A rapid, accurate ultra-trace mass spectrometric metal analysis using chelates of 1,1,1,2,2,3,3-heptafluoro-7,7- dimethyl-4,6-octanedione has been developed. The analysis of fourteen metals (Al, Cr, Fe, Ni, Cu, Y, Pd, Nd, Sm, Dy, Ho, Tm, Yb, Pb) has been accomplished using direct insertion to the ionizing source. Quantitative results have been obtained on the order of 10-12 g of the metal and sensitivities as low as 10-14g. The fragmentation patterns are generally simple allowing analysis of mixtures without preconcentration or chemical separation. Sample preparation and introduction are discussed and mass spectra of pure compounds and mixtures are presented. © 1969, American Chemical Society. All rights reserved.