A duloxetina (DLX) é um duplo inibidor seletivo balanceado da recaptação de serotonina e norepinefrina empregado para o tratamento do transtorno depressivo maior e para o manejo da dor neuropática diabética periférica. O objetivo deste estudo foi desenvolver e validar métodos analíticos para determinação de DLX em cápsulas e realizar estudos da estabilidade do fármaco. A substância usada como padrão de referência nas análises foi caracterizada por espectroscopia no infravermelho, ressonância magnética nuclear (RMN), calorimetria diferencial de varredura e espectrometria de massas. As análises qualitativas foram realizadas por cromatografia em camada delgada (CCD), espectrofotometria na região do ultravioleta (UV) e cromatografia líquida de alta eficiência (CLAE) permitindo a identificação do fármaco no produto farmacêutico. A espectrofotometria UV, CLAE e voltametria de redissolução catódica (CSV) foram validadas para determinação quantitativa de DLX em cápsulas. Estes métodos propostos foram específicos, robustos, lineares, precisos e exatos para determinação de DLX em microgrânulos de revestimento entérico. Estudos preliminares da estabilidade da DLX durante o desenvolvimento do método indicativo de estabilidade por CLAE demonstraram que o fármaco foi rapidamente degradado em meio ácido, na presença de peróxido de hidrogênio e de radiação a luz UVC, enquanto que este foi mais estável em meio alcalino. A cinética de degradação descreveu as mudanças na concentração da DLX em condição ácida e sob fotodegradação. A degradação ácida da DLX, em solução de HCl 0,1 M, mostrou cinética aparente de zero ordem e a fotodegradação demonstrou uma cinética aparente de primeira ordem. O produto de degradação principal observado na hidrólise ácida (PDA-14) foi analisado e isolado por CCD preparativa. Espectros de RMN-1H, RMN-13C e COSY foram avaliados e a estrutura do PDA-14 foi confirmada como 1-naftol. Esta substância produz efeitos citotóxicos e consequentemente o produto farmacêutico é uma cápsula de gelatina contendo microgrânulos com revestimento entérico para evitar a degradação ácida da DLX no estômago. / The duloxetine (DLX) is a double balanced selective serotonin and norepinephrinereuptake inhibitor employed for the treatment of major depressive disorder and for the management of diabetic peripheral neuropathic pain. The aim of this study was to develop and validate analytical methods to the determination of DLX in capsules and accomplish studies of this drug stability. The substance used as reference standard in the analysis was characterized by infrared spectroscopy, nuclear magnetic resonance (NMR), differential scanning calorimetry, and mass spectrometry. The qualitative analyses were performed by thin layer chromatography (TLC), ultraviolet spectrophotometry (UV), and high performance liquid chromatography (HPLC) allowing the identification of the drug in pharmaceutical dosage form. The UV spectrophotometry, HPLC, and cathodic stripping voltammetry (CSV) were validated for quantitative determination of the DLX in capsules. These proposed methods were specific, robust, linear, precise, and accurate to the determination of DLX in entericcoated pellets. Preliminary studies of DLX stability during the development of stability-indicating HPLC method demonstrated that the drug was rapidly degraded in acid medium, in the presence of hydrogen peroxide and light UVC radiation, while it was more stable in alkali medium. The kinetics of degradation described the concentration changes of DLX in acid condition and on photodegradation. The acid degradation of DLX in 0.1M HCl solution showed apparent zero-order kinetics and the photodegradation demonstrated apparent first-order kinetics. The main degradation product observed in acid hydrolysis (DP-14) was analyzed and isolated by TLC preparative. 1H NMR, 13C NMR and COSY spectra were evaluated and the structure of DP-14 was confirmed as 1-naphthol. This substance produces cytotoxic effects and consequently the finished pharmaceutical dosage form is a gelatin capsule containing enteric-coated pellets to avoid the acid degradation of DLX in the stomach.

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No description available.

Solid phase extraction is one of the most widely used methods to concentrate diluted compounds in a solution. Substances can be extracted into admicelles and hemimicelles, which are surface adsorbed micelles and surfactant monolayers, respectively. Investigations of the electrical control of surfactants on surfaces for the purpose of analyte preconcentration prior to chromatographic analysis are presented. The surfactant layer serves as the “stationary phase” in a solid phase extraction sorbent scenario. Analytes are adsorbed on this layer, and then released from the solid phase via surfactant removal. The attachment and removal of the surfactant are controlled by means of an electric field. Because the surfactant-analyte association is released by electrical control, organic solvents, which are used in conventional solid phase extraction, are not required. Therefore, this procedure is advantageous for method development and environmental concerns. Presented is the preconcentration of a test probe, 2-naphthol, using electrical control of the formation and release of dodecyl sulfate on planar gold, gold coated stainless steel, and a porous stainless steel frit, using impedance spectroscopy to observe the layer formation with various surfactant concentrations and applied potentials.

Dans le cadre de l'élimination de composés réfractaires contenu dans une matrice complexe, les procédés d'oxydation avancée s'avèrent être une technologie de choix. Cette étude est donc consacrée à la sonolyse et à la photolyse de deux xénobiotiques organiques, le naphthol blue black (un colorant hydrophile, noté NBB) et le nonylphénol (un détergent, hydrophobe et volatil, noté NP), seuls ou en compétition. L'efficacité de la technique ultrasonore de haute fréquence (278 kHz) a été testée sur les molécules cibles et leur mélange. La décoloration du NBB est effective après 180 min de traitement et s'accompagne d'une minéralisation de 23% alors que le NP se dégrade après 120 min. L'effet des paramètres a été étudié, tels que la puissance ultrasonore, la concentration du substrat, le pH, les ions inorganiques (bicarbonates et phosphates) et la compétition. Ainsi dans le mélange, la présence du NBB n'a pas d'influence sur la disparition sur NP tandis que la décoloration du NBB est affectée par la présence du NP. Cependant, la présence des ions bicarbonates dans le mélange permet par l'intermédiaire des radicaux carbonates de contrebalancer l'effet inhibiteur du NP. L'utilisation de la photolyse directe a fait l'objet de la deuxième partie de ce travail, ce qui a permis de faire une étude comparative des deux techniques. Il a été montré que la sonochimie, fort de sa capacité à produire abondamment les radicaux HO•, est plus adaptée au traitement des effluents relativement plus concentrés. De plus, la sonochimie permet de mettre en valeur les ions inorganiques, constituants naturels de l'eau pour minimiser l'effet inhibiteur de la matrice. Ensuite, l'efficacité de certains Procédés d'Oxydation Avancée (POA) sur l'élimination des xénobiotiques sus-mentionnés a été testée et les résultats obtenus ont donné lieu à l'ordre suivant : UV < UV/H2O2 < Fe2+/H2O2 < UV/Fe2+/H2O2. / Within the framework of the destruction of refractory organics contained in a complex aqueous matrix, the advanced oxidation processes appear to be a first class technology. So this survey is dedicated to the sonolysis and the photolysis of two organics, namely the naphthol blue black (an acid azo-dye, hydrophilic, noted NBB) and the nonylphenol (a detergent, hydrophobic et volatile, noted NP), single or in competition. High frequency (278 kHz) ultrasound is found to be efficient. NBB decolorization is effective within 180 min and its mineralization reaches 23% while NP is degraded for 120 min. Different parameters were studied, such as ultrasound power, substrate concentration, pH, inorganic ions (bicarbonate and phosphate), and competition. In the NBB/NP mixture, NBB has no influence on the NP degradation whereas NP has a strong effect on the NBB decolorization. Nevertheless, the presence of bicarbonate ions in the mixture reduces the negative effect of NP, thanks to the formation of carbonates radicals. Direct photolysis is the topic of the second part of this study, so as to make a comparison of these two oxidative techniques. It was emphasizes that sonolysis is most adapted for the treatment of more concentrated pollutant, because of the intense production of HO• radicals. Moreover sonolysis is relevant when inorganic ions are present in the mixture, in order to minimize the competition between organics. Then the efficiency of different AOP was tested for the two target pollutants; results can be organized according the following: UV < UV/H2O2 < Fe2+/H2O2 < UV/Fe2+/H2O2.

O poli(5-amino 1-naftol) é um polímero que pertence à classe dos polímeros condutores e pode ser obtido através da oxidação do monômero bifuncionalizado, 5-amino 1-naftol, que possui dois grupos funcionais: -NH2 e -OH. Neste trabalho é apresentado um estudo dos polímeros provenientes do referido monômero quando polimerizado na presença de diferentes ácidos. As influências do meio eletrolítico na eletrodeposição, na morfologia e nos processos redox dos filmes, são estudadas. As transformações eletrocrômicas, conseqüência dos diferentes estados de oxidação dos filmes, são acompanhadas por experimentos espectroeletroquímicos na região do visível. É realizado um completo estudo espectroscópico, utilizando técnicas in situ e ex situ como Raman Ressonante, Infravermelho e Espectroscopia Fotoeletrônica de Raios-X, que permite a elucidação das distintas estruturas formadas durante a polimerização e a identificação das espécies encontradas nos diferentes estados de oxidação do filme. São também realizados testes para verificar a potencial aplicação do poli(5-amino 1-naftol) como componente na construção de biossensores, fazendo uso do grupamento funcional -OH que não participa do processo de polimerização e permanece livre na cadeia polimérica. / Poly(5-amino 1-naphthol) (poly(5-NH2 1-NAP)) is a polymer that belongs to the conducting polymer class obtained by the oxidation of a bifunctional monomer, 5-amino 1-naphthol, which presents two bifunctional groups: -NH2 e -OH. In this work it is showed a study about polimerization of 5-amino 1-naphthol and their polymer formed in different electrolytic acid medium. Influences of the electrolyte in the electrodeposition, morfology and the redox process are studied. Electrochromic transformations that appear as consequences of different films oxidation states are followed by spectroelectrochemical experiments in the visible range. An entire spectrocopic study using ex situ and in situ techniques as Resonante Raman Spectroscopy, Infrared Spectroscopy and X-Ray Photoelectron Spectroscopy is carried out. It allows the elucidation of distint structures formed during the polimerization and the identification of species in different oxidation states. Experiments are also carried out in order to verify the potential aplication of poly(5-amino 1-naphthol) as biosensor component. Poly(5amino 1-naphthol) is a candidate as polymeric matrix beca use of the -OH groups doesnt take part in the polymerization process and it remais free in the polymeric chain.

Neste trabalho, foram desenvolvidos sensores eletroquímicos para a detecção amperométrica do óxido nítrico (NO) fundamentada na aplicação da ftalocianina tetrasulfonada de níquel (NiTsPc) e do poli(5-amino 1-naftol) (poli(5-NH2 1-NAP)). NiTsPc foi eletrodepositada por voltametria cíclica sobre o eletrodo de platina e caracterizada eletroquimicamente em diferentes pHs. A detecção amperométrica de NO foi bastante sensível, mas o eletrodo não apresenta seletividade suficiente, motivo pelo qual este material foi substituído pelo poli(5-NH2 1-NAP) modificado com citocromo c. A imobilização foi caracterizada por voltametria cíclica e microbalança a cristal de quartzo. As detecções amperométricas do NO foram efetuadas aplicando o potencial em -0,6 V e foi observado que a variação da corrente devido à adição do NO ocorreu somente no segundo dia após a imobilização da proteína, o que pode estar relacionado a mudanças de estrutura do citcocromo c covalentemente ligado. O poli(5-NH2 1-NAP) foi também eletropolimerizado sobre nanotubos de carbono, obtendo assim um eletrodo nanoestruturado e o citocromo c foi imobilizado nessa estrutura. Assim como para os eletrodos maciços, ele não respondeu ao NO logo após a imobilização do citocromo c, respondendo somente no segundo dia e apresentou um melhor desempenho devido a sua maior área superficial. / In this work, electrochemical sensors for nitric oxide (NO) amperometric detection were prepared. For this purpose nickel tetrasulfonated phthalocyanine (NiTsPc) and poly(5-amino 1-naphthol) (poly(5-NH2 1-NAP)) modified with cytochrome c were applied. NiTsPc was electropolymerized by cyclic voltammery at platinum electrode and were electrochemically characterized in differents pHs. NO amperometric detections were very sensitive, but the electrode does not present satisfactory selectivity, and because of this, the material was replaced by poly(5-NH2 1-NAP) modified with cytochrome c. The immobilization was characterized by cyclic voltammetry and electrochemical crystal microbalance. NO amperometric detection has been carried out by applying -0.6 V and it was observed that the current due the NO sensing was only observed at the second day after protein immobilization. This can be related with cytochrome c structural change. For nanostructuring the surface of Poly(5-NH2 1-NAP) it was electropolymerized on carbon nanotubes felt electrodes and cytochrome c was immobilized. As well as the bulk electrode, the nanostructured one did not sense NO immediately after the cytochrome c immobilization, being possible to observe current only after the second day displaying a much better performance due to its high superficial area.

Η απορρύπανση των υδάτων αποτελεί αναγκαία και καθιερωμένη από δεκαετίες πρακτική. Η απορρύπανση με τη μέθοδο της ρόφησης είναι μία από την πληθώρα των τεχνικών που εφαρμόζονται. Το περισσότερο διαδεδομένο ροφητικό υλικό είναι ο ενεργός άνθρακας, του οποίου όμως το υψηλό κόστος παραγωγής, οδήγησε την επιστημονική έρευνα στην αναζήτηση εναλλακτικών, υλικών χαμηλότερου κόστους. Για το σκοπό αυτό, το επιστημονικό ενδιαφέρον έχει στραφεί σε πολλά υλικά κυρίως οργανικής προέλευσης, αλλά και σε ανόργανα υλικά, όπως τα οξείδια των μετάλλων, τα οποία αφθονούν στη φύση. Στην παρουσα εργασία έγινε μελέτη της ροφητικής ικανότητας φυσικών οξειδίων, για τη ρόφηση αρωματικών οργανικών ενώσεων και βαρέων μετάλλων. Πιο συγκεκριμένα, μελετήθηκε ο μηχανισμός της ρόφησης του φαινανθρενίου, της 2-ναφθόλης και του υδραργύρου από οξείδια αργιλίου, τιτανίου, αργιλίου/πυριτίου και σιδήρου, με σκοπό την αξιολόγηση των υλικών αυτών ως ροφητικών υλικών και τη σύγκριση των αποτελεσμάτων με αυτά της ρόφησης των αντίστοιχων ρύπων από υλικά που παρασκευάζονται από την πυρόλυση πρώτης ύλης βιολογικής προέλευσης. Για τη μελέτη της κινητικής της ρόφησης του φαινανθρενίου και της 2-ναφθόλης πραγματοποιήθηκαν πειράματα σε θερμοκρασία περιβάλλοντος, σε θαλασσινό και γλυκό συνθετικό νερό, με διαφορετικές ποσότητες ροφητικού υλικού (χωρίς χημική επεξεργασία) και για διαφορετικό χρόνο επαφής. Από τα πειράματα αυτά μετρήθηκε η κινητική της ρόφησης καθώς και το ποσοστό απομάκρυνσης των ρύπων από το διάλυμα. Από τις μετρήσεις που έγιναν, προέκυψε ότι το ποσοστό απομάκρυνσης του φαινανθρενίου από το διάλυμα αυξάνεται αυξανομένης της ποσότητας του ροφητικού υλικού. Η σταθερά της ρόφησης Kd, κυμάνθηκε σε ένα εύρος τιμών από 1 έως 10 L/Kg, τιμές 2 έως 4 τάξεις μεγέθους μικρότερες από αυτές άλλων ροφητικών υλικών βιολογικής προέλευσης, ή προϊόντων πυρόλυσης. Τη μεγαλύτερη ικανότητα ρόφησης φαινανθρενίου επέδειξε η γ-αλούμινα με ειδική επιφάνεια 270 m2/g, με μέγιστη απομάκρυνση φαινανθρενίου το 55 % της αρχικής συγκέντρωσης έπειτα από 8 ημέρες, ενώ τη μικρότερη ικανότητα ρόφησης η γ-αλούμινα με ειδική επιφάνεια 120 m2/g, με μέγιστη απομάκρυνση το 14 % της αρχικής συγκέντρωσης, έπειτα από 10 ημέρες. Η τιτάνια, με ειδική επιφάνεια 120 m2/g, είχε ως αποτέλεσμα την απομάκρυνση του 52 % της αρχικής συγκέντρωσης φαινανθρενίου, σε 8 ημέρες. Από τα πειράματα ρόφησης της 2-ναφθόλης από την γ-αλούμινα, δεν προέκυψε μετρήσιμη ρόφηση. Η ρόφηση του υδραργύρου από την γ-αλούμινα (ειδική επιφάνεια 131 m2/g), και τα οξείδια σιδήρου μελετήθηκε με πειράματα στους 25 °C, σε pH 5 και με χρόνο εξισορρόπησης τις 24 h. Από τα πειράματα προέκυψε ισόθερμη καμπύλη και έγινε προσπάθεια προσαρμογής της σε μοντέλα ρόφησης. Παρατηρήθηκε αύξηση του ποσοστού απομάκρυνσης του υδραργύρου, με αύξηση της μάζας της γ-αλούμινας. Το μέγιστο ποσοστό απομάκρυνσης, ήταν το 93 % της αρχικής συγκέντρωσης και επιτεύχθηκε με μάζα γ-αλούμινας ίση και μεγαλύτερη από 1 g. Για τιμή Ce=15 mg/L, μετρήθηκε qe=0,91 mg/g, τιμή 1 έως 2 τάξεις μεγέθους μικρότερη από αυτές άλλων ροφητικών υλικών βιολογικής προέλευσης ή προϊόντων πυρόλυσης. Τα οξείδια σιδήρου, παρότι είχαν ειδική επιφάνεια 55 m²/g, δεν παρουσίασαν μετρήσιμη ροφητική ικανότητα για κανέναν από τους ρύπους, που μελετήθηκαν στην παρούσα εργασία. Συνοψίζοντας μπορούμε να πούμε ότι τα ανόργανα υλικά που μελετήθηκαν στην παρούσα εργασία, παρόλο που παρουσιάζουν μεγάλες τιμές ειδικής επιφάνειας, δεν μπορούν να χαρακτηρισθούν ως αξιόλογα ροφητικά υλικά, τόσο για τη ρόφηση των οργανικών ρύπων φαινανθρένιο και 2-ναφθόλη, όσο και για τη ρόφηση του υδραργύρου. / Water treatment is a necessary and standard practice since decades. Adsorption technology in water treatment is one of many techniques being used. Activated carbon is the most widely applied adsorbent in water treatment, however its high production cost has led scientific research to investigate alternative low cost sorbent materials. This need has developed scientific interest towards novel materials most of them derived from biomass, but also inorganic oxides that are abundant in nature. The present study focuses on the investigation of the capacity of natural oxides to adsorb aromatic organic compounds and heavy metals. Specifically, sorption of phenanthrene, 2-naphthol and mercury onto aluminum, titanium, silicon and ferric oxides was examined, for the evaluation of these materials as sorbents, compared to pyrolized biomaterials. For the study of sorption of phenanthrene and 2-naphthol, batch experiments were conducted at room temperature, using artificial seawater and fresh water, different mass of sorbent material at different contact time. Sorption kinetics and the pollutant removal percentages were determined. The proportion of phenanthrene removal increased with the increase of the mass of the sorbent material. Sorption distribution coefficient Kd ranged between 1 and 10 L/Kg. These values are 2 to 4 orders of magnitude lower than the respective values shown for biomaterials and for pyrolysis products, respectively. Maximum sorption capacity of phenanthrene (55 % proportion removal) was shown by γ-alumina, with a specific surface area equal to 270 m2/g, after 8 days. Minimum sorption capacity (14 % proportion removal) was shown by γ-alumina, with a specific surface area equal to 120 m2/g, after 10 days. Titania, with a specific surface area equal to 120 m2/g, adsorbed a proportion of 52 % of the initial concentration of phenanthrene, after 8 days. Sorption experiments of 2-naphthol from γ-alumina, did not show a measurable sorption. Sorption of mercury from γ-alumina and ferric oxides was studied, conducting batch experiments at 25 °C, pH 5, 24 h contact time. The experiments resulted to an isotherm curve that was evaluated using different sorption isotherm models. An increase of the proportion of mercury removal, with the increase of the mass of γ-alumina was observed. Maximum proportion of mercury removal (93% of the initial concentration) was observed with the addition of γ-alumina of 1 g or more. At Ce=15 mg/L, qe=0,91 mg/g was measured. This value is 1 to 2 orders of magnitude lower, than the respective values shown for biomaterials and for pyrolysis products, respectively. Even though ferric oxides’ specific surface area was estimated at 55 m²/g, they did not show a measurable sorption capacity for any of the pollutants tested in the present study. Even though the materials examined in the present study, were of large specific surface area, their sorptive properties shown, are not competitive with the respective properties of biomaterials. Thus, they cannot be considered as promising sorbents for the removal of phenanthrene, 2-naphthol, or mercury from water.

Submitted by Ana Hilda Fonseca (anahilda@ufba.br) on 2014-09-17T17:51:04Z No. of bitstreams: 1 (Dissertação_mestrado__(03.11_)).pdf: 1756144 bytes, checksum: 6a5c8a2f486f154eba91b5aa9780dde0 (MD5) / Approved for entry into archive by Fatima Cleômenis Botelho Maria (botelho@ufba.br) on 2014-09-19T12:24:04Z (GMT) No. of bitstreams: 1 (Dissertação_mestrado__(03.11_)).pdf: 1756144 bytes, checksum: 6a5c8a2f486f154eba91b5aa9780dde0 (MD5) / Made available in DSpace on 2014-09-19T12:24:04Z (GMT). No. of bitstreams: 1 (Dissertação_mestrado__(03.11_)).pdf: 1756144 bytes, checksum: 6a5c8a2f486f154eba91b5aa9780dde0 (MD5) / CNPQ / A determinação de metais em águas naturais por Espectrometria de Emissão Óptica com Plasma Indutivamente Acoplado (ICP OES), em geral, deve envolver etapas de pré- concentração, devido os níveis de concentração dos metais em água serem muitas vezes abaixo dos limites de detecção da técnica. Dessa forma, o objetivo desse trabalho foi desenvolver um método de pré-concentração em fase sólida sensível e simples para a determinação de cobre, ferro, níquel, manganês, chumbo e zinco em amostras de água por ICP OES. As condições experimentais para pré-concentração foram otimizadas considerando os fatores: concentração do eluente, volume de eluente, volume da amostra, vazão e pH. As condições otimizadas corresponderam ao uso de 5 mL de solução de HCl 0,8 mol L-1 como eluente, volume da amostra de 50 mL, vazão de 1,9 mL min-1 e pH 9,0. Para a determinação dos metais, as amostras, após ajuste do pH, foram percoladas com o auxílio de uma bomba peristáltica em cartucho Sep-pak C18 com 1-(2-piridilazo)-2-naftol (PAN) imobilizado na sílica funcionalizada C18. A eluição dos analitos foi realizada com a passagem da solução de HCl pelo cartucho para posterior determinação por ICP OES. Nestas condições, os limites de detecção para Cu, Fe, Mn, Ni, Pb e Zn obtidos variaram entre 0,11 e 21 µg L-1 e os limites de quantificação entre 0,36-69 µg L-1, respectivamente. Os desvios padrão relativos (R.S.D.) para a determinação dos analitos não ultrapassaram 9 %. O efeito de possíveis espécies interferentes sobre a recuperação dos analitos também foram investigados. A exatidão do método foi avaliada mediante análise de material de referência certificado (SLEW-3 Estuariene Water Reference Material for Trace Metals) e o método proposto foi aplicado para análise de amostras de água subterrânea, água potável e água de rio coletadas nos municípios de Cachoeira e São Félix, Bahia, Brasil. As amostras foram analisadas por Espectrometria de Massas com Plasma Indutivamente Acoplado (ICP-MS) como método comparativo, não sendo observadas diferenças significativas entre estes resultados e os resultados obtidos pelo método proposto. / The determination of metals in natural waters by Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES), in general, involves pre-concentration steps, due the concentration levels of metals in water are often below the limits of detection of this technique. In this way, the objective of this work was to develop a pre-concentration solid phase method for sensitive and simple determination of copper, iron, nickel, manganese, lead and zinc in water samples by ICP OES. The experimental conditions for pre- concentration were optimized considering the following factors: the concentration of the eluent, eluent volume, sample volume, flow-rate and pH. The optimized conditions corresponded to the use of 5 mL of HCl solution 0.8 mol L-1 as an eluent sample volume 50 ml, flow-rate 1.9 mL min-1 and pH 9.0. For the determination of metals by the procedure, the samples after pH adjustment were percolated with the aid of a peristaltic pump on Sep-Pak C18 cartridge with 1-(2-pyridylazo)-2-naphthol (PAN). The analyte elution was carried out with the passage of the HCl solution in the cartridge for subsequent determination by ICP OES. In these conditions, the detection limit for Cu, Fe, Mn, Ni, Pb and Zn varied between 0.11 to 21 μg L-1 and the limits of quantification from 0.36 to 69 μg L-1, respectively. The relative standard deviation (RSD) for the analytes of this study did not exceed 9%. The effect of possible interfering species on the recovery of the analytes was also investigated. The accuracy of the method was evaluated by analysis of certified reference material (SLEW-3 Estuariene Water Reference Material for Trace Metals) and the proposed method was applied to samples of ground water, drinking water and river water collected in Cachoeira and São Félix cities, Bahia, Brazil. The samples were analyzed by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) as a comparative method do not being found significant differences among these results and the results obtained by the proposed method.

O poli(5-amino 1-naftol) é um polímero que pertence à classe dos polímeros condutores e pode ser obtido através da oxidação do monômero bifuncionalizado, 5-amino 1-naftol, que possui dois grupos funcionais: -NH2 e -OH. Neste trabalho é apresentado um estudo dos polímeros provenientes do referido monômero quando polimerizado na presença de diferentes ácidos. As influências do meio eletrolítico na eletrodeposição, na morfologia e nos processos redox dos filmes, são estudadas. As transformações eletrocrômicas, conseqüência dos diferentes estados de oxidação dos filmes, são acompanhadas por experimentos espectroeletroquímicos na região do visível. É realizado um completo estudo espectroscópico, utilizando técnicas in situ e ex situ como Raman Ressonante, Infravermelho e Espectroscopia Fotoeletrônica de Raios-X, que permite a elucidação das distintas estruturas formadas durante a polimerização e a identificação das espécies encontradas nos diferentes estados de oxidação do filme. São também realizados testes para verificar a potencial aplicação do poli(5-amino 1-naftol) como componente na construção de biossensores, fazendo uso do grupamento funcional -OH que não participa do processo de polimerização e permanece livre na cadeia polimérica. / Poly(5-amino 1-naphthol) (poly(5-NH2 1-NAP)) is a polymer that belongs to the conducting polymer class obtained by the oxidation of a bifunctional monomer, 5-amino 1-naphthol, which presents two bifunctional groups: -NH2 e -OH. In this work it is showed a study about polimerization of 5-amino 1-naphthol and their polymer formed in different electrolytic acid medium. Influences of the electrolyte in the electrodeposition, morfology and the redox process are studied. Electrochromic transformations that appear as consequences of different films oxidation states are followed by spectroelectrochemical experiments in the visible range. An entire spectrocopic study using ex situ and in situ techniques as Resonante Raman Spectroscopy, Infrared Spectroscopy and X-Ray Photoelectron Spectroscopy is carried out. It allows the elucidation of distint structures formed during the polimerization and the identification of species in different oxidation states. Experiments are also carried out in order to verify the potential aplication of poly(5-amino 1-naphthol) as biosensor component. Poly(5amino 1-naphthol) is a candidate as polymeric matrix beca use of the -OH groups doesnt take part in the polymerization process and it remais free in the polymeric chain.