Os ruídos, vibrações e asperezas de rodagem veicular (do acrônimo em inglês Road NVH), presentes de 20 Hz até 1000 Hz aproximadamente, originam-se das vibrações e propagações acústicas dos pneus ao interagir com as superfícies. Nestas fontes de ruído, ambas as vias de contribuições estruturais e aéreas, são relevantes para o refinamento veicular. Constantes são os esforços para estudar o veículo como um conjunto de caminhos de transferência entre a dinâmica dos pneus até o conforto dos passageiros. Sendo assim, o tratamento dos mecanismos que geram e propagam o ruído e vibração à cabine está avançando, graças aos testes e análises sistemáticas, fundamentadas na teoria de Análises dos Caminhos de Transferências de energia (TPA do inglês transfer path analysis). O objetivo deste trabalho é apresentar um estudo de um caso de Road NVH utilizando o TPA em veículo protótipo. Neste tema, é investigado o nível de ruído de rodagem em torno de 180 Hz, semelhante ao efeito de roncar (rumble, na expressão em inglês). Este ruído permanece presente no protótipo, em diversos tipos de pista e velocidades, porém em apenas um modelo de pneu (batizado de modelo \"A\"), entre os diversos testados. Das avaliações subjetivas prévias, defini-se que o foco das investigações são as contribuições estruturais da suspensão dianteira. Usando o TPA para demonstrar os caminhos críticos na formação do rumble, aplicou-se o método da matriz inversa para o calculo das forcas, considerando os seguintes pontos: buchas do braço de controle do A-Arm e de ligação da carroceria com a parte superior da suspensão dianteira (fig. 4.6 - tipo Mc Pherson). Foram obtidas experimentalmente as vibrações dos lados ativos e passivos destes pontos, nas condições de rolagem e as funções de resposta vibracionais e acústica do ponto, no laboratório. Após a correlação do ruído interno calculado com o medido, concluiu-se que o rumble deste caso foi gerado pela baixa eficiência de isolação das vibrações radiais nas buchas anteriores e pela força lateral do pneu \"A\". Por fim, propostas de bucha e pneu são apresentadas em termos das novas forças e respostas acústicas transmitidas, para minimizar o rumble. / The road noise, vibration and harshness (Road NVH) present from 20 Hz to 1000 Hz approximately, begins from the tires vibration and acoustic propagation and their interactions with the road surfaces. In these noise sources, both structural-borne and air-borne noise contributions are relevant to vehicle refinement. The constant efforts to study the vehicle as a set of transfer paths from tires dynamic behavior to passenger comfort to the final passenger comfort perception. Thus the treatment of generation and propagation mechanisms, have being forward thanks to the systematic tests and proceedings based on the transfer path analysis theory (TPA). The purpose of this work is to present a case study of Road NVH, using TPA in prototype vehicle. On this theme, it is investigated a higher noise level around 180 Hz, on the rumble narrow band. This noise remains in the prototype during several types of tracks and speeds conditions, whenever only a tire model, named as sample A, is used, despites all tires tested. From the previous subjective evaluation, the focus of the investigation is defined to be structure-borne of the front suspension. Using TPA to demonstrate the critical paths to rumble, it was applied the matrix inversion method to force calculation, considering the follow points: A-Arm type lower control arm bushings and top mounts of front suspension (picture 4.6 - Mc Pherson type). The vibration in the active and passive side of these points during test conditions and the FRFs driving points and body sensitivity for a target microphone were obtained experimentally. After correlation between internal road noise calculated and the measured, it was concluded the Rumble of this case had been formed by low radial vibration isolation of the front bushings and due lateral forces of tire A. At last, the bushing and tire proposals are presented in terms of new transmitted forces and acoustical responses, to minimize the rumble.

Submitted by Emanuel Varela Cardoso (emanuel.varela@ufcg.edu.br) on 2018-06-11T20:04:19Z No. of bitstreams: 1 RENATA DUARTE ALMEIDA – TESE (PPGEP) 2017.pdf: 2335363 bytes, checksum: 0dab812c856b00737582f4fa8aeb67f6 (MD5) / Made available in DSpace on 2018-06-11T20:04:19Z (GMT). No. of bitstreams: 1 RENATA DUARTE ALMEIDA – TESE (PPGEP) 2017.pdf: 2335363 bytes, checksum: 0dab812c856b00737582f4fa8aeb67f6 (MD5) Previous issue date: 2016-12 / O umbu apresenta um grande potencial a ser explorado e o desenvolvimento de novas tecnologias visa estabelecer condições que retardem o seu amadurecimento, mantendo a qualidade e prolongando a vida útil durante o armazenamento, possibilitando ainda minimizar as perdas pós-colheita e o surgimento de novos produtos no mercado, a exemplo dos doces de corte que podem estimular fortalecimento da agricultura familiar e o desenvolvimento de pequenas agroindústrias. Objetivou-se, com este trabalho, o desenvolvimento de uma tecnologia para produção de doce de umbu de corte com leite e sem leite preservando o sabor característico da fruta e de aceitação sensorial. Os frutos foram cozidos em água durante 5 minutos após fervura, em seguida foi feita a extração da polpa de forma manual, a massa obtida foi homogeneizada e acondicionadas em freezer horizontal à temperatura de -30ºC. Foram investigados, assim, as características, físicas, físico-quimicas, químicas, microbiológicas da polpa pré-cozida e dos doces de corte de umbu, o comportamento reológico das diferentes formulações para a elaboração dos doces a 5, 10, 15 e 25 ºC, as curvas de congelamento das formulações nas temperaturas de -20, -50 e -75ºC, além da avaliação instrumental de textura, teste TPA e da análise descritiva de ordenação dos doces de corte de umbu. Os doces que apresentaram maior porcentagem de leite/açúcar (I) 89,32% e açúcar (II) 85,21% em suas formulações resultaram em um maior rendimento e tempo de preparo dos doces. No estudo reológico para uma tensão de cisalhamento fixa a taxa de deformação diminui com o aumento da temperatura, confirmando o caráter não newtoniano e comportamento pseudoplástico, os modelos de Herschel-Bulkley e Mizrahi-Berk apresentaram ajustes semelhantes e também foram os melhores modelos para todas as formulações estudadas. As curvas de congelamento apresentaram as três fases bem definidas e um comportamento tendencioso, no qual a difusividade efetiva média aumenta à medida que diminui a quantidade de água e aumenta os sólidos presentes nas amostras. A avaliação do parâmetro de firmeza indica que o aumento da concentração de polpa de umbu aumenta o valor da adesividade, uma vez que o processo faz com que o tempo de cocção seja maior, tornando o produto mais firme e consequentemente, mais adesivo. Os valores de gomosidade e mastigabilidade apresentam o mesmo comportamento da firmeza, em que, quanto maior for a concentração da polpa de umbu nos doces elaborados, maior será a energia necessária para mastigar o produto. Percebe-se que o doce (II) sem adição de leite em sua formulação apresentou o maior valor médio (4,41) na análise de preferência, aparência (4,64), cor (5,05) e consistência (4,41), o que indica a maior preferência pelos julgadores. No entanto, mesmo os doces sem adição de leite possuindo coloração semelhante aos doces comerciais de goiaba a similaridade desses doces não influenciou nos resultados dessa pesquisa, conforme as médias de preferência foram verificadas também nos doces de umbu com adição de leite nas formulações, I (4,11), III (3,73) e V (4,12) o que resulta na boa aceitação pelos julgadores. / The umbu has great potential to be exploited and the development of new technologies aiming to establish conditions that delay ripening, maintain quality and prolong shelf life, will contribute to minimize postharvest losses and the emergence of new products on the market, such as fruit preserves that can stimulate the strengthening of family farming and the development of small agro-industries. The objective of this work was the development of a technology for the production of umbu sweet paste with milk and without milk preserving the characteristic fruit flavor and sensory acceptance. The fruits were boiled in after boiling water for 5 minutes, then the pulp was extracted manually, the mass obtained was homogenized and conditioned in a horizontal freezer at the temperature of -30 ° C. Several characterization techniques were employed namely: the physical, chemical, physicochemical, and microbiological characteristics of the precooked pulp and the umbu paste; the rheological behavior of the different formulations for the preparation of umbu pastes at 5, 10, 15 and 25 ºC; the freezing curves of those formulations at temperatures of -20, -50 and -75ºC; as well as the instrumental evaluation of texture, TPA test and the descriptive analysis of the order of the umbu paste. The sweets that presented the highest percentage of milk / sugar (I) 89.32% and sugar (II) 85.21% in their formulations resulted in a higher yield and higher preparation time of the umbu paste. In the rheological study, using a constant shear stress, the rate of deformation decreases with increasing temperature, confirming the non-Newtonian character and the pseudoplastic behavior, where the Herschel-Bulkley and Mizrahi-Berk models presented similar adjustments and were also the best models for all the formulations studied. The freezing curves presented the three well defined phases and a biased behavior, where the average effective diffusivity increases with decreasing water content and increasing solids content in samples. The evaluation of the firmness parameter indicates that the increase of the concentration of umbu pulp increases the value of the adhesiveness, due to the necessity of larger cooking times making the product firmer and consequently more adhesive. The guminess and chewiness values show the same firmness behavior, which is the higher the concentration of the umbu pulp in the umbu paste, the greater the energy required to chew the product. It was observed that the umbu paste (II) without added milk in its formulation had the highest mean value (4.41) in the analysis of preference, appearance (4.64), color (5.05) and consistency (4.41), which indicates the highest preference of the judges. However, eventhough the umbu paste without added milk had similar coloration to the commercial guava paste, the similarity of both pastes did not influence the results of the present research, as the averages of preference were also verified in the umbu paste with addition of milk in the formulations, I (4,11), III (3,73) and V (4,12) which results in a good acceptance by the judges.

Os ruídos, vibrações e asperezas de rodagem veicular (do acrônimo em inglês Road NVH), presentes de 20 Hz até 1000 Hz aproximadamente, originam-se das vibrações e propagações acústicas dos pneus ao interagir com as superfícies. Nestas fontes de ruído, ambas as vias de contribuições estruturais e aéreas, são relevantes para o refinamento veicular. Constantes são os esforços para estudar o veículo como um conjunto de caminhos de transferência entre a dinâmica dos pneus até o conforto dos passageiros. Sendo assim, o tratamento dos mecanismos que geram e propagam o ruído e vibração à cabine está avançando, graças aos testes e análises sistemáticas, fundamentadas na teoria de Análises dos Caminhos de Transferências de energia (TPA do inglês transfer path analysis). O objetivo deste trabalho é apresentar um estudo de um caso de Road NVH utilizando o TPA em veículo protótipo. Neste tema, é investigado o nível de ruído de rodagem em torno de 180 Hz, semelhante ao efeito de roncar (rumble, na expressão em inglês). Este ruído permanece presente no protótipo, em diversos tipos de pista e velocidades, porém em apenas um modelo de pneu (batizado de modelo \"A\"), entre os diversos testados. Das avaliações subjetivas prévias, defini-se que o foco das investigações são as contribuições estruturais da suspensão dianteira. Usando o TPA para demonstrar os caminhos críticos na formação do rumble, aplicou-se o método da matriz inversa para o calculo das forcas, considerando os seguintes pontos: buchas do braço de controle do A-Arm e de ligação da carroceria com a parte superior da suspensão dianteira (fig. 4.6 - tipo Mc Pherson). Foram obtidas experimentalmente as vibrações dos lados ativos e passivos destes pontos, nas condições de rolagem e as funções de resposta vibracionais e acústica do ponto, no laboratório. Após a correlação do ruído interno calculado com o medido, concluiu-se que o rumble deste caso foi gerado pela baixa eficiência de isolação das vibrações radiais nas buchas anteriores e pela força lateral do pneu \"A\". Por fim, propostas de bucha e pneu são apresentadas em termos das novas forças e respostas acústicas transmitidas, para minimizar o rumble. / The road noise, vibration and harshness (Road NVH) present from 20 Hz to 1000 Hz approximately, begins from the tires vibration and acoustic propagation and their interactions with the road surfaces. In these noise sources, both structural-borne and air-borne noise contributions are relevant to vehicle refinement. The constant efforts to study the vehicle as a set of transfer paths from tires dynamic behavior to passenger comfort to the final passenger comfort perception. Thus the treatment of generation and propagation mechanisms, have being forward thanks to the systematic tests and proceedings based on the transfer path analysis theory (TPA). The purpose of this work is to present a case study of Road NVH, using TPA in prototype vehicle. On this theme, it is investigated a higher noise level around 180 Hz, on the rumble narrow band. This noise remains in the prototype during several types of tracks and speeds conditions, whenever only a tire model, named as sample A, is used, despites all tires tested. From the previous subjective evaluation, the focus of the investigation is defined to be structure-borne of the front suspension. Using TPA to demonstrate the critical paths to rumble, it was applied the matrix inversion method to force calculation, considering the follow points: A-Arm type lower control arm bushings and top mounts of front suspension (picture 4.6 - Mc Pherson type). The vibration in the active and passive side of these points during test conditions and the FRFs driving points and body sensitivity for a target microphone were obtained experimentally. After correlation between internal road noise calculated and the measured, it was concluded the Rumble of this case had been formed by low radial vibration isolation of the front bushings and due lateral forces of tire A. At last, the bushing and tire proposals are presented in terms of new transmitted forces and acoustical responses, to minimize the rumble.

Over the last years, due to the development of quieter engines and drivetrains, the importance of addressing the vehicle wind noise problem has significantly increased.In this thesis work, several existing Transfer Path Analysis methods have been applied on an experimental database acquired during a wind tunnel test on a passenger car with the objective of analyzing the distribution of the wind noise sources and their contribution to the target microphones located inside the vehicle. A major challenge for the Transfer Path Analysis (TPA) consists of the high complexity of the aerodynamic sources exciting the structure. Moreover, the existence of multiple incoherent source phenomena, and the presence of distributed coherent source regions of different correlation scales make the analysis very complex.The thesis work provides a solid and comprehensive analysis of the results obtained by different methods. The outcomes can be potentially useful for optimizing the vehicle NVH performance in future practical cases. / Under de senaste åren har vikten av att arbeta med vägfordons problem med aerodynamisk ljudgenerering ökat avsevärt på grund av utvecklingen av tystare motorer och drivlinor. I det här projektet har flera existerande metoder för Transfer Path Analysis (TPA) tillämpats på en databas med experimentella data som samlats in vid vindtunneltest på en personbil, med målet att analysera fördelningen av källorna orsakade av vindbruset och deras påverkan på ljudnivån vid de uppsatta målmikrofonerna inuti fordonet. En stor utmaning för TPA är den höga komplexiteten hos de aerodynamiska källorna som exciterar strukturen. Vidare gör förekomsten av flera okorrelerade källor, och närvaron av distribuerade koherenta källregioner med olika korrelationsskalor, analysen mycket komplex. Arbetet presenterar en solid och omfattande analys av resultat som erhållits med olika metoder. Resultaten är potentiellt användbara för att optimera fordonets NVH-prestanda i praktiktiken i framtiden.

Experimental validations are widely used for studying dynamic structural behaviors and these studies involve defining the structures completely as being used in real time. While in numerical simulations such detailed features are not specified to ease the computation, thereby deviating from accurate results. Hence experimental validations are more desired in product developments process. Applications of experimental verification for noise and vibration (referred to as NVH inautomotive industry) are expanding over the last few decades. Researchers are exploring ways to predict the responses on the new receiver using receiver independent forces, which led to evolution of component based TPA (Transfer Path Analysis) concept. The Component based TPA concept is an important development in automotive industry. It allows the auto manufacturers to make use of their available subsystems (like motor or a gearbox) in their newly developing vehicles. This has been made possible by defining the dynamic forces exerted by the source independent of receiving structure, which are then used to predict the responses on the new receiver. Evaluation of such receiver independent forces allows measurements to be made in a test rig rather than in the vehicle. This indeed helps in better communication between different departments or between suppliers and vehicle manufacturers, saves design iterations and time, and would help vehicle manufactures to predict the vehicle structural behaviors much before the first prototype is made. The method is based on the international standard ISO 20270:2019 (en) Acoustics – Characterization of sources of structure-borne sound and vibration – indirect measurement of blocked forces. The thesis is based on evaluating the source characterized forces that are used for predicting responses on a new receiving structure. For this, different methods in TPA are explored and for the rear drive unit application, in-situ method is chosen. The source characterized forces also termed as blocked forces are computed in different test set up and a validation check is performed. The obtained results are also compared with FEM and useful conclusions are drawn. And finally contact forces evaluated by integrating the subsystems are compared to the contact forces derived from the source characterized forces. / Experimentell verifiering av dynamiska krafter och vibrationer som uppkommer i fordon innebär mätning av tids-, frekvens- och/eller varvtalsberoende kvantiteter. Numeriska beräkningar har utvecklats till en hög nivå, men kan ännu inte beskriva alla förlopp och detaljer som förekommer i de verkliga processerna. På grund av detta krävs det fortfarande mätningar som en del av produktionsutvecklingen. Valideringsmetoder för ljud och vibrationer har utvecklats mycket desenaste decennierna, och ett mål har varit att utveckla mätmetoder där de uppmätta krafterna från en komponent som bidrar till buller kan mätas på ett sätt som inte beror på den testrigg eller det fordon den mäts i. Komponentbaserad TPA Transfer Path Analysis är en analysmetod som är viktig inom fordonsindustrin. Den gör det möjligt för en tillverkare att använda modeller av existerande komponenter (t.ex. motorer eller växellådor) i modeller för nya fordon. En grundläggande förutsättning är att de krafter som mäts är oberoende av den mottagande strukturen, det vill säga fordonet. Om krafterna är oberoende av strukturen där de mäts innebär det att komponenten kan mätas i en test rigg på ett annat ställe (till exempel hos en underleverantör) och att tillgång till fordon inte krävs för karaktäriseringen. Det underlättar kommunikationen mellan olika delar av organisationen och mellan underleveratörer och tillverkare och bidrar till att prediktera ljud och vibrationer innan den första prototypen är tillgänglig. Den föreslagna metoden är baserad på den internationella normen ISO 20270:2019 (en) Acoustics – Characterization of sources of structure-borne sound and vibration – indirect measurement of blocked forces. Examensarbetet handlar om att utveckla en mätmetod för att kunna ta fram krafter genererade av komponenter som är oberoende av testriggens egenskaper. De framtagna krafterna kan då användas i en virtuell fordonsmodell för att se ljud och vibrationsbidragen på fordonsnivå. Källan som har studerats är en slutväxel (rear drive unit) för fyrhjulsdrift i bil. Flera olikametoder för TPA har undersöks, och för karaktärisering av slutväxeln har in-situ metoden valts. Krafter som är oberoende av den mottagande strukturen kallas även ‘blocked forces’. Krafterna beräknas baserat på resultaten från flera olika delmätningar. Validering och även jämförelse medFEM beräkningar har gjorts liksom jämförelser mellan mätningar på enbart komponenten och av hela systemet.

Based on the linear relationship between concentration of H2O2 and the decrease of electrochemiluminescence (ECL) intensity in a Ru(bpy)32+/TPA system, procedures for the indirect determination of glucose with a flow injection analysis were developed. By passing solutions of glucose through a FIA system containing a glucose oxidase (GOx) immobilized sol-gel column and an ECL system of Ru(bpy)32+ and TPA, glucose can be determined optimally with a detection limit of 1.0 £gM in a linear dynamic range of 1.0 ¡V 200.0 £gM. A repetitive injection of glucose (100 £gM) and human serum solutions gave satisfactory reproducibility with relative standard deviations of 1.3 (N=31) and 3.9 % (N=42) respectively. Interference due to the presence of ascorbic acid, uric acid or other reducible agents in solution can be corrected by passing sample solutions through another sol-gel column that contained no GOx. From the agreement between the contents of glucose in human serum and soft drink analyzed by the developed method and those obtained by the spectroscopy method based glucose assay kit and satisfactory recovery of glucose from interferent containing solutions, the feasibility of the developed method for real sample analysis was confirmed. One of the major purposes of this study was to develop new immobilization approaches and flow cell designs for the fabrication of regenerable ECL-based sensors with improved sensitivity, convenience and long-term stability. Silica particulates were used as immobilization support in ECL sensors for TPA and NAD(P)H and in biosensors for glucose and glucose-6-phosphate¡]G6P¡^. The first ECL flow cell was fabricated from a glass tube, and a platinum wire was used as working electrode held at +1.3 V. The volume of the flow cell was about 50 £gL. An Ag/AgCl electrode and a piece of Pt wire were used as the reference and counter electrode respectively and placed downstream of the working electrode. Ru(bpy)32+ immobilized silica particulates with 1/3 silica sol content showed the best performance for TPA determination, and the sensitivity of TPA determination was dependent upon the amount of Ru(bpy)32+ immobilized in silica particulates. The lowest level of analyte detected for TPA was 0.02£gM, and linear range was from 0.02£gM to 5£gM. Up to a certain concentration level, it was found that Ru(bpy)32+ was tightly held in silica particulates and did not leach out into aqueous solutions, even with continuous flow for up to ten hours. Ru(bpy)32+ immobilized silica particulates were characterized of well activity and high stability; that stored at 0¢J exhibited its original activity for up to one year. The second ECL flow cell was fabricated from a piece of epoxy block supported Pt electrode (1 ¡Ñ 2 cm) as counter electrode, a piece glass window and a polyethylene spacer with 78 £gL cell volume, two 2.0-cm length of 0.6-mm diameter platinum wires were used as working electrodes held at +1.1 V, and an Ag/AgCl electrode as reference electrode. All three electrodes were incorporated within the main body of the cell. One of the biosensor design packed Ru(bpy)32+ incorporated silica particulates in the ECL flow cell, and a glucose dehydrogenase (GDH) immobilized silica sol-gel column is placed between the sample injection valve and the flow cell. The ECL response to samples containing glucose and cofactor (NADP) results from the Ru(bpy)33+ ECL reaction with NADPH produced by glucose dehydrogenase. This ECL biosensor was shown applicable for both NAD+- and NADP+- dependent enzymes, where NADH detection ranged from 0.50£gM ¡V 5.0 mM NADH and NADPH detection ranged from 1.0£gM - 3.0 mM NADPH. Glucose can be determined in a linear dynamic range of 5.0 - 500 £gM. Another biosensor design immobilized glucose-6-phosphate dehydrogenase¡]G6PDH¡^onto the Ru(bpy)32+ -doped silica particulates through silica chemistry and then packed these particulates into the ECL flow cell. By passing samples containing G6P and cofactor (NAD) through the ECL flow cell, G6P can be determined in a linear dynamic range of 10.0 £gM-1.0 mM. The regenerable ECL biosensor was characterized of good reproducibility and well stability for flow injection analysis. A repetitive injection of NADH (100 £gM) and G6P¡]500£gM¡^gave satisfactory reproducibility with relative standard deviations of 2.8 %¡]N=105¡^and 2.8 % (N=40) respectively.

No description available.

The synthesis of pure tris(6-hydroxymethyl-2-pyridylmethyl)amine (H₃L₁₁) is reported for the first time. New complexes of H₃L₁₁ with copper(II), manganese(II) and iron(III) have been characterised by X-ray crystallography. Linear [Fe₃(L₁₁)₂](ClO₄)₃ reveals the tightest Fe-O-Fe angle (87.6°) and shortest Fe...Fe distance (2.834 Å) presently found for a weakly antiferromagnetically-coupled high spin alkoxide-bridged polyiron(III) system. H₃L₁₁ provides a route to various hydrophobic peralkylated TPA ligand derivatives for creating a hydrophobic pocket for the assembly of iron catalysts for the novel 1-hydroxylation of n-alkanes. New 6-py substituted TPA ligands containing methyl (L₁₅) and n-octyl (L₁₆) ether linkages were synthesised via alkylation. Two further novel 6-py substituted ligands were synthesized incorporating n-hexyl substituents on one (L₂₁) and two (L₂₂) of the py moieties. Here a urea spacer group was used to promote hydrogen–bond assisted heterolytic O-O cleavage (generation of the potent FeV=O oxidant) within the hydroxoperoxoiron(III) precursor. High spin [FeII(L)(CH₃CN)[subscript(x)]](CF₃SO₃)₂ complexes (x = 0–2, L = L₁₅,₁₆,₂₁,₂₂) were characterised in solution by ¹H NMR. The structure of [Fe(L₂₂)](CF₃SO₃)₂ reveals a distorted iron(II) centre bound to four N atoms and two urea carbonyls. Iron(II) complexes of H₃L₁₁, L₁₅,₁₆,₂₁,₂₂ and tris(6-Br)-TPA (L₂₄), were investigated for catalysis of the oxygenation of cyclohexane by H₂O₂. Reaction of the iron(II) complexes with H₂O₂ and [superscript(t)]BuOOH was followed by time-resolved EPR and UV-VIS spectrophotometry. A correlation between the observed catalytic activity and the nature of the FeIII(L)-OOR intermediates generated is apparent. A convenient ‘one-pot’ synthesis of benzene-1,3,5-triamido-tris(l-histidine methyl ester) is reported along with attempts at preparing N,N’-bis(pyridylmethyl)-1,3- diaminopropane-2-carboxylic acid (L₂₅), a new water soluble pyridine-amine ligand. The final demetallation step resulted in ligand hydrolysis to the novel amino acid; 1,3-diaminopropane- 2-carboxylic acid which was characterised as its HCl salt by X-ray crystallography.

A análise de caminhos de transferência de energia (TPA na sigla em inglês para Transfer Path Analysis) corresponde a um grupo de métodos numérico/experimental para análise e solução de problemas vibro-acústicos de sistemas lineares invariantes no tempo, sendo seu principal campo de aplicação a indústria automotiva. A TPA é uma técnica que identifica as principais fontes de vibração e ruído, e os caminhos estruturais e acústicos pelos quais são transmitidas para determinados locais de interesse. Conhecendo as fontes de ruído e vibração e os caminhos de propagação é possível propor modificações eficientes em minimizar o ruído/vibração nas regiões de interesse, ou atribuir características desejáveis para tais componentes, envolvendo técnicas de controle passivo e ativo. Este trabalho apresenta um estudo numérico e experimental das técnicas de TPA, utilizando métodos diretos e inversos de determinação de forças operacionais. Estes estudos foram realizados em um mockup de um veículo, com o objetivo de determinar o caminho de maior contribuição para o ruído no interior do protótipo, e a partir deste resultado, propor um sistema de controle ativo para minimizar este ruído interno. / The Transfer Path Analysis (TPA) is a group of numerical/experimental tools for the analysis and troubleshooting of noise and vibration problems in linear time invariant vibroacoustic systems, being the automotive sector its major user. TPA consists of a numerical/experimental analysis that allows the identification of the main noise and vibration sources and the structural/acoustic transfer paths to the Target points. Based on the sources and paths, it is possible to propose modifications that efficiently minimize noise and vibration at the target positions. By means of active control it is possible to modify noise and vibration in order to change, rather than minimize noise and vibration, achieving certain design targets. This work presents a numerical and experimental study of TPA techniques, using direct and inverse operational loads determination methods. These studies were performed on a vehicle mockup, in order to determine the path of greatest contribution to the noise inside the prototype, and from this result, propose an active control system to minimize this internal noise.

Cette thèse est consacrée à l’étude des mécanismes d’interaction laser-matière en régime femtoseconde pour l’analyse de circuits intégrés par stimulation photoélectrique non-linéaire. Cette technique permet d’accroitre la résolution pour répondre à la miniaturisation des composants électroniques. Les milieux étudiés dans ce travail sont plus particulièrement le silicium, matériau constitutif des circuits intégrés, et la silice pour le transport des impulsions laser dans une fibre optique. En effet, l’émergence de cette technique d’analyse en milieu industriel requiert l’utilisation de systèmes compacts, fiables et sécuritaires. Les simulations réalisées montrent la génération de charges dans le silicium et la propagation des impulsions dans des fibres photoniques à cœur creux identifiées pour limiter les effets non-linéaires. Des expérimentations sur composants permettent de les confronter aux simulations et de valider l’utilisation de ce type de fibres.Enfin, ce travail a permis de déterminer les paramètres optiques et laser essentiels ainsi que les technologies compatibles avec les contraintes industrielles en analyse de circuits intégrés. / This thesis is dedicated to the study of laser-matter interaction mechanisms in femtosecond regime for the analysis of integrated circuits by nonlinear photoelectric laser stimulation. This technique improves the resolution in order to deal with the miniaturization of electronic components. The materials studied in this work are silicon, a major chemical component in semiconductor electronics, and silica used for transporting laser pulses in optical fibers. Indeed, the emergence of this analysis technique in industrial environments needs the use of compact, reliable and safe systems. The performed simulations show charge generation in silicon and propagation of pulses in photonic fibers identified for limiting nonlinear effects. Some experiments on components allow a comparison with simulations and validation of the use of this type of fibers. Finally, this work was able to identify key optical and laser parameters along with technologies compatible with industrial constraints in integrated circuit analysis.