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1 Desorption and Adsorption of Subsurface Shale Gas Desorption and Adsorption of Subsurface Shale Gas DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By Fengyang Xiong, M.S. Graduate Program in School of Earth Sciences The Ohio State University 2020 Dissertation Committee: Joachim Moortgat, Advisor David Cole Tom Darrah Derek Sawyer 1 Copyrighted by Fengyang Xiong 2020 2 Abstract Storage of subsurface shale gas is challenging to characterize because nanoporous shales consist of almost all commonly observed minerals and develop a wide pore size distribution of 0.4 nm to 1 ��. Petroleum geoscientists classify the subsurface shale gas into three components: free gas in the pore space, adsorbed gas on mineral surfaces, and dissolved gas in formation fluids and organic matter. Based on investigations of shale gas plays in the United States, the adsorbed gas can contribute up to 85% of the total shale gas- in-place (GIP). And the storage of adsorbed shale gas, which mainly consists of methane, is determined by multiple geological properties, e.g., pore structure, mineral composition, temperature, pressure, and water saturation. These complex multivariate relationships complicate the assessment of subsurface adsorbed gas, which is still challenging for exploration geoscientists to quantitatively characterize. In this dissertation, we investigate the pore structure of shales, including the roles of organic matter, mainly insoluble kerogen, and inorganic minerals in pore development using Soxhlet extraction and low-pressure nitrogen and carbon dioxide adsorption isotherms. We then study the relationship between in-situ desorbed gas and mineralogy on large core samples. Most importantly, we propose an experimental procedure to estimate the pressure-dependent density of adsorption, which will significantly improve future estimates of adsorbed gas in shale GIP assessment. Finally, we modify and compare a ii number of currently widely used supercritical adsorption models to obtain critical thermodynamic parameters that are significant in the shale GIP evaluation and exploitational design. iii Dedication Dedicated to my advisors, committee members, and friends for your patient help; my family for unconditional encouragement and accompany. iv Acknowledgments As the one whom I learned from and admire most, Dr. Joachim Moortgat deserves all the honor that I received through the past four post-graduate years, for revision of all my submitted journal manuscripts, proposals of my research and travel grants, scholarship application, and writing all the letters of reference. Thanks for every group meeting, house cooking, and big event gathering at Ethyl & Tank. Beyond supervising, he is more like a good friend to me, shaping my professional attitude and value to his best. I am also deeply grateful to my committee members, Dr. Derek Sawyer, Dr. Tom Darrah, and Dr. David Cole for their time, advice, and strong support for my research and dissertation writing. Especially, specific thanks to Dr. Derek Sawyer for his guidance for the AAPG/SEG student chapter and training of seismology interpretation; Dr. Tom Darrah for providing shale samples for my research and sharing the room with me at GSA 2017 Annual Meeting; Dr. David Cole for communicating with ORNL, providing samples and facilities for my research, and SEED and CERTAIN grants for my research and student chapter outreach, respectively. Additionally, I would like to truly thank Dr. Amin Amooie and Dr. Reza Soltanian, who have left OSU and are currently pursuing a higher level of academic development. Their friendly advice, encouragement, and mentoring help me live through the beginning of my PhD life. Specific thanks to Dr. Amin Amooie for helping me settle v down at Columbus; Dr. Reza Soltanian for helping my search for postdoc positions. And I am grateful to my other group fellows, Dr. Di Zhu, Dr. Mengnan Li, Billy Eymold, and Derrick James, for their advice and encouragement. Also, I am thankful to my collaborators, Dr. David Tomasko, Dr. Gernot Rother, Julie Sheet, Susan Welch, Alex Swift, Bohyun Hwang, and Yiwen Gong. Big thanks for their time and help with my training and experiments at OSU and ORNL. I also acknowledge Theresa Mooney, Angie Rogers, Steven Lower, and Matthew Saltzman for their help with my travels and purchase orders, academic affairs, teaching associate, and scholarship application. Lastly, I want to thank my younger and older sister for taking care of my mother during my PhD study, which helps me comfort and focus on my study and life in the United States. And thanks to all my brothers, sisters, uncles and aunts for your love, support, and encouragement. vi Vita 2009-2013 China University of Petroleum, Beijing (B.Sc. of geological engineering) 2013-2016 China University of Petroleum, Beijing (Master of petroleum geology) 2016-2020 The Ohio State University (PhD program in Earth Sciences/Geology) 2019 Summer Oak Ridge National Lab (visiting student) Publications [18] Xiong, F., Rother, G., Tomasko, D., Pang, W., Moortgat, J. On the pressure and temperature dependence of adsorption density and other thermodynamic properties in gas shales. Chemical Engineering Journal 2020, 395, 124989. [17] Xiong, F., Jiang, Z., Huang, H., Wen, M., Moortgat, J. Mineralogy and gas content of Upper Paleozoic Shanxi and Benxi Shale Formations in the Ordos Basin, Energy & Fuels 2019, 33, 1061–1068. [16] Xiong, F.Y., Jiang, Z.X., Li, P., Wang, X.Z., Bi, H., Li, Y.R., Wang, Z.Y., Amooie, M.A., Soltanian, M.R., Moortgat, J. Pore structure of transitional shales in the Ordos Basin, NW China: effects of composition on gas storage capacity. Fuel 2017, 206, 504–515. [15] Xiong, F.Y., Jiang, Z.X., Chen, J.F., Wang, X.Z., Huang, Z.L., Liu, G.H., Chen, F.R., Li, Y.R., Chen, L., Zhang, L.X. The role of the residual bitumen in the gas storage vii capacity of mature lacustrine shale: A case study of the Triassic Yanchang shale, Ordos Basin, China. Marine and Petroleum Geology 2016, 69, 205-215. [14] Xiong, F.Y., Jiang, Z.X., Tang, X.L., Li, Z., Bi, H., Li, W.B., Yang, P.P. Characteristics and origin of the heterogeneity of the Lower Silurian Longmaxi marine shale in southeastern Chongqing, SW China. Journal of Natural Gas and Engineering 2015, 27, 1389-1399. [13] Huang, H., Li, R., Xiong, F., Huang, S., Sun, W., Jiang, Z., Chen, L., Wu, L., 2020. A method to probe the pore-throat structure of tight reservoirs based on low-field NMR: Insights from a cylindrical pore model, Marine and Petroleum Geology 2020, 104344. [12] Gong, Y., Mehana, M., El-Monier, I., Xu, F., Xiong, F., Machine learning for estimating rock mechanical properties beyond traditional considerations, Unconventional Resources Technology Conference, Denver, Colorado 2019, 466- 480. [11] Huang, H., Sun,W., Xiong, F., Chen, L., Li, X., Gao, T., Jiang, Z., Ji,W., Wu, Y., Han, J. A novel method to estimate subsurface shale gas capac- ities, Fuel 2018,232, 341– 350. [10] Gao, F., Song, Y., Li, Z., Xiong, F., Chen, L., Zhang, Y., Liang, Z., Zhang, X., Chen, Z., Moortgat, J. Lithofacies and reservoir characteristics of the Lower Cretaceous continental Shahezi Shale in the Changling Fault Depression of Songliao Basin, NE China, Marine and Petroleum Geology 2018, 98, 401-421. viii [9] Gao, F., Song, Y., Li, Z., Xiong, F.Y., Moortgat, J., Chen, L., Zhang, X., Chen, Z. Quantitative characterization of pore connectivity using NMR and MIP: A case study of the Wangyinpu and Guanyintang Shales in the Xiuwu Basin, Southern China, International Journal of Coal Geology 2018, 197, 53-65. [8] Wang, Z., Liu, L., Pan, M., Shi, Y., Xiong, F., High-Frequency Sequence Stratigraphy and Fine-Scale Reservoir Characterization of the Devonian Sandstone, Donghe Formation, North Uplift of the Tarim Basin, Acta Geologica Sinica-English Edition 2018, 92(5), 1917-1933. [7] Wang, Z., Pan, M., Shi, Y., Liu, L., Xiong, F., Qin, Z., Fractal analysis of Donghetang sandstones using NMR measurements, Energy & Fuel 2018, 32, 2973- 2982. [6] Huang, H., Chen, L., Sun, W., Xiong, F., Ji, W., Jia, J., Tang, X., Zhang, S., Gao, J., Luo, B., Investigation of Pore Structure and Fractal Characteristics in the Shihezi Formation Tight Gas Sandstone from the Ordos Basin, China, Fractals 2018, 26, 1840005,1-22. [5] Bi, H., Jiang, Z.X., Li, J.Z., Xiong, F.Y., Li, P. Ono-kondo model for supercritical shale gas storage: A case study of Silurian Longmaxi shale in southeastern Chongqing, SW China, Energy & Fuels 2017, 31(3), 2755-2764. [4] Amooie, M.A., Soltanian, M.R., Xiong, F., Dai, Z., Moortgat, J., Mixing and spreading of multiphase fluids in heterogeneous bimodal porous media, Geomechanics and Geophysics for Geo-Energy and Geo-Resources 2017, 3, 1-20. ix [3] Soltanian, M.R., Amooie, M.A., Gershenzon, N., Dai, Z., Ritzi, R., Xiong, F., Cole, D.R., Moortgat, J., Dissolution trapping of carbon dioxide in heterogeneous aquifers. Environmental Sciences & Technology 2017, 51(13), 7732-7741. [2] Li, P., Jiang, Z.X., Zheng, M., Bi, H., Yuan, Y., Xiong, F.Y. Prediction model for gas adsorption capacity of the Lower Ganchaigou Formation in the Qaidam Basin, China. Journal of Natural Gas and Engineering 2016, 31, 493-502. [1] Tang, X.L., Jiang, Z.X., Huang, H.X., Jiang, S., Yang, L., Xiong, F.Y., Chen, L., Feng, J. Lithofacies characteristics and its effect on gas storage of the Silurian Longmaxi marine shale in the southeast Sichuan Basin, China. Journal of Natural Gas and Engineering 2016, 28, 338-346. Fields of Study Major Field: Earth Sciences/Geology
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