An emission spectrometric detector is used in the determination of metal acetylacetonates. Spectra are excited in the plasma of a 2450 MHz electrodeless discharge. Measuring the intensities of the atomic emission lines of aluminium, beryllium and chromium after gas chromatography provides a highly sensitive and selective method for the determination of the acetylacetonates of these metals. Detection limits are 100 ng for aluminium, 0.01 ng for beryllium and 1 ng for chromium. An analytical procedure is proposed for beryllium down to 10 ppm in aluminium.