Keywords: Pyrolysis GC, Automated Pyrolysis, Thermal Desorption
This paper describes an automated pyrolysis system for gas chromatography (GC) based on a filament type pyrolyzer combined with a commercially available thermal desorption instrument, onto which the pyrolysis module is installed. Automated sample introduction for both pyrolysis and thermal desorption is performed using a commercially available autosampler. For pyrolysis of solid, liquid, or melting samples the use of different types of sample holders is investigated, for example cup-type holders for liquid samples. A special design has been developed that enables accelerated gas phase transport to help reduce the formation of secondary pyrolysis products. Sample holder design and complete fl ow path heating are essential design aspects in order to maximize recovery and minimize carry-over, enabling the system to reliably perform automated analysis of batches of different sample types. These aspect are discussed.
Keywords: Pyrolysis, Thermogravimetric Analysis, Gas Chromatography, Mass Spectrometery, Evolved Gas Analysis
This study shows the use of the GERSTEL MPS/TDU/CIS with pyrolysis module for generating simulated thermal gravimetric mass spectrometry data (TGA-MS) of polymer samples. This mode of operation is also referred to as evolved gas analysis (EGA). For EGA analysis, a short piece of uncoated capillary is attached from the GC inlet to the mass spectrometer. A relatively slow temperature ramp is run similar to that used for actual TGA analysis. The total ion chromatogram can be plotted as a function of temperature to produce simulated TGA-MS data. The mass spectral data is used to identify degradation products at various temperatures. Several types of polymers are examined in this study. Simulated TGA-MS data is compared with actual TGA data.
Keywords: Pyrolysis-GC/MS, Methylationm TMAH, Fatty Acid Methyl Esters, FAME, Linseed Oil, Amber
In order to improve pyrolysis chromatographic analysis of materials that release polar functional groups e.g. carboxylic acids, a simple and rapid methylation method based on TDU pyrolysis/GC-MS in the presence of tetramethylammonium hydroxide (TMAH) was developed. Linseed oil was selected as test material because of its high triglyceride content comprising both saturated and unsaturated fatty acids. Pyrolysis was performed at 500, 600 and 700°C using GERSTEL pyrolysis module (PYRO) with a heated platinum filament.
Keywords: Whiskey, Oak Barrel, Pyrolysis GC/MS
Pyrolysis GC/MS was used to profile residual solids after drying aged whiskey samples. The samples in question were both 20 years old from the same un-aged parent distillate but matured in the very different wood species of Quercus Robur and Quercus Alba. Fractionated pyrolysis chromatograms generated at 450°C were obtained for both the different whiskey residues and samples of the respective wood species. The whiskey residues showed differences in peak pattern profiles and the same differences were observed between each residue and its originating wood. Pyrolysis GC/MS could be applied to whiskey maturation investigations and can help to establish a link between the spirit non-volatile fraction and the type of wood used for maturation.