Made available in DSpace on 2015-05-14T13:21:45Z (GMT). No. of bitstreams: 1 parte1.pdf: 2326464 bytes, checksum: edf040b92b5fdf343007a3626c02e26b (MD5) Previous issue date: 2009-02-19 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / The present work aimed at investigating the biodiesel issuing from the transesterification of used frying oil with ethanol, via alkaline catalysis. Such investigation covers its thermo-oxidative stability during heating (thermal analysis and rheological properties) as well the kinetic profiles of the samples in the best oxidative induction time by the technique of Pressurized Differential Scanning Calorimetry (PDSC). The behavior of such biodiesel, as part of binary blends with fossil diesel at the proportions of 3, 5, 10, 25, 50, 75 and 100%, was also studied. The biodiesel synthesis used the ethanol route and was carried out under the following conditions: oil/alcohol molar ratio of 1:6 (m/m), 1 % de KOH, temperature of 32 °C, washing with 0.1M HCl and hot water. The reaction yield, determined by means of a mass balance aided by the technique of gas chromatography coupled to mass spectrometry, was of 90.56% and the ester content was of 99.56%. According to the physicochemical analyses, all the specifications for the biodiesel and blends met the requirements from Technical Regulation # 7 from the Brazilian National Agency of Petroleum, Natural Gas and Biofuels, with the exceptions of the odixative induction time (1.72 h) and kinematic viscosity (6.10 mm2s-1), which displayed values outside the limits established by the standard. In the thermal study, the thermogravimetric curves showed that the biodiesel blends in diesel are more volatile than the biodiesel derived from used frying oil (B100), whereas at lower concentrations (3, 5, 10 and 25%) are similar to fossil diesel. At higher concentrations (50 and 75%) the blends presented lower volatility and higher thermal stability in relation to fossil diesel and thus, biodiesel and its more concentrated blends showed higher safety in relation to transport, storage, handling and utilization. The study of the fluid dynamic properties of biodiesel and its blends showed that all the samples behave as Newtonian fluids at the studied (10, 25 and 40 ºC) temperatures. Also the results of cloud point, pour point and cold filter plugging point showed that the behavior of the blends with 3, 5 and 10% are similar to fossil diesel, therefore at these concentrations biodiesel acts as a lubricity additive to fossil diesel. The study by Pressurized Differential Scanning Calorimetry (PDSC) in the dynamic mode and the Rancimat technique revealed that the best antioxidant for the storage of biodiesel is BHT at the concentration of 2500 ppm. The determination of the kinetic parameters by the isothermal PDSC technique allowed determining the theoretical value of the shelf life of used frying oil biodiesel with 2500 ppm of the antioxidant BHT. Therefore, used frying oil biodiesel and its blends B3, B5, B10, B25, B50 and B75 may be used as an alternative source of biofuels. / O presente trabalho buscou investigar o biodiesel proveniente da transesterificação do óleo de fritura usado com álcool etílico, via catálise básica, e elucidar a sua estabilidade termo-oxidativa durante o aquecimento (análise térmica e propriedade reologicas) e estudar o perfil cinético da amostra com o melhor tempo de indução oxidativa pela técnica de calorimetria exploratória diferencial pressurizada (PDSC). Também, foi observado o comportamento do referido biodiesel, inserido em misturas binárias com o diesel fóssil nas proporções de 3, 5, 10, 25, 50, 75 e 100% também foi estudada. A síntese do biodiesel na rota etanólica processou-se sob condições de: razão molar óleo-álcool de 1:6 (m/m), 1 % de KOH, temperatura de 32 °C, lavagem com HCl 0,1 M e água quente. O rendimento reacional determinado por balanço de massa com auxilio da técnica de cromatografia gasosa acoplada a espectrometria de massa, foi de 90,56 %, com teor de esteres de 99,56 %. Nas análises físicoquímicas, todos as especificações para ambos biodiesel e blendas satisfizeram as exigências dos limites permitidos pelo Regulamento Técnico nº 7 da Agência Nacional do Petróleo, Gás Natural e Biocombustíveis. Com exceção do tempo de indução oxidativa (1,72 h) e a viscosidade cinemática (6,10 mm2s-1) que apresentaram valores fora dos limites estabelecidos pela norma. No estudo térmico, as curvas termogravimétricas evidenciaram que as blendas de biodiesel em diesel são mais voláteis em relação ao biodiesel derivado de óleo de fritura usado (B100) e em baixas concentrações (3, 5, 10 e 25%) se assemelham ao diesel fóssil. Em concentrações mais elevadas (50 e 75%) as blendas apresentam menor volatilidade e maior estabilidade térmica em relação ao diesel fóssil, e, portanto, o biodiesel e suas blendas mais concentradas apresentam maior segurança em relação ao transporte, armazenagem, manuseio e utilização. O estudo das propriedades fluído-dinâmicas do biodiesel e suas blendas, demostraram que todas as amostras comportam como fluídos newtonianos a temperatura (10, 25 e 40 ºC) e que tanto os resultados de ponto de nevoa, fluidez e ponto de entupimento de filtro a frio, apresentaram comportamento para as blendas 3, 5 e 10% semelhantes ao observado para o diesel fossil, e, portanto nestas concentrações o biodiesel atua como um aditivo de lubricidade do óleo diesel fossil. O estudo por calorimetria exploratória diferencial pressurizada no modo dinâmico e a técnica de rancimat revelou que o melhor antioxidante para o armazenamento do biodiesel é o BHT com concentração de 2500 ppm. A determinação dos parâmetros cinéticos pela técnica de PDSC isotérmica foi possível determinar teoricamente o tempo de vida de prateleira do biodiesel derivado de óleo de fritura usado com 2500 ppm do antioxidante BHT. Então, o biodiesel de fritura usado e blendas B3, B5, B10, B25, B50 e B75 podem ser utilizados como uma fonte alternativa de biocombustíveis.

O composto SbxCoSb3-x foi produzido em altas pressões e altas temperaturas em uma reação de auto-inserção a partir da escuterudita binária CoSb3. A reação de auto-inserção é caracterizada pelo colapso de átomos de Sb para o sítio 2a, no interior das cavidades formadas pelos átomos de Co e Sb na estrutura da escuterudita. A reação inversa, de desinserção de Sb, ocorre quando o composto SbxCoSb3-x é aquecido à pressão ambiente. O acompanhamento desta reação de desinserção por meio de medidas de calorimetria exploratória diferencial (DSC), difração de raios X (DRX) e de resistividade elétrica constitui o objetivo principal deste trabalho. A amostra de CoSb3 foi sintetizada conforme rota proposta pela literatura. A síntese foi confirmada por meio de DRX, e não foi observada a presença de fases contaminantes. Amostras cilíndricas da fase SbxCoSb3-x foram obtidas submetendo CoSb3 a pressões de 7,7 GPa e temperaturas de até 550ºC, com o auxílio de prensas hidráulicas e câmaras toroidais disponíveis no Laboratório de Altas Pressões e Materiais Avançados LAPMA no Instituto de Física da Universidade Federal do Rio Grande do Sul IF/UFRGS. A presença da fase SbxCoSb3-x foi comprovada por meio de análises de DRX. Para determinação da resistividade elétrica de amostras ricas de fase SbxCoSb3-x foi desenvolvido um sistema DC, aplicável a amostras cilíndricas de pequeno volume tal como as obtidas em altas pressões e altas temperaturas. A aferição do sistema foi feita através de medidas de resistividade elétrica de materiais de referência (NIST-SRM 1461 e NIST-SRM 8426). As medidas de DSC revelaram a presença de dois eventos térmicos. Um pico endotérmico foi observado em 118ºC e não está associado a alterações estruturais e nem a variações significativas na resistividade elétrica. O evento exotérmico, que inicia em 180ºC, constitui a assinatura da desinserção dos átomos de Sb do interior da escuterudita, como verificado por análises de DRX e medidas elétricas. Após aquecimento até 350ºC, a amostra rica na fase SbxCoSb3-x retorna à fase estável, CoSb3. A reação de desinserção obedece a uma cinética de primeira ordem, cuja entalpia de transição é de aproximadamente 50 J /g e uma energia de ativação de 83 kJ/mol. A resistividade elétrica à temperatura ambiente de amostras ricas em SbxCoSb3-x é cerca de dez vezes inferior à do CoSb3. Este resultado, aliado possivelmente a uma baixa condutividade térmica, sugere que a fase de auto-inserção SbxCoSb3-x pode constituir um material termoelétrico de alto desempenho. / The compound SbxCoSb3-x was produced at high pressures and high temperatures in a self-insertion reaction from the binary skutterudite CoSb3. The self-insertion reaction is characterized by the collapse of Sb atoms to the 2a site, into the cage formed by the Co and Sb atoms in the skutterudite structure. The opposite reaction, i.e., Sb desinsertion, occurs when the SbxCoSb3-x compound is heated at room pressure. This desinsertion reaction was followed by means of differential scanning calorimetry (DSC), X-ray diffraction (XRD) and electrical resistivity measurements, and its study constitutes the main objective of this work. The CoSb3 sample was synthesized as described in the literature. The synthesis was confirmed by XRD, and the presence of contaminant phases was not observed. Cylindrical samples of the SbxCoSb3-x phase were obtained by submitting CoSb3 at pressures of 7.7 GPa and temperatures up to 550ºC, with the aid of a toroidal high pressure cell available at the Laboratório de Altas Pressões e Materiais Avançados - LAPMA in the Instituto de Física of the Universidade Federal do Rio Grande do Sul - IF/UFRGS. The presence of the SbxCoSb3-x phase was confirmed by XRD analysis. In order to determine the electrical resistivity of samples rich in SbxCoSb3-x phase, a DC system was developed which is applicable to small volume cylindrical samples such as those obtained at high pressures and high temperatures. The calibration of the DC system was made by measurements of the electrical resistivity of reference materials (NIST-SRM 1461 and NIST-SRM 8426). The DSC measurements revealed the presence of two thermal events. An endothermic peak was observed at 118ºC which is not associated to structural changes neither significant variation in the electrical resistivity. The exothermic event that starts at 180ºC is the signature of the desinsertion of Sb atoms from the skutterudite cage, as verified by XRD analysis and electrical measurements. After heating to 350°C, the sample rich in the SbxCoSb3-x phase converts back to the stable phase, CoSb3. The desinsertion reaction follows a first-order kinetics, with a transition enthalpy of approximately 50 J/g and an activation energy of 83 kJ/mol. The electrical resistivity at room temperature of samples rich in SbxCoSb3-x is about ten times smaller than that of CoSb3. This result, along with a possible low thermal conductivity, suggests that SbxCoSb3-x may constitute a high performance thermoelectric material.

Submitted by Divisão de Documentação/BC Biblioteca Central (ddbc@ufam.edu.br) on 2018-08-06T15:17:49Z No. of bitstreams: 1 DISSERTAÇÃO-Francisco Maciel de Brito Neto PPGCEM.pdf: 4657821 bytes, checksum: bfb975014ce10e6a646fdd1c54e9758b (MD5) / Approved for entry into archive by Divisão de Documentação/BC Biblioteca Central (ddbc@ufam.edu.br) on 2018-08-06T15:18:13Z (GMT) No. of bitstreams: 1 DISSERTAÇÃO-Francisco Maciel de Brito Neto PPGCEM.pdf: 4657821 bytes, checksum: bfb975014ce10e6a646fdd1c54e9758b (MD5) / Made available in DSpace on 2018-08-06T15:18:13Z (GMT). No. of bitstreams: 1 DISSERTAÇÃO-Francisco Maciel de Brito Neto PPGCEM.pdf: 4657821 bytes, checksum: bfb975014ce10e6a646fdd1c54e9758b (MD5) Previous issue date: 2018-05-17 / CNPq - Conselho Nacional de Desenvolvimento Científico e Tecnológico / Samples of samarium oxide (Sm2O3) and niobium oxide (Nb2O5) were submitted to Mechanical alloying technique and their structural evolution was accompanied by x-ray diffraction (XRD) measurements. In a few hours of milling SmNbO4 crystals were identified with two polymorphisms, one monoclinic and the other tetragonal. The diffractograms were simulated by Rietveld method and all crystallographic parameters were obtained, as well as the respective amounts of phases. The average crystallite sizes were estimated by the single-line method, indicating that both polymorphs have nanosized dimensions, that is, they are nanostructured. Combining calorimetric measurements, thermal treatments and x-ray diffraction the structural stability of the samples was studied. It was observed that the monoclinic structure undergoes phase transition to tetragonal structure in an exothermic process around 850 °C. The energy needed to promote the process was obtained by the Kissinger method and the XRD measurements indicate that the transition is irreversible. / Amostras de óxido de samário (Sm2O3) e óxido de nióbio (Nb2O5) foram submetidas à técnica moagem mecânica de alta energia e sua evolução estrutural foi acompanhada por medidas de difração de raios X (DRX). Em poucas horas de moagem foram identificados cristais de SmNbO4 com dois polimorfismos, um monoclínico e outro tetragonal. Os difratogramas foram simulados por método de Rietveld e todos os parâmetros cristalográficos foram obtidos, assim como as respectivas quantidades de fases. Os tamanhos médios de cristalitos foram estimados pelo método da linha única (single-line) indicando que ambos polimorfos possuem dimensões nanométricas, ou seja, são nanoestruturados. Combinando medidas calorimétricas, tratamentos térmicos e difração de raios x a estabilidade estrutural das amostras foi estudada. Foi observado que a estrutura monoclínica sofre transição de fase para estrutura tetragonal em um processo exotérmico em torno de 850°C. A energia necessária para promover o processo foi obtida pelo método de Kissinger e as medidas de DRX indicam que a transição é irreversível.

This work deals with the study of the influence of metallocene type polypropylene (mPP) molecular weight on isothermal crystallization of its nanocomposites filled with hydrophobic and hydrophilic nanosilica (1 and 2 vol.%). Real amount of nanosilica was determined by thermogravimetry. Isothermal crystallization was performed on differential scanning calorimeter (DSC) at 119–125 °C and observed in-situ under optical polarizing microscope (POM) at 128 °C using hot stage. The increase of mPP crystallinity degree in time was determined on DSC and spherulite type and growth rate was determined using POM. Supramolecular surface structure of the original and isothermally crystallited nanocomposites was observed directly or after chemical etching (mixture of mineral acids with KMnO4) on confocal laser scanning microscope. The crystal structure of mPP was in all tested materials verified by X-ray diffraction.

Les méthodes d’amélioration des procédures de cryoconservation sont traditionnellement basées sur l’empirisme. Pour s’en démarquer, nous sommes repartis des modèles biophysiques développés pour décrire les procédures en s’appuyant sur 2 méthodes. La 1ère méthode a consisté au développement de techniques de simulation des procédures en caractérisant l’utilisation du Snomax dans l’appareil DSC. Nous avons montré que le contrôle de la température de nucléation (Tn) est possible en choisissant les conditions expérimentales (volume d’échantillon et concentration en Snomax) qui influencent les probabilités de présence de 3 sous-populations d’INA des protéines de P. syringae. La possibilité d’effectuer des simulations a pu être validée pour certaines plages de surfusion dans les solutions de cryoconservation. Ceci a permis la caractérisation des effets physiques influencés par Tn et qui interviennent au cours des procédures et d’alimenter les modèles biophysiques de cryoconservation. La 2ème méthode a consisté à la modification de la composition des solutions afin de réduire le recours au DMSO (cytotoxique) en utilisant des composés de type oligosaccharides : les COS. Après vérification de la biocompatibilité des COS avec des cellules embryonnaires, la caractérisation de l’influence thermodynamique des COS a été effectuée. Il a été montré que les COS sont des cryostabilisateurs qui se lient à une petite quantité de molécule d’eau et n’en affecte pas les propriétés physicochimiques. Les COS peuvent donc être introduits dans le milieu extracellulaire sans risque d’accélérer la déshydratation cellulaire. De plus, il a été montré qu’ils favorisent la gélification du milieu extracellulaire, laquelle est fonction de la proportion massique d’eau en solution résiduelle. Cette gélification fige une partie du système ce qui favorise sa stabilisation au passage des zones de températures à risques de recristallisation / We wished to move aside classical cryopreservation procedure improvements that are based on empiricism and to focus on existing biophysical models in order to describe procedures. We based our study on two methods. The first method consisted in developing the methods for the simulations of procedures, by characterizing the use of Snomax in a DSC device. This study highlighted that the nucleation temperature (Tn) control is possible under precise experimental conditions (sample volume and Snomax concentration) that influence the presence probability of 3 INA subpopulations of the P. syringae protein aggregates. The possibility to simulate the cryopreservation procedures has been achieved for some supercooling ranges within complex cryopreservation solutions. Consequently, it has been possible to characterize the physical effects influenced by Tn and involved within procedures. These results will participate in supplying cryopreservation biophysical models. The second method aimed to modify the composition of cryopreservative solutions in order to reduce the DMSO use (because of its cytotoxicity), using extracellular CPA components: the chitooligosaccharides COS. Subsequent to the biocompatibility verification of the COS with embryonic cells, the thermodynamic influence of the COS has been characterized. Therefore, it has been demonstrated that COS are cryostabilizers that link themselves to a small number of water molecules and does not influence its physicochemical properties. Consequently, COS can be added within the extracellular space without any risk to accelerate the cell dehydration. It has been demonstrated that COS favor the gelation of the extracellular space and that this gelation relies on the mass proportion of water in the residual solution. This gelation immobilizes a part of the system and therefore favor its stabilization when the temperature reaches the risky recrystallization range

<p>Predmet istraživanja ove doktorske disertacije su bila halkogenidna stakla iz sistema Ag_x(As₄₀S₃₀Se₃₀)_100&ndash;x (x = 0, 0.5, 1, 2, 3, 4, 5, 10, 12, 13, 15 at. % Ag) &ndash; 3D forma i tanki filmovi preparirani iz prethodno sintetisanih stakala (x &le; 5 at. % Ag) &ndash; 2D forma.<br />Utvrđena je oblasti amorfnosti u faznom dijagramu po odabranom preseku.&nbsp; Ispitivan je uticaj procentualnog udela srebra&nbsp; na&nbsp; fizičke&nbsp; karakteristike sintetisanih stakala i prepariranih tankih filmova koje su&nbsp; od&nbsp; značaja&nbsp; za&nbsp; primenu&nbsp; ovakvih&nbsp; materijala.<br />Izvr&scaron;ena je karakterizacija električnih,&nbsp; optičkih, strukturnih&nbsp; i&nbsp; termičkih&nbsp; osobina&nbsp; na&nbsp; osnovu&nbsp; kojih&nbsp; su izvedeni&nbsp; zaključci&nbsp; o&nbsp; uticaju&nbsp; i&nbsp; modifikaciji&nbsp; strukture As₄₀S₃₀Se₃₀halkogenidne matrice usled inkorporacije atoma srebra. Strukturna analiza ispitivanih sastava je potvrdila homogenost uzoraka sa manjom koncentracijom srebra (x &le; 5 at. %&nbsp; Ag), dok je&nbsp; kod uzoraka sa većim procentualnim udelom ovog metala (x = 10, 13, 15 at. % Ag) pokazano da postoji fazna separacija. Kod sastava sa x = 13 i 15 at. % Ag potvrđena&nbsp; je&nbsp; prisutnost kristalnih centara AgAsSe_2. Na osnovu rezultata dobijenih DSC tehnikom, pokazano je da pri zagrevanju balk uzoraka dolazi do delimične kristalizacije koja se odvija zapreminski sa dvodimenzionalnim&nbsp; i&nbsp; trodimenzionalnim rastomkristalnih centara. Optička i spektralna ispitivanja su pokazala&nbsp; da uvođenje&nbsp; Ag&nbsp; u&nbsp; matricu&nbsp; stakla As₄₀S₃₀Se₃₀&nbsp; dovodi&nbsp; do&nbsp; smanjenja&nbsp; &scaron;irine&nbsp; optički zabranjene zone i kod 3D i 2D uzoraka, kao i da svi sastavi ispoljavaju normalan oblik disperzije indeksa prelamanja. Takođe, rezultati Raman&nbsp; spektroskopije su ukazali&nbsp; na&nbsp; činjenicu&nbsp; da&nbsp; inkorporacija&nbsp; srebra&nbsp; u strukturnu&nbsp; mrežu&nbsp; ispitivanih&nbsp; stakala&nbsp; utiče&nbsp; na formiranje Ag&ndash;(S,Se)&ndash;As veza, odnosno uzrokuje formiranje novih strukturnih jedinica koje bi mogle uticati na provodljivost ovih sastava.&nbsp; Merenja električnih karakteristika 3D uzoraka izvr&scaron;ena su u jednosmernom i naizmeničnom režimu i pokazano je da&nbsp; koncentracija&nbsp; srebra&nbsp; ima&nbsp; značajan&nbsp; uticaj&nbsp; na električne&nbsp; osobine.&nbsp; Utvrđeni&nbsp; su&nbsp; različiti&nbsp; mehanizmi odgovorni za transport&nbsp; nosilaca naelektrisanja zavisno od&nbsp; koncentracije dopanta.&nbsp; Kompleksni impedansni spektri svih sastava&nbsp; su&nbsp; ukazali&nbsp; na prisustvo temperaturske zavisnosti procesa relaksacije, na ne idealan Debye&ndash;vski tip relaksacije, kao i negativni temperaturski koeficijent otpornosti koji je karakterističan za poluprovodnike.</p> / <p>The subject of this dissertation are chalcogenide&nbsp; glasses from the system Agx(As₄₀S₃₀Se₃₀)_100&ndash;x (x = 0, 0.5, 1, 2, 3, 4, 5, 10, 12, 13, 15 at. % Ag) &ndash; 3D form and thin films prepared from previously synthesised&nbsp; glasses (x &le; 5 at. % Ag) &ndash; 2D form. The amorphous&nbsp; area in the phase diagram was determined by the&nbsp; selected&nbsp;&nbsp;&nbsp; tie&ndash; line. The influence of the silver&nbsp; percentage on the physical characteristics of the&nbsp; synthesized glasses and prepared thin films was&nbsp; investigated due to the importance of such materials&nbsp; for the application. Characterization of electrical, optical, structural and thermal properties has been performed, based on which conclusions on theinfluence and structure modification of the As₄₀S₃₀Se₃₀&nbsp; chalcogenide&nbsp; matrix due to the&nbsp; incorporation of silver atoms have been derived. Structural analysis of the investigated samples confirmed the homogeneity of samples with a lower silver concentration (x&nbsp; &le;&nbsp; 5&nbsp; at.%&nbsp; Ag),&nbsp; while&nbsp; in samples with a higher percentage content of&nbsp; this metal (x = 10, 13, 15 at.% Ag) it was shown that&nbsp; there was a phase separation. The presence of crystal&nbsp; centers AgAsSe₂ was confirmed in the samples with x = 13 and 15 at. % Ag. Based on the results obtained with the DSC technique, it has been shown that by heating the samples, partial crystallization takes place voluminously, with two&ndash;dimensional and three&ndash;dimensional growth of crystalline centers.&nbsp; Opticaland spectral investigations have shown that the introduction of Ag into the glass matrix As₄₀S₃₀Se₃₀ leads to a reduction in the optical band gap in both 3D and 2D samples, and that all compositions exhibit a normal dispersion of index of&nbsp; refraction. Also, the Raman spectroscopy results pointed to the fact that the incorporation of silver into the structural network of the investigated samples influences the formation of&nbsp; Ag&ndash;(S,Se)&ndash;As structures that is, causes the formation of new structural units that could affect the conductivity of these compositions. Measurements of the electrical characteristics of the 3D samples were performed in&nbsp; DC and AC regime and it was shown that silver concentration has a significant effect on electrical properties. Different mechanisms that are responsible for the transport of charge carriers depending on dopant concentration were determined. The complex&nbsp; impedance spectra of all compositions indicated the presence of the temperature dependence of the relaxation process, the non&ndash;Debye relaxation and the negative temperature coefficient of resistance which is characteristic of the semiconductors.</p>

The study of protein and surfactant interactions is of great significance in a number of applications, such as the cosmetic, food or pharmaceutical industries and many others. However, they require further study due to their compositional complexity and the limitations of current analytical approaches. In this thesis, the cationic surfactant septonex in combination with two differently charged proteins lysozyme and bovine serum albumin under different physiological conditions (temperature, surfactant concentration, environment and others) was selected to study the interactions. Characterization of protein-surfactant interactions is a very important but challenging task, therefore it is essential to use appropriate approaches to explore the nature of these interactions. In order to unify the information to provide rational models, calorimetric methods (DSC, ITC) and dynamic light scattering were used. Isothermal titration calorimetry monitors the evidence for the formation of the system of the mentioned substances and information on aggregation behavior, differential scanning calorimetry characterizes the thermal stability of proteins and dynamic light scattering made it possible to monitor changes in particle size. Both proteins have been proven to interact with positive septonex, even if the lysozyme molecule is also positively charged. However, significant differences were found between the two proteins. From the obtained results it is evident that the identical charge of the protein with the surfactant has an effect on the intensity of the measurement, although all measured interactions showed an endothermic character.

The presented diploma thesis deals with the evaluation of the influence of the addition of 30, 60 and 90 % of recycled material on the structure and mechanical properties of high-density polyethylene (HDPE), where recycled material represents both HDPE from a several years old part and material multiple reprocessed by extrusion. The changes of supramolecular structure were examined by calorimetric measurement, which did not indicate degradation of the material due to multiple extrusion. Mechanical properties were investigated by tensile tests and dynamic-mechanical analysis. Both measurements showed the same trend, where the first and second pass of the material through the extruder led to improved mechanical properties, e.g. to increase stiffness, while the influence of the third and fourth passes through the extruder had not a significant effect on the mechanical properties. In terms of the structure and mechanical properties, a positive effect of the combination of material after the second extrusion passing (30%) with virgin material was recorded.

Cíle této práce jsou: (i) vyhodnocení vlivu Y2O3 kelímku na kontaminaci indukčně tavené NiTi slitiny obohacené niklem, (ii) optimalizace podmínek, při kterých jsou tavby uskutečněny a (iii) získání nových DSC a 3D AP dat o vlivu vodíkové atmosféry na martenzitickou transformaci a na strukturu NiTi slitin obohacené niklem s tvarovou pamětí. Byly provedeny následující experimenty: – Pět taveb bylo navrženo a provedeno tak, aby byla snížena maximální tavící teplota. – Pět přetaveb bylo uskutečněno při teplotě 1500 C s dobou výdrže 2, 10 a 20 minut a při teplotách 1450 C a 1550 C s 20 minutovou dobou výdrže. Experiment byl navržen tak, aby byl vyšetřen vliv tavící teploty a doby výdrže na obsah kyslíku pocházejícího z kelímku Y2O3 v tavenině. – Tepelné zpracování NiTi slitiny obohacené niklem v režimu I (žíhání) a v režimu II (kombinace žíhání se stárnutím) pod atmosférou vodíku, směsi vodíku s héliem a pod referenční atmosférou čistého hélia. Získané výsledky jsou: – Navržené tavící postupy vedou ke snížení maximální tavící teploty a to z 1800 C na 1400 C. Přesto toto velké snížení maximální tavící teploty nevedlo k významnému poklesu obsahu kyslíku. – Během přetavby uskutečněné při teplotě 1500 C s dobou výdrže 2 minuty se obsah kyslíku navýšil o trojnásobek jeho počáteční hodnoty a příliš se nelišil od obsahu kyslíku naměřeného ve slitině, která byla přetavena při stejné teplotě s dobou výdrže 10 minut. K nárustu o čtyřnásobek počáteční hodnoty obsahu kyslíku došlo u přetavby vedené na teplotě 1450 C po dobu 20 minut a hodnota obsahu kyslíku se příliš nelišila od hodnoty naměřené ve slitině přetavené při teplotě 1550 C se stejnou dobou výdrže. – S rostoucím parciálním tlakem vodíku dochází k potlačení jednokrokové martenzitické transformace. Významný pokles výšky DSC píku nastává při parciálním tlaku 100 mbar. 3D AP analýza odhalila, že nedochází k žádné lokální změně koncentrace a nebo pozic niklových a titanových atomů ve vzorku, který byl žíhán v režimu I ve vodíku. Bylo objeveno, že vodík tvoří stabilní intersticiální tuhý roztok v NiTi B2 mřížce, kde vytváří systém nanodomén s obsahem vodíku vyšší než 10 at%.

The work deals with structrural and morphological characterization of polyamide buckles used to fasten webbins. The buckles were produced in five different years, a few of those produced in 2000 and 2004 were broken. The aime is to determine the type of polyamide and the cause of fracture of the buckles during using. The buckles were characterized in terms of structure and composition by Fourier-transform infrared spectroscopy in a mode of attenuated total reflaction, differential scanning calorimetry, thermogravimetry and X-ray diffraction. The buckles were made of polyamide 12. The broken buckles showed higher melting point, lower thermal stability and, in addition to modification it also contains modification, which is more fragile and probably represents the cause of fracture.