Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica.
Autor(a) principal: | |
---|---|
Data de Publicação: | 2004 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFSCAR |
Texto Completo: | https://repositorio.ufscar.br/handle/ufscar/6313 |
Resumo: | In the present work is described computer-controlled flow systems designed for process control of L-alanine synthesis and for bromide determination in this amino acid, presented as a contaminant species. Since the analytical systems were computer controlled, all the procedures steps, such as, stopped flow, dilution, pH adjustment, analyte concentration and sample clean up, were performed without operator assistance. In order to carry out chemiluminescent reaction, a simple and low cost device (ca. US$ 150) that comprises two photodiodes fixed in lab-made Perspex flow cell was proposed. Regarding L-alanina determination, it was exploited the L-amino acid oxidize enzyme reaction. In this system, the sample was injected into a carrier stream, passing through a column packed with this immobilized enzyme. The product of the amino acid oxidation, hydrogen peroxide, was determined by the chemiluminescent reaction with luminol. The interfering species of the enzymatic reaction was suppressed by coupling in the flow system a column packed with a strong anionic resin. A linear concentration range between 0.5 and 25 mmol L-1 and a 0.08 mmol L-1limit of detection were some of the analytical characteristics of this system. Regarding the chemiluminescent bromide determination, the procedure was based on bromide oxidation by chloramine-T followed by the reaction of the formed bromine with luminol. In order to minimize the interference of alanina in the chemiluminescent reaction, a column packed with a strong anionic resin was used for analyte concentration and sample clean up. The analytical features obtained were a linear range between 0.010 and 1.000 mg L-1 (r=0.999) and a limit of detection of 1 µg L-1 of Br-. Also in this work is reported the development and the characterization of a lowcost device for NO2 determination in atmosphere exploiting the Griess-Slatzman reaction. The NO2 was sampled from the atmosphere by a porous membrane tube, which was also used as flow cell. To monitor the colored-forming reaction, it was constructed a dual-wavelength LED-based spectrophotometer. With the proposed device it was obtained a 0.5 ppbv limit of detection of NO2, a low reagent consumption (100 µL per determination), 5 % relative standard deviation for 5 ppbv NO2 sample concentration and long term stability, at least 168 hours without requiring calibration procedure. |
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Borges, Eduardo Poggi eReis, Boaventura Freire doshttp://genos.cnpq.br:12010/dwlattes/owa/prc_imp_cv_int?f_cod=K4788963T0http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4777513T26ca69764-add4-451e-a06b-b6a946a111dc2016-06-02T20:34:54Z2005-05-062016-06-02T20:34:54Z2004-05-14BORGES, Eduardo Poggi e. Development of a device and automatic analytical procedures exploiting chemiluminescent and spectrophotometric detection. 2004. 135 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2004.https://repositorio.ufscar.br/handle/ufscar/6313In the present work is described computer-controlled flow systems designed for process control of L-alanine synthesis and for bromide determination in this amino acid, presented as a contaminant species. Since the analytical systems were computer controlled, all the procedures steps, such as, stopped flow, dilution, pH adjustment, analyte concentration and sample clean up, were performed without operator assistance. In order to carry out chemiluminescent reaction, a simple and low cost device (ca. US$ 150) that comprises two photodiodes fixed in lab-made Perspex flow cell was proposed. Regarding L-alanina determination, it was exploited the L-amino acid oxidize enzyme reaction. In this system, the sample was injected into a carrier stream, passing through a column packed with this immobilized enzyme. The product of the amino acid oxidation, hydrogen peroxide, was determined by the chemiluminescent reaction with luminol. The interfering species of the enzymatic reaction was suppressed by coupling in the flow system a column packed with a strong anionic resin. A linear concentration range between 0.5 and 25 mmol L-1 and a 0.08 mmol L-1limit of detection were some of the analytical characteristics of this system. Regarding the chemiluminescent bromide determination, the procedure was based on bromide oxidation by chloramine-T followed by the reaction of the formed bromine with luminol. In order to minimize the interference of alanina in the chemiluminescent reaction, a column packed with a strong anionic resin was used for analyte concentration and sample clean up. The analytical features obtained were a linear range between 0.010 and 1.000 mg L-1 (r=0.999) and a limit of detection of 1 µg L-1 of Br-. Also in this work is reported the development and the characterization of a lowcost device for NO2 determination in atmosphere exploiting the Griess-Slatzman reaction. The NO2 was sampled from the atmosphere by a porous membrane tube, which was also used as flow cell. To monitor the colored-forming reaction, it was constructed a dual-wavelength LED-based spectrophotometer. With the proposed device it was obtained a 0.5 ppbv limit of detection of NO2, a low reagent consumption (100 µL per determination), 5 % relative standard deviation for 5 ppbv NO2 sample concentration and long term stability, at least 168 hours without requiring calibration procedure.No presente trabalho são apresentados sistemas de análises em fluxo projetados para o controle do processo de síntese de L-alanina e para a determinação de brometo presente como contaminante no aminoácido. Os sistemas analíticos foram controlados por um computador, de forma que todas as etapas do procedimento de análise eram realizadas automaticamente sem a interferência do operador. Como os procedimentos foram propostos utilizando detecção quimiluminescente, inicialmente foi desenvolvido um luminômetro utilizando dois fotodiodos e uma cela de fluxo construída em acrílico. Em relação ao procedimento para determinação de L-alanina, foi utilizada a enzima L-aminoácido oxidase. Neste sistema, a amostra era inserida em um fluxo transportador e em seguida passava por uma coluna contendo a enzima. O peróxido de hidrogênio, formado na reação de oxidação do aminoácido pela enzima, foi determinado pela reação de quimiluminescência do luminol catalisada pelo hexacianoferrato de potássio. As espécies interferentes na reação enzimática foram eliminadas com o uso de uma resina aniônica forte. Como características analíticas pode-se citar uma faixa de resposta linear entre 0,5 e 25,0 mmol L-1 e um limite de detecção de 0,08 mmol L-1 de L-alanina. Com respeito ao sistema para determinação de brometo por quimiluminescência, foi utilizado o reagente cloramina-T para oxidação deste íon a Br2 e posterior reação com o luminol. Para minimizar a interferência causada pela alanina, foi utilizada uma coluna preenchida com resina aniônica, que tinha a dupla função: concentrar os íons brometo e eliminar a alanina. Como características analíticas obteve-se uma resposta linear na faixa de concentração entre 0,010 e 1,000 mg L-1 (r=0,999) e um limite de detecção estimado em 1 µg L-1. Ainda neste trabalho, é relatado o desenvolvimento de um micro-dispositivo de fluxo de baixo custo para a determinação de NO2 na atmosfera. Para a detecção do analito foi explorada a reação colorimétrica de Griss-Saltzman. O NO2 foi coletado do ar atmosférico através de um microtubo de membrana porosa que devido à capacidade de transmitir luz, foi também utilizado como cela de fluxo. Para o monitoramento do produto colorido da reação, foi construído um espectrofotômetro utilizando LEDs (Light Emitting Diode) e um fotodiodo. Com a instrumentação proposta, obteve-se um baixo limite de detecção para NO2 de 0,5 ppbv, um baixo consumo de reagente (100 µL por determinação) e um desvio padrão relativo de 5 % para amostras típicas de 5,0 ppbv. Outra característica analítica favorável deste sistema foi a possibilidade de operação contínua durante longos períodos de tempo (pelo menos 168 horas) sem a necessidade de calibração.Universidade Federal de Minas Geraisapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarBRInstrumentaçãoAnálise por injeção de fluxoEspectrofotometriaQuimiluminescenciaCIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICADesenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica.Development of a device and automatic analytical procedures exploiting chemiluminescent and spectrophotometric detectioninfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesis-1-12b413d0a-54cd-4772-9b04-7f420af93d9ainfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINALTeseEPB.pdfapplication/pdf1174021https://repositorio.ufscar.br/bitstream/ufscar/6313/1/TeseEPB.pdf702dba663d651289ad9360726a6fb0bfMD51THUMBNAILTeseEPB.pdf.jpgTeseEPB.pdf.jpgIM Thumbnailimage/jpeg9177https://repositorio.ufscar.br/bitstream/ufscar/6313/2/TeseEPB.pdf.jpg2513d2b322bab237ed8dfe5de888fd79MD52ufscar/63132023-09-18 18:31:11.061oai:repositorio.ufscar.br:ufscar/6313Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-09-18T18:31:11Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false |
dc.title.por.fl_str_mv |
Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica. |
dc.title.alternative.eng.fl_str_mv |
Development of a device and automatic analytical procedures exploiting chemiluminescent and spectrophotometric detection |
title |
Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica. |
spellingShingle |
Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica. Borges, Eduardo Poggi e Instrumentação Análise por injeção de fluxo Espectrofotometria Quimiluminescencia CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
title_short |
Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica. |
title_full |
Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica. |
title_fullStr |
Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica. |
title_full_unstemmed |
Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica. |
title_sort |
Desenvolvimento de instrumentos e procedimentos analíticos automáticos com detecção quimiluminescente e espectrofotométrica. |
author |
Borges, Eduardo Poggi e |
author_facet |
Borges, Eduardo Poggi e |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4777513T2 |
dc.contributor.author.fl_str_mv |
Borges, Eduardo Poggi e |
dc.contributor.advisor1.fl_str_mv |
Reis, Boaventura Freire dos |
dc.contributor.advisor1Lattes.fl_str_mv |
http://genos.cnpq.br:12010/dwlattes/owa/prc_imp_cv_int?f_cod=K4788963T0 |
dc.contributor.authorID.fl_str_mv |
6ca69764-add4-451e-a06b-b6a946a111dc |
contributor_str_mv |
Reis, Boaventura Freire dos |
dc.subject.por.fl_str_mv |
Instrumentação Análise por injeção de fluxo Espectrofotometria Quimiluminescencia |
topic |
Instrumentação Análise por injeção de fluxo Espectrofotometria Quimiluminescencia CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
description |
In the present work is described computer-controlled flow systems designed for process control of L-alanine synthesis and for bromide determination in this amino acid, presented as a contaminant species. Since the analytical systems were computer controlled, all the procedures steps, such as, stopped flow, dilution, pH adjustment, analyte concentration and sample clean up, were performed without operator assistance. In order to carry out chemiluminescent reaction, a simple and low cost device (ca. US$ 150) that comprises two photodiodes fixed in lab-made Perspex flow cell was proposed. Regarding L-alanina determination, it was exploited the L-amino acid oxidize enzyme reaction. In this system, the sample was injected into a carrier stream, passing through a column packed with this immobilized enzyme. The product of the amino acid oxidation, hydrogen peroxide, was determined by the chemiluminescent reaction with luminol. The interfering species of the enzymatic reaction was suppressed by coupling in the flow system a column packed with a strong anionic resin. A linear concentration range between 0.5 and 25 mmol L-1 and a 0.08 mmol L-1limit of detection were some of the analytical characteristics of this system. Regarding the chemiluminescent bromide determination, the procedure was based on bromide oxidation by chloramine-T followed by the reaction of the formed bromine with luminol. In order to minimize the interference of alanina in the chemiluminescent reaction, a column packed with a strong anionic resin was used for analyte concentration and sample clean up. The analytical features obtained were a linear range between 0.010 and 1.000 mg L-1 (r=0.999) and a limit of detection of 1 µg L-1 of Br-. Also in this work is reported the development and the characterization of a lowcost device for NO2 determination in atmosphere exploiting the Griess-Slatzman reaction. The NO2 was sampled from the atmosphere by a porous membrane tube, which was also used as flow cell. To monitor the colored-forming reaction, it was constructed a dual-wavelength LED-based spectrophotometer. With the proposed device it was obtained a 0.5 ppbv limit of detection of NO2, a low reagent consumption (100 µL per determination), 5 % relative standard deviation for 5 ppbv NO2 sample concentration and long term stability, at least 168 hours without requiring calibration procedure. |
publishDate |
2004 |
dc.date.issued.fl_str_mv |
2004-05-14 |
dc.date.available.fl_str_mv |
2005-05-06 2016-06-02T20:34:54Z |
dc.date.accessioned.fl_str_mv |
2016-06-02T20:34:54Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
BORGES, Eduardo Poggi e. Development of a device and automatic analytical procedures exploiting chemiluminescent and spectrophotometric detection. 2004. 135 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2004. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/6313 |
identifier_str_mv |
BORGES, Eduardo Poggi e. Development of a device and automatic analytical procedures exploiting chemiluminescent and spectrophotometric detection. 2004. 135 f. Tese (Doutorado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2004. |
url |
https://repositorio.ufscar.br/handle/ufscar/6313 |
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por |
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por |
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-1 -1 |
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info:eu-repo/semantics/openAccess |
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openAccess |
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application/pdf |
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Universidade Federal de São Carlos |
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Programa de Pós-Graduação em Química - PPGQ |
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UFSCar |
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BR |
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Universidade Federal de São Carlos |
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