Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho
Autor(a) principal: | |
---|---|
Data de Publicação: | 2017 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Repositório Institucional Manancial UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/11287 |
Resumo: | Quality control of food and medicines is largely done using methods recommended in official compendia, including titration and gravimetry, which involve several negative aspects and are at odds with the principles of green analytical chemistry. Enthalpy methods are based on the enthalpy determination of chemical reactions. In the entalpimétrica analysis the quantitative determination of a reagent or catalyst is made through the enthalpy variation of a chemical reaction, that can be measured directly or indirectly. The main approaches for the entalpimetric analysis are thermometric titration, direct injection enthalpymetry (DIE) and flow entalpimetry. However, despite the availability of commercial instruments for this purpose today, these techniques have been replaced and almost disappeared from the literature, probably due to the high cost of microcalorimetry devices and the limitation of the low frequency of analysis, leading to the choice of Other analytical methods. Currently, there is a need for the development of analytical methods that provide quick results, low cost, low reagent consumption and waste disposal, and minimal sample preparation and manipulation. In this study, infrared thermography was, for the first time, combined with enthalpymetry for the determination of different analytes (eg, iron, calcium, sodium, chlorides and acidity) in foods. In this way, the so-called Thermal Infrared Enthalpyimetry (TIE) was established using neutralization, complexation, precipitation and oxidation reactions, in which the temperature variation generated in the reactions for the construction of calibration curves was verified. The TIE was performed on microplates using a multichannel pipette for the addition of the reagents and an infrared camera for monitoring the temperature generated inside the wells after the addition of the reagents. The results of the proposed method were compared with those obtained through conventional (volumetric) techniques recommended in official compendia. In this way, TIE was optimized and validated for the determination of total, fixed and volatile acidity of vinegars, and was also applied in the simultaneous determination of sodium chloride and total acidity of pickle brine. The obtained results showed good agreement with conventional techniques, performing the analyzes in a fast, efficient and with potential to be applied as routine analysis, due to the simplicity, speed and high frequency of analysis. Thus, it has been demonstrated that TIE can be considered an important tool for the determination of several analytes in foods. Also in this work, it was also done the evaluation of the TIE using different cameras (with refrigerated detector or not), in order to verify and compare the performance of infrared cameras for application to TIE. It was verified that a refrigerated camera presents better results, however equipment without refrigerated detector, of lower resolution and of low cost presented excellent and promising results. |
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2017-08-01T14:27:28Z2017-08-01T14:27:28Z2017-01-11http://repositorio.ufsm.br/handle/1/11287Quality control of food and medicines is largely done using methods recommended in official compendia, including titration and gravimetry, which involve several negative aspects and are at odds with the principles of green analytical chemistry. Enthalpy methods are based on the enthalpy determination of chemical reactions. In the entalpimétrica analysis the quantitative determination of a reagent or catalyst is made through the enthalpy variation of a chemical reaction, that can be measured directly or indirectly. The main approaches for the entalpimetric analysis are thermometric titration, direct injection enthalpymetry (DIE) and flow entalpimetry. However, despite the availability of commercial instruments for this purpose today, these techniques have been replaced and almost disappeared from the literature, probably due to the high cost of microcalorimetry devices and the limitation of the low frequency of analysis, leading to the choice of Other analytical methods. Currently, there is a need for the development of analytical methods that provide quick results, low cost, low reagent consumption and waste disposal, and minimal sample preparation and manipulation. In this study, infrared thermography was, for the first time, combined with enthalpymetry for the determination of different analytes (eg, iron, calcium, sodium, chlorides and acidity) in foods. In this way, the so-called Thermal Infrared Enthalpyimetry (TIE) was established using neutralization, complexation, precipitation and oxidation reactions, in which the temperature variation generated in the reactions for the construction of calibration curves was verified. The TIE was performed on microplates using a multichannel pipette for the addition of the reagents and an infrared camera for monitoring the temperature generated inside the wells after the addition of the reagents. The results of the proposed method were compared with those obtained through conventional (volumetric) techniques recommended in official compendia. In this way, TIE was optimized and validated for the determination of total, fixed and volatile acidity of vinegars, and was also applied in the simultaneous determination of sodium chloride and total acidity of pickle brine. The obtained results showed good agreement with conventional techniques, performing the analyzes in a fast, efficient and with potential to be applied as routine analysis, due to the simplicity, speed and high frequency of analysis. Thus, it has been demonstrated that TIE can be considered an important tool for the determination of several analytes in foods. Also in this work, it was also done the evaluation of the TIE using different cameras (with refrigerated detector or not), in order to verify and compare the performance of infrared cameras for application to TIE. It was verified that a refrigerated camera presents better results, however equipment without refrigerated detector, of lower resolution and of low cost presented excellent and promising results.O controle de qualidade de alimentos e de medicamentos é feito em grande parte utilizando métodos recomendados nos compêndios oficiais, entre eles a titulação e a gravimetria, os quais envolvem vários aspectos negativos e em desacordo com os princípios da química analítica verde. Métodos entalpimétricos se baseiam na determinação da entalpia das reações químicas. Na análise entalpimétrica é efetuada a determinação quantitativa de um reagente ou catalisador através da variação de entalpia de uma reação química, que pode ser medida direta ou indiretamente. As principais abordagens para a análise entalpimétrica são a titulação termométrica, entalpimetria por injeção direta (DIE, do inglês Direct Inject Entalpimetry) e entalpimetria em fluxo. No entanto, apesar de hoje em dia haver a disponibilidade de instrumentos comerciais para este fim, essas técnicas foram substituídas e quase desapareceram da literatura, provavelmente devido ao custo elevado de dispositivos de microcalorimetria e pela limitação da baixa frequência de análise, levando à escolha de outros métodos analíticos. Atualmente, existe a necessidade do desenvolvimento de métodos analíticos que forneçam resultados rápidos, com baixo custo, pequeno consumo de reagentes e descarte de resíduos, além de mínimo preparo e manipulação da amostra. Neste estudo, a termografia no infravermelho foi, pela primeira vez, combinada com a entalpimetria visando determinação de diferentes analitos (p. ex., ferro, cálcio, sódio, cloretos e acidez) em alimentos. Desta forma, a chamada entalpimetria no infravermelho (TIE, do inglês Thermal Infrared Enthalpimetry) foi estabelecida empregando reações de neutralização, complexação, precipitação e oxirredução, onde foi verificada a variação da temperatura gerada nas reações para a construção de curvas de calibração. A TIE foi realizada em microplacas, empregando pipeta multicanal para a adição dos reagentes e uma câmera no infravermelho para monitoramento de temperatura gerada no interior dos poços após a adição dos reagentes. Os resultados do método proposto foram comparados com aqueles obtidos através de técnicas convencionais (volumétricas) recomendadas nos compêndios oficiais. Desta forma, a TIE foi otimizada e validada para a determinação da acidez total, fixa e volátil de vinagres, e também foi aplicada na determinação simultânea de cloreto de sódio e acidez total da salmoura de picles. Os resultados obtidos mostraram boa concordância com técnicas convencionais, efetuando as análises de maneira rápida, eficaz e com potencial para ser aplicada como análise de rotina, devido à simplicidade, rapidez e elevada frequência de análise. Desta forma, foi demonstrado que a TIE pode ser considerada uma importante ferramenta para a determinação de diversos analitos em alimentos. Ainda neste trabalho, foi feita também a avaliação da TIE usando diferentes câmeras (com detector refrigerado ou não), a fim de verificar e comparar o desempenho de câmeras no infravermelho para aplicação a TIE. Verificou-se que uma câmera refrigerada apresenta melhores resultados, entretanto equipamentos sem detector refrigerado, de menor resolução e de baixo custo apresentaram resultados excelentes e promissores.porUniversidade Federal de Santa MariaCentro de Ciências RuraisPrograma de Pós-Graduação em Ciência e Tecnologia dos AlimentosUFSMBrasilCiência e Tecnologia dos AlimentosAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessTermografiaEntalpimetriaMicroplacasInfravermelhoAnálise simultâneaThermographyEntalpimetryMicroplatesInfraredSimultaneous analysisCNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOS::CIENCIA DE ALIMENTOSDesenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelhoDevelopment of analytical methods using thermal infrared enthalpimetryinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisBarin, Juliano Smaniotohttp://lattes.cnpq.br/7545847424095994Costa, Adilson Ben dahttp://lattes.cnpq.br/2604778196819181Codevilla, Cristiane Francohttp://lattes.cnpq.br/3165544867590900Duarte, Fábio Andrei Duartehttp://lattes.cnpq.br/3503633944419329Barcia, Milene Teixeirahttp://lattes.cnpq.br/3415182271638119http://lattes.cnpq.br/3191079744869985Tischer, Bruna500700100002600600600600600600f4cb9cf1-d105-4e6c-b0fa-acdf690e8cab5ae2b854-90a0-4609-80ea-389ba27af4a98fd7d402-38cb-487a-ae04-60b751dc48d6bc9cd8f5-e992-432f-b644-bc35b05757e2f60c61ec-2b88-485f-8d1e-83d62038970dfb1e5518-82fc-4c0b-9660-7f47850115f0reponame:Repositório Institucional Manancial UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTischer, Bruna.pdfTischer, Bruna.pdfTese de Doutoradoapplication/pdf2156481http://repositorio.ufsm.br/bitstream/1/11287/1/Tischer%2c%20Bruna.pdf7840a38bec38d6392ff1e38c2be73975MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho |
dc.title.alternative.eng.fl_str_mv |
Development of analytical methods using thermal infrared enthalpimetry |
title |
Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho |
spellingShingle |
Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho Tischer, Bruna Termografia Entalpimetria Microplacas Infravermelho Análise simultânea Thermography Entalpimetry Microplates Infrared Simultaneous analysis CNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOS::CIENCIA DE ALIMENTOS |
title_short |
Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho |
title_full |
Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho |
title_fullStr |
Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho |
title_full_unstemmed |
Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho |
title_sort |
Desenvolvimento de métodos analíticos envolvendo entalpimetria no infravermelho |
author |
Tischer, Bruna |
author_facet |
Tischer, Bruna |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Barin, Juliano Smanioto |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/7545847424095994 |
dc.contributor.referee1.fl_str_mv |
Costa, Adilson Ben da |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/2604778196819181 |
dc.contributor.referee2.fl_str_mv |
Codevilla, Cristiane Franco |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/3165544867590900 |
dc.contributor.referee3.fl_str_mv |
Duarte, Fábio Andrei Duarte |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/3503633944419329 |
dc.contributor.referee4.fl_str_mv |
Barcia, Milene Teixeira |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/3415182271638119 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3191079744869985 |
dc.contributor.author.fl_str_mv |
Tischer, Bruna |
contributor_str_mv |
Barin, Juliano Smanioto Costa, Adilson Ben da Codevilla, Cristiane Franco Duarte, Fábio Andrei Duarte Barcia, Milene Teixeira |
dc.subject.por.fl_str_mv |
Termografia Entalpimetria Microplacas Infravermelho Análise simultânea |
topic |
Termografia Entalpimetria Microplacas Infravermelho Análise simultânea Thermography Entalpimetry Microplates Infrared Simultaneous analysis CNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOS::CIENCIA DE ALIMENTOS |
dc.subject.eng.fl_str_mv |
Thermography Entalpimetry Microplates Infrared Simultaneous analysis |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS AGRARIAS::CIENCIA E TECNOLOGIA DE ALIMENTOS::CIENCIA DE ALIMENTOS |
description |
Quality control of food and medicines is largely done using methods recommended in official compendia, including titration and gravimetry, which involve several negative aspects and are at odds with the principles of green analytical chemistry. Enthalpy methods are based on the enthalpy determination of chemical reactions. In the entalpimétrica analysis the quantitative determination of a reagent or catalyst is made through the enthalpy variation of a chemical reaction, that can be measured directly or indirectly. The main approaches for the entalpimetric analysis are thermometric titration, direct injection enthalpymetry (DIE) and flow entalpimetry. However, despite the availability of commercial instruments for this purpose today, these techniques have been replaced and almost disappeared from the literature, probably due to the high cost of microcalorimetry devices and the limitation of the low frequency of analysis, leading to the choice of Other analytical methods. Currently, there is a need for the development of analytical methods that provide quick results, low cost, low reagent consumption and waste disposal, and minimal sample preparation and manipulation. In this study, infrared thermography was, for the first time, combined with enthalpymetry for the determination of different analytes (eg, iron, calcium, sodium, chlorides and acidity) in foods. In this way, the so-called Thermal Infrared Enthalpyimetry (TIE) was established using neutralization, complexation, precipitation and oxidation reactions, in which the temperature variation generated in the reactions for the construction of calibration curves was verified. The TIE was performed on microplates using a multichannel pipette for the addition of the reagents and an infrared camera for monitoring the temperature generated inside the wells after the addition of the reagents. The results of the proposed method were compared with those obtained through conventional (volumetric) techniques recommended in official compendia. In this way, TIE was optimized and validated for the determination of total, fixed and volatile acidity of vinegars, and was also applied in the simultaneous determination of sodium chloride and total acidity of pickle brine. The obtained results showed good agreement with conventional techniques, performing the analyzes in a fast, efficient and with potential to be applied as routine analysis, due to the simplicity, speed and high frequency of analysis. Thus, it has been demonstrated that TIE can be considered an important tool for the determination of several analytes in foods. Also in this work, it was also done the evaluation of the TIE using different cameras (with refrigerated detector or not), in order to verify and compare the performance of infrared cameras for application to TIE. It was verified that a refrigerated camera presents better results, however equipment without refrigerated detector, of lower resolution and of low cost presented excellent and promising results. |
publishDate |
2017 |
dc.date.accessioned.fl_str_mv |
2017-08-01T14:27:28Z |
dc.date.available.fl_str_mv |
2017-08-01T14:27:28Z |
dc.date.issued.fl_str_mv |
2017-01-11 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/11287 |
url |
http://repositorio.ufsm.br/handle/1/11287 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
500700100002 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 |
dc.relation.authority.fl_str_mv |
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dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
eu_rights_str_mv |
openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Rurais |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Ciência e Tecnologia dos Alimentos |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Ciência e Tecnologia dos Alimentos |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Rurais |
dc.source.none.fl_str_mv |
reponame:Repositório Institucional Manancial UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Repositório Institucional Manancial UFSM |
collection |
Repositório Institucional Manancial UFSM |
bitstream.url.fl_str_mv |
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bitstream.checksum.fl_str_mv |
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bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 MD5 MD5 |
repository.name.fl_str_mv |
Repositório Institucional Manancial UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
ouvidoria@ufsm.br |
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1808854728655765504 |