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Home My WebLink About2019.08.21_CCO.p11_SedimentCharacterizationPlan Sediment Characterization Plan Prepared for The Chemours Company FC, LLC 1007 Market Street PO Box 2047 Wilmington, DE 19899 Prepared by Geosyntec Consultants of NC, P.C. 2501 Blue Ridge Road, Suite 430 Raleigh, NC 27607 Geosyntec Project Number TR0795 August 2019 TR0795 ii August 2019 TABLE OF CONTENTS 1. INTRODUCTION ................................................................................................ 1 2. CHARACTERIZATION PLAN .......................................................................... 2 2.1 Sampling Locations ..................................................................................... 2 2.2 Sampling Schedule ...................................................................................... 2 2.3 General Sample Collection Considerations ................................................. 3 2.4 Sediment Sampling Procedures ................................................................... 5 2.5 Collection of Field Data .............................................................................. 6 2.6 Decontamination Protocol ........................................................................... 7 2.7 Sample Labels, Shipping, Chain of Custody, and Holding Times .............. 7 2.8 Quality Assurance/Quality Control ............................................................. 8 2.8.1 Field Documentation ....................................................................... 8 2.8.2 Bottleware ....................................................................................... 9 2.8.3 Field QA/QC ................................................................................... 9 3. TEST METHODS AND LABORATORY STANDARDS ............................... 10 3.1 Sample Analysis ........................................................................................ 10 3.2 Data Quality Objectives ............................................................................. 10 3.3 Data Verification ....................................................................................... 10 4. REPORTING ...................................................................................................... 13 5. REFERENCES ................................................................................................... 14 LIST OF TABLES Table 1: PFAS and Associated Methods Table 2: Description of Sampling Locations Table 3: Sampling Containers, Preservation, and Holding Times Table 4: Quality Assurance/Quality Control Samples Table 5: Criteria for Achieving Data Quality Objectives TR0795 iii August 2019 LIST OF FIGURES Figure 1: Sample Locations Figure 2: Conceptual Layout of Transect Sampling Location ACRONYMS AND ABBREVIATIONS ADQM – analytical data quality management COC – chain of custody DO – dissolved oxygen DQOs – data quality objectives DVM – data verification module HDPE – high-density polyethylene LDPE – low-density polyethylene NCDEQ – North Carolina Department of Environmental Quality ORP – oxygen/reduction potential PFAS – per- and polyfluoroalkyl substances PTFE – polytetrafluoroethylene QA/QC – quality assurance/quality control QAPP – quality assurance project plan RPD – relative percent difference SOPs – standard operating procedures USEPA – United States Environmental Protection Agency TR0795 1 August 2019 1. INTRODUCTION This Characterization plan (the Characterization Plan) was prepared by Geosyntec Consultants of NC, P.C. (Geosyntec) for The Chemours Company FC, LLC (Chemours) to provide a plan for sampling and analysis of sediment in the Cape Fear River. This Characterization Plan has been prepared pursuant to Paragraph 11.2 of the Consent Order (CO) between the North Carolina Department of Environmental Quality (NCDEQ), Cape Fear River Watch and Chemours entered into court on 25 February 2019. This paragraph requires Chemours to develop a plan to assess the nature and extent of per- and polyfluoroalkyl substances (PFAS) sediment contamination in the Cape Fear River originating from the Fayetteville Works (Site) by 26 August 2019. TR0795 2 August 2019 2. CHARACTERIZATION PLAN The purpose of this plan is to obtain information regarding concentrations of PFAS in sediment upstream, adjacent to, and downstream of the Site in order to further define the PFAS contributions originating from the Site and PFAS originating from other sources. This sampling may occur in two phases. The first phase described in this Characterization Plan is scheduled, contingent on NCDEQ approval, to be conducted in Fall 2019. Following review of initial sampling data, a second phase of sampling to refine initial findings may be planned, and if needed, an addendum to this Characterization Plan will be prepared (potential timeframe: Spring/Summer 2020). Samples collected will be analyzed for EPA Method 537 Mod and Table 3+ laboratory-specific Standard Operating Procedures (SOPs) as listed in Table 1. 2.1 Sampling Locations Investigative transects are proposed as indicated in Table 2 and Figure 1. The field team may collect samples from different or additional locations depending on field conditions, in-person observations, and/or accessibility considerations upon consultation with the Geosyntec project manager. Three sediment samples will be collected from each transect: one from the eastern side, one from the western side, and one from a location between the other two samples (conceptual layout provided in Figure 2). By collecting samples along a transect from each location, analytical results will be correlated with a range of sediment transport environments (depositional and erosional) and from a range of physical and chemical sediment environments (e.g., potential variation in particle size and organic content to be analyzed according to Table 3). Samples will be collected from upstream locations, locations adjacent to the Site, and downstream locations as shown in Table 2 and Figure 1. In addition to collecting sediment for analysis, field conditions in each transect location will be recorded. Water depth and velocity will be measured in the same locations where samples are collected from each transect. Sediment will be collected for visual evaluation. 2.2 Sampling Schedule The proposed sampling associated with this first phase of work will be performed according to the proposed schedule: • Submission of Characterization Plan; TR0795 3 August 2019 • NCDEQ Approval (logistical planning to begin within 30 days after approval); • 0 to 45 days – logistical planning; • 45 to 75 days – Characterization Plan implementation, provided suitable weather (contingent on NCDEQ approval timing); and • Reporting within 90 days of receipt of full scope of validated analytical data. If a second phase of sampling is performed, the report will be prepared to include both phases. 2.3 General Sample Collection Considerations Sediment sample collection considerations are outlined below and summarized in Table 2. Samples will be collected in accordance with the PFAS Quality Assurance Project Plan (QAPP; AECOM, 2018). The sampling team will attempt to collect samples when there has been no precipitation for a minimum of 72 hours to limit the potential for suspended loads associated with rain events to impact the interpretation of data. Where sample locations are within 0.5 miles of each other, work will be conducted from downstream to upstream to the extent possible to avoid disturbing sediment. Whenever possible, sample locations will be approached from a downstream position for this same reason. All work will be performed in compliance with the project Health and Safety Plan prepared by Parsons (Parsons Health and Safety Plan Chemours Fayetteville Site, 2018). A Plan on Action Discussion and Project Safety Analysis will be held prior to commencing field activities. All work will be performed under Nationwide Permit 6 (USACE, 2017). The following items are acceptable for use during PFAS sampling: • High-density polyethylene (HDPE)1, silicone, acetate, and stainless-steel sampling equipment and materials (e.g., sampling containers and lids, bowls, pans, trays, spoons, trowels); • Low-density polyethylene (LDPE)2 materials not in direct contact with the sample (e.g., Ziploc® bags); 1 HDPE plastics are commonly identified by a recycling symbol with a number 2 inside it. 2 LDPE plastics are commonly identified by a recycling symbol with a number 4 inside it. TR0795 4 August 2019 • Plastic sleeves, core liners, and caps that do not contain TeflonTM or other fluoropolymers (e.g., acetate, polyvinyl chloride, polycarbonate); • Masonite or aluminum clipboards; • Ballpoint pens; • Sampling forms, loose paper or field notebooks, chain of custody (COC) record, and sample container labels; • Alconox®, Liquinox® and Luminox® detergents; • Paper towels; • Trash bags; • HDPE sheeting; • Hard-shell coolers; • Shipping and handling labels; • Regular (wet) ice; • Bubble wrap; and • Duct tape and packing tape. The following products likely contain PFAS and will therefore be avoided during sampling: • Water-resistant paper, notebooks, and labels (e.g., certain Rite in the Rain® products), due to use of PFAS in water-resistant inks and coatings; • Sticky notes (e.g., certain Post-It® products), due to potential use of a paper coating product Zonyl™ or similar fluorotelomer compounds; • Plastic clipboards, binders, and spiral hardcover notebooks; • Pens with water-resistant ink; • Felt pens and markers (e.g., certain Sharpie® products) – some PFAS SOPs (e.g., Michigan) specifically allow Fine or Ultra-Fine Point Sharpies® and TestAmerica Laboratories, Inc. routinely uses Sharpies® in the laboratory following TR0795 5 August 2019 unpublished analytical tests that reportedly showed no impact on PFAS sample results; • Aluminum foil, as PFAS are sometimes used as a protective layer; • Decon 90™ liquid detergent, which reportedly contain fluorosurfactants; • Chemical (e.g., blue) ice packs, unless it is contained in a sealed bag. Blue ice has the potential to be contaminated from previous field sampling events; • Materials containing polytetrafluoroethylene (PTFE), including Teflon™ and Hostaflon®; • Equipment with Viton™ components (i.e., fluoroelastomers); • Stain- or water-resistant materials, as these are typically fluoropolymer-based; • Material containing LDPE, particularly if used in direct contact with the sample (e.g., LDPE tubing, as PFAS can sorb to the porous tubing); and • Material containing “fluoro” in the name – this includes, but is not limited to, fluorinated ethylene propylene, ethylene tetrafluoroethylene, and polyvinylidene fluoride. 2.4 Sediment Sampling Procedures Surface sediment samples will be collected from the sediment-water interface (i.e., mudline). Sediment samples will be collected with a petite ponar or similar device. Field personnel will make three attempts to collect samples per location. If the initial location does not provide a minimum recovery of 2 inches of material, sampling will be attempted three additional times within a 20-ft radius of the original location. If samples meeting minimum sample recovery cannot be retrieved after three attempts, field personnel may relocate the sample to an area where recovery is feasible and which maintains the Data Quality Objectives (DQOs). If multiple recoveries are required to meet sample mass requirements, the samples will be located as closely as reasonably possible together, and samples will be homogenized by stirring the sample with a stainless-steel spoon (or similar) prior to filling sample jars. Sediment sampling will be conducted in general accordance with EPA SOP SESDPROC- 200-R3 Sediment Sampling (EPA 2014). The following sample procedures will be followed: TR0795 6 August 2019 • The sampling location will be field-located using a handheld GPS device. After setting up on the sampling location, the as-built location coordinates will be collected using the GPS device. • Sampling personnel will use a new pair of nitrile sampling gloves at each location. • Surface samples will be collected using a petite ponar or similar device. • The sample will be transferred to a decontaminated stainless-steel bowl. A photo of the sample will be taken prior to disturbing the sample. Sediment texture and other relevant observations will be noted on a field form. The sample will be homogenized using a stainless-steel spoon to mix the sediment in the bowl prior to filling the sample containers. Any large materials present in the sediment (e.g., gravel, vegetation) will be avoided when filling sample bottles. • Sediment will be transferred into the sampling containers using a stainless-steel spoon or other appropriate device. • Each sampling container will be capped, labeled as described in Section 2.7, and temporarily stored on ice (4 ± 2°C) in a cooler to await transport or preparation for shipment to the laboratory as directed in the QAPP. • All reusable equipment will be decontaminated according to the procedures described in Section 2.6. • Disposable equipment and investigation derived waste will be transferred to the Chemours plant for offsite disposal. • Documentation will be maintained as described in Section 2.8.1. 2.5 Collection of Field Data Water depths and water velocities will be measured at each location along each transect. Sediment will be observed for color and texture. The flow rate of the Cape Fear River will be measured using a submersible flow meter. The height of the water and river bottom will be recorded at each point along each transect. The flow meter will be submerged at each point, and the water velocity will be recorded at 2 water depths at each point along the transect (e.g. top-half and bottom-half of the water column). TR0795 7 August 2019 2.6 Decontamination Protocol Sample containers will be new and used only once for each sample and disposable equipment (e.g., gloves, tubing, etc.) will not be reused; therefore, these items will not require decontamination. All non-dedicated or non-disposable sampling equipment (e.g., stainless steel reusable equipment used in sediment sampling) will be decontaminated between samples in the following manner: • Water rinse; • Scrub with de-ionized water containing non-phosphate detergent (e.g., Alconox®); • Tap water rinse; and • De-ionized water rinse. If there is a delay between decontamination and sample collection, decontaminated sampling equipment will be covered with PFAS-free plastic until it is ready for use (Ziploc® bags are acceptable for this purpose). 2.7 Sample Labels, Shipping, Chain of Custody, and Holding Times Upon sample collection, each containerized sample will be labelled. Sediment sample naming convention is as follows: FAY-SED-CFR-RM-##-x-MMDDYY Where: o FAY indicates Fayetteville o SED indicates sediment o CFR indicates Cape Fear River o RM indicates Rivermile o ## to be replaced by the Rivermile associated with the sample (in whole numbers or using decimal places for partial Rivermiles) o x to be replaced by “a” to indicate western portion of River, “b” to indicate middle area of river, and “c” to indicate eastern portion of River TR0795 8 August 2019 o MMDDYY indicates month, day, year, in 2-digit format (e.g., August 1, 2019 would be 080119) Sample bottles will be placed as soon as possible into a durable zip-top plastic bag inside an insulated sample cooler with ice. The cooler will serve as a shipping container and will be provided by the laboratory along with the appropriate sample containers. Samples will be shipped to either TestAmerica Sacramento, or Eurofins Lancaster Laboratories depending on laboratory availability at the time of sampling. Chemours will request that samples be analyzed by the laboratory within the holding times specified in Table 3. The additional samples collected at each location for potential future analyses will be stored under COC protocol in a secured, refrigerated location on Site. Prior to shipment of the samples to the laboratory, a COC form will be completed by the field sample custodian. Sample locations, sample identification numbers, description of samples, number of samples collected, and specific laboratory analyses to be performed on each sample will be recorded on the COC. The COC will be signed by the field personnel relinquishing the samples to the courier and will be signed by the laboratory upon receipt of the cooler. Prior to shipping, the cooler will be taped shut and a custody seal will be taped across the lid of the cooler; laboratory personnel will confirm the signature is intact upon receipt. 2.8 Quality Assurance/Quality Control Quality assurance/quality control (QA/QC) activities will be performed in the field and in the laboratories to document the data quality. 2.8.1 Field Documentation Each sample will be labelled with a unique sample identification number as described in Section 2.7, date, time, and the initials of the individual collecting the sample. A field form will be used to record information regarding additional items such as QA/QC, sample identifications, color, odor, turbidity, and other field parameters. The project field team will keep a daily record of field activities during the execution of field work including sampling notes and observations, instrument calibration records, measured field parameters, sample COC and shipping records. All field collected data will be furnished to Chemours within 10 business days of the conclusion of the field event. TR0795 9 August 2019 2.8.2 Bottleware Bottleware requirements are listed in Table 3. Bottleware will be pre-cleaned and will be supplied by a vendor to minimize the risk of unplanned sample contamination from the sample container (i.e., blank contamination). 2.8.3 Field QA/QC Field QA/QC samples will be collected and analyzed along with the investigative samples to evaluate potential bias and variability introduced in sample collection, storage, handling and shipping. Criteria for achieving data quality objectives for field QA/QC samples are summarized in Table 4. Four types of field QA/QC samples will be collected: equipment blanks, trip blanks, field blanks, and field duplicates. Equipment Blanks Equipment blanks (field rinsate blanks) are used to evaluate equipment and cleaning or decontamination procedures. At the sample location, laboratory-supplied analyte-free water will be poured over or through the clean, non-dedicated sampling equipment, and collected in a sample container. The equipment blank samples will then be shipped, stored and handled with the other samples and will be analyzed for the same parameters as other samples collected using the same device. Equipment blanks will be collected at a frequency of one per day during sampling activities. Trip Blanks Trip blanks are used to assess whether samples might be inadvertently contaminated during shipment and handling. The trip blanks will consist of a series of new containers filled with analyte-free water prepared by the laboratory analyzing the samples and will travel to the Site with the empty sample bottles and back from the Site with the investigative samples. Trip blanks will not be opened in the field. Trip blanks will be collected at a frequency of one per day during sampling activities. Field Blanks Field blanks are used to assess whether field conditions pose a potential for bias or variability in the results of analysis. The field blank will be collected by transferring laboratory-supplied analyte-free water into a sample container without contacting any other sampling equipment. Field blanks will be collected at a frequency of one per day during sampling activities. TR0795 10 August 2019 Field Duplicates Duplicate samples are collected to assess the precision of the laboratory analysis through calculation of the relative percent difference (RPD) between duplicate samples. The equation for calculating RPD is shown below: 𝑅𝑅𝑅𝑅𝑅𝑅(%)= |(𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 1 −𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 2)|�(𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 1 +𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 2)2 � × 100% RPDs less than or equal to 25% indicate acceptable precision at mid and high range concentrations; RPDs less than or equal to 50% indicate acceptable precision within a factor of five of the reporting limit. Duplicates will be collected in the same manner as investigative samples and the duplicate samples will be analyzed for the same parameters as the collocated investigative sample. Duplicates will be numbered sequentially with investigative samples so they are not identifiable by the analytical laboratories (i.e., “blind” duplicates). Field duplicate samples will be collected at a minimum frequency of one duplicate for every 20 investigative samples. 3. TEST METHODS AND LABORATORY STANDARDS 3.1 Sample Analysis Samples will be collected and analyzed for methods according to Table 3. 3.2 Data Quality Objectives DQOs are established here to provide data of known and sufficient quality to accomplish the following: • Characterize concentrations of PFAS in Cape Fear River sediment upstream, adjacent to, and downstream of the Site; • Collect related data on field conditions at each sampling transect. The analytical criteria for achieving the DQOs are provided in Table 5. 3.3 Data Verification The analytical laboratory performing the analysis will provide all analytical data to Chemours’s data verification contractor, AECOM’s in-house Analytical Data Quality Management (ADQM) group. The data package will be reviewed by ADQM for TR0795 11 August 2019 compliance with the laboratory SOPs and usability. The laboratory will also deliver the analytical data electronically for upload to the Chemours Locus EIM™ database. All data will be reviewed using the Data Verification Module (DVM). The DVM is an automated database algorithm developed by the ADQM group that includes a series of data quality checks, which are binary (yes/no) and do not require professional judgement. Manual review is performed after the DVM process to address validation components that are not readily automated. The data are evaluated against the following data usability checks: • Field and laboratory blank contamination; • United States Environmental Protection Agency (USEPA) hold time criteria; • Missing quality control samples; • Matrix spike recoveries to verify measurement precision; • Laboratory control sample recoveries verify measurement precision; • Surrogate spike recoveries to verify measurement accuracy; • RPD between field duplicate sample pairs to verify field duplicate precision; • Completeness as a percentage of the planned samples actually collected and analyzed; and • Sensitivity of the practical quantitation limits compared to regulatory standards or screening levels. The DVM applies the following data evaluation qualifiers to analysis results, as warranted: • R - Unusable result. Analyte may or may not be present in the sample. • B – Not detected substantially above the level reported in the laboratory or field blanks. • J – Analyte present. Reported value may not be accurate or precise. • UJ – Not detected. Reporting limit may not be accurate or precise. An individual DVM narrative report will be generated for each lot entered into the EIM™ database which will summarize any samples that are qualified, the specific reasons for the qualification, and the potential bias in reported results. The DVM review process described above will be performed on 100% of the data generated for the sampling event. The DVM review process will be supplemented by a manual review of the instrument- related QC results for calibration standards, blanks, and recoveries to elevate the overall review process to be consistent with Stage 2b of the EPA TR0795 12 August 2019 Guidance for Labelling Externally Validated Laboratory Analytical Data for Superfund Use (EPA-540-R-08-005, 2009). TR0795 13 August 2019 4. REPORTING A report will be submitted following receipt of results. The report will include a map of sample locations, data tables of measured concentrations, and a data review summary. TR0795 14 August 2019 5. REFERENCES AECOM, 2018. Poly and Perfluoroalkyl Substance Quality Assurance Project Plan for the Chemours Corporate Remediation Group. August, 2018. EPA, 2009. Guidance for Labelling Externally Validated Laboratory Analytical Data for Superfund Use. EPA-540-R-08-005, 2009. Stage 2b. EPA, 2014. Region 4. Operating Procedure: Sediment Sampling. EPA SOP SESDPROC-200-R3. August 2014. Parsons, 2018. Health and Safety Plan Chemours Fayetteville Site. United States Army Corps of Engineers. Nationwide Permit 6. 19 March 2017. http://saw- reg.usace.army.mil/NWP2017/2017NWP06.pdf. Accessed 30 January 2019. Table 1 PFAS and Associated Methods Chemours Fayetteville Works, North Carolina Geosyntec Consultants NC, PC TestAmerica Eurofins Lancaster HFPO-DA* Hexafluoropropylene oxide dimer acid 13252-13-6 C6HF11O3 1.00 TBD PEPA Perfluoroethoxypropyl carboxylic acid 267239-61-2 C5HF9O3 1.00 TBD PFECA-G Perfluoro-4-isopropoxybutanoic acid 801212-59-9 C12H9F9O3S 1.00 TBD PFMOAA Perfluoro-2-methoxyaceticacid 674-13-5 C3HF5O3 1.00 TBD PFO2HxA Perfluoro(3,5-dioxahexanoic) acid 39492-88-1 C4HF7O4 1.00 TBD PFO3OA Perfluoro(3,5,7-trioxaoctanoic) acid 39492-89-2 C5HF9O5 1.00 TBD PFO4DA Perfluoro(3,5,7,9-tetraoxadecanoic) acid 39492-90-5 C6HF11O6 1.00 TBD PMPA Perfluoromethoxypropyl carboxylic acid 13140-29-9 C4HF7O3 1.00 TBD Hydro-EVE Acid Perfluoroethoxsypropanoic acid 773804-62-9 C8H2F14O4 1.00 TBD EVE Acid Perfluoroethoxypropionic acid 69087-46-3 C8HF13O4 1.00 TBD PFECA B Perfluoro-3,6-dioxaheptanoic acid 151772-58-6 C5HF9O4 1.00 TBD R-EVE R-EVE NA1 C8H2F12O5 1.00 TBD PFO5DA Perfluoro-3,5,7,9,11-pentaoxadodecanoic acid 39492-91-6 C7HF13O7 1.00 TBD Byproduct 4 Byproduct 4 NA1 C7H2F12O6S 1.00 TBD Byproduct 6 Byproduct 6 NA1 C6H2F12O4S 1.00 TBD Byproduct 5 Byproduct 5 NA1 C7H3F11O7S 1.00 TBD NVHOS Perfluoroethoxysulfonic acid 1132933-86-8 C4H2F8O4S 1.00 TBD PES Perfluoroethoxyethanesulfonic acid 113507-82-7 C4HF9O4S 1.00 TBD NEtPFOSA NEtPFOSA 4151-50-2 C10H6F17NO2S 1.00 NA2 NEtPFOSAE NEtPFOSAE 1691-99-2 C12H10F17NO3S 1.00 NA2 NMePFOSA NMePFOSA 31506-32-8 C9H4F17NO2S 1.00 NA2 NMePFOSAE NMePFOSAE 24448-09-7 C11H8F17NO3S 1.00 NA2 PFESA-BP1 Byproduct 1 29311-67-9 C7HF13O5S 1.00 TBD PFESA-BP2 Byproduct 2 749836-20-2 C7H2F14O5S 1.00 TBD PFBA Perfluorobutanoic acid 375-22-4 C4HF7O2 0.200 2.0 PFDA Perfluorodecanoic acid 335-76-2 C10HF19O2 0.200 0.6 PFDoA Perfluorododecanoic acid 307-55-1 C12HF23O2 0.200 0.6 PFHpA Perfluoroheptanoic acid 375-85-9 C7HF13O2 0.200 0.6 PFNA Perfluorononanoic acid 375-95-1 C9HF17O2 0.200 0.6 PFOA Perfluorooctanoic acid 335-67-1 C8HF15O 0.200 0.6 PFHxA Perfluorohexanoic acid 307-24-4 C6HF11O2 0.200 0.6 PFPeA Perfluoropentanoic acid 2706-90-3 C5HF9O2 0.200 0.6 PFTeA Perfluorotetradecanoic acid 376-06-7 C14HF27O2 0.200 0.6 PFTriA Perfluorotridecanoic acid 72629-94-8 C13HF25O2 0.200 0.6 PFUnA Perfluoroundecanoic acid 2058-94-8 C11HF21O2 0.200 0.6 PFBS Perfluorobutanesulfonic acid 375-73-5 C4HF9SO 0.200 0.6 PFDS Perfluorodecanesulfonic acid 335-77-3 C10HF21O3S 0.200 1.0 PFHpS Perfluoroheptanesulfonic acid 375-92-8 C7HF15O3S 0.200 0.6 PFHxS Perfluorohexanesulfonic acid 355-46-4 C6HF13SO3 0.200 0.6 PFNS Perfluorononanesulfonic acid 68259-12-1 C9HF19O3S 0.200 0.6 PFOS Perfluorooctanesulfonic acid 1763-23-1 C8HF17SO3 0.500 0.9 PFPeS Perfluoropentanesulfonic acid 2706-91-4 C5HF11O3S 0.200 0.6 10:2 FTS 10:2-fluorotelomersulfonic acid 120226-60-0 C12H5F21O3 2.00 3.0 4:2 FTS 4:2 fluorotelomersulfonic acid 757124-72-4 C6H5F9O3S 2.00 3.0 6:2 FTS 6:2 fluorotelomersulfonic acid 27619-97-2 C8H5F13SO3 2.00 2.0 8:2 FTS 8:2 fluorotelomersulfonic acid 39108-34-4 C10H5F17O3S 2.00 2.0 NEtFOSAA NEtFOSAA 2991-50-6 C12H8F17NO4S 2.00 2.0 NEtPFOSA NEtPFOSA 4151-50-2 C10H6F17NO2S NA3 2.0 NEtPFOSAE NEtPFOSAE 1691-99-2 C12H10F17NO3S NA3 2.0 NMeFOSAA NMeFOSAA 2355-31-9 C11H6F17NO4S 2.00 2.0 NMePFOSA NMePFOSA 31506-32-8 C9H4F17NO2S NA3 2.0 NMePFOSAE NMePFOSAE 24448-09-7 C11H8F17NO3S NA3 2.0 PFDOS Perfluorododecanesulfonic acid 79780-39-5 C12HF25O3S 0.200 0.9 PFHxDA Perfluorohexadecanoic acid 67905-19-5 C16HF31O2 0.200 0.6 PFODA Perfluorooctadecanoic acid 16517-11-6 C18HF35O2 0.200 0.6 PFOSA Perfluorooctanesulfonamide 754-91-6 C8H2F17NO2S 0.200 0.6 Notes: PQLs are as of March 31, 2019 EPA - Environmental Protection Agency ng/g - nanograms per gram PFAS - per- and polyfluoroalkyl substances PQL - practical quantitation limit SOP - Standard Operating Procedure TBD - PQL is to be determined NA1 - no CAS number assigned NA2 - Eurofins Lancaster uses EPA Method 537 Mod for these analytes. See EPA Method 537 Mod list for the associated PQL. NA3 - Table 3+ Method is used by TestAmerica for these analytes. See Table 3+ list for the associated PQL. *Depending on the laboratory, HFPO-DA may also appear on the EPA Method 537 Mod analyte list Chemical Formula Soil/Sediment (ng/g) Table 3+ Lab SOP EPA Method 537 Mod Analytical Method Common Name Chemical Name CASN August 2019 Table 2Description of Sampling LocationsChemours Fayetteville Works, North CarolinaGeosyntec Consultants NC, PCSampling MethodTarget ConcentrationsSedimentCFR-RM-20Co-located with Mile 20 surface water sample collected June 2018; representative of background conditions; near USGS Stream Gage 02102500 and Harnett County's drinking water intake.Grab Background 3 samplesCFR-RM-52Co-located with Mile 52 surface water sample collected June 2018; representative of background conditions; near Fayetteville's drinking water intake.Grab Background 3 samplesCFR-RM-76.2Co-located with CFR-05 surface water samples collected Sept 2017 and May 2018; adjacent to Site.Grab Site 3 samplesCFR-RM-77.25 Located downstream of Outfall 002, immediately upstream of dam. Grab Site 3 samplesCFR-RM-84Co-located with Mile 84 surface water sample collected June 2018; downstream of Site; highest concentrations of HFPO-DA, PFECA, and PFESA detected during June 2018 surface water sampling event. Locate upstream and within 1000 ft of Blden Bluff Drinking Water Intake (RM 84.8).Grab Downstream 3 samplesCFR-RM-100Co-located with Mile 100 surface water sample collected June 2018; downstream of Site.Grab Downstream 3 samplesCFR-RM-116Co-located with Mile 116 surface water sample collected June 2018; downstream of Site.Grab Downstream 3 samplesCFR-RM-132Co-located Mile 132 surface water samples collected June 2018; HFPO-DA was ND June 2018.Grab Downstream 3 samplesNotesSample identifications (IDs) refer to locations identified in Figure 1. Sample IDs are abbreviations, full sample IDs are provided in text. Sample IdentificationCo-located Sediment Sample Location DescriptionSample CategoryAugust 2019 Table 3 Sampling Containers, Preservation, and Holding TimesChemours Fayetteville Works, North CarolinaGeosyntec Consultants NC, PCTestAmerica Eurofins LancasterPFOS/PFOA Compounds EPA Method 537 Mod 250 mL HDPE 100 g Homogenized 2 Cool to 4ºC± 2ºC14 days to extraction, 40 days to analysis14 days to extraction, 28 days to analysisSite-associated Compounds Table 3+ Lab SOP 250 mL HDPE 100 g Homogenized 1 Cool to 4ºC± 2ºC 28 Days 14 daysTotal Organic Carbon Lloyd Kahn 4 oz glass 50 mg Homogenized 1 Cool to 4ºC± 2ºC 28 Days 28 DaysGrainsize Distribution ASTM D422; D7928 16 oz glass fill containerHomogenized 1 NoneSample to be sent to TA BurlingtonSample to be sent to TA BurlingtonMoisture Content ASTM D2216 2 oz glass fill container Homogenized 1 NoneSample to be sent to TA BurlingtonSample to be sent to TA BurlingtonArchived for potential future analysesTBD 250 mL HDPE fill container Homogenized 2 Cool to 4ºC± 2ºC TBD TBDArchived for potential future analysesTBD 4 oz glass fill container Homogenized 4 Cool to 4ºC± 2ºC TBD TBDNotes:HDPE - high density polyethyleneSOP - Standard Operating ProcedureN/A - not applicableMatrix AnalysisSample Volume or Mass RequiredSedimentHolding Times PreservationNumber of ContainersContainer Type and VolumeAnalytical Method Field PrepAugust 2019 Table 4Quality Assurance/Quality Control Samples Chemours Fayetteville Works, North CarolinaGeosyntec Consultants NC, PCInvestigative SamplesEquipment Blank Trip Blank Field BlankField DuplicateMethod Blank Matrix SpikeLab ReplicateLab Control SampleIsotope Dilution AnalytesContinuing Calibration Verification(per event) (per day) (per shipment) (per day) (per 20 samples)(per sample group)(per sample group)(per sample group)(per sample group)(every sample)(beginning of each group)EPA Method 537 Mod2411111111321Table 3+ Lab SOP2411111111N/A1Notes:N/A - none available at presentSOP - Standard Operating ProcedureSedimentAnalytical MethodLabFieldMatrixAugust 2019 Table 5 Criteria for Achieving Data Quality Objectives Chemours Fayetteville Works, North Carolina Geosyntec Consultants NC, PC Category Data Quality Objective Sediment Criteria Field Duplicate RPD (%) 40* Lab Replicate RPD (%) 30* MS % Recovery 70-130 LCS % Recovery 70-130 Isotope Dilution Analyte % Recovery 25-150 Calibration CCV % Difference 70-130 Completeness % Complete 90 Notes * RPD criteria apply if result is within a factor of five of the reporting limit. Criteria may be replaced by statistical limits generated by the laboratory(ies). CCV - continuing calibration verification LCS - laboratory control sample MS - matrix spike RPD - relative percent difference Precision Accuracy August 2019 Cape Fear Lockand Dam #1 /Kings Bluff Intake Canal ChemoursFayettevilleWorks Start ofCape FearRiver USGS Gauge02102500 USGS Gauge02105769 USGS Gauge02104000 USGS Gauge02105500 CFR-RM-20 CFR-RM-52 CFR-RM-84 CFR-RM-100 CFR-RM-116 CFR-RM-132 Proposed Sampling Transect Locations Chemours Fayetteville Works, North Carolina Figure 1Raleigh 8 0 84 Miles Path: P:\PRJ\Projects\TR0795 - Confidential\Database and GIS\GIS\Sediment Characterization Workplan\TR0726_Confidential_SedimentSampleLocations.mxd; SSomnarain; 08/15/2019August 2019 Notes:1. Sample IDs shown here are abbreviations, see Characterization Plan for full sample IDs.2. Basemap source provided by ESRI OpenStreetMapcontributors, and the GIS User Community Legend Sampling Transect USGS Stream Gauge Site Features Chemours Fayetteville Works Cape Fear River Outfall 002 W.O. Huske Dam Willis CreekMouth Site RiverWater Intake Old Outfall Channel Mouth Georgia Branch Creek Mouth CFR-RM-76.2 CFR-RM-77.25 0 10.5 Miles USGS Gauge02102500 CFR-RM-20 Conceptual Layout of Transect Sampling Location Chemours Fayetteville Works, North Carolina Figure 2Raleigh 300 0 300150 Feet Path: P:\PRJ\Projects\TR0795 - Confidential\Database and GIS\GIS\Sediment Characterization Workplan\TR0726_Confidential_ConceptualSedimentTranset.mxd; SSomnarain; 08/15/2019August 2019 Notes:1. Sample IDs shown here are abbreviations, see Characterization Plan for full sample IDs.2. Basemap source provided by ESRI OpenStreetMapcontributors, and the GIS User Community Legend USGS Stream Gauge Conceptual Sampling Location in Transect Chemours Fayetteville Works CFR-RM-20 0 105 Miles CapeFearRiver