This master thesis deals with the optimization of the procedure of modification of hyaluronic acid structure for the use in the artificial synovial liquids. Based on the literature research, the amino acid alanine was used for the modification of carboxylic group in the glucuronic acid. The main subject of study is the improvement of the stability and mechanical properties of synovial liquid. DLS microrheology, macrorheology, thermogravimetric analysis (TGA), multi-angle light scattering with flow-field flow fractionation (AF4-MALS) and infrared spectroscopy (FTIR) were used for characterization. The theoretical part of this theses submits review of the musculoskeletal system, role of hyaluronic acid in metabolism and summary of synovial liquid. The experimental part focuses on the measurement of the stability and mechanical properties of three artificial samples (first with no modification, second with modified hyaluronic acid and third with modified hyaluronic acid and chondroitin sulphate). These samples were compared with real horse synovial fluid and artificial viscosupplement Orthovisc®.

This thesis is interested in new materials for lithium – ion batteries. Two different samples were investigated, one intercalation and one conversion cathode material. The theoretical part is focused to the structure of cells, their advantages and disadvantages compared to other secondary batteries. Also other materials used in batteries are described. The practical part describes the preparation of cathode materials for subsequent testing by scanning elektron microscopy and thermogravimetric analysis. In conclusions two different materials were evaluated and compared with each other.

Tato dizertační práce je napsána jako termoanalytická studie humifikovaných substrátů, tj. huminových látek a půdních vzorků, získaných z několika různých zdrojů tak, aby byl pokryt co nejširší rozsah primárních charakteristik. Práce hledá lineární korelace (s využitím Pearsonova korelačního koeficientu) mezi kinetikou termo-oxidační degradace (sledovanou pomocí termogravimetrie (TGA) a vyjádřenou konverzním časem stanoveným neizotermickou izokonverzní metodou) a standardními charakteristikami, jako je množství aromatického a karboxylového uhlíku přítomného v huminových látkách stanoveného spektroskopií nukleární magnetické rezonance (NMR). Hlavním cílem této práce je objasnit proces termo-oxidační degradace humifikované části přírodní organické hmoty a hledat závislosti mezi primární a sekundární strukturou huminových látek. Dalším úkolem je nalezení korelace mezi termogravimetrickým úbytkem hmotnosti půdních vzorků a jejich mikrobiální stabilitou měřenou v laboratorních experimentech jakožto půdní respirace (tedy uvolňování oxidu uhličitého). Účelem je zjistit, zdali vzájemné propojení vůbec existuje, a objasnit jaké druhy procesů, které provázejí půdní respiraci, je možné jednoduše odhalit pomocí TGA. Výsledky práce skýtají detailnější pohled na termickou analýzu půdních vzorků a jiných humifikovaných materiálů. Hlavním přínosem této práce je prezentace vyskytujících se aplikací termické analýzy pro charakterizaci půdní organické hmoty a dále také příspěvek k rozvoji aplikací technik termické analýzy v půdní vědě.

Orientador: Ivonete Ávila / Resumo: A biomassa apresenta-se como uma promissora alternativa aos combustíveis fósseis por ser renovável, de baixo custo e amplamente disponível. Esta pode ser obtida a partir de resíduos agroindustriais mostrando-se como um importante modelo de energia sustentável. Os principais componentes da biomassa são hemicelulose, celulose e lignina e, por possuírem diferentes propriedades químicas, influenciam diretamente na eficiência de um processo de conversão termoquímica. Metodologias convencionais atualmente aceitas na determinação dos principais componentes da biomassa requerem maior tempo e possuem alto custo. A análise termogravimétrica (TG) é uma técnica rápida e de baixo custo, resultando em curvas TG/DTG que fornecem uma indicação do percentual de cada um dos componentes da biomassa. Entretanto, não há uma metodologia aceita no sentido de substituir o método convencional por via úmida na determinação dos constituintes de materiais lignocelulósicos. Portanto, o objetivo deste estudo é avaliar o efeito da interação entre os componentes do bagaço e da palha de cana-de-açúcar (hemicelulose, celulose e lignina), isolados por diferentes tratamentos químicos, por meio da análise de sinergismo em ensaios termogravimétricos. Este estudo contribuirá para a elaboração de uma metodologia para determinação dos teores desses componentes por meio da análise termogravimétrica, com precisão similar aos métodos convencionais. Os resultados da caracterização química e a caracterização físico-quími... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Biomass presents itself as a promising alternative energy source to replace or reduce the use of fossil fuels because it is renewable, low cost and widely available. This can be obtained from agro-industrial waste, showing itself as an important model of sustainable energy. The main components of biomass are hemicellulose, cellulose and lignin and, due to their different chemical properties, they directly influence the efficiency of a thermochemical conversion process. Currently, the accepted methodologies for determining the main components of biomass require time and are expensive. Thermogravimetric analysis (TGA) is a fast and low-cost technique, resulting in TGA/DTG curves that provide an indication of the percentage of each biomass components. However, there is no accepted methodology in the sense to replace the conventional wet method use to determining the lignocellulosic materials components. Therefore, the objective of this study is to evaluate the effect of the interaction between the components of sugarcane bagasse and straw (hemicellulose, cellulose and lignin), isolated by different chemical treatments, through the analysis of synergism in thermogravimetric tests. This study will contribute to the development of a methodology for determining the content of these components through thermogravimetric analysis, with precision similar to conventional methods. The results of chemical characterization and physico-chemical characterization by FTIR and DRX technique of t... (Complete abstract click electronic access below) / Mestre

M.Tech. (Department of Chemistry, Faculty of Applied and Computer Sciences), Vaal University of Technology / This study reports the synthesis and characterization of cobalt oxide nanoparticles using a microwave technique and chemical precipitation with oxidation method. Cobalt complexes were prepared using carboxylic acids (acetic acid, heptanoic acid, and stearic acid) as ligands. The complexes were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric Analysis (TGA) and Elemental analyses (EA). Cobalt oxide nanoparticles were synthesized from the complexes via a microwave-assisted technique. A precipitation oxidation preparation reaction was used varying different parameters like pH, time, oxidising agent, heating method and cobalt precursor. The use of the cobalt nitrate and cobalt acetate as cobalt precursors resulted in spherical and cubic nanoparticles respectively. Cobalt precursors containing a longer hydrocarbon chain length, for instance cobalt heptanoate, did not yield cobalt oxide nanoparticles with the precipitation oxidation reaction due non- solubility of the complex. Using cobalt acetate as precursor, an increase in the pH from 7.91 to 10.18 caused the cobalt oxide nanoparticles shape to become well defined cubes with a narrower size range and CoOOH needles formed when the pH was further increased to 12.26. The optimum pH of 10.18 yielded cubic cobalt oxide particles having an average size of 25.45 nm with a standard deviation of 6.12. The nanoparticle size decreased from 35.70 nm to 4.45 nm when the oxygen oxidant was replaced with hydrogen peroxide. Conventional heating with a hotplate yielded nanoparticles with a more homogenous shape and size than microwave heating. The size of the nanoparticles increased from 22.81 nm to 25.45 nm when reaction time changed from 16 hours to72 hours.

The knowledge of kinetics of pyrolysis is important. It is also challenging to find parameters for kinetic which can be applied at different sizes of biomass. Many researchers have been investigating the pyrolysis behavior of wood powders due to heat and mass transfer limitations. They have also been focusing on determining the effects of feedstock characterization, residence time, gas environment, heating rate and the final temperature as well as the arrangement of the pyrolysis reactor and modeling of the kinetics. This project presents a qualitative understanding of the pyrolysis process based on data from slow heating rates. Samples of spruce chips at different masses, namely 4 mg, 200 mg, 500 mg and 800 mg and also 4 mg powder have been used in experiments with thermogravimetric analysis to understand the mass loss behavior. Furthermore, kinetic parameters for biomass are taken from literature and have been used in modeling to understand to which extent these parameters are different for different particle sizes. The kinetic model that is chosen to investigate in this project is where each component of biomass shows different characteristics during the thermal decomposition. The experimental results on wood chips at different sample masses show same behavior for all of them and there is no heat and mass transfer limitations. The results from experiments on powders shows different behavior than for chips at the end of the mass loss curve only. This means less char is produced for powders than it is for the chips. The results from modeling show that kinetic parameters such as activation energy and the prefactor are the same for both powders and chips. The only parameter that is different is the pre-determined char yield for hemicellulose second reaction. The kinetic model and the kinetic parameters used in this report are in good agreement to the experimental results. The model used, where each component show different behavior during its thermal decomposition and the final products are volatiles and char is a reliable model to describe the mass loss behavior of biomass. The difference in the experimental results between powders and chips can be explained by the modeling. It can be stated that the difference is in the char yield from thermal decomposition of hemicellulose. / Kunskap om kinetiken för pyrolysprocessen är viktig. Det är även en utmaning att finna parametrar för kinetiken som kan tillämpas till olika massor och storlekar av biomassa. Många forskare har undersökt pyrolys beteenden på bara träpulver på grund av värme- och massöverföring begränsningar. De har också fokuserat på att undersöka effekterna av råvara karakterisering, uppehållstid, gasmiljö, uppvärmningshastighet och den slutliga temperaturen samt arrangemanget av pyrolysreaktorn och modellering av kinetiken. I detta projekt presenteras en kvalitativ förståelse av pyrolysprocessen baserad på data från långsamma uppvärmningshastigheter. Prover av granflis vid olika massor; 4 mg, 200 mg, 500 mg och 800 mg och även 4 mg pulver har använts i experimenten med thermogravimetric analys för att förstå massförlust uppträdandet. Dessutom har kinetiska parametrar för biomassa tagits från litteratur och har använts i modelleringen för att förstå i vilken utsträckning dessa parametrar skiljer sig åt för pulver och flis. Den kinetiska modellen som har valts att undersökas i detta projekt är den där varje komponent av biomassa visar separata och olika egenskaper under termisk nedbrytning. De experimentella resultat på flis vid olika provmassorna uppvisar samma beteende för dem alla och det finns ingen värme- och massöverföringsbegränsningar. Resultaten från experiment på pulver visar annorluna beteende än för träflis endast i slutet av massförlust kurvan. Detta innebär att mindre kol produceras för pulver än vad det gör för flis. Resultaten från modelleringen visar att kinetiska parametrar såsom aktiveringsenergin och prefactor är densamma för båda pulver och flis. Den enda parameter som skiljer sig är den förutbestämda utbytet av kol för hemicellulosa’s andra reaktion. Den kinetiska modellen och kinetiska parametrar som används i denna rapport är i god överensstämmelse med de experimentella resultaten. Denna modell som används, där varje komponent visar enskilt beteende under dess termisk nedbrytning och slutprodukterna är bara gaser och kol, är en pålitlig modell för att beskriva beteendet för massförlust av biomassa. Skillnaden i de experimentella resultaten mellan pulver och flis kan förklaras av modelleringen. Det kan konstateras att skillnaden är i kol utbytet från sönderdelningen av hemicellulosa.

New resin-based composites and resin-infiltrated ceramics are used to fabricate computer-aided design (CAD) and computer-aided manufacturing (CAM)-based restorations, although little information is available on the long-term performance of these materials. The aim of this investigation was to determine the effects of storage time (24 h, 90 days, 180 days) on the thermophysical properties of resin-based CAD/CAM materials. Thermogravimetric Analysis (TGA), differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) were used in the study. TGA provided insight into the composition of the resin-based materials and the influence of internal plasticization and water sorption. Resin-based composites showed different decomposition, heat energy and mechanical behavior, which was influenced by storage time in water. Individual materials such as Grandio bloc showed lower influence of water storage while maintaining good mechanical properties.

No description available.

[pt] A demanda energética mundial está em constante crescimento e tal cenário faz aumentar a preocupação com os impactos ambientais, muitos deles decorrentes da exploração de combustíveis fósseis e sua utilização desmedida. Neste contexto, o estudo da pirólise da biomassa apresenta uma alternativa para a produção direta de calor que pode vir a ser utilizado em usinas termoelétricas sustentáveis. Uma investigação foi realizada abordando o tema da reciclagem de madeira sobre a possibilidade de aproveitá-la a biomassa principal deste processo. Este trabalho apresenta a caracterização da madeira reciclada bem como da madeira de eucalipto para poder averiguar a similaridade química entre as duas biomassas. Para tanto foram realizadas análises de espectroscopia de infravermelhos (FTIR) e difração de raios-X (DRX), além de análises de microscopia eletrônica de varredura com espectroscopia por dispersão de energia (MEV/EDS). Com o auxílio da técnica de termogravimetria (TG) foram realizados experimentos de pirólise lenta da madeira reciclada, a partir dos quais foram identificados eventos térmicos, caracterizados por perdas de massa. Para verificar um possível efeito oxidante dos óxidos Fe2CoO4 e Co3O4, realizou-se também pirólise lenta da mistura da madeira reciclada com cada um dos óxidos, tendo sido identificados eventos térmicos que não estavam presentes nos experimentos com a madeira pura. Os principais eventos foram avaliados cineticamente por métodos model-free que permitem a determinação da energia de ativação sem a necessidade de assumir uma ordem de reação. Foram utilizados os métodos de Kissinger (KS) e Kissinger-Akahira-Sunose (KAS), empregando os dados de experimentos realizados no TG com cinco taxas de aquecimento diferentes até 1100 graus Celsius. Para o evento térmico de maior importância, entre 200 e 390 graus Celsius tanto na madeira pura quanto na mistura, o ajuste de ambos o métodos foi satisfatório e está de acordo com a literatura. / [en] World s energy demand is constantly growing, and this scenario raises the concern about environmental impacts, many of them resulting from the constant manipulation of fossil fuels and their excessive use. In this context, the study of biomass pyrolysis presents an alternative for the direct production of heat that can be used in sustainable thermoeletric plants. To this end, a research has been carried out on the possibility of taking advantage of recycled wood as the main biomass of this process, an investigation that has been carried out along with a company in the field of wood recycling. This work presents the characterization of a recylced and a typical Brazilian eucalyptus wood with the purpose of proving their chemical similarity. Therefore, analysis of Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM/EDS), X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) was performed. Thermogravimetric (TG) experiments were carried out with slow pyrolysis of recycled wood and eucalyptus wood, from wich were identified thermal events, characterized by mass losses. To verify a possible oxidative effect of the compounds Fe2CoO4 and Co3O4, slow pyrolysis of a mixture of the recycled wood with each of the oxides was also performed, and thermal events that were not present in the experiments with the pure wood were identified. The main thermal events were kinetic investigated with model-free methods wich allows the determination of the activation energy without the need of a reaction order pre-stipulated. In this workk were tested the Kissinger (KS) and Kissinger-Akahira-Sunose (KAS) model-free methods and the TG data of five different heating rate were collected until 1100 Celsius degrees. For the most relevant thermal event, wich occurs from 200 to 390 Celsius degrees (for recycled wood and its mixture with the oxides) the adjustment of both methods was fine and accordance with literature.

Concrete is the most widely used man-made material in the world. Its versatility, strength, and relative ease of construction allow it to be used in the majority of civil infrastructure. However, concrete production plays a significant role in greenhouse gas emissions, accounting for around 8% of CO2 emissions worldwide. This thesis aims to reduce the demand for cement in concrete construction, thus reducing the carbon footprint of the concrete, by focusing on classifying and determining the effectiveness of seven different quarry by-products as partial replacements of cement. Several methods were utilized in this study to characterize the quarry by-products: particle size distribution, helium pycnometry, X-Ray diffraction, X-Ray fluorescence, scanning electron microscopy, and a modified ASTM C1897 Method A that utilizes isothermal calorimetry and thermogravimetric analysis. These various methods allowed for the determination of the physical properties (e.g., gradation, specific gravity, and morphology) and the chemical properties (e.g., mineralogy and reactivity in a cementitious system). The quarry by-products were classified as four granites, two limestones, and one greenstone. These quarry by-products were found to be non-pozzolanic and non-hydraulic. However, there are indications that there may be reactions with the various clays and feldspars in the quarry by-products with calcium hydroxide, which suggests a degree of reactivity that is not necessarily pozzolanic or hydraulic. / Master of Science / Concrete is the most widely used man-made material in the world. Its versatility, strength, and relative ease of construction allow it to be used in the majority of civil infrastructure. However, concrete production plays a significant role in greenhouse gas emissions, accounting for around 8% of CO2 emissions worldwide. This thesis aims to reduce the demand for cement in concrete construction, thus reducing the carbon footprint of the concrete, by focusing on classifying and determining the effectiveness of seven different quarry by-products as partial replacements of cement. Several methods were utilized in this study to determine the physical properties (e.g., gradation, specific gravity, and morphology) and the chemical properties (e.g., mineralogy and reactivity in a cementitious solution) of the materials. The quarry by-products were classified as four granites, two limestones, and one greenstone. In general, these quarry by-products were not found to be reactive as a supplementary cementitious material, although the data may suggest some degree of reactivity between calcium hydroxide and the clays and/or feldspars in the quarry by-products.