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

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

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LIST OF FIGURES
Figure 1: Sample Locations
Figure 2: Conceptual Layout of Transect Sampling Location
ACRONYMS AND ABBREVIATIONSADQM – 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

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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 paragraphrequires Chemours to develop a plan to assess the nature and extent of per- andpolyfluoroalkyl substances (PFAS) sediment contamination in the Cape Fear Riveroriginating from the Fayetteville Works (Site) by 26 August 2019.

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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 beanalyzed 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 fromeach 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 beanalyzed 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 Figure1.
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;

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•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 bothphases.

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 milesof each other, work will be conducted from downstream to upstream to the extent possible
to avoid disturbing sediment. Whenever possible, sample locations will be approachedfrom 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 tocommencing field activities. All work will be performed under Nationwide Permit 6(USACE, 2017).
The following items are acceptable for use during PFAS sampling:1
2•

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);

HDPE plastics are commonly identified by a recycling symbol with a number 2 inside it.
LDPE plastics are commonly identified by a recycling symbol with a number 4 inside it.

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•

Plastic sleeves, core liners, and caps that do not contain TeflonTM or otherfluoropolymers (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

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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 massrequirements, the samples will be located as closely as reasonably possible together, andsamples will be homogenized by stirring the sample with a stainless-steel spoon (orsimilar) prior to filling sample jars.
Sediment sampling will be conducted in general accordance with EPA SOP SESDPROC200-R3 Sediment Sampling (EPA 2014).
The following sample procedures will be followed:

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•

•
•
•

•
•

•
•
•
2.5

The sampling location will be field-located using a handheld GPS device. Aftersetting up on the sampling location, the as-built location coordinates will becollected using the GPS device.
Sampling personnel will use a new pair of nitrile sampling gloves at eachlocation.
Surface samples will be collected using a petite ponar or similar device.
The sample will be transferred to a decontaminated stainless-steel bowl. A photoof the sample will be taken prior to disturbing the sample. Sediment texture andother relevant observations will be noted on a field form. The sample will behomogenized 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, andtemporarily 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.
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 eachtransect. The flow meter will be submerged at each point, and the water velocity will berecorded at 2 water depths at each point along the transect (e.g. top-half and bottom-halfof the water column).

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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 thefollowing manner:••••

Water rinse;
Scrub with de-ionized water containing non-phosphate detergent (e.g.,
Alconox®);
Tap water rinse; andDe-ionized water rinse.

If there is a delay between decontamination and sample collection, decontaminatedsampling 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 Fayettevilleo SED indicates sedimento CFR indicates Cape Fear Rivero RM indicates Rivermileo ## 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

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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 andwill 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 inTable 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 thefield sample custodian. Sample locations, sample identification numbers, description ofsamples, number of samples collected, and specific laboratory analyses to be performedon 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 custodyseal will be taped across the lid of the cooler; laboratory personnel will confirm thesignature is intact upon receipt.
2.8

Quality Assurance/Quality Control

Quality assurance/quality control (QA/QC) activities will be performed in the field andin 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 fieldform 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 offield 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.

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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 thesample 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-freewater will be poured over or through the clean, non-dedicated sampling equipment, andcollected 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 ata frequency of one per day during sampling activities.
Trip Blanks
Trip blanks are used to assess whether samples might be inadvertently contaminatedduring 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 willtravel to the Site with the empty sample bottles and back from the Site with theinvestigative samples. Trip blanks will not be opened in the field. Trip blanks will becollected 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 orvariability in the results of analysis. The field blank will be collected by transferringlaboratory-supplied analyte-free water into a sample container without contacting anyother sampling equipment. Field blanks will be collected at a frequency of one per day
during sampling activities.

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Field Duplicates
Duplicate samples are collected to assess the precision of the laboratory analysis throughcalculation of the relative percent difference (RPD) between duplicate samples. The
equation for calculating RPD is shown below:
𝑅𝑅𝑅𝑅𝑅𝑅(%) =|(𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 1 − 𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 2)|
× 100%(𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 1 + 𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 2)��2

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 afactor 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 withinvestigative 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 forTR0795

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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 ofdata quality checks, which are binary (yes/no) and do not require professional judgement.
Manual review is performed after the DVM process to address validation componentsthat 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 andanalyzed; andSensitivity of the practical quantitation limits compared to regulatory standards orscreening levels.

The DVM applies the following data evaluation qualifiers to analysis results, aswarranted:••••

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 fieldblanks.
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 forthe 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 amanual review of the instrument- related QC results for calibration standards, blanks, andrecoveries to elevate the overall review process to be consistent with Stage 2b of the EPA
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Guidance for Labelling Externally Validated Laboratory Analytical Data for Superfund
Use (EPA-540-R-08-005, 2009).

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4.

REPORTING

A report will be submitted following receipt of results. The report will include a map ofsample locations, data tables of measured concentrations, and a data review summary.

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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 SOPSESDPROC-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://sawreg.usace.army.mil/NWP2017/2017NWP06.pdf. Accessed 30 January 2019.

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Table 1
PFAS and Associated Methods
Chemours Fayetteville Works, North Carolina

Analytical Method

Common Name

Chemical Name

CASN

Geosyntec Consultants NC, PC

Chemical Formula

Soil/Sediment (ng/g)
Eurofins
Lancaster

TestAmerica

Table 3+ Lab SOP

EPA Method 537 Mod

HFPO-DA*

Hexafluoropropylene oxide dimer acid13252-13-6

C6HF11O3

1.00

TBD

PEPA

Perfluoroethoxypropyl carboxylic acid267239-61-2

C5HF9O3

1.00

TBD

PFECA-G

Perfluoro-4-isopropoxybutanoic acid

801212-59-9

C12H9F9O3S

1.00

TBD

PFMOAA

Perfluoro-2-methoxyaceticacid674-13-5

C3HF5O3

1.00

TBD

PFO2HxA

Perfluoro(3,5-dioxahexanoic) acid39492-88-1

C4HF7O4

1.00

TBD

PFO3OA

Perfluoro(3,5,7-trioxaoctanoic) acid39492-89-2

C5HF9O5

1.00

TBD

PFO4DA

Perfluoro(3,5,7,9-tetraoxadecanoic) acid39492-90-5

C6HF11O6

1.00

TBD

PMPA

Perfluoromethoxypropyl carboxylic acid

13140-29-9

C4HF7O3

1.00

TBD

Hydro-EVE Acid

Perfluoroethoxsypropanoic acid773804-62-9

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
TBD

R-EVE

R-EVE

1.00

Perfluoro-3,5,7,9,11-pentaoxadodecanoic acidNA1
39492-91-6

C8H2F12O5

PFO5DAC7HF13O7

1.00

TBD

Byproduct 4

Byproduct 4

NA1

C7H2F12O6S

1.00

TBD

Byproduct 6

Byproduct 6NA1

C6H2F12O4S

1.00

TBD

Byproduct 5

Byproduct 5

C7H3F11O7S

1.00

TBD

NVHOS

Perfluoroethoxysulfonic acidNA1
1132933-86-8

C4H2F8O4S

1.00

TBD

PES

Perfluoroethoxyethanesulfonic acid

113507-82-7

C4HF9O4S

1.00

TBD

NEtPFOSANEtPFOSA

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

PFESA-BP1
PFESA-BP2

Byproduct 1
Byproduct 2

29311-67-9749836-20-2

C7HF13O5S
C7H2F14O5S

1.00
1.00

NA2
TBD
TBD

PFBA

Perfluorobutanoic acid375-22-4

C4HF7O2

0.200

2.0

PFDA

Perfluorodecanoic acid335-76-2

C10HF19O2

0.200

0.6

PFDoA

Perfluorododecanoic acid307-55-1

0.200

0.6

PFHpA

Perfluoroheptanoic acid375-85-9

C12HF23O2
C7HF13O2

0.200

0.6
0.6

PFNA

Perfluorononanoic acid375-95-1

C9HF17O2

0.200

PFOA

Perfluorooctanoic acid335-67-1

C8HF15O

0.200

0.6

PFHxA

Perfluorohexanoic acid307-24-4

C6HF11O2

0.200

0.6
0.6

PFPeA

Perfluoropentanoic acid2706-90-3

C5HF9O2

0.200

PFTeA

Perfluorotetradecanoic acid376-06-7

C14HF27O2

0.200

0.6

PFTriA

Perfluorotridecanoic acid72629-94-8

C13HF25O2

0.200

0.6

PFUnA

Perfluoroundecanoic acid2058-94-8

0.6

Perfluorobutanesulfonic acid375-73-5

C11HF21O2
C4HF9SO

0.200

PFBS

0.200

0.6

PFDS

Perfluorodecanesulfonic acid335-77-3

C10HF21O3S

0.200

1.0

PFHpS

Perfluoroheptanesulfonic acid375-92-8

0.200

0.6

PFHxS

Perfluorohexanesulfonic acid355-46-4

C7HF15O3SC6HF13SO3

0.200

0.6

PFNS

Perfluorononanesulfonic acid68259-12-1

C9HF19O3S

0.200

0.6

PFOS

Perfluorooctanesulfonic acid

1763-23-1

C8HF17SO3

0.500

0.9

PFPeS

Perfluoropentanesulfonic acid2706-91-4

C5HF11O3S

0.200

0.6

10:2 FTS

10:2-fluorotelomersulfonic acid120226-60-0

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

NEtPFOSANEtPFOSA

4151-50-2

C10H6F17NO2S

NA3

2.0

NEtPFOSAE

NEtPFOSAE

1691-99-2

C12H10F17NO3S

NMeFOSAA

NMeFOSAA

2355-31-9

C11H6F17NO4S

NA3
2.00

2.0

NMePFOSA

NMePFOSA

31506-32-8

C9H4F17NO2S

NA3

2.0

NMePFOSAE

NMePFOSAE

24448-09-7

C11H8F17NO3S

2.0

PFDOS

Perfluorododecanesulfonic acid

79780-39-5

C12HF25O3S

NA3
0.200

PFHxDA

Perfluorohexadecanoic acid

67905-19-5

C16HF31O2

0.200

0.6

PFODA

Perfluorooctadecanoic acid16517-11-6

C18HF35O2

0.200

0.6

PFOSA

Perfluorooctanesulfonamide

754-91-6

C8H2F17NO2S

0.200

0.6

2.0

0.9

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

August 2019

Geosyntec Consultants NC, PC
Table 2
Description of Sampling Locations
Chemours Fayetteville Works, North Carolina

Sample Category
SampleIdentification

CFR-RM-20

CFR-RM-52
CFR-RM-76.2
CFR-RM-77.25

CFR-RM-84

CFR-RM-100
CFR-RM-116
CFR-RM-132

Co-located Sediment
Sample Location Description

Co-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.
Co-located with Mile 52 surface water sample collected June 2018;
representative of background conditions; near Fayetteville's drinking water
intake.
Co-located with CFR-05 surface water samples collected Sept 2017 and May
2018; adjacent to Site.
Located downstream of Outfall 002, immediately upstream of dam.
Co-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).
Co-located with Mile 100 surface water sample collected June 2018;
downstream of Site.
Co-located with Mile 116 surface water sample collected June 2018;
downstream of Site.
Co-located Mile 132 surface water samples collected June 2018; HFPO-DA
was ND June 2018.

Sampling
MethodTargetConcentrations

Sediment

Grab

Background3 samples

Grab

Background3 samples

Grab

Site

3 samples

Grab

Site

3 samples

Grab

Downstream

3 samples

Grab

Downstream

3 samples

Grab

Downstream

3 samples

Grab

Downstream

3 samples

Notes
Sample identifications (IDs) refer to locations identified in Figure 1. Sample IDs are abbreviations, full sample IDs are provided in text.

August 2019

Table 3
Sampling Containers, Preservation, and Holding Times
Chemours Fayetteville Works, North Carolina

Matrix

Sediment

Geosyntec Consultants NC, PC

Holding Times
TestAmerica
Eurofins Lancaster14 days to extraction, 14 days to extraction,
40 days to analysis
28 days to analysis

AnalysisAnalytical Method

Container Type andVolumeSample Volume or
Mass Required

Field Prep

Number of Containers

Preservation

PFOS/PFOA Compounds

EPA Method 537 Mod

250 mL HDPE

100 g

Homogenized2

Cool to 4ºC± 2ºC

Site-associated Compounds

Table 3+ Lab SOP

250 mL HDPE

100 g

Homogenized1

Cool to 4ºC± 2ºC

28 Days

14 days

Total Organic Carbon

Lloyd Kahn

4 oz glass

50 mg

Homogenized1

Cool to 4ºC± 2ºC

28 Days

28 DaysGrainsize Distribution

ASTM D422; D7928

16 oz glass

fill container

Homogenized

1

None

Sample to be sent to
TA Burlington

Sample to be sent to
TA Burlington

Moisture Content

ASTM D2216

2 oz glass

fill container

Homogenized

1

None

Sample to be sent to
TA Burlington

Sample to be sent to
TA Burlington

Archived for potential future
analyses

TBD

250 mL HDPE

fill container

Homogenized2

Cool to 4ºC± 2ºC

TBD

TBD

Archived for potential future
analyses

TBD

4 oz glass

fill container

Homogenized

4

Cool to 4ºC± 2ºC

TBD

TBD

Notes:HDPE - high density polyethylene
SOP - Standard Operating Procedure
N/A - not applicable

August 2019

Table 4
Quality Assurance/Quality Control Samples
Chemours Fayetteville Works, North Carolina

Geosyntec Consultants NC, PC

Field

MatrixAnalytical
MethodInvestigative
Samples(per event)

EPA Method
537 Mod24

1

1

Table 3+ Lab
SOP

24

1

1

Lab

Equipment
Blank
Trip Blank Field Blank(per day)(per shipment)(per day)Matrix Spike(per sample
group)

Lab
Replicate(per sample
group)Lab Control
Sample(per sample
group)

Isotope
Dilution
Analytes(everysample)Continuing
Calibration
Verification(beginning ofeach group)

1

1

1

1

32

1

1

1

1

1

N/A

1

Field
Duplicate(per 20
samples)

MethodBlank(per sample
group)

1

1

1

1

Sediment

Notes:
N/A - none available at present
SOP - Standard Operating Procedure

August 2019

Geosyntec Consultants NC, PC
Table 5
Criteria for Achieving Data Quality Objectives
Chemours Fayetteville Works, North Carolina

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 %Recovery25-150Calibration

CCV % Difference70-130Completeness% Complete

90

Precision

Accuracy

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

August 2019

Start ofCape FearRiver

CFR-RM-20
USGS Gauge
02102500

Willis Creek
Mouth

CFR-RM-52
USGS Gauge
02104000

CFR-RM-76.2

Site River
Water Intake
Outfall 002
W.O. Huske Dam

Chemours
Fayetteville
Works

USGS Gauge
02105500

CFR-RM-77.25

Old Outfall
Channel Mouth

CFR-RM-84
00.5

Georgia Branch
Creek Mouth
1 Miles

CFR-RM-100

CFR-RM-116

Cape Fear Lockand Dam #1 /Kings Bluff
Intake Canal

CFR-RM-132
USGS Gauge
02105769

LegendSampling Transect
USGS Stream Gauge
Site Features
Chemours Fayetteville Works
Cape Fear River
Notes:
1. Sample IDs shown here are abbreviations, see Characterization
Plan for full sample IDs.
2. Basemap source provided by ESRI OpenStreetMap
contributors, and the GIS User Community

8

4

0

8 Miles

Proposed Sampling Transect Locations
Chemours Fayetteville Works, North Carolina

FigureRaleigh

August 20191

CFR-RM-20

0

5

10 Miles

Ca

pe

Fe
ar
R

iv e

r

USGS Gauge
02102500

CFR-RM-20

300

LegendUSGS Stream Gauge
Conceptual Sampling Location in Transect
Chemours Fayetteville Works
Notes:
1. Sample IDs shown here are abbreviations, see Characterization
Plan for full sample IDs.
2. Basemap source provided by ESRI OpenStreetMap
contributors, and the GIS User Community

150

0

300 Feet

Conceptual Layout of Transect
Sampling Location

Chemours Fayetteville Works, North Carolina

FigureRaleigh

August 20192