The selection of outgas temperature for shale in low-pressure N adsorption: An evidence from thermogravimetry

Low-pressure N 2 adsorption (LPNA) could provide quantitative data for characterizing the pores in gas shale. However, the inconsistencies of outgas temperature have caused significant deviations in LPNA experiments. To explore the effects of outgas temperature on pore characteristics, two shale samples of Lower Cambrian Niutitang formation from Northern Guizhou, China, were collected for LPNA experiments and thermogravimetry-fourier transform infrared (TG-FTIR) spectroscopy. The samples were outgassed at six temperatures: 80°C, 100°C, 150°C, 200°C, 250°C, 300°C. Larger adsorbed volumes were presented in the isotherms at higher outgas temperatures. Similar regularity is obtained from the relationship between specific surface area, micropore volume and outgas temperature. Comprehensive analysis of TG-FTIR and LPNA at different outgas temperature indicated that at lower outgas temperatures (from 80°C to 100°C), the free water was unlikely to be removed completely, and resulted in large amounts of micropores couldn’t be accessed. An excessive outgas temperature might expulse liquid hydrocarbons or decompose organic matter (from 200°C to 300°C), and could lead to the generation of micropores. When the sample were outgassed at 150°C, TG-FTIR analysis indicated that the sample composition unchanged and a better removal of free water happened. Therefore, 150°C should be a suitable outgas temperature for shale in LPNA experiments. The findings in this research not only provide reliable evidence for the selection of outgas procedure in LPNA for shale, but clarify the important effects of free water and volatile materials on pore accessibility in shale.