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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.
1

Estudo sobre a aplicaÃÃo da espectrofotometria derivativa na anÃlise de nitrogÃnio em diversas matrizes de Ãguas / Study on the application in derivative spectrophotometry analysis of nitrogen in several matrices of waters

Maria do Socorro Pinheiro da Silva 19 July 2013 (has links)
A determinaÃÃo dos nÃveis de nitratos e nitrogÃnio total (NT) em Ãguas constitui uma ferramenta importante no sentido de avaliar o controle de seus nÃveis para proteÃÃo da saÃde humana bem como para caracterizar a eutrofizaÃÃo dos corpos aquÃticos. O presente trabalho faz um estudo da espectrofotometria derivativa (ED) para determinaÃÃo de nitratos e NT pelo mÃtodo zero-pico por ED, em segunda derivada, no mÃximo de absorÃÃo do nitrato (225nm). Neste estudo foram avaliados os interferentes comumente encontrados nas matrizes onde a metodologia foi aplicada, que foram Ãguas minerais, Ãguas adicionadas de sais e Ãguas superficiais (aÃudes e rios): bicarbonato, carbonato, ferro, cobre, sulfato, cloreto, brometo, iodeto, fosfato, sulfato, nitrito e matÃria orgÃnica dissolvida (MOD). Esta metodologia foi aplicada na determinaÃÃo de nitratos em amostras Ãguas minerais, adicionada de sais e Ãguas de aÃudes monitorados pela COGERH, onde nesta Ãltima matriz foi determinado tambÃm NT. Os interferentes avaliados nÃo apresentaram interferÃncia na segunda derivada do nitrato dentro de limites aceitÃveis, com exceÃÃo dos Ãons nitrito e carbonato, onde foi necessÃrio a remoÃÃo destes pela adiÃÃo de uma soluÃÃo de Ãcido sulfÃmico com HCl. Segundo o teste t (student) pareado, para amostras de Ãguas minerais e adicionadas sais, que foram analisados os teores de nitratos tanto por ED quanto pelo mÃtodo da reduÃÃo em coluna de cÃdmio com posterior determinaÃÃo pelo mÃtodo da sulfanilamida, nÃo apresentaram diferenÃas significativas a um nÃvel de confianÃa de 95%. Para as amostras de Ãguas superficiais, a determinaÃÃo de nitratos por ED demonstrou nÃo ser aplicÃvel. JÃ determinaÃÃo de NT demonstrou-se promissora, porÃm, estudos preliminares sugerem que a MOD presente nas amostras dos aÃudes estudados apresenta interferÃncia espectral, uma vez que, tais aÃudes estudados apresentaram indÃcios de contaminaÃÃo de origem alÃctone, se encontrando, na maioria, eutrofizados. / The determination of the levels of nitrates and total nitrogen (TN) in water is an important tool to assess the control levels for the protection of human health as well as to characterize the eutrophication of water bodies. The present work is a study of derivative spectrophotometry (DS) for the determination of nitrate and TN zero-peak method for DS in the second derivative maximum absorption of nitrate (225nm). In this study we evaluated the interferences commonly found in matrices where the methodology was applied, which were mineral water, added salts and surface water (reservoirs and rivers): bicarbonate, carbonate, iron, copper, sulfate, chloride, bromide, iodide, phosphate, sulphate, nitrite and dissolved organic matter (DOM). This methodology was applied in the determination of nitrate in mineral water samples, added salt and water reservoirs monitored by COGERH where the latter matrix was also determined TN. The interfering evaluated showed no interference in the second derivative of nitrate within acceptable limits, with the exception of nitrite and carbonate ions, where it was necessary to remove these by adding a solution of sulfamic acid with HCl. According to the t test (student) paired samples of mineral waters and added salts, which were analyzed nitrate levels both DS as the method of cadmium reduction column with subsequent determination by the method of sulfanilamide, showed no significant differences a confidence level of 95%. For surface water samples, the determination of nitrates by DS proved not to be applicable. Determination of TN already proved to be promising, however preliminary studies suggest that the DOM present in the samples studied the reservoirs presents spectral interference, since such, dams studied showed signs of contamination of allochthonous origin, lying mostly eutrophic.

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