglycan involved in proliferation and cell survival. Several reports demonstrated that GPC3 is downregulated in some tumors, such as breast cancer. Previously, we determined that GPC3 reexpression in the murine mammary adenocarcinoma LM3 cells induced an impairment of their invasive and metastatic capacities, associated with a decrease of their motility and an increase of their cell death. We demonstrated that GPC3 inhibits canonical Wnt signaling, as well as it activates non canonical pathway. Now, we identified signaling pathways responsible for the pro-apoptotic role of GPC3 in LM3 cells. We found for the first time that GPC3 inhibits the PI3K/Akt anti-apoptotic pathway while it stimulates the p38MAPK stress-activated one. We report a concomitant modulation of CDK inhibitors as well as of pro- and anti-apoptotic molecules. Our results provide new clues regarding the mechanism involved in the modulation induced by GPC3 of mammary tumor cell growth and survival.

ABNORMAL EXPRESSION OF VOLTAGE-GATED SODIUM CHANNELS Nav1.7, Nav1.3 AND Nav1.8 IN TRIGEMINAL NEURALGIA

Voltage-gated sodium channels have been implicated in acute and chronic neuropathic pain. Among subtypes, Nav1.7 single mutations can cause congenital indifference to pain or chronic neuropathic pain syndromes, including paroxysmal ones. This channel is co-expressed with Nav1.8, which sustains the initial action potential; Nav1.3 is an embrionary channel which is expressed in neurons after injury, as in neuropathic conditions. Few studies are focused on the expression of these molecules in human tissues having chronic pain. Trigeminal neuralgia (TN) is an idiopathic paroxysmal pain treated with sodium channel blockers. The aim of this study was to investigate the expression of Nav1.3, Nav1.7 and Nav1.8 by RT-PCR in patients with TN, compared to controls. The gingival tissue was removed from the correspondent trigeminal area affected. We found that Nav1.7 was downregulated in TN (P=0.017) and Nav1.3 was upregulated in these patients (P=0.043). We propose a physiopathological mechanism for these findings. Besides vascular compression of TN, this disease might be also a channelopathy. (C) 2009 IBRO. Published by Elsevier Ltd. All rights reserved.

Sequential Injection Analysis (SIA) for Arsenic Speciation by Capillary Electrophoresis Hyphenated to Inductively Coupled Plasma Sector Field Mass Spectrometry (CE-ICP-SFMS)

Sequential injection analysis (SIA) is proposed for managing microvolumes of sample and arsenic species solutions for speciation analysis by capillary electrophoresis focusing on the reduction of hazardous waste residues. An electronically controlled hydrodynamic injector was projected to introduce microvolumes of solutions prepared by SIA into the CE capillary with precision better than 2%. The determination of arsenite, arsenate, monomethylarsonic acid, dimethylarsinic acid, and arsenobetaine was performed from 50 mu L volumes of lyophilized urine and extract of shrimp with the system hyphenated to inductively coupled plasma mass spectrometry (CE-ICP-SFMS).

Optimization of Heat Treatment Profiles Applied to Nanometric-Scale Nb(3)Sn Wires With Cu-Sn Artificial Pinning Centers

Nb(3)Sn is one of the most used superconducting materials for applications in high magnetic fields. The improvement of the critical current densities (J(c)) is important, and must be analyzed together with the optimization of the flux pinning acting in the material. For Nb(3)Sn, it is known that the grain boundaries are the most effective pinning centers. However, the introduction of artificial pinning centers (APCs) with different superconducting properties has been proved to be beneficial for J(c). As these APCs are normally in the nanometric-scale, the conventional heat treatment profiles used for Nb(3)Sn wires cannot be directly applied, leading to excessive grain growth and/or increase of the APCs cross sections. In this work, the heat treatment profiles for Nb(3)Sn superconductor wires with Cu(Sn) artificial pinning centers in nanometric-scale were analyzed in an attempt to improve J(c) . It is described a methodology to optimize the heat treatment profiles in respect to diffusion, reaction and formation of the superconducting phases. Microstructural, transport and magnetic characterization were performed in an attempt to find the pinning mechanisms acting in the samples. It was concluded that the maximum current densities were found when normal phases (due to the introduction of the APCs) are acting as main pinning centers in the global behavior of the Nb(3)Sn superconducting wire.

Linoleic acid peroxidation initiated by Fe(3+)-reducing compounds recovered from Eucalyptus grandis biotreated with Ceriporiopsis subvermispora

This work work evaluates linoleic acid peroxidation reactions initiated by Fe(3+)-reducing compounds recovered from Eucalyptus grandis, biotreated with the biopulping fungus Ceriporiopsis subvermispora. The aqueous extracts from biotreated wood had the ability to reduce Fe(3+) ions from freshly prepared solutions. The compounds responsible for the Fe(3+)-reducing activity corresponded to UV-absorbing substances with apparent molar masses from 3 kDa to 5 kDa. Linoleic acid peroxidation reactions conducted in the presence of Fe(3+) ions and the Fe(3+)-reducing compounds showed that the rate of O(2) consumption during peroxidation was proportional to the Fe(3+)-reducing activity present in each extract obtained from biotreated wood. This peroxidation reaction was coupled with in-vitro treatment of ball-milled E. grandis wood. Ultraviolet data showed that the reaction system released lignin fragments from the milled wood. Size exclusion chromatography data indicated that the solubilized material contained a minor fraction representing high-molar-mass molecules excluded by the column and a main low-molar-mass peak. Overall evaluation of the data suggested that the Fe(3+)-reducing compounds formed during wood biodegradation by C subvermispora can mediate lignin degradation through linoleic acid peroxidation. (C) 2010 Elsevier Ltd. All rights reserved.

Heat treatment influence on the superconducting properties of nanometric-scale Nb(3)Sn wires with Cu-Sn artificial pinning centers

Since the discovery of Nb(3)Sn superconductors many efforts have been expended to improve the transport properties in these materials. In this work, the heat treatment profiles for Nb(3)Sn superconductor wires with Cu(Sn) artificial pinning centers (APCs) with nanometric-scale sizes were analyzed in an attempt to improve the critical current densities and upper critical magnetic field. The methodology to optimize the heat treatment profiles in respect to the diffusion, reaction and formation of the superconducting phases is described. Microstructural characterization, transport and magnetic measurements were performed in an attempt to relate the microstructure to the pinning mechanisms acting in the samples. It was concluded that the maximum current densities occur due to normal phases (APCs) that act as the main pinning centers in the global behavior of the Nb(3)Sn superconducting wire. The APC technique was shown to be very powerful because it permitted mixing of the pinning mechanism. This achievement was not possible in other studies in Nb(3)Sn wires reported up to now.

Superconductivity in Th(3)Ni(5)C(5)

The existence of a new metallic carbide of composition Th(3)Ni(5)C(5) was reported in the literature in 1991. This compound is a new orthorhombic prototype structure. In this work we report a reinvestigation of the synthesis of this material and we find that the Th(3)Ni(5)C(5) compound is a new bulk superconducting material. Despite the high concentration of Ni in this compound, we find bulk superconductivity with superconducting critical temperature of T(c) = 5.0 K and an upper critical field of mu(o)H(c2) = 5.8 T. Details of the superconducting state with specific heat, magnetization, and resistivity measurements are discussed.

Thermal expansion of the V(5)Si(3) and T(2) phases of the V-Si-B system investigated by high-temperature X-ray diffraction

The thermal expansion anisotropy of the V(5)Si(3) and T(2)-phase of the V-Si-B system were determined by high-temperature X-ray diffraction from 298 to 1273 K. Alloys with nominal compositions V(62.5)Si(37.5) (V5Si3 phase) and V(63)Si(12)B(25) (T(2)-phase) were prepared from high-purity materials through arc-melting followed by heat-treatment at 1873 K by 24 h, under argon atmosphere. The V(5)Si(3) phase exhibits thermal expansion anisotropy equals to 1.3, with thermal expansion coefficients along the a and c-axis equal to 9.3 x 10(-6) K(-1) and 11.7 x 10(-6) K(-1), respectively. Similarly, the thermal expansion anisotropy value of the T(2)-phase is 0.9 with thermal expansion coefficients equal to 8.8 x 10(-6) K(-1) and 8.3 x 10(-6) K(-1) along the, a and c-axis respectively. Compared to other isostructural silicides of the 5:3 type and the Ti(5)Si(3) phase, the V(5)Si(3) phase presents lower thermal expansion anisotropy. The T(2)-phase present in the V-Si-B system exhibits low thermal expansion anisotropy, as the T(2)-phase of the Mo-Si-B, Nb-Si-B and W-Si-B systems. (C) 2009 Elsevier Ltd. All rights reserved.

Magnetic characterization of Mn(5)SiB(2) and Mn(5)Si(3) phases

In this work the Mn(5)Si(3) and Mn(5)SiB(2) phases were produced via arc melting and heat treatment at 1000 degrees C for 50 h under argon. A detailed microstructure characterization indicated the formation of single-phase Mn(5)Si(3) and near single-phase Mn(5)SiB(2) microstructures. The magnetic behavior of the Mn(5)Si(3) phase was investigated and the results are in agreement with previous data from the literature, which indicates the existence of two anti-ferromagnetic structures for temperatures below 98 K. The Mn(5)SiB(2) phase shows a ferromagnetic behavior presenting a saturation magnetization M(s) of about 5.35 x 10(5) A/m (0.67 T) at room temperature and an estimated Curie temperature between 470 and 490 K. In addition, AC susceptibility data indicates no evidence of any other magnetic ordering in 4-300 K temperature range. The magnetization values are smaller than that calculated using the magnetic moment from previous literature NMR results. This result suggests a probable ferrimagnetic arrangement of the Mn moments. (C) 2009 Elsevier B. V. All rights reserved.