Uniformity and volume-representativity of consecutive submillimetre wafers of shale for SANS and USANS investigations
(Ultra) Small Angle Neutron Scattering (SANS/USANS) is a non-destructive technique suitable for characterization of porous structures from nano- to micro-pore size (1 nm to 20 μm), which has been widely used to characterize accessible and inaccessible porosity in tight unconventional hydrocarbon reservoirs (e.g., shales). Here, in this study, SANS and USANS are used to examine the degree of nano- to micropore uniformity of the rock body on sub-millimetre to centimetre scale. This study presents a test of the hypothesis of volume representativity of pore structure information measured by SANS and USANS for shale wafers (0.22–1 mm) cut from six North American unconventional shale cores of different maturities (New Albany Shale and Marcellus Shale). Experimental reproducibility of USANS is further investigated for two wafers measured using various acquisition times. All samples show that fluctuations of the relative intensity generally decrease from the USANS Q-range (pore size from around 200 nm to 20 μm) to most of the SANS Q-range (pore size from around 5 nm to 700 nm), and peaks in the SANS large-Q region (for pores smaller than about 5 nm). There is a positive correlation between the spatial fluctuation of the relative SANS intensity and the scattering power of shales. In addition, the scattering intensity and its fluctuations is larger for the less mature shale cores. Shale is known to be highly heterogenous and the hypothesis of uniformity does not apply at sub-millimetre scale even for samples that appear homogeneous at visual inspection. This study presents an approach to minimise the variation through sample selection, data interpretation methodology and instrumental reproducibility tests. The best values of the microstructural spatial uniformity for the apparently homogeneous sections of a core (i.e., the SANS and USANS intensity variation) is less than ±10%.