Alisa Shtabnoy Aaron M. Jubb Paul C. Hackley Ryan J. McAleer Jing Qu 20250325 tabular digital data Reston, VA U.S. Geological Survey https://doi.org/10.5066/P13EDR3S Aaron M. Jubb Paul C. Hackley Ryan J. McAleer Jing Qu 202506 publication Organic Geochemistry vol. 204 n/a Elsevier BV ppg. 104990 https://doi.org/10.1016/j.orggeochem.2025.104990 This data release describes optical photothermal infrared (OPTIR) spectroscopy data used to map sedimentary organic matter functional group distributions at 500 nm resolution in a sample from the Lower Cretaceous Sunniland Limestone from the South Florida Basin. Examined fields of view include occurrences of amorphous organic matter (AOM), inertinite, micrinite, solid bitumen, telalginite, and vitrinite. Data also include traditional organic petrographic data from the same organic grains including fluorescence intensity, reflectance, and scanning electron microscopy as well as against cathodoluminescence response. Data were collected to characterize sedimentary organic matter of the Lower Cretaceous Sunniland Limestone through use of optical photothermal infrared (OTPIR) spectroscopy and comparison against traditional organic petrographic data. 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. 20220822 observed Complete None planned -81.3041 -81.3041 26.2592 26.2592 ISO 19115 Topic Category geoscientificInformation None - Free Keywords Optical photothermal infrared spectroscopy organic matter oxygen-content solid bitumen telalginite vitrinite Limestone Sedimentary organic matter USGS Metadata Identifier USGS:678fc4fdd34e28977994cfae Common geographic areas Florida Collier County South Florida Basin Geolex, https://ngmdb.usgs.gov/Geolex/search Sunniland Limestone 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. Aaron M Jubb U.S. Geological Survey, Northeast Region Research Chemist mailing and physical

12201 Sunrise Valley Drive, Reston, VA, 20192

Reston VA 20192 United States 703-648-6481 ajubb@usgs.gov No formal attribute accuracy tests were conducted. No formal logical accuracy tests were conducted. Data set is considered complete for the information presented, as described in the abstract. 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. Tina L. Roberts-Ashby Paul C. Hackley Celeste D. Lohr Christopher J. Schenk Tracey J. Mercier Katherine J. Whidden Phuong A. Le Marilyn E. Tennyson Stephanie B. Gaswirth Cheryl A. Woodall Michael E. Brownfield Heidi M. Leathers-Miller Kristen R. Marra Thomas M. Finn 2019 publication n/a US Geological Survey https://doi.org/10.3133/fs20183074 Digital and/or Hardcopy 20190201 publication date Roberts-Ashby et al., 2018 USGS Publication Warehouse Paul C. Hackley Ryan J. McAleer Aaron M. Jubb Brett J. Valentine Justin E. Birdwell 20240312 publication Scientific Reports vol. 14, issue 1 n/a Springer Science and Business Media LLC https://doi.org/10.1038/s41598-024-53168-z Digital and/or Hardcopy 20240312 publication date Hackley et al., 2024 Scientific Reports ASTM 2011 publication ASTM D2797 https://doi.org/10.1520/D2797 Digital and/or Hardcopy 2011 publication date ASTM, 2011 ASTM International ASTM 20140528 publication ASTM D7708-11 https://doi.org/10.1520/D7708-11 Digital and/or Hardcopy 20140528 publication date ASTM, 2014 ASTM International Daimay Lin-Vien Norman B. Colthup William G. Fateley Jeanette G. Grasselli 1991 publication Digital and/or Hardcopy 1991 publication date Lin-Vien et al., 1991 Academic Press, Inc. The Lower Cretaceous Sunniland Limestone source rock sample evaluated here was collected in 2014 from the core repository of the Florida Geological Survey (FGS) (sample ID Calumet 34-5 Collier 13574’) in support of petroleum resource assessment in the South Florida Basin (Roberts-Ashby et al., 2018). The 13574’ depth is the measured depth of sample collection in a directional workover and true vertical depth is 11558’, according to well log records available from the FGS and IHS. The well is in Collier County in the Bear Island field (API 09021201280000, surface latitude 26.25918, longitude -81.3041). Roberts-Ashby et al., 2018 2014 Complete details on sample preparation and white light, fluorescence, and electron microscopic analyses are provided in (Hackley et al., 2024). Briefly, the sample was crushed (to ~1 mm) and homogenized prior to preparation into petrographic briquettes via ASTM D2797 (ASTM, 2011) with a final polish of 0.05 um. Hackley et al., 2024 ASTM, 2011 2024 White light and fluorescence images and maceral reflectance (Ro) values were collected under oil immersion with a Leica DM 4000 microscope using LED illumination and a 50x (0.85 NA) objective. Fluorescence was excited with a 455 nm LED and signal was detected using a 482 nm beam splitter and a 510 nm longpass filter. Individual maceral Ro values were collected via a modification to ASTM D7708 (ASTM, 2014) with the DISKUS-FOSSIL program (Hilgers Technisches Buero) using a yttrium-aluminum-garnet calibration standard (0.908% Ro, Klein&Becker). Scanning electron microscopy (SEM) and CL imaging were performed using a Hitachi SU-5000 field emission scanning electron microscope and Delmic SPARC modular CL detector, respectively, following the sample being coated with ~10 nm of carbon with a Leica ACE600. CL images were collected using 10 keV, ~1.5 nA beam current, and 300 us dwell time. White light, fluorescence, reflectance analyses, SEM, and CL imaging were all carried out at the U.S. Geological Survey (USGS) laboratories in Reston, Virginia, USA. ASTM, 2014 2024 OPTIR mapping was carried out using a mIRage instrument (Photothermal Inc.) in the Advanced Materials Characterization Laboratory at the University of Delaware (https://amcl.udel.edu). Tunable infrared light in the mIRage instrument was generated using a quantum cascade laser (QCL) with a 10 ns pulse width, a 120 kHz repetition rate, and was operated at 20% power output. The input probe was a 532 nm continuous wave laser operated at 0.2% power. OPTIR maps were collected across the field of view at 1716 cm-1, 1600 cm-1, and 1458 cm-1 corresponding to carbonyl (C=O) stretching, sp2 hybridized carbon-carbon bond (C=C) stretching, and methylene (CH2) scissoring modes, respectively (Lin-Vien et al., 1991). The spatial resolution of the mIRage instrument is ~500 nm and OPTIR maps were collected with 500 nm steps in the x- and y-directions, yielding near continuous compositional maps of the sample surface. The sample was analyzed in order 1) white light and fluorescence imaging, 2) OPTIR, and then 3) SEM and CL to avoid issues with sample damage from the electron beam and the necessity to carbon coat the sample for SEM and CL analysis. Lin-Vien et al., 1991 2024 Image analysis to extract maceral specific fluorescence, CL, and OPTIR intensities were conducted in IgorPro 9 software suite using a built-in image analysis routine. In this routine, a region of interest (ROI) was defined by drawing a polygon around a specific maceral and then extracting the relevant intensity values from the ROI (i.e., red-green-blue intensity for fluorescence and CL images and mV for OPTIR maps). For fluorescence and CL images, “integrated intensity” represents the sum of the intensities in the red, green, and blue channels. 2024 Table1.csv Maceral specific mean OPTIR spectroscopy carbonyl (C=O) signal at 1716 cm-1, mean fluorescence, mean cathodoluminescence (CL), and reflectance (Ro) values. Standard deviations given at the 1-sigma level. OPTIR = optical photothermal infrared. n corresponds to the= number of OPTIR datapoints represented by mean value. aom = amorphous organic matter. mic = micrinite. iner = inertinite. sb = solid bitumen. tel = telalginite. vit = vitrinite. arb = arbitrary. Maceral locations are provided in Figure 1H (Jubb et al., 2025). Producer Defined Maceral Identifier for individual maceral polygons. Enumerated categorically by organic matter type. Producer Defined aom = amorphous organic matter numbered 1 through 4. iner = inertinite numbered 1 through 2. sb = solid bitumen numbered 1 through 10. tel = telalginite numbered 1 through 7. vit = vitrinite numbered 1 through 3. mic = micrinite. C=O (mV) Maceral specific mean OPTIR carbonyl (C=O) signal at 1716 cm-1. Producer Defined 153 1310 mV C=O stdev (mV) Standard deviation (1-sigma level) of maceral specific mean OPTIR carbonyl (C=O) signal at 1716 cm-1. Producer Defined 74 385 mV n Number of OPTIR datapoints represented by mean value. Producer Defined 307 8147 counts Fluorescence (arb.) Mean fluorescence. Producer Defined 139 486 arbitrary Fluorescence stdev (arb.) Standard deviation (1-sigma level) of mean fluorescence. Producer Defined 3 59 arbitrary CL (arb.) Mean cathodoluminescence. Producer Defined 21 337 arbitrary CL stdev (arb.) Standard deviation (1-sigma level) of mean cathodoluminescence. Producer Defined 13 79 arbitrary Ro (%) Reflectance. Producer Defined - No data Producer defined 0.08 1.03 % Figure2.csv OPTIR detector response at three mapped frequencies (1716 cm-1 corresponding to C=O stretching modes, 1600 cm-1 corresponding to C=C stretching modes, and 1458 cm-1 corresponding to CH2 scissoring modes and the shoulder of the CO3 stretching mode) for individual data points of each maceral type. AOM = amorphous organic matter; CO3 = carbonate. Producer Defined AOM C=O (mV) Response at 1716 cm-1 corresponding to C=O stretching modes for amorphous organic matter maceral data points. Producer Defined - No Data Producer defined 1.6 915.2 mV AOM C=C (mV) Response at 1600 cm-1 corresponding to C=C stretching modes for amorphous organic matter maceral data points. Producer Defined - No Data Producer defined 4.1 922.4 mV AOM CH2 (mV) Response at 1458 cm-1 corresponding to CH2 scissoring modes and the shoulder of the CO3 stretching mode for amorphous organic matter maceral data points. Producer Defined - No Data Producer defined 9.5 4962.4 mV Inertinite C=O (mV) Response at 1716 cm-1 corresponding to C=O stretching modes for inertinite maceral data points. Producer Defined - No Data Producer defined 15.9 717.5 mV Inertinite C=C (mV) Response at 1600 cm-1 corresponding to C=C stretching modes for inertinite maceral data points. Producer Defined - No Data Producer defined 30.6 1127.1 mV Inertinite CH2 (mV) Response at 1458 cm-1 corresponding to CH2 scissoring modes and the shoulder of the CO3 stretching mode for inertinite maceral data points. Producer Defined - No Data Producer defined 330.4 2388.7 mV Micrinite C=O (mV) Response at 1716 cm-1 corresponding to C=O stretching modes for micrinite maceral data points. Producer Defined - No Data Producer defined 120.8 992.3 mV Micrinite C=C (mV) Response at 1600 cm-1 corresponding to C=C stretching modes for micrinite maceral data points. Producer Defined - No Data Producer defined 6.2 905.8 mV Micrinite CH2 (mV) Response at 1458 cm-1 corresponding to CH2 scissoring modes and the shoulder of the CO3 stretching mode for micrinite maceral data points. Producer Defined - No Data Producer defined 326.4 4604.7 mV Solid Bitumen C=O (mV) Response at 1716 cm-1 corresponding to C=O stretching modes for solid bitumen maceral data points. Producer Defined - No Data Producer defined 149.9 1107.4 mV Solid Bitumen C=C (mV) Response at 1600 cm-1 corresponding to C=C stretching modes for solid bitumen maceral data points. Producer Defined - No Data Producer defined 2.5 1447.4 mV Solid Bitumen CH2 (mV) Response at 1458 cm-1 corresponding to CH2 scissoring modes and the shoulder of the CO3 stretching mode for solid bitumen maceral data points. Producer Defined - No Data Producer defined 2.2 4407.5 mV Telalginite C=O (mV) Response at 1716 cm-1 corresponding to C=O stretching modes for telalginite maceral data points. Producer Defined - No Data Producer defined 212.4 2371.6 mV Telalginite C=C (mV) Response at 1600 cm-1 corresponding to C=C stretching modes for telalginite maceral data points. Producer Defined - No Data Producer defined 4.2 1175.1 mV Telalginite CH2 (mV) Response at 1458 cm-1 corresponding to CH2 scissoring modes and the shoulder of the CO3 stretching mode for telalginite maceral data points. Producer Defined - No Data Producer defined 13.6 5015.5 mV Vitrinite C=O (mV) Response at 1716 cm-1 corresponding to C=O stretching modes for vitrinite maceral data points. Producer Defined - No Data Producer defined 15.4 1206.4 mV Vitrinite C=C (mV) Response at 1600 cm-1 corresponding to C=C stretching modes for vitrinite maceral data points. Producer Defined - No Data Producer defined 4.7 1068.4 mV Vitrinite CH2 (mV) Response at 1458 cm-1 corresponding to CH2 scissoring modes and the shoulder of the CO3 stretching mode for vitrinite maceral data points. Producer Defined - No Data Producer defined 2.7 3189.4 mV U.S. Geological Survey - ScienceBase 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/P13EDR3S None 20251203 Alisa Shtabnoy U.S. Geological Survey, Northeast Region Physical Scientist mailing and physical

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Reston VA 20192 United States 443-498-5500 ashtabnoy@usgs.gov FGDC Content Standard for Digital Geospatial Metadata FGDC-STD-001-1998