Techn. Universiẗat, Diss., 2001--Berlin.

Techn. Universiẗat, Diss., 2000--Berlin.

Techn. Universiẗat, Diss., 2003--Berlin.

Universiẗat, Diss., 2003--Bonn.

Universiẗat, Diss., 2003--Bielefeld.

Techn. Universiẗat, Diss., 2005--Berlin.

O objetivo deste trabalho é analisar a influência dos parâmetros de um sistema mecanizado de soldagem, composto por uma tocha TIG e outra MAG em tandem, sobre a geometria do cordão de solda resultante. Os resultados obtidos foram comparados com soldas realizadas pelos processos TIG e MAG operando isoladamente. Os testes foram executados por meio de simples deposição de cordões sobre chapas de aço ao carbono AISI 1010 com espessura de 6,3 mm. Os parâmetros analisados foram: corrente de soldagem e distância da ponta do eletrodo até a peça no processo TIG, velocidade de alimentação de arame e tensão do arco no processo MAG, além de velocidade de soldagem e distância entre as tochas. Os cordões de solda foram executados em um dispositivo de soldagem mecanizado, que permite a variação da velocidade de soldagem, distância da ponta do eletrodo TIG e a distância entre as tochas. Os ajustes de corrente e tensão de soldagem foram feitos em duas fontes de potência separadas, ambas do tipo transformador-retificador, uma para cada tocha, devido às diferentes curvas características de cada processo. Através do projeto de experimento fatorial fracionado, foram avaliados os efeitos de dois níveis, um mínimo e outro máximo, mais quatro réplicas dos seus níveis intermediários, resultando em 20 experimentos para cada processo de soldagem. Os valores dos resultados finais indicam uma diferença ao utilizar uma tocha TIG para pré-aquecer o material base, porém, estatisticamente, essa diferença não é significativa entre os processos TIG e MAG em tandem e MAG convencional para a faixa de parâmetros de soldagem adotada. / This study aims to investigate the influence of process parameters of a mechanized welding system, comprising a GTAW torch and a GMAW torch in tandem configuration, on the geometry of the resulting weld bead, performed using GTAW and GMAW welding processes in tandem. The results were compared with weld beads performed by conventional GTAW and GMAW welding processes. The tests were conducted performing bead-on-plate deposits over AISI 1010 6,3 mm thick carbon steel plates. GTAW current, GMAW wire feed speed, GTAW arc length, GMAW voltage, welding speed and the distance between GTAW and GMAW torches were the analyzed parameters. The weld beads were performed in a mechanized welding bench, which allows the variation of speed, distance between torches and arc length of the GTAW torch. Current and voltage adjustments were made in two separate transformer-rectifier power sources, one for each welding torch, due to their different characteristic curves of each process. Through the fractional factorial design of experiment, the effects of two different levels for each parameter were analyzed, plus four replicates of the average values of these levels, resulting in 20 experiments for each welding process. The results show a difference on the weld bead geometry using a GTAW torch to preheat the base metal, however, this difference is not statistically significant between GTAW and GMAW welding process in tandem and GMAW welding process for the adopted range of welding parameters.

A dispersive liquid-liquid microextraction (DLLME) method has been developed, optimized and validated for the extraction of seven beta-agonists (Cimaterol, Cimbuterol, Clenproperol, Clenbuterol, Ractopamine, Isoxsuprine and Ritodrine) from bovine muscle. The homogenized tissue samples were hydrolyzed enzymaticaly by beta-glucuronidase and extracted with DLLME. The extraction parameters (pH, extraction solvent, extraction solvent volume, disperser solvent) were accurately optimized. Separation of the beta-agonists was by gradient elution on C18 LC column using acetonitrile and formic acid aqueous solutions as mobile phases, multiple reaction monitoring (MRM) scan mode was used. The seven beta-agonists were then simultaneous determined and identified in single analysis using 4000 Qtrap LC-MS/MS system. The DLLME method was validated using ISO 17025 and the EU criteria (Commission Decision 2002/657/EC) for validation of analytical method, good precision, repeatability and spiked recoveries were obtained. The limits of detection and quantification for the residues were between 0.0728 – 0.0922 μg/kg and 0.243 – 0.307 μg/kg respectively for beta-agonists. The overall recoveries were between 85% and 100% with the relative standard deviation of (RSDs) between 3.0% and 10%. The recoveries from the developed DLLME method were compared with those obtained from dSPE. DLLME proved to be comparable to SPE. The real samples test showed that the DLLME method developed is accurate and sensitive for the determination of beta-agonist residues in bovine muscle. / Chemistry / M. Sc. (Analytical Chemistry)

Focus of this study was on the development of one of the faster, simpler, cost effective and environmentally friendly sample pre-treatment techniques which employs a supported liquid membrane, in this case a Hollow-fiber supported liquid membrane (HF-SLM) for determination of seven (7) quinolone antibiotics (enrofloxacin, ciprofloxacin, danofloxacin, difloxacin, norfloxacin, nalidixic acid and sarafloxacin) in bovine kidney samples followed by LC-MS/MS analysis. The key parameters of the method were optimized and the method was validated following the 2002/657 EC guidelines. The optimum HF-SLM conditions were therefore; NaH2PO4 as a donor phase at pH 7, 0.1% formic acid at pH 3 as acceptor phase. Triethylamine was the optimized liquid membrane and the stirring time was optimized at 1 hour. Separation of the 7 quinolones including 3 internal standards (enrofloxacin-d5, norfloxacin-d5 and difloxacin-d3) was carried out on a Phenomenex Kinetex 2.6 μm XB-C18, 100 mm x 4.6 mm, 100Å column. Validation parameters such as Correlation coefficients (r2) ranging from 0.9714-0.9975 were obtained, while limit of detection (LOD) ranged between 3-39 ug kg-1 and limit of quantification (LOQ) ranged between 10-130 ug kg-1. The obtained limits at which it can be concluded with an error probability of α = 95% that a sample is non-compliant (CCα) ranged from 28 – 422 ug kg-1 while CCβ; the smallest content of the substance that may be detected, identified or quantified in a sample with an error probability of β = 95%, ranged from 29 – 454 ug kg-1. The method was found to be reproducible with CVs ≤ 23 %. The tested samples from Botswana local abattoirs showed no presence of quinolone antibiotics when the method was applied to real bovine kidney samples. Hollow-fiber supported liquid membrane can therefore be used for extraction of biological samples since it is a “greener technique” which uses less solvent which are less harmful to the environment when disposed as compared to dispersive Solid Phase Extraction (dSPE). / Chemistry / M. Sc. (Chemistry)

Les systèmes à énergies renouvelables couplés à un stockage hydrogène apportent des solutions nouvelles et innovantes à l'alimentation électrique des milieux peu ou non électrifiés. Le concept de batterie H2 qui équipe ce type de système est une forme de stockage originale qui apporte l'autonomie et l'indépendance électrique pour des longues durées (typiquement stockage saisonnier). Le fonctionnement de cette batterie H2 est le suivant : un électrolyseur produit des gaz (H2 et O2) avec les surplus d'énergie de la source renouvelable ; l'hydrogène, voire l'oxygène, est ensuite stocké dans des réservoirs pour être utilisé ultérieurement grâce à une pile à combustible lorsque la source renouvelable est insuffisante. Dans cette étude, nous nous intéresserons spécifiquement au couplage entre des générateurs photovoltaïques avec une batterie H2/O2 pour l'alimentation d'un site isolé sans interruption. Ces travaux de recherche s'inscrivent dans le projet ANR PEPITE (ANR-PanH 2007-2012) et ont été menés en partenariat avec HELION Hydrogen Power, le CEA Liten et l'Université de Corse. Le projet est également labellisé par les pôles de compétitivité CAPENERGIES et TENERRDIS. Tout d'abord, une réflexion générale s'appuyant sur les propriétés d'une batterie H2/O2 démontre la nécessité d'introduire une batterie (ici au plomb) pour garantir un fonctionnement instantané et sans interruption. Puis, une étude qualitative sur les architectures électriques possibles (bus de tension DC, AC…) a été menée pour s'achever sur une étude quantitative réalisée spécifiquement pour le projet PEPITE. Parallèlement à cela, différentes stratégies de gestions énergétiques ont été proposées afin d'utiliser les deux stockages dans les meilleures conditions, de limiter leur vieillissement ainsi que les pertes. Deux bancs d'essais à échelle réduite (un premier à bus DC et un second à bus AC) ont été réalisés au sein du laboratoire LAPLACE afin de valider les études et de préparer le prototype final qui sera testé sur le site de HELION Hydrogen Power au cours de l'été 2011.