Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno
Autor(a) principal: | |
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Data de Publicação: | 2021 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFS |
Texto Completo: | https://ri.ufs.br/jspui/handle/riufs/14907 |
Resumo: | This work consisted in synthesizing magnetic hybrid materials consisting of cobalt ferrite, natural organic matter and graphene (CoFe2O4 /NOM/Graphene), and applying it as an adsorbent in the analytical methodology of BPA magnetic extraction in aqueous matrices. Initially, four hybrid materials were synthesized: ferrite from chloride (HFC), ferrite from sulfate (HFS), graphene from chloride (HGC) and graphene from sulfate (HGS). The X-ray diffraction technique demonstrated the formation of the cobalt ferrite phase in all synthesized materials, as well as that of graphene in hybrids. Spectroscopy in the infrared region revealed the presence of functional groups by stretching the O-H and C = O bonds characteristic of the presence of NOM, C = C of graphene, in addition to Fe-O of the ferrites. Transmission electron microscopy images revealed spherical nanoparticles with dimensions of 9.72 nm (HFC), 34.0 nm (HFS); 8.75 nm (HGC) e 43.9 nm (HGS). In addition, graphene sheets were observed in a few layers. Raman spectra confirmed the formation of cobalt ferrite, highlighting its inverse spinel type, and indicated the formation of graphene. The graphene formed showed few structural defects, and the number of layers was estimated as mono and double layer. The adsorption experiments showed the potential of graphene hybrids in the adsorption stage, 94.19% (HGS) and 97.95% (HGC). Optimization of this step resulted in the use of 50 mg of HGC and orbital agitation at 150 rpm for 5 minutes. Desorption was performed in 2.5 minutes at 150 rpm, using methanol as solvent, obtaining 99.19% of BPA desorbed. The analytical validation showed a correlation coefficient r = 1.00, LD = 0.022 μg L-1 and LQ = 0.072 μg L-1 . The reproducibility of the extraction procedure varies from 2.13 - 2.21% and shows excellent recoveries in the range of 99.33 – 104.4%. The method proved to be feasible for application in bottled, river and supply water samples with recoveries of 99.87 - 104.7%. Furthermore, the MSPE methodology used proved to be simple, fast and efficient for the extraction of BPA in aqueous matrices, in addition to the use of an eco-friendly adsorbent as a support. |
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Oliveira, Rhayza Victoria MatosRomão, Luciane Pimenta CruzCunha, Graziele da Costa2021-12-17T16:45:40Z2021-12-17T16:45:40Z2021-05-31OLIVEIRA, Rhayza Victoria Matos. Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno. 2021. 99 f. Dissertação (Mestrado em Química) – Universidade Federal de Sergipe, São Cristóvão, 2021.https://ri.ufs.br/jspui/handle/riufs/14907This work consisted in synthesizing magnetic hybrid materials consisting of cobalt ferrite, natural organic matter and graphene (CoFe2O4 /NOM/Graphene), and applying it as an adsorbent in the analytical methodology of BPA magnetic extraction in aqueous matrices. Initially, four hybrid materials were synthesized: ferrite from chloride (HFC), ferrite from sulfate (HFS), graphene from chloride (HGC) and graphene from sulfate (HGS). The X-ray diffraction technique demonstrated the formation of the cobalt ferrite phase in all synthesized materials, as well as that of graphene in hybrids. Spectroscopy in the infrared region revealed the presence of functional groups by stretching the O-H and C = O bonds characteristic of the presence of NOM, C = C of graphene, in addition to Fe-O of the ferrites. Transmission electron microscopy images revealed spherical nanoparticles with dimensions of 9.72 nm (HFC), 34.0 nm (HFS); 8.75 nm (HGC) e 43.9 nm (HGS). In addition, graphene sheets were observed in a few layers. Raman spectra confirmed the formation of cobalt ferrite, highlighting its inverse spinel type, and indicated the formation of graphene. The graphene formed showed few structural defects, and the number of layers was estimated as mono and double layer. The adsorption experiments showed the potential of graphene hybrids in the adsorption stage, 94.19% (HGS) and 97.95% (HGC). Optimization of this step resulted in the use of 50 mg of HGC and orbital agitation at 150 rpm for 5 minutes. Desorption was performed in 2.5 minutes at 150 rpm, using methanol as solvent, obtaining 99.19% of BPA desorbed. The analytical validation showed a correlation coefficient r = 1.00, LD = 0.022 μg L-1 and LQ = 0.072 μg L-1 . The reproducibility of the extraction procedure varies from 2.13 - 2.21% and shows excellent recoveries in the range of 99.33 – 104.4%. The method proved to be feasible for application in bottled, river and supply water samples with recoveries of 99.87 - 104.7%. Furthermore, the MSPE methodology used proved to be simple, fast and efficient for the extraction of BPA in aqueous matrices, in addition to the use of an eco-friendly adsorbent as a support.Este trabalho consistiu em sintetizar materiais híbridos magnéticos constituídos por ferrita de cobalto, matéria orgânica natural e grafeno (CoFe2O4/MON/Grafeno), e aplicá-los como adsorventes na metodologia analítica de extração em fase sólida magnética (MSPE) de BPA em matrizes aquosas. Inicialmente foram sintetizados quatro materiais híbridos: de ferrita a partir do cloreto (HFC), de ferrita a partir de sulfato (HFS), de grafeno a partir de cloreto (HGC) e de grafeno a partir de sulfato (HGS). A técnica de difração de raios X demonstrou a formação da fase de ferrita de cobalto em todos os materiais sintetizados, bem como a do grafeno nos híbridos. A espectroscopia na região de infravermelho revelou a presença de grupos funcionais através do estiramento das ligações O-H e C=O característicos da presença da MON, C=C de grafeno, além de Fe-O das ferritas. As imagens de microscopia eletrônica de transmissão revelaram nanopartículas esféricas com dimensão de 9,72 nm (HFC), 34,0 nm (HFS); 8,75 nm (HGC) e 43,9 nm (HGS). Além disso, foram observadas folhas de grafeno em poucas camadas. Os espectros Raman confirmaram a formação da ferrita de cobalto, destacando seu tipo espinélio inverso, e indicaram a formação do grafeno. O grafeno formado apresentou poucos defeitos estruturais, e o número de camadas foi estimado como mono e dupla camada. Os ensaios de adsorção mostraram o potencial dos híbridos de grafeno na etapa de adsorção, 94,19% (HGS) e 97,95% (HGC). A otimização desta etapa resultou na utilização de 50 mg de HGC e agitação orbital a 150 rpm durante 5 minutos. A dessorção foi realizada em 2,5 minutos, a 150 rpm, utilizando metanol como solvente, obtendo 99,19% de BPA dessorvido. A validação analítica apresentou coeficiente de correlação r = 1,00, LD= 0,022 μg L -1 e LQ = 0,072 μg L-1 . O procedimento de extração variou de 2,13 – 2,21% e apresentou excelentes recuperações na faixa de 99,33 -104,4%. O método mostrou-se viável para aplicação em amostras de água engarrafada, do rio e de abastecimento,com recuperações de 99,87 - 104,7%. Assim, a metodologia MSPE utilizada mostrou-se simples, rápida e eficiente para a extração de BPA em matrizes aquosas, além do emprego de um adsorvente ecoamigável como suporte.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESSão CristóvãoporQuímicaNanopartículasMateriais magnéticosExtraçãoDesregulador endócrinoEsfoliação em fase líquidaHíbrido magnéticoMatéria orgânica naturalExtração em fase sólidaEndocrine disruptorLiquid phase exfoliationNanoparticlesMagnetic hybridNatural organic matterSolid phase extractionCIENCIAS EXATAS E DA TERRA::QUIMICAExtração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/GrafenoMagnetic solid phase extraction of bisphenol A using hybrid CoFe2O4/NOM/Grapheneinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPós-Graduação em QuímicaUniversidade Federal de Sergipereponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSinfo:eu-repo/semantics/openAccessLICENSElicense.txtlicense.txttext/plain; charset=utf-81475https://ri.ufs.br/jspui/bitstream/riufs/14907/1/license.txt098cbbf65c2c15e1fb2e49c5d306a44cMD51ORIGINALRHAYZA_VICTORIA_MATOS_OLIVEIRA.pdfRHAYZA_VICTORIA_MATOS_OLIVEIRA.pdfapplication/pdf2205360https://ri.ufs.br/jspui/bitstream/riufs/14907/2/RHAYZA_VICTORIA_MATOS_OLIVEIRA.pdf4905a6e6efd81cfdabaf8aba754c2082MD52TEXTRHAYZA_VICTORIA_MATOS_OLIVEIRA.pdf.txtRHAYZA_VICTORIA_MATOS_OLIVEIRA.pdf.txtExtracted texttext/plain150417https://ri.ufs.br/jspui/bitstream/riufs/14907/3/RHAYZA_VICTORIA_MATOS_OLIVEIRA.pdf.txtbfa569a3fdd06c7ecf6d145d80c0a860MD53THUMBNAILRHAYZA_VICTORIA_MATOS_OLIVEIRA.pdf.jpgRHAYZA_VICTORIA_MATOS_OLIVEIRA.pdf.jpgGenerated Thumbnailimage/jpeg1424https://ri.ufs.br/jspui/bitstream/riufs/14907/4/RHAYZA_VICTORIA_MATOS_OLIVEIRA.pdf.jpg72a137daf727454f3b0ccc964b89ded6MD54riufs/149072021-12-17 13:45:40.803oai:ufs.br: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Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2021-12-17T16:45:40Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false |
dc.title.pt_BR.fl_str_mv |
Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno |
dc.title.alternative.eng.fl_str_mv |
Magnetic solid phase extraction of bisphenol A using hybrid CoFe2O4/NOM/Graphene |
title |
Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno |
spellingShingle |
Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno Oliveira, Rhayza Victoria Matos Química Nanopartículas Materiais magnéticos Extração Desregulador endócrino Esfoliação em fase líquida Híbrido magnético Matéria orgânica natural Extração em fase sólida Endocrine disruptor Liquid phase exfoliation Nanoparticles Magnetic hybrid Natural organic matter Solid phase extraction CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno |
title_full |
Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno |
title_fullStr |
Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno |
title_full_unstemmed |
Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno |
title_sort |
Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno |
author |
Oliveira, Rhayza Victoria Matos |
author_facet |
Oliveira, Rhayza Victoria Matos |
author_role |
author |
dc.contributor.author.fl_str_mv |
Oliveira, Rhayza Victoria Matos |
dc.contributor.advisor1.fl_str_mv |
Romão, Luciane Pimenta Cruz |
dc.contributor.advisor-co1.fl_str_mv |
Cunha, Graziele da Costa |
contributor_str_mv |
Romão, Luciane Pimenta Cruz Cunha, Graziele da Costa |
dc.subject.por.fl_str_mv |
Química Nanopartículas Materiais magnéticos Extração Desregulador endócrino Esfoliação em fase líquida Híbrido magnético Matéria orgânica natural Extração em fase sólida |
topic |
Química Nanopartículas Materiais magnéticos Extração Desregulador endócrino Esfoliação em fase líquida Híbrido magnético Matéria orgânica natural Extração em fase sólida Endocrine disruptor Liquid phase exfoliation Nanoparticles Magnetic hybrid Natural organic matter Solid phase extraction CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Endocrine disruptor Liquid phase exfoliation Nanoparticles Magnetic hybrid Natural organic matter Solid phase extraction |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
This work consisted in synthesizing magnetic hybrid materials consisting of cobalt ferrite, natural organic matter and graphene (CoFe2O4 /NOM/Graphene), and applying it as an adsorbent in the analytical methodology of BPA magnetic extraction in aqueous matrices. Initially, four hybrid materials were synthesized: ferrite from chloride (HFC), ferrite from sulfate (HFS), graphene from chloride (HGC) and graphene from sulfate (HGS). The X-ray diffraction technique demonstrated the formation of the cobalt ferrite phase in all synthesized materials, as well as that of graphene in hybrids. Spectroscopy in the infrared region revealed the presence of functional groups by stretching the O-H and C = O bonds characteristic of the presence of NOM, C = C of graphene, in addition to Fe-O of the ferrites. Transmission electron microscopy images revealed spherical nanoparticles with dimensions of 9.72 nm (HFC), 34.0 nm (HFS); 8.75 nm (HGC) e 43.9 nm (HGS). In addition, graphene sheets were observed in a few layers. Raman spectra confirmed the formation of cobalt ferrite, highlighting its inverse spinel type, and indicated the formation of graphene. The graphene formed showed few structural defects, and the number of layers was estimated as mono and double layer. The adsorption experiments showed the potential of graphene hybrids in the adsorption stage, 94.19% (HGS) and 97.95% (HGC). Optimization of this step resulted in the use of 50 mg of HGC and orbital agitation at 150 rpm for 5 minutes. Desorption was performed in 2.5 minutes at 150 rpm, using methanol as solvent, obtaining 99.19% of BPA desorbed. The analytical validation showed a correlation coefficient r = 1.00, LD = 0.022 μg L-1 and LQ = 0.072 μg L-1 . The reproducibility of the extraction procedure varies from 2.13 - 2.21% and shows excellent recoveries in the range of 99.33 – 104.4%. The method proved to be feasible for application in bottled, river and supply water samples with recoveries of 99.87 - 104.7%. Furthermore, the MSPE methodology used proved to be simple, fast and efficient for the extraction of BPA in aqueous matrices, in addition to the use of an eco-friendly adsorbent as a support. |
publishDate |
2021 |
dc.date.accessioned.fl_str_mv |
2021-12-17T16:45:40Z |
dc.date.available.fl_str_mv |
2021-12-17T16:45:40Z |
dc.date.issued.fl_str_mv |
2021-05-31 |
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 |
OLIVEIRA, Rhayza Victoria Matos. Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno. 2021. 99 f. Dissertação (Mestrado em Química) – Universidade Federal de Sergipe, São Cristóvão, 2021. |
dc.identifier.uri.fl_str_mv |
https://ri.ufs.br/jspui/handle/riufs/14907 |
identifier_str_mv |
OLIVEIRA, Rhayza Victoria Matos. Extração em fase sólida magnética de bisfenol A utilizando híbrido CoFe2O4/MON/Grafeno. 2021. 99 f. Dissertação (Mestrado em Química) – Universidade Federal de Sergipe, São Cristóvão, 2021. |
url |
https://ri.ufs.br/jspui/handle/riufs/14907 |
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por |
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openAccess |
dc.publisher.program.fl_str_mv |
Pós-Graduação em Química |
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Universidade Federal de Sergipe |
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