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Exploiting the Use of a Liquid Waveguide Capillary Cell for Spectrophotometric Determinations in Flow-Based Systems.
紀錄類型:
書目-語言資料,印刷品 : Monograph/item
正題名/作者:
Exploiting the Use of a Liquid Waveguide Capillary Cell for Spectrophotometric Determinations in Flow-Based Systems./
作者:
Pascoa, Ricardo Nuno Mendes de Jorge.
出版者:
Ann Arbor : ProQuest Dissertations & Theses, : 2011,
面頁冊數:
248 p.
附註:
Source: Dissertations Abstracts International, Volume: 79-11, Section: C.
Contained By:
Dissertations Abstracts International79-11C.
標題:
Chemistry. -
電子資源:
http://pqdd.sinica.edu.tw/twdaoapp/servlet/advanced?query=10644043
ISBN:
9781088356982
Exploiting the Use of a Liquid Waveguide Capillary Cell for Spectrophotometric Determinations in Flow-Based Systems.
Pascoa, Ricardo Nuno Mendes de Jorge.
Exploiting the Use of a Liquid Waveguide Capillary Cell for Spectrophotometric Determinations in Flow-Based Systems.
- Ann Arbor : ProQuest Dissertations & Theses, 2011 - 248 p.
Source: Dissertations Abstracts International, Volume: 79-11, Section: C.
Thesis (Ph.D.)--Universidade Catolica Portugesa (Portugal), 2011.
This item must not be sold to any third party vendors.
In this thesis, the use of a liquid waveguide capillary cell (LWCC) was exploited for the spectrophotometric determination of several analytes in different types of water. With the purpose of in-line sample handling, different flow approaches were used for the development of simple, robust, cheap and automated analytical procedures. The first procedure was based on a sequential injection analysis (SIA) system for the determination of iron in coastal waters. With the goal of reaching low levels of iron, a LWCC was coupled to the system. This procedure used a doubled-line SIA system to improve mixing conditions between sample and reagents. The detection was based on a colorimetric reaction and two different reagents (ferrozine and 1,10-phenanthroline) were tested. The absorbance measurements were carried out at the wavelengths of 512 and 562 nm for the detection of iron-1,10-phenathroline and iron-ferrozine complex, respectively. An interference study was performed for both reagents. The developed method was also applied to natural waters (river, well, ground, potable and sea waters) and then compared with the reference procedure. One certified reference water sample was used to test the accuracy of the developed method. The objective of the second work was to determine iron at lower levels than the previous work and, as a consequence, to measure the levels of iron in ocean waters. With this in mind, a LWCC and a pre-concentration resin were coupled to a multisyringe flow injection analysis (MSFIA) system. Two different pre-concentration resins (Chelex 100 and NTA Superflow) were tested and evaluated. The determination of iron was also based on a colorimetric reaction and two reagents were tested, ferrozine and ammonium thiocyanate. The reactions were monitored at the wavelengths of 480 and 562 nm for the detection of iron-ammonium thiocyanate and iron-ferrozine complex, respectively. The accuracy was assessed using a certified reference water sample. A multi-parametric system for the spectrophotometric determination of zinc and copper at low levels in waters was the third work of this thesis. To attain this objective, a LWCC was coupled to a MSFIA system. The developed procedure for both analytes was based on a colorimetric reaction with zincon reagent at different pH values and monitored at 620 nm. Zincon reagent reacts only with copper at pH 5 and with copper and zinc at pH 9. An interference study for both determinations was carried out. The developed work was also applied to natural waters and three certified reference water samples. Subsequently, a multi-pumping flow system (MPFS) coupled with a LWCC was developed for the determination of titanium. This determination was based on the colorimetric reaction of titanium with chromotropic acid and the absorbance measurements were carried out at 425 nm. An interference study was performed in order to evaluate possible interferences. The developed procedure was applied to natural waters as well as to sunscreen formulations (the results were compared with the reference procedure). The accuracy was assessed with one certified lake sediment. The development of a spectrophotmetric method for bromate determination in waters at trace levels was the last work of this thesis. With this objective, a LWCC was coupled to a MPFS. The proposed methodology was based on a colorimetric reaction and two different colour reagents were tested, chlorpromazine and trifluoperazine. The lack of repeatability detected in this approach led to the development of a FIA approach in order to find out the reasons of this occurrence.
ISBN: 9781088356982Subjects--Topical Terms:
593913
Chemistry.
Subjects--Index Terms:
Biotechnology
Exploiting the Use of a Liquid Waveguide Capillary Cell for Spectrophotometric Determinations in Flow-Based Systems.
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In this thesis, the use of a liquid waveguide capillary cell (LWCC) was exploited for the spectrophotometric determination of several analytes in different types of water. With the purpose of in-line sample handling, different flow approaches were used for the development of simple, robust, cheap and automated analytical procedures. The first procedure was based on a sequential injection analysis (SIA) system for the determination of iron in coastal waters. With the goal of reaching low levels of iron, a LWCC was coupled to the system. This procedure used a doubled-line SIA system to improve mixing conditions between sample and reagents. The detection was based on a colorimetric reaction and two different reagents (ferrozine and 1,10-phenanthroline) were tested. The absorbance measurements were carried out at the wavelengths of 512 and 562 nm for the detection of iron-1,10-phenathroline and iron-ferrozine complex, respectively. An interference study was performed for both reagents. The developed method was also applied to natural waters (river, well, ground, potable and sea waters) and then compared with the reference procedure. One certified reference water sample was used to test the accuracy of the developed method. The objective of the second work was to determine iron at lower levels than the previous work and, as a consequence, to measure the levels of iron in ocean waters. With this in mind, a LWCC and a pre-concentration resin were coupled to a multisyringe flow injection analysis (MSFIA) system. Two different pre-concentration resins (Chelex 100 and NTA Superflow) were tested and evaluated. The determination of iron was also based on a colorimetric reaction and two reagents were tested, ferrozine and ammonium thiocyanate. The reactions were monitored at the wavelengths of 480 and 562 nm for the detection of iron-ammonium thiocyanate and iron-ferrozine complex, respectively. The accuracy was assessed using a certified reference water sample. A multi-parametric system for the spectrophotometric determination of zinc and copper at low levels in waters was the third work of this thesis. To attain this objective, a LWCC was coupled to a MSFIA system. The developed procedure for both analytes was based on a colorimetric reaction with zincon reagent at different pH values and monitored at 620 nm. Zincon reagent reacts only with copper at pH 5 and with copper and zinc at pH 9. An interference study for both determinations was carried out. The developed work was also applied to natural waters and three certified reference water samples. Subsequently, a multi-pumping flow system (MPFS) coupled with a LWCC was developed for the determination of titanium. This determination was based on the colorimetric reaction of titanium with chromotropic acid and the absorbance measurements were carried out at 425 nm. An interference study was performed in order to evaluate possible interferences. The developed procedure was applied to natural waters as well as to sunscreen formulations (the results were compared with the reference procedure). The accuracy was assessed with one certified lake sediment. The development of a spectrophotmetric method for bromate determination in waters at trace levels was the last work of this thesis. With this objective, a LWCC was coupled to a MPFS. The proposed methodology was based on a colorimetric reaction and two different colour reagents were tested, chlorpromazine and trifluoperazine. The lack of repeatability detected in this approach led to the development of a FIA approach in order to find out the reasons of this occurrence.
520
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Nesta tese, utilizou-se uma celula de fluxo de percurso optico longo na determinacao espectrofotometrica de varios analitos em diferentes tipos de agua. Com o proposito de manusear/transportar as amostras, varios sistemas de fluxo foram utilizados de forma a desenvolver procedimentos analiticos mais simples, robustos, automatizados e de baixo custo. O primeiro procedimento baseou-se no uso de um sistema de injeccao sequencial para a determinacao de ferro em aguas estuarinas. Com o objectivo de determinar os niveis baixos de ferro presente neste tipo de amostra, acoplou-se ao sistema uma celula de fluxo de percurso optico longo. Este procedimento utilizou um sistema de injeccao sequencial de duplo canal de forma a melhorar a mistura entre amostra e reagentes. A deteccao baseou-se numa reaccao colorimetrica e dois reagentes foram testados (ferrozina e 1,10-fenantrolina). As medidas espectrofotometricas foram realizadas aos comprimentos de onde de 512 e 562 nm para a deteccao dos complexos formados de ferro-1,10-fenantrolina e ferro-ferrozina, respectivamente. Realizou-se um estudo de possiveis interferentes para ambos os reagentes. O metodo desenvolvido foi igualmente aplicado a diferentes tipos de agua (aguas de rio, poco, mina, mar e amostras de agua potaveis) e os resultados obtidos foram comparados com o procedimento de referencia. Usou-se uma amostra de agua certificada de forma a comprovar a exactidao do metodo desenvolvido. O segundo metodo desenvolvido teve como principal objectivo determinar ferro em concentracoes mais baixas do que no trabalho anterior e assim atingir os valores de ferro presentes em aguas do mar. De forma a poder atingir este objectivo, uma celula de percurso optico longo e uma coluna de pre-concentracao foram acopladas a um sistema de fluxo baseado numa multi-seringa. Dois tipos de colunas de pre-concentracao, Chelex 100 e NTA Superflow, foram testadas e avaliadas. A determinacao de ferro baseou-se numa reaccao colorimetrica e foram testados dois reagents (ferrozina e tiocianato de amonio). As medidas espectrofotometricas foram realizadas aos comprimentos de onda de 480 e 562 nm para a deteccao dos complexos formados de ferro-tiocianato de amonio e ferro-ferrozina, respectivamente. A exactidao deste procedimento foi avaliada atraves de uma amostra de agua certificada. O terceiro procedimento realizado nesta tese envolveu um sistema multiparametrico para a determinacao espectrofotometrica de zinco e cobre em aguas a concentracoes baixas foi. Com este intuito, acoplou-se uma celula de fluxo de percurso optico longo a um sistema de fluxo baseado numa multi-seringa. O procedimento desenvolvido para ambos os analitos baseou-se numa reaccao colorimetrica com o reagente zincon a diferentes valores de pH e monitorizada a 620 nm. A pH 5 o reagente zincon reage apenas com o cobre e a pH 9 com ambos. Foi efectuado para ambos os analitos um estudo de possiveis interferentes. O procedimento desenvolvido foi igualmente aplicado a diferentes tipos de amostras de agua e a tres amostras de aguas certificadas. O quarto metodo desenvolvido visou determinar titanio a concentracoes muito baixas. Neste procedimento utilizou-se um sistema de fluxo baseado em micro-bombas com uma celula de fluxo de percurso optico longo acoplada. A determinacao baseou-se novamente numa reaccao colorimetrica entre o titanio e o acido cromotropico e a deteccao foi realizada a 425 nm. Foi efectuado um estudo de interferentes com o intuito de avaliar possiveis interferencias. O procedimento desenvolvido foi aplicado a diferentes tipos de agua e a amostras de cremes solares (os resultados obtidos para os cremes solares foram comparados com o procedimento de referencia). A exactidao deste metodo foi avaliada atraves de uma amostra certificada de um sedimento de lago O desenvolvimento de um metodo espectrofotometrico para a determinacao de bromato em aguas a concentracoes baixas foi o ultimo trabalho desta tese. Com este objectivo utilizou-se uma celula de fluxo de percurso optico longo acoplada a um sistema de fluxo baseado em multi-bombas. A metodologia proposta baseou-se igualmente numa reaccao colorimetrica e foram testados dois reagentes (cloropromazina e trifluoperazina). A falta de repetibilidade detectada neste sistema levou ao desenvolvimento de um sistema de analise por injeccao em fluxo com o objectivo de determinar as causas deste acontecimento.
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