2012•Physical Testing and Chemical AnalysisRequires access
AFS Determination of Pb,As and Hg in Crude Oil with Microwave Assisted Sample Digestion
Pan Yi-long
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Abstract
AFS was applied to the determination of Pb,As and Hg in crude oil.The sample was digested with mixed solution of HNO3-H2O2(10+2),and thiourea solution was added to the sample solution as pre-reductant and KBH4 solution(dissolved in KOH solution) as reductant.Flow-rates of 300 mL·min-1 for carrier gas and 800 mL·min-1 for shielding gas were taken in the analysis.Linear relationships between values of fluorescence intensity and mass concentration of Pb,As and Hg found were in the ranges of 2.0-80.0,2.0-100.0 and 1.0-20.0 μg·L-1,with detection limit(3S/N) of 0.05,0.05 and 0.01 mg·kg-1 respectively.The proposed method was applied to the analysis of samples of crude oil,giving values of recovery in the ranges of 103%-115% for Pb,87.5%-92.1% for As and 87.5%-102% for Hg.