Les BTEX est une famille de polluants très répandue en air intérieur. Ils présentent des effets nocifs sur la santé humaine à des faibles concentrations ce qui a emmené le législateur à fixer des seuils afin de limiter l'exposition des gens. L'objectif de ce travail de recherche est de développer et de mettre en place une méthode analytique sensible, précise et rapide basée sur un dispositif de mesure. Le dispositif ainsi mis en place est un chromatographe en phase gazeuse miniaturisé équipé d'un mini détecteur à photo ionisation dédié à la détection des BTEX en temps quasi-réel. Le système analytique est très portable ayant une consommation gazeuse très faible assurant une autonomie élevée sur de longues durées. Son mode de fonctionnement se base sur l'échantillonnage de l'air dans une boucle connecté à une vanne six voies. L'injection de l'échantillon sur une colonne analytique placée dans un four pour la séparation est assurée par le changement de la position de la vanne avant la détection par photo ionisation. Le nouveau dispositif miniaturisé a été déployé lors de deux campagnes intensives menées dans un collège énergétiquement performant. Cette étude a porté sur la surveillance temporelle de la concentration des polluants présents en air intérieur, y compris les BTEX. Les résultats ainsi obtenus pour les BTEX avec notre dispositif ont été comparés à ceux fournis par d'autres techniques dites techniques de référence. Ces campagnes de terrain ont permis donc de valider les performances analytiques, la robustesse et l'autonomie de cette nouvelle méthodologie. / BTEX are very widespread indoor air pollutants. Their harmful effects on human health had led the legislator to set thresholds in order to limit the population exposure. The aim of this thesis is to develop a sensitive, accurate and fast analytical method based on a measurement device. Therefore, the device implemented is a miniaturized gas chromatography (GC) equipped with a mini photo ionization detector dedicated to BTEX detection in indoor air in near-real time. The miniaturized GC is very portable with a very low gas consumption which enhances its autonomy over a long period. Its operation mode is based on air sampling inside a sample loop which is connected to a six port valve. The injection over a heated analytical column is ensured by switching the valve position before detection by a photo ionization detector. This novel device was used in real conditions during two field campaigns conducted in an energy efficient college. This study focused on the temporal monitoring of indoor air pollutant concentrations including BTEX. The results obtained with our miniaturized device for BTEX were compared to those given by other techniques known as reference techniques. These field campaigns have therefore enabled us to validate the analytical performances, the robustness and the autonomy of this novel analytical method.

Cieľom predloženej diplomovej práce je numerické riešenie šírenia elektromagnetických vĺn v tuneli. Za týmto účelom bola sformulovaná integrálna rovnica a numericky riešená pomocou metódy hraničných prvkov (BEM). Implementácia v prostredí MATLAB sľubne poukazuje na nízke výpočtové nároky oproti štandardným diferenciálnych diskretizačným metódam. Súčasťou projektu je vykreslenie rozloženia elektromagnetického poľa pre rôzne profily tunelov. Overenie výsledkov je vykonané pomocou zjednodušeného analytického modelu. V rámci práce je pozorované štúdium vplyvov zmien profilu tunela a rôznych impedančných podmienok na stenách tunela na výsledné rozloženie elektromagnetického poľa vo vnútri tunela.

The aim of the thesis is to determine the amount of indemnity for damage to the family house caused by excessive snow loads, calculation of material value (time value) immovable assets immediately before the insured event cost method using analytical methods wear, determining the cost of putting immovable in working condition, the calculation of substantive value of intangible assets for the repairs. In this thesis, the emphasis on the clarification process when the risk to the family house and a practical example of an insured event the immovable. At the same time the analysis of the results, which display graphs show how the event affected the development of insurance rates immovable.

The thesis focuses on the valuation of damage caused by torrential rain to the family house in the village Nesovice. In the first part the basic terms and assessing methods are defined. In the second part, there are applied methods of appraisal of damage on the family house. There is the value of the property calculated before the insurance event. In the itemized budget, there are quantified the cost of repairs of damaged constructions and then detected current value after repairs. The aim of the thesis is to dedicate readers to the problem of assessment.

Title: Chiral recognition by mass spectrometry Author: Bc. Lenka Kosíková Department: Department of Organic Chemistry Supervisor: doc. Mgr. Jana Roithová, Ph.D. This work is focused on the use of mass spectrometry as the analytical method for chiral recognition in the gas phase. We have examined formation of complexes (S and R) isomers [dimethyl-2,2'-dihydroxy-1,1'binaphthalene-3,3'-dicarboxylate] with sodium. Chiral effect for the fomation of sodium dimers is 1,34±0,06 and that for formation of trimers 2,38±0,22 in favor of the formation of homochiral complexes. Part of the work is devoted to the preparation of isotopically labeled ester [(R)-(−)- di(D3-methyl)-2,2'-dihydroxy-1,1'binaphthalene-3,3'-dicarboxylate]. Mixing of equimolar amounts of D3-(R) and unlabeled (S) isomers leads to the artificial racemate, while we can still distinguish the enantiomers using mass spectrometry. Another part represents the study of the complex formation between (S and R) isomers of [dimethyl-2,2'-dihydroxy-1,1'binaphthalene-3,3'-dicarboxylate] with the metal complex [(S,S)-1,5-diaza-cis-decalin]Cu(OH)I depending on the molar ratios in the solution. I have showed that the molar concetration of the catalyst in the solution plays an important role in the complex formation and that the ESI source spectra of...

Проведен анализ перспектив применения и достоинств теплообменников на базе закрытых двухфазных термосифонов по сравнению с распространёнными аналогами других конструкций и теоретических ограничений теплового потока в термосифонных теплообменниках, сформулированы требования к исследовательскому стенду. Проведено сравнение коэффициентов теплопередачи, полученные аналитическим методом, с помощью компьютерного моделирования и экспериментальным путём. / Analysis of prospects of application and advantages of heat exchangers on the basis of closed two-phase thermosyphones compared to common analogues of other designs and theoretical limitations of heat flow in thermosyphon heat exchangers was carried out, requirements to research bench were formulated. Heat transfer coefficients obtained by analytical method are compared by computer simulation and experimental method.

Thin-walled cold-formed steel (CFS) has exhibited inherent structural and architectural advantages over other constructional materials, for example, high strength-to-weight ratio, ease of fabrication, economy in transportation and the flexibility of sectional profiles, which make CFS ideal for modern residential and industrial buildings. They have been increasingly used as purlins as the intermediate members in a roof system, or load-bearing components in low- and mid-rise buildings. However, using CFS members in building structures has been facing challenges due to the lack of knowledge to the fire performance of CFS at elevated temperatures and the lack of fire design guidelines. Among all available design specifications of CFS, EN1993-1-2 is the only one which provided design guidelines for CFS at elevated temperatures, which, however, is based on the same theory and material properties of hot-rolled steel. Since the material properties of CFS are found to be considerably different from those of hot-rolled steel, the applicability of hot-rolled steel design guidelines into CFS needs to be verified. Besides, the effect of non-uniform temperature distribution on the failure of CFS members is not properly addressed in literature and has not been specified in the existing design guidelines. Therefore, a better understanding of fire performance of CFS members is of great significance to further explore the potential application of CFS. Since CFS members are always with thin thickness (normally from 0.9 to 8 mm), open cross-section, and great flexural rigidity about one axis at the expense of low flexural rigidity about a perpendicular axis, the members are usually susceptible to various buckling modes which often govern the ultimate failure of CFS members. When CFS members are exposed to a fire, not only the reduced mechanical properties will influence the buckling capacity of CFS members, but also the thermal strains which can lead additional stresses in loaded members. The buckling behaviour of the member can be analysed based on uniformly reduced material properties when the member is unprotected or uniformly protected surrounded by a fire that the temperature distribution within the member is uniform. However if the temperature distribution in a member is not uniform, which usually happens in walls and/or roof panels when CFS members are protected by plaster boards and exposed to fire on one side, the analysis of the member becomes very complicated since the mechanical properties such as Young’s modulus and yield strength and thermal strains vary within the member. This project has the aim of providing better understanding of the buckling performance of CFS channel members under non-uniform temperatures. The primary objective is to investigate the fire performance of plasterboard protected CFS members exposed to fire on one side, in the aspects of pre-buckling stress distribution, elastic buckling behaviour and nonlinear failure models. Heat transfer analyses of one-side protected CFS members have been conducted firstly to investigate the temperature distributions within the cross-section, which have been applied to the analytical study for the prediction of flexural buckling loads of CFS columns at elevated temperatures. A simplified numerical method based on the second order elastic – plastic analysis has also been proposed for the calculation of the flexural buckling load of CFS columns under non-uniform temperature distributions. The effects of temperature distributions and stress-strain relationships on the flexure buckling of CFS columns are discussed. Afterwards a modified finite strip method combined with the classical Fourier series solutions have been presented to investigate the elastic buckling behaviour of CFS members at elevated temperatures, in which the effects of temperatures on both strain and mechanical properties have been considered. The variations of the elastic buckling loads/moments, buckling modes and slenderness of CFS columns/beams with increasing temperatures have been examined. The finite element method is also used to carry out the failure analysis of one-side protected beams at elevated temperatures. The effects of geometric imperfection, stress-strain relationships and temperature distributions on the ultimate moment capacities of CFS beams under uniform and non-uniform temperature distributions are examined. At the end the direct strength method based design methods have been discussed and corresponding recommendations for the designing of CFS beams at elevated temperatures are presented. This thesis has contributed to improve the knowledge of the buckling and failure behaviour of CFS members at elevated temperatures, and the essential data provided in the numerical studies has laid the foundation for further design-oriented studies.

The Counter-Rotating Open Rotors (CROR) are identified as a possible alternative to turbofan engines for middle-range aircrafts. Providing significant fuel savings and reducing the green-house gas emissions, they may lead however to an increased noise radiation due to the absence of nacelle shielding. To properly predict the acoustic radiation of such systems is then mandatory both to reduce the source mechanisms of the isolated engine and to offer an optimal noise installation solution. Such an objective is tackled in the present thesis in two steps. In a first part, the research aims at predicting the tonal noise radiated from the first propeller of CROR mounted on the rear fuselage by means of a pylon (pusher configuration), considering both the pylon-wake and the uniform ow effects. From the Ffowcs Williams & Hawkings' formalism, three noise sources are identified. First the unsteady loading is computed using a similar procedure to the one used for the rotor-rotor wake interaction noise prediction. The velocity deficit in the pylon wake is locally expanded in two-dimensional Fourier gusts in a reference frame attached to the front rotor. The unsteady lift induced by each gust on a blade segment is calculated using a linearized analytical response function that accounts for a realistic geometry. The steady loading is the second source contribution and is evaluated using both a software based on the lifting-line theory and some numerical simulations for different reference source surfaces. Finally the thickness noise due to the blade volume displacement is included in the analysis using Isom's formulation. From the linear acoustic assumptions, all these sources modelled as equivalent acoustic dipoles rotating in a uniformly moving atmosphere are then summed to calculate the far-field noise. The whole methodology is assessed against wind-tunnel test data and reference software predictions. A parametric study considering several pylon positionings and pylon-wake configurations with blowing is performed in order to emphasize the relative contribution of the three noise sources. Secondly, the rotor- rotor wake interaction noise being recognized as the most significant contribution in isolated configuration, its modelling is completed by introducing the dynamics of the vortex occurring near the rear-rotor leading edge. A semi-analytical methodology is developed to determine a vortex attached over a at plate embedded in a uniform ow with incidence. Applied to the case of a rear blade going through a front-rotor wake, it provides a first estimate of the noise contribution of the vortex. / Les hélices contrarotatives constituent une alternative possible aux turboréacteurs pour les avions moyens- courriers. Réduisant significativement la consommation de carburant et les émissions de gaz à effet de serre, ils peuvent néanmoins conduire à un rayonnement sonore accru de par l'absence de carénage. Prédire correctement le rayonnement sonore de telles motorisations est donc indispensable pour réduire les mécanismes sources propres au moteur isolé ou assurer une solution d'installation acoustique optimale. Un tel objectif est abordé dans cette thèse en deux temps. Dans un premier temps, l’étude vise à prédire le bruit tonal rayonné par la première hélice d'un moteur monté à l'arrière du fuselage (configuration dite en pousseur), en considérant les effets du sillage du pylône supportant le moteur et de l'écoulement moyen. Partant du formalisme de Ffowcs Williams & Hawkings, trois sources sonores sont identifiées à cet effet. La charge instationnaire, tout d'abord, est calculée en s'appuyant sur une méthodologie similaire à celle utilisée pour la prédiction du bruit d'interaction de sillages entre les deux rotors. Le déficit de vitesse dans le sillage du mât est décomposé localement en rafales bidimensionnelles dans un repère attaché au rotor amont. La portance instationnaire induite par chaque rafale sur un segment de pale est calculée en utilisant une fonction de réponse analytique linéarisée considérant une géométrie réaliste. Deuxième contribution, la charge stationnaire est évaluée au moyen d'un logiciel s'appuyant sur la théorie de la ligne portante mais également via des simulations numériques pour différentes surfaces sources de référence. Enfin, le bruit d'épaisseur associé au déplacement du volume de la pale est inclus dans l'analyse à partir de la formulation d'Isom. D'après les hypothèses de l'acoustique linéaire, toutes ces sources modélisées comme des dipôles acoustiques tournant dans une atmosphère uniforme en mouvement sont ensuite sommées pour calculer le bruit en champ lointain. L'ensemble de la méthodologie est comparé à des données d'essai et des prédictions d'un logiciel de référence. Une étude paramétrique considérant plusieurs positionnements du pylône et des configurations avec soufflage est effectuée afin de bien mettre en évidence les contributions relatives des trois sources sonores. Dans un deuxième temps, le bruit d'interaction de sillages étant reconnu comme la contribution majoritaire en configuration isolée, sa modélisation est complétée en introduisant la dynamique du tourbillon se développant au voisinage du bord d'attaque du rotor aval. Une méthodologie semi-analytique est développée pour déterminer un tourbillon attaché au-dessus d'une plaque plane plongée dans un écoulement uniforme avec incidence. Appliquée au cas d'une pale aval traversant le sillage du rotor amont, elle fournit une première estimation de la contribution sonore du tourbillon.

O desenvolvimento e validação de métodos analíticos é um procedimento necessário quando um método não normalizado é utilizado por um laboratório de ensaios. A validação de métodos também é um requisito específico da norma ABNT NBR ISO/IEC 17025, que determina os requisitos gerais para a competência dos laboratórios de ensaio e calibração. O objetivo da validação é demonstrar que o método analítico, nas condições em que é executado, produz resultados com a exatidão requerida. O Laboratório de Corrosão, Proteção e Reciclagem de Materiais (LACOR), da UFRGS, tem o ensaio de determinação de metais por fluorescência de raios X, acreditado pelo CGCRE/INMETRO, conforme ABNT NBR ISO/IEC 17025. O ensaio é feito usando o método de espectrometria de fluorescência de raios X por dispersão de energia (EDXRF). Este método, contudo, não é normalizado e, portanto, o mesmo foi validado, neste trabalho de pesquisa, para atender a este requisito. A validação foi feita com base no documento orientativo DOQ-CGCRE-08 e no guia EURACHEM. Os parâmetros de validação, para o ensaio quantitativo por EDXRF, que foram calculados neste trabalho são: seletividade; limite de detecção (LD) e limite de quantificação (LQ); linearidade e faixa de trabalho; veracidade de medição (tendência, erro normalizado, Z-score e comparação com método de referência) e precisão (repetibilidade, precisão intermediária e reprodutibilidade). Além disso, foi desenvolvida uma metodologia de cálculo de incerteza de medição para o ensaio por EDXRF Os resultados obtidos neste estudo demonstram que o método EDXRF, usado na determinação de metais em aços, é um método não normalizado validado e compatível com os resultados obtidos com os métodos de referência: espectrometria de fluorescência de raios X por dispersão de comprimento de onda (WDXRF), fotométricos e espectrometria de absorção atômica (AAS). Inclusive, o WDXRF é um método de referência usado em muitas normas internacionais, que descrevem métodos de análise de aços por fluorescência de raios X, como ASTM E572 ou ASTM E1085. O estudo desenvolvido nesta dissertação permitiu que o LACOR mantivesse sua acreditação no ensaio de determinação de metais por fluorescência de raios X, na avaliação do CGCRE/INMETRO, no presente ano. Outros frutos deste trabalho foram a confecção das curvas de calibração do espectrômetro NITON XL3t GOLDD+ e a revisão do procedimento de ensaio, onde esses novos conhecimentos sobre a técnica EDXRF foram aplicados. Futuramente, este trabalho pode ser usado por outros pesquisadores para desenvolver estudos em outras matrizes metálicas, como cobre, alumínio, titânio ou níquel, e, também, em outras áreas de aplicação como jóias, reciclagem de materiais metálicos ou, até mesmo, para análise elementar de resíduos retidos em membranas de troca iônica. / The development and validation of analytical methods is a required procedure when a non-standard method is used by a testing laboratory. Method validation is also a specific requirement of the ABNT NBR ISO / IEC 17025, which determines the general requirements for the competence of testing and calibration laboratories. The purpose of validation is to demonstrate that the analytical method, under the conditions in which it is performed, produces results with the required accuracy. The Corrosion, Protection and Recycling Materials Laboratory (LACOR), at UFRGS, has the X-ray fluorescence metal analysis, accredited by CGCRE / INMETRO, according to ABNT NBR ISO / IEC 17025. The test is performed using Energy Dispersive X-Ray Fluorescence spectrometry, EDXRF method. This method, however, is not standardized; therefore, it was validated in this research to meet this requirement. The validation was based on the DOQ-CGCRE-08 document and the EURACHEM guide. The method performance calculated in this study for quantitative testing by EDXRF are: selectivity; limit of detection (LOD) and limit of quantification (LOQ); linearity and working range; trueness (bias, normalized error, Z-score and comparison with reference method) and precision (repeatability, intermediate precision and reproducibility). In addition, a measurement uncertainty calculation methodology was developed for the EDXRF testing The results obtained in this study demonstrate that the EDXRF method, used in the determination in the chemical analysis of steels, is a validated non-standard method and compatible with the results obtained with the reference methods: Wavelength Dispersive X-Ray Fluorescence spectrometry (WDXRF), photometric and atomic absorption spectrometry (AAS). In addition, WDXRF is a reference method used in many international standards, which describes analysis of steels by X-ray fluorescence spectrometry such ASTM E572 or ASTM E1085. The study developed in this dissertation allowed LACOR to maintain its accreditation in the test of metal by X-ray fluorescence analysis, in the CGCRE / INMETRO audit, this year. Other fruits of this work were the preparation of calibration curves of NITON XL3t GOLDD + spectrometer and complete revision of testing procedure, where this new knowledge about the EDXRF technique was applied. In the future, this work can be used by other researchers to develop studies in other base metals such as copper, aluminum, titanium or nickel, and also in other areas of application such as jewelry, recycling of metallic materials or even for analysis elemental residues retained in ion exchange membranes.

A hidrolipodistrofia ginóide, popularmente denominada de celulite, é caracterizada como um processo distrófico que produz alterações estruturais dos elementos presentes na pele, como: modificações no tecido conjuntivo, comprometimento da microcirculação periférica cutânea, hipertrofia e hiperplasia dos adipócitos e edema. Os flavonóides são utilizados como substâncias ativas em preparações anticelulíticas por reduzirem a permeabilidade capilar. Os objetivos estabelecidos para esta pesquisa foram: (1) desenvolver emulsões cosméticas com finalidades anticelulíticas; (2) validar metodologia analítica para o doseamento de flavonóides totais, equivalentes em rutina, por espectrofotometria na região do ultravioleta; (3) avaliar a estabilidade física, físico-química e química das formulações. Formulações cosméticas anticelulíticas foram desenvolvidas contendo o extrato vegetal comercial de Trichilia catiguá Adr. Juss (e) Ptychopetalum olacoides Bentham (Slimbuster® H1), padronizado em flavonóides totais, equivalentes em rutina, e avaliadas quanto à estabilidade física, físico-química e química. Para sua quantificação, o método espectrofotométrico na região do ultravioleta a 361,0 nm foi empregado, comparando-se com rutina padrão secundário de referência (T = 96,1%). A avaliação da estabilidade envolveu três condições distintas de temperatura (5,0 + 0,5; 24 + 2 e 40,0 + 0,5 °C), pelo período de três meses, e as variáveis analisadas foram as características organolépticas, valor de pH, viscosidade aparente e teor de flavonóides totais. A metodologia foi validada quanto à linearidade, limites de detecção e quantificação, especificidade e pesquisa de interferentes, recuperação do padrão, precisão e exatidão intra e inter-dias. Os resultados da estabilidade indicaram que o teor de flavonóides totais, equivalentes em rutina, sofreu decaimento inferior a 10% nas condições de exposição à luz solar direta e/ou indireta, à temperatura ambiente (24 + 2 °C) e de refrigerador (5,0 + 0,5 °C), sendo que a 40,0 + 0,5 °C, condição de estufa, ocorreu redução de, aproximadamente, 35%. / Gynoid hydrolipodystrophy, popularly known as cellulite, is characterized as a dystrophic process that generates structural alterations of skin elements, as: connective tissue modifications, cutaneous microcirculation abnormalities, hypertrophy and hyperplasia of adipocytes and edema. Flavonoids are employed as raw materials in anticellulitic products by their capability to reduce capillary permeability. The objectives established for this research were: (1) development of anticellulitic cosmetic emulsions; (2) analytical method validation for total flavonoids, expressed in rutin, by ultraviolet spectrophotometry; (3) physical, physicochemical and chemical stability assay for the preparations. Anticellulitic cosmetic formulations containing the Trichilia catigua Adr. Juss (and) Ptychopetalum olacoides Bentham commercial extract (Slimbuster® H1), standardized in total flavonoids, expressed in rutin, were developed and their physical, physicochemical and chemical stability was assessed. Flavonoids were quantified within the ultraviolet spectrophotometric method at 361.0 nm as rutin equivalents by comparison with secondary standard rutin (T = 96.1%). Stability assay was conducted in three temperature conditions (5.0 + 0.5; 24 + 2 e 40.0 + 0.5 °C) and the following parameters were analyzed: aspect, color and odor, pH and apparent viscosity values and flavonoid content. Analytical methodology was validated determining linearity, limits of detection and quantification, specificity and interferent assay, recovery and intra and inter-run precision and accuracy. Results from stability evaluation have indicated decrease of flavonoid content inferior than 10% at sunlight exposure (room temperature, 24 + 2 °C) and at 5.0 + 0.5 °C; high temperature (40.0 + 0.5 °C) has reduced the flavonoid content at, approximately, 35%.