Geology Reference
In-Depth Information
Stankiewicz et al.
2000
) and, thus, they represent the macromolecular component.
Pyrolysis after either solvent extraction or thermodesorption lead to very similar
results. Thermodesorption was used in all samples for thermal extraction of com-
pounds not bound to macromolecule (e.g. encapsulated lipids generated during the
heating protocol), furthermore this technique had been previously used in a similar
heating protocol successfully (Stankiewicz et al.
2000
; Gupta et al.
2006b
). Solvent
extraction was used for select samples (e.g. saponifi ed residue of post matured leaf)
but both methods lead to very similar results.
Preparing the Gold Cell
A 50 cm gold tube of 10 mm diameter was cut into 10 pieces and heated at 700 °C
for 3 h in a furnace to make it permanently malleable. Subsequently, one side of
each cell was sealed with a clamp and welded at 1,400 °C with a graphite rod. The
cell was weighed in a balance, the experimental sample was inserted, and the cell
and sample were weighed.
The cells was then sealed in an argon chamber to eliminate oxygen. The cell was
cooled with a blast of liquid nitrogen to ensure that welding did not affect the sam-
ple. Following this the gold cell + sample was weighed again.
Autoclave Experiment
Gold cells were inserted into the body of a stainless steel reactor (Fig.
5.1
) and
the cylinder was fi lled with water. A high-pressure sealing head was screwed to
the reactor and the entire set-up was installed into the heater. The reactor head
Confined pyrolysis apparatus
Heater
Temperature
Control
Heater
Heater
Internal
thermocouple
High pressure
Valve + line
Gold cell
+Sample
Pressurizing
medium
Stainless steel
reactor
Fig. 5.1
Confi ned pyrolysis autoclave setup
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