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Otimiza??o de metodologia para determina??o de enxofre na forma de sulfato em petr?leo pesado por cromatografia de ?ons

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Previous issue date: 2017-06-30 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Enxofre ? o terceiro elemento mais abundante no petr?leo e ? considerado um dos principais
contaminantes presentes nessa matriz, podendo ocorrer nas formas de sulfetos, tiofenos,
mol?culas polic?clicas contendo oxig?nio e nitrog?nio etc. Podem provocar corros?o,
envenenamento de catalisadores automotivos e de processos do refino. Na queima dos
combust?veis, quando presentes, d?o origem aos ?xidos SOX, que contribuem com a forma??o
da chuva ?cida, acidez do solo e problemas respirat?rios na popula??o. Logo, a determina??o
de enxofre ? de primordial interesse tanto para a ind?stria petroqu?mica quanto na ?rea da
qu?mica anal?tica. Diante dessa conjuntura, ? proposto neste trabalho o desenvolvimento de um
procedimento de preparo de amostras de petr?leo para determina??o por Cromatografia de ?ons
(IC) do teor de enxofre como sulfato (SO4
2-). Para tal, a decomposi??o por via ?mida em sistema
fechado assistida por radia??o micro-ondas, auxiliada pela a??o oxidativa de H2O2, foi o
procedimento adotado, onde a temperatura e pot?ncia m?xima de 230 ?C e 1000 W,
respectivamente, foram utilizadas no programa de aquecimento. Seis amostras de petr?leo
(?API entre 18,75-25,17) foram analisadas, sendo as concentra??es m?dias de enxofre obtidas
entre 377,50 e 3321,74 mg Kg-1, com DP entre ? 1,02 e ? 9,56. Para efeitos da avalia??o dos
resultados obtidos, realizou-se a determina??o do teor de enxofre nas amostras em estudo
utilizando a t?cnica UVF, fundamentada na norma oficial ASTM D5453-12, onde correla??es
entre 85,43 e 106,43% foram alcan?adas, evidenciando a efici?ncia do m?todo proposto na
convers?o das esp?cies de enxofre contidas nas amostras a sulfato e sua determina??o por IC.
A efici?ncia do procedimento de decomposi??o adotado foi testada atrav?s do RCC% e do
EOMD%, sendo alcan?ados teores entre 6,72 e 15,73% e 85,85 e 94,14%, respectivamente,
demonstrando a efici?ncia do procedimento de decomposi??o utilizado. / Sulfur is the third most abundant element in petroleum and is considered one of the main
contaminants present in this matrix, and may occur in the forms of sulfides, thiophenes,
polycyclic molecules containing oxygen and nitrogen etc. They can cause corrosion, poisoning
of catalysts used in refining and in automobiles. In fuel combustion, when present, they give
rise to SOX oxides, which contribute to the formation of acid rain, soil acidity and respiratory
problems in the population. Therefore, the determination of sulfur is of primary interest for the
petrochemical industry as well as for analytical chemistry. Considering this situation, it is
proposed the development of a procedure for the preparation of petroleum samples for the
determination of the sulfur content of sulfur (SO4
2-) by Ion Chromatography (IC). For this, the
wet decomposition assisted by microwave radiation, assisted by the oxidative action of H2O2,
was the adopted procedure, where the maximum temperature and power of 230 ?C and 1000
W, respectively, were used in the program of heating. Six petroleum samples (?API between
18.75-5.17) were analyzed, with the mean concentrations of sulfur being between 377.50 and
3321.74 mg Kg-1, with a standard deviation between ? 1.02 and ? 9.56. For the purposes of the
evaluation of the obtained results, the sulfur content in the samples under study was evaluated
using the UVF technique, based on the official standard ASTM D 5453-12, where correlations
between 85.43 and 106.43% were reached, evidencing the efficiency of the method proposed
in the conversion of the sulfur species contained in the samples to sulfate and its determination
by IC. The efficiency of the adopted decomposition procedure was tested using RCC% and
EDMO%, with levels between 6.72 and 15.73% and 85.85 and 94.14% being respectively
achieved, demonstrating the efficiency of the decomposition procedure used.

Identiferoai:union.ndltd.org:IBICT/oai:repositorio.ufrn.br:123456789/23875
Date30 June 2017
CreatorsGalv?o, ?lvaro Gustavo Paulo
Contributors13893734449, http://lattes.cnpq.br/2791074318745945, Costa, Emily Cintia Tossi de Ara?jo, 01282478435, http://lattes.cnpq.br/5051808662192151, Cunha, Jardel Dantas da, 01063473497, http://lattes.cnpq.br/3658783471840574, Dantas, Tereza Neuma de Castro, 07286937391, http://lattes.cnpq.br/0676872399141537, Silva, Djalma Ribeiro da
PublisherPROGRAMA DE P?S-GRADUA??O EM CI?NCIA E ENGENHARIA DE PETR?LEO, UFRN, Brasil
Source SetsIBICT Brazilian ETDs
LanguagePortuguese
Detected LanguageEnglish
Typeinfo:eu-repo/semantics/publishedVersion, info:eu-repo/semantics/masterThesis
Sourcereponame:Repositório Institucional da UFRN, instname:Universidade Federal do Rio Grande do Norte, instacron:UFRN
Rightsinfo:eu-repo/semantics/openAccess

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