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Previous issue date: 2016-04-15 / The analysis of mixtures is a common place challenge in the laboratory. Conventional methods demand a previous treatment which may be time consuming. At present, Nuclear Magnetic Resonance may be employed for the analysis of mixtures by using the DOSY (diffusion ordered spectroscopy) technique, whereby the different components of a mixture are separated by their diffusion coefficients. Pitches, in general, are products which are employed as starting material for the production of a variety of carbon materials, such as anodes for the production of aluminum, graphite electrodes for the steel industry, and carbon fibers. Pitches obtained from coal tar, itself a residue in the production of coke, are the most traditionally used. However, it is a carcinogen and therefore has had its use greatly diminished. Petroleum pitches, which are produced from decanted oil, may be a safer and less expensive alternative. The decanted oil is a heavy fraction obtained from catalytic cracking of petroleum. The difficulties in controlling its processing are derived from its complex composition, which includes paraffins, aromatic and heteroaromatic compounds. The present work investigates the analysis by NMR-DOSY of a mixture of model compounds present in decanted oil. Thus, a mixture of Tetracosane, Phenanthrene, 9-Mehylanthracene, Pyrene, Carbazole, 9-metil Carbazol, Dibenzothiophene, Dibenzofuran, Hexadecane, 1-Methylnaphthalene, Thiophene, Tetrahydrofuran was analyzed by NMR with an Avance III 500 MHz NMR spectrometer equipped with a BBO probe with a gradient on z-axis, at 20?C. To help in the separation by diffusion, the following polymers were used: poly-(ethyleneglycol), poly-(vinylpyrrolidone), poly-(dimethylsiloxan), poly-(butylmethacrylate) e poly-(vinylacetate).The shift reagent Eu(fod)3 was also employed. The results from DOSY-INEPT experiments show that poly-(butylmethacrylate) is the matrix which afforded the best separation of the different components of the mixture, followed by poly-(vinylacetate), poly-(ethyleneglycol) and finally, poly-(vinylpyrrolidone), which showed satisfactory results / Um grande desafio, muitas das vezes at? comum nos laborat?rios, ? a an?lise de misturas. Os m?todos convencionais em sua maioria exigem um tratamento pr?vio das misturas, o que demanda tempo, al?m de interferir diretamente no equil?brio do sistema. Hoje em dia, a t?cnica de Resson?ncia Magn?tica Nuclear pode ser usada na an?lise de misturas medindo-se o coeficiente de difus?o dos componentes da mistura, permitindo a obten??o dos espectros de cada componente individualmente por meio de um experimento r?pido que n?o interfere na mistura em si. O experimento mais comum ? o DOSY, do ingl?s Espectroscopia de Difus?o Ordenada. Piches, em geral, s?o produtos que s?o empregados como mat?rias-primas na produ??o de uma variedade de materiais de carbono, tais como: anodos de carbono para produ??o de alum?nio, eletrodos de grafite para a ind?stria sider?rgia e fibras de carbono. Piches obtidos a partir do alcatr?o da hulha, res?duo da produ??o de coque metal?rgico, s?o os tradicionalmente mais usados, mas apresentam alto potencial carcinog?nico e tem demanda decrescente em fun??o de novas tecnologias empregadas nas coquerias. Piches de petr?leo, produzidos a partir de ?leos decantados, podem potencialmente constituir uma alternativa mais segura e com maior disponibilidade. O ?leo decantado ? uma fra??o pesada obtida nas unidades de craqueamento catal?tico fluido no refino de petr?leo, e o controle de seu processamento ? dificultado pela complexidade de sua composi??o, que inclui compostos paraf?nicos, homoarom?ticos e heteroarom?ticos. O presente trabalho se prop?em a investigar a an?lise por RMN de uma mistura de padr?es de subst?ncias representativas dos tipos de compostos presentes no ?leo decantado. Assim, foram escolhidos padr?es de Tetracosano, Fenantreno, 9-metil Antraceno, Pireno, Carbazol, 9-metil Carbazol, Dibenzotiofeno, Dibenzofurano, Hexadecano, 1-metil Naftaleno, Tiofeno, Tetrahidrofurano. Todos os experimentos foram realizados no laborat?rio de RMN do PPGQ-UFRRJ a 20?C com o espectr?metro de RMN de 500 MHz Bruker Avance III, equipado com sonda BBO, gradiente no eixo z. Para auxiliar na separa??o dos componentes da mistura foram usados o pol?mero poli-(etilenoglicol), poli-(vinilpirrolidona), poli-(dimetilsiloxano), poli-(metacrilato de butila) e poli-(acetato de vinila), al?m do reagente de deslocamento Eu(fod)3. Os resultados obtidos a partir dos experimentos de DOSY-INEPT mostraram que o pol?mero PMAB foi a matriz que mais auxiliou na separa??o dos componentes da mistura em quest?o no presente trabalho, sendo seguido pelas matrizes PAV, PEG e PVP, que tamb?m apresentaram resultados satisfat?rios
Identifer | oai:union.ndltd.org:IBICT/oai:localhost:jspui/1437 |
Date | 15 April 2016 |
Creators | Almeida , Vitor dos Santos |
Contributors | Rumjanek, Victor Marcos, Castro, Alexandre Taschetto de, Ruiz, Naira Machado da Silva, Barreto Jr., Cleber Bomfim |
Publisher | Universidade Federal Rural do Rio de Janeiro, Programa de P?s-Gradua??o em Qu?mica, UFRRJ, Brasil, Instituto de Ci?ncias Exatas |
Source Sets | IBICT Brazilian ETDs |
Language | Portuguese |
Detected Language | Unknown |
Type | info:eu-repo/semantics/publishedVersion, info:eu-repo/semantics/masterThesis |
Format | application/pdf |
Source | reponame:Biblioteca Digital de Teses e Dissertações da UFRRJ, instname:Universidade Federal Rural do Rio de Janeiro, instacron:UFRRJ |
Rights | info:eu-repo/semantics/openAccess |
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