Estudo do polimorfismo do ácido palmítico sob variação da polaridade do solvente
| Ano de defesa: | 2018 |
|---|---|
| Autor(a) principal: | |
| Orientador(a): | |
| Banca de defesa: | , , , |
| 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 BmC. 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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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 BmC. 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 BmC. 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 BmC. 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 |
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info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/masterThesis |
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masterThesis |
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publishedVersion |
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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 . |
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por |
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por |
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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 do Maranhão |
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PROGRAMA DE PÓS-GRADUAÇÃO EM CIÊNCIA DOS MATERIAIS/CCSST |
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UFMA |
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Brasil |
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DEPARTAMENTO DE FÍSICA/CCET |
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Universidade Federal do Maranhão |
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