Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais

Bibliographic Details
Main Author: Freire, Emerson dos Santos
Publication Date: 2019
Format: Master thesis
Language: por
Source: Repositório Institucional da Universidade Federal de Alagoas (UFAL)
Download full: http://www.repositorio.ufal.br/handle/riufal/6619
Summary: The contamination of aquatic environments by trace elements, such as Hg, has revealed the importance of developing studies that involve the determination and removal of these elements in aquatic environments, highlighting, in this context, the use of resins that act as promising chelating agents for the removal of metals in water, due to the multiadsorbent function of these materials. The objective of this work was to synthesize a resin based on Melamina-Tiourea-Formaldehyde (MTF), characterize and apply in aqueous samples of the Mundaú lagoon, Alagoas - Brazil. The resin was synthesized by a polymerization reaction in a molar ratio of 1:5:1, melamine, formaldehyde and thiourea, respectively. By way of comparison, Melamine-Urea-Formaldehyde (MUF) was also synthesized under the same conditions as MTF. The characterization of the resin was performed by X-ray diffraction (XRD), adsorption-desorption analysis of nitrogen by the BET method, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The application was initially performed with standard of inorganic Hg(II). Resin mass (5 to 50 mg), standard concentration (5 to 8000 μg L-1) adsorption time, pH (5.0, 7.0 and 9.0) and study of adsorption kinetics were evaluated. After optimization, the adsorption profiles of different mercury species by MTF resin (Hg(II); CH3Hg+; C2H5Hg+; PhHg+) were evaluated, initially in standards and then in water samples collected in Mundaú Lagoon, by comparing the concentrations before and after adsorption, which were determined using atomic fluorescence spectrometry with cold vapor (CV AFS). From the DRX analysis, it can be inferred that MTF and MUF resins have characteristics of amorphous material. The BET data revealed information about the pore volume of the MTF resin, the diameter and the surface area with measurements of 0.027 cm3 g-1, 33 Å and 47.7 m2 g-1, respectively. Through TGA characterization, it was observed that MTF and MUF resins have a thermal stability between 75 and 80 °C and their combustion processes are composed of three stages. MTF does not have a hygroscopic profile. The images obtained by SEM showed an irregular structure with microspheres for MTF and a more compact structure, with a rough surface for MUF. Preliminary adsorption tests performed with standard solutions of Hg(II) were promising and thus, the optimization of adsorption conditions were performed with inorganic Hg(II) standards.Applying the results in the pseudo-primary and second order and Weber-Morris kinetics equations, a better linearity of the results was observed when applied to the pseudo-second order equation for adsorption of Hg(II) by MTF. The adsorption of inorganic Hg(II) by MTF was immediate in all pH conditions, reaching 92 % when using mass of 30 mg of resin. With a view to environmental application, the pH condition selected was pH 7.0. The maximum adsorption capacity was not reached for the concentration range used (5 to 8000 μg L-1of Hg(II)), being increasing. The adsorption capacities for each species of mercury used were: 87 % of Hg(II); 85 % of CH3Hg+; 93 % of C2H5Hg+ and 96 % of PhHg+ at pH 7.0. The results demonstrated a promising application of synthesised resin for the removal of Hg(II) species in aquatic environments contaminated with this element.
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spelling Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientaisSynthesis and characterization of melamine, formaldehyde and thiourea resin for mercury remediation in environmental samplesÁgua – Teor de Elementos traçosResinasPolimerizaçãoÁgua contaminadaProdutos químicosMercúrioMundaú, Lagoa (AL)Water - Content of trace elementsResinPolymerizationContaminated waterChemicalsMercuryMundaú LagoonCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICAThe contamination of aquatic environments by trace elements, such as Hg, has revealed the importance of developing studies that involve the determination and removal of these elements in aquatic environments, highlighting, in this context, the use of resins that act as promising chelating agents for the removal of metals in water, due to the multiadsorbent function of these materials. The objective of this work was to synthesize a resin based on Melamina-Tiourea-Formaldehyde (MTF), characterize and apply in aqueous samples of the Mundaú lagoon, Alagoas - Brazil. The resin was synthesized by a polymerization reaction in a molar ratio of 1:5:1, melamine, formaldehyde and thiourea, respectively. By way of comparison, Melamine-Urea-Formaldehyde (MUF) was also synthesized under the same conditions as MTF. The characterization of the resin was performed by X-ray diffraction (XRD), adsorption-desorption analysis of nitrogen by the BET method, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The application was initially performed with standard of inorganic Hg(II). Resin mass (5 to 50 mg), standard concentration (5 to 8000 μg L-1) adsorption time, pH (5.0, 7.0 and 9.0) and study of adsorption kinetics were evaluated. After optimization, the adsorption profiles of different mercury species by MTF resin (Hg(II); CH3Hg+; C2H5Hg+; PhHg+) were evaluated, initially in standards and then in water samples collected in Mundaú Lagoon, by comparing the concentrations before and after adsorption, which were determined using atomic fluorescence spectrometry with cold vapor (CV AFS). From the DRX analysis, it can be inferred that MTF and MUF resins have characteristics of amorphous material. The BET data revealed information about the pore volume of the MTF resin, the diameter and the surface area with measurements of 0.027 cm3 g-1, 33 Å and 47.7 m2 g-1, respectively. Through TGA characterization, it was observed that MTF and MUF resins have a thermal stability between 75 and 80 °C and their combustion processes are composed of three stages. MTF does not have a hygroscopic profile. The images obtained by SEM showed an irregular structure with microspheres for MTF and a more compact structure, with a rough surface for MUF. Preliminary adsorption tests performed with standard solutions of Hg(II) were promising and thus, the optimization of adsorption conditions were performed with inorganic Hg(II) standards.Applying the results in the pseudo-primary and second order and Weber-Morris kinetics equations, a better linearity of the results was observed when applied to the pseudo-second order equation for adsorption of Hg(II) by MTF. The adsorption of inorganic Hg(II) by MTF was immediate in all pH conditions, reaching 92 % when using mass of 30 mg of resin. With a view to environmental application, the pH condition selected was pH 7.0. The maximum adsorption capacity was not reached for the concentration range used (5 to 8000 μg L-1of Hg(II)), being increasing. The adsorption capacities for each species of mercury used were: 87 % of Hg(II); 85 % of CH3Hg+; 93 % of C2H5Hg+ and 96 % of PhHg+ at pH 7.0. The results demonstrated a promising application of synthesised resin for the removal of Hg(II) species in aquatic environments contaminated with this element.CAPES - Coordenação de Aperfeiçoamento de Pessoal de Nível SuperiorA contaminação de corpos d’água por elementos traço, a exemplo do Hg, tem revelado a importância do desenvolvimento de estudos que envolvam a determinação e remoção desses elementos nos ambientes aquáticos, destacando, neste contexto, o emprego de resinas que atuem como agentes quelantes promissores para a remoção de metais em águas, devido à função multiadsorvente destes materiais. O objetivo deste trabalho foi sintetizar uma resina à base de Melamina-Tioureia-Formaldeído (MTF), caracterizar e aplicar em amostras aquosas da lagoa Mundaú, Alagoas – Brasil. A resina foi sintetizada por meio de uma reação de polimerização numa razão molar de 1:5:1, melamina, formaldeído e tioureia, respectivamente. A título comparativo, também foi sintetizada a resina Melamina-Ureia-Formaldeído (MUF) nas mesmas condições da MTF. A caracterização da resina foi realizada por difração de raios- X (DRX), análise de adsorção-dessorção de nitrogênio pelo método de BET, análise termogravimétrica (TGA), microscopia eletrônica de varredura (MEV) e análise de adsorçãodessorção de nitrogênio pelo método de BET, essa última apenas para a resina MTF. A aplicação foi realizada inicialmente com padrão de Hg(II) inorgânico. Foram avaliados massa de resina (5 a 50 mg), concentração de padrão (5 a 8000 μg L-1) tempo de adsorção, pH (5,0; 7,0 e 9,0) e estudo da cinética de adsorção. Após a otimização, foram avaliados os perfis de adsorção de diferentes espécies de mercúrio pela resina MTF (Hg(II); CH3Hg+; C2H5Hg+; PhHg+), inicialmente em padrões e, em seguida, em amostras de água coletadas na lagoa Mundaú, mediante comparação das concentrações antes e após a adsorção as quais foram determinadas, empregando espectrometria de fluorescência atômica com vapor frio (CV AFS). A partir da análise de DRX, pode-se inferir que as resinas MTF e MUF possuem característica de material amorfo. Os dados de BET revelaram informações acerca do volume do poro da resina MTF, do diâmetro e da área superficial com medidas de 0,027 cm3 g-1, 33 Å e 47,7 m2 g-1, respectivamente. Através da caracterização por TGA, observou-se que as resinas MTF e MUF têm uma estabilidade térmica entre 75 e 80 °C e seus processos de combustão são compostos por três estágios. A MTF não possui perfil higroscópico. As imagens obtidas por MEV evidenciaram estrutura irregular com microesferas para MTF e uma estrutura mais compacta, com superfície rugosa para a MUF. Os ensaios preliminares de adsorção realizados com soluções padrão de Hg(II) foram promissores e, dessa forma, a otimização das condições de adsorção foram realizadas com padrões de Hg(II) inorgânico. Aplicando os resultados nas equações de cinética de pseudo-primeira e segunda ordem, e Weber-Morris, observou-se uma melhor linearidade dos resultados quando aplicados à equação de pseudo-segunda ordem para a adsorção de Hg(II) por MTF. A adsorção do Hg(II) inorgânico pela MTF foi imediata em todas as condições de pH, chegando a 92 % ao empregar a massa de 30 mg de resina. Com vistas à aplicação ambiental, a condição de pH selecionada foi pH 7,0. A capacidade máxima de adsorção não foi atingida para o intervalo de concentrações empregado (5 a 8000 μg L-1) de Hg(II), apresentando-se crescente. As capacidades de adosorção para cada espécie de mercúrio empregada foram: 87 % de Hg(II); 85 % de CH3Hg+; 93 % de C2H5Hg+ e 96 % de PhHg+ em pH 7,0. Os resultados demonstraram uma aplicação promissora da resina sintetizada para a remoção de espécies de mercúrio em corpos d’água contaminados com este elemento.Universidade Federal de AlagoasBrasilPrograma de Pós-Graduação em Química e BiotecnologiaUFALAnunciação, Daniela Santoshttp://lattes.cnpq.br/9549507796312647Santos, Josué Carinhanha Caldashttp://lattes.cnpq.br/3735618604163061Barbosa, Cintya D’Angeles do Espírito Santohttp://lattes.cnpq.br/1197509333716425Silva, Julio Cosme Santos dahttp://lattes.cnpq.br/0911191668534666Godoi, Madson dehttp://lattes.cnpq.br/2526885257147343Freire, Emerson dos Santos2020-02-10T18:52:30Z2019-12-202020-02-10T18:52:30Z2019-06-23info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfFreire, Emerson dos Santos. Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais. 2019. 82 f. Dissertação (Mestrado em Química Analítica) – Instituto de Química e Biotecnologia, Programa de Pós-Graduação em Química e Biotecnologia, Universidade Federal de Alagoas, Maceió, 2019.http://www.repositorio.ufal.br/handle/riufal/6619porinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da Universidade Federal de Alagoas (UFAL)instname:Universidade Federal de Alagoas (UFAL)instacron:UFAL2020-02-10T18:52:30Zoai:www.repositorio.ufal.br:riufal/6619Repositório InstitucionalPUBhttp://www.repositorio.ufal.br/oai/requestri@sibi.ufal.bropendoar:2020-02-10T18:52:30Repositório Institucional da Universidade Federal de Alagoas (UFAL) - Universidade Federal de Alagoas (UFAL)false
dc.title.none.fl_str_mv Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais
Synthesis and characterization of melamine, formaldehyde and thiourea resin for mercury remediation in environmental samples
title Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais
spellingShingle Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais
Freire, Emerson dos Santos
Água – Teor de Elementos traços
Resinas
Polimerização
Água contaminada
Produtos químicos
Mercúrio
Mundaú, Lagoa (AL)
Water - Content of trace elements
Resin
Polymerization
Contaminated water
Chemicals
Mercury
Mundaú Lagoon
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
title_short Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais
title_full Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais
title_fullStr Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais
title_full_unstemmed Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais
title_sort Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais
author Freire, Emerson dos Santos
author_facet Freire, Emerson dos Santos
author_role author
dc.contributor.none.fl_str_mv Anunciação, Daniela Santos
http://lattes.cnpq.br/9549507796312647
Santos, Josué Carinhanha Caldas
http://lattes.cnpq.br/3735618604163061
Barbosa, Cintya D’Angeles do Espírito Santo
http://lattes.cnpq.br/1197509333716425
Silva, Julio Cosme Santos da
http://lattes.cnpq.br/0911191668534666
Godoi, Madson de
http://lattes.cnpq.br/2526885257147343
dc.contributor.author.fl_str_mv Freire, Emerson dos Santos
dc.subject.por.fl_str_mv Água – Teor de Elementos traços
Resinas
Polimerização
Água contaminada
Produtos químicos
Mercúrio
Mundaú, Lagoa (AL)
Water - Content of trace elements
Resin
Polymerization
Contaminated water
Chemicals
Mercury
Mundaú Lagoon
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
topic Água – Teor de Elementos traços
Resinas
Polimerização
Água contaminada
Produtos químicos
Mercúrio
Mundaú, Lagoa (AL)
Water - Content of trace elements
Resin
Polymerization
Contaminated water
Chemicals
Mercury
Mundaú Lagoon
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
description The contamination of aquatic environments by trace elements, such as Hg, has revealed the importance of developing studies that involve the determination and removal of these elements in aquatic environments, highlighting, in this context, the use of resins that act as promising chelating agents for the removal of metals in water, due to the multiadsorbent function of these materials. The objective of this work was to synthesize a resin based on Melamina-Tiourea-Formaldehyde (MTF), characterize and apply in aqueous samples of the Mundaú lagoon, Alagoas - Brazil. The resin was synthesized by a polymerization reaction in a molar ratio of 1:5:1, melamine, formaldehyde and thiourea, respectively. By way of comparison, Melamine-Urea-Formaldehyde (MUF) was also synthesized under the same conditions as MTF. The characterization of the resin was performed by X-ray diffraction (XRD), adsorption-desorption analysis of nitrogen by the BET method, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The application was initially performed with standard of inorganic Hg(II). Resin mass (5 to 50 mg), standard concentration (5 to 8000 μg L-1) adsorption time, pH (5.0, 7.0 and 9.0) and study of adsorption kinetics were evaluated. After optimization, the adsorption profiles of different mercury species by MTF resin (Hg(II); CH3Hg+; C2H5Hg+; PhHg+) were evaluated, initially in standards and then in water samples collected in Mundaú Lagoon, by comparing the concentrations before and after adsorption, which were determined using atomic fluorescence spectrometry with cold vapor (CV AFS). From the DRX analysis, it can be inferred that MTF and MUF resins have characteristics of amorphous material. The BET data revealed information about the pore volume of the MTF resin, the diameter and the surface area with measurements of 0.027 cm3 g-1, 33 Å and 47.7 m2 g-1, respectively. Through TGA characterization, it was observed that MTF and MUF resins have a thermal stability between 75 and 80 °C and their combustion processes are composed of three stages. MTF does not have a hygroscopic profile. The images obtained by SEM showed an irregular structure with microspheres for MTF and a more compact structure, with a rough surface for MUF. Preliminary adsorption tests performed with standard solutions of Hg(II) were promising and thus, the optimization of adsorption conditions were performed with inorganic Hg(II) standards.Applying the results in the pseudo-primary and second order and Weber-Morris kinetics equations, a better linearity of the results was observed when applied to the pseudo-second order equation for adsorption of Hg(II) by MTF. The adsorption of inorganic Hg(II) by MTF was immediate in all pH conditions, reaching 92 % when using mass of 30 mg of resin. With a view to environmental application, the pH condition selected was pH 7.0. The maximum adsorption capacity was not reached for the concentration range used (5 to 8000 μg L-1of Hg(II)), being increasing. The adsorption capacities for each species of mercury used were: 87 % of Hg(II); 85 % of CH3Hg+; 93 % of C2H5Hg+ and 96 % of PhHg+ at pH 7.0. The results demonstrated a promising application of synthesised resin for the removal of Hg(II) species in aquatic environments contaminated with this element.
publishDate 2019
dc.date.none.fl_str_mv 2019-12-20
2019-06-23
2020-02-10T18:52:30Z
2020-02-10T18:52:30Z
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.uri.fl_str_mv Freire, Emerson dos Santos. Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais. 2019. 82 f. Dissertação (Mestrado em Química Analítica) – Instituto de Química e Biotecnologia, Programa de Pós-Graduação em Química e Biotecnologia, Universidade Federal de Alagoas, Maceió, 2019.
http://www.repositorio.ufal.br/handle/riufal/6619
identifier_str_mv Freire, Emerson dos Santos. Síntese e caracterização de resina à base de melamina, tioureia e formaldeído para remediação de mercúrio em amostras ambientais. 2019. 82 f. Dissertação (Mestrado em Química Analítica) – Instituto de Química e Biotecnologia, Programa de Pós-Graduação em Química e Biotecnologia, Universidade Federal de Alagoas, Maceió, 2019.
url http://www.repositorio.ufal.br/handle/riufal/6619
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal de Alagoas
Brasil
Programa de Pós-Graduação em Química e Biotecnologia
UFAL
publisher.none.fl_str_mv Universidade Federal de Alagoas
Brasil
Programa de Pós-Graduação em Química e Biotecnologia
UFAL
dc.source.none.fl_str_mv reponame:Repositório Institucional da Universidade Federal de Alagoas (UFAL)
instname:Universidade Federal de Alagoas (UFAL)
instacron:UFAL
instname_str Universidade Federal de Alagoas (UFAL)
instacron_str UFAL
institution UFAL
reponame_str Repositório Institucional da Universidade Federal de Alagoas (UFAL)
collection Repositório Institucional da Universidade Federal de Alagoas (UFAL)
repository.name.fl_str_mv Repositório Institucional da Universidade Federal de Alagoas (UFAL) - Universidade Federal de Alagoas (UFAL)
repository.mail.fl_str_mv ri@sibi.ufal.br
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