Andrea K. Tokranov Sydney M. Welch Leah M. Santangelo Douglas B. Kent Deborah A. Repert Kimberlie Perkins Paul A. Bliznik David A. Roth Anthony F. Drouin Tricia A. Lincoln Noel A. Deyette Kate Emma A. Schlosser Jeffrey M. Marts 20230209 spreadsheet https://doi.org/10.5066/P9TKSM8S Data from a laboratory study undertaken at the U.S. Geological Survey to investigate solid/water partitioning of per- and polyfluoroalkyl substances (PFAS) in New Hampshire soils and biosolids are presented here. Soils and biosolids used for the experiments were collected using PFAS-free sampling equipment, air dried, gently homogenized, and sieved (soils only). Soil samples were collected from locations with known PFAS contamination (n = 5) and nearby sites with similar soil characteristics but low expected PFAS concentrations (n = 4). Finished biosolids were collected directly from facilities at the final stage of processing and before distribution. Air-dried soils and biosolids were then used for a series of batch and column experiments to determine water/solid distribution coefficient (Kd) values. This study investigated the impact of pH, ionic strength, adsorption versus desorption, soil/biosolid type, experimental setup (batch versus column), and influence of sodium azide on Kd values. All batch and column experiments were run for 10 days as determined by a 16-day kinetics test. The dataset presented here includes concentration of PFAS, concentration of PFAS post total oxidizable precursor assay (TOPA), pH, moisture content, total organic carbon concentrations, aluminum concentrations, iron concentrations, sodium concentrations, cation exchange capacity, anion exchange capacity, grain size, and protein concentrations for the unprocessed soil and biosolids collected from the site (soils) or facility (biosolids). These are denoted as "Environmental - Biosolid" or "Environmental - Soil" samples in the data release. The dataset also includes the solid and water results (PFAS, TOPA, pH, specific conductivity, dissolved organic carbon, major anions, and metals) from the batch and column experiments, along with the calculated Kd values. Calculated Kd values are presented for every PFAS compound with detections in the solid and water phases and, with caution, can be used to help constrain estimates for PFAS mobility in the New Hampshire environment. Data were obtained in order to assess solid-water partitioning of per- and polyfluoroalkyl substances (PFAS) in soils and biosolids from New Hampshire. 20210510 20221212 ground condition Complete None planned -72.5500 -70.7100 45.3000 42.6900 ISO 19115 Topic Category environment USGS Thesaurus contaminant transport USGS Metadata Identifier USGS:63c9aaa1d34e06fef14f3a99 Common geographic areas New Hampshire None. Please see 'Distribution Info' for details. Although these data have been processed successfully on a computer system at the U.S. Geological Survey (USGS), no warranty expressed or implied is made regarding the display or utility of the data for other purposes, nor on all computer systems, nor shall the act of distribution constitute any such warranty. The USGS or the U.S. Government shall not be held liable for improper or incorrect use of the data described and/or contained herein. Andrea K Tokranov U.S. Geological Survey, Northeast Region Hydrologist mailing address

331 Commerce Way

Pembroke NH 03275 United States 508-490-5017 508-490-5068 atokranov@usgs.gov New Hampshire Department of Environmental Services (NHDES) No formal attribute accuracy tests were conducted No formal logical accuracy tests were conducted Data set is considered complete for the information presented, as described in the abstract. Users are advised to read the rest of the metadata record carefully for additional details. No formal positional accuracy tests were conducted No formal positional accuracy tests were conducted Soil and biosolid samples were collected as described in the abstract, air dried, gently homogenized, and sieved (soils only) before use in batch and column experiments. For kinetics batch experiments, 7.15 ± 0.05 grams (g) soil, 7 ± 0.05 g soil, or 3.5 ± 0.05 g biosolid was added to a 50-milliliter polypropylene centrifuge tube along with approximately 35 milliliters of artificial groundwater (AGW). For all other batch experiments, 7 ± 0.05 g soil or 1 ± 0.05 g biosolid was added to a 50-milliliter polypropylene centrifuge tube along with approximately 35 milliliters of AGW. For batch samples receiving methanol (for PFAS spike, or as a control), 20 µL of a 80:20 methanol:water mixture was added to each tube. For batch samples that required a methanol spike, soils were equilibrated for approximately 24 hours before addition of the methanol (day 0 of the experiment). Batch experiment samples were placed on a rotator for end-over-end shaking. On each sampling day for the batch experiments, the solid/water slurry in the tube was centrifuged at 6000 rotations per minute for 30 minutes and the aqueous phase supernatant was removed to a second 50-milliliter polypropylene centrifuge tube. Sample weights were recorded throughout the process. For the batch and column experiments (except for the experiments testing the effects of ionic strength), the AGW was constructed to contain 0.62 milligrams per liter (mg/L) calcium, 0.19 mg/L magnesium, 0.69 mg/L sodium, 0.16 mg/L potassium, 0.38 mg/L chloride, 3.25 mg/L sulfate, and 0.16 mg/L nitrate, and was designed to replicate the major ion composition in stream water of Watershed 6 at the Hubbard Brook Experimental Forest in New Hampshire (Likens, 2013). For ionic strength experiments with soils, the AGW was constructed to contain either the ionic composition as described above (samples with names containing “-IS1”), or 10 times these concentrations (samples with names containing “-IS2”). For ionic strength experiments with biosolids, the AGW contained either 10 times (samples with names containing “-IS1”) or 100 times (samples with names containing “-IS2”) the concentrations of ions described above. For pH adjustment experiments, the target pH was 1 standard pH unit less (samples with names containing “-PH1”) or one standard pH unit more (samples with names containing “-PH2”) than the samples with no pH adjustment. Actual pH adjustment values differed slightly from the targets and can be found in the pH data results. Hydrochloric acid or sodium hydroxide was used for pH adjustment. Column experiments were conducted using the same soil or biosolid as in the batch experiments. Borosilicate glass columns (1.5-centimeter internal diameter, 20 centimeter length) with high density polyethylene bed support (20 micrometers pore size) and polypropylene outlets were tightly packed using soil or biosolid and saturated in upflow mode to prevent formation of air pockets. For the AGW used in the column experiments, the 500 milliliter bottles receiving methanol (for a PFAS spike) were dosed with 25 µL of a 80:20 methanol:water mixture. The source water was pumped through the column in upflow mode at 0.1 milliliters per minute using a 12-channel peristaltic pump. Column effluent was recirculated back into the source water to create a continuous loop. Samples were collected from the source water between days 0 and 10. All PFAS and TOPA analysis was completed by Eurofins Lancaster Laboratories Environment Testing, LLC (Eurofins) using liquid chromatography tandem mass spectrometry (LC-MS/MS) and isotope dilution analysis as described previously (Santangelo and others, 2021). Total organic carbon for the soil and biosolid samples collected in the field (prior to air drying) was analyzed by Eurofins using the EPA Lloyd Kahn method (solids) or EPA method 415.1 (aqueous). Moisture content was measured by Eurofins using standard method 2540. All pH, specific conductivity, grain size, major anion, dissolved organic carbon (laboratory experiments only), and metals (laboratory experiments only) data were generated at the U.S. Geological Survey. A Hach HQ40d multi-parameter meter was used for pH and specific conductivity measurements. Anion concentrations were measured using a DX600 ion chromatograph (IC) with suppressed electrical conductivity detection, AS18/AG18 analytical and guard columns, 15 millimolar sodium hydroxide eluent, and isocratic separation (Brinton and others, 1995), or with an ICS-5000 IC with suppressed electrical conductivity detection, AS22/AG22 or AS4a-SC/AG4a-SC analytical and guard columns, 1.8 millimolar carbonate/1.7 millimolar bicarbonate eluent, and isocratic separation (Smith and others, 2019). Metals in the laboratory experiment samples were analyzed using the method outlined in Roth and others, 2022. Particle size distributions were characterized by optical diffraction (Gee and Or, 2002) using a Coulter LS 13 320 Particle Size Analyzer. For environmental samples (fresh, unprocessed soils and biosolids), Eurofins analyzed iron, aluminum, and sodium concentrations using EPA Method 6010D and cation exchange capacity using EPA Method 9081. Autoclave citrate extractable protein and anion exchange capacity (following 40 CFR Part 160) analyses were completed by Agvise Laboratories using proprietary methods. Kd values were calculated as described in Weber and others, 2017. The solid concentration (nanograms per kilogram) was corrected for residual water content and then divided by the aqueous concentration (nanograms per liter). The Kd values were not corrected for PFAS sorption to the side walls of the container based upon the minimal observed loss to container side walls in samples containing the artificial groundwater, soil, and PFAS. Note that loss of PFAS to the container side walls was greater in tests where no solid was added (blank samples), which does not accurately reflect experimental conditions. References: Brinton, T.I., Antweiler, R.C., and Taylor, H.E., 1995, Method for the determination of dissolved chloride, nitrate, and sulfate in natural water using ion chromatography: U.S. Geological Survey Open-File Report 95-426A, 16 p. U.S. Environmental Protection Agency, 1983, Organic carbon, total, method 415.1 (combustion or oxidation), Methods for chemical analysis of water and wastes: Office of Research and Development, Washington, DC, 20460, EPA/600/4-79/020. U.S. Environmental Protection Agency , 1986, Method 9081, Cation-exchange capacity of soils (sodium acetate), Third Edition of the Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, U.S. Environmental Protection Agency publication SW‐846. U.S. Environmental Protection Agency , Revision 5, 2018, Method 6010D, Inductively coupled plasma-optical emission spectrometry, Third Edition of the Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, U.S. Environmental Protection Agency publication SW‐846. Gee, G.W., and Or, D., 2002, Particle-size analysis, in Dane, J.H., and Topp, G.C., eds., Methods of soil analysis, Part 4--Physical methods: Soil Science Society of America Book Series No. 5, Soil Science Society of America, Madison, Wisconsin, p. 255-293. Kahn, L., 1988, Determination of Total Organic Carbon in Sediment, U.S. Environmental Protection Agency, Region II, Environmental Services Division, Edison, New Jersey, 08837. Likens, G.E., 2013, Biogeochemistry of a forested ecosystem (Third ed.), Springer New York, NY. Roth, D.A., Johnson, M.O., McCleskey, R.B., Riskin, M.L., and Bliznik, P.A., 2022, Evaluation of preservation techniques for trace metals and major cations for surface waters collected from the U.S. Geological Survey's National Water Quality Network Sites: U.S. Geological Survey data release, https://doi.org/10.5066/P9SMPZ3M. Santangelo, L.M., Tokranov, A.K., Welch, S.M., Schlosser, K.E.A., Marts, J.M., Drouin, A.F., Ayotte, J.D., Rousseau, A.E., and Harfmann, J.L., 2022, Statewide survey of shallow soil concentrations of per- and polyfluoroalkyl substances (PFAS) and related chemical and physical data across New Hampshire, 2021: U.S. Geological Survey data release, https://doi.org/10.5066/P9KG38B5. Smith, R. L., Repert, D. A., Stoliker, D. L., Kent, D. B., Song, B., LeBlanc, D. R., and others, 2019, Seasonal and spatial variation in the location and reactivity of a nitrate‐contaminated groundwater discharge zone in a lakebed, Journal of Geophysical Research: Biogeosciences, 124(7), 2186-2207, https://doi.org/10.1029/2018jg004635. Standard Methods Committee of the American Public Health Association, American Water Works Association, and Water Environment Federation. 2540 solids In: Standard Methods For the Examination of Water and Wastewater. Lipps WC, Baxter TE, Braun-Howland E, editors. Washington DC: APHA Press. Weber, A.K., Barber, L.B., LeBlanc, D.R., Sunderland, E.M., and Vecitis, C.D., 2017, Geochemical and hydrologic factors controlling subsurface transport of poly- and perfluoroalkyl substances, Cape Cod, Massachusetts: Environmental Science & Technology, v. 51, no. 8, p. 4269-4279, https://doi.org/10.1021/acs.est.6b05573. 20230123 Andrea K Tokranov U.S. Geological Survey, Northeast Region Hydrologist mailing address

331 Commerce Way

Pembroke NH 03275 United States 508-490-5017 508-490-5068 atokranov@usgs.gov Three files are provided with this data release: 1. A data dictionary specific to this dataset (file "Data_Dictionary_NH_PFAS_Partitioning.xlsx"). The file contains four tabs: Dictionary, Qualifiers, Abbreviations, and Chemical Abstracts Service Registry Number (CASRN). In the Dictionary tab, the definitions for each column in each data file are provided. In the Qualifiers tab, flags used to qualify data are defined. In the Abbreviations tab, definitions and detailed descriptions are provided for abbreviations found in the data files. In the CASRN tab, the Chemical Abstracts Service Registry Number is provided for each native PFAS compound analyzed. 2. The study data (file "Study_Data_NH_PFAS_Partitioning.xlsx"). The file contains 14 tabs of results, as outlined in the data dictionary. 3. Quality Assurance and Quality Control data (file "QC_Data_NH_PFAS_Partitioning.xlsx"). The file contains the quality assurance and quality control data for the analyses conducted by Eurofins Lancaster Laboratories Environment Testing, LLC. A data dictionary specific to this dataset is provided on the landing page (file "Data_Dictionary_NH_PFAS_Partitioning.xlsx"), https://doi.org/10.5066/P9TKSM8S, and describes the contents of the other two files in this data release, "Study_Data_NH_PFAS_Partitioning.xlsx" and "QC_Data_NH_PFAS_Partitioning.xlsx". GS ScienceBase U.S. Geological Survey mailing address

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Denver CO 80225 United States 1-888-275-8747 sciencebase@usgs.gov Unless otherwise stated, all data, metadata and related materials are considered to satisfy the quality standards relative to the purpose for which the data were collected. Although these data and associated metadata have been reviewed for accuracy and completeness and approved for release by the U.S. Geological Survey (USGS), no warranty expressed or implied is made regarding the display or utility of the data on any other system or for general or scientific purposes, nor shall the act of distribution constitute any such warranty. Any use of trade, firm, or product names is for descriptive purposes only and does not imply endorsement by the U.S. Government. Digital Data https://doi.org/10.5066/P9TKSM8S None 20230209 Andrea K Tokranov U.S. Geological Survey, Northeast Region Hydrologist mailing address

331 Commerce Way

Pembroke NH 03275 United States 508-490-5017 508-490-5068 atokranov@usgs.gov FGDC Content Standard for Digital Geospatial Metadata FGDC-STD-001-1998