Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

摘要

A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed.Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling.Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO_3 at a 3.3:6.5:1 volume ratio.For Pb,efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier.The drying temperature and ramp rate influenced the sensitivity obtained for Ni,and had to be carefully optimized.Taking this into account,the same sensitivity was attained in all investigated organic media stabilized as microemulsion.Thus,calibration with microemulsions prepared with a single organic solvent was possible,using aqueous or organic stock solutions.Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures.n-Hexane microemulsions were used for calibration,and good agreement was obtained between the results using the proposed and comparative procedures.Typical coefficients of variation (n=6) ranged from 1% to 4%,and from 1% to 3% for Ni and Pb,respectively.Detection limits (k=3) in the original gasoline or diesel samples,derived from 10 blank measurements,were 4.5 and 3.6 mug 1~(-1) for Ni and Pb,respectively,comfortably below the values found in the analyzed samples.