Determinação de fósforo e enxofre em petróleo em ICP OES: comparação de diferentes procedimentos para o preparo de amostras

• Ano de defesa: 2015
• Autor(a) principal: Ribeiro, Maria Aparecida
• Tipo de documento: Dissertação
• Tipo de acesso: Acesso aberto
• Idioma: por
• Instituição de defesa: Universidade Federal do Espírito Santo; BR; Mestrado em Química; Centro de Ciências Exatas; UFES; Programa de Pós-Graduação em Química
• Palavras-chave em Português: Microwave oven; Microemulsion; Sample Preparation; micro-ondas; Microemulsão; Preparo de amostras; Petróleo; Fósforo; Enxofre; Emulsões; Preparação de amostra (Química); Química; 54
• Link de acesso: http://repositorio.ufes.br/handle/10/4736

The presence of sulfur and phosphorus in thecrude oil can causes several problems in the petroleum industryascatalysts deactivation,deposited in distillation towers, corrosion and decrease in quality of crude oil as well as environmental pollution. Thus are required sensitive analytical techniques, efficient and fast for the determination of these elements in crude oil allowing preventive and / or corrective are taken in the same extraction and during its refining. This study aims to develop a procedure for determination of phosphorus and sulfur by ICP OES technique in oil, for different sample preparation procedures: hot extraction with solventorganics, acid microwave-assisted acid digestion using and formation of microemulsion. The spectral lines for sulfur 181.975 nm (I) in the radial configuration and 213.617 nm (I) phosphorus in the axial configuration was used for this. The first sample preparation procedure that used the extraction with solvent organics did not represent a good alternative to the full determination of the elements, because the extraction efficiency of them was very low. For the acid digestion assisted by microwave and microemulsion formation have been found LOD: 0.01 mgL-1for phosphorus and 0.05 mgL-1for sulfur using the digestion procedure, and 0.02 mg L-1for phosphorus and 2.5mgL-1for sulfur using the microemulsion formation process. Good accuracy us were achieved in both procedures was evaluated when the recovery percentage for the match and reference material (Nist 1634.c) for sulfur. However, for its simplicity of preparation and low cost, the microemulsion formation can be a good alternative to oil samples preparation for subsequent determination of phosphorus and sulfur by ICP OES