A method for digestion of crude oil distillation residues (atmospheric residue, AR and vacuum residue, VR) using microwave-induced combustion (MIC) was developed for simultaneous determination of metals (Ba, Co, Fe, Mg, Mn, Ni and V) and sulfur by inductively coupled plasma optical emission spectrometry (ICP-OES). Samples were wrapped in polyethylene films and combusted using 20 bar of oxygen. Nitric acid solutions were evaluated using 5 min of reflux after combustion. Accuracy was evaluated using certified reference material and comparison with the results obtained by microwave-assisted wet digestion (MAWD). No statistical difference was observed between the certified values and those obtained using MIC as well as between the values obtained using MAWD or MIC. In spite of both methods have been apparently suitable for crude oil digestion, MIC was preferable in view of the possibility of using 3 mol L-1 HNO3 as absorbing solution. Furthermore, it is important to notice that using MIC, C content in digests was lower than 10 mg L-1, preventing interferences in ICP-OES. In addition, the simultaneous digestion of eight samples was possible in less than 30 min and without using concentrated acids and/or longer heating times, making the proposed method well-suited for routine analysis.

Radiação micro-ondas em sistema fechado foi utilizada para a remoção de sedimentos de emulsão de petróleo para a posterior caracterização em laboratório. O programa de aquecimento do forno de micro-ondas foi otimizado através da avaliação do tempo de aquecimento (5 a 30 s) e da potência de micro-ondas (300 a 1400 W). O teor de sedimentos foi determinado usando um procedimento de filtração com membrana conforme recomendado pela norma ASTM D 4807-05, antes e após a remoção de sedimentos. Os teores de água e cloreto foram determinados no óleo obtido após a remoção de sedimentos. Até oito amostras de 20 g puderam ser processadas simultaneamente. A eficiência de remoção de sedimentos foi superior a 95%. Foi possível a obtenção de petróleo virtualmente isento de água, sal e sedimentos, permitindo a determinação de parâmetros como gravidade API, densidade, viscosidade e número de acidez total sem interferências causadas por sedimentos ou mesmo sal e água.

Microwave radiation in closed vessels was applied for removal of sediments from crude oil allowing the subsequent crude oil characterization in laboratory. Heating time and microwave power were evaluated in the range of 5 to 30 s and 300 to 1400 W, respectively. Sediment content was determined using the method recommended by ASTM D 4807-05 based on a filtration step in a membrane before and after sediment removal. Water and chloride contents were determined in the oil phase obtained after sediment removal. Up to eight samples of 20 g of crude oil could be simultaneously processed. Sediment removal efficiency was better than 95%. It was possible to obtain crude oil in a suitable condition for determination of routine parameters as API gravity, density, viscosity and total acid number without interferences caused by sediments or even water and salt.

O potencial da técnica de espectroscopia de infravermelho com transformada de Fourier e acessório de reflexão total atenuada (FTIR-ATR) foi avaliado para o monitoramento da degradação da poliamida 11 (PA-11) usada em dutos flexíveis. As amostras foram submetidas a envelhecimento em reatores com pressão controlada e atmosfera inerte. Os corpos de prova foram imersos em água deionizada (pH 7), nas temperaturas de 110, 120 e 140 ºC por um período de até 50 dias. A técnica recomendada para monitoramento da degradação da PA-11 é a viscosimetria, através de medidas da viscosidade inerente corrigida (VIC) e a análise termogravimétrica (TGA). O comportamento observado para a VIC e TGA durante o envelhecimento possibilitou a construção de modelos que correlacionam com a técnica de FTIR-ATR. A partir dos resultados de FTIR-ATR, a variação na intensidade da banda atribuída à fase amorfa, 1161 cm-1, possibilitou o monitoramento do envelhecimento quando associamos a técnica a modelos quimiométricos como o de regressão dos mínimos quadrados parciais, PLS. Portanto, a técnica FTIR-ATR pode ser uma nova alternativa no monitoramento da degradação hidrolítica da PA-11, eliminando assim o uso de solventes orgânicos tóxicos e reduzindo, consequentemente, o tempo de análise.

The potential of the infrared spectroscopy with the attenuated total reflection technique (FTIR-ATR) was evaluated to monitor degradation of polyamide 11, PA-11, applied in flexible pipes. The samples were subjected to aging on reactors with controlled pressure and atmosphere. The samples were immersed in deionized water, pH 7, at temperatures of 110, 120 and 140 ºC over a period of up to 50 days. The typical technique recommended for monitoring PA-11 degradation is viscometry from inherent viscosity corrected (VIC) and thermogravimetric (TGA) measurements. TGA and VIC results allowed the use of chemometric models that can be related to FTIR-ATR spectra, with assignment of a band to the amorphous phase (1161 cm-1) of PA-11. The chemometric model generated from PLS data was satisfactory in predicting the aging of PA-11. Therefore, FTIR-ATR can be used as a new analytical methodology to monitor PA-11 degradation, thus eliminating the use of toxic organic solvents and reducing the time required for the analysis.