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We measured steady-state liquid (dodecane) permeability in four horizontal core plugs from the middle member of the Bakken Formation at multiple effective stress conditions to investigate how permeability evolves with confining stress and to infer the matrix permeability. Three of the four tested samples behaved almost perfectly elastically as the hysteresis effect was negligible. In contrast, the fourth sample showed a permeability decrease of ~40% at the end of the test program. Our interpretation is that the closure of open artificial micro-fractures initially present in the sample (based on micro-CT imaging) caused that permeability hysteresis. The matrix permeability to dodecane (oil) of the tested samples is between ~50 nD and ~520 nD at the confining pressure of 9500 psi. The 520 nD sample exhibited the lowest porosity, the highest calcite content, and the largest dominant pore throat radii. In contrast, the 50 nD sample was more porous, and exhibited the highest dolomite content and the smallest dominant pore throat radii. This study shows that our multi-stress testing protocol allows the study of the permeability hysteresis effect to interpret the matrix permeability. We also document the presence of middle Bakken lithologies with permeabilities up to one order of magnitude greater than others. These permeable lithologies may have a significant contribution to well production rates.

Argon gas and liquid (dodecane) permeability measurements in two mixed quality siliceous mudstone samples within the Wolfcamp formation demonstrate that it is possible to close multiple bedding parallel open artificial micro-fractures and obtain representative matrix permeability by applying two confining stress cycles at a constant pore pressure under effective stresses ranging from 6.9 MPa to 59.7 MPa. The clearly micro-fractured sample exhibited a three-order decrease in permeability from 4.4 × 10−17 m2 to 2.1 × 10−20 m2. In contrast, the relatively intact sample exhibited initial liquid permeability of 1.6 × 10−19 m2 that declined gradually with stress to 3.0 × 10−20 m2. In this study, we developed a new permeability testing protocol and analytical approaches to interpret the evolution of micro-fractures and estimate the matrix permeability based on initial pulse-decay gas permeability measurements. The insights gained are useful to identify pore-scale controls on fluid flow behavior using SEM petrography and pore-space characterization and validate fundamental fluid flow mechanisms examined using pore-scale numerical models.

International audience; The Vaca Muerta Formation is currently regarded as the most prolific source rock interval for unconventional petroleum exploration in Argentina. In this study, we integrate recent CT-scanner, nuclear magnetic resonance (NMR) T1-T2 and Rock-Eval Shale Play® analytical techniques, combined with classical geochemical, petrological and petrophysical methods to characterize Vaca Muerta source rocks along a vertical profile. The proposed analytical workflow was tested here on 4 samples derived from one core: the LJE-1010 borehole drilled in the lowermost Jurassic Vaca Muerta member (Neuquén Basin – Argentina), to evaluate the unconventional hydrocarbon potential and pore network attributes. First, entire rock samples were analyzed by dual energy CT scanner to evaluate possible heterogeneities; this also helped in the selection of representative samples. Then the organic matter properties were investigated by open-system pyrolysis techniques, organic petrography and biomarker analyses as a function of the core depth. A comparative approach between open-system pyrolysis methods (e.g. Rock-Eval Basic/Bulk-Rock & Shale Play® methods vs. Source Rock Analyzer) is also illustrated in this work. Finally, petrophysical characteristics and pore network attributes in shale were estimated by gas permeability (steady-state method corrected for Klinkenberg effect), porosity and NMR methods. The investigated samples have oil-window maturity and are characterized by a network of solid bitumen. Based on new Rock-Eval Shale Play® data, the potentially producible oil present in the rock samples was estimated using the modified oil saturation index (OSI = Sh0 + Sh1 peaks × 100/TOC). Results indicate that the oil crossover effect and potential productive oils occur within intervals showing higher TOC values (~ 3 to 8 wt%). We also illustrated here that, for unconventional shale play perspectives, Rock-Eval Shale Play® parameters (Sh0 & Sh1) allow to obtain both a better quantification of free and retained hydrocarbons in source-reservoir rock samples and correct original oil in place (OOIP) estimations in early exploration campaign for shale oil and shale gas assessment. For Vaca Muerta rock samples, OOIP estimations range from 60 to 160 bbl oil/acre-ft, approximately. We also demonstrated that the solid bitumen, oil and organic matter are clearly distinguished in the studied samples using advanced NMR T1-T2 maps obtained at different temperatures. The solid bitumen was clearly evidenced as a peak with T1/T2 ratio ~ 14 on NMR T1-T2 maps. Concerning the matrix bulk rock permeability, the obtained results showed that the most deep sample is characterized by a permeability of about 140 nanoDarcy (nD) whereas the shallower sample containing also higher amounts of organic matter is more permeable (~ 213 nD), indicating that TOC values play a main control on Vaca Muerta poromechanical characteristics. The maximum total porosity values range between 6.5 and 21.8% and were calculated in this work integrating NMR and helium porosity values. Finally, global interpretations of these obtained results suggest that the Vaca Muerta Formation could be considered as a prolific shale play interval for unconventional petroleum exploration in the near future.