The submitted thesis is focused on the development, optimization, testing and practical application of the new microextraction method called Bell Shaped Extraction Device assisted Liquid-Liquid Microextraction (BSED-LLME). The method is based on the application of a miniature bell-shaped extraction tool in which the extraction takes place, so that only minimal solvent losses can occur, and which allows a reproducible dosing and collection of a small volume of the extraction solvent. The BSED- LLME method was used to preconcentrate selected volatile and less volatile analytes from aqueous samples into organic solvents of a density lower than water. After the extraction, the analytes were determined by fast gas chromatography with flame ionization detection and gas chromatography with mass spectrometry. The statistical methods known as Design of Experiment (DOE) were used for determination of the optimal extraction conditions for BSED-LLME procedure. DOE is based on a mathematical description of the system and the prediction of the optimal setting of experimental parameters that may influence extraction efficiency. Factors such as extraction time, volume of extraction solvent, addition of sodium chloride (ionic strength), stirring rate and the diameter of the extraction vessel ect., have been tested....

Évaluer la capacité de remplissage des cinq différentes techniques d’obturation canalaire dans l’obturation des canaux ovales. Matériel et méthodes : Un total de 220 molaires mandibulaires, avec 1 canal dans la racine distale, a été sélectionné. Chaque canal a été mise en forme jusqu’à la longueur de travail en utilisant un système mono-instrument le WaveOne Gold Primary Les dents préparées ont été divisées au hasard en cinq groupes égaux (n = 40 par groupe) pour l'obturation: condensation à onde continue (CWC), technique avec tuteur GuttaCore (GC), technique avec tuteur Thermafil (TH), technique utilisant un cône unique (SC), condensation hydraulique à froid (CHC). Les pourcentages de GPFA, SFA et VA ainsi que la présence des matériaux d’obturation à l’intérieur des tubulis dentinaires (tag)à longueur de travail (LT) -4mm et -2 mm a été évalué à par microscopie numérique optique, microscopie électronique à balayage (SEM) et microanalyse par rayons X à dispersion d'énergie (EDX). Analyse statistique : Les données collectées ont été analysées avec la version 11.2 de SigmaPlot (Systat Software, Inc., San José, CA, USA). Les pourcentages de GPFA, SFA, VA correspondant aux différentes groupes ont été comparés en utilisant le test de Kruskal-Wallis avec α=0,05. Résultats: à LT-4 et LT-2 mm, cette étude à montré une différence statistiquement significative en terme de capacité d’obturation pour le cinq techniques. À LT-4, les groupes GC et TH ont montré une différence statistiquement significative par rapport aux trois autres groupes en terme de GPFA et SFA. En terme de VA, il y a une différence statistiquement significative avec les groupes SC et CHC tandis qu’aucune différence n’a été démontrée entre les groupes GC , TH et CWC . À LT-2, les groupes GC et TH ont montré une différence statistiquement significative par rapport aux trois autres groupes en terme de GPFA, SFA, VA. Conclusion : 
Cette étude montre clairement que les obturations par GC et TH sont en mesure de remplir les canaux ovales d’une manière plus appropriée que les autres techniques d’obturation. 
Les groupes GC et TH, à LT -4 et -2mm, présentaient des tags de gutta-percha à l’intérieur des tubulis dentinaires. La présence de tags de gutta-percha à l’intérieur des tubulis dentinaires (à la place de tags de ciment beaucoup plus vulnérables) pourrait se comporter comme une barrière physique, capable de sceller les bactéries à l’intérieur des tubulis et surtout non résorbable dans le temps. / Assess the filling ability in oval-shaped canals using five different filling techniques. Materials and Methods : 220 human mandibular first molars with one distal oval canal were selected. Distal Canals were shaped using WaveOne Gold Primary. The prepared teeth were randomly divided in four equal groups (n = 40) for obturation : Continuous Wave Condensation (CWC), GuttaCore carrier based technique (GC), Thermafil (TH) carrier based technique, Single Cone technique (SC), Cold hydraulic Condensation (CHC). The proportions of gutta-percha filled areas (GPFA), sealer filled areas (SFA), void areas (VA) and the tags into dentinal tubules at 4 mm and 2 mm were analyzed by Optical numeric microscope, SEM and EDX. Statistical analysis : they were compared by Kruskal-Wallis one-way ANOVA on ranks, with statistical significance set at α = 0.05. Results : At 4 and 2 mm from the apex, this study discloses statistically different filling ability for the five techniques. At 4 mm from the apex, the GC et TH groups showed significantly higher PGFAs than lateral condensation and System B techniques. The GC et TH groups showed a statistically significance difference compared with the others three groups in terms of higher PGFA, lower SFA. It showed a statistically significance difference with SC and CHC groups in term of VA. At 2 mm level from the apex, the GC et TH groups showed a statistically significance differece compared with the others three groups in terms of higher PGFA, lower SFA and VA. Conclusions : GC obturation is able to fill oval-shaped canals in a more appropriate way than the other filling techniques. GC was the only group which showed the presence of gutta-tags at 4 and 2 mm from the apex. The gutta- percha tags could behave as a physical barrier able to entomb bacteria.

京都大学 / 0048 / 新制・課程博士 / 博士(医学) / 甲第18855号 / 医博第3966号 / 新制||医||1007(附属図書館) / 31806 / 京都大学大学院医学研究科医学専攻 / (主査)教授 河野 憲二, 教授 黒田 知宏, 教授 富樫 かおり / 学位規則第4条第1項該当 / Doctor of Medical Science / Kyoto University / DFAM

The use of synthetic materials for tissue and organ reconstruction, i. e. tissue engineering, has become a promising alternative to current surgical therapies and may overcome the shortcomings of the methods in use today. The challenge is in the design and reproducible fabrication of biocompatible and bioresorbable polymers, with suitable surface chemistry, desirable mechanical properties, and the wanted degradation profile. These material properties can be achieved in various manners, including the synthesis of homo- and copolymers along with linear and star-shaped architectures. In many applications the materials’ three-dimensional structure is almost as important as its composition and porous scaffolds with high porosity and interconnected pores that facilitate the in-growth of cells and transportation of nutrients and metabolic waste is desired. In this work linear and star-shaped polymers have been synthesized by ring-opening polymerization using a stannous-based catalyst and a spirocyclic tin initiator. A series of linear copolymers with various combinations of 1,5-dioxepane-2-one (DXO), Llactide (LLA) and ε-caprolactone (CL) have been polymerized using stannous octoate as catalyst. It is shown that the composition of the polymers can be chosen in such a manner that the materials’ mechanical and thermal properties can be predetermined. A solvent-casting and particulate leaching scaffold preparation technique has been developed and used to create three-dimensional structures with interconnected pores. The achieved physical properties of these materials’ should facilitate their use in both soft and hard tissue regeneration. Well defined star-shaped polyesters have been synthesized using a spirocyclic tin initiator where L-lactide was chosen as a model system for the investigation of the polymerization kinetics. Neither the temperature nor the solvent affects the molecular weight or the molecular weight distribution of the star-shaped polymers, which all show a molecular weight distribution below 1.19 and a molecular weight determined by the initial monomer-to-initiator concentration. / QC 20101217

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Druckbauteile sind essentielle Elemente eines jeden Bauwerks, denn in Form von Stützen oder Wänden tragen sie die Lasten in den Baugrund ab. Heutzutage werden sie zumeist mit einem rechteckigen Querschnitt und konstanten Abmaßen über die Höhe ausgeführt. Bereits runde Stützen stellen eine Ausnahme dar und werden vor allem aus architektonischen Gründen angeordnet. Aber wie würde die möglichst optimale Geometrie eines Druckbauteils aussehen? Im Rahmen des Projekts wurde dieser zentralen Fragestellung nach einer günstigen Adaption der Querschnittsgeometrie von Stützen in Quer- und in Längsrichtung nachgegangen. Wesentliche Zielsetzung war dabei, Stützen so entwerfen und berechnen zu können, dass sie in allen Querschnittsbereichen gleichmäßig ausgelastet sind. Dadurch werden schlankere Bauteile möglich, die aufgrund der Materialersparnis nicht nur zur Schonung unserer natürlichen Ressourcen beitragen, sondern auch wirtschaftlich von Vorteil sind und zu einem ästhetischeren Erscheinungsbild führen. [Aus: Einleitung] / Pressure components are essential elements for any structure, because in the form of columns or walls they transfer the loads into the subsoil. Nowadays, they are usually designed with a constant rectangular cross-section over the full height. Already round columns are an exception and are arranged mainly for architectural reasons. But what would the optimum geometry of a pressure component look like? Within the framework of the project, this central question of a favourable adaptation of the cross-section geometry of columns in transverse and longitudinal direction was investigated. The main objective was to be able to design and calculate columns in such a way that they are equally loaded in all cross-section areas. This enables slimmer components which, due to the material savings, not only contribute to the conservation of our natural resources, but are also economically advantageous and lead to a more aesthetic appearance. [Off: Introduction]

Das Prinzip „Leicht Bauen mit Beton“ kann durch stabförmige Bauelemente außerordentlich gut umgesetzt werden, da einwirkende Beanspruchungen konzentriert und optimiert aufgenommen werden können. Stabförmige Bauelemente gehören zu den maßgebenden Bestandteilen von Mast- und Turmkonstruktionen sowie Fachwerk- und Rahmenstrukturen (Bild 1). Obgleich die Stäbe in diesen Konstruktionen überwiegend normalkraftbeansprucht sind, führen horizontale Beanspruchungen z. B. infolge Wind sowie Einspannungen in den Verbindungsknoten zu Biege- und Querkraftbeanspruchungen. Daneben sind nahezu alle räumlichen Konstruktionen durch einseitige oder unsymmetrische Beanspruchungen einer gewollten oder ungewollten Torsionsbeanspruchung unterworfen. [Aus: Einleitung] / The principles of “Concrete Light“ apply extraordinarily well to tubular concrete members, as applied stresses can be absorbed in a concentrated and optimized way. Tubular members are decisive components of mast and tower constructions as well as of truss and frame structures (Fig. 1). Although tubular members in such constructions are predominantly subjected to normal forces, horizontal loads (e.g. due to wind) and rigid joints lead to secondary bending moments and shear forces. In addition, as a result of one-sided or asymmetrical loads, almost all spatial constructions are subjected to intentional or unintentional torsion. [Off: Introduction]

El efecto multipactor de ruptura en RF ha sido objeto de numerosos estudios desde hace más de 80 años, a partir del desarrollo de los primeros aceleradores de partículas en la primera mitad del siglo XX. A mediados de ese siglo, con el desarrollo de fuentes de alta potencia para aplicaciones radar y la llegada de los satélites artificiales, la investigación del multipactor cobró una considerable relevancia, al convertirse este fenómeno en un riesgo determinante para costosos proyectos comerciales. Las guías de onda con secciones rectas canónicas, como las rectangulares o las coaxiales, han sido tradicionalmente las más utilizadas en dispositivos de microondas. Sus principales ventajas son que sus campos electromagnéticos pueden resolverse analíticamente, lo que permite su aplicación directa en diseños complejos, y la simplicidad de su fabricación. Pero las capacidades de computación y las prestaciones de los algoritmos se han multiplicado con los años, lo que ha permitido ampliar el espectro de posibles topologías a geometrías casi arbitrarias, ofreciendo al diseñador una mayor libertad creativa. En todo caso, gran parte de los dispositivos de microondas actuales siguen confiando en la madurez y fiabilidad de las tecnologías de guía de onda tradicionales, que no requieren una inversión adicional en equipos de fabricación. La supresión del efecto multipactor es la motivación para arriesgarse a probar topologías de guía de onda innovadoras, como la guía en forma de cuña. Es en este contexto donde este trabajo de doctorado pretende ofrecer una contribuci'on. En primer lugar, se ha desarrollado un modelo numérico para predecir el efecto multipactor de ruptura en guías de onda huecas en forma de cuña. Esta herramienta ha permitido la identificación de criterios óptimos de diseño. Así mismo, se ha adaptado un método de síntesis de filtros paso-banda en guía rectangular para poder realizar un diseño similar pero basado en la nueva topología. Como culminación, las estructuras diseñadas se han fabricado y medido, con el fin de comprobar sus prestaciones electromagnéticas y su sensibilidad al efecto multipactor. Se ha registrado además una patente para proteger estos nuevos filtros. En resumen, el trabajo ha abarcado el ciclo de actividades relacionadas con el desarrollo industrial completo de un dispositivo pasivo de microondas: investigación básica, análisis, diseño, fabricación y calificación con medidas en el laboratorio. Estas medidas han comprobado la mejora prevista en los umbrales de multipactor de los filtros de microondas con topología en forma de cu¿na, y han confirmado que pueden ofrecer respuestas en frecuencia similares a aquellas de filtros basados en una guía de onda rectangular equivalente. Las implicaciones de los resultados han sido evaluadas a fondo y resumidas en este documento. Como observación final, se ha intentado redactar esta investigación de manera que refleje el proceso natural de aprendizaje, mostrando los aciertos y errores experimentados en el camino, todos los cuales han conducido al resultado final. Este reto no hubiera sido posible sin el apoyo y compromiso de varios profesionales de diferentes centros de investigación e industrias europeas (Universidad Politécnica de Valencia, Universidad de Valencia, Agencia Espacial Europea, Thales Alenia Espacio Espa¿na, Technische Universit¿at Darmstadt, 'Ecole Polythecnique F'ed'erale de Lausanne, Tesat, Aurora Software and Testing y Val Space Consortium), a los cuales estoy agradecido. / The multipactor RF breakdown effect has been object of numerous studies for over 80 years, since the development of the first particle accelerators in the beginning of the 20th century. Around the middle of that century, with the development of high power sources for radar applications and with the emergence of the artificial satellites, a new impulse was given to the multipactor research, since it became a risk for expensive commercial projects. Traditionally, waveguides with canonical cross sections, like rectangular or coaxial ones, have been the building blocks of most microwave devices. Their main advantages are that their electromagnetic fields can be solved analytically, enabling their direct application in complex designs, as well as their manufacturing simplicity. But over the years the computation capabilities and algorithms have continuously evolved, which has broadened the spectrum of possible topologies to almost arbitrary geometries, offering the designer more room for creativity. However, most of the current microwave devices still trust on the mature canonical waveguide technologies, which do not require an additional investment in manufacturing equipment. The suppression of the multipactor effect is the motivation for considering an innovative waveguide topology, like the wedge-shaped waveguide. It is within this context where this PhD work aims to offer a contribution. On the one hand, a numerical model for predicting the multipactor breakdown effect in wedge-shaped hollow waveguides has been developed. This tool has aided in the derivation of optimised design criteria. On the other hand, a bandpass filter synthesis method for rectangular waveguide has been adapted in order to calculate a similar design based on the new topology. As a culmination, the designed structures have been manufactured and tested, in order to verify their electromagnetic performance and their multipactor sensibility. A patent was also filed to protect these new filters. In short, this work has comprised the cycle of activities related to the whole industrial development of a passive microwave device: basic research, analysis, design, manufacturing and qualification through testing. These measurements have verified the predicted improvement in the multipactor thresholds of microwave filters with wedge-shaped topology, and have confirmed that they can offer similar frequency responses to the equivalent rectangular waveguide ones. The implications of the results have been thoroughly evaluated and summarised in this document. As a final remark, this research document has been drafted to reflect the natural learning process, and to show the rights and wrongs experienced in the way, which all have led to the final result. Such an endeavour would not have been possible without the support and commitment of several professionals from different European research centres and industries (Universidad Polit'ecnica de Valencia, Universidad de Valencia, European Space Agency, Thales Alenia Espacio Spain, Technische Universit¿at Darmstadt, 'Ecole Polythecnique F'ed'erale de Lausanne, Tesat, Aurora Software and Testing and Val Space Consortium), for which I am grateful. / Hueso González, J. (2013). Analysis of wedge-shaped waveguides and design of multipactor-resistant microwave bandpass filters. Análisis de guías de onda en forma de cuña y diseño de filtros de microondas paso-banda resistentes al efecto multipactor [Tesis doctoral]. Editorial Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/33750