This “Possinger_NatureCommunications_2020_CryoEELSdata_readme.txt” file was generated on 20201027 by Angela R. Possinger, and updated on 20210604 to add related publication information by Sarah J. Wright, data curator. ------------------- GENERAL INFORMATION ------------------- Title of Dataset: “Data From: Organo-Organic and Organo-Mineral Interfaces in Soil at the Nanometer Scale” Author Information (Name, Institution, Address, Email) Associate or co-investigator (first author): Angela R. Possinger# Cornell University School of Integrative Plant Science Soil and Crop Sciences Section 306 Tower Road Ithaca, NY 14853 USA #Current Affiliation: Department of Forest Resources and Environmental Conservation, Virginia Tech, Blacksburg, VA 24061, USA Associate or co-investigator: Michael J. Zachman## Cornell University School of Applied and Engineering Physics 271 Clark Hall Ithaca, NY 14853 USA ##Current Affiliation: Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA Associate or co-investigator: Akio Enders Cornell University School of Integrative Plant Science Soil and Crop Sciences Section 306 Tower Road Ithaca, NY 14853 USA Associate or Co-investigator: Barnaby D.A. Levin Cornell University School of Applied and Engineering Physics 271 Clark Hall Ithaca, NY 14853 USA Associate or co-investigator: David A. Muller [1] Cornell University School of Applied and Engineering Physics 271 Clark Hall Ithaca, NY 14853 USA [2] Kavli Institute at Cornell for Nanoscale Science 420 Physical Sciences Building
Ithaca, NY 14853 USA Associate or co-investigator: Lena F. Kourkoutis Cornell University [1] School of Applied and Engineering Physics 271 Clark Hall Ithaca, NY 14853 USA [2] Kavli Institute at Cornell for Nanoscale Science 420 Physical Sciences Building
Ithaca, NY 14853 USA Principal Investigator (corresponding author): Johannes Lehmann [1] Cornell University School of Integrative Plant Science Soil and Crop Sciences Section 306 Tower Road Ithaca, NY 14853 USA [2] Technical University of Munich Institute for Advanced Study Lichtenbergstraße 2 a 85748 Garching bei München Germany [3] Cornell Atkinson Center for Sustainability 340 Tower Road Ithaca, NY 14853 USA Email: cl274@cornell.edu Date of data collection (single date, range, approximate date): 01/01/2014-08/01/2019 Geographic location of data collection: Soil samples were collected from the Pololu Flow on Kohala, HI, USA. Standard materials were prepared at Bradfield Hall (Cornell University, Ithaca, NY). Imaging and microscopy work was conducted at the Cornell Center for Materials Research (Cornell University, Ithaca, NY). Information about funding sources or sponsorship that supported the collection of the data: Funding for this study was provided by the Technical University of Munich Institute for Advanced Study, the NSF IGERT in Cross-Scale Biogeochemistry and Climate at Cornell University (NSF Award #1069193), the Cornell College of Agriculture and Life Sciences Alumni Foundation, and the Andrew W. Mellon Foundation. L.F.K. and M.J.Z. acknowledge support from the Packard Foundation and the NSF (DMR-1654596). Work was conducted at the Cornell Center for Materials Research Shared Facilities, supported through NSF MRSEC program (DMR-1719875). The FIB/SEM cryo-stage and transfer system was supported by the Kavli Institute at Cornell (KIC) for Nanoscale Science and the Energy Materials Center at Cornell, DOE EFRC BES (DE-SC0001086). The FEI Titan Themis 300 was acquired through NSF-MRI-1429155, and with additional support from Weill Institute, KIC and Cornell University. -------------------------- SHARING/ACCESS INFORMATION -------------------------- Licenses/restrictions placed on the data, or limitations of reuse: This data is shared under a CC BY-NC license (https: //creativecommons.org/licenses/by-nc/4.0/); the data are free to use with proper attribution and acknowledgment of the original authors, and may not be used for commercial purposes. Users must also indicate that the conclusions and assumptions made from analysis of these data are not necessarily the view of the original authors, Cornell University, or the project funders (see funding agency information above). Recommended citation for the data: Angela R. Possinger, Michael J. Zachman, Akio Enders, Barnaby D. A. Levin, David A. Muller, Lena F. Kourkoutis and Johannes Lehmann. (2020) Data from: Organo-organic and organo-mineral interfaces in soil at the nanometer scale. [Dataset] Cornell University eCommons Repository. https: //doi.org/10.7298/6vtr-c668 Citation for and links to publications that cite or use the data: Possinger, A.R., Zachman, M.J., Enders, A., Levin, B.D.A., Muller, D.A., Kourkoutis, L.F., & Lehmann, J. Organo–organic and organo–mineral interfaces in soil at the nanometer scale. Nat Commun 11, 6103 (2020). https://doi.org/10.1038/s41467-020-19792-9 -------------------- DATA & FILE OVERVIEW -------------------- File list (filenames, directory structure (for zipped files) and brief description of all data files): Abbreviations used in file list: STEM: Scanning transmission electron microscopy EELS: Electron energy loss spectroscopy EDX: Electron dispersive X-ray HAADF: High angle annular dark field ADF: Annular dark field MCR: Multivariate curve resolution AUC: Area under the curve #Set 1 Organo-mineral interface linescan (EELS)##################### 1.1. Filename: Linescan280nm.tif Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: Image showing location of EELS linescan at organo-mineral interface # 1.2. Filename: Org-min_03_02_LinePEELS_240eVshift_mono60_5sx1fx10pts_280nmline_EELS_0001.emi Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: Metadata for EELS linescan at organo-mineral interface # 1.3. Filename: Org-min_02_02_LinePEELS_240eVshift_mono60_5sx1fx10pts_280nmline_EELS_0001_1.ser Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: EELS data for linescan at organo-mineral interface # 1.4. Filename: Org-min_01_Linescan_EnergyShift_Mill3_ZLP_1.27IMFP_Post1stCEdge_mono300_50mssx100fr_EELS.dm3 Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: Low-loss EELS measurement for energy shift correction of linescan # 1.5. Filename: Org-min_ZLP.csv Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: Calculated energy shift for EELS linescan # 1.6. Filename: Linescan_EELS_C.csv Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: EELS carbon K-edge spectra for linescan region # 1.7. Filename: Linescan_EELS_N.csv Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: EELS nitrogen K-edge spectra for linescan region # 1.8. Filename: Linescan_AUC.csv Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: Calculated area under the curve (AUC) estimates for linescan region # 1.9. Filename: Metadata_Org-min_01_Linescan_EnergyShift_Mill3_ZLP_1.27IMFP_Post1stCEdge_mono300_50mssx100fr_EELS.txt Directory: Set 1 Organo-mineral interface linescan (EELS) Brief description: Metadata text file for zero-loss spectrum # #Set 2: Organo-mineral adjacent region (EELS)####################### # 2.1. Filename: 17_Mill3_320kx_ThinCArea_32usx1024fr_30mm_ADF.bin Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Overview annular dark field image of analysis region # 2.2. Filename: AdjC_01_Point1_240eVshift_ThinC_Point_mono60_5sx1f_EELS_.dm3 Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Point EELS scan (1 of 3) of area adjacent to mineral interface # 2.3. Filename: AdjC_02_Point2_EELS_240eVshift_ThinC_Point2_mono40_8sx1f_EELS.dm3 Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Point EELS scan (2 of 3) of area adjacent to mineral interface # 2.4. Filename: AdjC_03_Point3_EELS_240eVshift_ThinC_mono40_10sx1f_EELS.dm3 Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Point EELS scan (3 of 3) of area adjacent to mineral interface # 2.5. Filename: Adjacent_EELS_C.csv Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Processed EELS spectra (carbon K-edge) for three points in area adjacent to mineral interface # 2.6. Filename: Adjacent_EELS_N.csv Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Processed EELS spectra (nitrogen K-edge) for three points in area adjacent to mineral interface # 2.7. Filename: Adjacent_AUC.csv Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Calculated area under the curve for EELS data in adjacent region # 2.8. Filename: Metadata_AdjC_01_Point1_240eVshift_ThinC_Point_mono60_5sx1f_EELS.txt Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Metadata text file for Point 1 spectrum (2.2) # 2.9. Filename: Metadata_AdjC_02_Point2_EELS_240eVshift_ThinC_Point2_mono40_8sx1f_EELS.txt Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Metadata text file for Point 2 spectrum (2.3) # 2.10. Filename: Metadata_AdjC_03_Point3_EELS_240eVshift_ThinC_mono40_10sx1f_EELS.txt Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Metadata text file for Point 3 spectrum (2.4) # #Set 3: Organo-mineral overview (EDX)###################### # 3.1. Filename: 18_Mill3_29kx_Overview_32usx1024fr_100mm_Spot5_Tilt30_HAADF.bin Directory: Set 3 Organo-mineral overview (EDX) Brief Description: STEM HAADF image of analysis region in Set 3 # 3.2. Filename: Mill3_Al.tif Directory: Set 3 Organo-mineral overview (EDX) Brief Description: EDX aluminum elemental map # 3.3. Filename: Mill3_C.tif Directory: Set 3 Organo-mineral overview (EDX) Brief Description: EDX carbon elemental map # 3.4. Filename: Mineral_Sample_EDX.csv Directory: Set 3 Organo-mineral overview (EDX) Brief Description: Sum EDX spectrum of analysis area # #Set 4: Organo-organic nitrogen map (EELS)######################### # 4.1. Filename: 15_Lamella after first EELS_12 deg tilt_10 kx_0-5 nA_50 um apert_130mm_12 us_1024.tif Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: STEM image showing overview of location for EELS in Set 4 # 4.2. Filename: Org-org_02_17_Overview_5 kx_0-5 nA_38 mm_CL_10 ms_94x111.dm3 Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: EELS core-loss spectrum image (overview) # 4.3. Filename: Overview_Calibration.csv Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Measurements used to calibrate scale bar in 4.2 and 4.4 # 4.4. Filename: N_integrated_scale_bar.txt Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Integrated nitrogen (N) K-edge intensity values for region of interest in 4.2 (text image) # 4.5. Filename: N_integrated_tif.tif Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Greyscale image of 4.4 # 4.6. Filename: Org-org_Overview_EELS.csv Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Example EELS spectra from higher and lower N regions of in 4.2 # 4.7. Filename: Metadata_Org-org_02_17_Overview_5 kx_0-5 nA_38 mm_CL_10 ms_94x111.txt Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Metatdata text file for overview EELS map (4.2) # #Set 5: Organo-organic features (EELS)############################ # 5.1. Filename: Org-org_04_19_28-5 kx_0-5 nA_38 mm_CL_10 ms_108x102_15-88 nm.dm3 Directory: Set 5 Organo-organic features (EELS) Brief Description: EELS core-loss spectrum image (high N features, 15.88 nm pixel) # 5.2. Filename: Org-org_03_19_28-5 kx_0-5 nA_38 mm_LL_200 us_108x102_15-88 nm.dm3 Directory: Set 5 Organo-organic features (EELS) Brief Description: EELS low-loss spectrum image associated with 5.1 # 5.3. Filename: Features-EELS-Components.csv Directory: Set 5 Organo-organic features (EELS) Brief Description: MCR output component spectra (carbon) associated with 5.1 # 5.4. Filename: C fit MCR comp1.tif Directory: Set 5 Organo-organic features (EELS) Brief Description: MCR output component #1 map associated with 5.1 # 5.5. Filename: C fit MCR comp2.tif Directory: Set 5 Organo-organic features (EELS) Brief Description: MCR output component #2 map associated with 5.1 # 5.6. Filename: Metadata_Org-org_03_19_28-5 kx_0-5 nA_38 mm_LL_200 us_108x102_15-88 nm.txt Directory: Set 5 Organo-organic features (EELS) Brief Description: Metadata for EELS low-loss map (5.2) # 5.7. Filename: Metadata_Org-org_04_19_28-5 kx_0-5 nA_38 mm_CL_10 ms_108x102_15-88.txt Directory: Set 5 Organo-organic features (EELS) Brief Description: Metadata for EELS core-loss map (5.1) # #Set 6: Organo-organic interface MCR (EELS)######################## # 6.1. Filename: Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x735_0-9381 nm.dm3 Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: EELS core-loss spectrum image (organo-organic interface, 0.9381 nm pixel) # 6.2. Filename: Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x735_0-9381 nm.dm3 Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: EELS low-loss spectrum image associated with 6.1 # 6.3. Filename: Interface-EELS-components-2comp.csv Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (2-component) output component spectra (carbon) associated with 6.1 # 6.4. Filename: Org-org_3components.csv Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (3-component) output component spectra (carbon) associated with 6.1 # 6.5. Filename: Interface C fitMCR comp1.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (2-component) component #1 map associated with 6.1 # 6.6. Filename: Interface C fitMCR comp2.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (2-component) component #2 map associated with 6.1 # 6.7. Filename: Interface C3 fitMCR comp1.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (3-component) component #1 map associated with 6.1 # 6.8. Filename: Interface C3 fitMCR comp2.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (3-component) component #2 map associated with 6.1 # 6.9. Filename: Interface C3 fitMCR comp3.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (3-component) component #3 map associated with 6.1 # 6.10. Filename: Org-org_3components_profile.csv Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: Distribution of MCR component pixel intensity across image (line profile) (3-component MCR) # 6.11. Filename: Metadata_Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x75_0-9381 nm.txt Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: Metadata text file for low-loss EELS map (6.2) # 6.12. Filename: Metadata_Org-org_06_25_320 kx_0-5 nA_38 mm_CL_20 ms_142x75_0-9381 nm.txt Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: Metadata text file for core-loss EELS map (6.1) # #Set 7: Organo-organic interface average boxes (EELS)################### # 7.1. Filename: Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x735_0-9381 nm.dm3 ###Same file as 6.1####: Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: EELS core-loss spectrum image (organo-organic interface, 0.9381 nm pixel) # 7.2. Filename: Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x735_0-9381 nm.dm3 ###Same file as 6.2####: Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: EELS low-loss spectrum image associated with 6.1 # 7.3. Filename: 25_320 kx_0-5 nA_38 mm_ADF_142x75_0-9381 nm.dm3 Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: ADF image showing analysis area in 7.1 and 7.2 # 7.4. Filename: Locations_Lateral.pdf Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Locations for EELS average boxes across the organo-organic interface # 7.5. Filename: Locations_Vertical.pdf Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Locations of EELS average boxes along the organo-organic interface in the vertical direction # 7.6. Filename: C-12nm-1.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 1 in 7.4 # 7.7. Filename: C-12nm-2.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 2 in 7.4 # 7.8. Filename: C-12nm-3.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 3 in 7.4 # 7.9. Filename: C-12nm-4.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 4 in 7.4 # 7.10. Filename: C-12nm-5.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 5 in 7.4 # 7.11. Filename: N-12nm-1.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 1 in 7.4 # 7.12. Filename: N-12nm-2.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 2 in 7.4 # 7.13. Filename: N-12nm-3.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 3 in 7.4 # 7.14. Filename: N-12nm-4.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 4 in 7.4 # 7.15. Filename: N-12nm-5.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 5 in 7.4 # 7.16. Filename: O-12nm-1.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 1 in 7.4 # 7.17. Filename: O-12nm-2.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 2 in 7.4 # 7.18. Filename: O-12nm-3.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 3 in 7.4 # 7.19. Filename: O-12nm-4.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 4 in 7.4 # 7.20. Filename: O-12nm-5.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 5 in 7.4 # 7.21. Filename: Interface_2pixel_C.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for regions a through l in 7.4 # 7.22. Filename: Interface_2pixel_N.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for regions a through l in 7.4 # 7.23. Filename: Interface_2pixel_O.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for regions a through l in 7.4 # 7.24. Filename: Vertical_Box_1.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for region x in 7.5 # 7.25. Filename: Vertical_Box_1_N.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for region x in 7.5 # 7.26. Filename: Vertical_Box_2.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for region y in 7.5 # 7.27. Filename: Vertical_Box_2_N.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for region y in 7.5 # 7.28. Filename: Vertical_Box_3.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for region z in 7.5 # 7.29. Filename: Vertical_Box_3_N.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for region z in 7.5 # 7.30. Filename: Organic_Interface_AUC.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Estimated AUC for carbon, nitrogen, oxygen, and carbon fine structure across organo-organic interface in 7.4 # 7.31. Filename: Vertical_Box_AUC.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Estimated AUC for carbon, nitrogen, and carbon fine structure across vertical boxes in 7.5 # 7.32. Filename: Org-org_interface_rate_change.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Calculated rate of change of ratios across interface # 7.33. Filename: final_2nm_data.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Estimated area under the curve and ratios for high-resolution organo-organic interface # 7.34. Filename: Metadata_Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x75_0-9381 nm.txt Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Metadata for low-loss EELS map (7.2) # 7.35. Filename: Metadata_Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x75_0-9381 nm.txt Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Metadata for core-loss EELS map (7.1) # #Set 8: Organo-organic sample composition (EDX)################## # 8.1. Filename: Organic_Sample_EDX.csv Directory: Set 8 Organo-organic sample composition (EDX) Brief Description: Point scan EDX sum spectrum for sample analyzed in Sets 4-7 # #Set 9: Damage test########################################## # 9.1. Filename: Damage_01_17_Near grid bar_640 kx_3 nA_10 ms_0-1 eV_0 eV shift_100x100.dm3 Directory: Set 9 Damage test Brief Description: EELS low-loss measurement for 9.2-9.8 # 9.2. Filename: Damage_02_19a_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.dm3 Directory: Set 9 Damage test Brief Description: EELS core-loss measurement a for damage test # 9.3. Filename: Damage_03_19b_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test Brief Description: EELS core-loss measurement b for damage test # 9.4. Filename: Damage_04_19c_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test Brief Description: EELS core-loss measurement c for damage test # 9.5. Filename: Damage_05_19d_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test Brief Description: EELS core-loss measurement d for damage test # 9.6. Filename: Damage_06_19e_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test Brief Description: EELS core-loss measurement e for damage test # 9.7. Filename: Damage_07_19f_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test Brief Description: EELS core-loss measurement f for damage test # 9.8. Filename: Damage_08_19g_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test Brief Description: EELS core-loss measurement g for damage test # 9.9. Filename: Damage_ZLP.csv Directory: Set 9 Damage test Brief Description: Zero-loss peak position for energy offset in 9.10 # 9.10. Filename: DamageTest_Spectra.csv Directory: Set 9 Damage test Brief Description: Corrected EELS carbon K-edge spectra from files 9.2-9.8 # 9.11. Filename: Damage_AUC.csv Directory: Set 9 Damage test Brief Description: Estimations of AUC for carbon and carbon fine structure in damage test spectra (file 9.10) # 9.12. Filename: Metadata_Damage_02_19a_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test Brief Description: Metadata text file for damage test 9.2 # 9.13. Filename: Metadata_Damage_03_19b_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test Brief Description: Metadata text file for damage test 9.3 # 9.14. Filename: Metadata_Damage_04_19c_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test Brief Description: Metadata text file for damage test 9.4 # 9.15. Filename: Metadata_Damage_05_19d_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txtage_AUC.csv Directory: Set 9 Damage test Brief Description: Metadata text file for damage test 9.5 # 9.16. Filename: Metadata_Damage_06_19e_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test Brief Description: Metadata text file for damage test 9.6 # 9.17. Filename: Metadata_Damage_07_19f_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test Brief Description: Metadata text file for damage test 9.7 # 9.18. Filename: Metadata_Damage_08_19g_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test Brief Description: Metadata text file for damage test 9.8 # 9.19. Filename: DamageTest_Dose.csv Directory: Set 9 Damage test Brief Description: Calculated dose for damage test series # Relationship between files, if important for context: Additional related data collected that was not included in the current data package: If data was derived from another source, list source: If there are there multiple versions of the dataset, list the file updated, when and why update was made: -------------------------- METHODOLOGICAL INFORMATION -------------------------- Description of methods used for collection/generation of data: Data collection and generation methods are included in Chapter 3 of “Electrons, X-rays, and Soil Augers: Probing Soil Organo-Mineral Interactions with a Cross-Scale Analytical Toolbox”, a dissertation by Angela R. Possinger (Cornell University, https: //doi.org/10.7298/tbx6-s287). This study used high spatial resolution imaging and spectroscopy to gain insight into the characteristics of interfaces between organic matter and minerals in soil at a very small scale. We used scanning transmission electron microscopy (STEM) with electron energy loss spectroscopy (EELS) under cryogenic conditions, referring to from here as cryo-STEM-EELS. Soil sample collection: We used two subsoils (0.7-0.9 m) collected from volcanic-ash soils on the Pololu Flow, Kohala, HI. Here, we refer to Sample 1 (in this dataset) as a high mineral content sample and Sample 2 as a high organic content sample. Soil pits (depth ~1m) were excavated by hand. Soil samples were collected by horizon (in 2014) as described previously (Kramer et al., 2012; Grant et al., 2019). Prior to imaging and spectroscopy analysis, soils were stored under field moisture conditions and kept cool (4-9 °C range) during sampling, transport, and storage. Thin sectioning: Soils were sieved to the 53-150 m size fraction at field moisture. Aggregates were gradually hydrated with deionized (DI) water (SPT Ultrasonic Humidfier, Sunpentown, Inc., City of Industry, CA, on low setting) after being distributed on glass fiber filter paper (Whatman GF/A), following Kinyangi et al. (2006). Single intact micro-aggregates were transferred to an aluminum cryo-microtome pedestal and suspended within a droplet of deionized (DI) water, then inverted and immersed in slush nitrogen (N2). Thin sections (1-5 μm) were made using a Leica EM UC7/FC7 (Leica Microsystems, Inc., Buffalo Grove, IL) diamond knife, kept at -60°C. The samples were transferred to either 300 or 400-mesh, adhesive-coated, copper TEM grids and stored under liquid N2. These samples were transferred to a FEI Strata 400 STEM DualBeam focused ion beam (FIB) instrument (FEI Company, Hillsboro, OR), equipped with a Quorum PP3010T Cryo-FIB/SEM Preparation System (Laughton, East Sussex, UK). The cryo-transfer system is described further in Zachman et al. (2016). The pre-thinned samples were further thinned in selected regions to <100-200 nm thick, employing two cryogenic focused ion beam (FIB) approaches: (1) a “wedge” (Sample 1), with the Ga+ ion beam at a shallow angle to the surface of the soil section, and (2) a “lamella” (Sample 2), with milling both above and below the targeted area at a shallow angle. An ion beam voltage of 30 kV and varying current (between approximately 5 pA and 500 pA) was used for milling. Imaging and Spectroscopy: Sample 1 (high mineral content sample, “wedge” thin-section): FEI F20 TEM STEM instrument (FEI Company, Hillsboro, OR) (operated at 200 kV and approximately -180°C), equipped with a Gatan Tridium spectrometer (Gatan Inc., Pleasanton, CA) and Gatan Model 626 cryo-transfer holder. Sample 2 (high organic content, “lamella” thin-section): Aberration-corrected FEI Titan Themis S/TEM instrument (FEI Company, Hillsboro, OR) (operated at 120 kV and approximately -180°C), equipped with a Gatan GIF Quantum 965 spectrometer (Gatan Inc., Pleasanton, CA). Before and after collection of EELS data, overview annular dark-field (ADF) STEM images were obtained. EELS measurements used parameters that optimized counts but minimized sample damage (see Analysis section below). Elemental Analysis: We used electron dispersive X-ray (EDX) spectroscopy to assess the overall elemental composition of the samples. For Sample 1 (high mineral content soil sample, “wedge” thin section), EDX data was collected using the FEI F20 TEM-STEM instrument (FEI Company, Hillsboro, OR) equipped with an Oxford Instruments X-Max 80mm2 EDX detector (Oxford Instruments, Abingdon, Oxfordshire, UK). For Sample 2 (high organic content sample, “lamella” thin section) an EDX point scan was collected (5 kV voltage) near the analysis area using the FEI Strata FIB/SEM instrument described above, equipped with an Oxford Instruments X-Max 80mm2 EDX detector. Damage Tests: An iron-organic synthetic reference material (Sample 3) was used to test potential cryo-STEM-EELS damage. The material was prepared by precipitation of ferrihydrite (nominally Fe2O30.5H2O) (modified method from Schwertmann & Cornell, 2000) together with water-extractable organic matter (WEOM), which was derived from an organic soil (10: 1 C: Fe ratio). The co-precipitate material was purified by dialysis (1000 D molecular weight cut-off), drop-cast on copper (Cu) TEM grid and air-dried. The damage test samples were transferred at room temperature into the FEI Titan instrument described above (operated at 120 kV). The samples were cooled to approximately -180°C after loading into the instrument. We collected 7 repeated EELS measurements (at 640 kx magnification) over the same field of view to assess changes in spectra with increasing dose (to maximum of ~67,000 electrons Å-2). References Grant, K. E., Galy, V. V., Chadwick, O. A., Derry, L. A. Thermal oxidation of carbon in organic matter rich volcanic soils: insights into SOC age differentiation and mineral stabilization. Biogeochem. 144, 291–304 (2019). Kinyangi, J. et al. Nanoscale biogeocomplexity of the organomineral assemblage in soil: Application of STXM microscopy and C 1s-NEXAFS spectroscopy. Soil Sci. Soc. Am. J. 70, 1708–1718 (2006). Kramer, M. G., Sanderman, J., Chadwick, O. A., Chorover, J. & Vitousek, P. M. Long-term carbon storage through retention of dissolved aromatic acids by reactive particles in soil. Glob. Chang. Biol. 18, 2594–2605 (2012). Possinger, A .R., et al. Organo-mineral interactions and soil carbon mineralizability with variable saturation cycle frequency. Geoderma 375, 114483 (2020). Schwertmann, U. & Cornell R. M. Iron Oxides in the Laboratory: Preparation and Characterization, 2nd Edition (Wiley-VCG Verlag GmbH, Weinheim, DE, 2000). Zachman, M. J., Asenath-Smith, E., Estroff, L. A. & Kourkoutis, L. F. Site-specific preparation of intact solid-liquid interfaces by label-free in situ localization and cryo-focused ion beam lift-out. Microsc. Microanal. 22, 1338–1349 (2016). Methods for processing the data: The following describes in detail the analysis steps used to generate electron energy loss spectroscopy (EELS) and auxiliary data. Data acquisition parameters for EELS are described in the manuscript text and metadata text files. For EELS data, dose was determined based on estimated actual exposure time (based on acquisition start and end times in metadata files, or recorded acquisition times for point measurements in set 2). Set 1: Organo-mineral interface linescan (EELS) Filename(s): 1.1. Linescan280nm.tif 1.2. Org-min_03_02_LinePEELS_240eVshift_mono60_5sx1fx10pts_280nmline_EELS_0001.emi 1.3. Org-min_02_02_LinePEELS_240eVshift_mono60_5sx1fx10pts_280nmline_EELS_0001_1.ser 1.4. Org-min_01_Linescan_EnergyShift_Mill3_ZLP_1.27IMFP_Post1stCEdge_mono300_50mssx100fr_EELS.dm3 1.5. Org-min_ZLP.csv 1.6. Linescan_EELS_C.csv 1.7. Linescan_EELS_N.csv 1.8. Linescan_AUC.csv 1.9. Metadata_Org-min_01_Linescan_EnergyShift_Mill3_ZLP_1.27IMFP_Post1stCEdge_mono300_50mssx100fr_EELS.txt Data collection: Sample: Sample 1 (high mineral content sample, “wedge” thin-section): Data type: Electron energy loss linescan (280 nm length) of region within soil sample thin section, with approximate location shown in File 1.1 (annular dark field image, .tif file). Note that scale bar is approximate. Instrument: FEI F20 S/TEM instrument (FEI Company, Hillsboro, OR) Other information: Experimental metadata is included in File 1.2 (.emi format) and File 1.9 (text file). The pertinent information can be extracted from opening the .emi file as a text file under . Analysis: The .ser file (File 1.3) was imported into ImageJ (v. 2.0.0) (Schneider et al., 2012) using the TIA Reader tool included in the Cornell Spectrum Imager package (Cueva et al., 2012). The entire spectrum image was selected using the ImageJ rectangle selection tool, and the CSI Spectrum Analyzer was used to generate a background-subtracted dataset for the image using the linear combination of power laws (LCPL) fit and 3.0-pixel full-width half-maximum (FWHM) oversampling. The 260.0-277.0 eV background subtraction region was used for carbon and the 377.7-394.2 eV region was used for nitrogen. Using the background-subtracted dataset, the EELS spectra for five 2 x 2048 pixel regions of interest (ROI) were selected using the ImageJ rectangle selection tool. From all N spectra, one outlier point (at 405.8 eV) was excluded due to detector error. The energy axis for each EELS spectrum was corrected for energy shift using a low-loss spectrum collected adjacent to the linescan region (File 1.4). The low-loss .dm3 file was imported into ImageJ using the CSI DM3 Reader tool and converted to a text file using the Spectrum Analyzer tool. The data were sorted by intensity (count) (highest to lowest) to determine offset (energy position) of the zero-loss peak (ZLP), and the final spectra used for plotting and area under the curve (AUC) computations were adjusted by the ZLP offset (File 1.5). Final spectra used for AUC computations and figures are included in Files 1.6 and 1.7. Energy region ratios were computed using integrated area, approximated by the “AUC” function (trapezoidal method) in the “DescTools” package for R (R Core Team, 2017; Signorell et al., 2019). Counts less than 0 were excluded for AUC estimation. Final AUC calculations are included in File 1.8. Set 2: Organo-mineral adjacent region (EELS) Filename(s): 2.1. 17_Mill3_320kx_ThinCArea_32usx1024fr_30mm_ADF.bin 2.2. AdjC_01_Point1_240eVshift_ThinC_Point_mono60_5sx1f_EELS_.dm3 2.3. AdjC_02_Point2_EELS_240eVshift_ThinC_Point2_mono40_8sx1f_EELS.dm3 2.4. AdjC_03_Point3_EELS_240eVshift_ThinC_mono40_10sx1f_EELS.dm3 2.5. Adjacent_EELS_C.csv 2.6. Adjacent_EELS_N.csv 2.7. Adjacent_AUC.csv 2.8. Metadata_AdjC_01_Point1_240eVshift_ThinC_Point_mono60_5sx1f_EELS.txt 2.9. Metadata_AdjC_02_Point2_EELS_240eVshift_ThinC_Point2_mono40_8sx1f_EELS.txt 2.10. Metadata_AdjC_03_Point3_EELS_240eVshift_ThinC_mono40_10sx1f_EELS.txt Data collection: Sample: Sample 1 (high mineral content sample, “wedge” thin-section): Data type: Electron energy loss point scans of region adjacent to mineral interface in Set 1. Approximate location shown in File 2.1 (annular dark field image, .bin file). Scale corrected by in-house instrument field of view calibration. Instrument: FEI F20 S/TEM instrument (FEI Company, Hillsboro, OR) Other information: NA Analysis: The overview .bin image file was imported into ImageJ (16-bit unsigned, 1024x1024 pixel, little-endian byte order). The .dm3 files (Files 2.2-2.4) were imported into ImageJ using the DM3 Reader tool included in the CSI package. The CSI Spectrum Analyzer was used to generate a background-subtracted dataset for the image using the linear combination of power laws (LCPL) fit and 3.0-pixel full-width half-maximum (FWHM) oversampling. The 260.0-277.0 eV background subtraction region was used for carbon. For nitrogen, the 378.8-390.8, 373.4-385.4, and 369.0-381.0 eV regions were used for Files 2.2, 2.3, and 2.4, respectively. AUC calculations were conducted as above (File 2.7). Set 3: Organo-mineral overview (EDX) Filename(s): 3.1. 18_Mill3_29kx_Overview_32usx1024fr_100mm_Spot5_Tilt30_HAADF.bin 3.2. Mill3_Al.tif 3.3. Mill3_C.tif 3.4. Mineral_Sample_EDX.csv Data collection: Sample: Sample 1 (high mineral content sample, “wedge” thin-section): Data type: Energy-dispersive X-ray spectroscopy elemental maps and average sum spectrum. Approximate location shown in File 3.1 (high-angle annular dark field image, .bin file). Scale corrected by in-house instrument field of view calibration. Instrument: FEI F20 S/TEM instrument (FEI Company, Hillsboro, OR) Other information: Oxford Instruments X-Max 80mm2 EDX detector (Oxford Instruments, Abingdon, Oxfordshire, UK) Analysis: The overview .bin image file was imported into ImageJ (16-bit unsigned, 1024x1024 pixel, little-endian byte order). A composite aluminum (Al, File 3.2) and carbon (C, File 3.3) elemental map was derived using the channel merge tool in ImageJ. The overview EDX spectrum (0.1-10 keV) (File 3.4) was normalized to the maximum intensity, and peaks were assigned using K-α edge energy positions.  Set 4: Organo-organic nitrogen map (EELS) Filename(s): 4.1. 15_Lamella after first EELS_12 deg tilt_10 kx_0-5 nA_50 um apert_130mm_12 us_1024.tif 4.2. Org-org_02_17_Overview_5 kx_0-5 nA_38 mm_CL_10 ms_94x111.dm3 4.3. Overview_Calibration.csv 4.4. N_integrated_scale_bar.txt 4.5. N_integrated_tif.tif 4.6. Org-org_Overview_EELS.csv 4.7. Metadata_Org-org_02_17_Overview_5 kx_0-5 nA_38 mm_CL_10 ms_94x111.txt Data collection: Sample: Sample 2 (high organic content, “lamella” thin-section): Data type: Electron energy loss 2-D maps of soil thin section (high organic matter content), focused on the approximate location shown in File 4.1 (.tif image). Instrument: FEI Titan Themis S/TEM instrument (FEI Company, Hillsboro, OR) Other information: NA Analysis: The EELS map (.dm3 file, File 4.2) was imported into ImageJ using the DM3 Reader tool included in the CSI package. Within the ROI (approximate location indicated in the manuscript), the CSI Spectrum Analyzer was used to generate a background-subtracted and integrated dataset for nitrogen (N) image using the linear combination of power laws (LCPL) fit and 3.0-pixel full-width half-maximum (FWHM) oversampling. The 369.8-388.8 eV background subtraction region and 395.0-430.0 eV integration region was used for N. Because the analysis is an approximate overview to show relatively coarse scale difference in N, the spectrum energy position was not adjusted. The scale bar was also estimated by converting the size of an ice crystal in File 4.1 to the size of the same ice crystal in File 4.2 (measurements in File 4.3). In addition to the N map, example EELS full spectra (not background subtracted) (File 4.6) were extracted from the EELS spectrum image (File 4.2) by selection of ROI in ImageJ and CSI. Set 5: Organo-organic features (EELS) Filename(s): 5.1. Org-org_04_19_28-5 kx_0-5 nA_38 mm_CL_10 ms_108x102_15-88 nm.dm3 5.2. Org-org_03_19_28-5 kx_0-5 nA_38 mm_LL_200 us_108x102_15-88 nm.dm3 5.3. Features-EELS-Components.csv 5.4. C fit MCR comp1.tif 5.5. C fit MCR comp2.tif 5.6. Metadata_Org-org_03_19_28-5 kx_0-5 nA_38 mm_LL_200 us_108x102_15-88 nm.txt 5.7. Metadata_Org-org_04_19_28-5 kx_0-5 nA_38 mm_CL_10 ms_108x102_15-88.txt Data collection: Sample: Sample 2 (high organic content, “lamella” thin-section): Data type: Electron energy loss 2-D maps of soil thin section (high organic matter content), focused on low N features in a high N matrix, approximate location shown in File 4.1 of Set 4 (.tif image). Instrument: FEI Titan Themis S/TEM instrument (FEI Company, Hillsboro, OR) Other information: NA Analysis: The EELS spectrum image (2-D map) (File 5.1) was statistically analyzed using a modified multivariate curve resolution (MCR) approach as described in Baek et al. (2016), Mundy et al. (2014) and Zachman et al. (2018). A corresponding low-loss EELS spectrum image (File 5.2) was used for energy shift correction as part of the MCR analysis (MCR code available on reasonable request to authors). The output includes two spectral components (File 5.3) and component spatial distribution maps (Files 5.4 and 5.5). The scale is based on pixel size as defined during data collection (15.88 nm). Set 6: Organo-organic interface MCR (EELS) Filename(s): 6.1. Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x735_0-9381 nm.dm3 6.2. Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x735_0-9381 nm.dm3 6.3. Interface-EELS-components-2comp.csv 6.4. Org-org_3components.csv 6.5. Interface C fitMCR comp1.tif 6.6. Interface C fitMCR comp2.tif 6.7. Interface C3 fitMCR comp1.tif 6.8. Interface C3 fitMCR comp2.tif 6.9. Interface C3 fitMCR comp3.tif 6.10. Org-org_3components_profile.csv 6.11. Metadata_Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x75_0-9381 nm.txt 6.12. Metadata_Org-org_06_25_320 kx_0-5 nA_38 mm_CL_20 ms_142x75_0-9381 nm.txt Data collection: Sample: Sample 2 (high organic content, “lamella” thin-section): Data type: Electron energy loss 2-D maps of soil thin section (high organic matter content), focused on interface between high N and low N organic forms. Instrument: FEI Titan Themis S/TEM instrument (FEI Company, Hillsboro, OR) Other information: NA Analysis: The EELS spectrum image (File 6.1) was analyzed using MCR as described above for Set 5. In this case, two and three component MCR approaches were tested, resulting in either two or three EELS components (Files 6.3 and 6.4). The change in component intensity across the interface was completed by measuring intensity line profiles (line selection tool across the interface) in ImageJ (File 6.10). Set 7: Organo-organic interface average boxes (EELS) Filename(s): 7.1. Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x735_0-9381 nm.dm3 7.2. Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x735_0-9381 nm.dm3 7.3. 25_320 kx_0-5 nA_38 mm_1ADF_142x75_0-9381 nm.dm3 7.4. Locations_Lateral.pdf 7.5. Locations_Vertical.pdf 7.6. C-12nm-1.csv 7.7. C-12nm-2.csv 7.8. C-12nm-3.csv 7.9. C-12nm-4.csv 7.10. C-12nm-5.csv 7.11. N-12nm-1.csv 7.12. N-12nm-2.csv 7.13. N-12nm-3.csv 7.14. N-12nm-4.csv 7.15. N-12nm-5.csv 7.16. O-12nm-1.csv 7.17. O-12nm-2.csv 7.18. O-12nm-3.csv 7.19. O-12nm-4.csv 7.20. O-12nm-5.csv 7.21. Interface_2pixel_C.csv 7.22. Interface_2pixel_N.csv 7.23. Interface_2pixel_O.csv 7.24. Vertical_Box_1.csv 7.25. Vertical_Box_1_N.csv 7.26. Vertical_Box_2.csv 7.27. Vertical_Box_2_N.csv 7.28. Vertical_Box_3.csv 7.29. Vertical_Box_3_N.csv 7.30. Organic_Interface_AUC.csv 7.31. Vertical_Box_AUC.csv 7.32. Org-org_interface_rate_change.csv 7.33. final_2nm_data.csv 7.34. Metadata_Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x75_0-9381 nm.txt 7.35. Metadata_Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x75_0-9381 nm.txt Data collection: Sample: Sample 2 (high organic content, “lamella” thin-section): Data type: Electron energy loss 2-D maps of soil thin section (high organic matter content), focused on interface between high N and low N organic forms. Instrument: FEI Titan Themis S/TEM instrument (FEI Company, Hillsboro, OR) Other information: NA Analysis: The EELS maps and ADF image (Files 7.1-7.3) were imported into ImageJ using the DM3 import tool in CSI. For the core-loss spectrum image (File 7.1), background subtraction was performed over the entire image using a linear combination of power laws (LCPL) function (3-pixel oversampling) using the regions 210.0 to 259.5 eV (C K-edge), 369.8 to 388.8 eV (N K-edge), 488.0 to 510.0 eV (O K-edge). For both the background-subtracted core loss and low-loss (File 7.2) images, the rectangle selection tool in ImageJ was used to extract box average spectra across the interface in either 12x45 or 2x45 pixel boxes rotated (from the box center) 15 degrees to the right. The box averages correspond with the approximate locations in File 7.4. In addition, three regions were selected in the vertical direction, with approximate locations shown in File 7.5. For each average core-loss spectrum (C, N, and O), the energy position was corrected based on the location of the zero-loss peak in the associated low-loss spectrum to generate corrected spectra (Files 7.6-7.29) used to estimate area under the curve (AUC) (Files 7.30-7.31) using methods described for Set 1 above. The 12x45 pixel box averages were used to calculate the percent change of rescaled C/N and aromatic/alkyl C ratios (based on AUC area) between boxes 1 and 2, 1 and 3, and 1 and 4, following the formula: (Box 1 – Box X)/Box 1 * 100 (File 7.32). Calculated AUC for 2x45 pixel boxes are included in File 7.33. Set 8: Organo-organic sample composition (EDX) Filename(s): 8.1. Organic_Sample_EDX.csv Data collection: Sample: Sample 2 (high organic content, “lamella” thin-section): Data type: Energy-dispersive X-ray spectroscopy point scan (collected near EELS analysis region) Instrument: FEI Strata 400 STEM DualBeam FIB (FEI Company, Hillsboro, OR) (operated at 5 kV) Other information: Oxford Instruments X-Max 80mm2 EDX detector (Oxford Instruments, Abingdon, Oxfordshire, UK). Analysis: The EDX spectrum was normalized to the maximum intensity, and peaks were assigned using K-α edge energy positions. Set 9: Damage test Filename(s): 9.1. Damage_01_17_Near grid bar_640 kx_3 nA_10 ms_0-1 eV_0 eV shift_100x100.dm3 9.2. Damage_02_19a_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.dm3 9.3. Damage_03_19b_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 9.4. Damage_04_19c_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 9.5. Damage_05_19d_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 9.6. Damage_06_19e_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 9.7. Damage_07_19f_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 9.8. Damage_08_19g_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 9.9. Damage_ZLP.csv 9.10. DamageTest_Spectra.csv 9.11. Damage_AUC.csv 9.12. Metadata_Damage_02_19a_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt 9.13. Metadata_Damage_03_19b_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt 9.14. Metadata_Damage_04_19c_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt 9.15. Metadata_Damage_05_19d_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt 9.16. Metadata_Damage_06_19e_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt 9.17. Metadata_Damage_07_19f_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt 9.18. Metadata_Damage_08_19g_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt 9.19 DamageTest_Dose.csv Data collection: Sample: Sample 3 (iron-organic synthetic co-precipitate) Data type: Electron energy loss data for carbon-iron co-precipitate used to estimate sample damage for carbon in Titan instrument. Instrument: FEI Titan Themis S/TEM instrument (FEI Company, Hillsboro, OR) Other information: Sequential files (Damage_02_19a to Damage_08_19g) are repeated measurements in the same region to determine the effect of continuous beam exposure. Analysis: The .dm3 files (Files 9.2-9.8) was imported into ImageJ using the DM3 Reader tool in the CSI package. The CSI Spectrum Analyzer was used to generate a background-subtracted dataset for the scan using the linear combination of power laws (LCPL) fit and 3.0-pixel full-width half-maximum (FWHM) oversampling. The 209.9-249.3 eV background subtraction region was used for carbon. The energy axis for each EELS spectrum was corrected for energy shift using a low-loss spectrum collected adjacent to the analysis region (File 9.1). The low-loss .dm3 file was imported into ImageJ using the CSI DM3 Reader tool and converted to a text file using the Spectrum Analyzer tool. The data were sorted by intensity (count) (highest to lowest) to determine offset (energy position) of the zero-loss peak (ZLP), and the final spectra used for plotting and area under the curve (AUC) computations were adjusted by the ZLP offset (File 9.9). Final spectra used for AUC computations and figures are included in File 9.10. Spectrum AUC calculations (File 9.11) were performed as described above for Set 1. Calculated dose for repeated measurements is included in File 9.19. References Baek, D. J. et al. Ultrathin epitaxial barrier layer to avoid thermally induced phase transformation in oxide heterostructures. ACS Appl. Mater. Interfaces 9, 54–59 (2016). Cueva, P., Hovden, R., Mundy, J. A., Xin, H. L. & Muller, D. A. Data processing for atomic resolution electron energy loss spectroscopy. Micros. Microanal. 18, 667–675 (2012). Mundy, J. A. et al. Visualizing the interfacial evolution from charge compensation to metallic screening across the manganite metal-insulator transition. Nature Commun. 5, 3464 (2014). R Core Team. R: A language and environment for statistical computing. R Foundation for Statistical Computing, Vienna, Austria. URL: https: //www.R-project.org/ (2019). Schneider, C. A., Rasband, W. S. & Eliceiri, K. W. NIH Image to ImageJ: 25 years of image analysis. Nature Methods 9(7): 671–675 (2012). Signorell, A. et al. DescTools: Tools for descriptive statistics. R package version 0.99.28 (2019). Zachman, M. J. et al. Cryo-STEM mapping of solid-liquid interfaces and dendrites in lithium-metal batteries. Nature 560, 345–349 (2018). Software- or Instrument-specific information needed to interpret the data, including software and hardware version numbers: ImageJ Version: 2.0.0-rc-65/1.51w Cornell Spectrum Imager Version: 1.6 Standards and calibration information, if appropriate: Environmental/experimental conditions: Describe any quality-assurance procedures performed on the data: People involved with sample collection, processing, analysis and/or submission: All authors, and in addition, Katherine E. Grant and Louis A. Derry (Cornell University Earth and Atmospheric Sciences) (soil sampling), John Grazul (Cornell Center for Materials Research, TEM and STEM), and Malcolm Thomas (Cornell Center for Materials Research, FIB). -------------------------- DATA-SPECIFIC INFORMATION -------------------------- #Set 1 Organo-mineral interface linescan (EELS)##################### 1.1. Filename: Linescan280nm.tif Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: TIF image showing location of EELS linescan at organo-mineral interface Number of variables: 1 (RGB value) Number of cases/rows: 495 x 417 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 1.2. Filename: Org-min_03_02_LinePEELS_240eVshift_mono60_5sx1fx10pts_280nmline_EELS_0001.emi Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: Metadata for EELS linescan at organo-mineral interface Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: Metadata associated with electron energy loss spectroscopy (EELS) linescan collected using TIA software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 1.3. Filename: Org-min_02_02_LinePEELS_240eVshift_mono60_5sx1fx10pts_280nmline_EELS_0001_1.ser Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: EELS data for linescan at organo-mineral interface Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS linescan collected using TIA software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 1.4. Filename: Org-min_01_Linescan_EnergyShift_Mill3_ZLP_1.27IMFP_Post1stCEdge_mono300_50mssx100fr_EELS.dm3 Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: Low-loss EELS measurement for energy shift correction of linescan Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS point scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 1.5. Filename: Org-min_ZLP.csv Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: Calculated energy shift for EELS linescan Number of variables: 4 Number of cases/rows: 2048 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy_eV Description: Electron energy loss (eV) for low-loss region Column 2: Counts Description: Electron energy loss intensity (counts) Column 3: Energy_sorted_eV Description: Electron energy loss (eV) sorted by maximum counts (column 4) Column 4: Counts_sorted Description: Electron energy loss intensity (counts) sorted by maximum Missing data codes: NA Specialized formats or other abbreviations used: NA # 1.6. Filename: Linescan_EELS_C.csv Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: EELS carbon K-edge spectra for linescan region Number of variables: 7 Number of cases/rows: 2048 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) for carbon K-edge Column 2: Energy_corrected Description: Electron energy loss (eV) corrected for energy shift Column 3: Point_A Description: Electron energy loss intensity (counts) for point A on linescan Column 4: Point_B Description: Electron energy loss intensity (counts) for point B on linescan Column 5: Point_C Description: Electron energy loss intensity (counts) for point C on linescan Column 6: Point_D Description: Electron energy loss intensity (counts) for point D on linescan Column 7: Point_E Description: Electron energy loss intensity (counts) for point E on linescan Missing data codes: Missing values indicated by "NA" Specialized formats or other abbreviations used: NA # 1.7. Filename: Linescan_EELS_N.csv Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: EELS nitrogen K-edge spectra for linescan region Number of variables: 7 Number of cases/rows: 2048 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) for carbon K-edge Column 2: Energy_corrected Description: Electron energy loss (eV) corrected for energy shift Column 3: Point_A Description: Electron energy loss intensity (counts) for point A on linescan Column 4: Point_B Description: Electron energy loss intensity (counts) for point B on linescan Column 5: Point_C Description: Electron energy loss intensity (counts) for point C on linescan Column 6: Point_D Description: Electron energy loss intensity (counts) for point D on linescan Column 7: Point_E Description: Electron energy loss intensity (counts) for point E on linescan Missing data codes: Missing values indicated by "NA" Specialized formats or other abbreviations used: NA # 1.8. Filename: Linescan_AUC.csv Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: Calculated area under the curve (AUC) estimates for linescan region Number of variables: 9 Number of cases/rows: 5 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: X Description: Rownames (positions on linescan, A-E) Column 2: TotalC Description: Total carbon integrated area (by area under the curve, AUC) Column 3: LowEC Description: Lower energy carbon integrated area (by area under the curve, AUC) Column 4: HighEC Description: Higher energy carbon integrated area (by area under the curve, AUC) Column 5: TotalN Description: Total nitrogen integrated area (by area under the curve, AUC) Column 6: CN Description: Ratio of total carbon and nitrogen AUC Column 7: high.norm Description: Higher energy carbon AUC normalized by maximum AUC value Column 8: low.norm Description: Lower energy carbon AUC normalized by maximum AUC value Column 9: high.low Description: Ratio of higher and lower energy carbon AUC Missing data codes: Missing values indicated by "NA" Specialized formats or other abbreviations used: NA # 1.9. Filename: Metadata_Org-min_01_Linescan_EnergyShift_Mill3_ZLP_1.27IMFP_Post1stCEdge_mono300_50mssx100fr_EELS.txt Directory: Set 1 Organo-mineral interface linescan (EELS) Brief Description: Metadata text file for zero-loss spectrum Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # #Set 2: Organo-mineral adjacent region (EELS) # 2.1. Filename: 17_Mill3_320kx_ThinCArea_32usx1024fr_30mm_ADF.bin Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Overview annular dark field image of analysis region Number of variables: 1 (greyscale value) Number of cases/rows: 1024 x 1024 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 2.2. Filename: AdjC_01_Point1_240eVshift_ThinC_Point_mono60_5sx1f_EELS_.dm3 Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Point EELS scan (1 of 3) of area adjacent to mineral interface Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS point scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 2.3. Filename: AdjC_02_Point2_EELS_240eVshift_ThinC_Point2_mono40_8sx1f_EELS.dm3 Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Point EELS scan (2 of 3) of area adjacent to mineral interface Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS point scan collected using DM3 (Digital Micrograph) software. See analysis sectiion for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 2.4. Filename: AdjC_03_Point3_EELS_240eVshift_ThinC_mono40_10sx1f_EELS.dm3 Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Point EELS scan (3 of 3) of area adjacent to mineral interface Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS point scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 2.5. Filename: Adjacent_EELS_C.csv Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Processed EELS spectra (carbon K-edge) for three points in area adjacent to mineral interface Number of variables: 4 Number of cases/rows: 2048 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) (carbon K-edge) Column 2: Point_1 Description: Electron energy loss intensity (counts) for point 1 of 3 Column 3: Point_2 Description: Electron energy loss intensity (counts) for point 2 of 3 Column 4: Point_3 Description: Electron energy loss intensity (counts) for point 3 of 3 Missing data codes: Missing values indicated by "NA" Specialized formats or other abbreviations used: NA # 2.6. Filename: Adjacent_EELS_N.csv Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Processed EELS spectra (nitrogen K-edge) for three points in area adjacent to mineral interface Number of variables: 4 Number of cases/rows: 2048 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) (nitrogen K-edge) Column 1: Point_1 Description: Electron energy loss intensity (counts) for point 1 of 3 Column 1: Point_2 Description: Electron energy loss intensity (counts) for point 2 of 3 Column 1: Point_3 Description: Electron energy loss intensity (counts) for point 3 of 3 Missing data codes: Missing values indicated by "NA" Specialized formats or other abbreviations used: # 2.7. Filename: Adjacent_AUC.csv Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Calculated area under the curve for EELS data in adjacent region Number of variables: 9 Number of cases/rows: 5 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: X Description: Rownames (positions on linescan, A-E) Column 2: TotalC Description: Total carbon integrated area (by area under the curve, AUC) Column 3: LowEC Description: Lower energy carbon integrated area (by area under the curve, AUC) Column 4: HighEC Description: Higher energy carbon integrated area (by area under the curve, AUC) Column 5: TotalN Description: Total nitrogen integrated area (by area under the curve, AUC) Column 6: CN Description: Ratio of total carbon and nitrogen AUC Column 7: high.norm Description: Higher energy carbon AUC normalized by maximum AUC value Column 8: low.norm Description: Lower energy carbon AUC normalized by maximum AUC value Column 9: high.low Description: Ratio of higher and lower energy carbon AUC Missing data codes: Missing values indicated by "NA" Specialized formats or other abbreviations used: NA # 2.8. Filename: Metadata_AdjC_01_Point1_240eVshift_ThinC_Point_mono60_5sx1f_EELS.txt Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Metadata text file for Point 1 spectrum (2.2) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 2.9. Filename: Metadata_AdjC_02_Point2_EELS_240eVshift_ThinC_Point2_mono40_8sx1f_EELS.txt Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Metadata text file for Point 2 spectrum (2.3) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 2.10. Filename: Metadata_AdjC_03_Point3_EELS_240eVshift_ThinC_mono40_10sx1f_EELS.txt Directory: Set 2 Organo-mineral adjacent region (EELS) Brief Description: Metadata text file for Point 3 spectrum (2.4) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # #Set 3 Organo-mineral overview (EDX)###################### # 3.1. Filename: 18_Mill3_29kx_Overview_32usx1024fr_100mm_Spot5_Tilt30_HAADF.bin Directory: Set 3 Organo-mineral overview (EDX) Brief Description: STEM HAADF image of analysis region in Set 3 Number of variables: 1 (greyscale value) Number of cases/rows: 1024 x 1024 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 3.2. Filename: Mill3_Al.tif Directory: Set 3 Organo-mineral overview (EDX) Brief Description: EDX aluminum elemental map Number of variables: 1 (greyscale value) Number of cases/rows: 128 x 128 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 3.3. Filename: Mill3_C.tif Directory: Set 3 Organo-mineral overview (EDX) Brief Description: EDX carbon elemental map Number of variables: 1 (greyscale value) Number of cases/rows: 128 x 128 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 3.4. Filename: Mineral_Sample_EDX.csv Directory: Set 3 Organo-mineral overview (EDX) Brief Description: Sum EDX spectrum of analysis area Number of variables: 3 Number of cases/rows: 1003 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: X-ray energy (keV) Column 2: Counts Description: Intensity (counts) Column 3: NormCounts Description: Normalized intensity (divided by maximum) (arbitrary units) Missing data codes: Missing values indicated by "NA" Specialized formats or other abbreviations used: NA # #Set 4 Organo-organic nitrogen map (EELS)######################### 4.1. Filename: 15_Lamella after first EELS_12 deg tilt_10 kx_0-5 nA_50 um apert_130mm_12 us_1024.tif Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: STEM image showing overview of location for EELS in Set 4 Number of variables: 1 (greyscale intensity) Number of cases/rows: 1024 x 1059 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 4.2. Filename: Org-org_02_17_Overview_5 kx_0-5 nA_38 mm_CL_10 ms_94x111.dm3 Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: EELS core-loss spectrum image (overview) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS map collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 4.3. Filename: Overview_Calibration.csv Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Measurements used to calibrate scale bar in 4.2 and 4.4 Number of variables: 6 Number of cases/rows: 6 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Feature Description: Feature used to estimate scale from known size in TIF image (factors, levels = Ice_crystal, Scale_bar, Pixel) Column 2: Pixel Description: Measured or calculated pixel size of feature (column 1) Column 3: Length_nm Description: Measured or calculated size of feature (column 1) in nanometers Column 4: Length_um Description: Measured or calculated size of feature (column 1) in micrometers Column 5: Image Description: Identity of image type, either TIF (tagged image file) or CoreLoss (EELS core loss map) Column 6: File Description: File in Set 4 (File1 or File2) Missing data codes: NA Specialized formats or other abbreviations used: NA # 4.4. Filename: N_integrated_scale_bar.txt Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Integrated nitrogen (N) K-edge intensity values for region of interest in 4.2 (text image) Number of variables: 1 (greyscale intensity) Number of cases/rows: 43 x 62 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 4.5. Filename: N_integrated_tif.tif Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Greyscale image of 4.4 Number of variables: 1 (RGB value) Number of cases/rows: 43 x 62 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 4.6. Filename: Org-org_Overview_EELS.csv Directory: Set 4 Organo-organic nitrogen map (EELS) Brief Description: Example EELS spectra from higher and lower N regions of in 4.2 Number of variables: 3 Number of cases/rows: 2048 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) Column 2: R1_LowN Description: Electron energy loss intensity (counts) for area of 4.2 lower in nitrogen Column 3: R2_HighN Description: Electron energy loss intensity (counts) for area of 4.2 higher in nitrogen Missing data codes: Specialized formats or other abbreviations used: # 4.7. Filename: Metadata_Org-org_02_17_Overview_5 kx_0-5 nA_38 mm_CL_10 ms_94x111.txt Directory: Set 4 Brief Description: Metatdata text file for overview EELS map (4.2) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # #Set 5 Organo-organic features (EELS)############################ # 5.1. Filename: Org-org_04_19_28-5 kx_0-5 nA_38 mm_CL_10 ms_108x102_15-88 nm.dm3 Directory: Set 5 Organo-organic features (EELS) Brief Description: EELS core-loss spectrum image (high N features, 15.88 nm pixel) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS map collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 5.2. Filename: Org-org_03_19_28-5 kx_0-5 nA_38 mm_LL_200 us_108x102_15-88 nm.dm3 Directory: Set 5 Organo-organic features (EELS) Brief Description: EELS low-loss spectrum image associated with 5.1 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS map collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 5.3. Filename: Features-EELS-Components.csv Directory: Set 5 Organo-organic features (EELS) Brief Description: MCR output component spectra (carbon) associated with 5.1 Number of variables: 3 Number of cases/rows: 65 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) Column 2: C1 Description: Electron energy loss intensity (counts) for component 1 Column 3: C2 Description: Electron energy loss intensity (counts) for component 2 Missing data codes: NA Specialized formats or other abbreviations used: NA # 5.4. Filename: C fit MCR comp1.tif Directory: Set 5 Organo-organic features (EELS) Brief Description: MCR output component #1 map associated with 5.1 Number of variables: 1 (greyscale intensity) Number of cases/rows: 108 x 102 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 5.5. Filename: C fit MCR comp2.tif Directory: Set 5 Organo-organic features (EELS) Brief Description: MCR output component #2 map associated with 5.1 Number of variables: 1 (greyscale intensity) Number of cases/rows: 108 x 102 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 5.6. Filename: Metadata_Org-org_03_19_28-5 kx_0-5 nA_38 mm_LL_200 us_108x102_15-88 nm.txt Directory: Set 5 Organo-organic features (EELS) Brief Description: Metadata for low-loss EELS map (5.2) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 5.7. Filename: Metadata_Org-org_04_19_28-5 kx_0-5 nA_38 mm_CL_10 ms_108x102_15-88.txt Directory: Set 5 Organo-organic features (EELS) Brief Description: Metadata for EELS core-loss map (5.1) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # #Set 6 Organo-organic interface MCR (EELS)######################## # 6.1. Filename: Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x735_0-9381 nm.dm3 Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: EELS core-loss spectrum image (organo-organic interface, 0.9381 nm pixel) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS map collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 6.2. Filename: Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x735_0-9381 nm.dm3 Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: EELS low-loss spectrum image associated with 6.1 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS map collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 6.3. Filename: Interface-EELS-components-2comp.csv Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (2-component) output component spectra (carbon) associated with 6.1 Number of variables: 3 Number of cases/rows: 65 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) Column 2: C1 Description: Electron energy loss intensity (counts) for component 1 Column 3: C2 Description: Electron energy loss intensity (counts) for component 2 Missing data codes: NA Specialized formats or other abbreviations used: NA # 6.4. Filename: Org-org_3components.csv Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (3-component) output component spectra (carbon) associated with 6.1 Number of variables: 4 Number of cases/rows: 65 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) Column 2: C1 Description: Electron energy loss intensity (counts) for component 1 Column 3: C2 Description: Electron energy loss intensity (counts) for component 2 Column 4: C3 Description: Electron energy loss intensity (counts) for component 3 Missing data codes: Specialized formats or other abbreviations used: # 6.5. Filename: Interface C fitMCR comp1.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (2-component) component #1 map associated with 6.1 Number of variables: 1 (greyscale intensity) Number of cases/rows: 142 x 75 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 6.6. Filename: Interface C fitMCR comp2.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (2-component) component #2 map associated with 6.1 Number of variables: 1 (greyscale intensity) Number of cases/rows: 142 x 75 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 6.7. Filename: Interface C3 fitMCR comp1.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (3-component) component #1 map associated with 6.1 Number of variables: 1 (greyscale intensity) Number of cases/rows: 142 x 75 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 6.8. Filename: Interface C3 fitMCR comp2.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (3-component) component #2 map associated with 6.1 Number of variables: 1 (greyscale intensity) Number of cases/rows: 142 x 75 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 6.9. Filename: Interface C3 fitMCR comp3.tif Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: MCR (3-component) component #3 map associated with 6.1 Number of variables: 1 (greyscale intensity) Number of cases/rows: 142 x 75 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 6.10. Filename: Org-org_3components_profile.csv Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: Distribution of MCR component pixel intensity across image (line profile) (3-component MCR) Number of variables: 4 Number of cases/rows: 142 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Pixel Description: Position on line profile (pixel number) Column 2: C3_profile Description: Pixel intensity on line profile (counts) for component 3 Column 3: C2_profile Description: Pixel intensity on line profile (counts) for component 2 Column 4: C1_profile Description: Pixel intensity on line profile (counts) for component 1 Missing data codes: NA Specialized formats or other abbreviations used: NA # 6.11. Filename: Metadata_Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x75_0-9381 nm.txt Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: Metadata text file for low-loss EELS map (6.2) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 6.12. Filename: Metadata_Org-org_06_25_320 kx_0-5 nA_38 mm_CL_20 ms_142x75_0-9381 nm.txt Directory: Set 6 Organo-organic interface MCR (EELS) Brief Description: Metadata text file for core-loss EELS map (6.1) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # #Set 7 Organo-organic interface average boxes (EELS)################### # 7.1. Filename: Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x735_0-9381 nm.dm3 ###Same file as 6.1#### Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: EELS core-loss spectrum image (organo-organic interface, 0.9381 nm pixel) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS map collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 7.2. Filename: Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x735_0-9381 nm.dm3 ###Same file as 6.2####: Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: EELS low-loss spectrum image associated with 6.1 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS map collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 7.3. Filename: 25_320 kx_0-5 nA_38 mm_ADF_142x75_0-9381 nm.dm3 Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: ADF image showing analysis area in 7.1 and 7.2 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS map collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 7.4. Filename: Locations_Lateral.jpg Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Locations for EELS average boxes across the organo-organic interface (.jpg image) Number of variables: 1 (greyscale intensity) Number of cases/rows: 508 x 341 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.5. Filename: Locations_Vertical.jpg Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Locations of EELS average boxes along the organo-organic interface in the vertical direction (.jpg image) Number of variables: 1 (RGB value) Number of cases/rows: 328 x 268 pixels Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.6. Filename: C-12nm-1.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 1 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: C-1-36 Description: Electron energy loss intensity (counts) for Box 1 (in 7.4), 36 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.7. Filename: C-12nm-2.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 2 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: C-2-24 Description: Electron energy loss intensity (counts) for Box 2 (in 7.4), 24 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.8. Filename: C-12nm-3.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 3 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: C-3-12 Description: Electron energy loss intensity (counts) for Box 3 (in 7.4), 12 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.9. Filename: C-12nm-4.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 4 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: C-4-center Description: Electron energy loss intensity (counts) for Box 4 (in 7.4) Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.10. Filename: C-12nm-5.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for Box 5 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: C.5.12 Description: Electron energy loss intensity (counts) for Box 5 (in 7.4), 12 pixels to right of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.11. Filename: N-12nm-1.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 1 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: N-1-36 Description: Electron energy loss intensity (counts) for Box 1 (in 7.4), 36 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.12. Filename: N-12nm-2.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 2 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: N-2-24 Description: Electron energy loss intensity (counts) for Box 2 (in 7.4), 24 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.13. Filename: N-12nm-3.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 3 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: N-3-12 Description: Electron energy loss intensity (counts) for Box 3 (in 7.4), 12 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.14. Filename: N-12nm-4.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 4 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: N-4-center Description: Electron energy loss intensity (counts) for Box 4 (in 7.4) Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.15. Filename: N-12nm-5.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for Box 5 in 7.4 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: N-5+12 Description: Electron energy loss intensity (counts) for Box 5 (in 7.4), 12 pixels to right of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.16. Filename: O-12nm-1.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 1 in 7.4 Number of variables: 2 Number of cases/rows: 401 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: O-1-36 Description: Electron energy loss intensity (counts) for Box 1 (in 7.4), 36 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.17. Filename: O-12nm-2.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 2 in 7.4 Number of variables: 2 Number of cases/rows: 401 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: O-2-24 Description: Electron energy loss intensity (counts) for Box 2 (in 7.4), 24 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.18. Filename: O-12nm-3.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 3 in 7.4 Number of variables: 2 Number of cases/rows: 401 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: O-3-12 Description: Electron energy loss intensity (counts) for Box 3 (in 7.4), 12 pixels to left of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.19. Filename: O-12nm-4.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 4 in 7.4 Number of variables: 2 Number of cases/rows: 401 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: O-4-center Description: Electron energy loss intensity (counts) for Box 4 (in 7.4) Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.20. Filename: O-12nm-5.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for Box 5 in 7.4 Number of variables: 2 Number of cases/rows: 401 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CorrectedEEL Description: Electron energy loss (eV) Column 2: O-5+12 Description: Electron energy loss intensity (counts) for Box 5 (in 7.4), 12 pixels to right of box 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.21. Filename: Interface_2pixel_C.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for regions a through l in 7.4 Number of variables: 13 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy_C Description: Electron energy loss (eV) for carbon K-edge Column 2: Counts_C_a Description: Electron energy loss intensity (counts) for position a in 7.4 Column 3: Counts_C_b Description: Electron energy loss intensity (counts) for position b in 7.4 Column 4: Counts_C_c Description: Electron energy loss intensity (counts) for position c in 7.4 Column 5: Counts_C_d Description: Electron energy loss intensity (counts) for position d in 7.4 Column 6: Counts_C_e Description: Electron energy loss intensity (counts) for position e in 7.4 Column 7: Counts_C_f Description: Electron energy loss intensity (counts) for position f in 7.4 Column 8: Counts_C_g Description: Electron energy loss intensity (counts) for position g in 7.4 Column 9: Counts_C_h Description: Electron energy loss intensity (counts) for position h in 7.4 Column 10: Counts_C_i Description: Electron energy loss intensity (counts) for position i in 7.4 Column 11: Counts_C_j Description: Electron energy loss intensity (counts) for position j in 7.4 Column 12: Counts_C_k Description: Electron energy loss intensity (counts) for position k in 7.4 Column 13: Counts_C_l Description: Electron energy loss intensity (counts) for position l in 7.4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.22. Filename: Interface_2pixel_N.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for regions a through l in 7.4 Number of variables: 13 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy_N Description: Electron energy loss (eV) for nitrogen K-edge Column 2: Counts_N_a Description: Electron energy loss intensity (counts) for position a in 7.4 Column 3: Counts_N_b Description: Electron energy loss intensity (counts) for position b in 7.4 Column 4: Counts_N_c Description: Electron energy loss intensity (counts) for position c in 7.4 Column 5: Counts_N_d Description: Electron energy loss intensity (counts) for position d in 7.4 Column 6: Counts_N_e Description: Electron energy loss intensity (counts) for position e in 7.4 Column 7: Counts_N_f Description: Electron energy loss intensity (counts) for position f in 7.4 Column 8: Counts_N_g Description: Electron energy loss intensity (counts) for position g in 7.4 Column 9: Counts_N_h Description: Electron energy loss intensity (counts) for position h in 7.4 Column 10: Counts_N_i Description: Electron energy loss intensity (counts) for position i in 7.4 Column 11: Counts_N_j Description: Electron energy loss intensity (counts) for position j in 7.4 Column 12: Counts_N_k Description: Electron energy loss intensity (counts) for position k in 7.4 Column 13: Counts_N_l Description: Electron energy loss intensity (counts) for position l in 7.4 Missing data codes: Specialized formats or other abbreviations used: # 7.23. Filename: Interface_2pixel_O.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected oxygen K-edge EELS for regions a through l in 7.4 Number of variables: 13 Number of cases/rows: 401 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy_N Description: Electron energy loss (eV) for nitrogen K-edge Column 2: Counts_O_a Description: Electron energy loss intensity (counts) for position a in 7.4 Column 3: Counts_O_b Description: Electron energy loss intensity (counts) for position b in 7.4 Column 4: Counts_O_c Description: Electron energy loss intensity (counts) for position c in 7.4 Column 5: Counts_O_d Description: Electron energy loss intensity (counts) for position d in 7.4 Column 6: Counts_O_e Description: Electron energy loss intensity (counts) for position e in 7.4 Column 7: Counts_O_f Description: Electron energy loss intensity (counts) for position f in 7.4 Column 8: Counts_O_g Description: Electron energy loss intensity (counts) for position g in 7.4 Column 9: Counts_O_h Description: Electron energy loss intensity (counts) for position h in 7.4 Column 10: Counts_O_i Description: Electron energy loss intensity (counts) for position i in 7.4 Column 11: Counts_O_j Description: Electron energy loss intensity (counts) for position j in 7.4 Column 12: Counts_O_k Description: Electron energy loss intensity (counts) for position k in 7.4 Column 13: Counts_O_l Description: Electron energy loss intensity (counts) for position l in 7.4 Missing data codes: Specialized formats or other abbreviations used: # 7.24. Filename: Vertical_Box_1.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for region x in 7.5 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: EEL Description: Electron energy loss (eV) Column 2: C1 Description: Carbon electron energy loss intensity (counts) for region x Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.25. Filename: Vertical_Box_1_N.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for region x in 7.5 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: EEL Description: Electron energy loss (eV) Column 2: N1 Description: Nitrogen electron energy loss intensity (counts) for region x Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.26. Filename: Vertical_Box_2.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for region y in 7.5 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: EEL Description: Electron energy loss (eV) Column 2: C2 Description: Carbon electron energy loss intensity (counts) for region y Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.27. Filename: Vertical_Box_2_N.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for region y in 7.5 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: EEL Description: Electron energy loss (eV) Column 2: N2 Description: Nitrogen electron energy loss intensity (counts) for region y Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.28. Filename: Vertical_Box_3.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected carbon K-edge EELS for region z in 7.5 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: EEL Description: Electron energy loss (eV) Column 2: C3 Description: Carbon electron energy loss intensity (counts) for region z Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.29. Filename: Vertical_Box_3_N.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Corrected nitrogen K-edge EELS for region z in 7.5 Number of variables: 2 Number of cases/rows: 221 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: EEL Description: Electron energy loss (eV) Column 2: N3 Description: Nitrogen electron energy loss intensity (counts) for region z Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.30. Filename: Organic_Interface_AUC.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Estimated AUC for carbon, nitrogen, oxygen, and carbon fine structure across organo-organic interface in 7.4 Number of variables: 19 Number of cases/rows: 5 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: X Description: Analysis region (Box 1-5) Column 2: Distance Description: Distance across interface in nanometers Column 3: TotalC Description: Estimated total carbon intensity by area under the curve Column 4: AromaticC Description: Estimated total aromatic carbon intensity by area under the curve Column 5: AlkylC Description: Estimated total alkyl carbon intensity by area under the curve Column 6: TotalN Description: Estimated total nitrogen intensity by area under the curve Column 7: TotalO Description: Estimated total oxygen intensity by area under the curve Column 8: CN Description: Ratio of carbon to nitrogen intensity Column 9: NormArom Description: Aromatic carbon normalized to total carbon Column 10: NormAlkyl Description: Alkyl carbon normalized to total carbon Column 11: AromAlkyl Description: Aromatic/alkyl carbon ratio Column 12: CO Description: Carbon/oxygen ratio Column 13: NormCN Description: Normalized carbon/nitrogen ratio (to maximum) Column 14: NormAromAlkyl Description: Normalized aromatic/alkyl ratio (to maximum) Column 15: NormCO Description: Normalized carbon/oxygen ratio (to maximum) Column 16: NormCNrescale Description: Normalized carbon/nitrogen ratio, rescaled to 0 to 1 Column 17: NormAromAlkylrescale Description: Normalized aromatic/alkyl ratio, rescaled to 0 to 1 Column 18: CN_percent_change Description: Percent change in carbon/nitrogen ratio between boxes 1 and 2, 1 and 3, and 1 and 4 Column 19: AromAlkyl_percent_change Description: Percent change in aromatic/alkyl ratio between boxes 1 and 2, 1 and 3, and 1 and 4 Missing data codes: NA Specialized formats or other abbreviations used: NA # 7.31. Vertical_Box_AUC.csv: Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Estimated AUC for carbon, nitrogen, and carbon fine structure across vertical boxes in 7.5 Number of variables: 12 Number of cases/rows: 3 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: X Description: Analysis region (Box X-Z) Column 2: Distance Description: Distance along interface in nanometers Column 3: TotalC Description: Estimated total carbon intensity by area under the curve Column 4: AromaticC Description: Estimated total aromatic carbon intensity by area under the curve Column 5: AlkylC Description: Estimated total alkyl carbon intensity by area under the curve Column 6: TotalN Description: Estimated total nitrogen intensity by area under the curve Column 7: CN Description: Ratio of carbon to nitrogen intensity Column 8: NormArom Description: Aromatic carbon normalized to total carbon Column 9: NormAlkyl Description: Alkyl carbon normalized to total carbon Column 10: AromAlkyl Description: Aromatic/alkyl carbon ratio Column 11: NormCN Description: Normalized carbon/nitrogen ratio (to maximum) Column 12: NormAromAlkyl Description: Normalized aromatic/alkyl ratio (to maximum) Missing data codes: Specialized formats or other abbreviations used: # 7.32. Filename: Org-org_interface_rate_change.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Calculated rate of change of ratios across interface Number of variables: 4 Number of cases/rows: 5 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: CN Description: Rescaled (0 to 1) change in C/N ratio across interface (unitless) Column 2: AromAlkyl Description: Rescaled (0 to 1) change in aromatic/alkyl ratio across interface (unitless) Column 3: CN_percent Description: Percent change in C/N across locations (%) Column 4: AromAlkyl_percent Description: Percent change in atomatic/alkyl across locations (%) Missing data codes: Not applicable rows labeled with "NA" Specialized formats or other abbreviations used: NA # 7.33. Filename: final_2nm_data.csv Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Estimated area under the curve and ratios for high-resolution organo-organic interface Number of variables: 13 Number of cases/rows: 14 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: X Description: Position (a through l) Column 2: Distance Description: Lateral distance across interface (nm) Column 3: DEF_aromalkyl Description: Aromatic/alkyl ratio for boxes 2, 3, 4, center corresponding to 6, 11, and 17 in Supplementary Figure 5 Column 4: DEF_CO Description: Carbon/oxygen ratio for boxes 2, 3, 4 (center corresponding to 6, 11, and 17 in Supplementary Figure 5) Column 5: DEF_CN Description: Carbon/nitrogen ratio for boxes 2, 3, 4 (center corresponding to 6, 11, and 17 in Supplementary Figure 5) Column 6: CN Description: Carbon/nitrogen ratio for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 7: CO Description: Carbon/oxygen ratio for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 8: TotalC Description: Total carbon for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 9: LowC Description: Lower-energy carbon for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 10: HighC Description: Higher-energy carbon for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 11: TotalN Description: Total nitrogen for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 12: TotalO Description: Total oxygen for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 13: arom.norm Description: Normalized lower-energy carbon for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 14: alkyl.norm Description: Normalized higher-energy carbon for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Column 15: arom.alkyl Description: Normalized atomatic/alkyl ratio for 2x44 nm boxes across interface (1 - 17 in Supplementary Figure 5) Missing data codes: Not applicable data noted with "NA" Specialized formats or other abbreviations used: NA # 7.34. Filename: Metadata_Org-org_05_25_320 kx_0-5 nA_38 mm_LL_200 us_142x75_0-9381 nm.txt Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Metadata for low-loss EELS map (7.2) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 7.35. Filename: Metadata_Org-org_06_25_320 kx_0-5 nA_38 mm_CL_10 ms_142x75_0-9381 nm.txt Directory: Set 7 Organo-organic interface average boxes (EELS) Brief Description: Metadata for core-loss EELS map (7.1) Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # #Set 8 Organo-organic sample composition (EDX)################## 8.1. Filename: Organic_Sample_EDX.csv Directory: Set 8 Organo-organic sample composition (EDX) Brief Description: Point scan EDX sum spectrum for sample analyzed in Sets 4-7 Number of variables: 3 Number of cases/rows: 2008 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: X-ray energy (keV) Column 2: Counts Description: Intensity (counts) Column 3: NormCounts Description: Normalized intensity (divided by maximum), arbitrary units Missing data codes: NA Specialized formats or other abbreviations used: NA # #Set 9 Damage test (EELS)########################################## 9.1. Filename: Damage_01_17_Near grid bar_640 kx_3 nA_10 ms_0-1 eV_0 eV shift_100x100.dm3 Directory: Set 9 Damage test (EELS) Brief Description: EELS low-loss measurement for 9.2-9.8 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS field of view scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 9.2. Filename: Damage_02_19a_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.dm3 Directory: Set 9 Damage test (EELS) Brief Description: EELS core-loss measurement (12 seconds total exposure) for damage test Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS field of view scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 9.3. Filename: Damage_03_19b_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test (EELS) Brief Description: EELS core-loss measurement (24 seconds total exposure) for damage test Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS field of view scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 9.4. Filename: Damage_04_19c_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test (EELS) Brief Description: EELS core-loss measurement (36 seconds total exposure) for damage test Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS field of view scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 9.5. Filename: Damage_05_19d_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test (EELS) Brief Description: EELS core-loss measurement (48 seconds total exposure) for damage test Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS field of view scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 9.6. Filename: Damage_06_19e_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test (EELS) Brief Description: EELS core-loss measurement (60 seconds total exposure) for damage test Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS field of view scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 9.7. Filename: Damage_07_19f_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test (EELS) Brief Description: EELS core-loss measurement (72 seconds total exposure) for damage test Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS field of view scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 9.8. Filename: Damage_08_19g_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_ 200 eV shift.dm3 Directory: Set 9 Damage test (EELS) Brief Description: EELS core-loss measurement (84 seconds total exposure) for damage test Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: EELS field of view scan collected using DM3 (Digital Micrograph) software. See analysis section for information on utilizing this file in ImageJ and the Cornell Spectrum Imager software. # 9.9. Filename: Damage_ZLP.csv Directory: Set 9 Damage test (EELS) Brief Description: Zero-loss peak position for energy offset in 9.10 Number of variables: 4 Number of cases/rows: 2048 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy_eV Description: Electron energy loss (eV) for low-loss region Column 2: Counts Description: Electron energy loss intensity (counts) Column 3: Energy_sorted_eV Description: Electron energy loss (eV), sorted by maximum count (column 4) Column 4: Counts_sorted Description: Electron energy loss intensity (counts), sorted by maximum intensity Missing data codes: NA Specialized formats or other abbreviations used: NA # 9.10. Filename: DamageTest_Spectra.csv Directory: Set 9 Damage test (EELS) Brief Description: Corrected EELS carbon K-edge spectra from files 9.2-9.8 Number of variables: 8 Number of cases/rows: 551 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Energy Description: Electron energy loss (eV) Column 2: T1 Description: Electron energy loss intensity (counts), for time = 1 (12 s exposure) Column 3: T2 Description: Electron energy loss intensity (counts), for time = 1 (24 s exposure) Column 4: T3 Description: Electron energy loss intensity (counts), for time = 1 (36 s exposure) Column 5: T4 Description: Electron energy loss intensity (counts), for time = 1 (48 s exposure) Column 6: T5 Description: Electron energy loss intensity (counts), for time = 1 (60 s exposure) Column 7: T6 Description: Electron energy loss intensity (counts), for time = 1 (72 s exposure) Column 8: T7 Description: Electron energy loss intensity (counts), for time = 1 (84 s exposure) Missing data codes: NA Specialized formats or other abbreviations used: NA # 9.11. Filename: Damage_AUC.csv Directory: Set 9 Damage test (EELS) Brief Description: Estimations of AUC for carbon and carbon fine structure in damage test spectra (file 9.10) Number of variables: 11 Number of cases/rows: 7 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: X Description: Measurement time, T1-T7 Column 2: Time Description: Exposure time (seconds) Column 3: Dose Description: Calculated dose (electrons per square angstrom) Column 4: TotalC Description: Estimated total carbon signal (area under the curve) Column 5: AromaticC Description: Estimated aromatic carbon signal (area under the curve) Column 6: AlkylC Description: Estimated alkyl carbon signal (area under the curve) Column 7: NormArom Description: Aromatic carbon normalized to total carbon Column 8: NormAlkyl Description: Alkyl carbon normalized to total carbon Column 9: AromAlkyl Description: Aromatic/alkyl carbon ratio Column 10: NormAromAlkyl Description: Aromatic/alkyl carbon ratio normalized to total carbon Column 11: NormTotalC Description: Normalized total carbon (to maximum total carbon) Missing data codes: NA Specialized formats or other abbreviations used: NA # 9.12. Filename: Metadata_Damage_02_19a_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test (EELS) Brief Description: Metadata text file for damage test 9.2 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 9.13. Filename: Metadata_Damage_03_19b_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test (EELS) Brief Description: Metadata text file for damage test 9.3 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 9.14. Filename: Metadata_Damage_04_19c_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test (EELS) Brief Description: Metadata text file for damage test 9.4 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 9.15. Filename: Metadata_Damage_05_19d_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txtage_AUC.csv Directory: Set 9 Damage test (EELS) Brief Description: Metadata text file for damage test 9.5 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 9.16. Filename: Metadata_Damage_06_19e_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test (EELS) Brief Description: Metadata text file for damage test 9.6 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 9.17. Filename: Metadata_Damage_07_19f_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test (EELS) Brief Description: Metadata text file for damage test 9.7 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 9.18. Filename: Metadata_Damage_08_19g_Near grid bar_640 kx_3-2 nA_10 s_0-1 eV_200 eV shift.txt Directory: Set 9 Damage test (EELS) Brief Description: Metadata text file for damage test 9.8 Number of variables: NA Number of cases/rows: NA Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: NA Description: NA Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) # 9.19. Filename: DamageTest_Dose.csv Directory: Set 9 Damage test (EELS) Brief Description: Calculated dose for damage test series Number of variables: 2 Number of cases/rows: 7 Variable list, defining any abbreviations, units of measure, codes or symbols used: Column 1: Time_s Description: Exposure time (seconds) Column 2: Dose Description: Calculated dose (electrons per square angstrom) Missing data codes: NA Specialized formats or other abbreviations used: NA (text file) #