Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro
Ano de defesa: | 2007 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
Tipo de documento: | Dissertação |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Santa Maria
|
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
BR
|
Palavras-chave em Português: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/10413 |
Resumo: | In this work, a method for chlorine determination in petroleum coke, vacuum and atmospheric residues and heavy petroleum was developed. The pyrohydrolysis sample decomposition method was used, which consists of sample pyrolysis at about 1000 oC in presence of water vapor. The influence of the main parameters on the pyrohydrolysis reaction, such as temperature, time of pyrohydrolysis, sample mass, presence of pyrohydrolysis reaction accelerator and chlorine absorption solution were studied. Best precision and accuracy were obtained by heating the sample for 10 min at temperatures in the range of 950 to 1000 oC. The accelerator investigated (V2O5) did not influence on chlorine releasing from the investigated samples. However, the vacuum residue and heavy petroleum samples needed to be partially decomposed prior to the pyrohydrolysis step. This previous decomposition step was carried out in the own pyrohydrolysis reactor. Nitric acid and Mg(NO3)2 were used for that purpose at temperature lower than that of pyrohydrolysis. Chlorine was determined by inductively coupled plasma mass spectrometry using dynamic reaction cell in order to minimize molecular ions interference on chlorine, whereas the 35Cl+ signal was monitored. Good precision (RSD < 8% for petroleum coke and < 12% for the other samples) and accuracy (agreement with certified values and results obtained by other sample decomposition methods) were observed. The limit of quantification was 1.5 mg g-1 of chlorine, while the sample mass was 250 mg and the final volume of the sample solution 20 ml. The sample throughput analysis was 3 h-1. It was concluded the developed method is suitable for the determination of relatively low chlorine concentrations in petroleum coke, vacuum and atmospheric residues and heavy petroleum. Additionally, the method is fast and can be easily used in routine work, while low amount of waste is produced in the laboratory. |
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2017-05-152017-05-152007-10-26ANTES, Fabiane Goldschmidt. Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro. 2007. 114 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007.http://repositorio.ufsm.br/handle/1/10413In this work, a method for chlorine determination in petroleum coke, vacuum and atmospheric residues and heavy petroleum was developed. The pyrohydrolysis sample decomposition method was used, which consists of sample pyrolysis at about 1000 oC in presence of water vapor. The influence of the main parameters on the pyrohydrolysis reaction, such as temperature, time of pyrohydrolysis, sample mass, presence of pyrohydrolysis reaction accelerator and chlorine absorption solution were studied. Best precision and accuracy were obtained by heating the sample for 10 min at temperatures in the range of 950 to 1000 oC. The accelerator investigated (V2O5) did not influence on chlorine releasing from the investigated samples. However, the vacuum residue and heavy petroleum samples needed to be partially decomposed prior to the pyrohydrolysis step. This previous decomposition step was carried out in the own pyrohydrolysis reactor. Nitric acid and Mg(NO3)2 were used for that purpose at temperature lower than that of pyrohydrolysis. Chlorine was determined by inductively coupled plasma mass spectrometry using dynamic reaction cell in order to minimize molecular ions interference on chlorine, whereas the 35Cl+ signal was monitored. Good precision (RSD < 8% for petroleum coke and < 12% for the other samples) and accuracy (agreement with certified values and results obtained by other sample decomposition methods) were observed. The limit of quantification was 1.5 mg g-1 of chlorine, while the sample mass was 250 mg and the final volume of the sample solution 20 ml. The sample throughput analysis was 3 h-1. It was concluded the developed method is suitable for the determination of relatively low chlorine concentrations in petroleum coke, vacuum and atmospheric residues and heavy petroleum. Additionally, the method is fast and can be easily used in routine work, while low amount of waste is produced in the laboratory.Neste trabalho foi desenvolvido um método para a determinação de cloro em coque de petróleo, resíduo de vácuo, resíduo atmosférico e petróleo extrapesado. Para tal, foi utilizada a técnica de piroidrólise, que consiste da pirólise da amostra em temperaturas de cerca de 1000 °C na presença de vapor d água. A influência dos principais parâmetros envolvidos na reação de piroidrólise, como temperatura, tempo de reação, massa de amostra, necessidade do uso de acelerador e solução absorvedora foram investigados. Foi observado que, nas condições experimentais empregadas, resultados mais precisos (RSD < 10%) e exatos foram obtidos em temperaturas entre 950 e 1000 °C durante cerca de 1 0 minutos. O acelerador testado (V2O5) não influenciou na liberação do cloro das amostras estudadas. Porém, para as amostras de petróleo extrapesado e resíduo de vácuo foi necessária a decomposição parcial da amostra previamente à piroidrólise. Esta etapa foi conduzida no próprio reator de piroidrólise. Para tanto, ácido nítrico foi usado, em temperatura inferior a da piroidrólise. As determinações de cloro foram feitas por espectrometria de massa com plasma indutivamente acoplado, empregando cela dinâmica de reação para minimizar interferências devido a íons poliatômicos sobre 35Cl+. Boa precisão (RSD < 8% para coque e < 12% para petróleo e resíduo) e exatidão (concordância com o valor certificado e/ou comparação com outro método) foram obtidas. O limite de quantificação do método para 35Cl+ foi de 1,5 mg g-1 de cloro, usando 250 mg de amostra e uma diluição final para 20 ml. A freqüência de determinação foi de 3 amostras h-1. Desta forma, o método proposto foi adequado para a determinação de concentrações relativamente baixas de cloro em coque de petróleo, resíduo de vácuo e atmosférico e petróleo extrapesado. Além disso, o procedimento é rápido, pode ser facilmente usado em trabalhos de rotina e praticamente não gera resíduos tóxicos no laboratório.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaQuímicaPetróleoCoquePiroidróliseCloroCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADecomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloroinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisDressler, Valderi Luizhttp://lattes.cnpq.br/4054740296547580Korn, Maurohttp://lattes.cnpq.br/3772927258951858Flores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212http://lattes.cnpq.br/1717311219430602Antes, Fabiane Goldschmidt10060000000040050050050050029c59cfe-a489-425c-88a5-18fdf7cbf258bca11c68-524c-4e7b-a36e-1123950714a699420716-ccff-4da2-acc2-fa740318453c62862614-b588-40e1-9d9a-b355c8ba3a6einfo:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALFABIANEGOLDSCHMIDT.pdfapplication/pdf1420261http://repositorio.ufsm.br/bitstream/1/10413/1/FABIANEGOLDSCHMIDT.pdf7c072ccf57e5f3187f4b3cd93b1d191dMD51TEXTFABIANEGOLDSCHMIDT.pdf.txtFABIANEGOLDSCHMIDT.pdf.txtExtracted texttext/plain214691http://repositorio.ufsm.br/bitstream/1/10413/2/FABIANEGOLDSCHMIDT.pdf.txt487f5854906e732552dbdbc5afbf1f1cMD52THUMBNAILFABIANEGOLDSCHMIDT.pdf.jpgFABIANEGOLDSCHMIDT.pdf.jpgIM Thumbnailimage/jpeg5829http://repositorio.ufsm.br/bitstream/1/10413/3/FABIANEGOLDSCHMIDT.pdf.jpg9a801dde36fed248bc17c2a180117d97MD531/104132022-12-28 09:58:02.358oai:repositorio.ufsm.br:1/10413Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-12-28T12:58:02Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro |
title |
Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro |
spellingShingle |
Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro Antes, Fabiane Goldschmidt Química Petróleo Coque Piroidrólise Cloro CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro |
title_full |
Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro |
title_fullStr |
Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro |
title_full_unstemmed |
Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro |
title_sort |
Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro |
author |
Antes, Fabiane Goldschmidt |
author_facet |
Antes, Fabiane Goldschmidt |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Dressler, Valderi Luiz |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4054740296547580 |
dc.contributor.referee1.fl_str_mv |
Korn, Mauro |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/3772927258951858 |
dc.contributor.referee2.fl_str_mv |
Flores, Érico Marlon de Moraes |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/7167629055579212 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/1717311219430602 |
dc.contributor.author.fl_str_mv |
Antes, Fabiane Goldschmidt |
contributor_str_mv |
Dressler, Valderi Luiz Korn, Mauro Flores, Érico Marlon de Moraes |
dc.subject.por.fl_str_mv |
Química Petróleo Coque Piroidrólise Cloro |
topic |
Química Petróleo Coque Piroidrólise Cloro CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, a method for chlorine determination in petroleum coke, vacuum and atmospheric residues and heavy petroleum was developed. The pyrohydrolysis sample decomposition method was used, which consists of sample pyrolysis at about 1000 oC in presence of water vapor. The influence of the main parameters on the pyrohydrolysis reaction, such as temperature, time of pyrohydrolysis, sample mass, presence of pyrohydrolysis reaction accelerator and chlorine absorption solution were studied. Best precision and accuracy were obtained by heating the sample for 10 min at temperatures in the range of 950 to 1000 oC. The accelerator investigated (V2O5) did not influence on chlorine releasing from the investigated samples. However, the vacuum residue and heavy petroleum samples needed to be partially decomposed prior to the pyrohydrolysis step. This previous decomposition step was carried out in the own pyrohydrolysis reactor. Nitric acid and Mg(NO3)2 were used for that purpose at temperature lower than that of pyrohydrolysis. Chlorine was determined by inductively coupled plasma mass spectrometry using dynamic reaction cell in order to minimize molecular ions interference on chlorine, whereas the 35Cl+ signal was monitored. Good precision (RSD < 8% for petroleum coke and < 12% for the other samples) and accuracy (agreement with certified values and results obtained by other sample decomposition methods) were observed. The limit of quantification was 1.5 mg g-1 of chlorine, while the sample mass was 250 mg and the final volume of the sample solution 20 ml. The sample throughput analysis was 3 h-1. It was concluded the developed method is suitable for the determination of relatively low chlorine concentrations in petroleum coke, vacuum and atmospheric residues and heavy petroleum. Additionally, the method is fast and can be easily used in routine work, while low amount of waste is produced in the laboratory. |
publishDate |
2007 |
dc.date.issued.fl_str_mv |
2007-10-26 |
dc.date.accessioned.fl_str_mv |
2017-05-15 |
dc.date.available.fl_str_mv |
2017-05-15 |
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 |
ANTES, Fabiane Goldschmidt. Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro. 2007. 114 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10413 |
identifier_str_mv |
ANTES, Fabiane Goldschmidt. Decomposição de coque, resíduo de vácuo e petróleo extrapesado por piroidrólise para a determinação de cloro. 2007. 114 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007. |
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http://repositorio.ufsm.br/handle/1/10413 |
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