Mishra, Divya K. Hackley, Paul C. Jubb, Aaron M. Sanders, Margaret M. Agrawal, Shailesh Varma, Atul K. 20220411 Tabular Reston, VA U.S. Geological Survey https://doi.org/10.5066/P9KNB6GP This study evaluated carbonaceous shales proximal to coal measures and coal samples via isothermal hydrous pyrolysis (HP) to compare differences in the maturation pathways of vitrinite in different matrices and with different starting aromaticity. Sample residues were analysed via vitrinite reflectance (VRo), geochemical screening tests (organic carbon and programmed temperature pyrolysis), and infrared spectroscopy. The study included samples from Indian and North American basins, to observe differences in vitrinite evolution with respect to enclosing mineral matrix, starting degree of aromaticity, organic matter types, stratigraphic age, and depositional environment. Tmax, production index (PI), and VRo show intuitive increasing values with respect to HP temperature. The least mature sample (0.48 ± 0.05% VRo) generally experienced the maximum change in these parameters during maturation, whereas the most mature sample (0.99 ± 26 0.06% VRo) generally showed the least change. This observation is consistent with higher kinetic barriers to reaction in more aromatic vitrinite which contains higher bond disassociation energies. Data were collected in order to evaluate carbonaceous shales proximal to coal measures and coal samples via isothermal hydrous pyrolysis (HP) to compare differences in the maturation pathways of vitrinite in different matrices and with different starting aromaticity. 2022 publication date Complete None planned -104.4141 95.976599999996 38.6855 3.6889 USGS Thesaurus Hydrous pyrolysis Reflectance TOC FTIR USGS Metadata Identifier USGS:6228cbfdd34ee0c6b38b87b2 Getty Thesaurus of Geographic Names (http://www.getty.edu/research/tools/vocabularies/tgn/index.html) Louisiana Illinois Alabama Jharkhand State, India Geolex https://ngmdb.usgs.gov/Geolex/search Wilcox Group Carbondale Formation Illinois Basin Pottsville Formation Barakar Formation USGS Thesaurus: Time Periods Palaeozoic Era Paleocene-Eocene Epoch Permian Period none none Paul C. Hackley NORTHEAST REGION: GEOLOGY, ENERGY&MINERALS SC Research Geologist mailing and physical

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Reston VA 20192 US 703-648-6458 phackley@usgs.gov Hackley, Paul Lewan, Michael 2018 Tulsa, OK AAPG Bulletin https://doi.org/10.1306/08291717097 Hackley, Paul Araujo, Carla Borrego, Angeles Bouzinos, Antonios Cardott, Brian Cook, Alan Eble, Cortland Flores, Deolinda Gentzis, Thomas Gonçalves, Paula Mendonça Filho, João Jelonek, Iwona Kommeren, Kees Knowles, Wayne Kus, Jolanta Mastalerz, Maria Menezes, Taíssa Newman, Jane Valentine, Brett 2015 Amsterdam, Netherlands Marine and Petroleum Geology https://doi.org/10.1016/j.marpetgeo.2014.07.015 Varma, Atul Mishra, Divya Samad, Suresh Prasad, Amal Panigrahi, Durga Mendhe, Vinod Singh, Bhagwan 2018 Amsterdam, Netherlands International Journal of Coal Geology https://doi.org/10.1016/j.coal.2017.12.002 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 Coals and carbonaceous shales samples used in this study were from formations of different age, lithology, and basin of deposition. Coal sample 4-LA-10 is from the Paleocene-Eocene Wilcox Group of Caldwell Parish, northern Louisiana, in the passive margin Gulf of Mexico Basin. Coal of northern Louisiana ranks from lignite to subbituminous C (Hackley et al., 2007; Warwick et al., 2008) and vitrinite in this sample has a measured VRo value of 0.48 ± 0.05% (Hackley and Cardott, 2020). Sample IL-08-01 is a subbituminous coal sample from the Palaeozoic (Desmoinesian) Carbondale Formation, from the Herrin coal bed in the cratonic interior Illinois Basin. Sample IL-08-1 has a measured VRo value of 0.54 ± 0.03% (Hackley and Lewan, 2018). Sample JWR-868-3 is a carbonaceous shale collected from Pennsylvanian coal measures in the Pottsville Formation of the foreland Appalachian Basin, Alabama. Vitrinite in this sample is of higher thermal maturity with a reported average VRo of 0.99 ± 0.06% (Hackley et al., 2015) consistent with reported bituminous rank of Pottsville Formation coals (Hatch and Pawlewicz, 2007). The three other carbonaceous shale samples (CG1304, CG1311, CG1530) used in this study were from the Auranga coalfield, India. The samples were from the lower Permian (Sakmarian Kungurian) Barakar Formation which was deposited in a fluviatile setting as discussed in previous work (Mendhe et al., 2018; Mishra et al., 2018; Mishra et al., 2021; Varma et al., 2018) in an intracratonic rift basin setting (Tewari and Maejima 2010). Thermal maturity of the starting materials is in the early mature range with VRo values of 0.60 ± 0.08%, 0.64 ± 0.03%, and 0.70 ± 0.07%, respectively (Mishra et al., 2021). Hackley, P.C., Warwick, P.D., Breland, F.C., Jr., 2007. Organic petrology and coalbed gas content, Wilcox Group, northern Louisiana. Int. J. Coal Geol. 71, 54-71. Warwick, P., Breland, F., Hackley, P., 2008. Biogenic origin of coalbed gas in the northern Gulf of Mexico Coastal Plain, USA. Int. J. Coal Geol. 76, 119-137 Hackley, P.C., Cardott, B.J., 2020. Sample mounting for organic petrology: no thermal effects from transient exposure to elevated temperatures. Int. J. Coal Geol. 223, Article No. 103446. Hackley, P.C., Lewan, M., 2018. Understanding and distinguishing reflectance measurements of solid bitumen and vitrinite using hydrous pyrolysis: Implications to petroleum assessment. AAPG Bulletin 102, 1119-1140. Hackley, P.C., Araujo, C.V., Borrego, A.G., Bouzinos, A., Cardott, B.J., Cook, A.C., Eble, C., Flores, D., Gentzis, T., Gonçalves, P.A., Mendonça Filho, J.G., Hámor-Vidó, M., Jelonek, I., 546 Kommeren, K., Knowles, W., Kus, J., Mastalerz, M., Menezes, T.R., Newman, J., Oikonomopoulos, I.K., Pawlewicz, M., Pickel, W., Potter, J., Ranasinghe, P., Read, H., Reyes, J., Rosa Rodriguez, G.D.L., Alves Fernandes de Souza, I.V., Suárez-Ruiz, I., Sýkorová, I., Valentine, B.J., 2015. Standardization of reflectance measurements in dispersed organic matter: Results of an exercise to improve interlaboratory agreement. Marine and Petroleum Geology 59, 22-34. Hatch, J.R., Pawlewicz, M.J., 2007. Petroleum assessment of the Pottsville Coal Total Petroleum System, Black Warrior Basin, Alabama and Mississippi, in: Hatch, J.R., Pawlewicz, M.J. (Eds.), Geologic assessment of undiscovered oil and gas resources of the Black Warrior Basin Province, Alabama and Mississippi. U.S. Geological Survey, U.S. Geological Survey Digital Data Series DDS-69-I, chap. 4, 28 p. Mendhe, V.A., Kumar, V., Saxena, V.K., Bannerjee, M., Kamble, A.D., Singh, B.D., Mishra, S., Sharma, S., Kumar, J., Varma, A.K., Mishra, D.K., Samad, S.K., 2018. Evaluation of gas resource potentiality, geochemical and mineralogical characteristics of Permian shale beds of Latehar-Auranga Coalfield, India. Int. J. Coal Geol. 196, 43-62. Mishra, D.K., Samad, S.K., Varma, A.K., Mendhe, V.A., 2018. Pore geometrical complexity and fractal facets of Permian shales and coals from Auranga Basin, Jharkhand, India. J. Nat. Gas Sci. Eng. 52, 25-43. Mishra, D.K., Varma, A.K., Mendhe, V.A., Agrawal, S., Singh, B.D., Hackley, P.C., 2021. Organo-facies and mineral effects on sorption capacity of low-maturity Permian Barakar shales from the Auranga Basin, Jharkhand, India. Energy & Fuels 35, 7717-7737. Varma, A.K., Mishra, D.K., Samad, S.K., Prasad, A.K., Panigrahi, D.C., Mendhe, V.A., Singh, B.D., 2018. Geochemical and organo-petrographic characterization for hydrocarbon generation from Barakar Formation in Auranga Basin, India. Int. J. Coal Geol. 186, 97-114. Tewari, R.C., Maejima, W., 2010. Origin of Gonwana basins of peninsular India. Journal of Geosciences 53, 43-49. 2021 Hydrous pyrolysis (HP) was used for thermal maturation experiments as discussed by Lewan (1993). Each experiment used isothermal heating of 2-4 g sample aliquots for 72 hrs. The temperatures selected were 320˚C, 350˚C, and 370˚C to provide a maturity range in HP residues from peak oil, to condensate, to dry gas thermal conditions, respectively. The crushed (1-3 mm particle size) samples were loaded into stainless-steel (SS-316) Swagelok mini-reactor vessels of 25-35 ml internal volume consisting of tubing caps and plugs of 3.81 cm internal diameter. Sample material was completely submerged in deionized water with sufficient water added to keep the sample material covered at the experimental temperature (Lewan, 1993). As described by Lewan (1993), the amounts of water and sample added to each reactor were based on calculations using the internal volume of the reactor, rock densities, and steam tables to avoid catastrophic rupture. Reactors were sealed with ~270 ft-lb torque using a Fel-Pro C5-A copper-based anti-seize thread lubricant. After sealing and weighing to +/-0.01 g, reactors were placed in gas chromatograph ovens and heated isothermally for 72 hrs. After cooling, reactors were weighed again to check for leakage, then opened and reweighed to estimate outgassing. Bitumen was removed from rock surfaces via an acetone rinse, followed by rinsing of the HP residue in deionized water. Pyrolyzed rock residues were left overnight in a vacuum oven at ~60°C and -50 to -60 kPa to remove moisture. Lewan, M.D., 1993. Laboratory Simulation of Petroleum Formation. In: Engel M.H., Macko S.A. (eds) Organic Geochemistry. Topics in Geobiology 11. 2021 The pyrolysis residues were analysed via programmed temperature pyrolysis (via Hydrocarbon Analyser with Kinetics, HAWK) and LECO carbon analyser for total organic carbon (TOC) content analysis. Analysis with the LECO C744 carbon analyser was after carbonate removal at room temperature using 6 M HCl (Oliver and Warden, 2020). Programmed temperature pyrolysis followed typical procedures (Dreier and Warden, 2021; Espitalié et al., 1985; Peters, 1986). The geochemical screening analyses were performed according to the instrument manuals and included internal laboratory standards. The unheated samples and pyrolysis residues were prepared into petrographic pellets for vitrinite reflectance analyses according to ASTM D2797 (ASTM, 2015a). Rock particles were mounted in a thermoplastic (poly-methyl methacrylate, PMMA) briquette which was ground and polished with consecutively finer abrasives to a final stage of 0.05 μm. The mean reflectance of vitrinite was determined with ~20 measurements on the carbonaceous shale samples and ~100 measurements on coal samples. Measurement used a Leica DM4000 microscope equipped with LED illumination and a monochromatic digital camera for reflected light detection operated by the Hilgers Fossil system per ASTM D7708 (ASTM, 2015b) for carbonaceous shale samples and ASTM D2798 (ASTM, 2015c) for coal samples. Maceral analysis was not performed quantitatively but visual estimations of the types and relative abundances of vitrinite, inertinite, and liptinite macerals were recorded qualitatively during vitrinite reflectance analysis. Oliver, T., Warden, A., 2020. Petroleum Geochemistry Research Laboratory Total Organic Carbon and Total Carbon Method. U.S. Geological Survey, U.S. Geological Survey webpage, https://doi.org/10.5066/P9X85HUF (accessed January 14, 2022). Dreier, M., Warden, A., 2021. Petroleum Geochemistry Research Laboratory Programmed Pyrolysis Method. U.S. Geological Survey, U.S. Geological Survey webpage, https://doi.org/10.5066/P9HQSBGH (accessed January 14, 2022). Espitalié, J., Deroo, G., Marquis, F., 1985. La pyrolyse Rock-Eval et ses applications. Première partie. Rev. Inst. Fr. Pét. 40, 563-579, 755-578. Peters, K.E., 1986. Guidelines for Evaluating Petroleum Source Rock Using Programmed Pyrolysis. AAPG Bulletin 70, 318-329. ASTM, 2015a. ASTM D2798 Standard Practice for Preparing Coal Samples for Microscopical Analysis by Reflected Light, Petroleum Products, Lubricants, and Fossil Fuels; Gaseous Fuels; Coal and coke. ASTM International, West Conshohocken, PA 5.06. ASTM, 2015b. ASTM 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. ASTM International, West Conshohocken, PA 5.06. ASTM, 2015c. ASTM D2798 Standard Test Method for Microscopical Determination of the Vitrinite Reflectance of Coal,. ASTM International, West Conshohocken, PA 2021 Micro-Fourier transform infrared spectroscopy (micro-FTIR) data collection used a Bruker Hyperion 3000 FTIR microscope equipped with a liquid-N2 cooled mercury cadmium tellurium (MCT) detector (Hackley et al., 2020, 2020a). Spectra were acquired using a 20× germanium attenuated total reflectance (Ge-ATR) objective (0.6 NA) with the background acquired from atmosphere. Spectra were acquired from 600 to 6,000 cm−1 with 100 co-added scans at a spectral resolution of 4 cm−1. The Ge147 ATR objective tip diameter is ∼100 μm and the vitrinite fragments selected for measurement were of sufficient size to allow probing of the entire objective contact point. For each sample, 1-5 fragments of vitrinite were selected for micro-FTIR analysis. Hackley, P.C., Cardott, B.J., 2020. Sample mounting for organic petrology: no thermal effects from transient exposure to elevated temperatures. Int. J. Coal Geol. 223, Article No. 103446. Hackley, P.C., Jubb, A.M., Valentine, B.J., Hatcherian, J.J., Yu, J.-J., Podrazky, W.K., 2020a. Investigating the effects of broad ion beam milling to sedimentary organic matter: surface flattening or heat-induced aromatization and condensation? Fuel 282, 118627. 2021 Geographic Names Information System (GNIS) placenames (https://www.usgs.gov/us-board-on-geographic-names/domestic-names?p=gnispq) Point Table 1.csv Coal and carbonaceous shale samples used in this study Producer defined Sample ID Identifier of sample used in study Producer defined Sample identifier Group or Formation Group or formation from which sample was collected Producer defined Wilcox Group Sample was taken from the Wilcox group Producer defined Carbondale Formation Sample was taken from the Carbondale Formation Producer defined Pottsville Group Sample was taken from the Pottsville Group Producer defined Barakar Formation Sample was taken from the Barakar Formation Producer defined Lithology Rock type of selected sample Producer defined Coal Coal sample Producer defined Carbonaceous shale Sample is Carbonaceous shale Producer defined Age Age of selected sample Producer defined International Commission on Stratigraphy Geologic Timescale https://stratigraphy.org/chart Country/Region Country and/or region where sample was collected Producer defined Geographic Names Information System https://www.usgs.gov/us-board-on-geographic-names Sources Original study for which sample was collected Producer defined Hackley and Lewan (2018) Sample taken from Hackley, Paul; Lewan, Michael. (2018). Understanding and distinguishing reflectance measurements of solid bitumen and vitrinite using hydrous pyrolysis: Implications to petroleum assessment. AAPG Bulletin. 102. 1119-1140. 10.1306/08291717097. Producer defined Hackley et al. (2015) Sample taken from Hackley, Paul; Araujo, Carla; Borrego, Angeles; Bouzinos, Antonios; Cardott, Brian; C.Cook, Alan; Eble, Cortland; Flores, Deolinda; Gentzis, Thomas; Gonçalves, Paula; Mendonça Filho, João; Jelonek, Iwona; Kommeren, Kees; Knowles, Wayne; Kus, Jolanta; Mastalerz, Maria; Menezes, Taíssa; Newman, Jane; Valentine, Brett. (2015). Standardization of reflectance measurements in dispersed organic matter: Results of an exercise to improve interlaboratory agreement. Marine and Petroleum Geology. 59. 22-34. 10.1016/j.marpetgeo.2014.07.015. Producer defined Varma et al. (2018) Varma, Atul; Mishra, Divya; Samad, Suresh; Prasad, Amal; Panigrahi, Durga; Mendhe, Vinod; Singh, Bhagwan (2018). Geochemical and organo-petrographic characterization for hydrocarbon generation from Barakar Formation in Auranga Basin, India. International Journal of Coal Geology. 186. 97-114. 10.1016/j.coal.2017.12.002. Producer defined Table 2 Geochemical parameters from screening analysis and vitrinite reflectance for the coal and carbonaceous shale samples used in this study. Producer defined Group or Formation Group or formation from which sample was collected. Samples labeled with "HP residue" are hydrous pyrolysis residue from preceding sample Producer defined Sample collection location Sample ID Identifier of sample, followed by temperature at which hydrous pyrolysis was performed Producer defined Sample identifiers USGS ID Internal USGS identifier, indicating date and order sample was processed. Producer defined Sample identifier, in the form EYYMMDD-Order VRo (%) Average vitrinite reflectance Producer defined 0.48 1.97 Percent reflectance Values followed by "ǂ" indicate values from group mean interlaboratory study (Hackley et al., 2015). no. Number of vitrinite reflectance measurements collected Producer defined 20 120 Number of measurements Values followed by "ǂ" indicate values from group mean interlaboratory study (Hackley et al., 2015). VRo SD Standard deviation of vitrinite reflectance measurements Producer defined 0.03 0.14 Percent reflectance Values followed by "ǂ" indicate values from group mean interlaboratory study (Hackley et al., 2015). TOC (wt%) Total Organic Carbon in weight percent; maximum value is reported Producer defined 1.95 73.75 Weight percent Tmax (˚C) The temperature at which maximum amount of hydrocarbons were produced during hydrous pyrolysis Espitalié, J., Laporte, J.L., Madec, M., Marquis, F., Leplat, P., Paulet, J., 1977. Méthode rapide de caractérisation des rochès, de leur potential pétrolier et de leur degree d’évolution. Revue de L’Institut Français du Pétrole 32, 23-43. 415.00 565.00 Degrees Celsius S1 (mg HC/g rock) S1 values (free hydrocarbons), measured in mg HC/g of rock; the free hydrocarbons already generated that are volatilized out of the rock without cracking the kerogen. Espitalié, J., Laporte, J.L., Madec, M., Marquis, F., Leplat, P., and Paulet, J., 1977, Méthode rapide de caractérisation des rochès, de leur potential pétrolier et de leur degree d’évolution: Revue de L’Institut Français du Pétrole, v. 32, p. 23–43. 0.02 21.09 Miligrams per gram (mg/g) S2 (mg HC/g rock) Values (generated hydrocarbons), measured in mg HC/g of rock; the amount of hydrocarbons generated through thermal cracking of kerogen and heavy hydrocarbons. Espitalié, J., Laporte, J.L., Madec, M., Marquis, F., Leplat, P., and Paulet, J., 1977, Méthode rapide de caractérisation des rochès, de leur potential pétrolier et de leur degree d’évolution: Revue de L’Institut Français du Pétrole, v. 32, p. 23–43. 0.49 119.10 miligrams per gram (mg/g) S3 (mg CO2/g rock) The CO2 produced in hydrous pyrolysis as a result of kerogen breakdown in milligrams CO2 to grams rock Espitalié, J., Laporte, J.L., Madec, M., Marquis, F., Leplat, P., and Paulet, J., 1977, Méthode rapide de caractérisation des rochès, de leur potential pétrolier et de leur degree d’évolution: Revue de L’Institut Français du Pétrole, v. 32, p. 23–43. 0.13 10.20 miligrams per gram (mg/g) HI (mg HC/g TOC) The ratio of hydrogen (S2 in mg HC/g) to TOC, as expressed in the formula [HI = (S2/TOC) x100]. Espitalié, J., Laporte, J.L., Madec, M., Marquis, F., Leplat, P., and Paulet, J., 1977, Méthode rapide de caractérisation des rochès, de leur potential pétrolier et de leur degree d’évolution: Revue de L’Institut Français du Pétrole, v. 32, p. 23–43. 19 230 miligrams per gram (mg/g) OI (mg HC/g TOC) The ratio of oxygen (S3 in mg HC/g) to TOC, as expressed in the formula [OI = (S3/TOC) x100]. Espitalié, J., Laporte, J.L., Madec, M., Marquis, F., Leplat, P., and Paulet, J., 1977, Méthode rapide de caractérisation des rochès, de leur potential pétrolier et de leur degree d’évolution: Revue de L’Institut Français du Pétrole, v. 32, p. 23–43. 3 19 miligrams per gram (mg/g) PI [S1/(S1+S2)] The ratio of the amount of petroleum already generated by the kerogen to the total amount of petroleum that the kerogen is capable of generating. The PI is expressed by the formula [PI = S1/(S1+S2)]. Espitalié, J., Laporte, J.L., Madec, M., Marquis, F., Leplat, P., and Paulet, J., 1977, Méthode rapide de caractérisation des rochès, de leur potential pétrolier et de leur degree d’évolution: Revue de L’Institut Français du Pétrole, v. 32, p. 23–43. 0.01 0.30 Ratio Comments Comments on values in table Producer defined Table comments -- USGS ID-U.S. Geological Survey identification number, VRo-vitrinite reflectance in %, no.-number of measurements, SD-standard deviation, TOC-total organic carbon content, Tmax-temperature of maximum pyrolyzate signal, S1-thermal distillate, S2-pyrolyzate, S3-CO2 yield; HI-hydrogen index (S2*100/TOC), OI-oxygen index (S3*100/TOC), PI-Production Index [S1/(S1+S2)], HC-hydrocarbons. Table 3.csv Micro-FTIR data parameters, error, and number of measurements. Producer defined Sample ID Identifier of sample used in study Producer defined Sample identifier T (°C) Temperature at which hydrous pyrolysis was performed on sample Producer defined 320 370 Degrees Celsius orig. Original sample material Producer defined no. Number of FTIR measurements taken Producer defined 1 6 Number of measurements A1 A1 factor, measured by FTIR Producer defined 0.176 0.47 Dimensionless A1 SD Standard deviation of A1 measurements Producer defined 0.007 0.203 Dimensionless Values followed by "*" indicate propagated uncertainty of fit precision used because only one measurement was available. A2 A2 factor, measured by FTIR Producer defined 0.764 0.925 Dimensionless A2 SD Standard deviation of A2 measurements Producer defined 0.006 0.114 Dimensionless Values followed by "*" indicate propagated uncertainty of fit precision used because only one measurement was available. C C factor, as measured by FTIR Producer defined 0.074 0.337 Dimensionless C SD Standard deviation of C factor measurements Producer defined 0.002 0.086 Dimensionless Values followed by "*" indicate propagated uncertainty of fit precision used because only one measurement was available. CH2/CH3 Branching ratio/chain length Producer defined 1.592 3.611 Dimensionless SD Standard deviation of CH2/CH3 measurements Producer defined 0.011 1.467 Dimensionless VRo (%) Average vitrinite reflectance measurement taken on sample Producer defined 0.48 1.97 Percent reflectance Values followed by "ǂ" indicate value taken from group mean interlaboratory study Comments Comments on data in table Producer defined Comments on table values GS ScienceBase U.S. Geological Survey mailing and physical

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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. This file contains data available in comma separated value (.csv) file format. The user must have software capable of opening and viewing a .csv file. 20220411 Mary R. Croke NORTHEAST REGION: GEOLOGY, ENERGY&MINERALS SC Pathways Student mailing and physical

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