The behaviour of Ni and Pb in different organic liquids relatively to their determination by GFAAS was investigated. The following organic liquids were studied: n- hexane, n-heptane, n-octane, isooctane, toluene, n-decane, hexadecane and mixtures of n-octane + acetone (99+1, v/v), n-octane + bromoform (99+1, v/v), and n-octane + carbon disulfide (99+1, v/v). Concerning stability, ng ml-1 solutions prepared by direct dissolution of organic standards in the different organic liquids showed significant Ni and Pb losses after only few minutes. No clear loss pattern related to chain length or form could be observed, although the losses were systematically slower when the O, S and Br compounds were present. Excellent long term sample stabilization was observed for the different organic media investigated if microemulsions are used. Microemulsions were prepared by mixing 6.5 ml of propan-1-ol with 3.3 ml of the organic liquid and 0.1 ml of 50% v/v HNO3. Ni and Pb could be added in the aqueous or aqueous forms. Conventional aqueous modification was allowed as well as Ir as permanent modifier. The dry and ramp steps showed to influence sensitivity, and must be carefully optimized. The same sensitivity was observed for the different microemulsion stabilized organic media. Thus, calibration with microemulsions prepared with a single organic solvent was possible. Commercial gasoline and diesel samples were analyzed after microemulsion stabilization and by a comparative procedure. Good concordance between both procedures was observed. Detection limits (k=3) in the original gasoline or diesel samples, derived from ten blank measurements were 4.5 and 3.6 µgl-1 for Ni and Pb, respectively, well above the values found in the analyzed samples.