This Master’s thesis deals with the determination of selected micro and macro elements in bottled water purchased in retail chains Czech Republic. There are described macro elements and micro elements that occur in the waters, bottled waters legislation and the most frequent used instrumental methods for elemental analysis. In this work for the analysis of bottled water were used methods optical emission spectrometry with inductively coupled plasma (ICP-OES) and ion chromatography (IC). Elemental composition of bottled water after analysis corresponded to the composition indicated on the labels, there were recorded only minor deviations from the reported concentrations. All bottled water meets the conditions of the legislation of the Czech Republic. The measured data were statistically processed in the XL Stat program and by multivariate data analysis was examined whether it is possible to individual bottled water from each other based on the analyzes differentiate, which can help in verifying the authenticity of bottled water and in the detection of adulteration of bottled water for profit.

This master thesis deals with the analysis of nutritional properties of paprika condiment with different geographic origin. The theoretical part contains botanical description of red pepper (Capsicum annuum L.), its chemical composition, process of production of paprika and then they are described analytical methods suitable for determination of fundamental nutrional properties. Experimental part is focused on the preparation of samples and their analysis. In total, 11 samples were selected for the experiment, 5 of them had a protected designation of origin. These samples were from Slovakia, Hungary, Bulgary, Romania, Turkey and Spain. The Soxhlet extraction was used for the analysis of the fat content, Kjeldahl method was used to determine gross protein. High-performance liquid chromatography (HPLC) was chosen to determine carbohydrates and capsaicin. Induction-coupled plasma emission spectroscopy (ICP-OES) was used for elemental analysis. The results were compared with each other and with available databases and literature. For comparing and finding certain connections, the principal component analysis (PCA) was selected.

En la presente Tesis Doctoral la técnica de ablación laser acoplada a ICP-OES/MS ha sido empleada para analizar muestras sólidas, como catalizadores usados en el refinado del petróleo y polímeros. Se han llevado a cabo dos tipos de análisis, un análisis global de las muestras que proporciona información general y un análisis localizado que permite obtener información acerca de la distribución espacial de los elementos de interés en las muestras. Las diferentes variables de la técnica ablación láser son estudiadas con el fin de seleccionar aquellas que conducen una señal alta y estable, así como a un menor grado de fraccionamiento. Este estudio se realiza para cada tipo de muestra, ya que los resultados dependen de la matriz estudiada. Además, en esta Tesis doctoral se desarrolla un método de calibración para llevar a cabo un análisis cuantitativo de las muestras sólidas, basado en la deposición de patrones líquidos sobre la muestra sólida. Este método es conocido como “dried droplet calibration approach” (DDCA), y permite cuantificar elementos presentes en muestras sólidas sin necesidad de usar materiales de referencia sólidos. Este nuevo método de calibración compensa el fraccionamiento elemental y los efectos de matriz, proporcionando resultados exactos y preciosos para muestras complejas tales como vidrios, catalizadores y polímeros.

En los últimos años, las nuevas legislaciones nacionales e internacionales, establecen nuevos límites de detección para la cuantificación de metales a niveles traza, en muestras de suelos, aguas y aguas residuales. Por otro lado, la literatura científica y los fabricantes de instrumentos analíticos muestran aplicaciones de mejora en los límites de detección del Espectrómetro de emisión óptica por plasma acoplado inductivamente (ICP OES) al utilizar un nebulizador ultrasónico. Esta mejora se debe, a su alta eficiencia de transporte (10-20%), en comparación con el nebulizador neumático (1-2%). El presente trabajo, demuestra la efectividad del nebulizador ultrasónico para mejorar los límites de detección del ICP OES axial. Para ello se aplicó inicialmente el método EPA 200.7, este método utiliza un nebulizador concéntrico (neumático) como parte del sistema de introducción de muestra del ICP OES (método A). Aplicando este método, se obtuvo un LDM de 0.0062 mg/L para arsénico y 0.0040 mg/L para plomo. Al utilizar el nebulizador ultrasónico acoplado al ICP OES axial (método B) se obtuvo un LDM de 0.0007 mg/L para arsénico y 0.0005 mg/L para plomo. Al comparar ambos métodos, se observa que el uso del nebulizador ultrasónico en conjunto con el ICP OES (método B), permite mejorar 8 veces los LDM de los elementos arsénico y plomo obtenidos con el método A. La veracidad del método fue comprobada, utilizando materiales de referencia certificados, marca ERA, en matrices tipo agua de consumo y agua residual. Los resultados de las pruebas t de 1 muestra, ejecutadas a través del software Minitab, muestran valores de P value > 0.05, esto nos permite concluir que los valores encontrados experimentalmente, son equivalentes estadísticamente a los valores certificados del material de referencia, concluyendo que el método B es veraz. / Tesis

Lithium phosphorus oxy-nitride (LiPON) thin films are widely studied and used as a thin film electrolyte for lithium ion battery applications. LiPON thin films may be prepared by many techniques, but RF sputter deposition is most frequently used and was investigated in this dissertation, in spite of its low deposition rate, because of it offers more reliable and controllable processing. This dissertation includes the methodologies of sputter deposition and materials characterization of the LiPON thin film electrolytes. The LiPON thin films were deposited under varying conditions of process gas, substrate bias, and deposition temperature. To understand the variations in ionic conductivity observed, the films were extensively characterized to examine structural and compositional differences, including examination by x-ray photoelectron spectroscopy (XPS), inductively coupled plasma optical emission spectroscopy (ICP/OES), and spectroscopic ellipsometry. In addition, film density, and the intrinsic stress of the deposited films were also studied. The highest ionic conductivity of 9.8 x 10-6 S/cm was obtained at elevated deposition temperature and is correlated to a reduced density of defects, as indicated from the optical characterization.

Studies of the interaction of the relevant metal, metalloid or nanoparticulate species with biological systems are underpinned by the provision of reliable information about chemical composition of the relevant materials. Often, no methods of chemical analysis are available. The work described in this dissertation centers on developing methods to help with studies for a variety of analytes and samples. A method was developed for the determination of 11 trace elements (As, Cd, Co, Cr, Cu, Fe, Mg, Mn, Pb, Ti, and Zn) in human breast milk and infant formulas by inductively coupled plasma optical emission spectrometry (ICP-OES) following microwave-assisted digestion. A method was established for the determination of trace elements, with an emphasis on titanium as titanium dioxide, in snack foods and consumer products. The interactions of some dissolved metals, including rare earth elements, and metallo-nanoparticles (silver, gold, titanium dioxide, aluminum oxide, and iron) with aquatic plants were studied. After exposure in a variety of mesocosms, the partitioning of the elemental species between various compartments was quantified by ICP-MS and ICP-OES following microwave-assisted digestion. An ICP mass spectrometry (MS) method has also been developed to quantify the uptake of gold and silver nanoparticles by C. elegans. Uptake of gold nanoparticles was size dependent, suggesting increased ingestion efficiency with increased particle diameter. The feasibility of discriminating between suspended TiO2 nanoparticles and dissolved titanium by the analysis of the rapid transient signal events obtained from the ICP-MS instrument operated in a rapid response mode was also developed. Data handling parameters were established that allowed a distinction in the signals for nanoparticulate and standard solutions. Spikes in the signal were defined by distinct parameters using the mean and standard deviation, where a spike in the signal was defined as a signal > + ks (k =3). This approach however did lead to a statistical difference in the spike signal events for solutions and nanosuspensions.

A method was developed for the determination of total arsenic in rice grain by microwave-assisted digestion inductively coupled plasma mass spectrometry. Standard calibration solutions were matrix-matched with respect to acid concentration and carbon content post-digest. The importance of eliminating the drying step during sample preparation procedures was investigated. The method was validated with spikes containing standard arsenate solutions into the rice matrix, and with certified reference material SRM1568a (rice flour) from NIST. The method was successfully applied to a commercially available rice sample. Four arsenic species [arsenate (As(V)), arsenite (As(III)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA)] were extracted from rice grains by microwave-assisted extraction and separated with high performance liquid chromatography inductively coupled plasma mass spectrometry. The method includes a novel sample clean-up step involving a dialysis procedure to decrease the amount of large starch molecules in the injection solution, in order to minimize poor resolution of chromatographic peaks and maximize column life. The method was validated with spikes of standard arsenic solutions, added to the rice matrix before the extraction procedure. Literature reference values for arsenic species quantification in SRM1568a (rice flour) were also compared. This method was successfully applied to a commercially available rice sample. A study into improvements in reverse phase-HPLC separations of arsenic species was conducted. For the first time, a Sunfire C8 column from Waters (Milford, CT) was employed for the separation of arsenic species in rice extracts. This column was compared to a Symmetry C8 column with respect to total elution time, detection limits, interference effects, and column life, and evaluated with respect to peak resolution, shifts in retention times, and peak symmetry.

Bottled drinking water is a common form of water consumption that has grown in popularity and dependency. With countless types and brands available, there are factors to consider regarding the variations in mineral content and microbiological quality, and environmental consequences associated with importing natural bottled waters. Saudi Arabia is the largest desalinated water producer, and although there are scarce natural water resources, consuming locally produced water can alleviate environmental pressures, so long as local bottled water is of good quality and provides the basic function of drinking water. The objective of this study is to scrutinize the variations in bottled waters available in the Saudi market and compare local and imported waters regarding water quality and compliance with health regulations. Surveying local bottled waters revealed that over 60% were imported, adding to the environmental significance. Results from inductively coupled plasma-atomic emission spectroscopy, ion chromatography, and pH meters indicate most bottled waters were compliant with health standards. Flow Cytometry (FCM) was used to determine microbial cell densities. Purified waters, on average, contained significantly lower concentrations than other water types, while mineral waters contained the most cells per milliliter. Microbiological stability was examined through incubating samples at 30°C to promote microbial growth, and results were analyzed using an online FCM system. Purified waters had the least amount of growth and to a lesser degree than mineral and sparkling, which varied in microbial growth responses. DNA extractions and microbial community analyses were performed on select mineral waters before and after incubation. Results showed microbial genera found were similar between samples from the same country and some were unique. All samples exhibited some change in microbial community composition after incubation, signifying that certain communities thrived more than others. Proteobacteria was the most common abundant phylum among samples. Although analysis was restricted to the genera level, there were no health concern associated with types of bacteria discovered. In conclusion, local purified waters had greater microbiological quality and stability than imported waters, and mineral compositions were within the healthy range. Reducing reliance on foreign natural waters may help alleviate environmental consequences and improve local economy

Studien har genomförts på ett antal stålplåtar från olika kulturhistoriska byggnader. När kulturhistoriskt värdefulla byggnader ska renoveras måste detta göras med så god kunskap som möjligt om byggnadens olika delar och de värden dessa representerar. Det problem som studien har ämnat att lösa har varit en bristande kunskap om historiska stålplåtar. Studien har därför utförts för att bidra med kunskap som kan användas när gamla byggnader ska renoveras.För att uppnå syftet att bidra med kunskap som kan vägleda renovering av kulturhistoriska byggnader har studiens mål varit att undersöka hur de olika plåtarna tillverkats och vilka resultat de processerna har fått.Detta har genomförts genom att utföra en metallografi på samtliga prover för att undersöka deras mikrostrukturer och få en förståelse för materialen. Även en kemisk analys av materialens innehåll har gjorts genom en optisk emissions spektroskopi.De resultat som hämtades från plåtarna visade hur stor skillnad det var mellan olika tillverkningsmetoder och deras konsekvenser. Genom att ha sett den mångfald av egenskaper som fanns bland plåtarna har slutsatserna dragits att det finns ett värde i att respektera de äldre materialen.Genom att vara medveten om att det kan finnas stora skillnader i materialen kan valet av plåt göras på ett bättre sätt. Under studiens gång blev det även uppenbart hur mycket historia som fanns lagrad i de gamla plåtarna som är viktig att ta vara på. / The study has been conducted on a number of steel plates from different buildings of cultural and historical value. When old, cultural buildings are to be renovated, it must be done with as much knowledge as possible about the different parts of the building and the values that they represent. The problem that the study has aimed to solve has been an inadequate level of knowledge in regards to historical steel plates. Because of this, the study has been conducted to contribute with knowledge that could be used when old buildings are to be renovated.To achieve the purpose of contributing knowledge to guide renovations of culturally and historically valuable buildings, the goal of the study has been to analyze how the different plates have been made and what the results of those processes were.This has been carried out by conducting a metallography on all of the samples to analyze their microstructures and to gain an understanding of the materials. A chemical analysis has also been conducted on the contents of the materials by using optical emission spectroscopy.The results showed how big of a difference there was between different manufacturing methods and their consequences. By discovering the diversity of the properties of the plates the conclusion has been drawn that there is value in respecting the values of the older materials.By being conscious of how large the difference is between different types of steel sheets, better decisions can be made during choice of steel sheet, and it is more obvious how much history that is stored within the old plates.

Le but de cette thèse était d’étudier la dynamique de croissance par pulvérisation par plasma RF magnétron des couches minces à base d’oxyde de zinc destinées à des applications électroniques, optoélectroniques et photoniques de pointe. Dans ce contexte, nous avons mis au point plusieurs diagnostics permettant de caractériser les espèces neutres et chargées dans ce type de plasmas, notamment la sonde électrostatique, la spectroscopie optique d’émission et d’absorption, ainsi que la spectrométrie de masse. Par la suite, nous avons tenté de corréler certaines caractéristiques physiques de croissance des couches de ZnO, en particulier la vitesse de dépôt, aux propriétés fondamentales du plasma. Nos résultats ont montré que l’éjection d’atomes de Zn, In et O au cours de la pulvérisation RF magnétron de cibles de Zn, ZnO et In2O3 n’influence que très peu la densité d’ions positifs (et donc la densité d’électrons en supposant la quasi-neutralité) ainsi que la fonction de distribution en énergie des électrons (populations de basse et haute énergie). Cependant, le rapport entre la densité d’atomes d’argon métastables (3P2) sur la densité électronique décroît lorsque la densité d’atomes de Zn augmente, un effet pouvant être attribué à l’ionisation des atomes de Zn par effet Penning. De plus, dans les conditions opératoires étudiées (plasmas de basse pression, < 100 mTorr), la thermalisation des atomes pulvérisés par collisions avec les atomes en phase gazeuse demeure incomplète. Nous avons montré que l’une des conséquences de ce résultat est la présence d’ions Zn+ suprathermiques près du substrat. Finalement, nous avons corrélé la quantité d’atomes de Zn pulvérisés déterminée par spectroscopie d’émission avec la vitesse de dépôt d’une couche mince de ZnO mesurée par ellipsométrie spectroscopique. Ces travaux ont permis de mettre en évidence que ce sont majoritairement les atomes de Zn (et non les espèces excitées et/ou ioniques) qui gouvernent la dynamique de croissance par pulvérisation RF magnétron des couches minces de ZnO. / The goal of this thesis was to study the growth dynamics of zinc oxide based thin films by RF magnetron sputtering plasmas for advanced electronic, optoelectronic, and photonic applications. In this context, we have developed several diagnostics to characterize neutral and charged species in such plasmas, in particular electrostatic probe, optical emission and absorption spectroscopy, as well as plasma sampling mass spectrometry. Afterward, we have tried to correlate specific physical characteristics of as-grown ZnO thin films, in particular the deposition rate, to fundamental plasma properties. Our results have shown that the ejection of Zn, In and O atoms during the RF magnetron sputtering of Zn, ZnO and In2O3 targets does not significantly influence the number density of positive ions (and thus the electron density assuming quasi-neutrality) as well as the electron energy distribution function (populations of low and high energy). However, the ratio of the number density of metastable argon atoms (3P2) to the electron density decreases with increasing concentration Zn atoms; a feature that can be ascribed to Penning ionization of RF sputtered Zn atoms. Furthermore, over the range operating conditions examined in this study (low-pressure plasmas), the thermalization of sputtered atoms by collisions with atoms in the gas phase remains incomplete. We have shown that one of the consequences of this result is the presence of suprathermic Zn+ ions near the target. Finally, we have correlated the quantity of sputtered Zn atoms determined by optical emission spectroscopy with the deposition rate of ZnO thin films measured by spectroscopic ellipsometry. This set of data lead us to the conclusion that mainly Zn atoms (and not excited and/or ionic Zn species) govern the growth dynamic of ZnO-based thin films during magnetron sputtering in argon RF plasmas.