The palladium and vanadium(IV) oxide complexes of bis(acetylacetone)-meso-stilbenediimine (meso-H2AA2S), bis(acetylacetone)dl-stilbenediimine (dl-H2AA2S), bis(trifluoroacetylacetone)meso-stilbenediimine(meso-H2F2AA2S) and bis(trifluoroacetylacetone)dl-stilbenediimine(dl-H2F3AA2S) have been prepared, and their DTA and TGA indicate that the complexes are somewhat volatile. The complexes eluted from the stainless steel gas chromatographic column (2 m x 3 mm) and (3 m x 3 mm) packed with OV101, 3% on Chromosorb 80-100 mesh size and Dexil 400 GC, 2% on Uniport HP 60-80. The linear calibration ranges were within 0.5-20-mu-g and detection limits were within 10-250 ng of metal complexes at the optimized conditions of separation. The relative elution of the metal complexes on nonpolar column indicated that introduction of phenyl groups increases and trifluoromethyl group decreases on column retention of the metal complexes.