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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1591

Development Of An Advanced Methodology For Automotive IC Engine Design Optimization Using A Multi-Physics CAE Approach

Sehemby, Amardeep A Singh 09 1900 (has links) (PDF)
The internal combustion engine is synonyms with the automobile since its invention in late 19th century. The internal combustion engine today is far more advanced and efficient compared to its early predecessors. An intense competition exists today amongst the automotive OEMs in various countries and regions for stepping up sales and increasing market share. The pressure on automotive OEMs to reduce fuel consumption and emission is enormous which has lead to innovations of many variations in engine and engine-related technologies. However, IC engines are in existence for well more than a century and hence have already evolved to a highly refined state. Changes in IC engine are therefore largely incremental in nature. A deterrent towards development of an engine configuration that is significantly different from its predecessor is the phenomenal cost involved in prototyping. Thus, the only viable alternative in exploring new engine concepts and even optimizing designs currently in operation is through extensive use of CAE. In light of published work in the field of analysis of IC engines, current research effort is directed towards development of a rational methodology for arriving at a weight-optimized engine design, which simultaneously meets performance of various attributes such as thermal, durability, vehicle dynamics and NVH. This is in contrast to the current methodology adopted in industry, according to which separate teams work on aspects of engine design such as combustion, NVH (Noise, Vibration and Harshness), acoustics, dynamics, heat transfer and durability. Because of the involvement of heterogeneous product development groups, optimization of an engine for weight, which can have a significant impact on its power-to-weight ratio, becomes a slow process beset with manual interventions and compromise solutions. Thus, following the traditional approach, it is quite difficult to claim that an unambiguous weight-optimized design has been achieved. As a departure from the practiced approach, the present research effort is directed at the deployment of a single multi-physics explicit analysis solver, viz. LS-DYNA - generally known for its contact-impact analysis capabilities, for simultaneously evaluating a given engine design for heat transfer, mechanical and thermal loading, and vibration. It may be mentioned that only combustion analysis is carried out in an uncoupled manner, using proven phenomenological thermodynamic relations, to initially arrive at mechanical and thermal loading/boundary conditions for the coupled thermo-mechanical analysis. The proposed methodology can thus be termed as a semi-integrated technique and its efficacy is established with the case study of designing a single cylinder air-cooled diesel engine from scratch and its optimization.
1592

Role Of Sea Surface Temperature Gradient In Intraseasonal Oscillation Of Convection In An Aquaplanet Model

Das, Surajit 09 1900 (has links) (PDF)
In this thesis we examine intra-seasonal oscillations (ISO) in the aqua-planet setup of the Community Atmospheric Model (CAM) version 5.1, mainly based on July and January climatological sea surface temperature (SST). We investigate mainly two questions -what should be the SST distribution for the existence of (a) northward moving ISO in summer, and (b) eastward moving MJO-like modes in winter. In the first part of the thesis we discuss the northward propagation. A series of experiments were performed with zonally symmetric and asymmetric SST distributions. The basic lower boundary condition is specified from zonally averaged observed July and January SST. The zonally symmetric July SST experiment produced an inter tropical convergence zone (ITCZ) on both sides of the equator. Poleward movement is not clear, and it is confined to the region between the double ITCZ. In July, the Bay of Bengal (BOB) and West Pacific SST is high compared to the rest of the northern tropics. When we impose a zonally asymmetric SST structure with warm SST spanning about 80 of longitude, the model shows a monsoon-like circulation, and some northward propagating convective events. Analysis of these events shows that two adjacent cells with cyclonic and anticyclonic vorticity are created over the warm SST anomaly and to the west. The propagation occurs due to the convective region drawn north in the convergence zone between these vortices. Zonally propagating Madden-Julian oscillations (MJO) are discussed in the second part of the thesis. All the experiments in this part are based on the zonally symmetric SST. The zonally symmetric January SST configuration gives an MJO-like mode, with zonal wave number 1 and a period of 40-90 days. The SST structure has a nearly meridionally symmetric structure, with local SST maxima on either side of the equator, and a small dip in the equatorial region. If we replace this dip with an SST maximum, the time-scale of MJO becomes significantly smaller (20-40 days). The implication is that an SST maximum in the equatorial region reduces the strength of MJO, and a flat SST profile in the equatorial region is required for more energetic of MJO. This result was tested and found to be valid in a series of further experiments.
1593

Experimental Study on the Engineering Properties of Gelfill

Abdul-Hussain, Najlaa January 2011 (has links)
Gelfill (GF) is made of tailings, water, binder and chemical additives (Fillset, sodium silicate gel). The components of GF are combined and mixed on the surface and transported (by gravity and/or pumping) to the underground mine workings, where the GF can be used for both underground mine support and tailings storage. Thermal (T), hydraulic (H), and mechanical (M) properties are important performance criteria of GF. The understanding of these engineering properties and their evolution with time are still limited due to the fact that GF is a new cemented backfill material. In this thesis, the evolution of the thermal, hydraulic, mechanical, and microstructural properties of small GF samples are determined. Various binder contents of Portland cement type I (PCI) are used. The GF is cured for 3, 7, 28, 90, and 120 days. It is found that the thermal, hydraulic and mechanical properties are time-dependent or affected by the degree of binder hydration index. Furthermore, a relationship is found between the compressive strength and the saturated hydraulic conductivity of the GF samples. The unsaturated hydraulic properties of GF samples have also been investigated. The outcomes show that unsaturated hydraulic conductivity is influenced by the degree of binder hydration index and binder content, especially at low suction ranges. Simple functions are proposed to predict the evolution of air-entry values (AEVs), residual water content, and fitting parameters from the van Genuchten model with the degree of hydration index (α). Furthermore, two columns are built to simulate the coupled thermo-hydro-mechanical (THM) behaviour of GF under drained and undrained conditions. The obtained results from the GF columns are compared with the small samples. It is observed that the mechanical properties, hydraulic properties (suction and water content), and temperature development are strongly coupled. The magnitude of these THM coupling factors is affected by the size of the GF. The findings also show that the mechanical, hydraulic and thermal properties of the GF columns are different from samples cured in plastic moulds.
1594

Systemization of RFID Tag Antenna Design Based on Optimization Techniques and Impedance Matching Charts

Butt, Munam January 2012 (has links)
The performance of commercial Radio Frequency Identification (RFID) tags is primarily limited by present techniques used for tag antenna design. Currently, industry techniques rely on identifying the RFID tag application (books, clothing, etc.) and then building antenna prototypes of different configurations in order to satisfy minimum read range requirements. However, these techniques inherently lack an electromagnetic basis and are unable to provide a low cost solution to the tag antenna design process. RFID tag performance characteristics (read-range, chip-antenna impedance matching, surrounding environment) can be very complex, and a thorough understanding of the RFID tag antenna design may be gained through an electromagnetic approach in order to reduce the tag antenna size and the overall cost of the RFID system. The research presented in this thesis addresses RFID tag antenna design process for passive RFID tags. With the growing number of applications (inventory, supply-chain, pharmaceuticals, etc), the proposed RFID antenna design process demonstrates procedures to design tag antennas for such applications. Electrical/geometrical properties of the antennas designed were investigated with the help of computer electromagnetic simulations in order to achieve optimal tag performance criteria such as read range, chip-impedance matching, antenna efficiency, etc. Experimental results were performed on the proposed antenna designs to compliment computer simulations and analytical modelling.
1595

Comportement local et performances électriques d'une pile à combustible à membrane : vers un outil de diagnostic / Proton exchange membrane fuel cell local behavior and electric performances : basis to a diagnosis tool

Chupin, Sylvain 11 December 2009 (has links)
Le travail de thèse présenté ici apporte des éléments de compréhension sur l'influence de la gestion de l'eau et de la gestion thermique d'une PEMFC sur ses performances électriques. Un modèle bidimensionnel représentant les transferts de matière et de chaleur dans l'épaisseur d'une cellule élémentaire et le long des canaux d'alimentation est mis en place. Une partie spécifique de l'étude concerne la modélisation microscopique des agglomérats réactionnels et l'influence de l'eau présente dans ces zones actives sur les performances électriques locales et globales de la pile. Dans l'optique de réaliser un modèle pouvant s'intégrer à un système de contrôle, les transports couplés de l'eau liquide et vapeur, de la chaleur et des charges sont résolus analytiquement. Quelles que soient les conditions de fonctionnement, le modèle permet de calculer quel est l'état interne de la pile en terme d'hydratation, de production de courant et de chaleur. Le diagnostic de l'état interne de la pile en fonction des conditions opératoires permet de connaître précisément comment adapter les paramètres d'alimentation de la pile pour obtenir des performances électriques optimales. Les distributions locales d'eau, de courant et de température sont présentées en fonction de la stratégie d'alimentation en gaz de la pile et de l'orientation du circuit de régulation thermique. Une partie consacrée au diagnostic de fonctionnement d'une pile illustre en quoi l'utilisation du modèle et la connaissance de l'état interne de la pile apporte des informations primordiales lors de l'utilisation d'une pile à combustible / The present work contributes to the understanding of water management and thermal management of a PEM fuel cell influences on the electrical performances. A bidimensional model representing mass and heat transfer in the cell thickness and along distribution channels is done. A specific part of the study concerns a microscopic representation of reactive agglomerates. This part presents the impact of the liquid water presence on local and global current densities. In te vein of integrating this model in a total fuel cell control system, simplifications have been done and coupled mass, heat and charge transfers are solved analytically. For any operating condition, the model gives a complete view of the hydric, thermal and electric inner situation of the cell. This diagnosis of the inner state of the cell leads to find the operating conditions giving to the optimal electric performances. Water, current and temperature distributions are presenting for different gas feeding strategies and different thermal management configurations. A specific part is dedicated to illustrate how this local diagnosis of the cell state can be used to estimate its global electric performances
1596

Etude expérimentale du comportement thermo-hydro-mécanique de l'argilite du Callovo-Oxfordien / Experimental study of thermo-hydro-mecanichal behaviour of Callovo-Oxfordian claystone

Mohajerani, Mehrdokht 29 March 2011 (has links)
Durant les différentes phases du stockage profond des déchets radio-actifs exothermiques (excavation, exploitation) jusqu'à la fermeture définitive, la roche hôte sera soumise à des sollicitations mécaniques, hydriques et thermiques couplées. Afin de connaître et de modéliser le comportement à court et long terme des dispositifs de stockage, une investigation approfondie du comportement de la roche est nécessaire afin de compléter les données existantes. C'est dans ce but que cette étude du comportement thermo-hydro-mécanique de la formation argileuse du Callovo-Oxfordien (COx) considérée par l'ANDRA comme roche hôte potentielle, a été développée. Dans un premier temps le comportement en compression–gonflement de l'argilite du COx a été étudié par la réalisation d'un programme d'essais oedométriques haute pression. Les résultats, interprétés en termes de couplage endommagement-gonflement, ont montré que l'ampleur du gonflement était lié à la densité de fissuration engendrée lors de la compression. Dans un second temps, le comportement hydromécanique et thermo-hydro-mécanique de l'argilite saturée sous une contrainte moyenne proche de l'in-situ a été étudié à l'aide de cellules à faible chemin de drainage (10 mm), dont une cellule isotrope et une cellule triaxiale à cylindre creux avec mesures locales d'un type nouveau. Ces appareils ont permis de résoudre deux problèmes difficiles typiques des argilites de très faible perméabilité : i) une saturation préalable correcte, attestée par de bonnes valeurs du coefficient de Skempton et ii) de bonnes conditions de drainage. Les paramètres caractéristiques du comportement de l'argilite à température ambiante (coefficients de Skempton et de Biot, compressibilité drainée et non-drainée) ont été déterminés à partir d'essais de compression isotrope qui ont également confirmé l'isotropie transverse du matériau. La cohérence des paramètres obtenus a été vérifiée dans un cadre poro-élastique saturé. Deux aspects du comportement thermo-hydro-mécanique de l'argilite du COx ont été étudiés à l'aide d'essais de chauffage et de compression volumique en température (80°C) : les effets de la température sur le comportement intrinsèque de l'argilite et le phénomène de pressurisation thermique. Un essai de chauffage drainé sous contrainte in-situ a mis en évidence, apparemment pour la première fois, un comportement plastique contractant de l'argilite (comme les argiles normalement consolidées), non pris en compte dans les modélisations thermo-élastiques actuelles des systèmes de stockage profond. Un autre élément nouveau et important observé est l'augmentation de la compressibilité avec la température, à la différence des argiles. L'étude de la pressurisation thermique (engendrée par la faible perméabilité de l'argilite et la forte différence entre les coefficients de dilatation thermique de l'eau et de la phase solide), a été réalisée à l'aide d'essais de chauffage non drainés, suite à une analyse détaillée des effets perturbateurs du système de mesure lors de variations de pression et de température (peut-être à considérer également dans les mesures in-situ). Le coefficient de pressurisation thermique s'est révélé être très sensible aux variations de température et de contrainte, il diminue de 0,14 à 0,1 MPa/°C entre 25 et 80°C. La nature des différentes réponses hydro-mécaniques et thermo-hydro-mécaniques obtenues au cours de ce travail permettront une interprétation et une modélisation plus précises du comportement du massif d'argilite autour des galeries, dans des zones qui sont pour la plupart saturées, sauf à proximité immédiate des galeries (quelques décimètres) / During the different phases of the exothermic radioactive waste deep disposal (excavation, operation) and after permanent closure, the host rock is submitted to various coupled mechanical, hydraulic and thermal phenomena. Hence, a thorough investigation of the thermo-hydro-mechanical behaviour of the rock is necessary to complete existing data and to better understand and model the short and long term behaviour of the Callovo-Oxfordian (COx) clay formation in Bure (Meuse/Haute-Marne - M/HM), considered by ANDRA as a potential host rock in France.In this work, the compression – swelling behaviour of the COx claystone was first investigated by carrying out a series of high-pressure oedometric tests. The results, interpreted in terms of coupling between damage and swelling, showed that the magnitude of swelling was linked to the density of the fissures created during compression. In a second step, the hydromechanical and thermo-hydro-mechanical behaviour of the saturated claystone under a mean stress close to the in situ one were investigated by using two devices with short drainage path (10 mm), namely a isotropic cell and a newly designed hollow cylinder triaxial cell with local displacement measurements. These devices helped to solve two majors problems related to testing very low permeability materials : i) a satisfactory previous sample saturation (indicated by good Skempton values) and ii) satisfactory drainage conditions. Some typical constitutive parameters (Skempton and Biot's coefficients, drained and undrained compressibility coefficients) have been determined at ambient temperature through isotropic compression tests that also confirmed the transverse isotropy of the claystone. The consistency of the obtained parameters has been checked in a saturated poroelastic framework. Two aspects of the thermo-hydro-mechanical behaviour of the COx claystone have then been investigated through different heating tests and through drained and undrained isotropic compression tests at elevated temperature (80°C) : the effects of temperature on the behaviour of claystone and thermal pressurization. A drained heating test under in-situ stress conditions evidenced, probably for first time, a plastic contractant response of the claystone (like normally consolidated clays), a feature not considered in the presently conducted numerical modelling of deep disposal systems. Another new important observed feature is the increase in drained compressibility of the COx claystone with temperature, not observed in clays. The investigation of thermal pressurization (caused by the low claystone permeability and by the significant difference in thermal expansion between water and the solid phase) has been carried out by means of undrained heating tests, after a detailed analysis of the major effects of the measurement system (which should perhaps be also analyzed when performing in-situ measurements). The thermal pressurization coefficient appeared to be quite sensitive to changes in temperature and stress, it decreased between 0.14 and 0.1 MPa/°C between 25 and 80°C. It is believed that the different thermo-hydro-mechanical volumetric responses obtained here allow a better interpretation and modelling of the behaviour of the claystone formation around the galleries in areas that are mostly saturated, except close to the galleries (a few decimetres)
1597

Modélisation DEM et approche expérimentale de la dynamique d'un système réactif en lit fluidisé dense : application à la gazéification de la biomasse

Cadile, Claudia 17 December 2014 (has links)
Le travail réalisé en collaboration entre l’entreprise CNIM et le laboratoire IUSTI a permis la miseen place d’un outil de simulation numérique afin d’étudier à l’échelle locale différents phénomènescouplés qui se produisent dans un réacteur de gazéification en lit fluidisé dense. L’approche choisie,DEM (Discrete Element Method), est basée sur le suivi de paquets de particules. Les résultats desimulation ont été comparés à des mesures expérimentales réalisées dans les laboratoires IUSTIet LERMAB : mesure de pression dans un lit fluidisé peu profond et caractérisation de la réactionde pyrolyse par suivis temporels de la masse volumique par une méthode innovante et de latempérature de la particule de biomasse ainsi que la composition des gaz produits. À plus grandeéchelle, les prédictions numériques du code ont été comparées à des mesures expérimentales deprofil de vitesse des particules et de mélange et ségrégation issues de la littérature. Les résultatsnumériques du lit fluidisé bisolide sans et avec réactions chimiques, obtenus sont en bon accordavec les mesures expérimentales. Ils ont permis de mettre en évidence le fort couplage entre lesphénomènes hydrodynamiques et thermochimiques.Ces travaux ouvrent de nouvelles perspectives tant sur le plan de l’expérimentation que de la simulation numérique où l’approche DEM retenue a montré un fort potentiel. L’extrapolation dumodèle DEM pour la simulation de la gazéification à des réacteurs industriels reste encore un défiau regard des ressources informatiques. / Energy production from green and renewable resources, such as biomass, are currently experiencinga significant growth. Thermochemical conversion of this biomass by gasification is a process usedfor over a century but still requires significant developments in terms of rentability optimizationand quality improvement of products gases.The work carried out in collaboration between the CNIM company and the IUSTI laboratoryallowed the establishment of a numerical simulation tool to study locally different coupled phenomenaoccurring in a dense fluidized bed gasification reactor. The chosen approach, DEM (DiscreteElement Method), is based on the monitoring of particle packets. The simulation results werecompared to experimental measurements realised in IUSTI and LERMAB laboratories : measuringpressure in a shallow fluidized bed and characterization of pyrolysis reaction with the timetracking of particle density by an innovative method, temperature and the composition of theproducts gases. On a larger scale, the numerical code predictions were compared with velocity,particles mixing and segregation profiles from experimental measurements of the literature. Theobtained numerical results of bi-solid fluidized bed with and without chemical reactions are ingood agreement with the experimental measurements. It helped to highlight the strong couplingbetween hydrodynamic and thermochemical phenomena.This work opens up new perspectives on the experimental plan and numerical simulation whichDEM approach has shown great potential. The extrapolation of the DEM model for the simulationof gasification industrial reactors remains a challenge in terms of computer resources.
1598

Applications of the coupled cluster method to pairing problems

Snape, Christopher January 2010 (has links)
The phenomenon of pairing in atomic and nuclear many-body systems gives rise to a great number of different physical properties of matter, from areas as seemingly diverse as the shape of stable nuclei to superconductivity in metals and superfluidity in neutron stars. With the experimental realisation of the long sought BCS-BEC crossover observed in trapped atomic gases - where it is possible to fine tune the s-wave scattering length a of a many-fermion system between a dilute, correlated BCS-like superfluid of Cooper pairs and a densely packed BEC of composite bosons - pairing problems in atomic physics have found renewed interest in recent years. Given the high precision techniques involved in producing these trapped gas condensates, we would like to employ a suitably accurate many-body method to study such systems, preferably one which goes beyond the simple mean-field picture.The Coupled Cluster Method (CCM) is a widely applied and highly successful ab initio method in the realm of quantum many-body physics and quantum chemistry, known to be capable of producing extremely accurate results for a wide variety of different many-body systems. It has not found many applications in pairing problems however, at least not in a general sense. Our aim, therefore, is to study various models of pairing using a variety of CCM techniques - we are interested in studying the generic features of pairing problems and in particular, we are especially interested in probing the collective modes of a system which exhibits the BCS-BEC crossover, in either the BCS or BEC limit. The CCM seems a rather good candidate for the job, given the high precision results it can produce.
1599

Séchage en continu du bois énergie comme moyen de préconditionnement en vue de sa conservation thermochimique : approches expérimentale et numérique / Continuous drying of wood energy as a way of preconditioning before its thermochemical conversion : experimental and numerical approaches

Colin, Julien 01 July 2011 (has links)
Les voies sèches de valorisation du bois énergie sont de plus en plus exigeantes vis-à-vis de la qualité de la matière première et notamment quant à sa teneur en eau. Ainsi, une étape intermédiaire de préconditionnement, sur site industriel, tend à se développer. La mise en œuvre de séchoirs en continu est alors séduisante de par son faible coût et sa parfaite intégration dans la ligne de production. Cependant, elle n'est pas sans écueil : la variabilité de la biomasse et l'hétérogénéité des conditions climatiques au sein du séchoir rendent fastidieux le dimensionnement du séchoir et de la source de chaleur associée d'une part et la maximisation du flux matière d'autre part.Notre étude a pour ambition de développer un outil informatique d'aide à la conception et à l'optimisation de séchoirs en continu traversés par un lit condensé de particules de bois. Pour y parvenir, nous associons une approche expérimentale et une approche numérique du procédé. La démarche scientifique s'articule autour de deux échelles représentatives :- A l'échelle de la particule de bois, le modèle de Van Meel, reposant sur le concept de courbe caractéristique de séchage, est étendu : le couplage entre transferts de chaleur et de masse est rendu explicite. Nous disposons dès lors d'un modèle réactif et prédictif en conditions climatiques variables. Parallèlement, un premier dispositif expérimental original est conçu et construit pour l'étude du séchage de particules de bois isolées. Les données recueillies sont alors analysées en vue d'alimenter en paramètres et de valider le modèle semi-analytique ;- A l'échelle du séchoir, une modélisation double-échelle est adoptée pour tenir compte de l'évolution des conditions climatiques. Un soin particulier est apporté à la modélisation, se voulant être la plus proche possible des installations existantes : à ce titre, les transferts au niveau de la paroi du séchoir sont pris en compte, ainsi que la variabilité des particules de bois. Parallèlement, un second dispositif expérimental original est conçu et construit pour l'étude du séchage de particules disposées en lit. Les données recueillies sont alors confrontées aux simulations du modèle double-échelle.La validation du modèle s'étant révélée probante tant à l'échelle de la particule qu'à celle du séchoir, une utilisation du code pour l'aide à la conception et à l'optimisation d'installations industrielles a pu être envisagée. Ainsi, ce travail s'achève-t-il par deux études de cas à travers lesquelles nous explorons le potentiel du modèle pour maximiser le flux matière tout en garantissant la qualité du produit et l'efficacité énergétique du séchoir. / The dry conversion routes of wood to energy require more and more improvement in the quality of raw material, particularly regarding to its moisture content. That is why a preliminary step of preconditioning tends to be developed on the industrial sites. The use of continuous dryers is then tempting because of their low cost and their perfect integration in the production line. However it is not without pitfall: the climatic conditions heterogeneity inside the dryer, on the one hand, and the biomass variability, on the other hand, make the utilization of these industrial plants tedious.Our study aims to develop a computing tool to help engineers optimizing and to designing continuous dryers passed through by a condensed bed of wood particles. For this result, an experimental approach of the process is associated to a numerical one. The scientific method revolves around two representative scales:• At the wood particle scale, the Van Meel model, based on the concept of characteristic drying curve, is enhanced: the coupling between heat and mass transfer is made explicit. So we obtain a reactive model which is predictive when the climatic conditions are variable. Meanwhile, a first original experimental device is designed and built in order to study the drying of single wood particles. Thanks to the collected data, the semi-analytical model is provided with parameters and is validated;• At the dryer scale, a dual-scale approach is chosen in order to take into account the evolution of the climatic conditions. A particular attention is paid to the modeling in order to make it as similar as possible to the existing installations: as such, the transfers at the wall surface and the variability of wood particles are included. Meanwhile, a second original experimental device is designed and built in order to study the drying of a wood particles stack. The data collected are then confronted with simulations of the double-scale model.The validation of the model has proven to be convincing at the particle scale and at the dryer one. Therefore a utilization of the code to help in the design and optimization of industrial plants can be considered. Thus, the work ends by two case studies through which we explore the potential of the model to maximize material flow while ensuring product quality and efficiency of the dryer.
1600

Desenvolvimento e validação de método analítico para determinação de multirresíduos de agrotóxicos em morango por LC-MS/MS e comparação com UHPLC / Development and validation of an analytical method for multiresidue determination of pesticides in strawberries by LC-MS/MS and comparison with UHPLC

Oshita, Daniele, 1981 12 December 2013 (has links)
Orientador: Isabel Cristina Sales Fontes Jardim / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Química / Made available in DSpace on 2018-08-24T08:24:02Z (GMT). No. of bitstreams: 1 Oshita_Daniele_D.pdf: 4645263 bytes, checksum: 6628dba7b8449d1cf1f86afa3dcae9e2 (MD5) Previous issue date: 2013 / Resumo: Este trabalho envolve o desenvolvimento, a otimização e a validação de um método analítico para determinação de multirresíduos de agrotóxicos em amostras de morango, por cromatografia líquida acoplada à espectrometria de massas sequencial (LC-MS/MS). No preparo de amostra utilizou o método QuEChERS (quick, easy, cheap, effective, rugged and safe), que foi testado nas três versões, Original, AOAC Official Method e European Committee for Standardization (CEN) Standard Method EN 15662, além da versão CEN 15662 modificada. Também foram otimizados os solventes de extração, massas do agente secante e, na etapa de clean-up por extração em fase sólida dispersiva (d-SPE), o sorvente comercial PSA (primary secondary amine), alguns preparados no laboratório à base de polímeros de siloxano, como octadecil, octil, amino, fenil, e a mistura PSA e octadecil. As avaliações dos métodos foram baseadas, principalmente, nos valores de recuperação e nos estudos sobre o uso de diferentes sorventes, outros parâmetros que estimam a eficiência do clean-up também foram utilizados, como aspecto físico do extrato final, quantidade de coextratos da matriz, obtida por medidas gravimétricas, e efeito matriz. O método desenvolvido foi validado por meio dos parâmetros analíticos de seletividade, limite de detecção (LOD), limite de quantificação (LOQ), linearidade, exatidão e precisão, conforme o guia Sanco para análises de resíduos de agrotóxicos em alimentos e, posteriormente, amostras comerciais de morango da região de Campinas foram analisadas. O método validado por LC-MS/MS apresentou-se seletivo, preciso, exato e atingiu concentrações abaixo dos respectivos limites máximos de resíduos (LMR) para determinação de agrotóxicos em morango. Este método foi transferido para cromatografia líquida de ultra eficiência (UHPLC), que mostrou redução no tempo de análise, na vazão da fase móvel (FM) e no volume de injeção de amostra e da FM, e similaridade na detectabilidade dos analitos / Abstract: This work involves the development, optimization and validation of an analytical method for multiresidue determination of pesticides in strawberry samples by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Sample preparation used the QuEChERS (quick, easy, cheap, effective, rugged and safe) method, which was tested in three versions, Original, AOAC Official Method and European Committee for Standardization (CEN) Standard Method EN 15662, and also CEN 15662 modified version. The factores optimized were extraction solvents, amount of drying agent and in the clean-up step by dispersive solid phase extraction (d-SPE), the commercial sorbent PSA (primary secondary amine), several prepared in the laboratory based on siloxane polymers, such as octadecyl, octyl, amine, phenyl, and the mixture PSA and octadecyl. The evaluation of the methods was based mainly on the recovery values and for the study of different sorbents, other parameters that estimate the efficiency of the clean-up were also used such as the physical aspect of the final extract, the amount of interference matrix obtained using gravimetric measurements, and the matrix effect. The developed method was validated by the analytical parameters of selectivity, limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy and precision, as described in the Sanco guide for analysis of pesticide residues in foods. After, commercial strawberry samples from the Campinas region were analyzed. The validated method by LC-MS/MS was selective, precise, accurate and reached levels below the respective maximum residue limits (MRLs) for the determination of pesticides in strawberries. This method was transferred to ultra high performance liquid chromatography (UHPLC), which showed a reduction in analysis time, the mobile phase (MP) flow rate and the injection volume of the sample and MP, and similarity in the detectability of the analytes / Doutorado / Quimica Analitica / Doutora em Ciências

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