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I NANO-PETROPHYSICAL CHARACTERIZATION of the OIL NANO-PETROPHYSICAL CHARACTERIZATION OF THE OIL WINDOW OF EAGLE FORD SHALE FROM SOUTHWESTERN TO CENTRAL TEXAS, U.S.A. by CHAD LARSEN Presented to the Faculty of the Graduate School of The University of Texas at Arlington in Partial Fulfillment of the Requirements for the Degree of MASTER OF SCIENCE IN EARTH AND ENVIRONMENTAL SCIENCES THE UNIVERSITY OF TEXAS AT ARLINGTON August 2020 i Copyright © by Chad Larsen 2020 All Rights Reserved ii Acknowledgements I would like to personally thank and acknowledge my thesis advisor, Dr. Qinhong Hu, along with my thesis committee of Dr. John Wickham, Dr. Arne Winguth, and Dr. Andrew Hunt. This opportunity was made possible through their support and assistance, along with the assistance of the administrative staff of the Earth and Environmental Science Department. I would like to thank The Bureau of Economic Geology at the University of Texas at Austin, specifically Dr. Steve Ruppel (in memoriam), Nathan Ivicic, Brandon Williamson, which provided the cores to select from; their colleague(s) who supplied me the well logs and the individual(s) who cut and shipped the samples. I want to thank the following members of Dr. Hu’s research group who trained me on the procedures plus their willingness to answer a multitude of questions, they are: Qiming Wang, Shawn Zhang, Ryan Jones, and Sam Becker. I would also like to thank several industry professionals who always found time to offer guidance (not limited to): Anthony Smallwood, Hugh Peace, Christy Glatz, Mark Varhaug, David Tucker, Ron Clark, Jamie Sher, and Jon Ross. Finally, I need to thank my family of friends, for their constant words of encouragement and support: Richard Bell, Jennifer and Eric Davis; Ben Fabian, Susanne Hilou, Rob Whitt and family; Evangeline Smallwood and family; Dr. Nancy Shosid and family; Leah Thorvilson, Michael Harmon, Melanie Baden, Brenda Kay Burg, Dr. Melanie Marketon and family; Dr. Britnee Crawford, Kay Hale, Tanya Lauer, Lucy and Rick Evans; Dr. Puloma Chakrabarty, Mark Hurley, Kimberly Fyffe, Derrick Shimcek and family; Jill Rochelle, Addy and Rachel Buigas; Patti Monzingo, Keisha Ragoobir and Family; Jojo Harmel and many more. Thank you. iii Abstract NANO-PETROPHYSICAL CHARACTERIZATION OF THE OIL WINDOW OF EAGLE FORD SHALE FROM SOUTHWESTERN TEXAS, U.S.A. Chad Larsen, MS The University of Texas at Arlington, 2020 Supervising Professor: Qinhong Hu Eagle Ford Shale and the overlying Austin Chalk are the main producing plays throughout Central Texas. Due to the high clastic nature of Eagle Ford Shale and its ability to produce and maintain fractures from hydraulic fracturing, this formation quickly became the favored target over Austin Chalk for unconventional hydrocarbon production. The purpose of this study is to gain an understanding of nano-petrophysical properties of Eagle Ford Shale, which is still lacking. Drilling cores from three wells within the oil window of Eagle Ford Shale were examined at the Bureau of Economic Geology in Austin, TX. Multiple plug samples were taken of three wells and analyzed using various tests of XRD, pyrolysis, TOC, mercury intrusion porosimetry (MIP), pycnometry, (DI water and n-decane) vacuum saturation, low-pressure nitrogen gas physisorption, and fluid (DI water and n-decane) imbibition. These experiments will shed light on the nano-petrophysical properties of the reservoir regarding porosity, pore throat distribution, permeability, and flow patterns. MIP results from this study show that Eagle Ford Shale has a wide range of pore structure parameters with porosity values varying from 0.11 to 7.25% and permeability from 0.005 to 11.6 iv mD; all samples are dominated by two pore types: micro fractures (1-50 µm) and inter-granular (0.01-1 uµ) pores. TOC % showed an increase when quartz % increased as minerology has a direct influence on TOC %. Bulk density averages 2.54% while the grain density is slightly increased with an average of 2.64%. Kerogen values plot between group II and III indicating a hydrocarbon potential. Based on the nano-petrophysical analysis of Eagle Ford Shale, the results of this thesis are beneficial to further the understanding of the pore structure and fluid migration within the shale, and to better facilitate increased production. v Table of Contents Acknowledgements ........................................................................................................................ iii Abstract .......................................................................................................................................... iv List of Illustrations ...................................................................................................................... viii List of Tables ...................................................................................................................................x List of Equations ............................................................................................................................ xi Chapter 1 Introduction .....................................................................................................................1 Chapter 2 Geologic Setting and Depositional Environment ...........................................................6 2-1 Well Log Interpretation .............................................................................................11 Chapter 3 Methods .........................................................................................................................16 3-1 Acquisition of Samples ................................................................................................16 3-2 X-Ray Powder Diffraction (XRD) ..............................................................................28 3-3 Total Organic Carbon (TOC) ......................................................................................29 3-3 Pyrolysis ......................................................................................................................29 3-4 Fluid Immersion Porosimetry (FIP) after Vacuum Saturation ....................................30 3-5 Mercury Intrusion Porosimetry (MIP) .........................................................................31 3-6 Contact Angle ..............................................................................................................34 3-7 Spontaneous Imbibition ...............................................................................................36 3-8 Liquid Pycnometry ......................................................................................................38 3-9 Low Pressure Nitrogen Gas Physisorption ..................................................................40 Chapter 4 Results ...........................................................................................................................40 4-1 X-Ray Powder Diffraction (XRD) ..............................................................................41 4-2 Total Organic Carbon (TOC) ......................................................................................46 4-3 Pyrolysis .....................................................................................................................46 4-4 Vacuum Saturation .....................................................................................................50 4-5 Contact Angle and Wettability ...................................................................................55 4-6 Liquid Pycnometry ......................................................................................................57 4-7 Spontaneous Imbibition ..............................................................................................59 4-8 Low-Pressure Nitrogen Gas Physisorption .................................................................61 vi Chapter 5 Discussion .....................................................................................................................65 5-1 Mineralogy and Geochemistry ....................................................................................65 5-2 Porosity Results from Different Approaches...............................................................68 5-3 Pore Structure Parameters ..........................................................................................72 5-4 Pore Connectivity and Wettability .............................................................................73 5-5 Density ........................................................................................................................73 Chapter 6 Conclusion and Recommendations ...............................................................................76 6-1 Conclusions ................................................................................................................76 6-2 Recommendations ......................................................................................................79 References ......................................................................................................................................81 Appendix A Laboratory Methods at Shimadzu Institute for Research Technologies ...................84 Appendix B Laboratory Methods at GeoMark Research, LLC .....................................................88 vii List of Illustrations Figure 1-1 Location of Eagle Ford Shale and Surrounding Reservoirs ..........................................2 Figure 1-2 Oil, Condensate, and Dry Gas Divisions ......................................................................3
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