Paul C. Hackley 20250103 tabular digital data Reston, Virginia U.S. Geological Survey https://doi.org/10.5066/P1GWQU3S https://www.sciencebase.gov/catalog/item/66eaebe9d34e0606a9dba9dd Paul C. Hackley Justin E. Birdwell Ryan McAleer 20250601 tabular digital data Reston, Virginia U.S. Geological Survey Paul C. Hackley, Justin E. Birdwell, Ryan McAleer, Properties of solid bitumen formed during hydrous, anhydrous, and brine pyrolysis of oil shale: Implications for solid bitumen reflectance in source-rock reservoirs, Applied Geochemistry, Volume 185, 2025, 106365, ISSN 0883-2927, https://doi.org/10.1016/j.apgeochem.2025.106365. https://doi.org/10.1016/j.apgeochem.2025.106365 Solid bitumen is widely used as a thermal proxy in source-rock reservoirs, yet its texture and presentation may be affected by varying environmental constraints during its formation, e.g., water concentration, mineral catalysis, or salinity. Herein we investigated the development of solid bitumen properties during artificial maturation using three diverse (lacustrine to marine) oil shale samples containing abundant H-rich sedimentary organic matter (bituminite). Bituminite in the oil shales was treated via pyrolysis (320°C, 72 hrs) using hydrous, anhydrous, and brine conditions, causing the development of a newly formed solid bitumen in the experiment residues. The properties of the newly formed solid bitumen then were evaluated via geochemical screening tests, optical and electron microscopy, and infrared spectroscopy. Experimental residues also were treated via solvent extraction, allowing characterization of the effects of extraction to solid bitumen. Data from the experiments are provided here in 5 tables. Table 1 contains extract and fractionation data for untreated samples. Table 2 contains gas chromatography ratios. Table 3 contains reflectance and geochemical screening data. Table 4 contains gas yields for each sample under the various conditions. Table 5 contains Micro-Fourier transform infrared (micro-FTIR) data. For analysis findings, interpretations, and results, refer to the accompanying larger work publication, "Properties of solid bitumen formed during hydrous, anhydrous, and brine pyrolysis of oil shale: implications for solid bitumen reflectance in source-rock reservoirs". The purpose of this dataset is to make publicly available data accompanying the manuscript titled "Properties of solid bitumen formed during hydrous, anhydrous, and brine pyrolysis of oil shale: implications for solid bitumen reflectance in source-rock reservoirs." It comprises five tables detailing the experimental results related to the formation and properties of solid bitumen under different pyrolysis conditions. The file contains data available in comma separated value (.csv) file format. The user must have software capable of opening and viewing a .csv file. 2024 ground condition Complete None planned -109.5000 77.0000 55.0000 23.7000 ISO 19115 Topic Category geoscientificInformation USGS thermal maturation None - Free Keywords solid bitumen reflectance pyrolysis aromatization petroleum generation solvent extraction source-rock reservoir USGS Metadata Identifier USGS:66eaebe9d34e0606a9dba9dd Common Place Names Pakistan Colorado England None. Please see 'Distribution Info' for details. None. Users are advised to read the dataset's metadata thoroughly to understand appropriate use and data limitations. Paul C. Hackley U.S. Geological Survey, Northeast Region Research Geologist mailing and physical

Mail Stop 954, 12201 Sunrise Valley Dr

Reston VA 20192 US 703-648-6458 phackley@usgs.gov U.S. Geological Survey, Central Energy Resources Science Center, Lakewood CO 80225, USA; U.S. Geological Survey, Florence Bascom Geoscience Center, Reston VA 20192, USA No formal accuracy tests were conducted. Users are advised to read the metadata record carefully for additional details. Detailed process steps are provided for further information on methodology. Internal laboratory standards and procedural duplicates were employed for screening analyses according to the instrument manuals. Users are advised to read the metadata record carefully for additional details. Detailed process steps are provided for further information on methodology. Samples were collected from the Salt Range Formation in Pakistan, Kimmeridge Formation in England, and Green River Formation in western Colorado, USA. Dataset is considered complete for the information presented, as described in the abstract. Not all samples were tested by all methods. Users are advised to read the rest of the metadata record carefully for additional details. No formal positional accuracy tests were conducted. No formal positional accuracy tests were conducted. E.E. Bray E.D. Evans 1961 publication Geochimica et Cosmochimica Acta Volume 22, Issue 1 https://doi.org/10.1016/0016-7037(61)90069-2 Digital and/or Hardcopy 1961 publication date Bray and Evans, 1961 Carbon preference index (CPI) Richard A. Bourbonniere Philip A. Meyers 1996 publication Limnology and Oceanography Volume 41, Issue 2 https://doi.org/10.4319/lo.1996.41.2.0352 Digital and/or Hardcopy 1996 publication date Bourbonniere and Meyers, 1996 Terrestrial aquatic ratio (TAR) Paul C. Painter Randy W. Snyder Michael Starsinic Michael M. Coleman Deborah W. Kuehn Alan Davis 1981 publication Applied Spectroscopy Volume 35, Issue 5 https://doi.org/10.1366/0003702814732256 Digital and/or Hardcopy 1981 publication date Painter et al., 1981 Branching ratio Grzegorz P. Lis Maria Mastalerz Arndt Schimmelmann Michael D. Lewan B. Artur Stankiewicz 2005 publication Organic Geochemistry Volume 36, Issue 11 https://doi.org/10.1016/j.orggeochem.2005.07.001 Digital and/or Hardcopy 2005 publication date Lis et al., 2005 A-factor Paul C. Hackley Aaron M. Jubb Patrick L. Smith Ryan J. McAleer Brett J. Valentine Javin J. Hatcherian Palma J. Botterell Justin E. Birdwell 2022 publication International Journal of Coal Geology Volume 258 https://doi.org/10.1016/j.coal.2022.104016 Digital and/or Hardcopy 2022 publication date Hackley et al., 2022a Eocene Green River Formation Mahogany zone Paul C. Hackley Jolanta Kus João Graciano Mendonça Filho Andrew D. Czaja Angeles G. Borrego Dragana Životić Brett J. Valentine Javin J. Hatcherian 2022 publication International Journal of Coal Geology Volume 251 https://doi.org/10.1016/j.coal.2022.103927 Digital and/or Hardcopy 2022 publication date Hackley et al., 2022b Upper Jurassic Kimmeridge Clay Formation Paul C. Hackley Brett J. Valentine Ryan J. McAleer Javin J. Hatcherian J.L. Nedzweckas Bonnie McDevitt I. Khan 2024 publication Journal of Analytical and Applied Pyrolysis Digital and/or Hardcopy 2024 publication date Hackley et al., 2024a Neoproterozoic–Lower Cambrian Salt Range Formation Paul C. Hackley Michael Lewan 2018 publication AAPG Bulletin Volume 102 https://doi.org/10.1306/08291717097 Digital and/or Hardcopy 2018 publication date Hackley and Lewan, 2018 Pyrolysis experiments methods using closed system batch reactors made from SwageLok reactor components Paul C. Hackley Clint Scott Justin E. Birdwell Jennifer L. Nedzweckas Brett J. Valentine Tongwei Zhang Timothy O. Nesheim 2024 publication ACS Omega Volume 9, Issue 31 https://doi.org/10.1021/acsomega.4c04547 Digital and/or Hardcopy 2024 publication date Hackley et al., 2024b Extraction process Zachary K. Lowry 2020 publication Lakewood, Colorado U.S. Geological Survey U.S. Geological Survey web page https://doi.org/10.5066/P901N4FH Digital and/or Hardcopy 2020 publication date Lowry, 2020a Extraction and gas chromatography for Green River and Kimmeridge samples Paul C. Hackley Thomas M. Parris Cortland F. Eble Stephen F. Greb David C. Harris 2021 publication AAPG Bulletin Volume 105 https://doi.org/10.1306/08192019077 Digital and/or Hardcopy 2021 publication date Hackley et al., 2021 Extraction and gas chromatography for Salt Range Formation sample ASTM, International 2021 publication West Conshohocken, Pennsylvania ASTM, International Section 5: Petroleum products, lubricants, and fossil fuels Volume 05.06 Digital and/or Hardcopy 2021 publication date ASTM, 2021 Petrographic mount preparation Paul C. Hackley Tongwei Zhang Aaron M. Jubb Brett J. Valentine Frank T. Dulong Javin J. Hatcherian 2020 publication Marine and Petroleum Geology Volume 112 https://doi.org/10.1016/j.marpetgeo.2019.104086 Digital and/or Hardcopy 2020 publication date Hackley et al., 2020 Micro-Fourier transform infrared (micro-FTIR) spectroscopy Mark Dreier Augusta Warden 2021 publication Lakewood, Colorado U.S. Geological Survey, Central Energy Resources Science Center USGS Web Page https://doi.org/10.5066/P9HQSBGH Digital and/or Hardcopy 2021 publication date Dreier and Warden, 2021 Programmed temperature pyrolysis analysis Thomas Oliver Augusta Warden 2020 publication Lakewood, Colorado U.S. Geological Survey, Central Energy Resources Science Center USGS Web Page https://doi.org/10.5066/P9X85HUF Digital and/or Hardcopy 2020 publication date Oliver and Warden, 2020 Total Organic Carbon (TOC) analysis Zachary K. Lowry 2020 publication U.S. Geological Survey web page https://doi.org/10.5066/P93XH0ZW Digital and/or Hardcopy 2020 publication date Lowry, 2020b Extraction and gas chromatography for Salt Range Formation sample ASTM, International 2023 publication West Conshohocken, Pennsylvania ASTM, International Section 5: Petroleum products, lubricants, and fossil fuels Volume 05.06 https://www.astm.org/astm-bos-05.06.html Digital and/or Hardcopy 2023 publication date ASTM, 2023 Reflectance analyses Roger W. Marzi B. E. Torkelson R. K. Olson 1993 publication Organic Chemistry Volume10, Issue 8 https://doi.org/10.1016/0146-6380(93)90016-5 Digital and/or Hardcopy 1993 publication date Marzi et al., 1993 Carbon preference index formula H. H. Ganz Wolfgang D. Kalkreuth 1987 publication Fuel Volume 66, Issue 5 https://doi.org/10.1016/0016-2361(87)90285-7 Digital and/or Hardcopy 1987 publication date Ganz and Kalkreuth, 1987 A-Factor calculation Sample collection: Three immature, organic-rich oil shale samples were selected for pyrolysis experiments, during which they produce a newly formed solid bitumen from indigenous H-rich amorphous sedimentary organic matter. The samples, representing a range from lacustrine to marine environments, included: 1. Eocene Green River Formation Mahogany Zone (Hackley et al., 2022a), 2. Upper Jurassic Kimmeridge Clay Formation (Hackley et al., 2022b), and 3. Neoproterozoic–Lower Cambrian Salt Range Formation (Hackley et al., 2024a). The following process steps outline the pyrolysis experiments, as well as the subsequent extraction and fractionation, gas chromatography, petrographic analyses, and geochemical screening. Hackley et al., 2022a Hackley et al., 2022b Hackley et al., 2024a 2024 Pyrolysis experiments: Homogeneous 4- or 8- mesh sample splits were used for pyrolysis experiments in closed system batch reactors made from Swagelok reactor components following methods previously described (Hackley and Lewan, 2018). Pyrolysis experiments were conducted at the U.S. Geological Survey (USGS) in Reston (USGS-Reston). The Swagelok reactor system approach does not allow a full mass-balance documentation for pyrolysis experiments (gas is vented, liquid effluent is not typically collected), but it is rapid and efficient for the evaluation of experimental changes induced in the spent rock pyrolyzate. Hydrous experiments were conducted using distilled water whereas no water was added to the reactor for anhydrous experiments (Hackley, 2022a). A third set of experiments used a synthetic brine in place of water. Experiments with the Salt Range Formation sample used synthetic brine with total dissolved solids (TDS) of ~35.8 g/L consisting of 21.7 g/L Cl, 1.1 g/L SO4, 1.5 g/L Ca, 0.5 g/L K, 1.2 g/L Mg, and 9.8 g/L Na as determined via inductively coupled plasma-optical emission spectroscopy and ion chromatography following standard methods. Experiments with the Green River Formation Mahogany zone and Kimmeridge Clay Formation used synthetic brine with TDS of ~33.1 g/L consisting of 19.6 g/L Cl, 1.4 g/L SO4, 1.1 g/L Ca, 0.5 g/L K, 0.8 g/L Mg, and 9.8 g/L Na. All pyrolysis experiments were for 72-hr duration at 320°C. Rock residues were rinsed with acetone to remove external tarry bitumens and dried in a vacuum oven prior to crushing to ~18 mesh (1 mm) for petrographic analyses or grinding to fine powder with a mortar and pestle for geochemical screening. See additional process steps for further information. Hackley et al., 2022a Hackley and Lewan, 2018 2024 Extraction and gas chromatography: The untreated Kimmeridge and Green River samples were quantitatively extracted by standard Soxhlet methods and fractionated via column chromatography (Lowry, 2020a) at the USGS Petroleum Geochemistry Research Laboratory in Lakewood, Colorado (USGS-Lakewood). The untreated Salt Range Formation sample was extracted and fractionated at GeoMark Research, Ltd., also using Soxhlet and column chromatography. Following pyrolysis experiments, the ~18-mesh splits of the experimental residues were non-quantitatively extracted at USGS-Lakewood, using a chloroform rinse procedure via vortex and centrifuge (Hackley et al., 2024b). Bitumen was extracted by adding ~6 mL of chloroform to 0.5–1.0 g of crushed rock, vortexing, centrifuging for ~5 min, and decanting the supernatant. This rinsing procedure was repeated at least 3 times until the extract was clear. The atypical ~18-mesh split size used for extraction was to permit post-extraction petrographic analyses on the extracted residues. Extracts from pyrolysis residues were not fractionated. Chromatograms on the saturate fraction of the Green River sample and the whole extracts from all experimental residues and for the untreated Kimmeridge sample were determined using an Agilent 6890 or 8890 gas chromatograph with parameters described by Lowry (2020b) at USGS-Lakewood. The temperature program started at 40°C and increased at 4.5°C/min to 325°C where it was held for 20 minutes. The helium carrier gas flow rate was 2.5 mL/min and injection volume was 1 µL using a splitless injection mode with injection temperature 325°C. A chromatogram for the whole extract from the Salt Range Formation sample was determined at GeoMark Research, Ltd. using methods previously described (Hackley et al., 2021). Hackley et al., 2024b Lowry, 2020a Lowry, 2020b Hackley et al., 2021 2024 Petrographic analyses - optical microscopy, reflectance analyses and Micro-Fourier transform infrared (micro-FTIR) spectroscopy: Polished petrographic mounts for all samples were prepared to a final polish of 0.05 µm according to ASTM D2797 (ASTM, 2021) using a poly (methyl methacrylate) mounting medium at USGS-Reston. A Leica DM 4000 optical microscope equipped with LED illumination and monochrome camera detection was used to image the samples under oil immersion in white and blue incident light. The computer program DISKUS-FOSSIL by Hilgers Technisches Buero was used to perform reflectance analyses following ASTM D7708 (ASTM, 2023) with a yttrium-aluminum-garnet calibration standard (0.908% Ro). Micro-Fourier transform infrared (micro-FTIR) spectroscopy was performed on the polished sample mounts at USGS-Reston using a Bruker Hyperion 3000 FTIR microscope equipped with a liquid-N2 cooled mercury cadmium telluride (MCT) detector. The background was acquired on laboratory atmosphere using a 20× Ge attenuated total reflectance (Ge-ATR) objective with 0.6 numerical aperture (Hackley et al., 2020). Spectra were acquired from 600–6000 cm-1 with 100 co-added scans at a spectral resolution of 4 cm-1. Five to seven organic-rich rock fragments were measured for each sample and fit in the C-H stretching region (~2600–3200 cm-1) using five or six Lorentzian peaks and a cubic or linear baseline dependent on the sample. The organic-rich nature of the samples enabled untargeted micro-FTIR analysis with the Ge-ATR objective, i.e., data collection was from indigenous H-rich amorphous sedimentary organic matter in the untreated samples and from its solid bitumen thermal conversion product in the pyrolysis residues. No fitting parameters were fixed during any spectral deconvolution step. Deconvoluted peak intensities were used to calculate CH3/CH2 branching ratio (Painter et al., 1981) for all spectra and A-factor (Lis et al., 2005) for select spectra as permitted by fitting. Spectral parameters were averaged for each sample. ASTM, 2021 Hackley et al., 2020 ASTM, 2023 Painter et al., 1981 Lis et al., 2005 2024 Geochemical screening: All samples were analyzed for total organic carbon (TOC) content at USGS-Lakewood using a LECO C744 carbon analyzer following carbonate removal at room temperature with 6 mol/L HCl (Oliver and Warden, 2020). A Wildcat Technologies Hydrocarbon Analyzer with Kinetics (HAWK; Humble, TX) instrument was used for programmed temperature pyrolysis analysis of all samples following typical procedures (Dreier and Warden, 2021). Internal laboratory standards and procedural duplicates were employed for screening analyses according to the instrument manuals. Not all samples were tested by all methods. Dreier and Warden, 2021 Oliver and Warden, 2020 2024 Table 1 Extract and Fractionation.csv Comma Separated Value (CSV) file containing data. Producer Defined Sample ID Sample identifier Producer Defined A descriptive sample identifier that includes the sample origin, an alpha-numeric indentifier, and "untreated" indicating the sample was analyzed untreated. ERP ID Energy Resources Program identification number Producer Defined Identification number assigned by the U.S. Geological Survey Energy Resources Program EOM Extractable organic matter Producer Defined 22642 40405 parts per million Sat Saturated hydrocarbons as a normalized percentage of the whole extract Producer Defined 4.7 18.3 percent Arom Aromatic hydrocarbons as a normalized percentage of the whole extract Producer Defined 13.6 27.4 percent NSO Resins content in % Producer Defined 17.9 42.4 percent Asph Asphaltenes content in % Producer Defined 11.9 63.6 percent Sat/Arom Ratio of saturated hydrocarbons to aromatic hydrocarbons Producer Defined 0.34 0.86 ratio Table 2 Gas Chromatography.csv Comma Separated Value (CSV) file containing data. Producer Defined Sample ID Sample identifier Producer Defined A descriptive sample identifier that includes the following: For samples that were untreated, the Sample ID includes the sample origin, an alpha-numeric identifier, and "untreated" indicating the sample was analyzed untreated. For samples that were extracted, the Sample ID includes "ext" indicating extract, an alpha-numeric identifier, and the extraction treatment conditions (temperature, duration, and whether extraction was hydrous, anhydrous or brine). ERP ID Energy Resources Program identification number Producer Defined Identification number assigned by the U.S. Geological Survey Energy Resources Program Pr/Ph Ratio of pristane to phytane; ratios are on whole extracts for all samples except sample APM, untreated, where data are from the saturate fraction. All ratios based on peak heights. Producer Defined 0.37 1.71 ratio Pr/n-C17 Isoprenoid ratio - pristane to 17C normal alkane; ratios are on whole extracts for all samples except untreated APM and untreated KC-1, where data are from the saturate fraction. All ratios based on peak heights. Producer Defined 0.44 2.63 ratio Ph/n-C18 Isoprenoid ratio - phytane to 18C normal alkane; ratios are on whole extracts for all samples except untreated APM and untreated KC-1, where data are from the saturate fraction. All ratios based on peak heights. Producer Defined 0.26 18.87 ratio CPI Carbon preference index using n-C23 to n-C29 (Marzi et al., 1993); an asterisk (*) indicates the use of n-C25 to n-C34 (Bray and Evans, 1961). The Bray and Evans (1961) formula ratio is noted as CPI02 in the USGS Energy Database; the Marzi et al. (1993) formula is noted as CPI04 in the USGS Energy Database. Ratios are on whole extracts for all samples except untreated APM and untreated KC-1, where data are from the saturate fraction. All ratios based on peak heights. Producer Defined 1.10 2.78 TAR Terrestrial aquatic ratio [Bourbonniere and Meyers, 1996: (n-C27+n-C29+n-C31)/(n-C15+n-C17+n-C19)] ; an asterisk (*) indicates the use of n-C27/n-C17; ratios are on whole extracts for all samples except untreated APM and untreated KC-1, where data are from the saturate fraction. All ratios based on peak heights. Producer Defined 0.09 2.39 ratio Table 3 Reflectance and Geochemical.csv Comma Separated Value (CSV) file containing data. Producer Defined Sample ID Sample identifier Producer Defined A descriptive sample identifier that includes the following: For samples that were untreated, the Sample Id includes the sample origin, an alpha-numeric identifier, and "untreated" indicating the sample was analyzed untreated. For samples that were extracted, the Sample ID includes "ext" indicating extract, the alpha-numeric identifier, and the extraction treatment conditions (temperature, duration, and whether extraction was hydrous, anhydrous or brine). ERP ID Energy Resources Program identification number Producer Defined Identification number assigned by the U.S. Geological Survey Energy Resources Program BRo Reflectance values of amorphous organic matter (in untreated samples) and solid bitumen thermal conversion product in the pyrolysis residues Producer Defined 0.06 0.91 percent s.d. Standard deviation of BRo Producer Defined 0.01 0.1 standard deviation no. Number of BRo measurements Producer Defined 30 65 count TOC Total organic carbon in wt % Producer Defined 7.6 46.39 weight percent S1 Thermal distillate in milligrams hydrocarbon per gram rock Producer Defined 0.23 77.93 milligrams hydrocarbon per gram rock S2 Pyrolyzate in milligrams hydrocarbon per gram rock Producer Defined 47.58 330.04 milligrams hydrocarbon per gram rock S3 CO2 peak in milligrams CO2 per gram rock Producer Defined 0.47 3.72 milligrams carbon dioxide per gram rock Tmax Temperature of S2 peak in °C Producer Defined 409 447 degrees Celsius HI Hydrogen index, as defined by the equation S2/TOC*100 in milligrams hydrocarbon per gram TOC Producer Defined 222 924 milligrams hydrocarbon per gram TOC OI Oxygen index, as defined by the equation S3/TOC*100 in milligrams CO2 per gram TOC Producer Defined 1 13 milligrams carbon dioxide per gram TOC PI Production index as defined by the equation S1/(S1+S2) Producer Defined 0.0 0.29 unitless Table 4 Gas Yields.csv Comma Separated Value (CSV) file containing data. Producer Defined Sample ID Sample identifier Producer Defined A descriptive sample identifier that includes the following: For samples that were untreated, the Sample ID includes the sample origin, an alpha-numeric identifier, and "untreated" indicating the sample was analyzed untreated. For samples that were extracted, the Sample ID includes "ext" indicating extract, the alpha-numeric identifier, and the extraction treatment conditions (temperature, duration, and whether extraction was hydrous, anhydrous or brine). ERP ID Energy Resources Proogram identification number Producer Defined Identification number assigned by the U.S. Geological Survey Energy Resources Program Rock (g) Rock content of sample in grams Producer Defined 2.84 4.63 grams Gas (g) Gas content of sample in grams Producer Defined 0.03 0.37 grams Gas Yield (mg/g) Gas yield of sample in milligrams per gram of rock Producer Defined 10.56 87.89 milligrams per grams Table 5 Micro-FTIR.csv Comma Separated Value (CSV) file containing data. Producer Defined Sample ID Sample identifier Producer Defined A descriptive sample identifier that includes the following: For samples that were untreated, the Sample ID includes the sample origin, an alpha-numeric identifier, and "untreated" indicating the sample was analyzed untreated. For samples that were extracted, the Sample ID includes "ext" indicating extract, the alpha-numeric identifier, and the extraction treatment conditions (temperature, duration, and whether extraction was hydrous, anhydrous or brine). ERP ID Energy Resources Program identification number Producer Defined Identification number assigned by the U.S. Geological Survey Energy Resources Program CH3/CH2 Ratio of methyl groups to methylene groups known as the inverse branching ratio (Painter et al., 1981) Producer Defined 0.21 0.69 ratio CH3/CH2_s.d. Inverse branching ratio standard deviation Producer Defined 0.01 0.27 standard deviation CH3/CH2_no. Branching ratio number of measurements Producer Defined 2 7 count A-factor A-factor is a specific factor used to represent the relationship between temperature and the rate of chemical processes such as the maturation of organic matter as defined in Ganz and Kalkreuth (1987) Producer Defined n.d. no data Producer Defined 0.93 0.99 unitless A-factor_s.d. A-factor standard deviation Producer Defined n.d. no data Producer Defined 0.01 .07 standard deviation A-factor_no. A-factor number of measurements Producer Defined n.d. no data Producer Defined 2 7 count GS ScienceBase U.S. Geological Survey mailing address

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