Consent Order Progress Report For
Third Quarter 2020

Submissions to the State of North Carolina and Cape Fear River Watch
The following table identifies submissions made by Chemours pursuant to the Consent Order and
Addendum (“COA”) for the period of July 1, 2020 through the end of the third quarter on
September 30, 2020. 1
COSection
11c

Title
PFAS Characterization Quarterly Report

Submitted
Date
07/31/2020

12/COA 04d

Stormwater Pollution Prevention Plan

07/01/2020

12/COA 01a

Cape Fear River PFAS Mass Loading Protocol

08/31/2020

12/COA 01b

Files for Current PFAS Loading Model

08/31/2020

12/COA 01c

Outfall 002 PFAS Mass Loading Protocol

08/31/2020

12/COA 02a

Interim Seep Remediation System Plan

08/31/2020

12/COA 01b

09/30/2020

12/COA 04b

Cape Fear River PFAS Mass Loading Assessment 2020 Q2
Stormwater Treatment System Sampling Plan

09/30/2020

28

Quarterly Progress Report

07/21/2020

1 Consent Order submissions by Chemours from lodging of the Proposed Consent Order in November

2018 through March 31, 2019 were presented in the 2019 1st quarter report, April 1, 2019 throughJune 30, 2019 in the 2019 2nd quarter report, July 1, 2019 through September 30, 2019 in the 2019
3rd quarter report, October 1, 2019 through December 31, 2019 in the 2019 4th quarter report,
January 1, 2020 through March 31, 2020 in the 2020 1st quarter report, and April 1, 2020 throughJune 30, 2020 in the 2020 2nd quarter report.

Consent Order Progress Report For
Third Quarter 2020

2020 Third Quarter Residential Summary

Item
Total Number of Residences
SampledResidences Exceeding GAC
Criteria (GenX >= 140 ng/L)
Residences Exceeding RO
Criteria (∑PFAS >= 70 ng/L)
Residences Exceeding RO
Criteria (PFAS >= 10 ng/L)
Residences Drinking Water Well
Detections (Results < 10 ng/L)
Residences Drinking Water Well
Non-Detections

Cumberland
County(East of River)

Cumberland
County(West of River)

BladenCounty(East of River)

BladenCounty(West of River)

RobesonCounty

Total

239

430

4

9

37

719

3

3

0

2

0

8

68

80

0

5

11

164

94

135

0

0

11

240

22

77

0

1

5

105

52

135

4

1

10

202

Consent Order Progress Report For
Third Quarter 2020

Replacement Drinking Water Actions(Replacement drinking water actions from November 20182 - September 30, 2020)

2 The date the proposed Consent Order was lodged.

Consent Order Progress Report For
Third Quarter 2020

Consent Order Progress Details
This section summarizes the activities that have been undertaken by Chemours pursuant to theConsent Order Compliance Measures for the period from July 1, 2020 through the end of the third
quarter of 2020 (September 30, 2020). On August 13, 2020, Chemours signed the Addendum toConsent Order Paragraph 12, and the Addendum was entered by the Bladen County Superior Court on
October 12, 2020.

Section 7 Control Technology
Improvements
The thermal oxidizer (see photo at right)
continues to control process emissions at an
average PFAS destruction efficiency exceeding
99.99%.

Section 10 No Discharge of Process
Wastewater from Chemours’
Manufacturing Areas
Chemours continues to not discharge its processwastewater and to ship its process wastewater
offsite for disposal. Chemours is recycling
treated water internally within several
manufacturing processes.

Section 11 Characterization of PFAS in Process and Non-Process Wastewater andStormwater at the Facility
During the third quarter of 2020, Chemours’ consultant Geosyntec prepared the 2020 second quarter
report describing and analyzing characterization sampling of process water, non-process wastewaterand stormwater that occurred in April and June 2020. Chemours submitted the report to NCDEQ on
July 31, 2020. During the third quarter, sampling occurred on August 26, 2020. Geosyntec is preparing
the 2020 third quarter report for submission under separate cover by December 19, 2020 to include
data from this sampling event. This report will be the final quarterly report under Paragraph 11(c) for
the initial characterization period, with ongoing sampling to continue pursuant to Paragraph 11(d).
Paragraph 11(c) requires the final quarterly report to be submitted 18 months after the sampling
workplan was approved. December 19, 2020 is 18 months after June 19, 2019, when the sampling
workplan was approved by NCDEQ.

Section 11.2 Characterization of PFAS Contamination in River SedimentDuring the third quarter of 2020, Chemours’ contractors began preparing the SedimentCharacterization Report. The report was submitted to NCDEQ, Cape Fear River Watch, anddownstream water utilities on October 23, 2020.

Consent Order Progress Report For
Third Quarter 2020

Section 12 Accelerated Reduction of PFAS Contamination in the Cape Fear River andDownstream Water Intakes, and Addendum to Consent Order Paragraph 12
On September 30, 2020, Chemours started operation of the treatment system for the Old Outfall
pursuant to Consent Order Paragraph 12(e) and a NPDES permit issued by NCDEQ.
As noted above, during the third quarter of 2020, Chemours signed the Addendum to Consent Order
Paragraph 12. Chemours’ Addendum implementation activities during the third quarter included:
Consent Order Addendum Paragraph 1
On August 31, 2020, Chemours submitted to DEQ three items pursuant to Consent Order Addendum
Paragraph 1:• Cape Fear River PFAS Mass Loading Calculation Protocol (01(a));• The files used to prepare the most recent version of the Mass Loading Model(01(b)); and• Site Conveyance Network and Outfall 002 PFAS Mass Loading Calculation Protocol(01(c)(ii)).
On August 31, 2020, Chemours also began collecting the following samples:• Twice weekly, 24-hour composite samples from the Cape Fear River at the Tar Heel
Ferry Road bridge, including samples up to twice per month when more than 1.5” ofrainfall occurred, and recording flows at W.O. Huske Dam (01(a)(i)(1-3)); and• Once weekly, 24-hour composite samples from Outfall 002, including samples whenmore than 1” of rain occurred (01(c)(i)).
On September 30th, Chemours submitted to DEQ the Cape Fear River PFAS Mass Loading Assessment –Second Quarter 2020 Report pursuant to Consent Order Addendum paragraph 01(b). This submission
was also pursuant to quarterly reporting of mass loading sampling outlined in the Corrective Action
Plan (Paragraph 16).
Consent Order Addendum Paragraph 2
On August 31st, Chemours submitted to DEQ the Interim Seep Remediation System Plan. In addition tosubmitting this plan, Chemours’ contractors advanced the design and required permit applications for
installing interim seep remediation systems.
Consent Order Addendum Paragraph 4
On July 1st, Chemours submitted to DEQ the Stormwater Pollution Prevention Plan.
On September 30th, Chemours submitted to DEQ the Stormwater Treatment System Sampling Plan.
Chemours’ internal engineering team and Chemours’ contractors also developed a plan during the third
quarter of 2020 to separate stormwater and non-contact cooling water flows in order to facilitate thefuture capture and treatment of stormwater in the Monomers/IXM area during storms producing
rainfall volumes and intensities up to 1” within a 24-hour period.

Section 14 Toxicity Studies
Chemours has all five Consent Order Attachment B substances synthesized. Four of the five test
substances have been delivered to the contract laboratory and the fifth is going through final
purification.

Consent Order Progress Report For
Third Quarter 2020
Mammalian Toxicology
There is little or no mammalian toxicology data available for these substances, therefore it wasnecessary to perform range finder studies prior to beginning the Consent Order studies. In thesestudies, rats and mice are dosed for two weeks and a number of toxicologically important endpoints
are measured. This data is necessary to set appropriate dose levels for the Consent Order studies. As
of September 30th, eight range finder studies (one rat study and one mouse study for each of the four
available test substances) have begun. When the final test substance is available, the range finder
studies for that substance can begin. Concurrently, the method for dose analysis is being developed.
This method will be submitted for approval by NCDEQ prior to the start of the 28-day Consent Orderstudies. The same method will be used for both the 28-day and 90-day studies. The protocols for the
28-day immunotoxicity studies are being finalized while Chemours is waiting for the range finder data.
The dose levels for the 90-day study depend on results obtained in the 28-day study; therefore thecurrent focus is on the 28-day study protocols.
Aquatic Toxicology
Protocols for the aquatic toxicity studies are being developed by the contract laboratory and will be
submitted to NCDEQ when available. Analytical method development for the analysis method is
beginning in October 2020; the final method will be submitted for approval by NCDEQ prior to thebeginning of the aquatic toxicology work.

Section 16 Groundwater Remediation
Chemours conducted a baseline mass loading monitoring event described in the Corrective Action Plan
(CAP) by collecting groundwater, surface water, and river samples and measuring flows in surface
water bodies at and around the Site in July 2020. These results will be described in the third quarterly
report for this program to be submitted by December 29, 2020 pursuant to Addendum to Consent
Order Paragraph 12, Paragraph 1(b).
During the third quarter, Chemours also collected groundwater samples from sitewide monitoring wells
and from Chemours’ installed offsite groundwater monitoring wells. These samples are presently
undergoing laboratory analysis and are planned to be reported to NCDEQ during the fourth quarter of2020.
On July 31st, Chemours submitted to DEQ the Cape Fear River Table 3+ PFAS Mass Loading Assessment– First Quarter 2020 Report as outlined in the CAP for quarterly reporting of mass loading sampling.
On September 30th, Chemours submitted to DEQ the Cape Fear River PFAS Mass Loading Assessment –Second Quarter 2020 Report as outlined in the CAP for quarterly reporting of mass loading sampling.
This submission was also pursuant to reporting requirements outlined in Consent Order Addendum
Paragraph 1(b).

Sections 19 and 20 Provision of Public Water Supplies, Whole Building Filtration
Systems, and Reverse Osmosis Drinking Water Systems
As shown in the summary tables above, Chemours continues to make significant progress in
implementing the Consent Order requirements of Paragraphs 19 and 20. Since resuming RO
installations in June 2020, following the COVID-19 postponement period, the pace of RO acceptanceConsent Order Progress Report For
Third Quarter 2020
rates and installations has been on the rise. O&M activities for installed GAC systems continues
uninterrupted. Bottled water delivery also continues uninterrupted, with three vendors serving 2,486
homes.

Section 21 Private Well Testing
The Adaptive Step Out and Infill Sampling Program has been ongoing since the 3rd quarter of 2019
(other than during the COVID-19 postponement period between March and May of 2020). Three toeight stages of step out sampling have occurred across the sectors and the current step out distanceintervals range from 5.5-6.5 miles to 13.5-14.5 miles from the Site. Results for some of the current
stage of Step Out sampling are still pending. Four of the sectors, 3, 6, 8, and 9, have been delineated(i.e., no further step outs for these sectors are needed) and an additional four, 5, 7, 14 and 15, are neardelineated (results pending). Distance intervals for current infill sampling for all sectors range from 2.57.5 miles to 5.5-14.5 miles from the Site.

Section 22 Provision of Sampling Results
Chemours provided (and continues to provide) sampling results to NCDEQ and residents as required
under the Consent Order. Chemours has provided sampling results to NCDEQ by sending a courtesy
email notification and by uploading sampling results to the state Equis database. Chemours has also
provided final lab reports to NCDEQ. Chemours has provided sampling results to residents by including
preliminary results with water filtration system initial offer letters and sending the final lab reports toresidents within the following 30 days. Chemours has also provided non-detect sampling results toresidents.

Section 23 Interim Replacement of Private Drinking Water Supplies
All residents eligible to receive the interim replacement drinking water supplies have received the
supplies (i.e., bottled water or voucher card for bottled water). As of September 30, 2020, there are
2,486 residences receiving bottled water.

Section 26 Total Organic Fluorine
Please see Appendix A for the quarterly progress report from Dr. Susan D. Richardson.

Section 28 Reporting
Chemours submitted the Consent Order 2nd quarter 2020 progress report on July 21, 2020.

Sections 29 and 30 Public Information
Chemours has continued to post its Consent Order submissions at
https://www.chemours.com/Fayetteville-Works/en-us/c3-dimer-acid/compliance-testing/.

Appendix A

4th Progress Report
Development of a Total Organic Fluorine (TOF) Method for the Analysis of Process
Wastewater Streams and Air from Fayetteville Works (NC)
Susan D. Richardson, Danielle C. Westerman, Alexandria L. Forster, and Ying Zhang
University of South Carolina
September 29, 2020
Since the last report on June 22, 2020 there have been several positive updates to our lab’s
instrumentation capabilities and working conditions. Because of the Covid-19 virus, theUniversity of South Carolina limited research hours in phases up until August 1, but sinceAugust 1, the University has allowed a full return to research without limitations. During theweek of August 17-21, a Thermo Fisher Scientific field engineer was able to come install a newion chromatography (IC) instrument, the Dionex Integrion HPIC System, and this engineer
conducted familiarization training for this instrument. During this training, it came to ourattention that the analytical/guard column set that was sent to our lab was not the correctcolumn for our needed applications, so a new set of columns were ordered, but did not arrive
until September 15.
1. Ion Chromatography Updates
1.1. IC Capability Improvements
The previous IC used for this TOF research project was the Dionex ICS-1600, which utilizes acarbonate eluent. Due to the high conductivity baseline with this eluent and the water dip(Figure 1), quantifying fluoride was problematic. After repair of a leak on the ICS-1600 system,
the fluoride peak moved closer to the water dip, which could hinder accurate quantification offluoride. As a result, we purchased the new Integrion IC system, which uses sodium hydroxide
as the eluent and eliminates the water dip (Figure 2) and lowers the background, allowing
improved detection and quantification of fluoride.

Conductivity (µS)

Water Dip

Time (min)Figure 1. Elution of fluoride by IC (IonPac AS9-HC carbonate eluent column).

Conductivity (µS)

Retention Time: 2.6 min

Time (min)Figure 2. Elution of fluoride by IC (Integrion HPIC AS28 hydroxide eluent column) using a sodium
fluoride standard to build a calibration curve for fluoride quantification.

1.2. IC Column Optimization
Experiments for percent recovery of total organic fluorine for several per-and polyfluoroalkyl
substances (PFAS) were conducted using an AS16, 4 µm analytical and guard column pair with
35 mM NaOH eluent concentration. The chromatograms from these experiments all showed
fluoride peaks coeluting with another anion (Figure 3), but the coeluting peak did not appear in
the blanks. Considering several factors, such as the similar affinities of fluoride and acetate withthe solid phase of the AS-16 columns, as well as the chemical structures of the standards
tested, the coeluting peak could potentially be acetate. Even with a gradient of the hydroxideeluent, the two peaks were unsuccessfully separated. In order to better detect fluoride, theThermo AS28 4µm analytical and guard columns were installed. The fluoride peaks for recovery

Conductivity (µS)

experiments have not presented any coeluting peaks thus far.

Coelutinganion

Time (min)Figure 3. Chromatogram of a fluoride peak resulting from 50 ppb PFOA standard tested forpercent recovery of absorbable organic fluorine (AOF) with the Dionex Integrion (AS16 35 mMhydroxide eluent).

Conductivity (µS)

Time (min)Figure 4. Chromatogram of the fluoride peak resulting from 50 ppb PFOA standard tested forpercent recovery of AOF with the Dionex Integrion (AS16 55mM hydroxide eluent).

2. Absorbable Organic Fluorine Optimization
2.1. Absorption Solution Optimization
After the process of combustion, off gasses are bubbled into an aqueous solution referred to as
the absorption solution. This solution should have the ability to efficiently cleanse the offgasses of fluoride, should be compatible with the IC analysis (i.e. does not interfere with thefluoride peak), and potentially contain a reducing agent in case any halides are oxidized tohalogens. Currently experiments with varying compositions and concentrations of absorbing
solutions are being conducted. At the time of this report, three different buffer solutions(carbonate, phosphate, and ammonium hydroxide) are being tested at 1 mmol with andwithout hydrogen peroxide as a reducing agent. A standard mix of 10 µL of 100 µg/L as F - ofthree PFAS standards was injected into the ceramic boats containing quartz wool. Future work
will include varying the concentration of these buffers and hydrogen peroxide to be used, as
well as testing 18MΩ water with and without hydrogen peroxide. Considering the weak bond
between two fluorine atoms compared to the strong polar bond in HF, 18MΩ water alone
might be sufficient as an absorption solution. Results of this experiment will be included in thenext monthly meeting with Chemours on October 8 since they are currently being analyzed byIC.
2.2. Activated Carbon Columns Breakthrough Test
While testing the recovery for several PFAS standards, the two carbons used in line per sample
were placed into separate ceramic boats and the off-gas from combustion was collected inseparate vials for IC analysis in order to understand the organic fluorine breakthrough potential
into the second carbon. This test is to ensure that organic fluorine is not being rinsed throughboth carbons and out to waste, which would therefore lower percent recoveries. Standard
consensus requirements for breakthrough is that the total organic halogen in the second
carbon should be less than 10% of the sum of the two carbons in line. For this set ofexperiments, only two carbons were placed in line and 50 mL of sample was passed througheach column, followed by 10 mL of potassium nitrate rinsing solution (Figure 5). The pH ofthese samples was adjusted to a pH <1 with nitric acid before rinsing through the columns assuggested by previous work.

Table 1. Recoveries and breakthrough of three PFAS standards*
CompoundAOF Percent Recovery (µg/L)

Carbon 2 BreakthroughPercent

Gen X

66%

8.2%

PFOS

72%

10.3%

PFOA

65%

12.9%

*Experiments were done in triplicate and blank subtracted. The pH was lowered to a pH <1
before passing water over carbons.

Total Organic Fluoride

Mean Fluoride Concentration ± Standard
Deviation (µg/L)

60
50

GenX
40

PFOA
PFOS

30
20
10
0

1

1
2

2

Acticated Carbon Column Number

1

2

Figure 5. Fluoride breakthrough analysis of two activated carbons in series from three PFAS
compounds.

3. Upcoming Absorbable Organic Fluorine WorkWork will continue to be done towards optimizing the percent recoveries for total AOF. Someof these parameters include a further in-depth analysis of the sample pre-treatment including
effect the pH of the samples has on fluorine recovery, which acid should be used to drop the pHof samples, and optimal sample holding time and temperature. Experiments will be done to test
the composition and pH of the solution rinse that removes inorganics from the carbon columns.
Currently, potassium nitrate is used. Several combustion factors, such as carrier gas flow rate,
combustion temperature, and time, will also be investigated.
4. Liquid Chromatography-High Resolution Mass Spectrometry Experiments
A mix of 26 standards (some purchased, some provided by Chemours) was analyzed at an initialconcentration of 500 ppb in 50:50 MeOH:water, utilizing an ultrahigh performance liquid
chromatograph coupled to an Agilent 6545 quadrupole time-of-flight (UHPLC-QTOF) mass
spectrometer with electrospray ionization in negative ion mode (ESI-). A full scan-MS analysis
was utilized for quantification due to the increased sensitivity of the QTOF instrument in MS
mode relative to product ion-MS/MS. The mass spectrometer was operated at a fragmentation
voltage of 110 V, capillary voltage 4000 V, gas temperature 300 °C, drying gas 12 L min −1, andnebulizer pressure of 35 psi. The scan range was from m/z 50 to 1300. UHPLC parameters areshown in Table 2.

Table 2. UHPLC Parameters
Parameter
Value
Instrument
1290 Infinity II UHPLC Binary Pump
A) 0.1% acetic acid in water
Mobile PhaseB) 0.1% acetic acid in methanol
Gradient
Time (min)
%B
0
5
14
95
15
100
18
100
18.1
5
25
5
Flow rate
0.4 mL/min
ColumnAgilent Zorbax RRHD Stable Bond C18 (50 x 2.1 mm, 1.8 µm)
Temperature 50 °C
Injection
10 µL
VolumeOnce a full scan spectrum is extracted for a detected standard, a mass match score (Table 3) isthen calculated based on the accurate mass, isotope distribution and isotope spacing. The scoreis defined as weighted aggregate of the three individual metrics, therefore, it is based on not
only the mass accuracy, but also the isotopic fidelity. Mass spectra with a mass difference of ±5
ppm and a score greater than 75 were considered of interest and reported below.

Table 3. UHPLC-High Resolution-MS Analysis of PFAS Standards
Name

Formula

PFDA
PFUdA
PFDoA
PFTeDA
PFPrA
PFBA
PMPA
PFBS
NVHOS
PFPeA
PEPA
PFO3OA
PFHxA
GenX
PFHxS
R-PSDCA
PFHpA
R-PSDA
HydrolizedPSDA
EVE Acid
PFOA
PFOS
R-EVE
Hydro-EVE Acid
PFNA
HFPO-TA

C10 H F19 O2
C11 H F21 O2
C12 H F23 O2
C14 H F27 O2
C3 H F5 O2
C4 H F7 O2
C4 H F7 O3
C4 H F9 O3 S
C4 H2 F8 O4 S
C5 H F9 O2
C5 H F9 O3
C5 H F9 O5
C6 H F11 O2
C6 H F11 O3
C6 H F13 O3 S
C6 H2 F12 O4 S
C7 H F13 O2
C7 H2 F12 O6 S

Observed Calculated Theoretical Diff
m/z
Mass
Mass
(ppm)
512.9600 513.9673
513.9673
0.02
562.9577 563.9651
563.9641
1.65
612.9546 613.9618
613.9609
1.35
712.9475 713.9554
713.9545
1.23
162.9824 163.9897
163.9897
0.34
212.9792 213.9865
213.9865
0.09
228.9739 229.9811
229.9814 -1.28
298.9430 299.9502
299.9503 -0.20
296.9473 297.9540
297.9546 -2.19
262.9756 263.9831
263.9833 -0.69
278.9706 279.9779
279.9782 -1.19
310.9606 311.9680
311.9680
0.02
312.9727 313.9799
313.9801 -0.46
328.9679 329.9754
329.975
1.25
398.9369 399.9440
399.9439
0.39
396.9408 397.9480
397.9482 -0.57
422.9911 363.9772
363.97690.86
440.9310 441.9383
441.9381
0.48

99.4
98.2
98.5
98.9
99.9
99.7
87.3
99.5
99.5
94.9
87.3
86.2
99.8
94.7
99.5
77.2
99.0
99.4

RT
(min)
11.55
12.17
12.73
5.48
11.11
9.25
3.09
5.87
4.26
5.48
6.10
7.83
7.58
10.81
9.06
8.85
7.39
3.34

C7 H3 F11 O7 S

438.9353

439.9426

439.9424

0.53

99.6

4.21

C8 H F13 O4
C8 H F15 O2
C8 H F17 O3 S
C8 H2 F12 O5
C8 H2 F14 O4
C9 H F17 O2
C9 H F17 O4

406.9597
412.9665
498.9312404.9637
426.9653
508.9690
540.9591

407.9670
413.9738
499.9383
405.9710
427.9727
463.9708
495.9609

407.9667
413.9737499.9375
405.9711
427.9730
463.9705
495.9603

0.72
0.15
1.70
-0.12
-0.65
0.66
1.13

99.5 9.66
98.9 9.97
98.1 10.39
99.7 3.11
97.9 9.12
99.3 9.13
98.7 9.49

Score

All standards were detected with high mass accuracy, with all but 4 compounds (PMPA, PEPA,
PFO3OA, and Byproduct 6) having a mass match score greater than 94. Compounds PEPA andPFO3OA were found to have the lowest sensitivity in this method, which may explain therelatively low mass accuracy (87.4, and 77.2, respectively). Especially with respect to these twocompounds, further method optimization is required before quantifying all compounds via
UHPLC-QTOF.