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Molecular and Carbon Isotopic Variation During Canister Degassing of Terrestrial Shale: a Case Study from Xiahuayuan Formation in the Xuanhua Basin, North China

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Molecular and Carbon Isotopic Variation During Canister Degassing of Terrestrial Shale: a Case Study from Xiahuayuan Formation in the Xuanhua Basin, North China minerals Article Molecular and Carbon Isotopic Variation during Canister Degassing of Terrestrial Shale: A Case Study from Xiahuayuan Formation in the Xuanhua Basin, North China Jia Tao 1, Jinchuan Zhang 1,2,*, Junlan Liu 3, Yang Liu 1, Wei Dang 4, Haicheng Yu 5, Zhe Cao 6,7, Sheng Wang 1 and Zhe Dong 1 1 School of Energy Resources, China University of Geosciences (Beijing), Beijing 100083, China; [email protected] (J.T.); [email protected] (Y.L.); [email protected] (S.W.); [email protected] (Z.D.) 2 Key Laboratory of Strategy Evaluation for Shale Gas, Ministry of Land and Resources, China University of Geosciences (Beijing), Beijing 100083, China 3 PetroChina Research Institute of Petroleum Exploration & Development, Beijing 100083, China; [email protected] 4 School of Earth Sciences and Engineering, Xi’an Shiyou University, Xi’an 710065, China; [email protected] 5 Hebei Province Coal Geological Exploration Institute, Xingtai 054000, China; [email protected] 6 Sinopec Petroleum Exploration and Production Research Institute, Beijing 102206, China; [email protected] 7 China State Key Laboratory of Shale Oil and Shale Gas Resources and Effective Development, Beijing 102206, China Citation: Tao, J.; Zhang, J.; Liu, J.; * Correspondence: [email protected] Liu, Y.; Dang, W.; Yu, H.; Cao, Z.; Wang, S.; Dong, Z. Molecular and Abstract: Molecular and carbon isotopic variation during degassing process have been observed Carbon Isotopic Variation during in marine shale reservoirs, however, this behavior remains largely unexplored in terrestrial shale Canister Degassing of Terrestrial Shale: A Case Study from reservoirs. Here, we investigate the rock parameters of five terrestrial shale core samples from Xiahuayuan Formation in the the Xiahuayuan Formation and the geochemical parameters of thirty natural gas samples collected Xuanhua Basin, North China. during field canister degassing experiments. Based on these new data, the gas composition and Minerals 2021, 11, 843. https:// carbon isotope variation during canister degassing are discussed and, further, the relationship doi.org/10.3390/min11080843 between petrophysics and the carbon isotope variation is explored. The results show that methane content first increases and then decreases, the concentrations of carbon dioxide (CO2) and nitrogen Academic Editors: Paula gas (N2) peak in the early degassing stage, while heavier hydrocarbons gradually increase over Alexandra Gonçalves time. Shale gas generated from humic source rocks contains more non-hydrocarbon and less heavy and Carolina Fonseca hydrocarbon components than that generated from sapropelic source rocks with similar maturity. 13 Time-series sampling presents an upward increase in δ C1 value during the degassing process with Received: 13 July 2021 13 13 the largest variation up to 5.7‰, while the variation in δ C3 and δ C2 is insignificant compared Accepted: 3 August 2021 to δ13C . Moreover, we find that there is only a small variation in δ13C in shale samples with high Published: 5 August 2021 1 1 13 permeability and relatively undeveloped micropores, which is similar to the limited δ C1 variation Publisher’s Note: MDPI stays neutral in conventional natural gas. For our studied samples, the degree of carbon isotope variation is with regard to jurisdictional claims in positively correlated with the TOC content, micropore volume, and micropore surface, suggesting published maps and institutional affil- that these three factors may play a significant role in carbon isotope shifts during shale gas degassing. 13 + iations. We further propose that the strong C1 and C2 depletion of shale gas observed during the early degassing stage may have resulted from the desorption and diffusion effect, which may lead to deviation in the identification of natural gas origin. It is therefore shale gas of the late degassing stage that would be more suitable for study to reduce analytic deviations. In most samples investigated, Copyright: © 2021 by the authors. significant isotopic variation occurred during the degassing stage at room temperature, indicating Licensee MDPI, Basel, Switzerland. that the adsorbed gas had already been desorbed at this stage Our results therefore suggest that more This article is an open access article parameters may need to be considered when evaluating the lost gas of shales. distributed under the terms and conditions of the Creative Commons Keywords: molecular variation; isotope variation; terrestrial shales; core degassing; reservoir physi- Attribution (CC BY) license (https:// cal properties; micropore parameters creativecommons.org/licenses/by/ 4.0/). Minerals 2021, 11, 843. https://doi.org/10.3390/min11080843 https://www.mdpi.com/journal/minerals Minerals 2021, 11, 843 2 of 18 1. Introduction Molecular and isotope compositions are fundamental geochemical parameters in the study of natural gas origin and genetic type [1–4]. In addition to genetic processes, some secondary processes, such as adsorption/desorption, migration, diffusion, and dissolution, can also cause variations in molecular and isotopic compositions [5–7]. Extensive studies have shown that the molecular composition varies constantly during canister degassing of marine shale [8,9]. As another major target of shale gas exploration in China, terrestrial shale reservoir has shown significant differences from marine shale reservoirs, thus the degassing behavior of these two types of shale may also be expressed differently. However, the molecular and carbon isotopic variation of terrestrial shale during canister degassing has not been well documented. The consideration of stable isotope fractionation associated with the migration process started with a study by Colombo et al. [10], and was further discussed in later studies [6,11–13]. The directions and magnitudes of isotope shifts vary greatly (ranging from −1‰ to −30‰) during the desorption experiments of coal consider- ing different gas species across a wide maturity range [14–17]. Diffusion-related isotope shifts have been emphasised in previous studies and have mainly focused on conventional gas accumulations and the evaluation of gas loss through the shale caprock [7,18,19]. More detailed quantification models were proposed later to characterise diffusion-related isotope shifts during natural gas transport [20–22]. The dissolution carbon isotope effect has shown 13 the preferential solution of CH4 in an aqueous medium [21,23–25]. The influence of the adsorption carbon isotope effect has been controversial in the past. Gunter and Glea- son (1971) addressed the quantum mechanical effect on the dispersion energy-dominated carbon isotope behaviour through silica gel [5], causing the preferential adsorption of lighter species to reverse the expected trends during gas chromatographic separations. The same conclusion was reported by Rahn and Eiler (2001), who analysed the carbon and oxygen isotope effects for carbon dioxide adsorption onto kaolinite, basalt, and fluorite between the adsorbate and vapour phases [26]. However, other studies have suggested that the difference in adsorption potential is caused by the isotope shift in the adsorp- 13 tion/desorption process [27], resulting in a more negative δ C1 value during desorption experiments [28,29]. The controversy regarding the adsorption/desorption effect may be caused by the difference in adsorbing material because the adsorbing materials used in gas chromatographic separation experiments are quite different from those in natural gas reservoirs. The factors influencing the isotopic shift have been investigated in previous studies. Studies on the temperature dependence of the isotope effect have shown an increase in the diffusion coefficient of methane with temperature [22,30]. Schloemer and Krooss (2004) conducted diffusion experiments and concluded that increasing pressure results in a decrease in the effective diffusion coefficient due to the reduction in overall molecular mobility [21]. In addition to external conditions, internal parameters also affect the diffusion isotope effect. Experimental work and mathematical simulation indicated that isotopic fractionation was enhanced by an increase in organic matter in sedimentary rocks [20,29]. The canister degassing of coal showed a more obvious expression of isotope variation in higher rank coals [15]. The petrophysical parameters of reservoir rocks may have played an important role in the carbon isotope variation during the degassing process, however, their relationship remains unclear. For example, some studies have shown that there is no correlation between isotopic fractionation and porosity/permeability in reservoir rocks [29,30], while others have argued that the isotopic shift is inversely related to the rock porosity and permeability properties through physical simulation experiments [31,32]. The shale gas field has become an essential component of hydrocarbon exploration and development [33–36]. Compared with the extensive studies on carbon isotope variation in conventional caprocks or coal reservoirs, limited studies have focused on carbon isotope variation in shale reservoirs, especially in terrestrial shale reservoirs. In the present study, we aim to (1) investigate the molecular and carbon isotopic variation during canister degassing of terrestrial shale based on time-series sampling, (2) explore the influence of Minerals 2021, 11, 843 3 of 18 petrophysics on carbon isotope variation during canister degassing by combining bulk rock petrophysical parameters with gas
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