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Elaboration et caractérisations de silicium polycristallin par cristallisation en phase liquide du silicium amorphe / Formation and characterizations of polycristalline silicon produced by liquid phase crystallization of amorphous siliconSaid-Bacar, Zabardjade 13 February 2012 (has links)
L’objectif de ce travail de thèse est l’élaboration du silicium polycristallin en phase liquide, sur substrat de verre borosilicate, en utilisant l’irradiation par laser continu de forte puissance d’un film de silicium amorphe. Des simulations numériques modélisant l’interaction laser-silicium amorphe ont été effectuées grâce à un modèle que nous avons développé sur l’outil COMSOL. Nous avons ainsi pu suivre l’évolution des transferts thermiques dans les différentes structures Si/verre irradiées par laser et ainsi pu évaluer l’impact des paramètres expérimentaux tels que la vitesse de balayage, la puissance du laser, la température du substrat sur les seuils de transition de phase du Si amorphe (fusion, cristallisation, évaporation). Ces résultats de simulation ont été confrontés à des données réelles obtenues en réalisant différentes expériences d’irradiation de films Si amorphe. Les résultats de cette comparaison ont été largement discutés. Dans une deuxième partie, nous avons étudié les propriétés structurales et morphologiques de films Si polycristallin obtenus par l’irradiation laser de films Si amorphe. En particulier, nous avons mis en évidence les effets de la présence d’impuretés tels que l’hydrogène ou l’argon présent dans les couches Si amorphe préalablement au traitement laser. Nous avons également montré que la croissance des cristaux silicium s’opère par épitaxie à partir d’un effet de gradient thermique latéral et longitudinal, produit respectivement par le profil énergétique du faisceau laser et la diffusion thermique par conduction, et par convection thermique dans la direction de balayage. L’optimisation des conditions opératoires nous a permis de réaliser des films Si polycristallin à larges grains, jusqu’à plusieurs centaines de µm de long sur plusieurs dizaines de µm de large. Ces structures sont très intéressantes pour des applications en électronique et en photovoltaïque. / The objective of this thesis is the elaboration of polycrystalline silicon, on borosilicate glass substrate, by a Continuous Wave laser annealing of amorphous silicon operating in the liquid phase regime. Numerical simulations of the laser-amorphous silicon interaction have been carried out using COMSOL tool. We were able to monitor the evolution of the heat transfer in the different laser irradiated Si/glass structures. Thus, we have evaluated the effects of experimental parameters such as the scan speed, the laser power, the substrate temperature on the phase transition thresholds (melting, crystallization, evaporation). The modeling data were compared to the experimental data obtained on laser irradiated amorphous Si films, and the results were thoroughly discussed. In a second part, we have investigated the structural and morphological properties of polysilicon films prepared by CW laser irradiation of different amorphous silicon. We have shown that the presence of impurities such as hydrogen or argon in the amorphous silicon affects strongly the quality of the formed polysilicon film. We also found that the Si crystal growth occurs epitaxially from lateral and longitudinal thermal gradient produced respectively by the laser beam profile and thermal conduction, and by thermal convection in the scanning direction. The optimization of the experimental procedure led to the formation of polysilicon films with large grains up to several hundred microns long and tens microns in width. Such materials are of great interest to electronic and photovoltaic devices.
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Avaliação de microtécnicas de extração para análise de lamotrigina em plasma de pacientes epilépticos por eletroforese capilar / Evaluation of microextraction techniques to analysis of lamotrigine in plasma samples of epileptic patients by capillary electrophoresisBarros, Luiza Saldanha Ribeiro 23 March 2016 (has links)
A lamotrigina (LTG) é um fármaco pertencente à classe das feniltriazinas utilizado no tratamento de crises epilépticas generalizadas e focais e no tratamento adjunto da epilepsia refratária. Devido à alta variabilidade interindividual, às interações medicamentosas e aos efeitos adversos apresentados durante a administração da LTG, a monitorização terapêutica nos pacientes que fazem uso deste fármaco é necessária para ajuste de dose individual e evitar os efeitos adversos. Assim, o objetivo deste trabalho foi a avaliação de duas técnicas de microextração: a microextração em fase líquida com fibras ocas (HF-LPME) e a microextração líquido-líquido dispersiva (DLLME) para análise da lamotrigina em amostras de plasma de pacientes epilépticos. Primeiramente foram definidas as condições eletroforéticas: foi utilizado um capilar de sílica fundida de 75 ?m de diâmetro interno e 50 cm de comprimento efetivo. O eletrólito de corrida (BGE) foi composto por ácido 2-morfolinoetanosulfônico (MES), na concentração de 130 mmol L-1 e pH 5,0. As análises foram realizadas à temperatura de 20°C e tensão de 15 kV. A amostra foi injetada hidrodinamicamente (0,5 psi por 10 s) e a detecção foi feita em 214 nm. Nestas condições a LTG e o padrão interno (PI), lidocaína, puderam ser analisados em menos de 7 minutos. A HF-LPME foi avaliada no modo de 3 fases, usando 500 ?L de plasma e 3,5 mL de solução fosfato de sódio 50 mmol L-1 pH 9,0 como fase doadora. O solvente utilizado para impregnar a fibra foi o 1-octanol. Como fase aceptora foram utilizados 60 ?L de solução de ácido clorídrico pH 4,0. Para avaliação da DLLME, foi necessária uma etapa de pré-tratamento da amostra (500 ?L de plasma) com 1 mL de acetonitrila. Após isto, 1,3 mL do sobrenadante foram adicionados a 4 mL de solução fosfato de sódio 50 mmol L-1 pH 9,0 e 120 ?L de clorofórmio (solvente extrator) foram injetados nesta amostra aquosa e 165 ?L de fase sedimentada foram recuperados. As características de desempenho analítico para ambos os métodos foram avaliadas, sendo obtida linearidade na faixa de concentração plasmática de 1-20 ?g/mL e limite inferior de quantificação (LIQ) de 1 ?g mL-1. Os ensaios de precisão e exatidão apresentaram valores de acordo com os guias oficiais. Além disso, os métodos foram seletivos, não apresentaram efeito residual e as amostras foram estáveis. Os valores de recuperação foram de 54,3 e 23% para HF-LPME e DLLME, respectivamente. Os métodos validados foram aplicados com sucesso em amostras de plasma de pacientes epilépticos em tratamento com a LTG. Além disso, as duas técnicas foram comparadas e a HF-LPME apresentou vantagens em relação à DLLME, mostrando ser uma técnica promissora para análise de matrizes complexas, com reduzido consumo de solvente orgânico e possibilidade de automação. / Lamotrigine (LTG) is an antiepileptic drug, which belongs to the class of phenyltriazine that can be used in the treatment of new-onset and refractory epilepsy. Due to its high interindividual variability, drug interactions and the adverse effects presented during the LTG administration, therapeutic drug monitoring is very important to dose adjustment and to avoid toxicity effects. Thus, the goal of this study was to develop and validate two microextraction techniques: the hollow fiber liquid-phase microextraction (HF-LPME) and the dispersive liquid-liquid microextraction (DLLME) to analyze LTG in plasma samples of epileptic patients. First of all, the eletroforetic conditions were optimized. A fused-silica uncoated capillary with 75 ?m internal diameter, and 50 cm effective length was used. The 2-(N-morpholino)ethanesulfonic acid (MES) 130 mmol L-1 pH 5.0 was chosen as background electrolyte (BGE). The temperature and the voltage were kept constant at 20°C and 15 kV respectively. For sample injection, hydrodynamic injection mode was used, with a pressure of 0.5 psi applied for 10 s. The wavelength was set at 214 nm. Under final conditions, LTG and the internal standard (IS) lidocaine were analyzed in less than 7 minutes. HF-LPME was evaluated in the three phase mode. The analyte was extracted from 4.0 mL of a basic donor phase (composed of 500 ?L of plasma and 3.5 mL of sodium phosphate solution 50 mmol L-1 pH 9.0) into an organic phase composed of 1-octanol immobilized in the pores of the hollow fiber, and further into an acidic acceptor phase (hydrochloric acid solution pH 4.0) placed in the lumen of the fiber. To evaluate DLLME, the plasma samples were pretreated to remove the proteins, and 500 ?L of plasma sample was mixed with 1 mL of acetonitrile. After that, 1,3 mL of the upper layer was added to 4 mL of sodium phosphate solution 50 mmol L-1 pH 9.0, and 120 ?L of chloroform (extracting solvent) was rapidly injected in the aqueous sample and 165 ?L of the sedimented phase was collected. Under the optimized conditions, both methods were linear over the plasmatic concentration range of 1.0-20.0 ?g mL-1 and the lower limit of quantification (LLOQ) was 1.0 ?g mL-1. Both methods showed good precision, accuracy, selectivity to LTG, with no carryover and the samples were stable under the studied conditions. The recovery were 54,3 and 23% to HF-LPME and DLLME respectively. The validated methods were successfully applied for the quantification of LTG in plasma samples of epileptic patients. The techniques were compared and HF-LPME was more advantageous for being more suitable to analysis of complex matrices using small amount of organic solvent, and also can be automated.
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2D materials : exfoliation in liquid-phase and electronics applications / Matériaux bidimensionnels : exfoliation en milieu liquide et application en électroniqueEredia, Matilde 24 May 2019 (has links)
Cette thèse est consacrée à la production de matériaux 2D en phase liquide, en utilisant des approches pouvant permettre la production en masse de graphène et de matériaux apparentés. Notre objectif est de surmonter certains problèmes critiques pour le traitement et l'utilisation pratique des encres à base de matériaux 2D et de fournir une compréhension approfondie de la relation structure-propriétés dans ces matériaux, constituant des étapes obligatoires pour leurs applications futures. Cette thèse porte principalement sur l'UILPE et l'exfoliation électrochimique du graphène et du disulfure de molybdène (MoS2), qui ont été choisis comme matériaux prototypes à 2 dimensions. Les approches synthétiques sont combinées à une caractérisation physico-chimique des matériaux produits, à l'aide de techniques telles que l'AFM, la microscopie électronique, la spectroscopie XPS et Raman, ainsi qu'à une caractérisation électrique. Des applications dans le domaine de la détection et de l'électronique ont été explorées et ont permis de démontrer que des approches d'exfoliation en phase liquide pouvaient être utilisées pour obtenir un contrôle précis des propriétés des matériaux 2D ouvrant la voie à leur intégration en tant que matériaux actifs dans de nouveaux dispositifs multifonctionnels. / This thesis is devoted to the production in liquid-phase of two-dimensional materials, by using approaches that may enable mass production of graphene and related materials. We aim to overcome some issues that are critical for the processing and practical use of 2D materials-inks and to provide a deep understanding of the structure-properties relationship in such materials being mandatory steps toward their future applications. This thesis mainly focuses on ultrasound-induced liquid-phase exfoliation and electrochemical exfoliation of graphene and molybdenum disulfide, which have been chosen as prototypical 2D materials. The synthetic approaches have been combined with a multiscale physico-chemical and electrical characterization of the produced materials, by employing techniques such as AFM, XPS and Raman spectroscopy. Applications in the field of sensing and electronics have been explored and allowed to demonstrate that liquid-phase exfoliation approaches can be conveniently employed to achieve a fine control on the properties of 2D materials paving the way to their integration as active materials in novel multifunctional devices.
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Croissance de couches minces de silicium pour applications photovoltaïques par epitaxie en phase liquide par évaporation du solvant / Growth of si thin films by isothermal liquid phase epitaxy driven by solvent evaporation for pv applicationsGiraud, Stephen 01 December 2014 (has links)
Une solution pour réduire la consommation de Si de haute pureté dans les cellules solaires à base de Si cristallin est de faire croître une couche active mince de haute qualité sur un substrat à faible coût. L'Epitaxie en Phase Liquide (EPL) est l'une des techniques les plus appropriées, car la croissance est réalisée dans des conditions proches de l'équilibre. On s'intéresse plus particulièrement au développement et l'optimisation d'une technique de croissance stationnaire et isotherme basée sur l'évaporation du solvant : l'Epitaxie en Phase Liquide par Evaporation d'un Solvant métallique (EPLES). Les principaux critères concernant le choix du solvant, de l'atmosphère de croissance et du creuset sont d'abord présentés et permettent de concevoir une première configuration d'étude. Un modèle analytique est ensuite développé pour comprendre les mécanismes mis en œuvre et étudier la cinétique d'évaporation du solvant et de croissance. Les différentes étapes du procédé de croissance dans le cas de l'EPLES de Si sont examinées et mettent en évidence un certain nombre de difficultés technologiques liées à cette technique : contrôle de la convection dans le bain, réactivité du bain Si-M avec le creuset, transport par différence de température et dépôt pendant la phase de refroidissement. Des solutions techniques sont proposées et mise en place pour contourner les difficultés rencontrées. Des couches épitaxiées de Si uniformes comprises entre 20 et 40 µm sont alors obtenues par EPLES avec des bains Sn-Si et In-Si sur substrat Si monocristallin entre 900 et 1200°C sous vide secondaire. Les vitesses de croissance expérimentales atteintes sont comprises entre 10 et 20 µm/h et sont conformes aux prédictions du modèle cinétique. La qualité structurale obtenue est comparable à celle des couches obtenues par EPL. Des couches de type P, avec un bain dopé In et In(Ga) sont obtenues avec une concentration en dopants proches de 1017 at.cm3 compatible avec une application PV. Enfin le potentiel de l'application de cette technique est évalué en basant la discussion sur la réalisation d'une couche de Si obtenue par EPLES sur substrat multicristallin avec un bain In-Si. / Crystalline Si thin films on low-cost substrates are expected to be alternatives to bulk Si materials for PV applications. Liquid Phase Epitaxy (LPE) is one of the most suitable techniques for the growth of high quality Si layers since LPE is performed under almost equilibrium conditions. We investigated a growth technology which allows growing Si epitaxial thin films in steady temperature conditions through the control of solvent evaporation from a metallic melt saturated with silicon: Liquid Phase Epitaxy by Solvent Evaporation (LPESE). We studied the main requirements regarding selection of solvent, crucible and growth ambient, and a first experimental set up is designed. An analytical model is described and discussed, aiming to predict solvent evaporation and Si crystallization rate. Growth experiments are implemented with a vertical dipping system. Growth procedure is presented and the influence, on Si growth, of melt convection, temperature gradient in the melt and Si-M reactivity with the material crucible are discussed. Solutions are proposed to improve and optimise the growth conditions. Experimentally, Si thin films were grown from Sn-Si and In-Si solution at temperatures between 900 and 1200°C under high vacuum. We are able to achieve epitaxial layers of several micrometers thickness (20-40µm). The predicted solvent evaporation rate and Si growth rate are in agreement with the experimental measurements. Regarding the structural quality, it is comparable to the crystal quality of layers grown by LPE. With In and In(Ga) melts, we can obtain P-type epitaxial layers with doping level in the range 1017 at.cm3, which is of great interest for the fabrication of solar cells. Finally, the growth of Si thin films on multicrystalline Si substrates by LPESE is discussed to assess the potential application of this technique.
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Heterojunctions of Zinc Selenide and Zinc Sulfide on Titanium Oxide Nano Particles and Their PhotocatalysesShih, Tsung-Hsiang 22 December 2006 (has links)
High quality ammonium oxofluorotitanate discoid crystal is successfully grown on glass with an aqueous solution of ammonium hexafluorotitanate and boric acid at the molar ratio of 0.6. The concentration of hydrofluoric acid is less on the glass substrate surface and enhances the ammonium oxofluorotitanate nucleation growth. The growth rate is much higher than that grown on dioctadecyldimethylammonium. From the examinations of X-ray diffraction and high-resolution transmission electron microscopy, the crystal shows high crystalline quality and uniformity. Each titanium oxide octahedral is linked with fluorine and nitrogen atoms. Therefore, ammonium oxofluorotitanate has high potential to be thermally decomposed into high crystalline fluorine and nitrogen co-doped titanium oxide.
A simple process for the preparation of nanocrystalline anatase phase titanium oxide converted from ammonium oxofluorotitanate by thermal treatment was developed. The nanocrystalline anatase phase titanium oxide shows a large bandgap reduction due to the co-doping of high concentrations of fluorine and nitrogen. Due to the excellent nanocrystalline quality and the co-doping of higher concentrations of fluorine and nitrogen at the thermal treatment temperature of 800 OC, it is 1.3 times the photocatalytic activities of P-25 due to the visble region usage of Hg lamp light source. The 11.2 times the visible photocatalytic activities of P-25 using blue light-emitting diode as the light source is obtained from thermal treatment temperature of 600 OC. There is one to one correspondence between carrier lifetime and photocatalytic activity. As a result, a highly reactive and visible-light-driven photocatalysis is achieved.
The heterostructure of zinc selenide/titanium oxide and zinc sulfide/titanium oxide were prepared by metal-organic chemical vapor deposition on the above-prepared titanium oxide. The energy bandgap of zinc sulfide is much larger than that of titanium oxide and can act as a window for titanium oxide. It would not hinder titanium oxide absorption and preserve the role of fluorine and nitrogen co-doping. The energy bandgap of zinc selenide is near the maximum intensity of solar spectrum and acts as a sensitizer of titanium oxide. The lifetime of electron and hole pairs of heterostructure are about 240 and 207 nsec, which are longer than 65 nsec of titanium oxide prepared at 800 oC thermal treatment. Their photocatalytic activities are further improved to 2.0 and 1.5 times higher than that of commercial P-25. The photocatalysis of titanium oxide is very sensitive to the surface states. Titanium oxide surface defects can act as trapping sites for photo-induced holes and facilitate the separation of photo-induced carriers. Zinc selenide and zinc sulfide can passivate the surface well. It may say that titanium oxide surface defects removal has a negative impact.
The density, height, diameter, PL wavelength and intensity of zinc selenide self-assembled quantum dots grown on zinc sulfide/gallium arsenide with the zinc sulfide thickness from 15 to 160 nm are studied. For a fixed 30 sec zinc selenide self-assembled quantum dots growth, it cannot be formed with the zinc sulfide thickness below 15 nm due to the close lattice match between zinc sulfide and gallium arsenide. The zinc sulfide/gallium arsenide is fully lattice relaxed with the zinc sulfide thickness higher than 130 nm examined by X-ray diffraction. The higher quality and density of zinc selenide self-assembled quantum dots can be obtained on zinc sulfide/gallium arsenide with the zinc sulfide thickness far beyond its critical thickness. The maximum zinc selenide self-assembled quantum dots density of 4.9 x 109 cm-2 with the strongest photoluminescence intensity is obtained at the zinc sulfide/gallium arsenide thickness of 130 nm. Clusters are formed on the surface of zinc selenide/gallium arsenide. The selenium segregation is the main mechanism for the formation of clusters. The dislocations will enhance the selenium segregation. Higher zinc selenide cluster corresponds to higher density of dislocations. The non-spherical cluster is formed from the mergence of the two clusters.
High quality zinc oxide rods and zinc hydroxide slices are successfully grown on gallium arsenide with the aqueous solution of zinc nitrate and hexamethylenetetramine. The growth can be controlled by the appropriate nitric acid concentration incorporation in the solution. After thermal annealing, the zinc oxide slices transformed from zinc hydroxide slices can contribute much higher photocatalytic activity to 1.2 times to P-25.
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On the Manufacturing of SFF Based Tooling and Development of SLS Steel MaterialBoivie, Klas January 2004 (has links)
No description available.
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Microextraction and gas chromatographic determination of parabens / Parabenų mikroekstrakcija ir dujų chromatografinis nustatymasPrichodko, Aleksandra 27 December 2012 (has links)
Parabens are effective antibacterial and anti-fungal agents and are used extensively as preservatives in cosmetics, food and pharmaceutical products. Because of the presence of parabens in the environment and their negative effects on human health, there is an increasing interest in their trace analysis. Since the concentration of parabens in the environment are rather low and cosmetics present rather complex matrices for the analysis, it is necessary to apply a preconcentration or isolation step prior to the chromatographic analysis. The aim of this work was to develop liquid-phase microextraction methods – single drop microextraction, hollow fibre liquid phase microextraction and dispersive liquid-liquid microextraction – for parabens and to apply the methods for determination of parabens in water samples and cosmetic products. Extraction conditions for single drop microextraction, hollow fibre liquid phase microextraction and dispersive liquid-liquid microextraction were optimized and the quality parameters of the suggested methods were calculated. The influence of derivatization on the paraben extraction efficiency was evaluated. Prepared microextraction methods were applied for the determination of parabens in real samples. / Parabenai pasižymi antibakterinėmis bei priešgrybelinėmis savybėmis ir plačiai naudojami kosmetikos, maisto, farmacijos pramonėje kaip konservantai, apsaugantys produktus nuo ankstyvo gedimo ir prailginantys jų galiojimo laiką. Padidėjus įtarimams, jog prasiskverbę per odą parabenai gali sukelti alergines reakcijas, ardyti endokrininę sistemą, skatinti vėžinių ląstelių gamybą, buvo pradėta kontroliuoti jų kiekį aplinkoje, maisto bei kosmetikos produktuose. Tačiau parabenų koncentracijos dažnai yra per mažos, o mėginiai per daug sudėtingi, kad juos būtų galima analizuoti nesukoncentravus ir neizoliavus nuo trukdančios matricos. Šioje daktaro disertacijoje apibendrintų mokslinių tyrimų tikslas – sukurti parabenų skysčių-skysčių mikroekstrakcijos metodus – mikroekstrakciją tirpiklio lašu, skystafazę mikroekstrakciją kapiliare ir dispersinę skysčių-skysčių mikroekstrakciją – bei pritaikyti juos parabenų nustatymui vandenyje bei kosmetikos produktuose. Optimizuotos mikroekstrakcijos tirpiklio lašu, skystafazės mikroekstrakcijos kapiliare ir dispersinės skysčių-skysčių mikroekstrakcijos ekstrakcijos sąlygos ir nustatytos pagrindinės analizinės charakteristikos. Ištirta parabenų derivatizacijos įtaka parabenų dujų chromatografinio nustatymo efektyvumui. Paruošti parabenų mikroekstrakcijos metodai pritaikyti vandens ir kosmetikos mėginių analizei.
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Parabenų mikroekstrakcija ir dujų chromatografinis nustatymas / Microextraction and gas chromatographic determination of parabensPrichodko, Aleksandra 27 December 2012 (has links)
Parabenai pasižymi antibakterinėmis bei priešgrybelinėmis savybėmis ir plačiai naudojami kosmetikos, maisto, farmacijos pramonėje kaip konservantai, apsaugantys produktus nuo ankstyvo gedimo ir prailginantys jų galiojimo laiką. Padidėjus įtarimams, jog prasiskverbę per odą parabenai gali sukelti alergines reakcijas, ardyti endokrininę sistemą, skatinti vėžinių ląstelių gamybą, buvo pradėta kontroliuoti jų kiekį aplinkoje, maisto bei kosmetikos produktuose. Tačiau parabenų koncentracijos dažnai yra per mažos, o mėginiai per daug sudėtingi, kad juos būtų galima analizuoti nesukoncentravus ir neizoliavus nuo trukdančios matricos. Šioje daktaro disertacijoje apibendrintų mokslinių tyrimų tikslas – sukurti parabenų skysčių-skysčių mikroekstrakcijos metodus – mikroekstrakciją tirpiklio lašu, skystafazę mikroekstrakciją kapiliare ir dispersinę skysčių-skysčių mikroekstrakciją – bei pritaikyti juos parabenų nustatymui vandenyje bei kosmetikos produktuose. Optimizuotos mikroekstrakcijos tirpiklio lašu, skystafazės mikroekstrakcijos kapiliare ir dispersinės skysčių-skysčių mikroekstrakcijos ekstrakcijos sąlygos ir nustatytos pagrindinės analizinės charakteristikos. Ištirta parabenų derivatizacijos įtaka parabenų dujų chromatografinio nustatymo efektyvumui. Paruošti parabenų mikroekstrakcijos metodai pritaikyti vandens ir kosmetikos mėginių analizei. / Parabens are effective antibacterial and anti-fungal agents and are used extensively as preservatives in cosmetics, food and pharmaceutical products. Because of the presence of parabens in the environment and their negative effects on human health, there is an increasing interest in their trace analysis. Since the concentration of parabens in the environment are rather low and cosmetics present rather complex matrices for the analysis, it is necessary to apply a preconcentration or isolation step prior to the chromatographic analysis. The aim of this work was to develop liquid-phase microextraction methods – single drop microextraction, hollow fibre liquid phase microextraction and dispersive liquid-liquid microextraction – for parabens and to apply the methods for determination of parabens in water samples and cosmetic products. Extraction conditions for single drop microextraction, hollow fibre liquid phase microextraction and dispersive liquid-liquid microextraction were optimized and the quality parameters of the suggested methods were calculated. The influence of derivatization on the paraben extraction efficiency was evaluated. Prepared microextraction methods were applied for the determination of parabens in real samples.
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Evaulation of liquid-exfoliatedgraphene as additive in Ag-basedsliding contactsJuhlin, Stina January 2018 (has links)
This master thesis work is performed at ABB Corporate Research Center inVästerås. The aim of this study is to investigate Ag:graphene composites as slidingelectrical contacts, suitable for use in e.g. tap-changers. Three different graphenematerials, all produced by a low-cost exfoliation process, are evaluated in this study. The results are compred to an ongoing work on Ag:GO (graphene oxide) composites. This material has shown very good tribological properties, however it hasbeen difficult to handle during sintering processing. The goal of this study is to geteven better tribological, electrical and mechanical properties than Ag:GO, and also todevelop a new powder-metallurgical method to produce the Ag:graphene composites.The study also investigates the influence of graphene flake size and concentration aswell as microstructure of the Ag:graphene composites. This report focuses on aninvestigation of the graphene raw material quality from the suppliers, and friction,wear and resistance analysis of the composites. This is done by using Ramanspectroscopy, SEM with EDS, LOM, tribometer tests and resistivity analysis. Raman and SEM analyses show that none of the supplied LEG materials are ofhigh-quality G (single or bilayer), but rather multi-layer graphene or even graphite.Small amounts of graphene added to Ag gave extremly low friction (μ<0.2 vs. pureAg μ~1.3, 5 N load and 5 cm/s speed). The composite manufacturing process hadcritical steps, which have to be optimized, to obtain low values of friction. Severedegassing of the composites was observed for some sampes, but the samples stillmaintained good friction values. SEM and EDS analyses of 2dfab’s wear track show abuild-up thin carbon-containing tribofilm on the Ag surface. Indicating that G ispresent, and works as a lubricant, creating good tribological properties. The resultsfrom this project may for sure be of importance for future ABB products in specificindustrial applications.
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Iterative synthesis of sequence-defined polymers using solid and soluble supports / Synthèse itérative de polymères à séquences définies en utilisant des supports solides ou solublesMeszynska, Anna 31 March 2014 (has links)
Dans ce travail, des méthodes itératives ont été étudiées afin de préparer des oligomères à séquences bien définies en utilisant des supports solides ou solubles. Trois stratégies de couplage de monomères ont été exploitées (i) AB + AB, (ii) AB + CD et (iii) AA + BB. La première méthode a permis la synthèse d’oligopeptides en utilisant les protocoles classiques de la synthèse peptidique à partir notamment d’amino-acides protégés par des groupements Fmoc. Les deux autres stratégies ont permis de préparer des oligo(alcoxyamine amide)s et des oligoamides, en l’absence de groupements protecteurs. Dans ces cas, le contrôle de la structure primaire de l’oligomère a été rendu possible soit par l’utilisation de réactions chimio-sélectives (AB + CD) soit en introduisant un large excès de monomères bifonctionnels (AA + BB). Ainsi, les oligo(alkoxyamine amide)s ont été préparés en utilisant des couplages successifs de bromo-anhydride et d’amino-nitroxide ; et les oligoamides ont été obtenus par couplages de diacides et de diamines.L'approche pratique permettant la formation de ces oligomères à séquence contrôlée ainsi que leur caractérisation seront décrites dans cette thèse. / In this work, iterative methods have been studied to prepare sequence-defined oligomers on solid and soluble supports. Three model monomer coupling strategies have been exploited, (i) AB + AB, (ii) AB + CD and (iii) AA + BB, for the synthesis of oligopeptides, oligo(alkoxyamine amide)s and oligoamides, respectively. In the first strategy (AB + AB), oligopeptides have been synthesized using classical peptide synthesis protocols, in which Fmoc-protected amino acids were used. The other two strategies (AB + CD and AA + BB) are protecting-group free methods. In this case, the control over the oligomer primary structure has been achieved using chemoselective reactions (AB + CD) or a large excess of bifunctional monomers (AA + BB). The oligo(alkoxyamine amide)s have been prepared using successive coupling of bromo-anhydride and amino-nitroxide building blocks. The oligoamides have been obtained by sequential coupling of diacid and diamine building blocks. The practical approach to these primary structures using solid- and liquid-phase methodologies followed by the characterization of formed oligomers is the scope of this thesis.
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