O objetivo deste trabalho foi obter dispersões sólidas microparticuladas contendo praziquantel a fim de aumentar sua solubilidade em água e consequentemente melhorar sua biodisponibilidade in vivo e estudar sua estabilidade acelerada. Foram preparadas 4 misturas físicas em proporções diferentes de PZQ e carreador e 8 dispersões sólidas microparticuladas foram obtidas por spray dryer. Para controle também foi seco em spray dryer o PZQ puro nas mesmas temperaturas do estudo das dispersões. Foi realizada a caracterização dessas amostras por DSC, Raios-x, Infravermelho e MEV. O aumento de solubilidade das misturas físicas não foi significante em relação ao PZQ puro, no entanto as DSM obtidas na temperatura de 70ºC foi significante, com p<=0,05, e chegaram a ser até 3 vezes maiores. O estudo de dissolução mostrou que ao final de 60 minutos de teste a dispersão sólida estudada obteve um desempenho 6x melhor que o PZQ puro. O MEV mostrou que as partículas ficaram esféricas, de superfície r?gosa, e a eficiência de encapsulação variou de 90 a 100%. Um estudo preliminar de estabilidade das amostras mostrou um aumento na solubilidade em relação ao tempo. Sendo assim algumas amostras foram escolhidas para recomeçar o estudo, fazendo um estudo de estabilidade acelerada mais aprofundado avaliando estabilidade quiral do fármaco, perfil de solubilidade, DSC, Raios-X e Infravermelho. Ao avaliar os dados dessa estabilidade acelerada percebemos que esse aumento de solubilidade com o tempo foi ocasionado por uma redução na cristalinidade do fármaco, também com o tempo. Observou-se nos dados de DSC o surgimento de um pico característico de transição vítrea para as DSMs 8, 10, 12 e PZQsd, e essa alteração na transição vítrea possivelmente levou a uma diminuição na mobilidade molecular do sistema dificultando o rearranjamento molecular do fármaco e assim sua recristalização. Foram realizados testes in vitro e in vivo de eficácia e os resultados mostraram que a dispersão sólida estudada teve excelente eficácia comparada ao PZQ puro. Podemos concluir, portanto, que a técnica escolhida nesse estudo atendeu aos objetivos propostos e foi eficaz no aumento de solubilidade e na eficácia para o tratamento da esquistossomose e que o estudo de estabilidade é de fato importante para dispersões sólidas / The aim of this study was to produce microparticulated solid dispersions of praziquantel in order to increase its solubility in water and thus improve its bioavailability in vivo. Were prepared 4 physical mixtures in different proportions of carrier and 8 solid dispersion microparticles was obtained by spray drying. To control was also dried by spray drying pure PZQ the same temperatures the study of dispersions. The characterization of these samples was performed by DSC, X-rays, infrared and SEM. The increased solubility of the physical mixtures was not significant compared to pure PZQ, but for the samples dried at 70°C was significant compared to pure PZQ and 3folder than PZQ. The dissolution study has shown that the end of the 60minutes test solid dispersion released about 90% dr?g, while releasing pure PZQ for the same time the study was about 15%. The SEM showed that the particles were spherical, and shown a \"sponge-like\" surface. The encapsulation efficiency varied from 90 to 100%. A preliminary study of the stability samples showed an increase in solubility over time. For this reason some samples were chosen for the recommence study, making a further study of accelerated stability evaluating chiral dr?g stability, solubility profile, DSC, X-rays, infrared. When considering data that accelerated stability realized that this increase in solubility with time was caused by a decrease in dr?g crystallinity, also in time. It was observed in the DSC data the appearance of a characteristic peak of glass transition for the samples 8, 10, 12 and PZQsd, and the change in glass transition possibly led to a decrease in the molecular mobility system avoiding molecular dr?g rearrangement and thus its recrystallization. in vitro in vivo efficacy tests were carried out and the results showed that the solid dispersion studied had excellent efficacy compared to pure PZQ. Than it can be concluded that the technique chosen in this study met the proposed objectives and was effective in increasing solubility and efficacy for the treatment of schistosomiasis

The diploma thesis deals with the preparation, crosslinking and characterization of collagen films from various animal sources. Collagen from pig, Tilapia, horse, cow and crocodile was used to prepare collagen films. Chemical crosslinking agents EDC/NHS and Lyofix were used to crosslink the prepared films. In the experimental part, differential scanning calorimetry (DSC) method was optimized to determine the denaturation temperature of individual collagen films before and after crosslinking. In addition, the ability of films to swell and degrade has been analyzed. The presence of characteristic groups present in the collagen structure was verified using infrared spectroscopy. The sample morphology was analyzed using Scanning Electron Cryomicroscopy (Cryo-SEM). The results show that EDC/NHS is a better collagen crosslinking agent compared to Lyofix. The best source for the preparation of thermally stable films is piggy collagen, whose denaturation temperature after crosslinking with EDC/NHS was about 69 °C and could represent more than adequate substitution for cow collagen, which is currently most used in the field of tissue engineering and food industry.

Les cellules photovoltaïques (PV) des modules ou panneaux solaires, sont protégées des agressions extérieures par des résines polymères encapsulantes qui, pour la plupart, sont des matériaux élastomériques réticulés. L’optimisation et le contrôle de l’étape d’encapsulation peut permettre un gain de productivité et augmenter la durée de vie des modules, ce qui réduit les coûts de l’électricité générée. Deux voies ont ainsi été explorées dans ce travail : 1) La première concerne l’étude de l’état de réticulation de l’encapsulant majoritairement utilisé actuellement, un copolymère d’éthylène et d’acétate de vinyle connu sous le nom d’EVA ; celui-ci est mis en œuvre sous forme de feuilles ou films. Une faible réticulation de l’encapsulant peut mener, entre autre, à son fluage lors de son utilisation, impactant directement la durée de vie du module. Il est donc important de suivre le niveau de réticulation de l’encapsulant lors des opérations de contrôle. La comparaison de différentes méthodes d’évaluation du degré de réticulation ont donc été menées ; 2) La deuxième voie concerne des études autour d’un nouveau procédé d’encapsulation. En effet, le procédé industriel actuel, inclut une étape dite de « lamination », pendant laquelle l’encapsulant est fondu et réticulé autour des cellules. Cette étape relativement longue crée des contraintes thermomécaniques pouvant limiter la durée de vie des modules PV. Le développement d’un nouveau procédé d’encapsulation où l’encapsulant en film est remplacé par un encapsulant liquide photopolymérisable permettrait de diminuer les coûts de production tout en augmentant potentiellement la durée de vie des modules. Les propriétés rhéologiques et la cinétique de polymérisation de ce nouvel encapsulant sont ainsi étudiées. Enfin les deux voies d’encapsulation sont comparées. Il a été montré que d’un point de vue des performances électriques le nouveau procédé présente un avantage potentiel et que d’un point de vue de la tenue au vieillissement il est équivalent au procédé industriel actuel / Photovoltaic (PV) cells, for solar modules or panels, are protected from environmental stresses by polymeric encapsulants, which are mostly crosslinked elastomers. The optimization and the control of the encapsulation step have a twofold interest by increasing PV module lifetime and productivity, thus leading to a decrease of the cost of generated electricity. Two main directions have been investigated in this work: 1) The first one is related to the study of the crosslinking degree of the main industrial PV polyolefin encapsulant, EVA, which is a copolymer composed of ethylene and vinyl acetate, used currently in film form. Indeed, poor crosslinking level can lead to its creep, impacting directly the module lifetime. To overcome this problem, the quality control needs to be improved, by the evaluation of the crosslinking degree obtained while using the conventional encapsulation process (through lamination of encapsulant foils). Thus, the comparison of several methods to evaluate this degree are led ;2) The second direction concerns the study of a new encapsulation process. Indeed, the conventional lamination process potentially creates mechanical stresses in the PV cells, which as a consequence may limit the PV module lifetime. Moreover, lamination requires a relatively long processing time. To overcome this problem, the development of a new encapsulation process using a photopolymerizable encapsulant, initially liquid, decreases the production costs of PV modules and potentially increases their lifetime. The rheology properties and the polymerization kinetics of the new encapsulant are studied. At the end of the present work, both encapsulation processes are compared. Electrical performances of PV cells are measured before and after encapsulation as well as before and after ageing cycles. It has been revealed that the new encapsulation process presents at least as good, if not better performances than the standard process, thus highlighting its big potential for the manufacturing of PV modules

Plast påverkar vårt samhälle i stor utsträckning och har hjälpt till att utveckla nya förbättringar och redskap i vår vardag. Trots alla bra egenskaper med plaster har några oönskade effekter kommit till ytan med negativ påverkan på miljön. Detta examensarbete undersökte hur plastmaterial bryts ned av vittring utanför den svenska västkusten. Plastmaterialen undersöktes med hjälp av Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC) och Scanning Electron Microscopy (SEM) för att fastställa om kemisk nedbrytning sker efter 12 månader. Följande frågor stod i fokus: Vilka plaster har brutits ned, och i vilken utsträckning? Hur har plastens egenskaper förändrats? Vilka förutsättningar har de olika plastmaterialen för nedbrytning på stränder, och vilka faktorer påverkar nedbrytningen? Resultatet indikerade att liten eller ingen detekterbar nedbrytning skett på proverna efter 12 månaders vittring genom FTIR analys. Några prover visade dock tecken på förändring i de fysiska egenskaperna vid DSC analys, vilket kan beror på nedbrytning. Trots detta resultat fanns det synliga tecken på fragmentering, fysisk skada från stress och yttre krafter, såsom sand- och vågtumling för EPS (Styrofoam), LD-PE (Candy Paper) och PP (Blårep). Fragmenteringens påverkan på havlsmiljön kunde dock inte bevisas i denna studie eftersom prover på sand eller vatten från området inte genomfördes. Detta gör att endast synliga indikationer på fragmentering var identifierbara, men inte bevisa att det bidragit till makro- eller mikroplaster i närmiljön. Samtliga plastmaterial i studien innehöll någon form av tillsatts så som stabilisatorer. Eftersom endast små variationer förekommer i analysen av plastmateralen kunde det antas att tillsatserna och stabilisatorerna i materialen var effektiva i att hindra polymererna från nedbrytning under 12-månaders vittring. / Plastic has greatly impacted our society today and helped develop new improvements and implements in the daily lives. Despite all the good things, some undesirable impacts have also been discovered, which have been shown to impact the climate negatively. This thesis was to investigte how plastic degrades when weathered outside the  Swedish West Coast. The plastic materials were analysed using Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Scanning Electron Microscopy (SEM) to determine whether degradation had occurred after 12 months. The following questions were at focus: What plastics have been degraded, and if so, which to the greatest extent? How have the properties of the plastic changed? What were theprerequisites for the different plastic materials for degradation on the shoreline, and what factors are affecting the degradation? The results indicated that the samples had little to no detectable degradation regarding the FTIR analysis after 12 months of weathering. Some of the samples showed a change in the physical properties from the DSC analysis, which could indicate degradation. Despite the result of degradation extent, there were clear signs of fragmentation, physical damage from stress, and external forces, such as rock and wave tumbling for EPS (Styrofoam), LD-PE(Candy Paper) and PP (Blue Rope). Fragmentation was not proven since no soil or water samples were made at the wethering site. This made the fragmentation only a visible parameter based on the samples after weathering, not proving that micro- or macro-plastic has been washed out in the ocean. All of the plastic materials used in the study were produced with some sort of additive, such as stabilisers. Since only small variations were shown in the analysis of the plastic materials, it can be assumed that additives and stabilisers were effective because there was no clear sign of degradation after 12 months of weathering.

Les travaux de recherche présentés ici avaient pour objectif principal la synthèse de copolymères statistiques à base d’éthylène et d’acide acrylique (AA). Pour cela, la déprotection des groupements esters d’un copolymère statistique précurseur, le poly(éthylène-co-(tert-butyl)acrylate), a été effectuée par hydrolyse à l’aide d’iodure de triméthylsilyle. La synthèse de ce précurseur est réalisée par polymérisation catalytique en présence d’un système à base de Palladium (Pd). Le deuxième objectif a été d’étudier et de caractériser des polymères synthétisés à l’état solide et en suspension colloïdale. Plusieurs copolymères précurseurs comprenant différents pourcentages molaires en tert-butyl acrylate (4 à 12% molaires) ont été synthétisés avec succès, puis déprotégés par hydrolyse pour obtenir des poly(éthylène-coacide acrylique) (pE-co-AA) avec différentes compositions. Seuls les copolymères comprenant 10% molaire ou plus de AA sont solubles dans le Tétrahydrofurane (THF) et uniquement dans ce solvant. De telles solutions peuvent être dialysées dans l’eau, ce qui conduit à un échange lent entre cette dernière et le THF, et l’autoassemblage du copolymère dans l’eau peut ensuite être étudié. C’est ainsi qu’ont pu être observées des nanoparticules stables dans le temps dont le comportement est sensible au pH et à la température. Les polymères synthétisés ont été caractérisés par Résonance Magnétique Nucléaire (RMN) ainsi que par spectroscopie Infra-Rouge (IR), avant et après déprotection. Les pourcentages molaires d’AA ont été déterminés par combinaison des résultats de RMN et ii de titrages conductimètriques. A l’état solide, les échantillons ont été analysés par Calorimétrie différentielle à balayage (DSC) et par Diffraction des rayons X. Les solutions colloïdales des polymères pE-co-AA ont été caractérisées par Diffusion dynamique de la lumière et par la DSC-haute sensibilité. De la microscopie électronique à transmission (TEM) a permis de visualiser la forme et la taille des nanoparticules. / The first objective of this research is to synthesize random linear copolymers of ethylene and acrylic acid (AA). The synthesis relies on the deprotection of the functional groups in the copolymer’s precursor, which is represented by poly(ethylene-co-tertbutyl acrylate). The synthesis of the precursor was realized by the catalytic approach, where Pd-based catalytic systems are frequently utilized nowadays. The deprotection was carried out by hydrolysis of the ester functionality using trimethylsilyl iodide agent. The second objective is to investigate and characterize the synthesized polymers in the bulk and in colloidal solution. A set of different precursor polymers with various degrees of molar incorporation of tertbutyl acrylate (from 4 to 12 mol %) was successfully synthesized and deprotected. The resulting poly(ethylene-co-acrylic acid) copolymers were found to be soluble in tetrahydrofuran THF, when the molar incorporation of AA reaches the value of 12 and more. This aspect gave the possibility to study the self-assembly of this copolymer in aqueous medium by slow THF to water exchange (dialysis). It was found that the copolymers self-assemble into nano-sized structures and these nanoparticles remain stable in colloidal solution for extended periods of time. Moreover, it was shown that the nanoparticles formed by the discussed copolymer possess thermo- and pH-responsive behaviour. The polymers synthesized were characterized by nuclear magnetic resonance (NMR) and infrared spectroscopies (IR) before and after deprotection. The bulk samples were analyzed by conventional differential scanning calorimetry and by X-ray diffraction iv technique. The molar percentages of AA were determined using a combination of NMR and conductimetric titration. Colloidal solutions of pE-co-AA copolymers were analyzed by dynamic light scattering and high-sensitivity differential scanning calorimetry techniques. The nanoparticles formed were visualized and characterized by transmission electron microscopy.

Farmaceutická fakulta, Katedra farmaceutické technologie, Hradec Králové, 2014 Vypracovala: Markéta Valentová Školitel: Doc. RNDr. Milan Dittrich, CSc. ABSTRACT STUDY OF POLYESTER DRUG CARRIERS DEGRADATION USING THE DSC METHOD The aim of this work was focused on the study of relations among various parameters of degradation process, such as time-dependent range of glass transition temperature, swelling, erosion, and molar weight decrease. Two model polyesters of two type architectures of polyester molecules were used and monitored during two-week period. In the theoretical part of this diploma thesis are in details described biopolymers with stimulus responsive activity and exploitation of these materials in various biomedical applications in the topic of tissue engineering. The experimental part of this work is directed into the study of molecule degradation parameters, eventually into simulated biodegradation in the in vitro conditions of two different in the type polyesters with the contrast polyester molecule constitution. It was demonstrated that parameter Mn decreases towards the limit values. Between the values of molar weight and glass transition temperature is not Flory-Fox relation in the advanced phase of degradation process. The erosion of the material begins after the lag-time in the dependency...

Cette étude s'inscrit dans le cadre du projet Européen VEGEPHY (VEGEtale-PHYtosanitaire) dont le but est de développer un produit support destiné à être pulvérisé pour protéger les plantes des viroses. Le produit étudié est une émulsion de type eau-dans-huile (E/H) à base d’une solution aqueuse de polysaccharide et d’esterméthylique de colza comme phase continue. Le polysaccharide est utilisé sous forme d'adjuvant afin de modifier les propriétés rhéologiques de la préparation phytosanitaire (bouillie) et ainsi de limiter la dérive des gouttelettes lors de la pulvérisation. Le but est également d’améliorer le contact des gouttes sur le végétal traité. L'objectif de ce travail est de formuler une émulsion (E/H) avec une concentration maximale de polysaccharide, qui soit stable sur le long terme (environ 2 ans) et d'étudier, lors de la mise en œuvre du produit, les mécanismes de relargage dans un laps de temps efficace devant rester inférieur à 600 s. Les émulsions (E/H) concentrées ont été réalisées à l'aide d'un système rotor stator à température ambiante. La phase aqueuse contenant le polysaccharide et du glycérol a été dispersée dans une phase huileuse agitée dans laquelle un surfactant (lécithine ou PolyRicinoléate de PolyGlycérol, PGPR) a préalablement été dissous. Des tests de stabilité ont été menés immédiatement après les phases de préparation ou par un vieillissement accéléré. Différents paramètres qui ont une influence sur cette stabilité ont été étudiés par DSC, observations microscopiques, diffraction laser et mesure des propriétés rhéologiques. Les analyses DSC ont été utilisées poursuivre l'évolution de la taille des gouttes en fonction du temps. En effet, le comportement thermique des émulsions pendant les phases de congélation et de fusion permet de calculer la fraction d’eau congelée dans les gouttelettes et sa mise en relation avec l’évolution de la stabilité des émulsions. Le relargage du polysaccharide (CarboxyMethylCellulose, CMC) est obtenu en deux étapes : déstabilisation de l'émulsion primaire E/H par un produit chimique puis dilution dans l'eau pour obtenir une émulsion (H/E) avec la concentration désirée de polysaccharide dans la phase aqueuse. La déstabilisation a été étudiée en observant l'évolution des gouttelettes par DSC. Le procédé de dilution a été étudié par une mesure de la conductivité de la solution aqueuse couplée à un modèle cinétique de relargage du CMC.La formulation et la stabilité de l'émulsion (E/H) ont montré que la DSC, complétée par d'autres techniques, est une méthode appropriée pour déterminer les caractéristiques des émulsions. L'étude du comportement lors de la congélation montre que la proportion de glace formée dans les gouttelettes durant les tests DSC est en bonne adéquation avec les mesures DSC et les calculs thermodynamiques. L'utilisation du PGPR comme tensioactif et l'ajout du glycérol dans la formulation permettent d'augmenter la stabilité de l'émulsion à long terme. La formulation optimum obtenue contient 3.5 % (m/m) de CMC, 10 % (m/m) de glycérol dans 75 % (v/v) de phase dispersée et 14 % (m/m) de PRPG dans la phase continue. Un modèle empirique peut être utilisé pour décrire la cinétique de relargage. Pour déstabiliser l'émulsion (E/H), la quantité optimum de tensioactif anionique Cynthiorex PMH1125 est de 10 % (m/m) dans première émulsion avec NRe ≥ 4200 et T ≥ 20°C. Dans les conditions réelles d’utilisation de la préparation au champ, le temps minimum de relargage est d'environ 200 secondes. / This study is a part of the European project VEGEPHY (VEGEtale-PHYtosanitaire) to develop a product for the crop protection purposes. The product is a concentrated W/O emulsion trapping of a polysaccharide in the aqueous phase and rapeseed methyl ester oil as a continuous phase. Polysaccharide is used as a thickening adjuvant to modify the rheology properties of the water-based spray solution in order to reduce the drift of thespray. The objective of this study is to formulate concentrated W/O emulsions incorporation with the maximum amount of polysaccharide which show long stability (for over 2 years) and to study the release mechanism of polysaccharide in suitable conditions with a goal of an efficiency time less than 600 seconds.Concentrated W/O emulsions were realized by using a rotor stator system at room temperature. Aqueous phase containing polysaccharide and glycerol was dispersed into the stirred oil continuous phase where in a surfactant (lecithin and/or polyglycerol polyricinoleate, PGPR) has been previously dissolved. Stability tests were performed immediately after preparation and after ageing tests. Various parameters having an influence on thestability have been interpreted from DSC thermogram parallel with microscopic observation, laser diffraction granulometry and rheology measurement. DSC technique was used to study the emulsions by following the evolution of the droplet size versus time. Thermal behaviour of emulsions may be evaluated when they under gofreezing and melting in which the proportion of ice formed in the droplets may be calculated and their link with the evolution of the emulsion versus time. The release of the polysaccharide (CarboxyMethyl Cellulose, CMC)from the emulsion system is obtained by a two steps process : destabilization of the primary W/O emulsion by achemical product and dilution in water that gives an O/W emulsion containing the required concentration of polysaccharide. Destabilization was observed by following the evolution of dispersed droplets using DSC. Dilution process was assessed by measuring electrical conductivity of the water solution and a mathematical model to represent the kinetic release of CMC in water was proposed.The formulation and the stability of concentrated W/O emulsion has shown that DSC completed with granulometry and rheometry is an appropriate technique to study the emulsion characteristics. The study offreezing behaviour of emulsions show that the proportion of ice formed in the dispersed droplets during DSC test indicates good agreement between DSC measurements and thermodynamics calculation. The use of PGPRas surfactant and the introduction of glycerol in the formulation are beneficial to improve the long‐term stabilityof the emulsion. The optimum formulation of concentrated W/O emulsion was obtained containing : 3.5% w/wof CMC, 10% w/w of glycerol in 75% v/v of dispersed phase and 14% w/w of PGPR in the continuous phase. From the release study, an empirical model may be used to describe the released kinetic. The optimum amount of nonionic surfactant Cynthiorex PMH 1125 to break primary W/O emulsion was found at 10% w/w in the primary emulsion with NRe ≥ 4200 and T ≥ 20°C. Under practical field conditions, the minimum release time isthen around 200 seconds.

L’utilisation d’adhésifs polyépoxy et plus particulièrement de pâte de calage dans l’aéronautique est chose très courante. L’augmentation des cadences de production des aéronefs poussent les fournisseurs à adapter les temps technologiques de ces produits (temps d’application et de complète polymérisation) : ainsi, la cinétique de réticulation des adhésifs de demain devra être lente à température ambiante et pouvant être accélérée à tout moment. Pour cela, la piste envisagée pour ces tra-vaux est la polymérisation sous rayonnement infrarouge. La cinétique de ré-action a été évaluée par analyse thermique (DSC) ou par analyse spectrosco-pique (MIR ou PIR). Les résultats obtenus ont mis en évidence un effet thermique et non thermique du rayonnement infrarouge. Grâce à plusieurs expérimentations, les résultats montrent que le rayonnement infrarouge interagit avec les groupe-ments époxydes dont l’énergie d’activation de la réaction avec les amines primaires diminue. Par ailleurs, l’utilisation d’un plan d’expérience a permis de montrer que l’adhérence et les propriétés mécaniques de ces adhésifs augmentaient suite à l’utilisation du rayonnement infrarouge. / The use of polyepoxy adhesives and more particularly of liquid shim in aero-nautics is very common. The increase in aircraft production rates is pushing suppli-ers to adapt the technological times of these sort of products (application and complete curing times): thus, the curing kinetics of tomorrow's adhesives must be slow at room temperature and can be accelerated at any time. For this purpose, this work paves the way of an infrared curing. The reaction kinetics were evalu-ated by thermal analysis (DSC) or spectroscopic analysis (MIR or NIR). The results obtained showed a thermal and non-thermal effects of infrared radiation. Thanks to several experiments, the results show that infrared radiation interacts with epoxide groups whose activation energy with primary amines reaction decreas-es. In addition, by the use of Design of Experiment (DoE) showed that the ad-hesion and mechanical properties of these adhesives increased as a result of the use of infrared radiation.

A transmissão de dados e informação na fibra óptica vem aumentando nos últimos anos. O interesse para avaliar melhor a confiabilidade mecânica tomou-se uma necessidade, depois que uma fibra, de um cabo instalado, estava se partindo com muita facilidade. O foco principal deste trabalho foi voltado para estabelecer metodologias para avaliar o estado de degradação dos polímeros usados. Através destas técnicas, buscou-se encontrar parâmetros (E\', E\", tan &#948, Tg, etc.) que pudessem indicar o estado de degradação dos revestimentos. Diferentes técnicas foram empregadas para avaliar o revestimento das fibras tais como: calorimetria exploratória diferencial (DSC), diferencial fotocalorimetria (DPC), análise térmica dinâmico mecânico (DMTA) e espectroscopia na região do infravermelho (FIIR). A partir da técnica desenvolvida, DMTA, esta pode ser empregada para avaliar a confiabilidade mecânica de várias fibras comercias. As técnicas DMTA e FIIR mostraram ser muito promissoras, pois consegue-se, através delas, obter muitos dados a respeito das características dos polímeros. / The datas and information transmission in the optical fiber have been increasing in the last years. The interest to evaluate the mechanical reliability became necessary, after that a optical fiber, from a cable installed, was cracking very easily. The principal aim of this work was establishing methodologies to evaluate the polymer degradation state. Through of this techniques we search to find out parameters (E\', E\", tan &#948, Tg. etc) that could denote the degradation state of the coatings. Different techniques were utilized to evaluate the coating of the optical fibers such as: differential scanning calorimeter (DSC), differential photocalorimeter (DPC), dynamic mechanic thermal analyzer (DMTA) and infrared spectroscopy (FIIR). From the method development (DMTA), it was possible to evaluate the mechanical realiability of many commercial fibers. DMTA and FTIR techniques shown to be very promising to obtain very dates to respect of polymer characteristics.

Este trabalho tem por objetivo a caracterização comparativa do comportamento de degradação e/ou decomposição térmica da esponja sintética dupla face, base poliuretana (parte amarela e parte verde), e da palha de aço, a partir das técnicas termoanalíticas. As esponjas sintéticas para limpeza doméstica, em substituição à palha de aço, apesar da vantagem econômica, podem apresentar restrições de descartes para o meio ambiente ou expor o usuário a riscos de contaminação. Amostras de esponja sintética dupla face (verde e amarela) e de palha de aço foram caracterizadas por análise térmica (TG/DTG, DTA e DSC) empregando atmosfera dinâmica de ar e de N2. Essas amostras foram estudadas por métodos cinéticos por termogravimetria isotérmica e não isotérmica. Os parâmetros cinéticos obtidos permitiram estimar os tempos necessários para a decomposição de ambas as partes da amostra da esponja sintética e também da palha de aço sob atmosfera de ar. Os resultados evidenciaram claramente que a matriz polimétrica da esponja sintética para ser degradada completamente exige um tempo muito longo, acima de 20.000 anos. Por outro lado, os resultados indicaram comportamento similar entre as amostras de esponja sintética e de palha de aço considerando apenas o efeito temperatura e tipo de atmosfera. Contudo, no cotidiano sabe-se que a palha de aço se oxida muito facilmente sob atmosfera de ar na presença de umidade. / This work aims at a comparative characterization of degradation behavior and/or thermal decomposition of synthetic double-face sponge, polyurethane base (yellow part and green part), and steel wool, from thermoanalytical techniques. Synthetic sponges for household cleaning, replacing steel wool, despite the economic advantage, may have restrictions on discharges to the environment or expose the user to risks of contamination. Samples dual synthetic sponge face (green and yellow) and steel wool were characterized by thermal analysis (TG/DTG and DTA DSC) employing an atmosphere of air and N2. These samples were studied by kinetic methods isothermal and non-isothermal thermogravimetric analysis. The kinetic parameters obtained allowed the estimation necessary for decomposition of the sample both sides of the synthetic spomge and also of steel straw times under air atmosphere. The results clearly showed that polymetric matrix of synthetic sponge to be degraded completely requires a very long time, over 20,000 years. Moreover, the results showed similar behavior among synthetic sponge and steel wool sample considering only the effect of temperature and type of atmosphere. However, in daily life it is known that the steel wool oxidizes very easily under air atmosphere in the presence of moisture.