Mémoire numérisé par la Division de la gestion de documents et des archives de l'Université de Montréal

Espectrometria de emissão óptica, utilizando plasmas acoplados indutivamente, torna-se uma ferramenta indispensável para análises de elementos químicos. Neste trabalho é descrita a construção detalhada de um oscilador de rádio frequência para obtenção de uma tocha de plasma indutivo. O projeto é estruturado a partir da elaboração da fonte retificadora, da malha de acoplamento, até a construção da tocha, além de análises com amostras líquidas e sólidas. Pelo fato de a tocha de plasma indutivo ser mais estável do que outros métodos de atomização, como laser ou chama, a torna uma escolha atraente para métodos analíticos, em vasta gama de aplicações. Os resultados do desempenho elétrico do oscilador de rádio frequência foram alcançados, embora as perdas sejam eminentes, foi obtida uma tensão na malha de acoplamento de 620 volts, potência na tocha de 1400 watts, e frequência do oscilador, com valor estável de 13,56 mega-hertz. Os resultados das análises também foi outro ponto de destaque, uma vez que, foi possível detectar através de um espectrômetro óptico, todos os elementos contidos numa solução de aço inox, tais como: silício, fósforo, manganês, molibdênio, cromo, níquel e cobre, embora os resultados quantitativos ainda necessitem de alguns ajustes. Com relação à análise de amostras sólidas, onde foram utilizados eletrodos consumíveis de alumínio e cobre, o resultado foi muito promissor, graças ao projeto da tocha que permite modificações em sua estrutura; os eletrodos consumíveis também foram analisados com as técnicas de difração de raio-X e microanálise por feixe de elétrons para confirmação dos resultados. / Optical emission spectrometry using inductively coupled plasma becomes an indispensable tool for analysis of chemical elements. This work describes the detailed construction of a radio frequency oscillator for obtaining an inductive plasma torch. The project is structured from the elaboration of the source rectifier, matching network, until the construction of the torch, and analyzes with liquid and solid samples. Because the inductive plasma torch to be more stable than other atomization methods such as laser or flame, becomes an attractive choice for analytical methods in wide range of applications. The results of the electrical performance of the radio frequency oscillator been achieved, although losses are distinguished was obtained at a voltage matching network 620 volts, the torch power of 1400 watts, and oscillator frequency, with a steady value of 13.56 mega-hertz. The results of analyzes was also another important point, since it was possible to detect through an optical spectrometer, all elements contained in a solution of stainless steel, such as silicon, phosphorus, manganese, molybdenum, chromium, nickel and copper, although the quantitative results still need some tweaking. Regarding the analysis of solid samples, which were consumable electrodes of aluminum and copper, the result was very promising, due to the torch project that allows modifications in its structure; consumable electrodes were also analyzed through the techniques x-ray diffraction and microanalysis by electron beam, to confirm the results.

A produção industrial do café solúvel brasileiro destina-se, na sua maior parte, ao mercado externo, constituindo-se em um importante ítem de exportação do país. O objetivo do presente trabalho foi o desenvolvimento e aprimoramento de métodos de análise química adequados à investigação de componentes inorgânicos em café solúvel. Inicialmente foi definido o método de mineralização das amostras através da avaliação de 6 procedimentos diferentes, classificados em 3 classes: (I) microondas focalizado; (II) via úmida convencional e (III) sistema sob pressão em frascos de decomposição com tampas (bombas de teflon). As determinações dos nutrientes e contaminantes inorgânicos: Na, K, Mg, Al, P, S, Ca, Mn, Fe, Ni, Cu, Zn, Cd, Sb, Pb, Cr, Sn, As, Se e Hg, após a utilização do procedimento de mineralização que emprega o sistema de microondas focalizado com os reagentes HNO3 e H2O2, foram realizadas por espectrometria de emissão atômica com plasma induzido, ICP-AES (da nomenclatura inglesa Inductively Coupled Plasma-Atomic Emission Spectrometry). Interferências de matriz e/ou espectrais foram detectadas nas determinações de Pb, Cr, Sn, As, Se e Hg. No caso do Sn, optou-se pela correção da radiação de fundo através do software do equipamento, pois outras linhas de emissão deste analito eram menos sensíveis e igualmente sujeitas a interferências espectrais. Para o Pb e Cr a escolha de comprimentos de ondas alternativos eliminou os problemas de interferências espectrais devido à matriz das amostras. A aplicação das técnicas de geração de hidretos para o As e Se e a geração de vapor frio para o Hg, possibilitaram as determinações destes analitos nas amostras de café solúvel, aumentando a sensibilidade das análises. Os resultados obtidos para os teores dos nutrientes e contaminantes inorgânicos em 21 amostras de café solúvel disponíveis no mercado brasileiro, foram aceitáveis para o consumo humano, tanto no aspecto nutricional como toxicológico, com exceção de uma amostra com teor de Cr igual a 0,52 ± 0,02 mgKg-1, acima do permitido pela legislação brasileira que fixa o valor máximo de 0,10 mgKg-1. A aplicação de técnicas estatísticas, análise de clusters hierárquicos e componentes principais aos resultados obtidos, possibilitaram investigar a variabilidade das composições minerais e classificar grupos de amostras similares. O emprego da técnica instrumental ICP-AES através do sistema de nebulização convencional e a utilização do sistema de geração de hidretos e vapor frio, mostraram-se adequados para as determinações dos nutrientes e contaminantes inorgânicos em café solúvel, uma vez que níveis de precisão e exatidão aceitáveis foram obtidos. / The production of Brazilian soluble coffee is almost entirely destined for exporting. Therefore, the objective of this work was the development and the establishment of appropriate methods of chemical analysis of inorganic components in soluble coffee. Firstly, the appropriate digestion procedure for soluble coffee samples was defined through the evaluation of six different digestion techniques that were classified into three groups: (I) focused microwave system, (II) conventional wet digestion and (III) pressure digestion system in teflon bombs. The determinations of nutrients and toxic elements: Na, K, Mg, Al, P, S, Ca, Mn, Fe, Ni, Cu, Zn, Cd, Sb, Pb, Cr, Sn, As, Se, and Hg after the utilization of the focused microwave system with HNO3 and H2O2 reagents, were made by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) technique. Matrix and spectral interferences were detected in the determination of Pb, Cr, Sn, As, Se and Hg. Correction of the background enhancement by the equipment software was made in the determination of Sn, as other analytical lines were unsuitable for this application. For Pb and Cr, the choice of other analytical lines eliminated the problem of matrix and spectral interferences. The application of the hydride generation technique for As and Se and cold atomic vapour with ICP-AES for Hg, were suitable methods to determine these analytes in soluble coffee samples with increased sensitivity of the analysis. The results obtained of nutrients and toxic elements in twenty-one samples of soluble coffee collected from Brazilian market were acceptable to human consumption at nutritional and toxic level with exception of a sample with 0,52 ± 0,02 mgKg-1 of Cr, above the value specified in Brazilian Food Legislation, that fixes the maximum Cr contend in 0,10 mgKg-1. The aplication of statistical techniques analysis of principal components and the hierarchical cluster on the results of mineral compositions, enabled to investigate the variability in the composition and to classify groups of similar samples. The application of the ICP-AES technique using the conventional pneumatic nebulization system, the hydride generation technique and the cold vapour for Hg were suitable to determine the nutrients and toxic elements in soluble coffee, as they provided acceptable results indicating accuracy and precision.

Submitted by Renata Lopes (renatasil82@gmail.com) on 2016-01-22T11:04:31Z No. of bitstreams: 1 wesleytinocoesteves.pdf: 1817304 bytes, checksum: 6ff6e2f42ca29b6d9a247cd5c28895ef (MD5) / Approved for entry into archive by Adriana Oliveira (adriana.oliveira@ufjf.edu.br) on 2016-01-25T18:50:19Z (GMT) No. of bitstreams: 1 wesleytinocoesteves.pdf: 1817304 bytes, checksum: 6ff6e2f42ca29b6d9a247cd5c28895ef (MD5) / Made available in DSpace on 2016-01-25T18:50:19Z (GMT). No. of bitstreams: 1 wesleytinocoesteves.pdf: 1817304 bytes, checksum: 6ff6e2f42ca29b6d9a247cd5c28895ef (MD5) Previous issue date: 2014-12-02 / CAPES - Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / O presente trabalho buscou estabelecer um método para a determinação de contaminantes inorgânicos em leite cru que fosse compatível com aplicações em larga escala, como os programas regulatórios de monitoramento de contaminantes em leite. Para tal, foi proposta uma abordagem utilizando a técnica de espectrometria de emissão atômica em plasma (ICP-AES) sem mineralização das amostras, que foram solubilizadas em solução contendo etanolamina e ácido cítrico. Estudos foram conduzidos a fim de estabelecer condições instrumentais em que fosse possível utilizar o preparo amostral proposto mantendo o compromisso com a sensibilidade, exatidão e desempenho analítico necessários a fim de se atingir os limites de detecção requeridos por legislações relacionadas à segurança alimentar. A proporção ideal de diluição da amostra na solução de etanolamina e ácido cítrico foi de 1:2 (amostra:solução) e os valores mais adequados dos parâmetros instrumentais foram 1300W para a radiofrequência do plasma, 0,50L.min-1 para a vazão do gás auxiliar e 0,60L.min-1 para a vazão do gás de nebulização. Os limites de quantificação obtidos para Cd, Co, Cr, Cu e Pb foram, respectivamente, 6,54, 6,57, 14,8, 14,3 e 27,4 μg.mL-1. / This study aimed to establish a method for the determination of inorganic contaminants in raw milk that was compatible with largescale applications, such as regulatory programs for the monitoring of contaminants in milk. For this purpose, an approach using the technique of atomic emission spectrometry (ICP-AES) with no mineralization of the samples, which was solubilized in a solution containing ethanolamine and citric acid, has been proposed. Studies were conducted in order to establish experimental conditions in which it was possible to use the proposed sample preparation and keeping the commitment to sensitivity, accuracy and the analytical performance required by legislations related to food safety. The ideal ratio of sample dilution was 1:2 (sample:solution) and the most suitable values for instrumental parameters were 1300W for the plasma radiofrequency power, 0.50L.min-1 for the flow of auxiliary gas and 0.60L.min-1 for the flow of nebulizer gas. The quantification limits obtained for Cd, Co, Cr, Cu and Pb were, respectively, 6.54, 6.57, 14.8, 14.3 and 27.4 μg.mL-1.

CICYT (PB88-0288 y PTRI91-0029)

No description available.

Les mécanismes d'oxydation, de décapage et sur-décapage d'un acier bas carbone est d'un acier fortement allié au silicium (1,6 et 3.2 % en masse de silicium) ont été étudiés. Le suivi de l'oxydation par thermogravimétrie et la caractérisation de la calamine des aciers fortement alliés au silicium a montré un effet très marquant de passivation de la couche de silice. Les calamines des échantillons modèles sont composées de couches d'hématite, magnétite et wüstite partiellement décomposée en fer et magnétite pour l'acier bas carbone. Pour l'acier au silicium, la fayalite est présente à l'interface acier/wüstite sous forme de grains ou d'une couche interne. Le suivi du potentiel de circuit ouvert pendant le décapage et sur-décapage de ces échantillons a montré un potentiel de corrosion stable et anodique pour les oxydes de fer et une chute drastique de ce potentiel au contact de l'acide avec le métal. Le suivi du taux de dissolution totale par ICP-AES combiné avec des mesures de courant de corrosion par la méthode de Tafel a montré une contribution importante de la dissolution électrochimique par oxydation de la wüstite et la magnétite et réduction de Fe3+ issu de la dissolution chimique de l'hématite et la magnétite. La fayalite est libérée dans la solution par dissolution de la wüstite ou du métal adjacents. Après le contact acide/metal, toutes les dissolutions sont exclusivement électrochimiques par corrosion du métal et réduction de la magnétite (cas des calamines industrielles). La spectroscopie d'impédance électrochimique a été utilisée pour la première fois pour ce type d'étude. L'estimation des valeurs de capacité a montré un comportement pseudo passif pour la couche d’hématite et d’électrode poreuse pour la wüstite. / Oxidation, pickling and over-pickling mechanisms of a low carbon steel and a high alloyed steel (1.6 and 3.2 wt.% Si) were investigated. The monitoring of oxidation with thermogravimetry and characterization of scale showed a very important passivating effect of the silica layer. Model scales are composed of layers of hematite, magnetite and partially decomposed wüstite into iron and magnetite for the low carbon steel. For the silicon steel, fayalite is present in the steel/wüstite interface as grains or an internal layer. Open circuit potential measurements during pickling and over-pickling of these samples showed a stable and anodic corrosion potential for iron oxides and a significant potential jump once the acid reaches the metal. The monitoring of the total dissolution rate with ICP-AES coupled with corrosion current measurements with the Tafel method showed an important contribution of electrochemical dissolution by oxidation of wüstite and magnetite and reduction of Fe+3 from chemical dissolution of hematite. Fayalite is liberated in the solution by dissolution of the surrounding wüstite or metal. After the contact acid/metal, all dissolutions are exclusively electrochemical by corrosion of the metal and reduction of magnetite (case for industrial scales). Electrochemical impedance spectroscopy was used for the first time for this kind of studies. The estimation of the capacitance values showed a passive like behaviour for hematite and a porous electrode one for wüstite.

Käppalaverket är ett avloppsreningsverk som är beläget på Lidingö. Avloppsreningsverket renar idag avloppsvatten från över en halv miljon människor. Varje år produceras det omkring 30 000 ton slam på Käppalaverket. Det näringsrika slammet används sedan som gödsel som sprids på åkermarken. Från 2007 fram till 2012 har kopparhalten stigit i det producerade slammet på Käppalaverket. Det har resulterat i att mängden koppar har överstigit det uppsatta gränsvärdet för att få sprida slam på åkermark (300 g koppar/ha och år). Därmed får endast en begränsad mängd av det producerade slammet spridas på åkermarken. Gränsvärdet är satt för att skyddamark- och vattenlevande organismer. Den tvåvärda kopparjonen har nämligen en toxisk effekt på organismerna. Även Bromma och Henriksdals avloppsreningsverk har haft en liknande ökning i kopparhalt hos slammet, men inte lika kraftig som Käppalaverket. Den största delen av den koppar som hamnar i slammet förutspås komma från kopparrör i hushållen. Därför har flera olika parametrar undersökts för att se hur mycket påverkan de har på korrosionen av kopparrören. pH, alkalinitet och naturligt organiskt material (NOM) är de parametrar som mest påverkar mängden koppar som löses ut genom korrosion i dricksvattnet. En sänkning av pH leder till högre halt koppar i dricksvattnet, men en sänkning av alkalinitet och NOM-halt bidrar istället till en lägre halt koppar i dricksvattnet. Även temperatur och stilleståndstid har betydelse för hur snabbt korrosionen av koppar sker. Majoriteten av Käppalas medlemskommuner får sitt dricksvatten från Görvälnverket. Lovö och Norsborgs vattenverklevererar dricksvatten till övriga kommuner inom Käppalas upptagningsområde. Hos Görvälnverket har alkaliniteten stigit svagt från år 2000 fram till idag. Denna stigning borde endast påverka i ytterst liten grad på den höga kopparhalten i Käppalaverkets slam. På övriga parametrar som anses ha påverkan på kopparhalten i slammet har det inte setts någon tydlig tendens. Ökningen av kopparhalter i slammet tyder istället på andra orsaker. I februari 2009 bytte Käppalaverket tillsammans med Bromma och Henriksdals reningsverk analyslaboratorium. Bytet av laboratorium tyckts påverka analysresultaten så att analysresultaten från det nya laboratoriet uppvisar en högre halt koppar i slammet. Dessutom har standardavvikelsen varit större för de analysresult som erhållits efter laboratoriebytet jämfört med analysresultaten före laboratoriebytet. Analysosäkerheten har emellertid varierat mellan åren då kopparhalten islammet steg. På Stockholm Vattens laboratorium dit proverna skickades innan laboratoriebytet var analysosäkerheten väldigt ospecifikt angivet. Enligt analysrapporten hade provresultatet en analysosäkerhet mellan 15-40 %. Proverna skickades efter laboratoriebytet till Eurofinslaboratorium i Lidköping. Där har analysosäkerheten på slamproverna minskat med tiden. Första tiden efter bytet var analysosäkerheten på proverna 30 % därefter har osäkerheten minskat till 15 %. Anledningen till att Käppalaverket haft en kraftigare stigning än Bromma och Henriksdalsreningsverk är oviss. En förklaring skulle kunna vara att slamkonditioneringsprocessen Kemicond påverkade analysresultatet eftersom en viss koncentrationsförändring skulle skett då processen var i drift. Men kopparhalten har inte sjunkit så kraftigt som förväntat efter att Kemicond avvecklades. Emellertid har den totala mängden koppar in till Käppalaverket ökat under tidsperioden då kopparhalten i slammet varit högre. Det tyder på att det är någon annan bakomliggande orsak till ökningen av koppar i slammet. / Käppala wastewater treatment plant (WWTP) is located in Lidingö and currently treats water from over half a million people. Every year the Käppala plant produces about 30 000 t sludge. The nutritious sludge is then used as fertilizer on farmland. From 2007 until 2012 the copper content has increased in the produced sludge. Eventually the amount of copper has exceeded the allowed limit for spreading sludge on farmland (300 g copper/ha and year). So only a limited amount of sludge can be spread on the farmland. The limit is set to protect the soil and aquatic organisms since the divalent copper ion has toxic effects on the organisms. Even Bromma and Henriksdal WWTP have had the same increase in copper content in the sludge, but not as highas the Käppala plant. The largest part of the copper that ends up in the sludge is predicted to originates from copper pipes in households. That is the reason why a number of different parameters has been investigated in order to see how much each parameter affects the amount of copper that is dissolved in the drinking water. The parameters that affect the most are; pH, alkalinity andnatural organic matter (NOM). When pH is decreasing, more copper will dissolve to the drinking water, but when the alkalinity and the NOM content is increasing, more copper will dissolve to the drinking water. Even the temperature and the stagnation time is important for how fast corrosion of copper pipes will occurs. The Görväln plant purifies and supplies drinking water to the majority of the member municipalities of the Käppala plant. Lovö’s and Norsborg’swaterworks supply drinking water to the other municipalities within the catchment area of Käppala. The alkalinity has slightly increased in the Görväln plant from 2000 to present. This increase should only affect in a very small degree on the increase in copper content in the sludge of Käppala plant. There is no clear trend on the other parameters that is considered to have an influence on the copper content in the sludge. The sharp increase in copper content has probably other causes. In February 2009, the Käppala plant, together with Bromma and Henriksdal WWTP, changed analysis laboratory. The change of laboratory seemed to affect the results of the analysis giving higher values of copper contentin the sludge. The standard deviation is also greater in the analysis results of the samples after the change of laboratory compared to with the analysis results before the change of laboratory. However, the uncertainty of the analysis has varied over the years when the rising in the copper content in the sludge occurred. At Stockholm Vatten’s laboratory where samples were sent before the laboratory change was the uncertainty of the analysis very unspecific given. According to the analysis report, the result of the sample had an uncertainty of the analysis between 15-40 %. The samples were after the laboratory change sent to Eurofins laboratory in Lidköping. Here the uncertainty of the analysis has been diminished with the time. After the first years after the change the uncertainty of the analysis was 30 %. But after that the uncertainty of the analysis has declined to 15 %. The reason why the Käppala plant had a stronger increase of copper content in the sludge than in Bromma and Henriksdal WWTP is unknown. One explanation could be that the sludge conditioning process Kemicond affected the analysis result since a certain change in concentration could have occurred when the process was in operation. However, the copper content has not decreased as much as expected after Kemicond was liquidated. But the total amount of copper in to the Käppala plant has increased during the period when the copper content in the sludge was higher. This indicates that there are other underlying reasons for the increase of copper in the sludge.

Nous avons caractérisé différents cristaux piézoélectriques de Langatate La3Ga5.5Ta0.5O14 (LGT), de différentes couleurs afin d’évaluer l’influence des défauts sur la qualité de dispositifs du domaine Temps-Fréquence (résonateurs acoustiques).Nous avons étudié la composition de ces cristaux dont les variations autour de la composition stoechiométrique sont surtout dues à l’évaporation du Ga2O au cours de la croissance compensée par un excès de Ga2O3 dans le mélange initial. Pour déterminer cette composition, la technique ICP-AES, précédée par une mise en solution par fusion alcaline, est la plus fiable.La présence d’impuretés chimiques, telles que les éléments métalliques ou les terres rares, liée à la pureté des oxydes de base, au frittage de la charge dans un creuset alumine… est étudiée. Nous expliquons ainsi la nature des centres colorés qui évolue selon l’atmosphère de tirage ou lors d’un recuit particulier.C’est ainsi que nous avons déterminé certaines propriétés de LGT permettant l’obtention de dispositifs comme les résonateurs à ondes de volume dont le produit Q.f est supérieur à celui des résonateurs à quartz. Pour cela, nous montrons notamment qu’il est nécessaire que :- la composition du cristal soit la plus proche possible de la stoechiométrie,- la résistivité électrique soit la plus grande possible,- l’étude spectroscopique ne révèle aucune absorption dans le domaine du visible.Dans ces conditions, le facteur de qualité Q d’une résonance à 10 MHz peut être de 1.44 million au point d’inversion de la courbe fréquence-température (1.35 pour le quartz) mais qu’il diminue notablement pour atteindre 0.35 million si nous pratiquons un recuit sous air à 1000°C pendant 48 h. / We have characterized Langatate piezoelectric crystals La3Ga5.5Ta0.5O14 (LGT), differently colored in order to evaluate the defects influence on the quality of Bulk Acoustic Waves resonators for the Time and Frequency domain.We have analyzed the composition of crystals whose variations around stoichiometric composition are mainly due to the evaporation of the Ga2O during growth compensated by adding an excess of Ga2O3 in the initial mixture. Among different techniques, the ICP-AES spectrometry, preceded by a dissolution by alkaline fusion seems to be the most accurate technique to determine the composition.The inevitable presence of chemical impurities, such as metallic elements, rare earth… linked to the purities of the raw materials, to the sintering of the load in an alumina crucible… is also studied. We try to explain in particular the nature of the color centers that evolve according to the growth atmosphere or during a particular annealing.So, we conclude by a list of necessary properties to obtain BAW resonators exhibiting a Q.f product higher than quartz. For this, we establish that it is necessary that:- the crystal composition is as close as possible to the stoichiometric composition,- the electrical resistivity is the highest possible,- the spectroscopic study does not reveal any absorption band in the visible domain.In these conditions, we were able to highlight that the quality factor of a 10 MHz resonance is of 1.44 million at the inversion temperature of the frequency-temperature curve (1.35 for the quartz crystal in the same conditions), but that this one decreases significantly to reach 0.35 million if we perform an annealing under air at 1000 °C during 48 hours.

L'utilisation de lasers est largement répandue dans le domaine de la microanalyse directe des solides. La matière vaporisée, en focalisant un faisceau laser de forte puissance sur la cible, peut être analysée soit par spectrométrie d'émission optique sur plasma induit (LIBS, acronyme anglais pour Laser Induced Breakdown Spectroscopy), soit par une source à plasma induit par haute fréquence couplée à la spectrométrie d'émission optique (ICP-AES) ou à la spectrométrie de masse (ICP-MS). Avec une résolution spatiale à l'échelle microscopique, les techniques d'ablation laser permettent ainsi d'accéder à la composition élémentaire locale de la surface d'un matériau. Néanmoins, les performances analytiques de ces techniques pourraient être améliorées par l'utilisation combinée des informations LIBS et ICP afin également de comprendre et maîtriser davantage l'interaction laser/matière. Dans ce but, ce travail a consisté à développer une technique de microanalyse par ablation laser couplée avec une détection en simultané par ICP et par LIBS afin d'étudier les potentialités analytiques de cet instrument pour cartographier la surface des matériaux. Les performances et les limitations de ce système ont été évaluées d'une part, en caractérisant les aérosols produits par ablation laser et d'autre part, en étudiant les signaux LIBS et ICP obtenus à partir d'un même prélèvement de matière. Le phénomène de fractionnement élémentaire rencontré sur des matrices critiques telles que le laiton a été mis en évidence en microablation malgré des caractéristiques de l'interaction laser/matière différente de la macroablation. Une méthode de correction, a posteriori, par l'efficacité d'extraction de la cellule d'ablation a été proposée afin de pallier ces effets limitatifs pour l'analyse quantitative. Une cellule d'ablation, optimisée à partir d'une étude de simulation numérique, a été développée afin de s'adapter aux applications de cartographies de surface. Les performances analytiques du système ont été évaluées en termes de stabilité (8-10%), de résolution spatiale (5 µm) et de limites de détection (de l'ordre de la ppm dans le solide avec un détecteur de masse). La complémentarité des mesures LIBS et ICP représente à la fois un outil de diagnostic de l'interaction laser/matière et un instrument d’analyse très complet grâce à la double détection qui permet de suivre simultanément des traces et des majeurs sur une large gamme d'éléments de la classification périodique / Laser ablation is widely spread for solid sample microanalysis. A tightly focused laser beam allows direct sampling of matter, the ablated mass can then be analysed either with LIBS (Laser Induced Breakdown Spectroscopy) or with an inductively coupled plasma source combined with an optical emission spectrometer (ICP-AES) or a mass spectrometer (ICP-MS). With spatial resolution down to the micron scale, laser ablation techniques permit local elemental analysis of sample surface. Nevertheless, analytical performances of such techniques could be improved by combining LIBS and ICP information to understand and control laser/matter interaction. For this purpose, this work aimed to develop a microanalytical technique based on laser ablation coupled to simultaneous detection with LIBS and ICP to study analytical potentialities of such technique for elemental mapping of material surface. Performances and limitations of the system were studied on one hand, by characterizing laser-induced aerosols and on the other hand, by studying simultaneous LIBS and ICP signals. Elemental fractionation on critical matrices such as brass was evidenced in microablation despite a different laser/matter interaction compared with macroablation. A correction procedure a posteriori using the total extraction efficiency of the ablation cell was proposed to overcome this problem for quantitative analysis. An ablation cell, optimized from a numerical simulation study, was developed for mapping applications. Analytical performances were evaluated in terms of stability (8-10 %), spatial resolution (5 µm) and detection limits (in the ppm range with ICP-MS). The LIBS and ICP complementarity makes the double detection system a diagnostic tool for laser/matter interaction and an analytical instrument allowing simultaneous monitoring of traces and majors from a large element range of the periodic classification