Paul C. Hackley Haolin Zhou Gelu Costin Justin E. Birdwell Daniel Minisini Tanguy Terlier Mark A. Torres 20240815 tabular digital data Reston, Virginia U.S. Geological Survey https://doi.org/10.5066/P1DU6KH4 Haolin Zhou Gelu Costin Justin E. Birdwell Paul C. Hackley Daniel Minisini Tanguy Terlier Mark A. Torres 20250515 publication Geostandards and Geoanalytical Research vol. 49, issue 3 n/a Wiley ppg. 591-605 https://doi.org/10.1111/ggr.12611 Conventional methods of assessing organic matter (OM) thermal maturity have limitations and often fail to reflect the geochemical heterogeneity between individual organic phases in mudstone samples. Vitrinite and solid bitumen reflectance, for example, is often measured to estimate OM thermal maturity but is restricted to specific types of OM. Alternative methods deserve exploration. This dataset provides the optical reflectance values that support a study investigating the application of fine-scale geochemical techniques to estimate OM thermal maturity. The study proposes a new analytical procedure using field emission-electron probe micro-analyzer (FE-EPMA). This instrument analyzes both the major elemental composition of the individual OM grains and the carbon X-ray spectrum. Past works suggest that the carbon X-ray spectrum may be sensitive to thermal maturity or OM types. To test this method, we analyzed a suite of mudstone samples with independent measurements of thermal maturity (i.e., vitrinite and solid bitumen reflectance) and compared a number of different spectral features. This data release provides the known vitrinite and solid bitumen optical reflectance values used in the analysis. The first data table contains the mean and standard deviation of multiple measurements taken from various samples reported in prior works (Birdwell and Wilson 2019, French et al. 2020, Zhou et al. 2022). The second data table is a collection of individual reflectance values, the maceral group and OM type from targeted spots for sample: Calumet Collier 34-5 13574 (Hackley et al. 2024). For the full study, refer to the larger work, "Using X-ray spectrum of carbon in electron micro-probe analysis to determine thermal maturity of organic matter in mudstones". The purpose of this dataset is to provide the supporting optical reflectance data for a study evaluating alternative methods of determining OM thermal maturity. 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 -140.0000 140.0000 60.0000 -60.0000 ISO 19115 Topic Category geoscientificInformation USGS Thesaurus Thermal maturation Optical methods None - Free Keywords Photoelectron spectroscopy Organic matter Reflectance Mudstone Liptinite Inertinite Solid bitumen USGS Metadata Identifier USGS:667d73b6d34ef010cb6d2139 Common Place Names New York Pennsylvania Alberta Oklahoma Texas Nebraska Ohio Wyoming Utah Colorado Florida 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 703-648-6419 phackley@usgs.gov ExxonMobil Technology and Engineering, Spring, TX USA, provided samples The attributes in the dataset are accepted as correct and accurate. Please refer to the detailed process steps for more information on measures and tests performed to ensure accuracy of values. The actual data matches up with the details provided. All values fall within expected ranges. Data has been checked for duplication/omission. Please refer to the detailed process steps for more information on tests performed to ensure logical consistency. This data set is considered complete for the information presented, as described in the abstract and the process step(s). Users are advised to read the rest of the metadata record carefully for additional details. No formal horizontal accuracy tests were performed. No formal vertical accuracy tests were performed. J. E. Birdwell S.A. Wilson 2019 publication https://pubs.usgs.gov/publication/70206010 Digital and/or Hardcopy 2019 publication date Birdwell and Wilson 2019 Known vitrinite or solid bitumen reflectance values K. L. French J. E. Birdwell M. D. Lewan 2020 tabular digital data https://pubs.usgs.gov/publication/70210389 Digital and/or Hardcopy 2020 publication date French et al. 2020 Known vitrinite or solid bitumen reflectance values H. Zhou N. B. Harris T. Dong K. Ayranci J. Feng B. Rivard J. Hatcherian 2022 tabular digital data https://pubs.geoscienceworld.org/gsa/gsabulletin/article-abstract/134/7-8/2130/610466/New-insights-into-organic-matter-accumulation-from Digital and/or Hardcopy 2022 publication date Zhou et al. 2022 Known vitrinite or solid bitumen reflectance values P. C. Hackley R. J. McAleer A. M. Jubb B. J. Valentine J. E. Birdwell 2024 tabular digital data https://pubs.usgs.gov/publication/70252645 Digital and/or Hardcopy 2024 publication date Hackley et al. 2024 Optical reflectance values for sample: Calumet Collier 34-5 13574' ASTM 2021 tabular digital data https://compass.astm.org/document/?contentCode=ASTM%7CD2797_D2797M-21A%7Cen-US Digital and/or Hardcopy 2021 publication date ASTM, 2021 Sample preparation technique Mudstone samples were analyzed from the Middle Devonian Marcellus, Middle-Late Devonian Horn River, Late Devonian Woodford, Middle Jurassic Lajas Formations, and Late Cretaceous formations: Boquillas, Mancos, Eagle Ford, and Niobrara using known vitrinite or solid bitumen reflectance values reported in prior works (Birdwell and Wilson 2019, French et al. 2020, Zhou et al. 2022). To investigate the relationship between geochemistry and optical reflectance in different types of macerals, samples were also analyzed from the Mesoproterozoic Xiamaling, Early Ordovician Alum, Devonian Ohio, Late Devonian to Early Mississippian Bakken, Late Jurassic Kimmeridge, Late Cretaceous Sunniland, and Eocene Green River Formations (Hackley et al. 2024). This study did not differentiate individual macerals; identifications of organic matter were made at the maceral group level only (i.e. liptinite, inertinite, etc.). Samples were prepared for petrographic analysis according to ASTM D2797 (ASTM, 2021) at the U.S. Geological Survey in Reston, Virginia, USA. All the samples were polished to 0.05 µm finish and mounted in epoxy resinpoly (methyl methacrylate) or copper with a 25 mm diameter. Samples were imaged under oil immersion on a Leica DM 4000 microscope with LED illumination and monochrome camera detection (QMS identity Hilgers1) in white and blue incident light. Mean random reflectance analyses of solid bitumen were conducted according to ASTM D7708 (ASTM, 2023) using the computer program ‘DISKUS-FOSSIL’ by Hilgers Technisches Buero with a YAG calibration standard (0.908 %Ro) manufactured by Klein and Becker. Birdwell and Wilson 2019 French et al. 2020 Zhou et al. 2022 Hackley et al. 2024 ASTM, 2021 2024 Table 1 Solid Bitumen and Vitrinite Mean Reflectance Values.csv Comma Separated Value (CSV) file containing data. Producer Defined Sample ID Sample identifier Producer Defined Sample identifier Ro The mean optical reflectance value of multiple measurements Producer Defined 0.18 3.84 percent reflectance Ro_std Optical reflectance value standard deviation Producer Defined nd NoData values are shown as nd, meaning "No Data". These legacy Ro values were obtained from a commercial laboratory prior to development of the ASTM D7708 reporting requirements, and did not include the associated standard deviation values or number of measurements. Producer defined 0.02 0.32 percent reflectance Maceral Group Maceral groups are classifications of organic particles found in coal and other sedimentary rocks Producer Defined Solid Bitumen Solid bitumen is a solid or semi-solid viscous petroleum phase which is observed petrographically and which has well defined optical and spectroscopic characteristics that allow it to be distinguished from other types of sedimentary organic matter. Producer defined Vitrinite Vitrinite is derived from woody plant material and is characterized by its bright appearance under a microscope and its high carbon content. Producer defined Reference/Source Source citation of the analysis Producer Defined Bob Ryder legacy data from Humble/Weatherford; shared by Dr. Hackley Bob Ryder legacy data from Humble/Weatherford; shared by Dr. Hackley Producer defined French et al. 2020 Full citation: French, K. L., Birdwell, J. E., & Lewan, M. D. (2020). Trends in thermal maturity indicators for the organic sulfur-rich Eagle Ford Shale. Marine and Petroleum Geology, 118, 104459 Producer defined Birdwell et al. 2019 Full citation: Birdwell, J. E., & Wilson, S. A. (2019, October). Variability in results from mineralogical and organic geochemical interlaboratory testing of US Geological Survey shale reference materials. In Unconventional Resources Technology Conference, Denver, Colorado, 22-24 July 2019 (pp. 2431-2449). Unconventional Resources Technology Conference (URTeC); Society of Exploration Geophysicists Producer defined measured by Dr. Hackley Measured values by Dr. Hackley in USGS laboratories, Reston, VA Producer defined Zhou et al. 2022 Zhou, H., Harris, N. B., Dong, T., Ayranci, K., Feng, J., Rivard, B., ... & Hatcherian, J. (2022). New insights into organic matter accumulation from high-resolution geochemical analysis of a black shale: Middle and Upper Devonian Horn River Group, Canada. GSA Bulletin, 134(7-8), 2130-2144 Producer defined Figure Corresponding figure in the supporting publication Producer Defined 2B, 2D, 2F, 2H, DR2B, DR2D, DR3B Data found in Figures 2B, 2D, 2F, 2H, DR2B, DR2D, DR3B Producer defined 2A, 2C, 2E, 2G, DR2A, DR2C, DR3A Data found in Figures 2A, 2C, 2E, 2G, DR2A, DR2C, DR3A Producer defined Table 2 Sample Calumet Collier 34-5 13574' Individual Reflectance Values.csv Comma Separated Value (CSV) file containing data. Producer Defined Maceral Group Maceral groups are classifications of organic particles found in coal and other sedimentary rocks Producer Defined Inertinite Inertinite consists of carbon-rich, unreactive material, often deriving from plant remains that have undergone oxidation or heat. Inertinite is usually indicative of higher ranks of coal and other thermal processes. Producer defined Liptinite Liptinite includes macerals derived from spores, cuticles, resins, and other organic remnants. Producer defined Solid bitumen Solid bitumen is a solid or semi-solid viscous petroleum phase which is observed petrographically and which has well defined optical and spectroscopic characteristics that allow it to be distinguished from other types of sedimentary organic matter. Producer defined Vitrinite Vitrinite is derived from woody plant material and is characterized by its bright appearance under a microscope and its high carbon content. Producer defined OM Type Organic matter type Producer Defined I-II This type is primarily derived from planktonic and algal material. It is rich in lipids and has a high hydrogen content. Producer defined II This type is primarily derived from higher plants and terrestrial sources. It has a moderate hydrogen content. Producer defined II-III This type represents a transitional phase between OM II and OM III, indicating a mix of both terrestrial and aquatic organic matter. Producer defined III This type is primarily derived from terrestrial plant material, particularly woody plants. It has a lower hydrogen content compared to OM I and II. Producer defined IV This type consists of highly decomposed organic matter, primarily from humic substances. It is characterized by very low hydrogen content. Producer defined Ro Value Individual optical reflectance value Producer Defined 0.04 1.23 percent reflectance This data release consists of two csv files containing reflectance data that supports the larger work publication: Using X-ray spectrum of carbon in electron microprobe analysis to determine thermal maturity of organic matter in mudstones. One csv file represents mean and standard deviation reflectance values plotted in Figure 2 (A-H) and Data Repositories 2 (A-D) and 3 (A-B). The data repositories 2B and 2D (DR2B and DR2D) are scatter plot figures representing quartile data. The table includes an attribute indicating which figure from the publication contains the reflectance values and an attribute referencing the value's source. The second csv file contains individual reflectance values from targeted spots for a single sample: Calumet Collier 34-5 13574' and these values are plotted in Figure 7 (B) of the publication. ASTM, 2023. D7708 Standard test method for microscopical determination of the reflectance of vitrinite dispersed in sedimentary rocks, Petroleum products, lubricants, and fossil fuels; Gaseous fuels; coal and coke, sec. 5, v. 05.06. ASTM International, West Conshohocken, PA. Birdwell, J. E., & Wilson, S. A. (2019, October). Variability in results from mineralogical and organic geochemical interlaboratory testing of US Geological Survey shale reference materials. In Unconventional Resources Technology Conference, Denver, Colorado, 22-24 July 2019 (pp. 2431-2449). Unconventional Resources Technology Conference (URTeC); Society of Exploration Geophysicists. French, K. L., Birdwell, J. E., & Lewan, M. D. (2020). Trends in thermal maturity indicators for the organic sulfur-rich Eagle Ford Shale. Marine and Petroleum Geology, 118, 104459. Hackley, P. C., McAleer, R. J., Jubb, A. M., Valentine, B. J., & Birdwell, J. E. (2024). Cathodoluminescence differentiates sedimentary organic matter types. Scientific Reports, 14(1), 5969. Zhou, H., Harris, N. B., Dong, T., Ayranci, K., Feng, J., Rivard, B., ... & Hatcherian, J. (2022). New insights into organic matter accumulation from high-resolution geochemical analysis of a black shale: Middle and Upper Devonian Horn River Group, Canada. GSA Bulletin, 134(7-8), 2130-2144. GS ScienceBase U.S. Geological Survey mailing address

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Denver CO 80225 United States 1-888-275-8747 sciencebase@usgs.gov Unless otherwise stated, all data, metadata and related materials are considered to satisfy the quality standards relative to the purpose for which the data were collected. Although these data and associated metadata have been reviewed for accuracy and completeness and approved for release by the U.S. Geological Survey (USGS), no warranty expressed or implied is made regarding the display or utility of the data for other purposes, nor on all computer systems, nor shall the act of distribution constitute any such warranty. Any use of trade, firm, or product names is for descriptive purposes only and does not imply endorsement by the U.S. Government. Digital Data https://doi.org/10.5066/P1DU6KH4 None 20260121 Jeremy K. Ray U.S. Geological Survey, Northeast Region Data Scientist mailing and physical

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