微波诱导燃烧样品处理技术测定轻油和重油中的金属与非金属

A method for light and heavy crude oil digestion using microwave-induced combustion (MIC) in closed vessels is described for further determination of Ag, As, Ba, Bi, Ca, Cd, Cr, Fe, K,Mg, Li,Mn, Mo,Ni, Pb, Rb, Se, Sr, Tl, V, and Zn by inductively coupled plasma mass spectrometry (ICP-MS). Conventional microwaveassisted acid digestion (MW-AD) in pressurized vessels and analyte determination by inductively coupled plasma optical emission spectrometry (ICP OES) were also used for results comparison. For MIC procedure,
samples were wrapped in polyethylene films and combusted using 20 bar of oxygen and 50 μl of 6 mol l−1 ammonium nitrate as aid for ignition. The concentration of nitric acid used as absorbing solution was evaluated (1, 2, 4, 7, 10 and 14 mol l−1) using an additional reflux step after combustion. Accuracy was evaluated for As, Ba, Ni, Se V, and Zn using certified reference material (CRM) with similar matrix composition and for Cr, Fe, K, Mg, Mn, and Mo by neutron activation analysis (NAA). Recovery tests were also performed for all the analytes by MIC and they were better than 97% using 2 mol l−1 nitric acid as absorbing solution (with reflux step). Agreementwith certified values and NAA results was better than 95%. Using MIC it was possible to obtain lower limits of detection (LODs) by ICP-MS and also by ICP OES in comparison with those obtained by MW-AD. In spite of both sample preparation techniques were apparently suitable for crude oil digestion, MIC was preferable in view of the possibility of using diluted nitric acid as absorbing solution that is an important aspect to minimize interferences by ICP-MS and ICP OES. In order to avoid polyatomic interferences on 52Cr and 56Fe determinations by ICP-MS, a dynamic reaction cell with ammonia gas was used. Residual carbon content in digests obtained by MW-AD and MIC was 15% and b1%, respectively. Using MIC the simultaneous digestion of 8 samples was possible in less than
30 min.