The
influence of degassing time and temperature on low-pressure
gas adsorption (LPGA) behavior of shales was examined in this study.
Two organic-rich shales of contrasting maturity, reactivity and organic
matter type, were crushed to <1 mm and <212 μm grain-sizes
and degassed at 110, 200, and 300 °C for 3 and 12 h, respectively.
Our results indicate that degassing duration has a minimal influence
on pore-character interpretations from LPGA experiments, while the
degassing temperature shows a strong influence on the pore attributes.
For both shales, reliable porosity estimates were obtained when the
samples were degassed at 110 °C. When the degassing temperature
was increased to 200 and further to 300 °C, distinct changes
in adsorption isotherms and other pore structural features were observed.
For the mesoporous low-mature shale (collected from a lignite mine)
when the degassing temperature was kept at 200 °C, a macroporous
character was induced with a manifold increase in pore diameter. Results
from thermogravimetry and Rock-Eval indicate abundance of reactive
kerogen, which undergoes alteration when degassed at higher temperatures.
When the degassing temperature was kept at 300 °C, the organic
matter underwent further alteration and showed an isotherm similar
to the shales degassed at 110 °C. Similarly, for the oil-window
mature shale sample, a transition towards macroporous structure was
observed when the sample was degassed at 200 and 300 °C, compared
to a mesoporous structure observed when degassed at 110 °C. The
results from fractal dimensions also support the above inferences,
indicating the presence of simpler structures at higher degassing
temperatures. Reduction in pore volume (110–200 °C) and
its further rise (200–300 °C) are also evident in the
micropore domain, more distinctly in the oil window mature shale.
Our results strongly indicate that degassing temperature should be
kept at around 110 °C for reliable shale pore character estimation.