Synthesis and pharmacological properties of TOAC-labeled angiotensin and bradykinin analogs

Angiotensin II (AngII) and bradykinin (BK) derivatives containing the TOAC (2,2,6,6-tetramethylpiperidine-N-oxyl-4-amino-4-carboxylic acid) spin label were synthesized by solid phase methodology. Ammonium hydroxide (pH 10, 50degreesC, 1 h) was the best means for reverting nitroxide protonation occurring during peptide cleavage. EPR spectra yielded rotational correlation times for internally labeled analogs that were nearly twice as large as those of N-terminally labeled analogs. Except for TOAC(1)-AngII and TOAC(0)-BK, which showed high intrinsic activities, other derivatives were inactive in smooth muscle preparations. These active paramagnetic analogs may be useful for conformational studies in solution and in the presence of model and biological membranes. (C) 2002 Elsevier B.V. All rights reserved.

Structural and surface properties of thermally prepared Ti/RhxTi(1-x)Oy electrodes: I - influence of preparation parameters

Electrodes of RhxTi(1-x) O-y nominal composition were prepared by thermal decomposition of the chloride or nitrate precursor salts dissolved in strongly acidic medium and applied by brush to both sides of a Tidegrees support. A systematic study of the influence of calcination temperature and time as well as oxygen flux was conducted. The coatings were characterised by SEM, EDAX, XRD, open circuit potential measurements and cyclic voltammetry (CV). Visible-ultraviolet spectrophotometry was employed to identify the chemical form of the precursor in solution while thermogravimetric analysis (TGA) was used to assess the decomposition temperature ranges. Optimisation of the coating preparation parameters showed coatings obtained from [Rh(H2O)(6)](NO3)(3) precursor dissolved in HNO3 1:2 (v/v) and fired at 430 degreesC for 2 h in a 5 1 min (-1) oxygen stream-furnished stable electrodes having the highest electrochemically active surface area. (C) 2002 Elsevier B.V. Ltd. All rights reserved.

Size effect on structure and dielectric properties of Nb-doped barium titanate

It is known that the dielectric properties of BaTiO3 (BT) are strongly dependent on its grain size. Coarse-grained ceramics of pure BT showed lower dielectric constant at room temperature then fine grained. Many authors considered that when the grain size is lower than 700 nm, the lattice of BT changes from tetragonal to pseudocubic, and the dielectric constant value is very low. In the doped BT this effect is more complex, because it is necessary to consider also the influence of dopants. The grain size effect on the structure and dielectric properties of niobium-doped barium titanate was investigated. Niobium-doped barium titanate was prepared from powders obtained by doping of commercial barium titanate and from organometallic complex using citrates as precursors (Pechini procedure). The crystal and microstructure of sintered niobium-doped barium titanate were determined. Dielectric constant and dissipation factor were measured. The observation confirmed that the structure and properties are strongly dependent on grain size. (C) 2003 Elsevier B.V. B.V. All rights reserved.

Ferroelectric and dielectric properties of lanthanum-modified bismuth titanate thin films obtained by the polymeric precursor method

Lanthanum-modified bismuth titanate, Bi4-xLaxTi3O12 (BLT), thin films with a La concentration of 0.75 was grown on Pt/Ti/SiO2/Si substrates by using the polymeric precursor solution and spin-coating method. The scanning electron microscopy (SEM) showed rounded grains, which is not typical for these system. The BLT films showed well-saturated polarization-electric field curve which 2P(r) = 41.4 muC/cm(2) and V-c = 0.99 V. The capacitance dependence on the voltage is strongly nonlinear, confirming the ferroelectric properties of the film resulting from the domains switching. These properties make BLT a promising material for FERAM applications.

Structural organization and thermal properties of the Sb2O3-SbPO4 glass system

The structural organization of Sb2O3-SbPO4 glasses has been studied by FTIR, Raman, P-31 MAS and spin echo NMR, Mossbauer and X-ray absorption spectroscopy (EXAFS and XANES at K and L-3,L-1-Sb edges). The combined results can be explained in terms of two potential mechanisms describing the change of the Sb(m) local environment upon incorporation of Q((4))-type phosphate. The formation of the latter species requires anionic compensation that may be adjusted by (a) formation of non bridging oxygen or (b) formation of SbO4E- groups (E = non-bonding electron pair). The second model is favored.

Synthesis, structure and redox properties of an unexpected trinuclear copper(II) complex with aspartame: [Cu(apm)(2)Cu(mu-N,O : O '-apm)(2)(H2O)Cu(apm)(2)(H2O)]center dot 5H(2)O

Structural, magnetic and spectroscopic data of a new trinuclear copper(II) complex with the ligand aspartame (apm) are described. [Cu(apm)(2)CU(mu-N,O:O'-apm)(2)(H2O)Cu(apm)(2)(H2O)]-5H(2)O crystallizes in the triclinic system, space group P1 (#1) with a = 7.3300(1) angstrom, b = 15.6840(1) angstrom, c = 21.5280(1) angstrom, alpha = 93.02(1)degrees, beta = 93.21 (1)degrees, gamma = 92.66(1)degrees and Z = 1. Aspartame coordinates to Cu(II) through the carboxylate and beta-amino groups. The carboxylate groups of the two central ligands act as bidentate bridges in a syn-anti conformation while the carboxylate groups of the four peripheral ligands are monodentate in a syn conformation. The central copper ion is in a distorted square pyramidal geometry with the apical position being occupied by one oxygen atom of the water molecule. The two terminal copper(II) atoms are coordinated to the ligands in the same position but their coordination sphere differs from each other due to the fact that one copper atom has a water molecule in an apical position leading to an octahedral coordination sphere while the other copper atom is exclusively coordinated to aspartame ligands forming a distorted square pyramidal coordination sphere. Thermal analysis is consistent with the X-ray structure. EPR spectra and CV curves indicate a rupture of the trinuclear framework when this complex is dissolved in ethanol or DMF, forming a mononuclear species, with a tetragonal structure. (c) 2005 Elsevier B.V. All rights reserved.

The effect of isostructural seeding on the microstructure and piezoelectric properties of PZT ceramics

Pechini's method was used to prepare lead titanate zirconate with Zr/Ti ratio equal to 53/47. X-ray diffraction data revealed the presence of a rhombohedral phase, rich in zirconium, due to difference in carbonate stabilities, in PZT ceramics calcined at 600 degrees C. Infrared spectroscopy presented COO- bonds in the 1400 cm(-1) region, which disappeared after calcining at 700 degrees C. Seeds with rhombohedral (PZT 57/43) or tetragonal structure (PZT 45/55) were added to the precursor. The microstructure was differentially influenced by the nature of seed particles. Rhombohedral nuclei promoted preferential crystallization of lead zirconate. This heterogeneity directly reflected on values of k(p) and d(33). (C) 1999 Elsevier B.V. Limited and Techna S.r.l. All rights reserved.

Luminescence and ESR properties of Brazilian feldspars

The IRSL and TL responses of three different feldspar crystals have been analysed. TL measurements were taken in the ultraviolet UV (290-370 nm) and the visible VIS (340-610 nm) regions of the spectrum. For the UV region and for a natural sample, peaks were observed at 283, 287 and 310 degrees C for grey, white and pink crystals, respectively. For samples irradiated after prior preheating, it was noted that TL peaks occurred at about 200 degrees C for all the samples; irradiation with high doses above 500 Gy induced the formation of one additional peak at 170 degrees C. The VIS region results were similar to those for the UV. ESR experiments have been developed to verify the influence of radiation and heat treatments on the centres and preliminary results showed great variation in the intensities of [TiO(4)](-), Al-O(-)-Al and Fe(3+) centres. (c) 2006 Elsevier Ltd. All rights reserved.

Structural electrical and optical properties of undoped and indium doped ZnO thin films prepared by the pyrosol process at different temperatures

The influence of the substrate temperature on the structural features and opto-electrical properties of undoped and indium-doped ZnO thin films deposited by pyrosol process was investigated. The addition of indium induces a drastic decrease (by a factor approximate to 10(10) for samples deposited at 300 degreesC) in the electrical resistivity of films, the lowest electrical resistivity (6 mOmega-cm) being observed for the film deposited at 450 degreesC. Films are highly transparent (>80%) in the Vis-NIR ranges, and the optical band gap exhibits a blue shift (from 3.29 to 3.33 eV) for the In-doped films deposited at increasing temperature. Preferential orientation of the ZnO crystallites with the c-axis perpendicular to the substrate surface and an anisotropic morphology of the nanoporous structure was observed for films growth at 300 and 350 degreesC. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Structure and electrical properties of potassium-doped siloxane-poly(oxypropylene) ormolytes

The structure and the ionic conduction properties of siloxane-poly(oxypropylene) (PPO) hybrids doped with different potassium salts (KCF3SO3, KI, KClO4 and KNO2) are reported for two polymer molecular weights (300 and 4000 g/mol), labelled PPO300 and PPO4000, respectively. The doping concentration, related to the concentration of the ether type oxygen of the PPO chain, is the same whatever the salt and verifies [O]/[K] = 20. Ionic room temperature conductivity shows the highest value for the KCF3SO3 doped PPO4000 hybrid (4 x 10(-7)Omega(-1).cm(-1)). The structure of these hybrids was investigated by X-ray powder diffraction (XRPD) and X-ray absorption spectroscopy (EXAFS and XANES) at the potassium K-edge (3607 eV). XRPD results show that the hybrid matrix is always amorphous and the formation of secondary potassium phases is observed for all the samples, except for the KCF3SO3 doped PPO4000 hybrid. EXAFS results evidence a good correlation between the ionic conductivity and the presence of oxygen atoms as first neighbours around potassium.

Dielectric and piezoelectric properties of the mechanochemically prepared PZT ceramics

Mechanochemical synthesis was applied to obtain nanocrystalline powders of composition Pb(Zr0.52Ti0.48)O-3 (PZT). Milling was performed in a planetary ball mill using vials and balls made of zirconia or steel-in order to investigate influence of milling media on the electrical properties of resulting ceramics. PZT ceramics showed high values for dielectric constant (epsilon(r)), reaching 970 at room temperature, as well as low dielectric loss (tandelta) under the optimal processing conditions. High values of remanent polarization (P-r) indicate high internal polarizability. The best samples showed piezoelectric strain constant d(33) = 347 pC/N and planar coupling factor k(P) = 0.44. Milling in ZrO2 medium prevents powder contamination and provides reproducibility of milling process. Also, PZT obtained from the powders milled in ZrO2 exhibited lower values of dielectric loss, in comparison with the PTZ obtained from the powders milled in Fe. This suggests that contamination of the powder with Fe could result in an increase of conductivity in final product. (C) 2004 Kluwer Academic Publishers.

Transport and sensors properties of nanostructured antimony-doped tin oxide films

Tin oxide thin films doped with 7 mol% antimony oxide multilayer were prepared by the polymeric precursor method. Morphological characterization revealed films with round-shaped grains, nanometric size (similar to 13 nm), and low roughness. These films display high transmittance (similar to 80%) in the visible range of transmittance spectra, which is desirable for transparent conductive oxide films. Analysis on electrical resistivity versus temperature data showed two different conduction mechanisms toward the temperature range. The gas sensor properties measurement of the thicker thin film revealed good sensibility for the NOx. (c) 2006 Elsevier B.V. All rights reserved.

Synthesis and some properties of hybrid gels of titanium oxide containing europium (III)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Microstructure and electric properties of a SnO2 based varistor

High non-linear J x E electrical characteristic (alpha=41) were obtained in the Nb2O5 and Cr2O3 doped CoO highly densified SnO2 ceramics. X-ray diffraction analysis showed that these ceramics are apparently single phase. Electrical properties and microstructure are highly dependent on the Cr2O3 concentration and on the sintering temperature. Excess of Cr2O3 leads to porous ceramics destroying the material's electrical characteristics probably due to precipitation of second phase of CoCr2O4 Dopant segregation and/or solid solution formation at the grain boundaries can be responsible for the formation of the electrical barriers which originate the varistor behaviour. (C) 1998 Elsevier B.V. Limited and Techna S.r.l. All rights reserved.

AN ACTINOMETRIC STUDY OF C2H2 PLASMA POLYMERIZATION AND FILM PROPERTIES

Thin polymer films were grown in radio frequency discharges containing C2H2. Actinometry revealed the trend in the plasma concentration of the CH species as a function of the operating pressure. The C-H bond density in the films, revealed by infrared analysis, was found to increase with the pressure of C2H2 in a similar way to that of the concentration of the CH species in the discharge. From transmission ultraviolet-visible spectroscopy data, optical parameters of the polymers, namely, the refractive index and the optical gap, were calculated. For the range of pressure studied, the refractive index decreased from 1.73 to 1.63 and the optical gap increased from 2.4 to 3.3 eV. Finally, measurements of the residual stress of the polymer films were carried out by the bending beam method, using a He-Ne laser, yielding values from 0.05 to 0.3 GPa. (C) 1995 American Vacuum Society.