Made available in DSpace on 2014-12-17T15:42:03Z (GMT). No. of bitstreams: 1 CyprianoGTN.pdf: 2726336 bytes, checksum: 398151afa4a714a39af458b59a347ead (MD5) Previous issue date: 2008-05-09 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Two methodologies were proposed to obtain micro and macroporous chitosan membranes, using two different porogenic agents. The methodologies proved to be effective in control the porosity as well as the pore size. Thus, microporous membranes were obtained through the physical blend of chitosan and polyethylene oxide (PEO) on an 80:20 (m/m) ratio, respectively, followed by the partial PEO solubilization in water at 80 ◦C. Macroporous chitosan membranes with asymmetric morphology were obtained using SiO2 as the porogenic agent. In this case, chiotsan-silica ratios used were 1:1, 1:3 and 1:5 (m/m). Membranes characterization were carried out by SEM (scanning electronic microscopy), X-ray diffraction, Fourier Transform Infrared Spectroscopy (FTIR), Thermal analysis (TG, DTG , DSC and DMTA). Permeability studies were performed using two model drugs: sodium sulfamerazine and sulfametoxipyridazine. By transmission FTIR it was possible to confirm the complete removal of SiO2. The SEM images confirmed the porous formation for both micro and macroporous membranes and also determined their respective sizes. By thermal analysis it was possible to show differences related with water sorption capacity as well as thermal stability for both membranes. DTG and DSC allowed evidencing the PEO presence on microporous membranes. The absorbance x time curves obtained on permeability tests for micro and macroporous membranes showed a linear behavior for both drugs in all range of concentration used. It was also observed, through P versus C curves, an increase in permeability of macroporous membranes according to the increase in porosity and also a decrease on P with increase in drug concentration. The influences of the drug molecular structure, as well as test temperatures were also evaluated / Duas metodologias foram propostas para a obten??o de membranas macro e microporosas de quitosana, utilizando dois diferentes agentes formadores de poros. As metodologias mostraram-se eficientes no controle da porosidade e do tamanho dos poros gerados. Deste modo, membranas microporosas foram obtidas atrav?s de mistura f?sica da quitosana com o poli(?xido de etileno) (PEO), na propor??o 80:20 (m/m), respectivamente, seguido da solubiliza??o parcial do PEO em ?gua a 80 ◦C, e membranas macroporosas de quitosana com morfologia assim?trica foram obtidas utilizando um agente inorg?nico gerador de poros (SiO2). Neste caso, as propor??es quitosana-s?lica utilizadas foram 1:1, 1:3 e 1:5 (m/m). A caracteriza??o das membranas foi realizada atrav?s de microscopia eletr?nica de varredura (MEV), difra??o de raios X (DRX), espectroscopia de absor??o na regi?o do infravermelho (FTIR), an?lise t?rmica (TG, DTG, DSC e DMTA) e do estudo de sua permeabilidade utilizando-se dois f?rmacos modelos (sulfamerazina de s?dio e sulfametoxipiridazina). Atrav?s da t?cnica de FTIR em pastilha de KBr foi poss?vel confirmar, nas membranas macroporosas, a retirada completa do gerador de poros (SiO2). As imagens obtidas com o MEV confirmam a forma??o dos poros, tanto para as microporosas quanto para as macroporosas e determinam os seus respectivos tamanhos. Atrav?s das an?lises de TG, DTG e DSC foi poss?vel mostrar as diferen?as na capacidade de reten??o de ?gua para todas as membranas e suas estabilidades t?rmicas. As an?lises de DTG e DSC permitiram tamb?m evidenciar a presen?a de PEO nas membranas microporosas. As curvas Absorb?ncia ? Tempo obtidas a partir dos ensaios de permeabilidade, para as membranas micro e macroporosas, apresentaram um comportamento linear para ambos os f?rmacos e em todas as concentra??es utilizadas. Foi observado tamb?m, atrav?s da curva P ? C, um aumento na permeabilidade das membranas de acordo com o aumento da porosidade, bem como uma diminui??o desta com o aumento da concentra??o (C) dos f?rmacos modelo. Fatores tais como a influ?ncia da estrutura do f?rmaco e o efeito da temperatura tamb?m foram avaliados

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-10-25T22:39:49Z No. of bitstreams: 1 GilbertoDeLima_DISSERT.pdf: 6145295 bytes, checksum: bc53e57020e12cd1c59df71eaa9312a9 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-12-16T20:13:09Z (GMT) No. of bitstreams: 1 GilbertoDeLima_DISSERT.pdf: 6145295 bytes, checksum: bc53e57020e12cd1c59df71eaa9312a9 (MD5) / Made available in DSpace on 2016-12-16T20:13:09Z (GMT). No. of bitstreams: 1 GilbertoDeLima_DISSERT.pdf: 6145295 bytes, checksum: bc53e57020e12cd1c59df71eaa9312a9 (MD5) Previous issue date: 2016-02-05 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Filmes polim?ricos autossustent?veis baseados em um novo eletr?lito polim?rico s?lido (EPS), tendo como matriz hospedeira o poli(?xido de etileno) (POE) e como agente dopante o tungstato de s?dio (Na2WO4), foram obtidos para diferentes composi??es do sal (m = 0,20; 0,26; 0,30; 0,40; 0,50 e 1,31 mg). Os filmes foram caracterizados por DRX, FTIR, MEV/EDS, TG/DTG, DSC e EI. Os difratogramas de raios X confirmaram a natureza semicristalina do pol?mero e sugeriram que a adi??o do sal provoca uma redu??o na cristalinidade dos filmes. Os dados de FTIR permitiram a an?lise da intera??o entre os ?ons do sal e as cadeias polim?ricas. As micrografias obtidas por MEV demonstraram morfologia esferul?tica intercaladas por liga??es interlamelares para todas as composi??es estudadas. O estudo de TG/DTG mostrou que a decomposi??o t?rmica do eletr?lito ocorre em uma ?nica etapa com a adi??o do sal aumentando a estabilidade t?rmica dos filmes. Os dados de TG/DTG permitiram, ainda, o estudo cin?tico da decomposi??o t?rmica do eletr?lito por meio dos m?todos de Briodo (BR), Coats-Redfern (CR) e Horowitz-Metzger (HM) sugerindo uma cin?tica de 1? ordem para a rea??o de decomposi??o t?rmica dos filmes, assim como, a determina??o dos par?metros termodin?micos de ativa??o: E*, ?H*, ?S* e ?G*. O grau de cristalinidade foi determinado atrav?s dos dados de DSC e mostrou uma redu??o ap?s a adi??o do sal ao pol?mero. O eletr?lito POE/Na2WO4 exibiu um m?ximo de condutividade i?nica de 3,24x10-4 S.cm-1, a temperatura ambiente, para o filme com 1,31 mg do sal. Atrav?s dos dados de imped?ncia foi poss?vel o estudo de relaxa??o das cadeias do POE, assim como, a difus?o do sal entre estas cadeias. Os diagramas de imped?ncia, nos formatos Bode e Nyquist, permitiram o ajuste dos dados experimentais ? circuitos el?tricos equivalentes o que facilitou a associa??o dos componentes dos circuitos aos fen?menos f?sicos e qu?micos observados para os filmes e revelaram que, ap?s a adi??o do sal ao pol?mero, os filmes t?m suas propriedades el?tricas melhoradas. / Self-sustainable polymeric films based on new solid polymer electrolyte, having the poly(ethylene oxide) (PEO) as host matrix and sodium tungstate as doping agent (Na2WO4), were obtained from different salt compositions (m = 0.20; 0.26; 0.30; 0.40; 0.50 and 1.31 mg). The films were characterized through XRD, FTIR, SEM/EDS, TG/DTG, DSC and IS. X-ray diffraction showed the semi crystalline nature of the polymer and confirmed that the addition of salt induces reduction in the crystalinity of the films. FTIR data allowed the identification of the interaction between salt ions and polymer chains and confirmed that these interactions are of a physical nature. The micrographs obtained through SEM showed spherulitic morphology interleaved by interlayered bonds for all of the compositions studied. The TG/DTG study revealed that the thermal decomposition of the electrolyte almost happens at a single stage with the addition of salt, increasing the thermal stability of the films. TG/DTG data also allowed the kinetic study of the thermal decomposition of the electrolyte through Broido (BR), Coats-Redfern (CR) and Horowitz-Metzger (HM) methods, suggesting a first-order kinetic for the reaction of the thermal decomposition of the films, as well as the setting of pre-exponential factor, A, and the thermodynamic activation parameters: E*, ?H*, ?S* and ?G*. The crystallinity degree was determined through DSC data and showed a reduction after the addition of salt to the polymer. The polymer has its conductivity increased after addition of the salt with the PEO-Na2WO4 electrolyte exhibiting maximum of ionic conductivity of 3.24x10-4 S cm-1, to room temperature, for the film with 1.31 mg of salt (F6 film). The impedance data allowed the study on relaxation on PEO chains, even as the diffusion of salt between these chains. The impedance diagrams, on Bode and Nyquist formats, enabled the adjustment of the experimental data to equivalent electric circuits, which facilitated the association of the circuit components to the physical and chemical phenomena observed for the films and revealed that, after the addition of salt to the polymer, the films have their electrical properties enhanced.