Studies of the serotonin type 3A receptor and the chemical preparation of tRNA

This thesis describes studies surrounding a ligand-gated ion channel (LGIC): the serotonin type 3A receptor (5-HT₃AR). Structure-function experiments using unnatural amino acid mutagenesis are described, as well as experiments on the methodology of unnatural amino acid mutagenesis. Chapter 1 introduces LGICs, experimental methods, and an overview of the unnatural amino acid mutagenesis.

In Chapter 2, the binding orientation of the clinically available drugs ondansetron and granisetron within 5-HT₃A is determined through a combination of unnatural amino acid mutagenesis and an inhibition based assay. A cation-π interaction is found for both ondansetron and granisetron with a specific tryptophan residue (Trp183, TrpB) of the mouse 5-HT₃AR, which establishes a binding orientation for these drugs.

In Chapter 3, further studies were performed with ondansetron and granisetron with 5-HT₃A. The primary determinant of binding for these drugs was determined to not include interactions with a specific tyrosine residue (Tyr234, TyrC2). In completing these studies, evidence supporting a cation-π interaction of a synthetic agonist, meta-chlorophenylbiguanide, was found with TyrC2.

In Chapter 4, a direct chemical acylation strategy was implemented to prepare full-length suppressor tRNA mediated by lanthanum(III) and amino acid phosphate esters. The derived aminoacyl-tRNA is shown to be translationally competent in Xenopus oocytes.

Appendix A.1 gives details of a pharmacological method for determining the equilibrium dissociation constant, K_B, of a competitive antagonist with a receptor, known as Schild analysis. Appendix A.2 describes an examination of the inhibitory activity of new chemical analogs of the 5-HT₃A antagonist ondansetron. Appendix A.3 reports an organic synthesis of an intermediate for a new unnatural amino acid. Appendix A.4 covers an additional methodological examination for the preparation of amino-acyl tRNA.

Synthesis of SnO2 by chemical routes and its use in varistors production

Tin oxide, SnO2. is a very used compound in industry and one of its uses is as varistor. For the current requirements of the technology is necessary a strict control of the chemical purity and the particle size of the raw material; for that reason the great interest that exists at the moment to develop synthesis methods that allow to get these requirements. In this work, ceramic powders of the Sn-Co-Nb-Ti-Al system using the controlled precipitation and polymeric precursor (Pechini) methods were synthesized. The raw material obtained was characterized using X-ray diffraction (XRD), thermal analysis (DTA/FG) and scanning electron microscopy (SEM). The sintering samples shown a good varistor behavior with non-linear coefficient (alpha) values similar to 22, and Er 2083 V/cm(2). (c) 2007 Elsevier Ltd. All rights reserved.

Development of metal oxide nanoparticles by soft chemical method

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

Photoluminescent properties of lead zirconate powders obtained by the polymeric precursor method

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Synthesis of YAP nanopowder by a soft chemistry route

Polycrystalline fine powder of YAlO(3) (YAP) was synthesized by the modified polymeric precursor method. A preliminary gradual pyrolytic decomposition under nitrogen flux was crucial in the removal process of organic residues to avoid the formation of molecular level inhomogeneities. YAP single phase was crystallized at temperatures between 950 degrees C and 1000 degrees C using chemically homogeneous ball-milled amorphous particles and very fast heating rates, corresponding to the lowest synthesis temperature of pure YAP nanopowder by soft chemistry routes. (C) 2009 Elsevier Ltd. All rights reserved.

Effect of processing route on the phase formation and properties of Bi4Ti3O12 ceramics

Our efforts were directed to the preparation of bismuth titanate-Bi4Ti3O12 (BIT) by two procedures: mechanically assisted synthesis and polymeric precursor method to display a variety of their advantages. To follow the nucleation and phase formation of BIT, XRD and Rietveld refinement analysis were used and it was shown that Bi4Ti3O12 ceramic can been successfully prepared from nano-sized powders obtained by both methods. The ferroelectric properties were determined and the loops from BIT obtained by polymeric precursor method were not fully saturated with a remnant polarization of 20 mu C/cm(2) and coercitive field of 1500 kV/cm. BIT obtained from powders prepared by mechanically assisted synthesis shows a remnant polarization of 0.65 mu C/cm(2) and coercitive field of 1050 kV/cm. The grain morphology may be the factor causing the observed differences. (C) 2005 Published by Elsevier Ltd and Techna Group S.r.l.

Effect of ceria content on the sintering of ZrO2 based ceramics synthesized from a polymeric precursor

Zirconia-ceria powders with ceria concentration varying from 0 to 12 mol% were synthesized using a polymeric precursor route based on the Pechini process. Powder characteristics were evaluated with regard to the crystallite size, BET surface area, phase distribution, nitrogen adsorption/desorption behavior, and agglomeration state. Sintering was studied considering the shrinkage rate, densification, grain size, and phase evolution. It was demonstrated that the synthesis method is effective to prepare nanosized powders of tetragonal zirconia single-phase. Sinterability mainly depended on the agglomeration state of powders and the monoclinic phase content, fully tetragonal zirconia ceramic, with grain size of 2.4 mu m, was obtained after addition of at least 9 mol% ceria and sintering at 1500 degrees C for 4 h. (C) 2000 Elsevier B.V. Ltd. All rights reserved.

Microstructural and morphological analysis of pure and Ce-doped tin dioxide nanoparticles

Structural morphological studies in pure and Ce-doped tin dioxide nanoparticles with high stability against particle growth were performed in samples, obtained using the polymeric precursor method and prepared at different annealing temperatures. A Ce-rich surface layer was used to control the particle size and stabilize SnO2 against particle growth. The formation of this segregated layer can contribute to a decreased surface energy, acting in the driving force, or reducing the surface mobility. Only the cassiterite SnO2 phase was observed below 1000 degreesC and a secondary phase (CeO2) was observed for the Ce-doped SnO2 at temperatures higher than 1000 degreesC, when de-mixing process occurs. The evolution of crystallite size, microstrain and morphology of the nanoparticles with annealing temperatures was investigated by X-ray diffraction (XRD), associated to Rietveld refinements, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). (C) 2002 Elsevier B.V. Ltd. All rights reserved.

Tin oxide nanoparticle formation using a surface modifying agent

This work presents results concerning the preparation of redispersible tin oxide nanoparticles achieved by using Tiron molecule ((OH)(2)C(6)H(2) (SO(3)Na)(2)) as surface modifying agent. The adsorption isotherm measurements show that an amount of 10 wt.% of Tiron is need to recover the SnO(2) nanoparticles surface with a monolayer. These nanoparticles can be easily redispersed in tetramethyl ammonium hydroxide at pH greater than or equal to11 until a powder concentration of 12 vol.% of tin. Under these conditions, hydrodynamic particle size is about 7 nm and increases until 52 nm at pH 6 due to the aggregation phenomenon. The time evolution of the viscoelastic properties indicates that the suspensions at pH 12.5, containing 12 vol.% tin oxide and 10 wt.% of surface modifier are kinetically stable. After thermal treatment at different temperature the powder characterisation evidences that the presence of Tiron monolayer at the nanoparticles surface increases the thermal stability of the porous texture and prevent the micropore size growth. This set of results contributes to satisfy the demand for more controlled synthesis of nanoparticles with high thermal stability as required for fabrication of ultrafiltration ceramic membranes. (C) 2004 Elsevier Ltd. All rights reserved.

The influence of the synthesis route on the final properties of SnO2-based varistors

A comparative study of two customary routes of ceramics processing applied to the synthesis of SnO2-based varistors is reported in this paper. Devices of equivalent composition were prepared through the Pechini method and through directly mixing the oxides without the addition of anti-agglomerants or binders. The microstructures of the sintered samples were characterised with X-ray diffraction and scanning and transmission electron microscopies. The electrical behaviour of the devices was studied on the basis of the current density versus electric field (J-E) characteristics and impedance spectroscopy measurements. The Pechini method ensures the homogeneity in the distribution of the additives in the tin oxide matrix but the formation of secondary phases seems to be independent of the synthesis route. Devices with similar non-linear coefficients of 18 and 21 were obtained through the mixed oxides route and the Pechini method, respectively. (C) 2007 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Effect of Eu substitution on the crystallographic and magnetic properties of the BiMn2O5 oxide obtained by urea combustion

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

Structure and properties of chemically synthesized BiFeO3. Influence of fuel and complexing agent

Perovskite, single multiferroic bismuth ferrite was prepared by two chemical methods: auto-combustion and soft chemical route. Influence of different fuels and complexing agents and thermal treatment on purity of bismuth ferrite powders and density of bismuth ferrite ceramics were investigated. X-ray diffraction technique (XRD) indicated that optimal temperatures and times for calcination and sintering are 600 degrees C for 2 h and 800 degrees C for 1 h with quenching, respectively. Scanning electron microscopy (SEM) analysis showed that soft route synthesized samples formed softer agglomerates and smaller grains with less secondary phases. Powders and pellets were characterized by Brunauer Emmett Teller (BET) specific surface area analysis, particle size distribution, Fourier transform infrared spectroscopy (FT-IR), dilatometry, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), dielectric and magnetic measurements. Resistivity and origin of electrical resistance were studied by means of impedance measurements. (C) 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

The effect of preparation method and Sb content on SnO2-CuO sintering

The sintering behavior of SnO2-CuO system has been investigated for two preparation methods and as a function of antimony concentration. A chemical preparation (Pechini's method) resulted in powders with smaller particle sizes than for a conventional oxide mixture. This led to smaller grain sizes in Pechini's method ceramics. The microstructures were heterogeneous in both systems, showing grain coarsening. The densification was aided by liquid phase formation, due to copper, in both systems, but the temperature of maximum shrinkage rate was larger for the Pechini's method ceramic because copper had to diffuse to the grain surface. Independently of the preparation method, antimony did not aid densification, and increasing its concentration led to a higher densification temperature and lower shrinkage rate. (C) 2003 Kluwer Academic Publishers.

Preparation of W-Al-Mo ternary alloys by mechanical alloying

Single phase WxAl(50)Mo(50)-X (X=40, 30, 20 and 10) powders have been synthesized directly by mechanical alloying (MA). The structural evolutions during MA and subsequent as-milled powders by annealing at 1400 degrees C have been analyzed using X-ray diffraction (XRD). Different from the Mo50Al50 alloy, W40Al50Mo10 and W30Al50Mo20 alloys were stable at 1400 degrees C under vacuum. The results of high-pressure sintering indicated that the microhardnesses of two compositions, namely W40Al50Mo10 and W30Al50Mo20 alloys have higher values compared with W50Al50 alloy.