Magister Scientiae - MSc / In electrochemical oxidation treatment of wastewater, the electrode material is an important parameter in optimizing oxidative electrochemical processes, since the mechanism and products of several anodic reactions are known to depend on the anode material. The electrochemical oxidation of benzaldehyde, nitrobenzene and m-cresol on bare boron-doped diamond (BDD) electrode was investigated. Cytochrome c was then electrochemically immobilsed onto the functionalized BDD electrode by cyclic voltammetry. Oxidation and reduction reaction mechanism of each flavonoid was studied. There was one oxidation and reduction peaks for quercitin and catechin respectively, and two oxidation and two reduction peaks for rutin. The cytochrome c modified BDD electrode showed good sensitivity for all three flavonoids and low detection limits i.e. 0.42 to 11.24 M as evaluated at oxidation and reduction peaks, respectively. / South Africa

Philosophiae Doctor - PhD / A highly dispersive gold nanoparticle-dotted 4-nitrophenylazo functionalised graphene nanocomposite (AuNp/G/PhNO2) was successfully synthesised and applied in enhancing sensing platform signals. Three label-free electrochemical immunosensors for the detection of deoxynivalenol mycotoxin (DON) based on the systematic modification of glassy carbon electrodes (GCE) with AuNp/G/PhNO2 was effectively achieved. General electrochemical impedance method was employed for the sensitive and selective detection of DON in standard solutions and reference material samples. A significant increase in charge transfer resistance (Rct) of the sensing interface was observed due to the formation of insulating immune-complexes by the binding of deoxynivalenol antibody (DONab) and deoxynivalenol antigen (DONag). Further attachments of DONab and DONag resulted in increases in the obtained Rct values, and the increases were linearly proportional to the concentration of DONag. The three immunosensors denoted as GCE/PDMA/AuNp/G/PhNH2/DONab, GCE/Nafion/[Ru(bpy)3]2+/AuNp/G/PhNH2/DONab and GCE/Nafion/[Ru(bpy)3]2+/G/PhNH2/DONab have detection range of 6 – 30 ng/mL for DONag in standard samples. Their sensitivity and detection limits were 43.45 ΩL/ng and 1.1 pg/L; 32.14ΩL/ng and 0.3 pg/L; 9.412 ΩL/ng and 1.1 pg/L respectively. This result was better than those reported in the literature and compares reasonably with Enzyme Linked Immunosorbent Assay (ELISA) results. The present sensing methodology represents an attractive alternative to the existing methods for the detection of deoxynivalenol mycotoxin and other big biomolecules of interest due to its simplicity, stability, sensitivity, reproducibility, selectivity, and inexpensive instrumentation. And they could be used to develop high-performance, ultra-sensitive electrochemiluminescence, voltammetric or amperometric sensors as well.

Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPq / In this work, we described the structural, morphological, optical and electrical properties of the ZnO thin films undoped and chromium (Cr), copper (Cu), aluminium (Al) doped deposited using magnetron sputtering and co-sputtering method on glasses, Cr and niobium (Nb) substrates. For characterization of the samples were used the X-ray diffraction (XRD), X-ray reflectometry (XRR), UV-Vis spectroscopy in the visible region techniques and IxV plots. This work was divided in two parts, in the study I, ZnO films were grown on glasses substrates and the influence of the substrate temperature, RF power and films thickness at the structural, morphological and optical properties was studied. The results showed that all films grown exhibit characteristic peaks of hexagonal wurtzite phase with axis-c preferential orientation, the films roughness was very influenced by thickness and temperature and the gap energy varied with the films thickness. In the study II, thin films undoped and doped were grown at 300ºC on different substrates and the influence of kind of substrate, dopants, dopant concentration on the structural, morphological, optical and electrical properties was studied. Generally, all samples deposited on Cr substrates exhibit resistance lower than the samples deposited on Nb substrates. For some samples, an unusual behavior was observed at the moment of electrical measurements, after any voltage, different for each sample, the current fell abruptly. / Neste trabalho, descrevemos as propriedades estruturais, morfológicas, ópticas e elétricas de filmes finos de ZnO puros e dopados com cromo (Cr), cobre (Cu) e alumínio (Al) depositados por sputtering e co-sputtering em substratos de vidro, Cr e nióbio (Nb). Foram utilizadas as técnicas de difração de raios X (DRX), reflectometria de raios X (XRR), espectroscopia óptica na região do UV-Vis e curvas de IxV para caracterização das amostras. O trabalho foi dividido em duas etapas, na primeira etapa foram estudados os efeitos da espessura, da temperatura do substrato e da potência RF nas propriedades estruturais, morfológicas e ópticas dos filmes de ZnO crescidos sobre substrato de vidro. Os resultados mostraram que todos os filmes produzidos apresentam picos característicos da fase hexagonal wurtzita com orientação preferencial ao longo do eixo-c, a rugosidade dos filmes foi bastante influenciada pela espessura e temperatura e a energia de gap variou com a espessura dos filmes. Na segunda etapa, filmes finos puros e dopados foram depositados a 300ºC em diferentes substratos. Nesta etapa foram investigados a influência do tipo de substrato e da concentração dos dopantes nas propriedades estruturais, morfológicas, ópticas e elétricas. Os resultados mostraram que a cristalinidade dos filmes de ZnO foi fortemente influenciada pela rugosidade do substrato. De modo geral, todas as amostras depositadas sob substratos de Cr apresentaram resistência menores do que as amostras depositadas sob Nb. Para algumas amostras, um comportamento não usual foi observado no momento das medidas elétricas onde após uma determinada tensão, diferente para cada amostra, a corrente caía abruptamente.

Brazil is a great producer and consumer of fruits in the world. The soursop (Annona muricata L.) is a fruit with special flavor and aroma and with growing demand for fresh or processed consumption, such as juices, jams, fruit jellies and ice cream. However, the culture of soursop is subjected to the action of different pests and diseases and the application of pesticides has been one of the main ways of control. The present work aims at developing a rapid and low-cost methodology based on matrix solid phase dispersion and high-performance liquid chromatography with diode-array detection (HPLC UV-Vis/DAD) for the determination of pesticide residues of Bifenthrin, Lufenuron, Teflubenzuron, Thiacloprid, Thiophanate-methyl and Thiamethoxam, in the exotic fruit soursop. Some tests conducted with the standards of pesticides allowed the adjustment of the chromatographic conditions for simultaneous analysis of analytes. The best extraction conditions were obtained using 1.0 g of Florisil to 0.5 g of fresh soursop and Elution with 5 mL of Acetonitrile. The miniaturization of the extraction procedure was shown to be efficient in the extraction of pesticides. Analytical validation was performed from the parameters: linearity and sensitivity, with coefficients of determination over 0.9995 and sensitive concentration range of 0.01 -10 g mL-1; selectivity, from the matrix effect studies; accuracy and precision, with recovery values between -118 79% and RSD in the range of 1- 15% for concentration levels 0.1, 0.25 and 0.5 g g-1 (n = 5); and limits of detection and quantification in the intervals of 0.01-0.25 g g-1 and 0.1-0.5 g g- 1, respectively. Metal Organic Frameworks (MOF) [(Nd0, 9Eu0.1)2(DPA)3(H2O)3] was tested as sorbent for the MSPD extraction process and presented satisfactory recovery results (78-87%) compared to those achieved with Florisil. / O Brasil é um importante produtor e consumidor de frutas no mundo. A graviola (Annona muricata L.) é uma fruta de sabor e aroma característicos e com crescente demanda, seja para o consumo in natura ou na forma processada, como sucos, doces, geleias e sorvetes. Todavia, a cultura da graviola está sujeita a ação de diferentes pragas e doenças e a aplicação de agrotóxicos tem sido uma das principais formas de controle. O presente trabalho tem como objetivo o desenvolvimento de uma metodologia rápida e de baixo custo baseada nas técnicas de dispersão da matriz em fase sólida (MSPD) e cromatografia líquida de alta eficiência com detector espectrofotométrico na região do ultravioleta e visível com arranjo de diodos (HPLC UV-Vis/DAD) para a determinação de resíduos dos agrotóxicos bifentrina, lufenuron, teflubenzuron, tiacloprido, tiofanato metílico e tiametoxam, na fruta exótica graviola. Testes realizados com os padrões dos agrotóxicos permitiram o ajuste das condições cromatográficas para análise simultânea dos analitos. As melhores condições de extração foram obtidas utilizando 1,0 g de Florisil para 0,5 g de graviola in natura e eluição com 5 mL de acetonitrila. A miniaturização do procedimento de extração mostrou-se eficiente à extração dos agrotóxicos. A validação analítica foi realizada a partir dos parâmetros: linearidade e sensibilidade, mostrando-se linear com coeficientes de determinação superiores a 0,9995 e sensível no intervalo de concentração de 0,01-10 g mL-1; seletividade, a partir dos estudos de efeito matriz; exatidão e precisão, com valores de recuperação entre 79 -118% e coeficientes de variação na faixa de 1-15 % para os níveis de concentração 0,1; 0,25 e 0,5 g g-1 (n=5); e limites de detecção e quantificação nos intervalos de 0,01 - 0,25 g g-1 e 0,1 - 0,5 g g-1 , respectivamente. O material metal-orgânico (MOF) [(Nd0,9Eu0,1)2(DPA)3(H2O)3] foi testado como adsorvente para o processo de extração por MSPD e apresentou resultados satisfatórios de recuperação (78-87%), comparados àqueles obtidos com o Florisil.

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Organometal halide perovskite absorbers such as methylammonium lead iodide chloride (CH3NH3PbI3-xClx), have emerged as an exciting new material family for photovoltaics due to its appealing features that include suitable direct bandgap with intense light absorbance, band gap tunability, ultra-fast charge carrier generation, slow electron-hole recombination rates, long electron and hole diffusion lengths, microsecond-long balanced carrier mobilities, and ambipolarity. The standard method of preparing CH3NH3PbI3-xClx perovskite precursors is a tedious process involving multiple synthesis steps and, the chemicals being used (hydroiodic acid and methylamine) are quite expensive. This work describes a novel, single-step, simple, and cost-effective solution approach to prepare CH3NH3PbI3-xClx thin films by the direct reaction of the commercially available CH3NH3Cl (or MACl) and PbI2. A detailed analysis of the structural and optical properties of CH3NH3PbI3-xClx thin films deposited by aerosol assisted chemical vapor deposition is presented. Optimum growth conditions have been identified. It is shown that the deposited thin films are highly crystalline with intense optical absorbance. Charge carrier separation of these thin films can be enhanced by establishing a local internal electric field that can reduce electron-hole recombination resulting in increased photo current. The intrinsic ferroelectricity in nanoparticles of Barium Titanate (BaTiO3 -BTO) embedded in the solar absorber can generate such an internal field. A hybrid structure of CH3NH3PbI3-xClx perovskite and ferroelectric BTO nanocomposite FTO/TiO2/CH3NH3PbI3-xClx: BTO/P3HT/Cu as a new type of photovoltaic device is investigated. Aerosol assisted chemical vapor deposition process that is scalable to large-scale manufacturing was used for the growth of the multilayer structure. TiO2 and P3HT with additives were used as ETL and HTL respectively. The growth process of the solar absorber layer includes the nebulization of a mixture of PbI2 and CH3NH3Cl perovskite precursors and BTO nanoparticles dissolved in DMF, and injection of the aerosol into the growth chamber and subsequent deposition on TiO2. While high percentage of BTO in the film increases the carrier separation, it also leads to reduced carrier generation. A model was developed to guide the optimum BTO nanoparticle concentration in the nanocomposite films. Characterization of perovskite solar cells indicated that ferroelectric polarization of BTO nanoparticles leads to the increase of the width of depletion regions in the perovskite layer hence the photo current was increased by one order of magnitude after poling the devices. The ferroelectric polarization of BTO nanoparticles within the perovskite solar absorber provides a new perspective for tailoring the working mechanism and photovoltaic performance of perovskite solar cells.

Le présent travail concerne principalement l'élaboration d'un nouveau ligand en l'occurrence le cyclen-hydrazone, luminescent et efficace pour une détection relativement sélective de l'ion d'intérêt biologique, Zn2+. La synthèse du groupement azaxanthone à greffer sur le cyclen a été décrite. A partir de ces ligands, la complexation de zinc, a été traitée dans le but de développer une sonde optique sélective pour les ions métalliques de la première série de transition. Une étude photophysique associée à un travail de modélisation théorique en solution a plus particulièrement montré la formation de deux nouveaux complexes de zinc. Finalement, le contrôle des conditions de déprotection par hydrazinolyse du cyclen-glyoxal-azaxanthone, a montré que le motif azaxanthone puisse être maintenu dans la conception de nouveaux complexant de métaux de la première série de transition. / This study deals with the development of a new ligand: the cyclen-hydrazone, luminescent and effective for a relatively selective detection of biological ion, Zn2+. The synthesis of graft azaxanthone group to the cyclen was described. From these ligands zinc complexation was treated in order to develop an optical probe selective for the first row transition metals. A photophysic study associated with theoretical modeling work in solution, specifically showed the formation of two new zinc complexes. Finally, the monitoring of deprotection by hydrazinolysis of cyclen-glyoxal-azaxanthone, showed that the azaxanthone deprotection could be maintained in the design of new metals complexes of the first serie of transition metals.

This thesis deals with the characterization and preparation of catanionic vesicular systems and their interaction with water-insoluble vitamins. Catanionic vesicles systems was prepared from two differently charged sufractants CTAB and SDS in formation ion pair amphiphile. Stability of vesicles was secured by adding cholesterol with positively charged surfactant DODAC. Were selected vitamin A and vitamin E for solubilization into these vesicles. The next part of this work was focused on determining the efficiency of incorporation these vitamins into the HTMA-DS vesicular system. The characterization of these systems was improved by measurement on a UV-VIS spectrometer, DLS and by HPLC with UV-VIS detector. During measurement by UV-VIS and HPLC the efficiency of solubilization of vitamin A and vitamin E into vesicles was determinated. In both cases higher efficiency was determinated for vesicles with incorporated vitamin A. Higher efficiency for both vitamins was determinated by HPLC. The reason is probably the higher sensitivity of the metod, work in labs with dark glass and preparing individuals samples into vials, which were inserted into the device for individual dosing by injector. The work serves primary evaluation results in view of the vesicular system for use in pharmaceutical application like carrier non-polar vitamins.

In der vorliegenden Arbeit werden eine neue mikrowellenassistierte Darstellungsmethode für Bismutvanadatnanopartikel ebenso wie ein ultraschallgestütztes Sprühverfahren zur Abscheidung von Bismut(III)-oxidschichten beschrieben. Nanopartikuläres m-BiVO4 wird durch die Umsetzung von Bi(OtBu)3 mit VO(OtBu)3 unter Zugabe von polymersierbaren Alkoholen, nicht polymerisierbaren Alkoholen sowie ohne Zusätze in einer nichtwässrigen Lösung gefolgt von einer thermischen Oxidation erhalten. Anschließend werden die Nanopartikel hinsichtlich ihrer Eigenschaften verglichen. Ausgehend von einem polynuklearen Bismutoxidocluster wird über ultraschallgestütztes Kaltsprühen, einer sich anschließenden kontrollierten Hydrolyse und einer finalen thermischen Behandlung die Beschichtung verschiedener Substrate mit α-Bi2O3, β-Bi2O3 sowie α/β-Bi2O3 erreicht. Die Charakterisierung der synthetisierten Materialien erfolgt unter anderem mittels Pulverröntgendiffraktometrie, NMR-Spektroskopie, CHN-Analysen, UV/VIS-, IR- und Ramanspektroskopie, thermogravimetrischen Analysen sowie elektronenmikrospische Aufnahmen. Zusätzlich werden die Halbleiterschichten mit einer Wirbelstromsonde vermessen. Die bismuthaltigen Halbleitermaterialien sind im sichtbaren Lichtspektrum anregbar und weisen eine hohe photokatalytische Aktivität beim Abbau von Rhodamin B auf, wobei die zugrunde liegenden Abbaumechanismen UV/VIS-spektroskopisch aufgeklärt werden. Darüber hinaus werden die Photokatalysatoraktivitäten gegenüber wässrigen Lösungen von Methylorange, Orange G, Methylenblau sowie Schadstofflösungen des Biozids Triclosan und des pharmazeutischen Wirkstoffs Ethinylestradiol diskutiert, deren photokatalytische Zersetzung ergänzend mit TOC-Analysen verfolgt wird.:Abkürzungsverzeichnis.....11 1 Einleitung und Motivation.....15 2 Grundlagen der Photokatalyse.....21 2.1 Photokatalyse mit Halbleitern.....21 2.1.1 Definition und Unterteilung von Photokatalysatoren.....21 2.1.2 Funktionsweise, Eigenschaften und weitere Anwendungsfelder von Halbleiterphotokatalysatoren.....22 2.1.3 Cokatalysatoren in der Photokatalyse.....26 2.1.4 Photokatalysatoren mit Heteroübergang.....28 2.2 Photokatalytischer Abbau von organischen Substanzen.....29 2.2.1 Grundlagen zu Reaktionspfaden und aktiven Spezies.....29 2.2.2 Mechanismen und Kinetik der photokatalytischen Zersetzung am Beispiel von Rhodamin B.....32 2.3 Bismutvanadat als Photokatalysator.....38 2.4 Bismut(III)-oxid als Photokatalysator.....41 3 Photokatalytische Untersuchungen an Bismutvanadatnanopartikeln aus mikrowellenassistierten Synthesen.....47 3.1 Synthesemethoden für Metalloxidnanostrukturen und Voruntersuchungen zur nichtwässrigen Darstellung von nanoskaligem Bismutvanadat.....47 3.2 Darstellung von Bismutvanadatnanopartikeln über die Umsetzung von Bismut(III)-alkoxiden und Vanadium(V)-alkoxiden im Mikrowellenreaktor.....53 3.2.1 Umsetzung von Bismut(III)-alkoxiden und Vanadium(V)-alkoxiden im Mikrowellenreaktor.....53 3.2.2 Darstellung von Bismutvanadatnanopartikeln durch thermische Oxidation der Materialien MW-II – MW-V.....57 3.3 Photokatalytische Untersuchungen an monoklinen Bismutvanadatnanopartikeln .....61 3.3.1 Untersuchungen zu den photoinduzierten Abbaumechanismen von Rhodamin B mit Bismutvanadatnanopartikeln.....61 3.3.2 Vergleich der photokatalytischen Aktivität von BiVO4-II – BiVO4-V und photokatalytische Untersuchungen zum Abbau weiterer Farbstoffe.....65 4 Photokatalytische Untersuchungen an Bismut(III)-oxidschichten aus einem ultraschallgestützten Sprühverfahren.....72 4.1 Darstellungsmethoden für β-Bismut(III)-oxidschichten.....72 4.2 Darstellung, Modifizierung und photokatalytische Untersuchungen von α- und β- Bismut(III)-oxidschichten aus einem ultraschallgestützten Sprühverfahren.....76 4.2.1 Darstellung von α- und β-Bismut(III)-oxidschichten über ein ultraschallgestütztes Sprühverfahren ausgehend von [Bi38O45(OMc)24(DMSO)9]·2DMSO·7H2O und deren photokatalytische Untersuchung.....76 4.2.2 Modifizierung der Präparationsmethode und die photokatalytische Zersetzung von Schadstoffen mit optimierten β-Bismut(III)-oxidschichten.....84 4.2.3 Darstellung von Au/β-Bismut(III)-oxidschichten und deren photokatalytische Untersuchung.....94 4.3 Darstellung und photokatalytische Untersuchungen von α/β-Bismut(III)- oxidschichten aus einem ultraschallgestützten Sprühverfahren.....99 4.3.1 Darstellung von α/β-Bismut(III)-oxidschichten über ein ultraschallgestütztes Sprühverfahren ausgehend von [Bi38O45(OMc)24(DMSO)9]·2DMSO·7H2O.....99 4.3.2 Photokatalytische Untersuchungen an α/β-Bismut(III)-oxidschichten.....104 5 Zusammenfassung und Ausblick.....108 6 Experimenteller Teil.....116 6.1 Eingesetzte Chemikalien und Arbeitstechniken.....116 6.2 Verwendete Gerätetechnik.....116 6.3 Umsetzungen von Alkoxiden und Chloriden des Bismut(III) und Vanadium(V) mit und ohne Zusatz von Alkoholen.....122 6.3.1 Umsetzung von Bi(OtBu)3 und VO(OtBu)3 in Benzylalkohol unter Rückfluss (RF-I).....122 6.3.2 Umsetzung von BiCl3 und VOCl3 in Benzylalkohol unter Rückfluss (RF-II)..123 6.3.3 Umsetzung von Bi(OtBu)3 und VO(OtBu)3 in Benzylalkohol im Mikrowellenreaktor (MW-I).....123 6.3.4 Umsetzung von Bi(OtBu)3, VO(OtBu)3 und 2-Methoxybenzylalkohol im Mikrowellenreaktor (MW-II).....123 6.3.5 Umsetzung von Bi(OtBu)3, VO(OtBu)3 und 2,4-Dimethoxybenzylalkohol im Mikrowellenreaktor (MW-III).....124 6.3.6 Umsetzung von Bi(OtBu)3, VO(OtBu)3 und 2-(Thiophen-2-yl)propan-2-ol im Mikrowellenreaktor (MW-IV).....124 6.3.7 Umsetzung von Bi(OtBu)3 und VO(OtBu)3 im Mikrowellenreaktor (MW-V)...125 6.4 Darstellung von BiVO4 durch thermische Oxidation der Materialien MW-II – MW-V.....125 6.5 Darstellung der Bismut(III)-oxidschichten über ein ultraschallgestütztes Sprühverfahren.....126 6.5.1 β-Bi2O3-Schichten ausgehend von [Bi38O45(OMc)24(DMSO)9]·2DMSO·7H2O.....126 6.5.2 α-Bi2O3-Schichten ausgehend von [Bi38O45(OMc)24(DMSO)9]·2DMSO·7H2O.....127 6.5.3 Au/β-Bi2O3-Schichten ausgehend von β-Bi2O3-Schichten mittels Photodeposition.....127 6.5.4 α/β-Bi2O3-Schichten ausgehend von [Bi38O45(OMc)24(DMSO)9]·2DMSO·7H2O.....128 6.6 Photokatalytische Untersuchungen.....128 7 Literaturverzeichnis.....131 8 Anhang.....159 Curriculum Vitae.....177 Publikationsverzeichnis.....178 Tagungsbeiträge.....179 Selbstständigkeitserklärung.....181

The diploma thesis is confused to verify the applicability of selected physicochemical and spectroscopic methods for characterization of cyanobacteria, with special emphasis on possibilities of qualitative and quantitative analysis of polyhydroxyalkanoates (specifically polyhydroxybutyrate (PHB)) accumulated in cyanobacterial cells. The sample basis of the work was formed by cultures of cyanobacterial strains of Synechocystis sp. PCC 6803 and Synechocystis salina CCALA 192. The cultures were were cultivated in several ways to cover the widest possible range of physiological conditions and PHB contents, in particular using an autotrophic way of cultivation on shakers and multicultural culture method in a basic culture medium,and in media enriched with 2% salt (NaCl ) as well as mixotrophic culture media with different types of the carbon substrate. After few weeks of cultivation, cyanobacterial cultures were obtained and complexly analyzed by following techniques- cell suspensions were analyzed by flow cytometry and UV-VIS spectrometry (transmission and diffusion transmission mode), dry cell biomass was characterised by gas chromatography to obtain a exact amount of PHB, and then FT-IR spectrometry and thermogravimetric analysis. The work aimed to assess whether any of these methods can be a quick and affordable alternative to the determination of PHB content to the most commonly used method of gas chromatography, but also to assess what additional information about the physiological state of cyanobacterial cells can provide test methods. The highest correlation on PHB content was determined for the parameters determined by infrared spectroscopy, in which specific peaks from the characteristic wavelengths for polyhydroxybutyrate were important. Weak correlations on PHB content were achieved in thermogravimetric analysis and cytometry, using the hydrophobic fluorescent probe BODIPY 439/503, which bound to lipophilic parts of cells. In addition to the determination of PHB, it was possible to determine pigments present in cyanobacteria (such as chlorophyll, phycocyanin and carotenoids) by flow cytometry and UV-VIS diffusion transmission spectrometry. In the end, results from all used techniques were compared by PCA analysis to determine the similarity of all analyzed samples.