This Master thesis is a part of a project: Hydride atomizers for atomic absorption and atomic fluorescence spectrometry - new horizons (GA ČR, P206/17-04329S, principal investigator: prof. RNDr. Jiří Dědina, CSc. DSc.) of which the general target is to make a leap towards the ideal hydride atomizer by optimization of atomization based on the knowledge of the distribution of free atoms and hydrogen radicals inside the atomizers. This thesis contributes to the project by optimizing the atomization parameters for atomic absorption spectrometry with hydride generation. The atomization parameters were optimized for three different types of atomizers - multiatomizer, diffusion flame and "flame-in-gas-shield" atomizer using three different analytes - bismuth, lead and tin. Optimal atomization parameters were found for each of the atomizer and each of the analyte - carrier gas flow and flow of other gases if needed for the analysis. Calibration curves and analytical figures of merit such as sensitivity, LOD and LOQ were estimated. Final comparison is based on the data obtained from calibration curves. MDF and FIGS atomizers are mostly used with AFS detection and they provide lower sensitivity and higher detection limits with AAS detection in comparison with MMQTA. Since the analytes are known to trap...

Generation and atomization of cadmium volatile compounds was optimized in this work in order to determine trace Cd concentration levels by volatile compound generation (VCG) with subsequent detection by atomic absorption spectrometry (AAS). Three designs of volatile compound generators have been tested including a conventional hydride generator in flow injection analysis (FIA) mode, a batch generator as well as a generator of volatile compounds of transition metals. The generation efficiency of Cd species was quantified as low as 4 % in the conventional hydride generator. Providing that dissolved oxygen was removed from the reaction solutions, the generation efficiency of Cd increased to 12 % in the same experimental arrangement. The highest Cd generation efficiency of 54 % was reached in the generator of volatile compounds of transition metals. In this set up a detection limit of 0.07 ng ml-1 Cd and a sensitivity of 3.2 s ng-1 Cd, respectively, were reached. Moreover, the structure of the volatile Cd species generated was identified as free atoms in all experimental arrangements of the generators investigated. Keywords atomic absorption spectrometry, cadmium, generation of volatile compounds, atomization of volatile compounds

This thesis work is focused on the influence of process parameters during gas atomization on the thermal spraying properties of a Ni-Cr-B-Si hardfacing alloy. The metal powder alloy, known as 1-60-20, is produced by Höganäs AB. There have been problems with insufficient fusing during flame spraying of this particular alloy sometimes, even though the chemical composition is always within spec. This has lead to a theory that the difference in performance is caused by differences in parameters during gas atomization. Several gas-gas and gas-water atomizations with varying parameters were performed at the Höganäs Pilot Centre. The powder samples were then analyzed by sieving, scanning electron microscopy, x-ray diffraction and finally tested by powder welding. The results show that by increasing the cooling rate during gas atomization the formation of unstable Ni-borides is possible for this alloy. If these Ni-borides will enhance the fusing properties of the alloy is unknown. According to the literature studied, it should however improve the fusing properties.

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El proceso de atomización desde una vena o lámina líquida hasta multitud de gotas dispersas en un medio gaseoso ha sido un fenómeno de interés desde hace varias décadas, especialmente en el campo de los motores de combustión interna alternativos. Multitud de estudios experimentales han sido publicados al respecto, pues una buena mezcla de aire-combustible asegura una evaporación y combustión mucho más eficientes, aumentando la potencia del motor y reduciendo la cantidad de contaminantes emitidos. Con el auge de las técnicas computacionales, muchos modelos han sido desarrollados para estudiar este proceso de atomización y mezcla. Uno de los últimos modelos que han aparecido es el llamado ELSA (Eulerian-Lagrangian Spray Atomization), que utiliza un modelo Euleriano para la parte densa del chorro y cambia a un modelo Lagrangiano cuando la concentración de líquido es suficientemente pequeña, aprovechando de esta manera las ventajas de ambos. En el presente trabajo se ha desarrollado un modelo puramente Euleriano para estudiar la influencia de la geometría interna de la tobera de inyección en el proceso de atomización y mezcla. Se ha estudiado únicamente el proceso de inyección diésel. Este modelo permite resolver en un único dominio el flujo interno y el externo, evitando así las comunes simplificaciones y limitaciones de la interpolación entre ambos dominios resueltos por separado. Los resultados actuales son prometedores, el modelo predice con un error aceptable la penetración del chorro, el flujo másico y de cantidad de movimiento, los perfiles de velocidad y concentración, así como otros parámetros característicos del chorro. / Martí Gómez-Aldaraví, P. (2014). DEVELOPMENT OF A COMPUTATIONAL MODEL FOR A SIMULTANEOUS SIMULATION OF INTERNAL FLOW AND SPRAY BREAK-UP OF THE DIESEL INJECTION PROCESS [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/43719 / Premios Extraordinarios de tesis doctorales

[ES] La comprensión de los fenómenos físicos que acontecen en la región densa (también conocida como campo cercano) durante la atomización de los sprays ha sido una de las mayores incógnitas a la hora de estudiar sus aplicaciones. En el sector industrial, el rango de interés abarca desde toberas en aplicaciones propulsivas a sprays en aplicaciones médicas, agrícolas o culinarias. Esta evidente falta de conocimiento obliga a realizar simplificaciones en la modelización, provocando resultados poco precisos y la necesidad de grandes caracterizaciones experimentales en la fase de diseño. De esta manera, los procesos de rotura del spray y atomización primaria se consideran problemas físicos fundamentales, cuya complejidad viene dada como resultado de un flujo multifásico en un régimen altamente turbulento, originando escenarios caóticos. El análisis de este problema es extremadamente complejo debido a la ausencia sustancial de teorías validadas referentes a los fenómenos físicos involucrados como son la turbulencia y la atomización. Además, la combinación de la naturaleza multifásica del flujo y su comportamiento turbulento resultan en una gran dificultad para afrontar el problema. Durante los últimos 10 años, las técnicas experimentales han sido finalmente capaces de visualizar la región densa, pero la confianza, análisis y efectividad de dichos experimentos en esta región del spray todavía requiere de mejoras sustanciales. En este contexto, esta tesis trata de contribuir al entendimiento de estos procesos físicos y de proporcionar herramientas de análisis para estos flujos tan complejos. Para ello, mediante Direct Numerical Simulations se ha afrontado el problema resolviendo las escalas de movimiento más pequeñas, y capturando todas las escalas de turbulencia y eventos de rotura. Uno de los objetivos de la tesis ha sido evaluar la influencia de las condiciones de contorno del flujo entrante en la atomización primaria y en el comportamiento turbulento del spray. Para ello, se han empleado dos condiciones de contorno diferentes. En primer lugar se ha empleado una condición de contorno sintética para producir turbulencia homogenea a la entrada, simulando el comporamiento de la tobera. Una de las características más interesantes de este método es la posibilidad de retocar los parámetros dentro del algoritmo. En particular, la escala de longitud integral se ha variado para evaluar la influencia de las estructuras mas grandes de la tobera en la atomización primaria. El análisis de la condición de contorno sintética también ha permitido el diseño óptimo de simulaciones de las cuales se han derivado estadísticas turbulentas significativas. En este escenario, se han llevado a cabo estudios más profundos sobre la influencia de propiedades de las estructuras turbulentas como la homogeneidad y la anisotropía tanto en el espectro de los flujos como en las estadísticas de las gotas. Para tal fin, se han desarrollado metodologías novedosas para computar el análisis espectral y la estadística de las gotas Entre los resultados de este análisis destaca la independencia de la condición de contorno de entrada en las estadísticas de las gotas, mientras que por otra parte, recalca que las características turbulentas desarrolladas en el interior de la tobera afectan a la cantidad total de masa atomizada. Estas consideraciones se encuentran respaldadas por el análisis espectral realizado, mediante el cuál se concluye que la turbulencia multifásica comparte el comportamiento universal descrito por las teorías de Kolmogorov. / [CA] La comprensió dels fenòmens físics que succeïxen en la regió densa (també coneguda com a camp pròxim) durant l'atomització dels sprays ha sigut una de les majors incògnites a l'hora d'estudiar les seues aplicacions. En el sector industrial, el rang d'interés comprén des de toveres en aplicacions propulsives a sprays en aplicacions mèdiques, agrícoles o culinàries. Esta evident falta de coneixement obliga a realitzar simplificacions en la modelització, provocant resultats poc precisos i la necessitat de grans caracteritzacions experimentals en la fase de disseny. D'esta manera, els processos de ruptura del spray i atomització primària es consideren problemes físics fonamentals, la complexitat dels quals ve donada com resultat d'un flux multifàsic en un règim altament turbulent, originant escenaris caòtics. L'anàlisi d'este problema és extremadament complex a causa de l'absència substancial de teories validades dels fenòmens físics involucrats com són la turbulència i l'atomització. A més, la combinació de la naturalesa multifàsica del flux i el seu comportament turbulent resulten en una gran dificultat per a afrontar el problema. Durant els últims 10 anys les tècniques experimentals han sigut finalment capaces de visualitzar la regió densa, però la confiança, anàlisi i efectivitat dels experiments en esta regió del spray encara requerix de millores substancials. En este context, esta tesi tracta de contribuir en l'enteniment d'estos processos físics i de proporcionar ferramentes d'anàlisi per a estos fluxos tan complexos. Per a això, per mitjà de Direct Numerical Simulations s'ha afrontat el problema resolent les escales de moviment més menudes, al mateix temps que es capturen totes les escales de turbulència i esdeveniments de ruptura. Un dels objectius de la tesi ha sigut avaluar la influència que les condicions de contorn del flux entrant tenen en l'atomització primària i en el comportament turbulent del spray. Per a això, s'han empleat dos condicions de contorn diferents. En primer lloc s'ha empleat una condició de contorn sintètica per a produir turbulència homogènia a l'entrada, simulant el comportament de la tovera. Una de les característiques més interessants d'este mètod és la possibilitat de retocar els paràmetres dins de l'algoritme. En particular, l'escala de longitud integral s'ha variat per a avaluar la influència de les estructures mes grans de la tovera en l'atomització primària. L'anàlisi de la condició de contorn sintètica també ha permés el disseny òptim de simulacions de les quals s'han derivat estadístiques turbulentes significatives. En este escenari, s'han dut a terme estudis més profunds sobre la influència de propietats de les estructures turbulentes com l'homogeneïtat i l'anisotropia tant en l'espectre dels fluxos com en les estadístiques de les gotes. Per a tal fi, s'han desenrotllat metodologies noves per a computar l'anàlisi espectral i l'estadística de les gotes. Entre els resultats d'esta anàlisi destaca la independència de la condició de contorn d'entrada en les estadístiques de les gotes, mentres que d'altra banda, es recalca que les característiques turbulentes desenrotllades en l'interior de la tovera afecten a la quantitat total de massa atomitzada. Estes consideracions es troben recolzades per l'anàlisi espectral realitzat, per mitjà del qual es conclou que la turbulència multifásica compartix el comportament universal descrit per les teories de Kolmogorov. / [EN] The understanding of the physical phenomena occurring in the dense region (also known as near field) of atomizing sprays has been long seen as one of the biggest unknown when studying sprays applications. The industrial range of interest goes from nozzles in combustion and propulsion applications to medical sprays, agricultural and food process applications. This substantial lack of knowledge is responsible for some important simplification in modeling, that often result to be inaccurate or simply partial, leading to the evident need of large experimental characterization during the design phase. In fact, the spray breakup and primary atomization processes are indeed fundamental problems of physics, which complexity results from the combination of a multiphase flow in a highly turbulent regime that leads to chaotic scenarios. The analysis of this problem is extremely problematic, due to a substantial lack of definitive theories about the physical phenomena involved, namely turbulence and atomization. Furthermore, the combination of the multiphase nature of the flow and its turbulent behavior makes substantially difficult to address the problem. Only within the last 10 years, experimental techniques have been capable of visualizing the dense region, but the experiments reliability, analysis and effectiveness in this region still requires vast improvements. In this scenario, this thesis aims to contribute in the understanding of these physical process and to provide analysis tools for these complex flows. In order to do so, Direct Numerical Simulations have been used for addressing the problem at its smallest scale of motion, while reliably capturing all turbulence scales and breakup events. The multiphase nature of the flow is accounted for by using the Volume of Fluid method. One of the goal of the thesis was to assess the influence of the inflow boundary conditions on the primary atomization and on the spray's turbulence behavior. In order to do so, two different boundary conditions were used. In a first place, a synthetic inflow boundary condition was used in order to produce a homogeneous turbulence inflow, simulating the nozzle behavior. One of the interesting features of this method was the possibility of tweaking the parameters within the algorithm. In particular, the integral length scale was varied in order to assess the influence of nozzle larger turbulent structures on the primary atomization. The analysis on the synthetic boundary condition also allowed to optimally design simulations from which derive meaningful turbulence statistics. On this framework, further studies were carried over on the influence of turbulent structures properties, namely homogeneity and anisotropy, on both the flows spectra and droplets statistics. In order to achieve this goal, novel procedures for both computing the flow spectra and analyzing droplets were developed and are carefully addressed in the thesis. The results of the analysis highlight the independence of droplets statistics from the inflow boundary condition, while, on the other hand, remarking how the total quantity of atomized mass is significantly affected by the turbulence features developed within the nozzle. This considerations are supported by the spectrum analysis performed, which also highlighted how multiphase turbulence shares the universal features described in Kolmogorov theories. / Crialesi Esposito, M. (2019). Analysis of primary atomization in sprays using Direct Numerical Simulation [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/133975

The present research is an experimental investigation of the atomization of a superheated pressurized liquid jet that is exposed to the ambient pressure due to a sudden depressurization. This phenomena is called flashing and occurs in several industrial environments. Liquid flashing phenomena holds an interest in many areas of science and engineering. Typical examples one can mention: a) the accidental release of flammable and toxic pressure-liquefied gases in chemical and nuclear industry; the failure of a vessel or pipe in the form of a small hole results in the formation of a two-phase jet containing a mixture of liquid droplets and vapor, b) atomisation improvement in the fuel injector technology, c) flashing mechanism occurrence in expansion devices of refrigerator cycles etc... The interest in flashing events is especially true in the safety field where any unexpected event is undesirable. In case of an accident, flammable or toxic gas clouds are anticipated in close regions of the release because of the sudden phase change . Due to the non-equilibrium nature of the flow in these near field regions, conducting accurate data measurements for droplet size and velocity is a challenging task resulting in scarce data in the very close area. This research has been carried out at the von Karman Institute (VKI) within the 5th framework of European Commission to fulfill the goal of understanding of source processes in flashing liquids in accidental releases. The program is carried out under name of FLIE (Flashing Liquids in Industrial Environments)(Contract no: EVG1-CT-2000-00025). The specific issues that are presented in this thesis study are the following:a) a comprehensive state of art of the jet break up patterns, spray characteristics and studies related to flashing phenomena; b)flashing jet breakup patterns and accurate characterization of the atomized jet such as droplet diameter size, velocity and temperature evolution through carefully designed laboratory-scale experiments; c) the influence of the initial storage conditions on the final atomized jet; d) a physical model on the droplet transformation and rapid evaporation in aerosol jets. In order to characterize the atomization of the superheated liquid jet, laser-based optical techniques like Particle Image Velocimetry (PIV), Phase Doppler Anemometry (PDA) are used to obtain information for particle diameter and velocity evolution at various axial and radial distances. Moreover, a high-speed video photography presents the possibility to understand the break-up pattern changes of the simulating liquid namely R-134A jet in function of driving pressure, superheat and discharge nozzle characteristics. Global temperature measurements with an intrusive technique such as thermocouples, non-intrusive measurements with Infrared Thermography are performed. Cases for different initial pressures, temperatures, orifice diameters and length-to-diameter ratios are studied. The break-up patterns, the evolution of the mean droplet size, velocity, RMS, turbulence intensity and temperature along the radial and axial directions are presented in function of initial parameters. Highly populated drop size and velocity count distributions are provided. Among the initial storage conditions, superheat effect is found to be very important in providing small droplets. A 1-D analytical rapid evaporation model is developed in order to explain the strong temperature decrease during the measurements. A sensitivity analysis of this model is provided.

This thesis is focused on increasing the senstitivity of gold determination by electrochemical volatile species generation using two different types of electrolytic cells in continuous flow setting. Externally heated quartz tube atomizer was used as means of atomization and detection of gold with atomic absorption spectrometer. Generation parameters were optimized for electrolytic cell with an ion exchange (nafion) membrane. After selection of new cathode material (Cu) the carrier gas (Ar) flow rate was optimized, where an additional inlet of carrier gas was found to have possitive effect on increasing the sensitivity of determination of gold and efficiency of volatile specie transport to the atomizer. Experiments with Antifoam B showed possitive effect on generation, thus calibration was carried out for optimized experimetal conditions reaching detection limit of 0,53 mg.dm−3 . The efficiency of volatile specie transfer from liquid to gaseous phase was determined between 60 - 65 % by measuring the residual gold content in liquid waste by F-AAS method. Subsequently the effieciency of electrolytic generation of volatile gold specie with radioactive tracer isotopes and autoradigraphy was determined to 0,6 %. These methods confirmed adsorption of generated species on apparatus surface. Using ICP-MS as...

La réduction des émissions polluantes est actuellement un enjeu majeur au sein du secteur aéronautique. Parmi les solutions développées par les motoristes, la combustion en régime pauvre apparaît comme une technologie efficace pour réduire l’impact de la combustion sur l’environnement.Or, ce type de technologie favorise l’apparition d’instabilités de combustion issues d’un couplage thermo-acoustique. Des études expérimentales précédemment menées à l’ONERA ont mis en évidence l’importance de l’atomisation au sein d’un injecteur multipoint sur le phénomène d’instabilités de combustion. L’objectif de cette thèse est de mettre en place la méthodologie multi-échelle pour reproduire les phénomènes de couplage entre l’atomisation du jet liquide en présence d’un écoulement gazeux transverse (configuration simplifiée d’un point d’injection d’un injecteur multipoint) et d’une perturbation acoustique imposée, représentative de l’effet d’une instabilité de combustion. Ce type d’approche pourra, à terme, être utilisé pour la simulation instationnaire LES d’un système de combustion, et permettra de déterminer les temps caractéristiques de convection du carburant liquide pouvant affecter les phénomènes d’évaporation et de combustion, et donc l’apparition des instabilités de combustions. Afin de valider cette approche,les résultats issus des simulations sont systématiquement comparés aux observations expérimentales obtenues dans le cadre du projet SIGMA. Dans un premier temps, une simulation du jet liquide en présence d’un écoulement gazeux transverse est réalisée. Cette simulation a permis de valider l’approche multi-échelle : pour cela, les grandes échelles du jet, ainsi que les mécanismes d’atomisation reproduits par les simulations, sont analysés. Ensuite, l’influence d’une perturbation acoustique sur l’atomisation du jet liquide est étudiée. Les comportements instationnaires du jet et du spray issu de l’atomisation sont comparés aux résultats expérimentaux à l’aide des moyennes temporelles et des moyennes de phase. / The reduction of polluting emissions is currently a major issue in the aeronautics industry.Among the solutions developed by the engine manufacturers, lean combustion appears as an effectivetechnology to reduce the impact of combustion on the environment. However, this type oftechnology enhances the onset of combustion instabilities, resulting from a thermo-acoustic coupling.Experimental studies previously conducted at ONERA have highlighted the importanceof atomization in a multipoint injector to the combustion instabilities. The aim of this thesis isto implement the multi-scale methodology to reproduce the coupling phenomena between theatomization of the liquid jet in the presence of a crossflow (which is a simplified configuration ofan injection point of a multipoint injector) and an imposed acoustic perturbation, representativeof the effect of combustion instabilities. This type of approach can ultimately be used for the unsteadysimulation of a combustion system, and will determine the characteristic convection timesof the liquid fuel that can affect the phenomena of evaporation and combustion, and therefore theappearance of combustion instabilities. In order to validate this approach, the results obtainedfrom the simulations are systematically compared with the experimental observations obtainedwithin the framework of the SIGMA project. First, a simulation of the liquid jet in gaseous crossflowis performed. This simulation enabled us to validate the multi-scale approach : to this end,the large scales of the jet, as well as the atomization mechanisms reproduced by the simulations,are analyzed. Then, the influence of an acoustic perturbation on the atomization of the liquidjet is studied. The unsteady behavior of the jet and the spray resulting from the atomization arecompared with the experimental results using time averages and phase averages.

Neste trabalho de pesquisa foram estudados os efeitos dos parâmetros geométricos e de processo nas características do escoamento bifásico no interior de oito bocais nebulizadores do tipo \"Y-Jet\" através de uma bancada de análise experimental utilizando-se como fluidos de trabalho ar comprimido e água. Os resultados indicaram que as vazões mássicas são altamente dependentes da pressão de suprimento de ar e da relação entre os diâmetros do duto de mistura e do bocal de alimentação de ar. Em muitas situações de operação, esses dispositivos nebulizadores operavam com o escoamento de ar blocado à saída do seu bocal de alimentação. Outro aspecto importante é que, devido a fortes irreversibilidades inerentes ao padrão de escoamento, a expansão do fluxo de ar do seu bocal de alimentação para o duto de mistura aproxima-se muito mais de uma expansão isoentálpica que isoentrópica. Para fluxos mássicos de água superiores a 6000 kg/m2.s a distribuição de pressão no interior do duto de mistura é praticamente linear, independentemente do valor da pressão de alimentação de ar. Uma correlação para a previsão do valor da pressão no ponto de mistura entre os fluxos de ar e água dentro do duto de mistura foi desenvolvida e mostrou-se adequada para valores dentro da faixa de variação de cada parâmetro no experimento. Através de um aparato óptico buscou-se a medição da espessura média local de filme de líquido e da velocidade das perturbações na interface ar/água. Os resultados para a medição da espessura de filme mostraram-se sensivelmente dispersos, apontando para um melhor desenvolvimento dessas técnicas ópticas em futuros trabalhos. Quanto às velocidades das perturbações os resultados indicaram um razoável aumento destas conforme o escoamento se aproxima da saída do duto de mistura. Para todos os oito bocais ensaiados o valor médio destas velocidades, à saída do duto de mistura, situou-se em torno de 60 a 65 m/s. Um modelo teórico-experimental, baseado na medição da queda de pressão no interior do duto de mistura desses bocais, foi desenvolvido. Através desse modelo foi possível prever, localmente, a espessura e a velocidade médias de filme de líquido, a fração de entranhamento, a tensão de cisalhamento na interface ar/água, a fração de vazio e a velocidade média do ar no núcleo do escoamento. / In this research work the effects of the process and geometrical parameters on the characteristics of the internal two-phase flow inside eight Y-Jet atomizers were studied using an apparatus working with air and water. The results show that the flow rates are very dependent on the air supply pressure and the diameter ratio of the mixing duct and the air port. It was also verified that, in many operational conditions, these atomizers worked in the critical condition at the exit of the air port. Due to the strong irreversibilities present in the flow, the expansion from the air port to the mixing duct is closer to an isoenthalpic process than to an isoentropic process. For water mass flux greater than 6000 kg/m2.s, the pressure distribution into the mixing duct is most of the time linear, independently on the air supply pressure. A correlation to predict the mixing point pressure was developed and showed a good agreement with the experimental data. Using an optical apparatus it was measured the local liquid film thickness and the perturbations velocities on the air/water interface. The results for the liquid film showed a reasonable data dispersion. Concerning the perturbation velocities the results indicated that they increase along the mixing duct. For the eight atomizers tested the mean values of these velocities, near the mixing duct exit, were around 60 to 65 m/s. A theoretical-experimental model which uses the pressure drop measured inside the mixing duct was developed to predict locally the mean liquid film velocity and thickness, the entrainment fraction, the shear stress on the air/water interface, the void fraction and the mean air velocity in the flow core.