Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente

Detalhes bibliográficos
Ano de defesa: 2018
Autor(a) principal: ABREU, Diego Coelho lattes
Orientador(a): SOUSA, Francisco Ferreira de lattes
Banca de defesa: SOUSA, Francisco Ferreira de lattes, FAÇANHA FILHO, Pedro de Freitas lattes, SANTOS, Adenilson Oliveira dos lattes, ANDRADE FILHO, Tarciso Silva de lattes
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal do Maranhão
Programa de Pós-Graduação: PROGRAMA DE PÓS-GRADUAÇÃO EM CIÊNCIA DOS MATERIAIS/CCSST
Departamento: DEPARTAMENTO DE FÍSICA/CCET
País: Brasil
Palavras-chave em Português:
Palavras-chave em Inglês:
Área do conhecimento CNPq:
Link de acesso: https://tedebc.ufma.br/jspui/handle/tede/2154
Resumo: Palmitic acid (PA) is a saturated fatty acid with a molecular structure CH3-(CH2)14- COOH, commonly found in animal and vegetable fats. It can crystallize in the Atriclinic, Bo, Bm, C, Eo and Em forms with crystalline triclinic, orthorhombic and monoclinic systems. In this study, polycrystalline samples of PA were obtained from the technique of slow evaporation in solvents with different polarities. The characterization of these polymorphic crystals was performed using Raman spectroscopy and infrared, as well as differential scanning calorimetry (DSC) and X-ray diffraction (XRD), the parameters obtained in the XRD were refined using the Rietveld method. According to the results, the crystals formed using polar solvents with high evaporation rate form crystals with the phases Em and C. Forms Bm e C are predominant for polar solvents with low evaporation rate and in nonpolar solvents. The Raman spectra of the samples obtained from nonpolar and polar solvents with low evaporation rate indicate shifts in lattice modes for larger wave numbers, which may be associated with an elongation at the hydrogen bonds (O−H...O). Bands around 1700 cm-1, associated with the vibration of the group C = O are presented as singlets for polar samples with high evaporation rate; Mode around 1700 cm- 1, associated with the vibration of the group C=O are presented as singlets for polar samples with high evaporation rate; and as doubts to the others. The spectra obtained in the infrared show the same behavior observed in the Raman spectra, indicating that the samples obtained in nonpolar or polar solvents with low evaporation rate, showing different phases of the other samples. The DSC analysis shows the occurrence of thermal events in the samples of polar solvents with low evaporation rate and nonpolar before melting, concerning the transformation BmC. The XDR in high temperature confirms the data obtained with thermal analysis and shows a preferential thermal expansion in the plane (020). Thus, it is evident that the polarity of the solvent directly influences the PA polymorphism, the evaporation rate of the solvent can also be included as a relevant factor in this phenomenon.
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spelling SOUSA, Francisco Ferreira de584648832-34http://lattes.cnpq.br/1275187715540959FAÇANHA FILHO, Pedro de Freitas689515313-68http://lattes.cnpq.br/7814089708845704SOUSA, Francisco Ferreira de584648832-34http://lattes.cnpq.br/1275187715540959FAÇANHA FILHO, Pedro de Freitas689515313-68http://lattes.cnpq.br/7814089708845704SANTOS, Adenilson Oliveira doshttp://lattes.cnpq.br/7760219759813661ANDRADE FILHO, Tarciso Silva deCV: http://lattes.cnpq.br/3128499030641448625261033-04http://lattes.cnpq.br/9134898878854196ABREU, Diego Coelho2018-04-05T14:13:42Z2018-03-21ABREU, Diego Coelho. Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente. 2018. 81f. Dissertação (Mestrado em Ciências dos Materiais/CCSST) - Universidade Federal do Maranhão, Imperatriz .https://tedebc.ufma.br/jspui/handle/tede/2154Palmitic acid (PA) is a saturated fatty acid with a molecular structure CH3-(CH2)14- COOH, commonly found in animal and vegetable fats. It can crystallize in the Atriclinic, Bo, Bm, C, Eo and Em forms with crystalline triclinic, orthorhombic and monoclinic systems. In this study, polycrystalline samples of PA were obtained from the technique of slow evaporation in solvents with different polarities. The characterization of these polymorphic crystals was performed using Raman spectroscopy and infrared, as well as differential scanning calorimetry (DSC) and X-ray diffraction (XRD), the parameters obtained in the XRD were refined using the Rietveld method. According to the results, the crystals formed using polar solvents with high evaporation rate form crystals with the phases Em and C. Forms Bm e C are predominant for polar solvents with low evaporation rate and in nonpolar solvents. The Raman spectra of the samples obtained from nonpolar and polar solvents with low evaporation rate indicate shifts in lattice modes for larger wave numbers, which may be associated with an elongation at the hydrogen bonds (O−H...O). Bands around 1700 cm-1, associated with the vibration of the group C = O are presented as singlets for polar samples with high evaporation rate; Mode around 1700 cm- 1, associated with the vibration of the group C=O are presented as singlets for polar samples with high evaporation rate; and as doubts to the others. The spectra obtained in the infrared show the same behavior observed in the Raman spectra, indicating that the samples obtained in nonpolar or polar solvents with low evaporation rate, showing different phases of the other samples. The DSC analysis shows the occurrence of thermal events in the samples of polar solvents with low evaporation rate and nonpolar before melting, concerning the transformation BmC. The XDR in high temperature confirms the data obtained with thermal analysis and shows a preferential thermal expansion in the plane (020). Thus, it is evident that the polarity of the solvent directly influences the PA polymorphism, the evaporation rate of the solvent can also be included as a relevant factor in this phenomenon.O ácido palmítico (AP) é um ácido graxo saturado com uma estrutura molecular CH3- (CH2)14-COOH, comumente encontrado em gorduras animais e vegetais. Pode cristalizar nas formas Atriclinico, Bo, Bm, C, Eo e Em com sistemas cristalinos do tipo triclínicos, ortorrômbico e monoclínicos. Neste trabalho, amostras policristalinas de AP foram obtidas a partir da técnica de evaporação lenta em solventes com diferentes polaridades. A caracterização polimórfica desses cristais foi realizada utilizando as espectroscopias Raman e no infravermelho, bem como por meio de calorimetria exploratória diferencial (CED) e difração de raios X (DRX), os parâmetros obtidos na DRX foram refinados usando o método de Rietveld. De acordo com os resultados, os cristais formados usando solventes polares com alta taxa de evaporação formam cristais com as fases Em e C. As formas Bm e C são predominantes para solventes polares com baixa taxa de evaporação e em solvente apolar. Os espectros Raman das amostras obtidas de solventes apolares e polares com baixa taxa de evaporação, indicam deslocamentos nos modos de rede para maiores números de onda, o que pode estar associado a um alongamento nas ligações de hidrogênio (O−H...O). Bandas em torno de 1700cm-1, associadas à vibração do grupo C=O apresentam-se como singletos para amostras polares com alta taxa de evaporação; e como dubletos para as demais. Os espectros obtidos no infravermelho mostram o mesmo comportamento observado nos espectros Raman, indicando que as amostras obtidas em solventes apolares ou polares com baixa taxa de evaporação, apresentam fases diferentes das demais amostras. A análise por CED mostra a ocorrência de eventos térmicos nas amostras de solventes polares com baixa taxa de evaporação e apolares antes da fusão, atribuídas à transformação BmC. O DRX de alta temperatura confirma os dados obtidos com análise térmica e mostra uma expansão térmica preferencial no plano (020). Assim, é evidente que a polaridade do solvente influencia diretamente no polimorfismo do AP, a taxa de evaporação do solvente também pode ser incluída como um fator relevante neste fenômeno.Submitted by Daniella Santos (daniella.santos@ufma.br) on 2018-04-05T14:13:42Z No. of bitstreams: 1 DiegoAbreu.pdf: 4710987 bytes, checksum: 5fb85c3792c618048e25fa5da70e561e (MD5)Made available in DSpace on 2018-04-05T14:13:42Z (GMT). No. of bitstreams: 1 DiegoAbreu.pdf: 4710987 bytes, checksum: 5fb85c3792c618048e25fa5da70e561e (MD5) Previous issue date: 2018-03-21application/pdfporUniversidade Federal do MaranhãoPROGRAMA DE PÓS-GRADUAÇÃO EM CIÊNCIA DOS MATERIAIS/CCSSTUFMABrasilDEPARTAMENTO DE FÍSICA/CCETPolimorfismoPolaridadeSolventePolymorphismPolaritySolventQuímicaEstudo do polimorfismo do ácido palmítico sob variação da polaridade do solventeStudy of palmitic acid polymorphism of the solvent polarityinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações da UFMAinstname:Universidade Federal do Maranhão (UFMA)instacron:UFMAORIGINALDiegoAbreu.pdfDiegoAbreu.pdfapplication/pdf4710987http://tedebc.ufma.br:8080/bitstream/tede/2154/2/DiegoAbreu.pdf5fb85c3792c618048e25fa5da70e561eMD52LICENSElicense.txtlicense.txttext/plain; charset=utf-82255http://tedebc.ufma.br:8080/bitstream/tede/2154/1/license.txt97eeade1fce43278e63fe063657f8083MD51tede/21542018-04-05 11:13:42.171oai:tede2: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Biblioteca Digital de Teses e Dissertaçõeshttps://tedebc.ufma.br/jspui/PUBhttp://tedebc.ufma.br:8080/oai/requestrepositorio@ufma.br||repositorio@ufma.bropendoar:21312018-04-05T14:13:42Biblioteca Digital de Teses e Dissertações da UFMA - Universidade Federal do Maranhão (UFMA)false
dc.title.por.fl_str_mv Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
dc.title.alternative.eng.fl_str_mv Study of palmitic acid polymorphism of the solvent polarity
title Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
spellingShingle Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
ABREU, Diego Coelho
Polimorfismo
Polaridade
Solvente
Polymorphism
Polarity
Solvent
Química
title_short Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
title_full Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
title_fullStr Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
title_full_unstemmed Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
title_sort Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
author ABREU, Diego Coelho
author_facet ABREU, Diego Coelho
author_role author
dc.contributor.advisor1.fl_str_mv SOUSA, Francisco Ferreira de
dc.contributor.advisor1ID.fl_str_mv 584648832-34
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/1275187715540959
dc.contributor.advisor-co1.fl_str_mv FAÇANHA FILHO, Pedro de Freitas
dc.contributor.advisor-co1ID.fl_str_mv 689515313-68
dc.contributor.advisor-co1Lattes.fl_str_mv http://lattes.cnpq.br/7814089708845704
dc.contributor.referee1.fl_str_mv SOUSA, Francisco Ferreira de
dc.contributor.referee1ID.fl_str_mv 584648832-34
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/1275187715540959
dc.contributor.referee2.fl_str_mv FAÇANHA FILHO, Pedro de Freitas
dc.contributor.referee2ID.fl_str_mv 689515313-68
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/7814089708845704
dc.contributor.referee3.fl_str_mv SANTOS, Adenilson Oliveira dos
dc.contributor.referee3Lattes.fl_str_mv http://lattes.cnpq.br/7760219759813661
dc.contributor.referee4.fl_str_mv ANDRADE FILHO, Tarciso Silva de
dc.contributor.referee4Lattes.fl_str_mv CV: http://lattes.cnpq.br/3128499030641448
dc.contributor.authorID.fl_str_mv 625261033-04
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/9134898878854196
dc.contributor.author.fl_str_mv ABREU, Diego Coelho
contributor_str_mv SOUSA, Francisco Ferreira de
FAÇANHA FILHO, Pedro de Freitas
SOUSA, Francisco Ferreira de
FAÇANHA FILHO, Pedro de Freitas
SANTOS, Adenilson Oliveira dos
ANDRADE FILHO, Tarciso Silva de
dc.subject.por.fl_str_mv Polimorfismo
Polaridade
Solvente
topic Polimorfismo
Polaridade
Solvente
Polymorphism
Polarity
Solvent
Química
dc.subject.eng.fl_str_mv Polymorphism
Polarity
Solvent
dc.subject.cnpq.fl_str_mv Química
description Palmitic acid (PA) is a saturated fatty acid with a molecular structure CH3-(CH2)14- COOH, commonly found in animal and vegetable fats. It can crystallize in the Atriclinic, Bo, Bm, C, Eo and Em forms with crystalline triclinic, orthorhombic and monoclinic systems. In this study, polycrystalline samples of PA were obtained from the technique of slow evaporation in solvents with different polarities. The characterization of these polymorphic crystals was performed using Raman spectroscopy and infrared, as well as differential scanning calorimetry (DSC) and X-ray diffraction (XRD), the parameters obtained in the XRD were refined using the Rietveld method. According to the results, the crystals formed using polar solvents with high evaporation rate form crystals with the phases Em and C. Forms Bm e C are predominant for polar solvents with low evaporation rate and in nonpolar solvents. The Raman spectra of the samples obtained from nonpolar and polar solvents with low evaporation rate indicate shifts in lattice modes for larger wave numbers, which may be associated with an elongation at the hydrogen bonds (O−H...O). Bands around 1700 cm-1, associated with the vibration of the group C = O are presented as singlets for polar samples with high evaporation rate; Mode around 1700 cm- 1, associated with the vibration of the group C=O are presented as singlets for polar samples with high evaporation rate; and as doubts to the others. The spectra obtained in the infrared show the same behavior observed in the Raman spectra, indicating that the samples obtained in nonpolar or polar solvents with low evaporation rate, showing different phases of the other samples. The DSC analysis shows the occurrence of thermal events in the samples of polar solvents with low evaporation rate and nonpolar before melting, concerning the transformation BmC. The XDR in high temperature confirms the data obtained with thermal analysis and shows a preferential thermal expansion in the plane (020). Thus, it is evident that the polarity of the solvent directly influences the PA polymorphism, the evaporation rate of the solvent can also be included as a relevant factor in this phenomenon.
publishDate 2018
dc.date.accessioned.fl_str_mv 2018-04-05T14:13:42Z
dc.date.issued.fl_str_mv 2018-03-21
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 ABREU, Diego Coelho. Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente. 2018. 81f. Dissertação (Mestrado em Ciências dos Materiais/CCSST) - Universidade Federal do Maranhão, Imperatriz .
dc.identifier.uri.fl_str_mv https://tedebc.ufma.br/jspui/handle/tede/2154
identifier_str_mv ABREU, Diego Coelho. Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente. 2018. 81f. Dissertação (Mestrado em Ciências dos Materiais/CCSST) - Universidade Federal do Maranhão, Imperatriz .
url https://tedebc.ufma.br/jspui/handle/tede/2154
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 do Maranhão
dc.publisher.program.fl_str_mv PROGRAMA DE PÓS-GRADUAÇÃO EM CIÊNCIA DOS MATERIAIS/CCSST
dc.publisher.initials.fl_str_mv UFMA
dc.publisher.country.fl_str_mv Brasil
dc.publisher.department.fl_str_mv DEPARTAMENTO DE FÍSICA/CCET
publisher.none.fl_str_mv Universidade Federal do Maranhão
dc.source.none.fl_str_mv reponame:Biblioteca Digital de Teses e Dissertações da UFMA
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