Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-09-05T19:25:25Z No. of bitstreams: 1 AlvaroGustavoPauloGalvao_DISSERT.pdf: 2667387 bytes, checksum: 5bf60c0285a5be566d4b19dddc68fd68 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-09-13T21:41:06Z (GMT) No. of bitstreams: 1 AlvaroGustavoPauloGalvao_DISSERT.pdf: 2667387 bytes, checksum: 5bf60c0285a5be566d4b19dddc68fd68 (MD5) / Made available in DSpace on 2017-09-13T21:41:06Z (GMT). No. of bitstreams: 1 AlvaroGustavoPauloGalvao_DISSERT.pdf: 2667387 bytes, checksum: 5bf60c0285a5be566d4b19dddc68fd68 (MD5) 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.