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A lithium-ion test cell for characterization of electrode materials and solid electrolyte interphaseGoel, Ekta, January 2008 (has links)
Thesis (M.S.)--Mississippi State University. Department of Chemistry. / Title from title screen. Includes bibliographical references.
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Spectroelectrochemical determination of the antioxidant properties of carpobrotus mellei and carpobrotus quadrifidus natural productsMaoela, Manki Sarah January 2009 (has links)
Philosophiae Doctor - PhD / South African Carpobrotus species have been found to contain hydrolysable tannins,various flavonoids e.g. rutin and hyperoside, phytosterols and aromatic acids which have a diverse range of pharmacological properties including antimicrobial and, antioxidant activities. The main aim of the thesis was to determine the natural products in C. mellei and C. quadrifidus using chromatographic techniques and electrochemical analysis. The antioxidant activity of both Carpobrotus species was determined by using a superoxide dismutase (SOD) biosensor. ESI-LC-MS was used to separate and determine flavonoids in C. mellei and C. quadrifidus. 8 flavonoid compounds: catechin, epicatechin, epicatechin-epicatechin, coumarylquinic acid, isorhamnetin, quercetin-hexose (hyperoside), rutin and myricetin-deoxyhexose were identified. Cyclic and square wave voltammetry were used to detect flavonoids from C. mellei and C. quadrifidus. Catechin was detected in the ethyl acetate extract of C. mellei and C. quadrifidus. The oxidation potential of the plant extracts were observed
at +150.6 mV to +1072.6 mV. The oxidation mechanism proceeds in sequential steps, related to the catechol moiety, -OH groups in C ring and the resorcinol group. The oxidation process of the catechol moiety involves a two electron - two proton reversible reaction and forms o-quinone. This occurs first at low potential and is a reversible reaction. The hydroxyl group in the C ring and resorcinol group oxidise there after and undergo an irreversible reaction. UV-vis and FTIR spectroscopy were used to confirm the presence of catechin in the ethyl acetate extract of both plants.UV-visible spectroelectrochemistry confirmed the oxidation process of catechin at constant potential. Since C. mellei and C. quadrifidus were confirmed to contain flavonoids by ESI-LC-MS and electrochemical analysis, the antioxidant activity was further investigated using a SOD biosensor. The superoxide dismutase (SOD) enzyme was immobilised with 1% Nafion on a platinum electrode. Detection limit and sensitivity of the SOD biosensor were found to be 0.03918 μmol L-1 and 1.44 μA(μmol L-1)-1, respectively. The results showed that C. mellei and C. quadrifidus have antioxidant activity, with relative antioxidant capacity (RAC) of 24% and 42%, respectively.
May 2009
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Evaluation and application of electroanalysis for the determination of antioxidantsRagubeer, Nasheen January 2007 (has links)
The role of antioxidants in the prevention of neurodegenerative diseases has been well documented. The use of synthetic antioxidants has decreased due to the ssociation of these compounds with certain cancers. Thus, the search for novel natural antioxidants has gained much focus in research. Most common methods of determining antioxidant capacity are the radical generated assays and biological assays such as lipid peroxidation and the nitroblue tetrazolium assay. Electrochemical methods have been proposed for the determination of bio-active compounds such as antioxidants. The electrochemical methods of cyclic voltammetry and square wave voltammetry were evaluated for the determination of antioxidant capacity initially examining known antioxidants and then using plant extracts of Sutherlandia frutescens as a case study. The antioxidant properties determined by electrochemical methods were validated utilising the non-biological methods of the DPPH, TEAC, ferrozine and FC assay and biological pharmacological methods. The results indicated that Sutherlandia frutescens contains potent antioxidant compounds that are able to reduce lipid peroxidation. The electrochemical techniques of square wave voltammetry and cyclic voltammetry were applied for the screening of a large number of extracts of various algae for the detection of antioxidant compounds. The results indicated that electrochemistry can be used as a preliminary method for the rapid screening of a large number of crude samples for antioxidant compounds. Electrochemical methods were also evaluated as a method for guiding the isolation and purification of antioxidant metabolites in Sargassum elegans. Solvent partitioning and fractionation of the marine alga allowed for the purification of antioxidant compounds. At each step of purification electrochemical methods were utilized to determine which fractions contained the more potent antioxidant compounds and thus guide further purification. The purified antioxidant compounds were elucidated using NMR to determine the structure of the antioxidant compounds.
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Spectroelectrochemical determination of the antioxidant properties of carpobrotus mellei and carpobrotus quadrifidus natural productsMaoela, Manki Sarah January 2009 (has links)
Philosophiae Doctor - PhD / South African Carpobrotus species have been found to contain hydrolysable tannins, various tlavonoids e.g. rutin and hyperoside, phytosterols and aromatic acids which have a diverse range of pharmacological properties including antimicrobial and, antioxidant activities. The main aim of the thesis was to determine the natural products in C. mellei and C. quadrifidus using chromatographic techniques and
electrochemical analysis. The antioxidant activity of both Carpobrotus species was determined by using a superoxide dismutase (SOD) biosensor. ESI-LC-MS was used to separate and determine tlavonoids in C. mellei and C. quadrifidus. 8 tlavonoid compounds: catechin, epicatechin, epicatechin-epicatechin, coumarylquinic acid, isorhamnetin, quercetin-hexose (hyperoside), rutin and myricetin-deoxyhexose were identified. Cyclic and square wave voltammetry were used to detect tlavonoids from C. mellei and C. quadrifidus. Catechin was detected in the ethyl acetate extract of C. mellei and C. quadrifidus. The oxidation potential of the plant extracts were observed at +150.6 mV to +1072.6 mV. The oxidation mechanism proceeds in sequential steps, related to the catechol moiety, -OH groups in C ring and the resorcinol group. The oxidation process of the catechol moiety involves a two electron - two proton reversible reaction and forms o-quinone. This occurs first at low potential and is a reversible reaction. The hydroxyl group in the C ring and resorcinol group oxidise there after and undergo an irreversible reaction. UV-vis and FTIR spectroscopy were used to confirm the presence of catechin in the ethyl acetate extract of both plants.
UV -visible spectroelectrochemistry confirmed the oxidation process of catechin at constant potential. Since C. mellei and C. quadrifidus were confirmed to contain flavonoids by ESI-LC-MS and electrochemical analysis, the antioxidant activity was further investigated using a SOD biosensor. The superoxide dismutase (SOD) enzyme was immobilised with 1% Nafion on a platinum electrode. Detection limit and
sensitivity of the SOD biosensor were found to be 0.03918 umol L-' and 1.44 !lA (umol i.'):', respectively. The results showed that C. mellei and C. quadrifidus have antioxidant activity, with relative antioxidant capacity (RAC) of 24% and 42%, respectively.
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A Portable Generator Incorporating Mini-Tubular Solid Oxide Fuel CellsHyde, Andrew Justin January 2008 (has links)
Modern society has become reliant on battery powered electronic devices such as cell phones and laptop computers. The standard way of recharging these devices is by connecting to a reticulated electricity supply. In situations with no electricity supply some other recharging method is required. Such a possibility is a small, portable, generator based on fuel cell technology, specifically mini-tubular solid oxide fuel cells (MT-SOFC). MT-SOFCs have been developed since the 1990s but there is limited analysis, discussion or research on developing and constructing a portable generator based on MT-SOFC technology. Such a generator, running on a portable gas supply, requires combining the key aspects of cell performance, a heating and fuel reforming system, and cell manifolds. Cell design, fuel type, fuel flow rate, current-collection method and operating temperature all greatly affected MT-SOFCs performance. Segmenting the cathode significantly increased the power output. Maximum power density from an electrolyte supported MT-SOFC was 140 mW/cm2. The partial oxidation reactor (POR) developed provided the required heat to maintain the MT-SOFCs at an operating temperature suitable for generating electricity. The exhaust gas from the POR was a suitable fuel for MT-SOFCs, having sufficient carbon monoxide and hydrogen to generate electricity. Various manifold materials were evaluated including solid metal blocks and folded sheet metal. It was found that manifolds made from easily worked alumina fibre board decreased the thermal stresses and therefore the fracture rate of the MT-SOFCs. The final prototype developed comprised a partial oxidation reactor and MT-SOFCs mounted in alumina fibre board manifolds within a well-insulated enclosure, which could be run on LPG. Calculated efficiency of the final prototype was 4%. If all the carbon monoxide and hydrogen produced by the partial oxidation reactor were converted to electrical energy, efficiency would increase to 39%. Under ideal conditions, efficiency would be 78%. Efficiency of the prototype can be improved by increasing the fuel and oxygen utilisation ratios, ensuring heat from the exhaust gases is transferred to the incoming gases, and improving the methods for collecting current at both the anode and cathode.
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Sn0.9In0.1P2O7-Based Organic/Inorganic Composite Membranes : Application to Intermediate-Temperature Fuel CellsHibino, Takashi, Tomita, Atsuko, Sano, Mitsuru, Kamiya, Toshio, Nagao, Masahiro, Heo, Pilwon January 2007 (has links)
No description available.
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[en] SYNTHESIS AND CHARACTERIZATION OF HYBRID SILICABASED NANOSTRUCTURES WITH IMMOBILIZED CARBOGENIC MATERIALS HAVING ENRICHED PI-ELECTRON SYSTEM AND THEIR ANALYTICAL APPLICATIONS / [pt] SÍNTESE E CARACTERIZAÇÃO DE NANOESTRUTURAS HÍBRIDAS BASEADAS EM SÍLICA COM MATERIAIS CARBOGÊNICOS IMOBILIZADOS TENDO SISTEMAS RICOS EM ELÉTRONS PI E SUAS APLICAÇÕES NA QUIMICA ANALÍTICAALBINA MIKHRALIIEVA 28 December 2020 (has links)
[pt] O objetivo da pesquisa foi dedicado à preparação de novos materiais híbridos à base de sílica contendo sistemas moleculares ou nanométricos de carbono com sistema de elétrons pi conjugados, imobilizados covalentemente para posterior aplicações como adsorventes e eletrodos para pré-concentração e determinação de compostos aromáticos. Deste modo, propôs-se o desenvolvimento das metodologias para as imobilizações covalentes de antraceno (Ant), pontos quânticos de óxido de grafeno (GOQDs) e nanopontos de carbono (CDs) na superfície da sílica (SiO2). Estes compostos são constituídos de sistemas conjugados de elétrons pi e, portanto, podem formar interação intramolecular de empilhamento pi–pi com compostos aromáticos. Nanocompósito de GOQDs imobilizados foi preparado através da interação covalente de fragmentos nanoméricos de óxido de grafeno (GO). Três tipos de SiO2-Ant foram obtidos através de abordagem de montagem da superfície pela reação de alquilação condensação de sílica modificada com grupos aminopropila. Estes materiais podem ter diferentes arranjos de ligantes de antraceno na superfície da sílica e, portanto, podem apresentar diferentes propriedades doadoras de elétrons-pi. Nanocompósitos de sílica gel com CDs imobilizados foram preparados por duas abordagens diferentes. Na primeira, os CDs foram obtidos a partir do ácido cítrico como material de partida e
posteriormente imobilizados em sílica. O segundo método consistiu no uso de sílica gel porosa como nanorreator para a preparação de CDs. Este método é simples e robusto, o qual permite um maior controle do tamanho e da composição do nanomaterial. Além disso, os efeitos da modificação da sílica, tamanho dos poros, tempo de síntese, estabilidade hidrolítica, tamanho das nanopartículas de carbono e rendimento quântico da fluorescência foram avaliados. Foi demonstrado que a carbonização do gel aminosilica com ácido cítrico incorporado resultou na formação de CDs não imobilizados e CDs imobilizados. Devido à forte fixação na superfície, os CDs podem ser facilmente purificados através de simples lavagem do nanocompósito com água. Os C-pontos preparados apresentaram fotoluminescência independente de
excitação a 445 nm com rendimento quântico até 80 porcento, o que os tornam atraentes para
aplicação bioanalítica. O nanocompósito imobilizado com GOQDs foi preparado por ligações covalentes dos fragmentos de GO em nanoescala. A composição da camada superficial de todos adsorventes foi determinada a partir de análises elementares e termogravimétricas, fotoelétrons de raios X, ressonância magnética nuclear no estado sólido, Raman, FTIR e espectroscopia de fluorescência. As propriedades texturais dos adsorventes foram determinadas, bem como a cinética de imobilização do ligante, o
grau de transformação da superfície e a estabilidade hidrolítica dos grupos enxertados, o efeito da porosidade da sílica no grau de conversão do ligante. As propriedades de adsorção dos materiais foram avaliados pela extração em fáse sólida nos modos dinâmico e estático para os compostos modelos azul de metileno e antraceno em várias fases móveis aquosas-orgânicas e orgânicas, na presença de componentes interferentes. Os nanomateriais obtidos apresentaram maior afinidade para compostos aromáticos do
que os cartuchos comerciais C18 para extração em fase sólida (SPE) de fases orgânicas móveis que permitem a separação em uma etapa dos hidrocarbonetos aromáticos policíclicos (PAHs) na matriz com alta concentração de ácidos graxos. Ademais, sílica gel com GOQDs imobilizados foi usado para análise eletroquímica de antibióticos e hormônios selecionados. O eletrodo demonstrou atividade eletrocatalítica em relação ao estriol (ET), dietilestilbestrol (DES), sulfametoxazol (SMZ) e trimetoprim (TMP) que possibilitaram determinar esses analitos com até 0.009 μmol L(-1) (ET). / [en] The objective of the present research was devoted to the preparation of new silica-based hybrid materials having covalently immobilized carbon-containing molecular and nanometric systems with delocalized pi-electrons that can be used as adsorbents and electrodes for preconcentration and determination of aromatic compounds. For this purpose, methodologies for covalent immobilization of anthracene (Ant), graphene oxide quantum dotes (GOQDs) and carbon nanodots (CDs) on silica surface (SiO2) have been developed. These compounds have a conjugated system of pi-electrons and thus can form intramolecular pi–pi stacking interaction with aromatic compounds. The nanocomposite with immobilized GOQDs was prepared by covalent immobilization of nanoscale graphene oxide (GO) fragments. Three sets of
SiO2-Ant were obtained using reaction surface assembling reactions by alkylation and condensation of silica with immobilized primary amines. These materials can have different arrangements of anthracene ligands on silica surface and so pi-donor properties. Silica gel nanocomposites with immobilized CDs were prepared by two different approaches. For the first one, the CDs were obtained from the molecular precursor and then immobilized on silica. For the second method, CDs were prepared by nanoreactor approach directly in silica gel pores. The second method is facile and robust and also allows better control of the particle size and composition. The effects of silica gel modification, pore size, synthesis time, hydrolytic stability, carbon
nanoparticle size and quantum yield of the fluorescence were studied. It was demonstrated that the carbonization of aminosilica gel with embedded citric acid resulted in the formation of unbound CDs and immobilized CDs. Due to firm attachment to the surface CDs can be easily separated from low-molecular-weight impurities and CDs by simple rinsing of the nanocomposite with water. As prepared CDs demonstrate excitation-independent photoluminescence at 445 nm with quantum yield up to 80 percent that makes them attractive for bioanalytical application. The composition of the surface layer of the adsorbents was determined from elemental and thermogravimetric analysis, X-ray photoelectron, solid nuclear magnetic resonance, Raman, FTIR, and fluorescent spectroscopy. The textural properties of the adsorbents were determined as well as ligand immobilization kinetics, the degree of surface
transformation and hydrolytic stability of the grafted groups, the effect of silica porosity on ligand conversion degree. The adsorption properties of the materials were studied in dynamic and static solid-phase extraction (SPE) modes for the model compounds methylene blue and anthracene in various aqueous-organic and organic mobile phases, in the presence of interfering components. It was demonstrated that studied materials have a higher affinity towards aromatic compounds than commercial
C18 SPE cartridges in organic mobile phases that allow one-step separation of polycyclic aromatic hydrocarbons in the matrix with a high concentration of fatty acids. Also, silica-immobilized GOQDs was used for electrochemical analysis of selected antibiotics and hormones. The electrode demonstrated electrocatalytic activity towards estriol (ET), diethylstilbestrol (DES), sulfamethoxazole (SMZ), and trimethoprim (TMP) that made it possible to determine these analytes with up to 9 nmol L(-1) (ET).
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Calculation of electrical conductivity and electrothermal analysis of multilayered carbon reinforced composites: application to damage detection / Προσδιορισμός της ηλεκτρικής αγωγιμότητας και ηλεκτροθερμική ανάλυση ανισότροπων πολύστρωτων υλικών ενισχυμένων με ίνες άνθρακα: εφαρμογή στην ανίχνευση βλάβης σε κατασκευές από σύνθετα υλικάΑθανασόπουλος, Νικόλαος 09 July 2013 (has links)
During this thesis, it has been proved that the electrical conductivity of multilayered and electrically anisotropic carbon fiber materials can be expressed by an equivalent second order tensor, which is equal to sum of each layer’s electrical conductivity tensor. The aforementioned equivalent electrical conductivity tensor is valid assuming that the material’s thickness is negligible compared to the other dimensions of the body. The mathematical expression for the prediction of the electrical conductivity of a multilayered material for any stacking sequence, is based on the electric current conservation, and was validated using different methods. Each layer’s electrical conductivity was experimentally studied at the two principal directions. Transverse to the fibers’ direction, an empirical model was developed for the prediction of the electrical conductivity as a function of the layer’s thickness, of the fibre volume fraction and of temperature. All cases involved the study of multidirectional and unidirectional carbon fiber materials without the presence of matrix (porous form – CF preform) as well as in the presence of polymeric matrix (CFRP).
The validation of the equivalent tensor was achieved through three different ways: a) through the measurement of the electric resistance, for various stacking sequences, b) through the Joule heating effect, by recording and comparing the developing temperature field to the respective numerically calculated, c) through 3D numerical models which approximate the analytical solution of the 2D domain problem. Moreover using the finite difference method, certain electrothermal models were developed in order to study the temperature field for different stacking sequences. The electrical problem can be expressed by an elliptic PDE, for the case where the material is electrically anisotropic and homogeneous, or non-homogeneous. On the other hand, the transient heat transfer problem involves the case where the material is thermally anisotropic and homogeneous. Using the equivalent tensor, the 3D domain problem is simplified to a 2D domain problem resulting in less computational requirements for the solution of the problem.
The present research study could be used in a plethora of application, such as the development of carbon fibre reinforced heating elements (direct heating CFRP molds) as well as damage detection in multidirectional composite materials with electrical conductive
reinforcement. / Κατά τη διάρκεια της παρούσας διδακτορική διατριβής, αποδείχθηκε ότι η ηλεκτρική αγωγιμότητα των πολύστρωτων και ηλεκτρικά ανισότροπων υλικών με ίνες άνθρακα, μπορεί να εκφραστεί από έναν ισοδύναμο τανυστή δεύτερης τάξης, ο οποίος είναι το άθροισμα των τανυστών κάθε στρώσης. Ο ισοδύναμος τανυστής ισχύει υποθέτοντας ότι το πάχος συγκριτικά με τις υπόλοιπες διαστάσεις του υλικού είναι πολύ μικρό. Η μαθηματική έκφραση με την οποία μπορεί να προβλεφθεί η ηλεκτρική αγωγιμότητα ενός πολύστρωτου υλικού για οποιαδήποτε αλληλουχία στρώσεων αποδείχτηκε με συστηματικό τρόπο και βασίζεται στην αρχή διατήρησης του ηλεκτρικού φορτίου. Η ηλεκτρική αγωγιμότητα κάθε στρώσης μελετήθηκε πειραματικά στις δύο κύριες διευθύνσεις. Κάθετα στη διεύθυνση των ινών αναπτύχθηκε ένα εμπειρικό μοντέλο πρόβλεψης της ηλεκτρικής αγωγιμότητας συναρτήσει του πάχους της στρώσης, της περιεκτικότητας σε ίνες άνθρακα και της θερμοκρασίας. Σε όλες τις περιπτώσεις μελετήθηκαν πολύστρωτα υλικά ινών άνθρακα χωρίς μήτρα (πορώδης μορφή-CF preforms) και με πολυμερική μήτρα (CFRPs).
Η επιβεβαίωση της εγκυρότητας του ισοδύναμου τανυστή έγινε με τρεις διαφορετικούς τρόπους: α) μέσω μετρήσεων της ηλεκτρικής αντίστασης, για διαφορετικές αλληλουχίες στρώσεων, β) μέσω του φαινομένου Joule, καταγράφοντας και συγκρίνοντας το αναπτυσσόμενο θερμοκρασιακό πεδίο με το θερμοκρασιακό πεδίο που υπολογίζεται αριθμητικά, γ) μέσω τρισδιάστατων αριθμητικών μοντέλων όπου τείνουν στην αναλυτική λύση του δισδιάστατου προβλήματος.
Στη συνέχεια αναπτύχτηκαν ηλεκτροθερμικά μοντέλα με τη μέθοδο των πεπερασμένων διαφορών με σκοπό τη μελέτη του θερμοκρασιακού πεδίου για διαφορετικές αλληλουχίες στρώσεων. Το ηλεκτρικό πρόβλημα εκφράζεται από μία ελλειπτική διαφορική εξίσωση όπου το υλικό είναι ηλεκτρικά ανισότροπο και ομογενές ή μη ομογενές ενώ το θερμικό πρόβλημα είναι θερμικά ανισότροπο και ομογενές. Χρησιμοποιώντας τον ισοδύναμο τανυστή το τρισδιάστατο πρόβλημα μετατρέπεται σε ένα δισδιάστατο πρόβλημα με αποτέλεσμα να απαιτούνται λιγότεροι πόροι για την επίλυση του προβλήματος.
Η συγκεκριμένη εργασία μπορεί να χρησιμοποιηθεί σε μία πληθώρα εφαρμογών όπως στην ανάπτυξη και στη λειτουργία θερμαινόμενων στοιχείων ενισχυμένων με ίνες άνθρακα (καλούπια όπου το θερμαντικό στοιχείο το αποτελούν οι ίνες άνθρακα) αλλά και στην ανίχνευση βλάβης συνθέτων υλικών με αγώγιμη ενίσχυση.
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Desenvolvimento de um sistema para medição do espectro de impedância em fluidos / Development of a system for measuring the impedance spectrum in fluidsPrzysiada, Felipe Augusto 23 November 2017 (has links)
A necessidade de monitoramento do comportamento de substâncias é fundamental em diversas áreas de da indústria atual, como por exemplo, a análise de produções provenientes de reações químicas ou a investigação de escoamentos com múltiplos componentes, como é o caso do sistema de extração de petróleo. A espectroscopia de impedância, onde a impedância elétrica de uma substancia é analisada em diversas frequências, é uma técnica candidata e tem seu uso difundido principalmente em laboratórios voltados para pesquisas na área de química analítica. No entanto, ainda é uma técnica pouco aplicada para monitoração em processos industriais. Este trabalho objetiva o desenvolvimento de um sistema simples e de baixo custo de espectroscopia de impedância contendo uma possível forma de aplicação em atividades industriais. Inicialmente foram revisadas diversas técnicas para obtenção do espectro de impedância. Para a implementação, optou-se pela utilização do sinal de multifrequência chirp para excitação na faixa de 1 Hz a 495 kHz e do circuito amplificador de transimpedância para recepção dos sinais de respostas. Além disso, foram utilizadas duas variações de sensores para uma investigação mais abrangente do funcionamento do sistema. O sistema desenvolvido é composto por um software de recepção de dados no computador, conectado diretamente a um sistema de medição microcontrolado, encarregado pela geração amostragem dos sinais do sensor. Para validação do sistema, realizaram-se medidas com resistores e capacitores de referência assim como o sistema foi testado com diversas substâncias conhecidas, tais como ar, água deionizada, óleo de silicone, isopropanol e etilenoglicol. Em comparação com valores teóricos, os resultados do sistema se mostraram apropriados para que seja possível identificar diferentes substâncias, por meio da medição da resposta em frequência da impedância das mesmas. Como exemplo de aplicação, o sistema foi utilizado para monitoração do processo de formação de gelo, onde pode-se constatar a transição de água líquida para gelo. Desta forma, o sistema pode ser aplicado em trabalhos futuros para monitoração outros processos. / The need to monitor the behavior of substances is fundamental in several areas of the industry, such as the analysis of reactions in chemical reactors or the investigation of flows with multiple components, such as in the oil and gas extraction. Impedance spectroscopy, where the electrical impedance of a substance is analyzed at different frequencies, is a candidate technique and its use is spread mainly in laboratories focused on research in the area of analytical chemistry. However, this technique is still only limitedly applied for monitoring industrial processes. Hence, this work aims at the development of a simple and low-cost system based on impedance spectroscopy with possible applications in industrial activities. Initially several techniques for obtaining the impedance spectrum were reviewed. For the implementation, we opted for the use of the chirp multifrequency signal in the range of 1 Hz to 495 kHz for excitation and the transimpedance amplifier circuit for receiving the signals of substances. In addition, two sensor variations were used for a more comprehensive investigation of the system operation. The developed system consists of data reception software on the computer, connected directly to a microcontrolled sensing electronics, in charge of the generation and sampling of the signals from the sensor. To validate the system, measurements were made with reference impedance (resistors and capacitors) as well as the system was applied to measure various known substances, such as air, water, silicon oil and isopropanol. In comparison with theoretical values, the results of the system proved to be appropriate for the identification of different substances by measuring the frequency response of the impedance. As an example of application, the system was applied to monitor the ice formation process, where was possible to verified the transition from liquid to ice water. In this way, the system can be applied in future work to monitor other processes.
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Desenvolvimento de um sistema para medição do espectro de impedância em fluidos / Development of a system for measuring the impedance spectrum in fluidsPrzysiada, Felipe Augusto 23 November 2017 (has links)
A necessidade de monitoramento do comportamento de substâncias é fundamental em diversas áreas de da indústria atual, como por exemplo, a análise de produções provenientes de reações químicas ou a investigação de escoamentos com múltiplos componentes, como é o caso do sistema de extração de petróleo. A espectroscopia de impedância, onde a impedância elétrica de uma substancia é analisada em diversas frequências, é uma técnica candidata e tem seu uso difundido principalmente em laboratórios voltados para pesquisas na área de química analítica. No entanto, ainda é uma técnica pouco aplicada para monitoração em processos industriais. Este trabalho objetiva o desenvolvimento de um sistema simples e de baixo custo de espectroscopia de impedância contendo uma possível forma de aplicação em atividades industriais. Inicialmente foram revisadas diversas técnicas para obtenção do espectro de impedância. Para a implementação, optou-se pela utilização do sinal de multifrequência chirp para excitação na faixa de 1 Hz a 495 kHz e do circuito amplificador de transimpedância para recepção dos sinais de respostas. Além disso, foram utilizadas duas variações de sensores para uma investigação mais abrangente do funcionamento do sistema. O sistema desenvolvido é composto por um software de recepção de dados no computador, conectado diretamente a um sistema de medição microcontrolado, encarregado pela geração amostragem dos sinais do sensor. Para validação do sistema, realizaram-se medidas com resistores e capacitores de referência assim como o sistema foi testado com diversas substâncias conhecidas, tais como ar, água deionizada, óleo de silicone, isopropanol e etilenoglicol. Em comparação com valores teóricos, os resultados do sistema se mostraram apropriados para que seja possível identificar diferentes substâncias, por meio da medição da resposta em frequência da impedância das mesmas. Como exemplo de aplicação, o sistema foi utilizado para monitoração do processo de formação de gelo, onde pode-se constatar a transição de água líquida para gelo. Desta forma, o sistema pode ser aplicado em trabalhos futuros para monitoração outros processos. / The need to monitor the behavior of substances is fundamental in several areas of the industry, such as the analysis of reactions in chemical reactors or the investigation of flows with multiple components, such as in the oil and gas extraction. Impedance spectroscopy, where the electrical impedance of a substance is analyzed at different frequencies, is a candidate technique and its use is spread mainly in laboratories focused on research in the area of analytical chemistry. However, this technique is still only limitedly applied for monitoring industrial processes. Hence, this work aims at the development of a simple and low-cost system based on impedance spectroscopy with possible applications in industrial activities. Initially several techniques for obtaining the impedance spectrum were reviewed. For the implementation, we opted for the use of the chirp multifrequency signal in the range of 1 Hz to 495 kHz for excitation and the transimpedance amplifier circuit for receiving the signals of substances. In addition, two sensor variations were used for a more comprehensive investigation of the system operation. The developed system consists of data reception software on the computer, connected directly to a microcontrolled sensing electronics, in charge of the generation and sampling of the signals from the sensor. To validate the system, measurements were made with reference impedance (resistors and capacitors) as well as the system was applied to measure various known substances, such as air, water, silicon oil and isopropanol. In comparison with theoretical values, the results of the system proved to be appropriate for the identification of different substances by measuring the frequency response of the impedance. As an example of application, the system was applied to monitor the ice formation process, where was possible to verified the transition from liquid to ice water. In this way, the system can be applied in future work to monitor other processes.
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