Controlled-pyrolysis chromatographic operations

Sharp and Paterson [41] used a Perkin Elmer filament pyrolysis unit fitted in a Perkin Elmer Ell gas chromatograph (pyrolysis temperature control 250-550 °C). The gas chromatographic column used is a 1.7 m x 3 mm od stainless steel column packed with 30% m/m silicone oil (Embaphase) on acid washed Celite, operated at 80 "C with a helium flow rate of 30 ml/min. The column effluent is split in the ratio 2 1 between a flame ionisation detector and an API MS12 mass spectrometer equipped with a glass fit type of molecular separator at 150 C. Mass spectra are scanned from m/e 200 to 20 at 8 seconds per decade under standard electron bombardment conditions, electron energy 70 eV, emission current 500 pA, accelerating voltage 8 kV and source temperature 200 °C. 

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