Dois métodos para determinação de vanádio em óleo combustível são propostos utilizando GF AAS. O primeiro é baseado na preparação de uma microemulsão da amostra que é diretamente injetada no tubo de grafite. As temperaturas de pirólise e atomização, 1500 e 2700 °C, respectivamente, foram otimizadas a partir das curvas de temperatura. Para este procedimento obteve-se um limite de detecção de 0,10 μg g -1 e uma massa característica de 87 pg. O outro método utiliza digestão da amostra com ácido sulfúrico, ácido nítrico e peróxido de hidrogênio. As temperaturas de pirólise e atomização, otimizadas, foram 1000 e 2700 °C, respectivamente. Para este procedimento, obteve-se um limite de detecção de 0,25 μg g -1 e uma massa característica de 63 pg. A exatidão de ambos os métodos foi confirmada pela análise do material de referência certificado NIST SRM 1634c-trace metals in fuel oil.Two methods for vanadium determination in fuel oil are proposed using GF AAS. The first is based on the preparation of a microemulsion followed by direct injection into the graphite tube. The pyrolysis and atomization temperatures, 1500 and 2700 °C, respectively, were chosen from the temperature curves. This procedure allows determination of vanadium with a detection limit of 0.10 μg g -1 and characteristic mass of 87 pg. The other method uses total acid digestion of the sample with sulfuric acid, nitric acid and hydrogen peroxide. In this procedure, the pyrolysis and atomization temperatures recommended were 1000 and 2700 °C, respectively. Among the analytical characteristics for this method are a detection limit of 0.25 μg g -1 and a characteristic mass of 63 pg. The accuracy of both procedures was confirmed by the determination of vanadium in the certified reference material NIST SRM 1634c-trace metals in fuel oil.Keywords: vanadium, fuel oil, microemulsion, digestion sample, GF AAS
IntroductionThe determination of metals and non-metals in petroleum and its derivatives is of great interest regarding the quality of oil and for environmental aspects. The most difficult part is usually the sample preparation, the most reliable procedure being ashing of the sample and analysis of the residue after taking up in hydrochloric acid. 1 However, this procedure is quite tedious and requires careful control to avoid analyte losses, and even microwave-assisted digestion procedures require relatively long time. 2 Graphite Furnace Atomic Absorption Spectrometry (GF AAS) is offering advantages over other techniques since the results from a simple dilution with an organic solvent and ashing were found to be practically identical. 3,4 However, stability of metal concentration in sample and calibration solutions might become a serious problem 1567 Amorim et al. Vol. 18, No. 8, 2007 under these conditions. 5,6 The formation and analysis of an oil-in-water emulsion or microemulsion instead of a dilution of the oil sample with an organic solvent has been proposed to avoid this problem. [7][8][9][10][11] Fuel oil is a highly viscous residual fraction of petrol...