Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns
Autor(a) principal: | |
---|---|
Data de Publicação: | 2015 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFU |
Texto Completo: | https://repositorio.ufu.br/handle/123456789/17448 https://doi.org/10.14393/ufu.di.2015.538 |
Resumo: | This work developed a flow system for pre-concentration and determination of fluoride by molecular absorption spectrophotometry using SPADNS method in water samples. The method is based on the reaction of fluoride ions with the complex zirconium and the trisodium salt of 1,8-dihydroxy-2- (4-sulfophenylazo) -naphthalene-3,6-disulphonic acid (SPADNS), leading to discoloration. The samples were pre-concentrated in a Tygon® minicolumn tube with 5 cm long and 2.0 mm internal diameter, containing Layered Double Hydroxides (NO3.Mg-Al LDH) used as adsorbent for the retention of fluoride ions. Thereafter, the fluorine ions were eluted with sodium hydroxide 0.5 mol L-1 and determined by SPADNS method. The flow system was constructed of solenoid valves, in order to improve analytical performance, as each independent valve injects the solutions so leading to a more efficient use of the reagents. The variables that affect the system such as the mass of adsorbent, type of eluent, eluent flow rate and pre-concentration, SPADNS concentration and pH effect were evaluated. The material was characterized by a variety of techniques, including Mid-Infrared Spectroscopy (FT-MIR) and Scanning Electron Microscopy (SEM). Surface area and the average diameter of the particles was also determined. The results of the optimal conditions, selected with the compromise between sensitivity and the analytical speed, was mass of adsorbent 150 mg; pre-concentration flow rate 3 mL min-1; elution flow rate 1 mL min-1, using as the eluent sodium hydroxide 0.5 mol L-1; hydrochloric acid concentration in SPADNS 1.8 mol L-1. The detection limit was 15 ug L-1, the limit of quantification of 50 ug L-1, relative standard deviation of 0.8 %, linear range of 50-500 ug L-1 and pre-concentration factor of 10.3. The accuracy of the method was evaluated by analysis of certified material ALPHA APS 1076 (Simulated Rain Water), the values were not significantly different at a 95% level of confidence with the certified value. The method was applied in the analysis of water and the levels found were below the maximum values established by Brazilian regulation. |
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2016-06-22T18:48:40Z2016-02-172016-06-22T18:48:40Z2015-12-16ROCHA, Diego Pessoa. Extraction and pre-concentration of fluoride in water and detection by the method of SPADNS. 2015. 81 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de Uberlândia, Uberlândia, 2015. Disponível em: https://doi.org/10.14393/ufu.di.2015.538https://repositorio.ufu.br/handle/123456789/17448https://doi.org/10.14393/ufu.di.2015.538This work developed a flow system for pre-concentration and determination of fluoride by molecular absorption spectrophotometry using SPADNS method in water samples. The method is based on the reaction of fluoride ions with the complex zirconium and the trisodium salt of 1,8-dihydroxy-2- (4-sulfophenylazo) -naphthalene-3,6-disulphonic acid (SPADNS), leading to discoloration. The samples were pre-concentrated in a Tygon® minicolumn tube with 5 cm long and 2.0 mm internal diameter, containing Layered Double Hydroxides (NO3.Mg-Al LDH) used as adsorbent for the retention of fluoride ions. Thereafter, the fluorine ions were eluted with sodium hydroxide 0.5 mol L-1 and determined by SPADNS method. The flow system was constructed of solenoid valves, in order to improve analytical performance, as each independent valve injects the solutions so leading to a more efficient use of the reagents. The variables that affect the system such as the mass of adsorbent, type of eluent, eluent flow rate and pre-concentration, SPADNS concentration and pH effect were evaluated. The material was characterized by a variety of techniques, including Mid-Infrared Spectroscopy (FT-MIR) and Scanning Electron Microscopy (SEM). Surface area and the average diameter of the particles was also determined. The results of the optimal conditions, selected with the compromise between sensitivity and the analytical speed, was mass of adsorbent 150 mg; pre-concentration flow rate 3 mL min-1; elution flow rate 1 mL min-1, using as the eluent sodium hydroxide 0.5 mol L-1; hydrochloric acid concentration in SPADNS 1.8 mol L-1. The detection limit was 15 ug L-1, the limit of quantification of 50 ug L-1, relative standard deviation of 0.8 %, linear range of 50-500 ug L-1 and pre-concentration factor of 10.3. The accuracy of the method was evaluated by analysis of certified material ALPHA APS 1076 (Simulated Rain Water), the values were not significantly different at a 95% level of confidence with the certified value. The method was applied in the analysis of water and the levels found were below the maximum values established by Brazilian regulation.O presente trabalho desenvolveu um sistema em fluxo para pré-concentração e determinação de fluoreto por espectrofotometria de absorção molecular utilizando o método de SPADNS em amostras de águas. O método baseia-se na reação de íons flúor com o complexo de zircônio e o sal trissódico do ácido 1,8- dihidroxi-2-(4-sulfofenilazo)-naftaleno-3,6-dissulfônico (SPADNS), levando a descoloração do mesmo. As amostras foram pré-concentradas em uma mini-coluna de tubo Tygon® com 5 cm de comprimento e 2,0 mm de diâmetro interno, contendo hidróxido duplo lamelar [NO3.Mg-Al HDL] como material adsorvente para retenção de íons flúor. Posteriormente, os íons flúor foram eluídos com hidróxido de sódio 0,5 mol L-1 e determinados pelo método de SPADNS. O sistema de análises por injeção em fluxo foi construído com válvulas solenoide, a fim de melhorar o desempenho analítico, uma vez que cada válvula gerencia independentemente as soluções levando a uma utilização mais eficiente dos reagentes. As variáveis que afetam a eficiência do sistema, tais como a massa do adsorvente, tipo de eluente, vazões do eluente e pré-concentração, concentração do SPADNS e efeito do pH foram avaliados. O material adsorvente foi caracterizado por meio de diversas técnicas, incluindo a espectroscopia de infravermelho médio (FT-MIR) e microscopia eletrônica de varredura (MEV). A área superficial, assim como o diâmetro médio das partículas também foi determinado. Os resultados das condições otimizadas, selecionados com o compromisso entre a sensibilidade e a velocidade analítica, foram massa do material adsorvente 150 mg; vazão de pré-concentração 3 mL min-1; vazão de eluição 1 mL min-1, utilizando como eluente hidróxido de sódio 0,5 mol L-1; concentração de ácido clorídrico no SPADNS 1,8 mol L-1. O limite de detecção foi de 15 μg L-1, limite de quantificação de 50 μg L-1, desvio padrão relativo de 0,8 %, faixa linear de 50-500 μg L-1 e fator de pré-concentração de 10,3. A exatidão do método foi avaliada pela análise do material de referência ALPHA APS 1076 (Simulated Rain Water), os valores obtidos não apresentaram diferença significativa a um nível de 95% de confiança com o valor de referência. O método foi aplicado na análise de águas e os níveis encontrados foram abaixo dos valores máximos estabelecidos pela legislação brasileira.Mestre em Químicaapplication/pdfporUniversidade Federal de UberlândiaPrograma de Pós-graduação em QuímicaUFUBRCiências Exatas e da TerraFIASPADNSFluoretoHidróxido duplo lamelarHidróxidosFluorideLayered double hydroxidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAExtração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de SpadnsExtraction and pre-concentration of fluoride in water and detection by the method of SPADNSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisCoelho, Nivia Maria Melohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4723022D3Veiga, Márcia Andreia Mesquita Silva dahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4797535U4Batista, Alex Domingueshttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4256613E7http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4465786Y6Rocha, Diego Pessoa81767346info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFUinstname:Universidade Federal de Uberlândia (UFU)instacron:UFUTHUMBNAILExtracaoPreConcentracaoLinha.pdf.jpgExtracaoPreConcentracaoLinha.pdf.jpgGenerated Thumbnailimage/jpeg1319https://repositorio.ufu.br/bitstream/123456789/17448/3/ExtracaoPreConcentracaoLinha.pdf.jpgfbbdc886ecb49004c495e66db84fef98MD53ORIGINALExtracaoPreConcentracaoLinha.pdfapplication/pdf2225257https://repositorio.ufu.br/bitstream/123456789/17448/1/ExtracaoPreConcentracaoLinha.pdfd68b82c5595356cacc4ce005a6377087MD51TEXTExtracaoPreConcentracaoLinha.pdf.txtExtracaoPreConcentracaoLinha.pdf.txtExtracted texttext/plain121662https://repositorio.ufu.br/bitstream/123456789/17448/2/ExtracaoPreConcentracaoLinha.pdf.txtebb075e7e1fffa6890c90808ae2c7330MD52123456789/174482021-07-21 23:50:47.436oai:repositorio.ufu.br:123456789/17448Repositório InstitucionalONGhttp://repositorio.ufu.br/oai/requestdiinf@dirbi.ufu.bropendoar:2024-04-26T15:12:05.272002Repositório Institucional da UFU - Universidade Federal de Uberlândia (UFU)false |
dc.title.por.fl_str_mv |
Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns |
dc.title.alternative.eng.fl_str_mv |
Extraction and pre-concentration of fluoride in water and detection by the method of SPADNS |
title |
Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns |
spellingShingle |
Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns Rocha, Diego Pessoa FIA SPADNS Fluoreto Hidróxido duplo lamelar Hidróxidos Fluoride Layered double hydroxides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns |
title_full |
Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns |
title_fullStr |
Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns |
title_full_unstemmed |
Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns |
title_sort |
Extração e pré-concentração em linha de flúor em águas e determinação pelo Metódo de Spadns |
author |
Rocha, Diego Pessoa |
author_facet |
Rocha, Diego Pessoa |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Coelho, Nivia Maria Melo |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4723022D3 |
dc.contributor.referee1.fl_str_mv |
Veiga, Márcia Andreia Mesquita Silva da |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4797535U4 |
dc.contributor.referee2.fl_str_mv |
Batista, Alex Domingues |
dc.contributor.referee2Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4256613E7 |
dc.contributor.authorLattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4465786Y6 |
dc.contributor.author.fl_str_mv |
Rocha, Diego Pessoa |
contributor_str_mv |
Coelho, Nivia Maria Melo Veiga, Márcia Andreia Mesquita Silva da Batista, Alex Domingues |
dc.subject.por.fl_str_mv |
FIA SPADNS Fluoreto Hidróxido duplo lamelar Hidróxidos |
topic |
FIA SPADNS Fluoreto Hidróxido duplo lamelar Hidróxidos Fluoride Layered double hydroxides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Fluoride Layered double hydroxides |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
This work developed a flow system for pre-concentration and determination of fluoride by molecular absorption spectrophotometry using SPADNS method in water samples. The method is based on the reaction of fluoride ions with the complex zirconium and the trisodium salt of 1,8-dihydroxy-2- (4-sulfophenylazo) -naphthalene-3,6-disulphonic acid (SPADNS), leading to discoloration. The samples were pre-concentrated in a Tygon® minicolumn tube with 5 cm long and 2.0 mm internal diameter, containing Layered Double Hydroxides (NO3.Mg-Al LDH) used as adsorbent for the retention of fluoride ions. Thereafter, the fluorine ions were eluted with sodium hydroxide 0.5 mol L-1 and determined by SPADNS method. The flow system was constructed of solenoid valves, in order to improve analytical performance, as each independent valve injects the solutions so leading to a more efficient use of the reagents. The variables that affect the system such as the mass of adsorbent, type of eluent, eluent flow rate and pre-concentration, SPADNS concentration and pH effect were evaluated. The material was characterized by a variety of techniques, including Mid-Infrared Spectroscopy (FT-MIR) and Scanning Electron Microscopy (SEM). Surface area and the average diameter of the particles was also determined. The results of the optimal conditions, selected with the compromise between sensitivity and the analytical speed, was mass of adsorbent 150 mg; pre-concentration flow rate 3 mL min-1; elution flow rate 1 mL min-1, using as the eluent sodium hydroxide 0.5 mol L-1; hydrochloric acid concentration in SPADNS 1.8 mol L-1. The detection limit was 15 ug L-1, the limit of quantification of 50 ug L-1, relative standard deviation of 0.8 %, linear range of 50-500 ug L-1 and pre-concentration factor of 10.3. The accuracy of the method was evaluated by analysis of certified material ALPHA APS 1076 (Simulated Rain Water), the values were not significantly different at a 95% level of confidence with the certified value. The method was applied in the analysis of water and the levels found were below the maximum values established by Brazilian regulation. |
publishDate |
2015 |
dc.date.issued.fl_str_mv |
2015-12-16 |
dc.date.accessioned.fl_str_mv |
2016-06-22T18:48:40Z |
dc.date.available.fl_str_mv |
2016-02-17 2016-06-22T18:48:40Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
ROCHA, Diego Pessoa. Extraction and pre-concentration of fluoride in water and detection by the method of SPADNS. 2015. 81 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de Uberlândia, Uberlândia, 2015. Disponível em: https://doi.org/10.14393/ufu.di.2015.538 |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufu.br/handle/123456789/17448 |
dc.identifier.doi.por.fl_str_mv |
https://doi.org/10.14393/ufu.di.2015.538 |
identifier_str_mv |
ROCHA, Diego Pessoa. Extraction and pre-concentration of fluoride in water and detection by the method of SPADNS. 2015. 81 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de Uberlândia, Uberlândia, 2015. Disponível em: https://doi.org/10.14393/ufu.di.2015.538 |
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https://repositorio.ufu.br/handle/123456789/17448 https://doi.org/10.14393/ufu.di.2015.538 |
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por |
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Universidade Federal de Uberlândia |
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Programa de Pós-graduação em Química |
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UFU |
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BR |
dc.publisher.department.fl_str_mv |
Ciências Exatas e da Terra |
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Universidade Federal de Uberlândia |
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