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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
71

Analisador de bilirrubina no soro de neonatos utilizando espectrofotometria direta / Neonate serum bilirubin meter using direct spectrophotometry

Leandro Augusto Lopes Azeka 11 February 2009 (has links)
A icterícia é uma manifestação caracterizada pelo amarelamento da pele e mucosas devido ao excesso de bilirrubina no sangue do paciente. Cerca de 60% dos recém nascidos (RN) manifestam a icterícia nas primeiras semanas de vida, sendo este índice muito maior em neonatos prematuros. Se não corretamente diagnosticada, a alta concentração de bilirrubina pode intoxicar a massa encefálica, provocando uma encefalopatia conhecida como kernicterus. Existem vários métodos para medir a concentração de bilirrubina, e entre eles pode-se citar: métodos bioquímicos laboratoriais que utilizam amostras de sangue coletadas e reagentes específicos, medidores de bilirrubina transcutâneos e espectrofotometria em amostras de soro. O princípio básico desses métodos é a análise colorimétrica, que se baseia na alta absorbância da molécula de bilirrubina no comprimento de onda de 455 nm. O presente trabalho descreve um bilirrubinômetro, que foi desenvolvido para medir a concentração da bilirrubina utilizando a espectrofotometria direta no soro de amostras sanguíneas de neonatos. No projeto do bilirrubinômetro levou-se em consideração o baixo custo de produção, uma boa precisão comparada com outros equipamentos, e a utilização de componentes de alta tecnologia tais como LED com alta intensidade luminosa e fotorreceptores especiais para medir concentrações nas faixas de luz específica. Para a validação do equipamento foram obtidas amostras de sangue de recém nascidos, junto ao Hospital das Clínicas da Faculdade de Medicina de Ribeirão Preto, e os resultados das medidas realizadas com o bilirrubinômetro construído foram comparados com os obtidos com um bilirrubinômetro comercial e com métodos bioquímicos clássicos. Os resultados da comparação mostraram que o bilirrubinômetro construído apresenta um erro relativo de ± 1,05 mg/dl, que se encontra dentro da média dos bilirrubinômetros diretos e custo de produção relativamente baixo. / Jaundice is a manifestation described as the yellowish staining of the skin and mucous membranes caused by the excessive levels of bilirubin in the patient blood. About 60% of the newborns present this feature in the first weeks of life, and this percentage is much higher in premature neonates. If not correctly detected and treated, the bilirubin can intoxicate the encephalic mass, causing an encephalopathy knowed as kernicterus. There are many methods to measure the bilirubin concentration such as: blood laboratory methods using specific reagents, transcutaneous bilirubin and serum spectrophotometric equipments. The basic principle of these devices is the colorimetric analysis based on the high absorption of the bilirubin molecule in the 455 nm wavelength. This work describes a bilirubin meter that was developed for measure the bilirubin concentration using direct spectrophotometry in the serum of neonates\' blood samples. In the bilirubin meter project it was considered the low production cost, a good precision compared with others similar equipments, and the use of high technology components as high intensity LED and special photoreceptors to measure specific wavelengths. For validation of the equipment it was used newborns blood samples from the Clinics Hospital at the Faculty of Medicine of Ribeirão Preto, and the results obtained with the equipment were compared with the values of a commercial bilirubin meter and with biochemical tests. The results showed that the developed bilirubin meter has a relative error around 1,05 mg/dl, similar to commercial bilirubin meters and a low relative cost.
72

Identification of anthocyanidin pigments in three varieties of Pelargonium hortorum by chromatographic and spectrophotometric methods

Ahmedullah, Mohammed. January 1961 (has links)
Call number: LD2668 .T4 1961 A43
73

Microheterogeneous solid polymer electrolyte (SPE) membranes for electrocatalysis

Michaels, W. C. 04 1900 (has links)
Dissertation (Ph.D.)--Stellenbosch University, 2002. / ENGLISH ABSTRACT: The deposition of platinum catalyst on cation-exchange membranes was achieved by a counter diffusion deposition method known as the Takenaka- Torikai method. The morphology of the platinum catalyst on the membranes were controlled by varying the conditions of the platinum deposition process, such as, temperature, type of reducing agent and concentration of the platinic acid solution. The effect of the sonication of platinic acid solution and the pre-treatment of membranes on the morphology of a platinum catalyst was also investigated. Platinum loading on cation-exchange membranes was determined by UV spectrophotometric and gravimetric analyses. Suitable conditions for the quantitative determination of the platinum loading on membranes by UV spectrophotometric analysis was established through the development of a protocol. Membranes were characterised using different techniques such as, Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM), Infrared spectrometry (IR), Dielectric analysis (DEA) and Brunauer Emmett Teller adsorption (BET). The roughness profile of a platinum catalyst embedded on a membrane was explored by various statistical methods. The statistical analysis of various data sets for a surface of a platinum-containing membrane was investigated using the Hurst exponent. The effect of surface modification of membranes on the deposition process, as well as the morphology of the platinum catalyst, was investigated. Membranes were modified with ethylene diamine (EDA) and cetyltrimethylammonium bromide surfactant. Modification of membranes with cetyltrimethylammonium bromide surfactant resulted in a unique textured platinum catalyst. The electrochemical "switching" phenomenon was investigated for EDAmodified membranes and EDA-modified membranes embedded with platinum catalyst. The "switching" phenomenon was observed in i-V cyclic curves, which were obtained by galvanodynamie measurements. The application of electro catalytic membrane systems in the anodic oxidation of water was investigated by electrochemical techniques such as galvanostatic and cyclic voltammetric measurements. / AFRIKAANSE OPSOMMING: Die deponering van 'n platinum katalis op katioon-uitruil membrane is suksesvol gedoen d.m.v. die Takenaka-Torikai metode. Die morfologie van die platinum katalis op die membrane is gekontrolleer deur variasie van die kondisies van die platinum deponeringsproses, bv. temperatuur, tipe reduseermiddel gebruik en konsentrasie van die platiensuuroplossing, asook die ultrasonifikasie van die platiensuuroplossing en voorafbehandeling van die membrane. UV spektrofotometriese asook gravimetriese analitiese metodes is gebruik om die platinumlading op katioon-uitruil membrane te bepaal. Geskikte kondisies vir die kwantitatiewe bepaling van die platinumlading op membrane d.m.v. UV spektrofotometriese analise is ontwikkel deur die skep van 'n protokol. Membrane is gekarakteriseer d.m.v. die volgende tegnieke: Atoomkrag Mikroskopie, Skanderingselektron Mikroskopie, Infrarooi Spektrometrie, di-elektriese analise en Brunauer Emmett Teller adsorpsie. Die skurtheidsprofiel van 'n platinum katalis op 'n membraan is ondersoek deur gebruik te maak van verskeie statistiese metodes. Statistiese analises van verskeie data stelsels van 'n platinum-bevattende membraan is ondersoek deur gebruik te maak van die Hurst eksponent. \ Die effek van oppervlakmodifikasie op membrane sowel as die deponeringsproses en morfologie van die platinum katalis is ondersoek deur die modifikasie van membrane met etileen diamien (EDA) en setieltrimetielammonium bromied as versepingsmiddel Die elektrochemiese omswaai van EDA-gemodifiseerde membrane sowel as gemodifiseerde platinum bevattende membrane is ondersoek d.m.v. galvanodinamiese metings. Die gebruik van elektro-katalitiese membraansisteme in die anodiese oksidasie van water is ondersoek deur gebruik te maak van elektrochemiese tegnieke, bv. galvanostatiese en sikliese voltammetriese metings.
74

Selective production of difluorodimethyl ether from chlorodifluoromethane - a kinetic study using a well-mixed batch absorber.

Prithipal, Rasmika. 14 May 2013 (has links)
The gas-liquid reaction between chlorodifluoromethane (R-22) and methanol, in the presence of sodium hydroxide, was investigated in an isothermal, stirred, semi-batch reactor. The objective of the study was to develop a model for the reaction and to identify the kinetic parameters. Reactor temperature was varied from 283 to 303 K, with inlet R-22 partial pressures between 40.5 and 60.8 kPa (absolute). Solutions containing sodium hydroxide concentrations of between 1.5 and 2.5 mol·dm-3 were charged into the reactor prior to each experiment. Preliminary investigations using the R-22-methanol system revealed that stainless steel was an inappropriate choice of material for the reactor as it displayed catalytic tendencies toward trimethyl orthoformate formation. Consequently, the reactor was constructed from glass and was equipped with an internal cooling coil, a single heating jacket and a temperature control unit. Liquid samples that were withdrawn from the reactor were degassed under vacuum to remove residual chlorodifluoromethane, and thereby inhibit further reaction. Spectrophotometry was used to analyze the liquid samples to determine the concentration of chloride ions in solution. The products obtained were difluorodimethyl ether (major product) and trimethyl orthoformate (by-product) as well as sodium chloride and sodium fluoride salts. Difluorodimethyl ether is a potential replacement for ozone depleting CFC refrigerants. A Box-Behnken experimental design was used to investigate the effect of reaction conditions on the product distribution. Variations in the reaction temperature, initial concentration of sodium hydroxide and inlet partial pressure of R-22 were considered. The modeling of the gas-liquid reactions was based on the -dehydrohalogenation mechanism. Since gas solubility in a liquid decreases in the presence of dissolved salts, the "salting-out" effect on mass transfer was included in the reactor model. Sechenov coefficients for sodium chloride and sodium fluoride were combined to give a salt Sechenov coefficient Ksalt . It was known from the literature that the presence of precipitated salts causes inefficient mixing and inhibits mass transfer, particularly in this system due to the relatively low salt solubilities in methanol. This mixing effect was also included in the appropriate mass transfer terms of the reactor model. The experimental data was fitted to a proposed kinetic scheme. Kinetic parameters for each of the proposed reactions, the Sechenov ‘salting out’ coefficients and the mixing parameter were obtained through the use of a non-linear, least-squares optimization algorithm. For the kinetic study, activation energies of 89.12 and 45.83 kJ·mol-1 were obtained for the difluorodimethyl ether and trimethyl orthoformate formation reactions, respectively, with a Sechenov salt coefficient of 0.712 and a mixing parameter of 22.43. / Thesis (M.Sc.Eng.)-University of KwaZulu-Natal, Durban, 2013.
75

Fyzikálně chemické vlastnosti léčiv / Physico-Chemical Properties of Drugs

Suchý, Miroslav January 2016 (has links)
1. Abstract Charles University in Prague Faculty of Pharmacy in Hradec Kralove Department of Biophysics and Physical Chemistry Candidate: Miroslav Suchy Supervisor: Ing. Vladimir Kubicek, CSc. Title of Diploma Thesis: Physico-Chemical properties of drugs To test physico-chemical properties of new molecules is necessary during drug development. It could be helpful to understand or predict the pharmacokinetic parametres of a new drug in vivo/in vitro experiments. One of this parameters is a dissociation constant (pK). Dissociation constant is defined as " Number on pH scale, wherein is just fifty percent of molecule in a ionization condition". In real case this number can help us to know where in the gastro-intestinal tract (GIT) the drug will be absorbed. In GIT only molecules exhibiting pK from 3 to 11 could be absorbed. Out of this range it is not possible. In this work I would like to introduce the ways of experimental measurement of pK values. I was working with two methods to measure the pK values of water-soluble compounds. The spectrophotometric method and the potentiometric one. I had to find out, that potentiometric titration is primary method which gets us good and accurate results. Based on my measurement I evaluated the spectrophotometric method as the secondary method. Spectrophotometric method...
76

Interference redukujících látek s hematoxylinovým stanovením chelatace měďnatých iontů / Interference of reducing agents with the hematoxylin assay for determination of cupric chelation

Zsáková, Emily January 2019 (has links)
Charles University Faculty of Pharmacy in Hradec Králové Department of Pharmacology & Toxicology Student: Emily Zsáková Supervisor: Assoc. Prof. Přemysl Mladěnka, PharmD., Ph.D. Title of diploma thesis: Interference of reducing agents with the hematoxylin assay for determination of cupric chelation Copper is an essential trace element of living organisms. Disorders of its homeostasis affect various pathological conditions. In excessive amounts, it is toxic due to its ability to form free radicals. Vitamin C, trolox (a water soluble form of vitamin E), glutathione and hydroxylamine possess reducing properties that protect our body from oxidative tissue damage. Oxidized glutathione (GSSG) was also tested for comparison. The object of study was to test the chelating ability of these substances. A simple and fast spectrophotometric method was used. The combination of reducing properties of copper and chelating agents could lead to an improvement in chelation therapy either in heavy metal poisoning, treatment of Wilson's disease, or other diseases. We found that all substances were chelators/copper-chelating agents in vitro in a slightly competitive environment, using hematoxylin as an indicator. However, by using the bathocuproine assays to verify chelating properties, none of the substances...
77

Avaliação da quantidade de formaldeído liberado por alguns cimentos endodônticos / Evaluation of the quantity of formaldehyde released by some endodontic sealers

Ozorio, Jose Estevam Vieira 27 April 2012 (has links)
Analisou-se, por meio de espectrofotometria, a liberação de formaldeído de cimentos endodônticos à base de óxido de zinco e eugenol, resinas epóxica e polimetacrilato, hidróxido de cálcio e biocerâmico, estudados em diferentes oportunidades: durante a espatulação; decorrido três vezes o tempo de endurecimento e, por fim, na extração de sua massa endurecida. As amostras foram adquiridas pela coleta do volume da água utilizada em cada período e, determinada a curva de calibração da liberação do formaldeído e análise controle com água, foram submetidas à análise colorimétrica com adição dos reagentes: 5,0 mL de solução tampão, 0,5 mL de solução de parafenilenodiamina e 2,5 mL de peróxido de hidrogênio em balões volumétricos de 50,0 mL mantendo-os em repouso por 20 minutos. Após, foi realizada leitura em espectrofotômetro duplo feixe nos comprimentos de onda 326, 334 e 462 nm. Detectou-se formaldeído em todos os cimentos à base de resina epóxica, no EndoREZ® e no Endomèthasone N, quantificado apenas no Sealer 26 (7.40 mg.L-1) e Endomèthasone N (9.13 mg.L-1) durante a espatulação; no AH Plus® (4.44 mg.L-1) e no Endomèthasone N (18.14 mg.L-1) durante o endurecimento, e somente no Endomèthasone N depois de endurecido (9.43 mg.L- 1). Concluiu-se que, durante a espatulação, todos os cimentos de resina epóxica liberaram formaldeído, com quantificação apenas para o Sealer 26, o Endomèthasone N apresentou a maior quantidade, e o Endorez liberou a substância em quantidade insuficiente para quantificação. Após a espatulação, todos os de resina epóxica liberaram formaldeído, com quantificação no AH Plus e o Endomèthasone N apresentou a maior quantidade da substância, que também foi encontrada no Endorez, sem quantificação. Endurecidos, todos os cimentos de resina epóxica e o Endorez liberaram formaldeído em quantidade insuficiente para quantificação, e o cimento Endomèthasone N liberou a maior quantidade dessa substância. / This study evaluated, by means of spectrophotometry, the release of formaldehyde in zinc oxide, epoxy resins and polymethylmethacrylate, calcium hydroxide and bioceramic based endodontic sealers in different situations: during mixing; after 3 time the setting time and, at extraction of its hardened mass. The samples were acquired by means of collection of the volume of water used in each period and - after determining the calibration curve of formaldehyde release and analyzing the control with water - were submitted to colorimetric analysis with the addition of the following reagents: 5.0mL of buffered solution, 0.5mL of paraphenylenediamine and 2.5mL of hydrogen peroxide to a 50.0mL volumetric flask, which was kept at rest for 20 minutes. Double-beam spectrophotometer readings were performed at 326, 334 and 462nm wavelengths. Formaldehyde was detected in all epoxy resin based sealers, in EndoREZ and in Endomèthasone N, quantified only in Sealer 26 (7.40 mg.L-1) and Endomèthasone N (9.13 mg.L-1) during mixing, and in AH Plus (4.44 mg.L-1) and Endomèthasone N (18.14 mg.L-1) during the setting time, and only in Endomèthasone N after setting (9.43 mg.L-1). It can be concluded that during mixing all epoxy resin based sealers released formaldehyde, with quantification being possible only for Sealer 26, Endomèthasone N showed higher quantities, and Endorez released the substance in insufficient quantity for detection. After mixing, all epoxy resin based sealers released formaldehyde, whereas quantification was possible for AH Plus and Endomèthasone N presented the highest quantity of the substance, that was also found in Endorez, but could not be quantified. When set, all epoxy resin sealers and Endorez released formaldehyde in insufficient quantity for quantification, and Endomèthasone N released the greater amount of this substance.
78

"Estudo espectrofotométrico do sistema crômio(III)/azoteto e seu aproveitamento analítico". / "Spectrophotometric study of chromium(III)/azide system and your analytical application".

Lourenço, Leandro Maranghetti 06 February 2004 (has links)
Na área de Química, uma das linhas mais tradicionais de pesquisa envolve o estudo de formação de complexos. Estes trabalhos são realizados de modo sistemático em nossos laboratórios, geralmente envolvendo cátions de metais de transição com vários ligantes (haletos, pseudo-haletos e carboxilatos). A intensa coloração desenvolvida pela maioria dessas reações de complexação, entre um metal e um pseudo-haleto, tem motivado o desenvolvimento de novos métodos espectrofotométricos para a determinação de íons em amostras reais. Espera-se que o crômio(III), da mesma forma que outros metais de transição, como o ferro, níquel e cobalto, forme complexos com o pseudo-haleto denominado azida ou azoteto (N3-). Desta forma, dando continuidade a esta linha de pesquisa, este trabalho teve como objetivo otimizar as condições experimentais para o sistema crômio(III)/azoteto. Diversos parâmetros como acidez, concentração de ligante, natureza e concentração de solvente, bem como o efeito da temperatura, foram investigados. Reunidas as melhores condições (otimização), montou-se o método analítico que possibilita a determinação do metal. As condições ideais empregadas foram: concentração analítica de ligante e ácido perclórico de 493 e 12,0 mmol L-1, respectivamente, numa temperatura de 25ºC, em meio aquoso. Para a determinação no ultravioleta, o tempo de espera para cada medida foi de 1 hora, enquanto que na região do visível, foi de apenas 30 minutos. Os máximos de absorção ocorreram em torno de 646, 480 e 287 nm, com coeficientes de absortividade molar médios de 184±1, 157±1 e (1,481±0,008) 104 L mol-1 cm-1, respectivamente. As condições estabelecidas foram promissoras, permitindo uma boa repetitividade nas regiões do visível e ultravioleta. Para o método desenvolvido, os íons mais interferentes na região do visível foram: Fe3+, Co2+ e Cu2+ e, na região do ultravioleta, foram HC8H4O4-, Fe3+, Cu2+ e Hg2+. Por meio de um sistema com duas equações, a determinação simultânea de crômio e ferro mostrou-se possível e com erros dentro dos limites analiticamente aceitáveis. Sem a utilização do sistema de equações, verificou-se ainda a possibilidade de se determinar crômio diretamente, mesmo na presença de ferro, no comprimento de onda de 646,5 nm, com um erro menor que 5%, desde que a concentração de ferro não ultrapasse 4 mg L-1. Aplicações analíticas para o método proposto foram testadas em dois suplementos alimentares contendo crômio. Os resultados foram comparados e mostraram-se concordantes com os da técnica de espectrometria de absorção atômica, para o suplemento contendo crômio quelato. Para o suplemento alimentar contendo picolinato de crômio, houve uma discordância dos resultados, indicando a existência de interferentes da matriz que não puderam ser eliminados. Um teste com uma amostra sintética de crômio mostrou um erro de cerca de 1,0% para o método proposto. Em condições ideais, e com um controle dos interferentes presentes, o método proposto mostra-se preciso, simples e barato. Considerando valores de absorbância entre 0,2 e 0,8 (faixa ideal), pode-se determinar o metal nos intervalos de 1,27 a 5,09 mmol L-1 a 480,5 nm, de 1,09 a 4,35 mmol L-1 a 646,5 nm e, finalmente, entre 0,702 a 2,81 mg L-1 no ultravioleta (287 nm). / In Chemistry, the study of complexes formation is one of the most traditional research lines. These studies are done under systematic manners in our laboratories, usually involving metallic transition cations with several ligands (halides, pseudohalides and carboxylates). The intense coloration developed by the major part of those complexation reactions, between a metal and a pseudohalide, has encouraged the development of new spectrophotometric methods for determination of ions in real samples. Conforming others transition metals, (iron, nickel and cobalt), which form complexes with the pseudohalide azide (N3-), we tried to observe the same behavior to chromium(III). Continuing this research line, this work had as principal objectives optimizes the experimental conditions for the chromium(III)/azide system. Several parameters were investigated as acidity, ligand concentration, nature and solvent concentration, as well as temperature effect for optimization of experimental conditions. Gathering all these conditions, the analytical methods were tested for the metal determination. The ideal conditions employed were: analytical ligand concentration and perchloric acid of 493 and 12.0 mmol L-l respectively, at 25 °C, in aqueous medium. For the studies in the ultraviolet region, the contact time before the measures was one hour, while for studies in the visible band measures were made after 30 minutes. The wavelengths of maximum absorption were encountered at 646, 480 and 287 nm, with molar absorptivity coefficients (mean) of 184±1, 157±1 and (1.481±0,008) 104 L mol-1 cm-1, respectively. The established conditions were promising, allowing a good precision in the visible and ultraviolet region. For the developed method, the more interfering ions on visible band were: Fe3+, Co2+ and Cu2+ and, on the ultraviolet band, were HC8H4O4-, Fe3+, Cu2+ and Hg2+. Through a system of two equations, the simultaneous determination of chromium and iron ions was possible with errors within the tolerance range. Without the simultaneous equations system, it was verified directly the possibility of chromium determination in the presence of iron, at a wavelength of 646.5 nm, with an error smaller than 5%, since the concentration of iron doesn’t exceed 4 mg L-l. In this proposed method, analytical applications were tested for two alimentary supplements containing chromium. The results were compared, being concordant with those of atomic absorption technique for the supplement containing chromium chelate, while for the alimentary supplement containing chromium picolinate, the results were in disagreement with the results, indicating the existence of matrix interferences which could not be eliminated. A test with a synthetic sample of chromium had an error of about 1.0% for the proposed method. Under ideal conditions, and with some control of possible interfering, the proposed method can be precise, accurate, simple and cheap. Considering the absorbance values between 0.2 and 0.8 (ideal range), the metal can be determined from 1.27 to 5.09 mmol L-l in 480 nm; 1.09 to 4.35 mmol L-l in 646 nm and, finally, from 0.702 to 2.81 mg L-l at 287 nm (ultraviolet).
79

Estudo in vitro da estabilidade de cor e opacidade de cinco sistemas cerâmicos sob influência do envelhecimento artificial acelerado / \"In vitro\" study of color stability and opacity of five ceramic systems under influence of accelerated aging

Porto, Luciana de Paula Ribeiro dos Santos 30 July 2007 (has links)
O objetivo deste estudo foi avaliar a estabilidade de cor e opacidade de cinco sistemas cerâmicos glazeados naturalmente e com pintura extrínseca, utilizando os espectrofotômetros Color Guide 45/0 (BYK-Gardner) e Easyshade (Vita), sob influência do envelhecimento artificial acelerado. Foram confeccionados 14 corpos de prova para cada grupo testado de cerâmica - metalocerâmica Ceramco 3 (Dentsply) (grupo 1), cerâmica pura Ceramco 3 (grupo 2), cerâmica pura EX -3 (Noritake) (grupo 3), Vitroceram (Angelus) recoberta com Allceram (Degudent) (grupo 4) e Vitroceram recoberta com Cerabien (Noritake) (grupo 5). Sete corpos de prova de cada grupo cerâmico foram glazeados naturalmente e sete foram submetidos à pintura extrínseca com pigmento Vita Chrom 712. Uma leitura inicial foi realizada em todos os corpos de prova utilizando o espectrofotômetro Color Guide, obtendo valores de opacidade e das coordenadas L*, a*, b* e E*; e utilizando o espectrofotômetro Easyshade, obtendo valores de L*, C*, h* e E*. Após o envelhecimento artificial de 500h, foram realizadas novas leituras nos espectrofotômetros. Os resultados encontrados foram submetidos à análise estatística e concluiu-se que os grupos 2, 3 e 4 foram influenciados estatisticamente pelo envelhecimento artificial acelerado quanto à opacidade; e que o grupo 5 foi o que obteve o pior desempenho de estabilidade de cor (E* = 3,32 - VTCE e E* = 2,68 = VTCEPE) para o espectrofotômetro Color Guide. Com o espectrofotômetro Easyshade os grupos 4 e 5 e as cerâmicas MC, CER, EX foram considerados ineficazes quanto à estabilidade de cor (p<0,05). / The aim of this study was to evaluate the color stability and opacity of five ceramic systems naturally glazed and with extrinsic porcelain colorant, under influence of accelerated aging, using two spectrophotometers Color Guide 45/0 (BYK-Gardner) and Easyshade (Vita) as a tool for color and opacity measurement. Fourteen samples were provided for each tested group of ceramics: metal-ceramic Ceramco3 (Dentsply) (Group 1), Ceramco3 (Group 2), EX3 (Noritake) (Group 3), Vitroceram (Angelus) with Allceram (Degudent) (Group 4) and Vitroceram with Cerabien (Noritake) (Group 5). Seven samples of each group were submitted to extrinsic colorant (Vita Chrom 712) and the other seven were naturally glazed. An initial measurement was performed and the values of opacity, L*, a*, b* and E* were obtained using the Color Guide spectrophotometer, and using Easyshade the values of L*, C*, h* and E* were obtained. After the process of 500h accelerated aging a new measurement was performed for all samples. The results were statistically analyzed and the conclusion was that the opacity of groups 2, 3 and 4 were statistically influenced by the accelerated aging and the group 5 had the worst assessment in color stability (E* = 3,32 - VTCE e E* = 2,68 - VTCEPE) with the Color Guide spectrophotometer. With Easyshade, groups 4 and 5 and MC, CER and EX ceramics were considered ineffective as for color stability (p<0,05).
80

Desenvolvimento de procedimento analítico para determinação de iodato em sal de mesa utilizando sistema com multicomutação e detecção espectrofotométrica / Development of analytical procedure for determination of iodate in table salt using a multicommuted system and spectrophotometric detection

Silva, Amanda Ribeiro Martins da 18 April 2016 (has links)
A iodação do sal de mesa é considerada o caminho mais eficiente para controlar os Distúrbios por Deficiência de Iodo. Em países tropicais, o elemento pode ser adicionado na forma de KIO3. Para garantir que os níveis ideais do ânion estejam disponíveis ao consumidor, o controle de qualidade do sal consiste numa estratégia fundamental. Sistemas em fluxo com multicomutação representam uma alternativa versátil para o desenvolvimento de procedimentos simples, rápidos e limpos, minimizando o consumo de reagentes e a geração de resíduos. Nesse contexto, um procedimento analítico utilizando sistema com multicomutação e detecção espectrofotométrica foi desenvolvido para a determinação de iodato em sal de mesa. A reação empregada foi baseada na formação de um composto roxo (540 nm) entre iodato (IO3-) e p-aminofenol (PAP) em meio ácido. O tempo de residência da zona de amostra no percurso analítico foi explorado a fim de favorecer a reação lenta e a frequência de amostragem para a melhoria do desempenho analítico. Foram selecionados 2 pulsos para inserção de amostra, 3 pulsos para reagente (PAP 0,25% (m/v) em HCl 0,025 mol L-1), 7 ciclos de amostragem, 200 pulsos de carregador (água), bolha de ar de 1 s (40 µL), reator de 70 cm (3 mm d.i.) e parada de fluxo de 480 s. Resposta linear foi observada entre 2,28x10-5 e 3,65x10-4 mol L-1, descrita pela equação A = 0,2443 + 2030 C, r = 0,997. Limite de detecção (99,7% de confiança), coeficiente de variação (n = 20) e frequência de amostragem foram estimados em 8,2x10-6 mol L-1, 0,42% e 70 determinações por hora, respectivamente. Houve consumo de 1,05 mg de PAP e geração de 0,70 mL de resíduos por determinação. As principais espécies concomitantes presentes na amostra não interferiram na determinação de iodato em concentrações até 8 vezes maiores que as usualmente encontradas. Estudos de adição e recuperação de iodato foram realizados pelo procedimento proposto, obtendo porcentagens de recuperação entre 88 e 104%. O procedimento analítico desenvolvido apresenta sensibilidade adequada para a determinação de iodato em amostra de sal de mesa e elevada frequência de amostragem quando comparado com procedimentos descritos na literatura / Table salt iodization is considered the most efficient way to control iodine-deficiency disorders. In tropical countries, the element can be added as KIO3. To ensure that ideal amounts of this anion are available to consumers, the quality control of iodized salt is fundamental strategy. Multicommuted flow systems represent a versatile alternative to the development of simple, fast and clean procedure, minimizing reagent consumption and waste generation. In this context, an analytical procedure using a multicommuted system and spectrophotometric detection was developed for determination of iodate in table salts. The chemical reaction was based on the formation of purple compound (540 nm) between iodate (IO3-) and p-aminophenol (PAP) in acidic medium. The sample residence time in the analytical path was explored in order to further the slow chemical reaction and the sampling rate for the improvement of the system analytical performance. Optimized conditions were 2 sample pulses, 3 reagent pulses (PAP 0.25% (w/v) in HCl 0.025 mol L-1) in 7 sampling cycles, 200 carrier pulses (water), 1 s air bubble (40 µL), a 70-cm long reactor coil (3 mm i.d.) and the flow was stopped for 480 s. A linear response was observed between 2.28x10-5 and 3.65x10-4 mol L-1 iodate, described by the equation A = 0.2443 + 2030 C, r = 0.997. Detection limit (99.7% confidence level), coefficient of variation (n = 20) and sampling rate were 8.2x10-6 mol L-1, 0.42% and 70 determination per hour, respectively. Only 1.05 mg of PAP was consumed and 0.70 mL of waste was generated per determination. Usual concomitant species found in table salts did not cause significant interference in concentrations up to 8-fold higher than those expected. Recoveries between 88 and 104% were obtained for iodate spiked samples. The developed analytical procedure presented adequate sensitivity for the determination of iodate in table salts sample and higher sampling rate compared to literature procedures

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