Mgr. Jan Fránek 2011: The optimization the production of selected medicinal substances The diploma thesis dealt with optimization of production of fingolimod by hydrogenation. During the optimization of production, there was reduction of benzylic hydroxygroup and nitrogroup of nitrofingotriol. Reduction of two different groups caused dividing process of hydrogenation into two phases. The original intention was to optimize production only in the autoclave, but the need of using acidic catalytical medium in first phase led to dividing the production into reduction in the reactor and following catalyzed hydrogenation, already in neutral conditions, in the autoclave. The way of preparation of active substance by using an autoclave had not been explored in detail before. Evaluation of optimization is a part of results. There are also production charges on pilot plant included in results. Because the results of procedure of the pilot unit were not uniform, it was necessary to continue in optimization even after finishing the production in pilot plant. Following procedure modified according to the latest experiments was passed to the operating process.

In this dissertation, we analyze the Life Cycle Assessment (LCA) of the Steam Sterilizer, popularly known as Autoclave. The LCA will help Getinge Sterilization AB to identify the stages of the life cycle of Autoclave model GSS-P 91413, which contributes more to the environmental footprint. We use the ISO 14040 LCA framework to conduct the Cradle to Grave boundary study of the Autoclave. The results have shown the use phase to be a dominant phase with almost 84% of carbon footprint. For Getinge to produce sustainable products and reach its long-term goal of becoming carbon neutral, they need to reduce its environmental footprint in every phase of the product life cycle. Thus, this report suggests the best way that the company can impact the changes to the users even though they have very little control over it. The results were obtained using the Sustainable Minds (SM 2013) software, which is ISO certified, henceforth the results are trustworthy. This Thesis has 8 parts: Introduction, Method, Theory, Results, Conclusion, Critical Review, References, and Appendices.

<p>QC 20150603</p>

Additively manufactured carbon fiber reinforced polymers (CFRP) are vastly studied for their remarkable mechanical properties compared to most other 3D printed materials. Different methods were employed to further increase mechanical performance of CFRP 3D printed parts. The objective of the study is to investigate the effect of autoclave postprocessing on the interlaminar shear behavior between 3D printed CFRP layers. 3D printed CFRP samples were processed with nine combinations of temperature and vacuum in an autoclave. Short beam shear (SBS) tests were performed to characterize the interlaminar shear strength (ILSS) of the samples after autoclave processing. Digital image correlation (DIC) was utilized to quantify the strain and failure mode of the samples during SBS tests. From SBS mechanical tests, the curing temperature and vacuum of 170 C and -90 kPa produced samples with the highest ILSS, 39 MPa, a 46% improvement compared to uncured samples. The observed failure modes were fracture and delamination. Little work in additive manufacturing has applied autoclave as a post-process procedure. This study aims to explore this technique and establish its viability in improving mechanical performance of 3D printed fiber-reinforced parts.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / This thesis aims to instigate the veterinary community to reflect on the theme, as well as to provide some concepts and information which may help in the diagnosis and also to fight against infection in hospitals, emphasizing the cats and dogs postsurgical infections. To do this, during six months the extrinsic and intrinsic factors related to the infection in cats and dogs in the surgical site in the Veterinary Hospital from the Federal University of Santa Maria (HVU-UFSM) were evaluated. This evaluation is described in the thesis in two papers. In the first paper the autoclave has been checked through chemical and biological tests accomplished every fortnight in the morning; all the tests presented a negative result for the bacterial growth, showing the process of sterilization is efficient. In the second paper the aim was to evaluate the frequency of infection in the surgical site of 156 animals that have underwent surgery at HVU-UFSM, which were submitted to elective and nonelective surgeries of soft tissues and orthopedic ones, without implants. The rate of infection for the surgical site was 1.3% and it is within the limits observed in literature. This way it is possible to conclude that the principles and the procedures used to control surgical infection in this institution are accomplished in an effective way, something that contributes for the low rates of infection in the surgical site. / Esta tese tem por objetivo instigar a comunidade médico veterinária a refletir sobre o tema, assim como disponibilizar conceitos e informações que possam auxiliar no diagnóstico e no combate das infecções hospitalares, com ênfase nas infecções pós-cirúrgicas de cães e gatos. Para isso, foram avaliados durantes seis meses os fatores extrínsecos e intrínsecos relacionados com a infecção no sítio cirúrgico de cães e gatos no Hospital Veterinário Universitário da Universidade Federal de Santa Maria (HVU UFSM). Esta avaliação está descrita na tese em forma de dois artigos. No primeiro artigo verificou-se a eficiência da esterilização por autoclavagem através de testes químicos e biológicos realizados quinzenalmente na primeira carga da manhã; todos os testes realizados geraram resultados negativos para o crescimento bacteriano, demonstrando a eficácia do processo de esterilização. No segundo artigo o objetivo foi avaliar a frequência da infecção no sítio cirúrgico de 156 animais operados na rotina do HVU UFSM, os quais foram submetidos a cirurgias eletivas e não eletivas de tecidos moles e ortopédicas, sem colocação de implantes. A taxa de infecção para o sítio cirúrgico foi de 1,3% e encontra-se dentro dos limites observados na literatura. Dessa forma conclui-se que os princípios e as práticas empregadas para o controle de infecções cirúrgicas nessa instituição, são realizados de maneira efetiva, contribuindo para os baixos índices de infecção no sítio cirúrgico.

Dans ce travail, le composé de structure apatite La9,33(SiO4)6O2+3x/2 (-0,2<x<0,27) a été synthétisé et caractérisé en vue d’applications comme matériau d’électrolyte dans les piles à combustible à conduction anionique (IT-SOFC) et potentiellement protonique (PC-SOFC).Des pastilles et membranes denses d’oxyapatite pure ont été élaborées à partir de poudres synthétisées par voie solide, mises en forme par pressage isostatique ou coulage en bande et thermocompression, et frittées à 1550°C. Les échantillons ont été caractérisés électrochimiquement par spectroscopie d’impédance complexe et semi-perméation à l’oxygène et à l’hydrogène. Les phases La2SiO5 et La2Si2O7, qui peuvent apparaître lors de la synthèse de l’oxyapatite, ont été élaborées selon un protocole similaire, afin de caractériser leurs propriétés de conduction anionique. Ces phases ont d’autre part été utilisées lors d’essais d’élaboration d’oxyapatite à microstructure orientée le long de l’axe c, par frittage réactif d’échantillons d’architecture multicouche composés initialement d’une alternance de bandes La2SiO5 et La2Si2O7.Des tests de protonation en autoclave, à 550°C et 50 bars de pression de vapeur d’eau, ont été réalisés afin d’étudier le mécanisme d’insertion des protons dans la structure de l’oxyapatite. Des analyses thermogravimétriques, effectuées sur les échantillons protonés, ont permis de localiser les espèces protoniques insérées (surface/cœur) et de faire une analyse semi-quantitative de ces dernières. Les pertes de masses observées sont d’autant plus importantes que le temps de protonation et la stœchiométrie en oxygène des échantillons sont élevés. Des caractérisations structurales par diffraction des rayons X et spectroscopie Raman ont mis en évidence une augmentation conséquente du volume de la maille et un élargissement des grands canaux de la structure, ainsi qu’un changement de symétrie et une augmentation du désordre au sein de ces derniers. Ainsi, il semble que l’insertion des protons dans l’oxyapatite se fasse de manière préférentielle à l’intérieur des grands canaux de la structure. / This work is devoted to the synthesis and characterization of apatite-type La9,33(SiO4)6O2+3x/2 (-0,2<x<0,27), as electrolyte material for Intermediate Temperature Solid Oxide Fuel Cells (IT-SOFC) and potentially Proton Conducting SOFC (PC-SOFC).Pure and dense oxyapatite pellets and membranes were prepared from powders synthetized by solid-state reaction and shaped by isostatic pressing or tape-casting process and thermocompression, then sintered at 1550�C. The electrochemical properties of the samples were characterized by complex impedance spectroscopy and O2 and H2 semi-permeation. La2SiO5 et La2Si2O7 phases, which may appear during the oxyapatite synthesis, were prepared following a similar process, in order to study their electrochemical properties. Theses phases were also used in an experiment whose purpose was to elaborate highly c-axis-oriented apatite-type lanthanum silicate polycrystals by combined use of tape casting and reactive diffusion between La2SiO5 and La2Si2O7.In order to study the protonation process of oxyapatite, tests were performed in autoclave with water at 550�C and 50 bars. Thermogravimetric analyses enabled to locate (surface/bulk) and to make a semi-quantitative analysis of inserted protonic species. The longer the protonation time and the higher the oxygen stoichiometry are, the greater the mass loss is. Moreover, structural studies by X ray diffraction and Raman spectroscopy revealed that the cell volume was increased and the channels of the structure enlarged, while the symmetry was modified and the disorder increased inside them. Thus, it appears that the protonic species insertion in oxyapatite takes place preferentially inside the channels of the structure.

L’introduction des matériaux composites à matrices thermoplastiques est étudiée depuis quelques années par les avionneurs. Les procédés actuellement investigués, soit par placement de mèches pré-imprégnées, soit par thermo-estampage de plaques préconsolidées, sont toutefois mal adaptés pour des pièces de forme complexe telles que des capotages, des volutes ou des entrées d’air. Pour s’affranchir de cette limitation, cette thèse vise à étudier une voie d’élaboration basée sur la mise en forme de textiles qui intègre par voie comélage/cotissage les renforts de carbone et les fils de thermoplastique. Le tout est suivi d’une consolidation en autoclave. Le projet de recherche comprend deux parties distinctes et complémentaires. La première partie est dédiée à l’étude de la mise en forme textile avant consolidation. La déformabilité en cisaillement des préformes textiles comélés a été caractérisée sur la base d’un essai « Bias Extension Test » instrumenté avec un dispositif optique pour mesurer les champs de déformation par corrélation d’images (2D-DIC). La mise en forme de la préforme textile sur des éprouvettes technologiques possédant une géométrie complexe de type double courbure a été effectuée à partir d’un pilote d’emboutissage. Une instrumentation optique a permis d’évaluer les champs de déformation en cisaillement (3D-DIC). La deuxième partie est consacrée à l’étude et à l’optimisation des conditions de consolidation en autoclave, des cycles de consolidation et l’étude de leur influence sur les performances mécaniques et la santé matière du matériau. Les relations matériau/procédé sont établies à partir de deux semi-produits FC/PPS : le Pipreg ® poudré de Porcher et le TPLF ® comélé avec fibres craquées de Schappe Techniques. Les résultats de ces deux thématiques ont permis la mise en oeuvre de pièces de faisabilité à double courbure aux propriétés microstructurales compatibles aux exigences aéronautiques pour des structures semi-structurelles. Une optimisation de la mesure de champ par stéréo- corrélation d’images et la prise en compte du comportement en tension et en flexion du renfort permettraient d’améliorer l’analyse des champs de déformation lors des essais de drapage. L’amélioration du cycle de consolidation et une sélection de produits d’environnement plus performants sont également des thématiques à explorer. / Thermoplastic resin composites have been studied for some years by aircraft manufacturer. Current processes studied concerning either prepreg bundle positioning or thermo-stamping of pre-consolidated laminates are not adapted for complex shape as air inlets. To overcome this limitation, this thesis investigates a method based on the manufacturing of fabrics made in commingled/co-woven yarns of carbon and thermoplastic fibres. Then fabrics are consolidated in autoclave. This research project has been divided into two distinct parts. The first part concerns textile shaping study before consolidation. Shear strains of textile preforms have been caracterized by « Bias Extension Test » instrumented with optical device to measure strain field by digital image correlation (2D-DIC ). Textile preform shaping on a double curvature technology test specimen was performed with stamping device. It was also intrumented by cameras to assess shear strain field (3D-DIC). The second part is focused on the study and the optimization of autoclave consolidation conditions and process parameters for thermoplastic composite part manufacturing. Process impacts on composite mechanical properties and microstructure are also studied. Material/process interactions assessment was performed with two CF/PPS semi-pregs : Pipreg ® powdered impregnated fabric from Porcher and TPLF ® commingled fabric with stretch-broken carbon fibers from Schappe Techniques. Results from these two research topics allow to manufacture double curvature composite parts with microstructural properties in accordance with aviation requirements for semi-structural parts. The optimisation of field measurements by 3D-DIC and the semi-preg characterisation in tensile and bending should be developed to improve strain field analysis during fabric shaping. Manufacturing process optimisation by the selection of more efficient materials used for vacumm bagging should also be investigated.

Resíduos de Serviços de Saúde (RSS), ainda que tratados e dispostos em aterros sanitários, podem ser causas de impactos ambientais por apresentarem algum indicador de periculosidade. Segundo o apêndice IV da Resolução da Agência Nacional de Vigilância Sanitária (Anvisa) RDC nº 306/2004, para as tecnologias de tratamento desses resíduos é necessário que se atinja pelo menos o Nível III de inativação microbiana. Perante a ausência de dados na literatura que revelassem o tempo de exposição, temperatura e pressão ideais para a inativação microbiana no tratamento de RSS por autoclavagem e se a fração ocupada dos resíduos na autoclave poderia interferir na eficiência da desinfecção definiu-se o objetivo do trabalho para otimização do processo. Para os testes foram utilizados endósporos de Geobacillus stearothermophilus como bioindicadores e instalados cinco termopares na autoclave para aferição da temperatura dentro de todo o espaço da câmara. O RSS foi sintetizado diante das caracterizações como composição gravimétrica, distribuição granulométrica, densidade específica aparente, massa específica aparente e teor de umidade. Apresentou-se uma proposta metodológica para a avaliação do tratamento de RSS frente às dificuldades encontradas. Realizou-se ensaios com 116ºC, 125ºC e 134ºC, observando a fração de inativação em seis tempos de exposição diferentes. Sabendo-se que é padronizada em estabelecimentos de saúde a temperatura ideal para esterilização de materiais de 121ºC, apesar de não terem sido encontrados trabalhos científicos que comprovem a eficiência da esterilização nessa circunstância, foram realizados testes a 50 e 60 minutos de exposição para avaliar essa condição. Inoculou-se 106 endósporos nas amostras e a recuperação foi feita com filtração após a lavagem dos resíduos, sendo realizada a técnica de pour plate para contagem das unidades formadoras de colônias (UFC). O mesmo procedimento foi feito com a amostra retirada da autoclave. A fração de inativação dos endósporos atingiu 100% no tempo de 30 minutos de exposição à temperatura máxima de 134ºC e pressão absoluta de 2,3 kgf/cm2, resultado obtido através da relação do número de micro-organismos recuperados considerados como inoculados e o número de micro-organismos sobreviventes ao tratamento. A 121ºC houve recuperação de UFC após tratamento. A fração de ocupação não foi um fator delimitante para a inativação de endósporos, pois a temperatura se manteve a mesma independentemente da quantidade de resíduo submetido à autoclavagem. Um outro objetivo era avaliar experimentalmente a reprodução dos micro-organismos frente às condições operacionais de autoclavagem e do tempo de permanência do rejeito em condições ambientais. Esse estudo comprovou que a inativação nessas condições otimizadas esteriliza o resíduo, sendo que nenhum micro-organismo voltou a se reproduzir após dias expostos em temperatura ambiente, ou seja, não haveria riscos de contaminação em aterro sanitário quando depositados os rejeitos. Ter encontrado essas condições ideais e avaliado o processo de autoclavagem pode significar um grande avanço nas próprias unidades de tratamento, que terão um parâmetro estabelecido para trabalho. / Healthcare waste, even when treated and disposed of in landfills, can be causes of environmental impacts because they present some hazard indicator. According to appendix IV of Resolution of the National Health Surveillance Agency of Brazil (Anvisa) RDC nº 306/2004, for technologies of healthcare waste treatment, it is necessary to achieve at least Level III of microbial inactivation. The purpose of this research to optimize the process was defined taking into account the absence of data in the literature that revealed the optimal exposure time, temperature and pressure for microbial inactivation through the healthcare treatment by autoclaving and whether the fraction occupied by waste in the autoclave could interfere with the effectiveness of the disinfection. For the tests, endospores of Geobacillus stearothermophilus were used as bioindicators and five thermocouples were installed in the autoclave for temperature measurement throughout the chamber space. The healthcare waste was synthesized by characterizations such as gravimetric composition, granulometric distribution, apparent specific density, apparent specific mass and moisture content. A methodological proposal for the evaluation of waste treatment was introduced taking into consideration the difficulties encountered. Tests were performed at 116ºC, 125ºC and 134ºC, observing the fraction of inactivation at six different exposure times. Since the sterilization of materials at 121ºC is standardized in health establishments, even though no scientific studies were found to prove the sterilization efficiency in these conditions, tests were performed at 50 and 60 minutes of exposure to evaluate this condition. The concentration of 106 endospores were inoculated in the samples and the recovery was done with filtration after washing the waste, and the \"pour plate\" technique was used to count the colony forming units. The same procedure was done with the sample removed from the autoclave. The inactivation fraction of the endospores reached 100% in the time of 30 minutes of exposure to the maximum temperature of 134ºC and absolute pressure of 2.3 kgf/cm2, a result obtained by the ratio of the number of recovered microorganisms considered as inoculated and the number of microorganisms surviving the treatment. At 121ºC there was recovery of colony forming units after treatment. The occupation fraction was not a limiting factor for the inactivation of endospores, since the temperature remained the same regardless of the amount of waste submitted to autoclaving. Another objective was to experimentally evaluate the reproduction of the microorganisms taking into consideration the operational conditions of autoclaving and the amount of time that the waste remains under environmental conditions. This study proved that the inactivation under these optimized conditions sterilizes the waste, and that no microorganism would reproduce again after days exposed at room temperature, therefore, there would be no risk of contamination in a landfill when the waste is deposited. Having found these ideal conditions and evaluated the autoclaving process can mean a major advance in the treatment units themselves, which will have an established parameter for work.

Este trabalho avaliou a influência da densidade de energia da pré-cura, e de diferentes tratamentos pós-cura na otimização das propriedades físicas (Resistência à Flexão e Dureza Knoop) de resinas compostas diretas, visando a possibilidade de indicação para restauraçoes indiretas. Foram usadas as resinas diretas Fillmagic, Concept, Glacier, Z100, Masterfill e W3D Master e as indiretas Solidex e Belleglass HP como controle. Para cada resina direta foram confeccionados 60 espécimes em barra (10x2x2mm), 30 irradiados em uma face e 30 nas duas faces (30 espécimes = 10 controle, 10 autoclave e 10 forno de luz). Para as resinas indiretas foram preparados 10 espécimes conforme processamento de seus fabricantes. 380 espécimes foram submetidos ao ensaio de resistência à flexão (Kratos). De cada condição experimental, 10 fragmentos foram usados para ensaio de microdureza Knoop (Shimadzu HMV-2). A análise de variância e o teste de Tukey demonstraram significância para resistência à flexão nos fatores Resina (p<0,001) e Tratamento (p=0,001) e na interação Resina x Tratamento (p=0,001). Para a microdureza Knoop os três fatores e as interações foram significantes: Resina (p=0,001); Face (p=0,001) Tratamento (p=0,017); Resina x Face (p=0,001); Resina x Tratamento (p=0,007); Face x Tratamento (p=0,001) e Resina x Face x Tratamento (p=0,024). A maior média de cada resina direta, independente da condição experimental, foi comparada às médias das resinas indiretas. Os resultados apontam que na resistência à flexão (Z100 = W3D = Fillmagic = Glacier) e (Z100 > Masterfill > Belleglass HP > Concept > Solidex). Na Dureza Knoop (Z100 > Belleglass HP, Fillmagic, W3D, Concept, Glacier, Masterfill e Solidex). Conclusão: as propriedades físicas (resistência à flexão e dureza Knoop) não são obstáculos na indicação de resinas compostas de uso direto para restaurações indiretas / This study evaluated the influence of pre-cure energy density, and additional post-cure treatments in optimizing the physical properties (Flexural strength and Knoop microhardness) of direct resin composites with the aim at allowing their use for indirect restorations. Direct resin composites evaluated were Fillmagic, Concept, Glacier, Z100, Masterfill and W3D Master; indirect composites were Solidex and Belleglass HP. Sixty bar-shaped specimens (10x2x2mm) were prepared for each material, so that 30 of them were light-cured by one surface and 30 on both surfaces. From the 30 specimens of each group, 10 were control, 10 were submitted to additional autoclave and 10 to light oven treatment. Ten specimens were prepared with each indirect composite following the manufactures’ recommendations. The 380 specimens were submitted to flexural strength test (Kratos universal testing machine), and values obtained at fracture were reported. After that, 10 fragments were chosen for each experimental condition and assessed for Knoop microhardness (Shimadzu HMV-2). Data were submitted to analysis of variance and Tukey’s test at p<0.05. Statistically significant differences were found among flexural strength results regarding composite materials (p<0.001), treatments (p<0.001) and interactions (composite x treatment, p<0.001). Regarding Knoop microhardness, both three factors and their interactions were also significant: composite (p<0.001), surface (p<0.001) and treatment (p<0.017), composite x surface (p<0.001), composite treatment (p<0.001), surface x treatment (p<0.001) and composite x surface x treatment (p<0.024). The highest mean value for each direct composite, regardless of the experimental condition, was compared to the mean values obtained for the indirect materials. With regard to flexural strength, comparisons point out that Z100 = W3D = Fillmagic = Glacier and Z100 > Masterfill > Belleglass HP > Concept > Solidex, whereas for Knoop microhardness Z100 > Belleglass HP, Fillmagic, W3D, Concept, Glacier, Masterfill and Solidex. Conclusion: considering the physical properties evaluated in this study, they are not an obstacle to the indication of direct composites for indirect restorations

Made available in DSpace on 2014-07-29T14:42:45Z (GMT). No. of bitstreams: 1 Dissertacao Marcos Humberto.pdf: 309390 bytes, checksum: 17847e7d57cdb47af008a9552ac17717 (MD5) Previous issue date: 2011-04-12 / Silicon is considered a beneficial element for plants and classified as a micronutrient. The use of Si brings innumerous for agriculture, particularly for grasses, up to now there are no reliable or efficient methodologies for quantifying available Si. Thus, methodologies able to quantify the available silicon in slags and fertilizers were evaluated. The aim of the work was to assess changes in the use of sodium carbonate + ammonium nitrate (NH4NO3 + Na2CO3) with disodium EDTA as extracting Si fertilizers through experiments with the cultivation of rice in an Oxisol and in a Haplortox Quartzipsamment soil typically displaced in a randomized design scheme in a green-house experiment in a factorial design with different sources, 5 Si extractors and 3 replicates. Extractions with four solutions were induced by autoclaving for 1 h at 121 °C in a water bath for 1:30 hours at 900 (± 30), also a standard Si extractor was used, consisting a solution that does not use an autoclave or water bath and rested for five days. The method using the autoclave was more efficient than the water bath and the best extracting solution was Na2CO3 0.1 mol L-1 + disodium EDTA 0.03 mol L-1 NH4NO3 and 0.2 mol L-1 / O Si (Silício) é considerado como sendo um elemento benéfico para as plantas e classificado como um micronutriente. Vários são os benefícios do Si para a agricultura, principalmente para as gramíneas, até o presente momento não existem metodologias confiáveis e eficientes para quantificar o Si disponível. Foram estudadas, então, metodologias capazes de quantificar o Si disponível em escória e fertilizantes. O objetivo do trabalho foi avaliar as variações do uso do Carbonato de Sódio + Nitrato de Amônio (Na2CO3+NH4NO3) com EDTA dissódico como extratores de Si em fertilizantes através de experimentos com a cultura de arroz em um Latossolo Vermelho distroférrico e um Neossolo Quartzarênico órtico típico, montado em delineamento inteiramente casualizado em casa-de-vegetação, com as soluções extratoras em esquema fatorial, com as diferentes fontes, 5 extratores de Si e 3 repetições. As extrações com as 4 soluções foram induzidas em autoclave por 1 h a 121º C e em banho-maria por 1:30 hora a 900 (±3º), além disso, foi utilizado o extrator S1 como padrão, que consistia em uma solução que não utilizou autoclave e nem banho-maria e repouso de 5 dias. O método utilizando a autoclave foi mais eficiente que o banho-maria e a melhor solução de extração foi com Na2CO3 0,1 mol L-1 + EDTA disódico 0,03 mol L-1 e NH4NO3 0,2 mol L-1.