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HomeMy WebLinkAbout2020.03.27_CCO.p7_Thermal Oxidizer Permformance Test Report THERMAL OXIDIZER PERFORMANCE TEST REPORT CHEMOURS COMPANY FAYETTEVILLE WORKS PREPARED FOR: THE CHEMOURS COMPANY FAYETTEVILLE WORKS PLANT 22828 NC HWY 87 WEST FAYETTEVILLE, NC 28306 MARCH 2020, REVISION 0 FOCUS PROJECT NO. P-001393 PREPARED BY: FOCUS ENVIRONMENTAL INC. 4700 PAPERMILL DRIVE KNOXVILLE, TENNESSEE 37909 (865) 694-7517 http://www.focusenv.com The Chemours Company Fayetteville Facility Thermal Oxidizer Test Report Revision: 0, March 2020 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc i Focus Project No. P-001393 Tables of Contents 1.0 EXECUTIVE SUMMARY .................................................................................................................... 1 2.0 INTRODUCTION ................................................................................................................................ 2 2.1 FACILITY BACKGROUND INFORMATION .............................................................................. 2 2.2 BRIEF ENGINEERING DESCRIPTION .................................................................................... 2 2.3 THERMAL OXIDIZER TEST PROTOCOL DEVELOPMENT ................................................... 2 2.3.1 Test Plan Target Compounds ...................................................................................... 3 2.3.2 Sampling and Analytical Design Basis ......................................................................... 3 2.3.3 Developed Sampling Methods ..................................................................................... 4 2.3.3.1 Modified Method 18 Sampling ...................................................................... 4 2.3.3.2 Modified Method 0010 Sampling .................................................................. 5 2.3.4 Sampling Locations and Methods ................................................................................ 6 2.3.4.1 Waste Gas Feed Line Sampling ................................................................... 6 2.3.4.2 Stack Gas Modified Method 18 Sampling .................................................... 7 2.3.4.3 Stack Gas Modified Method 0010 Sampling ................................................ 7 2.3.5 Sample Analyses .......................................................................................................... 7 2.3.5.1 Waste Gas Line Analyses ............................................................................. 7 2.3.5.2 Stack Gas Method 18 Analyses .................................................................... 8 2.3.5.3 Stack Gas Method 0010 Analyses ................................................................ 8 2.3.6 PFAS Feed and Stack Emission Rates ........................................................................ 9 2.3.7 Other Sampling and Analysis ....................................................................................... 9 3.0 TEST PROGRAM SUMMARY ......................................................................................................... 16 3.1 PERFORMANCE OBJECTIVE ................................................................................................ 16 3.2 TEST IMPLEMENTATION SUMMARY ................................................................................... 16 3.3 TEST OPERATING OBJECTIVES .......................................................................................... 16 3.4 DEVIATIONS FROM THE TEST PLAN .................................................................................. 16 4.0 TEST RESULTS ............................................................................................................................... 21 4.1 TEST DATA REDUCTION BASIS ........................................................................................... 21 4.2 WASTE GAS CHARACTERIZATION AND TARGET PFAS COMPOUND FEED RATES .......................................................................................................................... 21 4.3 TARGET PFAS COMPOUND STACK EMISSION RATES .................................................... 24 4.3.1 Modified Method 0010 Measured Emissions ............................................................. 24 4.3.2 Modified Method 18 Measured Emissions ................................................................. 25 4.4 TOTAL PFAS DESTRUCTION EFFICIENCY ......................................................................... 26 5.0 QUALITY CONTROL ........................................................................................................................ 36 5.1 WASTE GAS SAMPLING ........................................................................................................ 36 5.1.1 Modified Method 18 Capture Efficiency ...................................................................... 36 The Chemours Company Fayetteville Facility Thermal Oxidizer Test Report Revision: 0, March 2020 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc ii Focus Project No. P-001393 5.1.2 Monomer Waste Gas Sampling ................................................................................. 36 5.1.3 Polymer Waste Gas Sampling ................................................................................... 37 5.2 WASTE GAS ANALYSES ....................................................................................................... 37 5.2.1 Monomer Waste Gas Analyses .................................................................................. 37 5.2.2 Polymer Waste Gas Analyses .................................................................................... 38 5.3 STACK GAS SAMPLING ........................................................................................................ 38 5.3.1 Stack Gas Modified Method 18 Results ..................................................................... 38 5.3.2 Stack Gas Modified Method 0010 Results ................................................................. 39 5.3.3 Positive HFPO-DA Results ......................................................................................... 40 5.4 PROCESS WATER ANALYSES ............................................................................................. 40 5.5 OTHER ADDITIONAL TESTING PERFORMED ..................................................................... 41 5.6 OVERALL DATA QUALITY ASSESSMENT ........................................................................... 42 6.0 CONCLUSION .................................................................................................................................. 59 The Chemours Company Fayetteville Facility Thermal Oxidizer Test Report Revision: 0, March 2020 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc iii Focus Project No. P-001393 List of Tables Table 1-1. Thermal Oxidizer Total PFAS Destruction Efficiency ................................................................. 1 Table 2-1. Properties and Structures of Target Destruction Efficiency PFAS Compounds ....................... 10 Table 2-2. Analysis and Reporting Convention for Test Samples ............................................................. 11 Table 3-1. Thermal Oxidizer Performance Test Sampling and Analysis ................................................... 17 Table 3-2. Thermal Oxidizer Performance Test Sampling Dates and Times ............................................ 20 Table 3-3. Thermal Oxidizer Performance Test Operating Data ............................................................... 20 Table 4-1. Thermal Oxidizer Monomer Tank Feed (Line #1) Summary Analyses .................................... 28 Table 4-2. Thermal Oxidizer Polymer Tank Feed (Line #2) Summary Analyses ...................................... 29 Table 4-3. Thermal Oxidizer Monomer Tank (Line #1) Sampling Results and Feed Rates ..................... 30 Table 4-4. Thermal Oxidizer Polymer Tank (Line #2) Sampling Results and Feed Rates ........................ 31 Table 4-5. Thermal Oxidizer Modified Method 0010 Stack Emissions Sampling Results ......................... 32 Table 4-6. Thermal Oxidizer Stack Gas Modified Method 18 Sample Summary Analyses ...................... 33 Table 4-7. Thermal Oxidizer Modified Method 18 Stack Emissions Sampling Results ............................. 35 Table 4-8. Thermal Oxidizer Total PFAS Destruction Efficiency ............................................................... 35 Table 5-1. Monomer Waste Gas (Line #1) Method 8260B Analysis Surrogate Recoveries ..................... 43 Table 5-2. Monomer Waste Gas (Line #1) Method 537 Analysis IDIS Recoveries .................................. 44 Table 5-3. Polymer Waste Gas (Line #2) Method 8260B Analysis Surrogate Recoveries ....................... 45 Table 5-4. Polymer Waste Gas (Line #2) EPA Method 537 Analysis IDIS Recoveries ............................ 46 Table 5-5. Stack Gas Modified Method 18 Analysis Surrogate Recoveries .............................................. 47 Table 5-6. Stack Gas Modified Method 0010 Analysis IDIS Recoveries ................................................... 48 Table 5-7. Thermal Oxidizer Modified Method 0010 Analysis Results ...................................................... 49 Table 5-8. Thermal Oxidizer Process Water Analyses .............................................................................. 50 The Chemours Company Fayetteville Facility Thermal Oxidizer Test Report Revision: 0, March 2020 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc iv Focus Project No. P-001393 List of Figures Figure 2-1. Thermal Oxidizer Process Flow Schematic ............................................................................. 12 Figure 2-2. Modified Method 18 Sampling Train Schematic ...................................................................... 13 Figure 2-3. Modified Method 0010 Sampling Train Schematic .................................................................. 14 Figure 2-4. Installed Waste Gas Sampling Point Schematic ..................................................................... 15 Figure 5-1. Monomer Waste Gas (Line #1) Modified Method 18 Condensable Vapor Capture Efficiency 51 Figure 5-2. Polymer Waste Gas (Line #2) Modified Method 18 Condensable Vapor Capture Efficiency . 52 Figure 5-3. Monomer Waste Gas (Line #1) Modified Method 18 COF2 Capture ....................................... 53 Figure 5-4. Monomer Waste Gas (Line #1) Modified Method 18 HFPO Capture ...................................... 54 Figure 5-5. Monomer Waste Gas (Line #1) Modified Method 18 HFPO-DA Capture ............................... 55 Figure 5-6. Polymer Waste Gas (Line #2) Modified Method 18 HFPO-DAF Capture ............................... 56 Figure 5-7. Polymer Waste Gas (Line #2) Modified Method 18 Fluoroether E-1 Capture ........................ 57 Figure 5-8. Polymer Waste Gas (Line #2) Modified Method 18 HFPO-DA Capture ................................. 58 List of Attachments (Provided on Compact Disk) Thermal Oxidizer Control Efficiency Test Report, Test Dates 28-29 February 2020, Weston Solutions, Inc., 400 Weston Way P.O. Box 2653, West Chester, PA 19380, March 2020. Thermal Oxidizer Control Efficiency Test Report, Test Dates 4-5 February 2020, Weston Solutions, Inc., 400 Weston Way P.O. Box 2653, West Chester, PA 19380, March 2020. Thermal Oxidizer Control Efficiency Test Report, Test Dates 3-4 January 2020, Weston Solutions, Inc., 400 Weston Way P.O. Box 2653, West Chester, PA 19380, March 2020. Laboratory analytical data packages for all of the above referenced test reports. The Chemours Company Fayetteville Facility Thermal Oxidizer Test Report Revision: 0, March 2020 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc v Focus Project No. P-001393 List of Acronyms amu atomic mass units ASTM American Society for Testing and Materials CaF2 calcium fluoride CF4 tetrafluoromethane CO carbon monoxide CO2 carbon dioxide COC chain of custody COF2 carbonyl difluoride DE destruction efficiency DQO data quality objective DMC dimethyl carbonate dscf dry standard cubic feet (EPA standard at 68oF, 1 atmosphere) dscm dry standard cubic meter (EPA standard at 68oF, 1 atmosphere) E-1 Heptafluoropropyl-1,2,2,2-tetrafluoroethyl ether (Fluoroether E-1) EPA Environmental Protection Agency HF hydrogen fluoride (gas) or hydrofluoric acid (aqueous) HFPO hexafluoropropylene oxide (HFPO), a.k.a., “HFPO monomer” or simply “monomer” HFPO-DA hexafluoropropylene dimer acid or C3-dimer, a.k.a., “HFPO dimer”, “dimer acid”, “dimer”, or Gen X HFPO-DAF hexafluoropropylene dimer acid fluoride, a.k.a., “HFPO dimer fluoride”, “dimer acid fluoride”, or simply “dimer fluoride” HFPO-DOCH3 HFPO dimer, methyl ester HPLC/MS/MS high performance precision liquid chromatography/tandem mass spectrometry hr hour GC/MS gas chromatography/mass spectrometry LCS laboratory control sample lpm liters per minute MDL method detection limit min minute MMBtu million British thermal units 2-MTP methyl-2-methoxy-tetrafluoro-propionate NCDAQ North Carolina Department of Air Quality N2 nitrogen O2 oxygen OPL operating parameter limit PFAS per- or poly-fluorinate alkyl substance PFOA perfluorooctanoic acid PFOS perfluorooctane sulfonic acid psia pounds per square inch absolute (psig + atmospheric pressure) psig pounds per square inch gauge QA quality assurance QC quality control RFA request for analysis RL reporting limit RPD relative percent difference RSD relative standard deviation SOP standard operating procedure SVOC semi-volatile organic compound TFE tetrafluoroethylene VOC volatile organic compound Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 1 Focus Project No. P-001393 1.0 EXECUTIVE SUMMARY This report presents the results of per- and poly-fluoroalkyl substance (PFAS) destruction efficiency (DE) performance testing conducted on the thermal oxidizer located at The Chemours Company FC, LLC (Chemours) facility, Fayetteville, North Carolina. Chemours was required by consent order to have a thermal oxidizer installed by December 31, 2019 to control PFAS process stream emissions from identified manufacturing operations at the facility. Per the consent order, “Chemours shall demonstrate that the thermal oxidizer controls all PFAS at an efficiency of 99.99%”. Chemours also holds a Title V permit which contains the same thermal oxidizer requirements and requires the testing protocol “to address how the Permittee will ensure the Thermal Oxidizer and 4-Stage Scrubber System will achieve the emission reduction [of 99.99%], including the use of a surrogate for all PFAS, such as the hexafluoropropylene oxide (HFPO).” A test plan delineating the thermal oxidizer DE performance test target operating conditions, and the sampling and analytical protocols, was submitted to the North Carolina Department of Air Quality (NCDAQ) on December 9, 2019. NCDAQ conditionally approved the test plan prior to a pre-test originally planned for December 27, 2019, but actually performed on January 3-4, 2020, and gave final approval of the test plan via letter dated January 27, 2020. Chemours conducted the thermal oxidizer performance test on February 28-29, 2020 in substantial conformance with the approved test plan. Please refer to Sections 2.3.1 and 3.4 for details. During the test, both the monomer and polymer manufacturing operations directed PFAS-bearing waste gases to the thermal oxidizer. The test program characterized the waste gas feed materials and measured the emission rates of five (5) target PFAS compounds: • HFPO (Hexafluoropropylene oxide), a.k.a., “HFPO monomer” or simply “monomer”, • HFPO-DA (Hexafluoropropylene Dimer Acid or C3-Dimer), a.k.a., “HFPO dimer”, “dimer acid”, “dimer” or “Gen X”, • HFPO-DAF (Hexafluoropropylene Dimer Acid Fluoride), • COF2 (Carbonyl Difluoride), and • Fluoroether E-1 (Heptafluoropropyl-1,2,2,2-tetrafluoroethyl ether). System DE performance was calculated based on the sum of the system inlet feed rates and sum of the stack emissions rates of these five (5) compounds. “Total PFAS” is the arithmetic sum of HFPO, HFPO- DA, HFPO-DAF, COF2, and Fluoroether E-1 under these conditions. The total PFAS DE results are summarized in Table 1-1. Table 1-1. Thermal Oxidizer Total PFAS Destruction Efficiency Chemours Company FC, LLC, Fayetteville, North Carolina, February 28-29, 2020 Run 1 Run 2 Run 3 Average 99.99982% 99.99974% 99.99986% 99.99981% The total PFAS DE performance exceeded 99.999% during all three (3) test runs. The balance of this report presents the details of the testing performed. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 2 Focus Project No. P-001393 2.0 INTRODUCTION 2.1 FACILITY BACKGROUND INFORMATION The Chemours Company FC, LLC (Chemours) manufactures chemicals, plastic resins, plastic sheeting, and plastic film at the facility located at 22828 NC Highway 87 West, Fayetteville, Bladen County, North Carolina (the facility). Under the consent order executed and filed February 25, 2019 Chemours was required to install a thermal oxidizer for control of per- and poly-fluoroalkyl substance (PFAS) process stream emissions from identified manufacturing operations identified at the facility by December 31, 2019. The application for the addition of the thermal oxidizer system to the facility Air Quality Permit 03735T43 was made on June 29, 2018. Construction began in November 2018. A test plan delineating the thermal oxidizer destruction efficiency (DE) performance test target operating conditions, and the sampling and analytical protocols, was and submitted to the North Carolina Department of Air Quality (NCDAQ) on December 9, 2019. NCDAQ gave approval of the test plan via letter dated January 27, 2020. This test report summarizes the thermal oxidizer DE performance test operating conditions, and the sampling and analytical test results. 2.2 BRIEF ENGINEERING DESCRIPTION The thermal oxidizer and its associated 4-stage scrubber are identified in the Air Quality Permit respectively as control devices NCD-Q1 and NCD-Q2. Please refer to Figure 2-1. The thermal oxidizer is a 10 million BTU per hour (MMBtu), natural gas-fired device. Waste gases from the manufacturing operations process streams are collected via header systems, compressed and delivered by pipeline to the thermal oxidizer for destruction of the entrained PFAS compounds. Thermal oxidizer emissions are treated in the scrubber system to control hydrogen fluoride (HF) generated by PFAS compound combustion. The scrubber system consists of a 4-stage packed bed column with three water scrubbing stages and one caustic scrubbing stage. 2.3 THERMAL OXIDIZER TEST PROTOCOL DEVELOPMENT The properties of each PFAS compound are sufficiently unique such that no singular sampling and analysis approach is appropriate for a comprehensive characterization of all PFAS compounds handled at Chemours Fayetteville Works. The physical and chemical properties of each of the potential target PFAS compounds must be considered when developing a sampling and analytical protocol. The sampling and analytical protocols employed for this test program were developed by Chemours through consultation with Eurofins TestAmerica, Inc. (analytical contractor) and Weston Solutions, Inc. (sampling contractor). Prior to the thermal oxidizer DE performance test, the methodologies were developed and evaluated by sampling the target PFAS compounds at an existing scrubber unit used to control PFAS emissions at the facility. The technical discussion presented in the following sections Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 3 Focus Project No. P-001393 underlies the sampling and analytical technical basis used to conduct this performance test, and the performance conclusions derived from the results presented in this test report. 2.3.1 Test Plan Target Compounds The thermal oxidizer DE performance test program was designed to provide a basis for the characterization of site-specific target PFAS compounds. The original four (4) target compounds were: • HFPO (Hexafluoropropylene oxide), a.k.a., “HFPO monomer” or simply “monomer”, • HFPO-DA (Hexafluoropropylene Dimer Acid or C3-Dimer), a.k.a., “HFPO dimer”, “dimer acid”, “dimer” or “Gen X”, • HFPO-DAF (Hexafluoropropylene Dimer Acid Fluoride), and • COF2 (Carbonyl Difluoride). A fifth compound, heptafluoropropyl-1,2,2,2-tetrafluoroethyl ether (a.k.a., Fluoroether E-1), was added to the test scope subsequent to the initial submission of the test plan to NCDAQ. Table 2-1 presents a summary of the chemical composition and structural information, and key chemical and physical property data for the five (5) target PFAS compounds targeted for this test program. The base compounds handled and used at the Fayetteville facility are HFPO and HFPO-DA. HFPO-DAF is a synthetic precursor to HFPO-DA in the chemical process. The molecular structure of HFPO-DAF is identical to HFPO-DA except fluorine (F) is substituted in place of the hydroxyl (-OH) group. This difference between HFPO-DA and HFPO-DAF has substantial impact on the physical properties and chemical reactivity of these otherwise structurally similar compounds. An additional reactant compound, COF2, is a major constituent in the waste gas. Fluoroether E-1 is a thermal decarboxylation product of HFPO-DA and appears as an intermittent major constituent in the waste gas. The combined feed rates to the thermal oxidizer and the concurrently measured emission rates of HFPO, HFPO-DA, HFPO-DAF, COF2, and Fluoroether E-1 from the thermal oxidizer were established to demonstrate PFAS DE performance. 2.3.2 Sampling and Analytical Design Basis HFPO, HFPO-DAF, and COF2 react with methanol (MeOH) to form ester compounds as depicted below: • HFPO + MeOH → 2-MTP + 2HF • HFPO-DAF + MeOH → HFPO-DOCH3 + HF • COF2 + 2MeOH → DMC + 2HF. The 2-MTP stands for methyl-2-methoxy-tetrafluoro-propionate. The HFPO-DOCH3 stands for HFPO dimer, methyl ester. The DMC stands for dimethyl carbonate. All three (3) ester compounds are analyzed via SW-846 Method 8260. The sampling and analytical strategy for HFPO, HFPO-DAF, and Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 4 Focus Project No. P-001393 COF2 is designed based on the reaction of these compounds with methanol to form derivative reaction products, and quantifying them based on analysis of their reaction products. The Fluoroether E-1 and HFPO-DA sampling and analytical strategy was designed based on capturing the compounds via condensation and dissolution in the methanol impingers. Fluoroether E-1 is captured as a volatile organic compound (VOC), and then quantified via direct analysis using SW-846 Method 8260. HFPO-DA is captured as a semi-volatile organic compound (SVOC) and then quantified via direct analysis using EPA Method 537. 2.3.3 Developed Sampling Methods Two (2) sampling methods were developed and employed for this test program. Please refer to Figures 2-2 and 2-3. One method is based on EPA Method 18. The second is based on SW-846 Method 0010. The following sections describe the sampling methods, the associated specialized techniques, and their application during this test program. 2.3.3.1 Modified Method 18 Sampling The Modified Method 18 sampling method is described in Weston’s Thermal Oxidizer Control Efficiency Test Report, Test Dates 28-29 February 2020 included as an attachment to this test report. The Modified Method 18 (MM18) sampling train consists of six (6) PFA fluoropolymer impingers and connectors configured in series. The impingers are charged with methanol. For sampling, the impingers are immersed in a methanol bath chilled using dry ice to maintain a temperature of -73oC (-100oF) or less. The principle of operation is to capture the target PFAS compounds by condensation and/or chemical reaction within the methanol media. The six (6) successive impingers are designed to provide sufficient condensing, absorbing, and reaction capacity to capture the target PFAS analytes. The sampling train is connected to a dry gas meter sampling system to measure the volume of dry gas sampled. At the conclusion of a test run, the six (6) sampling train impingers are recovered as discrete (individual) samples and analyzed separately. The Modified Method 18 sampling method captures the target PFAS compound vapors via condensing and/or reaction with methanol as the sampled gas is sparged through the successive chilled methanol matrix. Two (2) of the five (5) target compounds, Fluoroether E-1 and HFPO-DA, are captured by simply condensing them from the gas stream and dissolving them in methanol. Three (3) of the five (5) compounds, HFPO, HFPO-DAF, and COF2, react with the methanol to form ester compounds as previously described. The HFPO and COF2 have respective boiling points of -28oC and -85oC, but their reaction with methanol to form the higher boiler point derivative ester compounds is key to facilitating the measurement of these compounds. The boiling points of the ester compounds formed from HFPO and COF2 are higher and therefore easier to recover and retain similar to standard EPA volatile organic Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 5 Focus Project No. P-001393 compound (VOC) analytes. Post-sampling preservation of these samples is by refrigeration using wet ice to 4oC. 2.3.3.2 Modified Method 0010 Sampling Based on its boiling point of 151oC, HFPO-DA is classified by EPA as a semi-volatile organic compound (SVOC) that can potentially condense and possibly attach to particulate matter. Therefore, to accurately measure the stack emissions of HFPO-DA, the sampling is conducted using an iso-kinetic sampling method. A thorough presentation of the Modified Method 0010 sampling method is described in Weston’s Thermal Oxidizer Control Efficiency Test Report, Test Dates 28-29 February 2020 included as an attachment to this test report. The sampling train is generally configured like a standard Method 0010 sampling train with a heated probe and filter, condenser coil, XAD-2 resin cartridge, deionized water impingers, and a silica gel impinger. An added feature is a second XAD-2 resin cartridge located between the last deionized water impinger and the silica gel impinger. The purpose of the second XAD-2 resin cartridge is to act as a quality indicator to assess possible target analyte breakthrough. Other specialized aspects of the Modified Method 0010 sampling are: • During sampling collection, the sampling probe temperature is maintained a few degrees above the dew point of the moisture in the gas stream, well below the normal Method 5 operating temperature range of 248oF (120oC) (to preclude thermal decarboxylation of HFPO- DA to form Fluoroether E-1) • Maintaining the coil condenser and XAD-2 resin jacket as cold as reasonably possible below the normal Method 0010 prescribed maximum of 68oF (20oC) temperature for best possible conditions for HFPO-DA retention on the resin, and • Use of 95% methanol / 5% NH4OH solution as the recovery solvent for the rinsing of sampling train components to recover HFPO-DA from glassware surfaces. A total of seven (7) sample fractions are generated during the Modified Method 0010 sampling train recovery: • Particulate filter • Solvent (95% methanol / 5% NH4OH) rinses of the probe, nozzle, and the front-half of the filter holder • Primary XAD-2 resin tube • Back-half of the filter holder, coil condenser, and connecting glassware 95% methanol / 5% NH4OH solvent glassware rinses • Condensate and impinger contents of Impingers #1, #2 and #3 charged with deionized (DI) water and includes DI water rinses of the glassware • Impingers #1, #2 and #3 solvent (95% methanol / 5% NH4OH) glassware rinses as a separate sample (NOT combined with the impinger water and DI water rinses), and • Breakthrough XAD-2 resin tube. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 6 Focus Project No. P-001393 2.3.4 Sampling Locations and Methods The test program sampling campaign was designed to characterize the feed materials to the thermal oxidizer and the corresponding emissions of the target PFAS compounds. The sampling locations are: 1) the monomer waste gas feed line (Line #1), 2) the polymer waste gas feed line (Line #2), and 3) the thermal oxidizer/scrubber stack. The sampling techniques used at each location are discussed in the following sections. During testing, all locations were sampled concurrently. 2.3.4.1 Waste Gas Feed Line Sampling The two (2) waste gas feed lines to the thermal oxidizer were sampled separately at points on the 3-inch lines from the accumulator tanks to the thermal oxidizer. The gas pressure in these lines is nominally 10- 30 psig. To perform the sampling, Chemours designed, fabricated, and installed permanent sampling probes in these lines. Please refer to Figure 2-4. The permanently installed probes include a nozzle centered in the line and oriented to face into the stream flow, similar to the orientation of an isokinetic sampling probe when sampling stack gas. The installed sampling probe apparatus includes Swagelok® connectors that allow for connection of the sampling trains to the feed lines without line breaks. Ball valves allow for starting and stopping the flow of pressurized gas. The “bleed” connection allows for connection to a compressed nitrogen line to purge and clear the sampling location of any buildup of liquid or debris prior to sampling, and after sampling is completed. The previously described Modified Method 18 sampling train was used to sample the waste gas lines for the five (5) target PFAS compounds: HFPO, HFPO-DA, HFPO-DAF, COF2, and Fluoroether E-1. The sampling train meter box includes a needle control valve. No vacuum pump is required; the waste gas feed line pressure provides the sampled gas motive force. The meter box needle control valve is used to throttle and control the flow rate of the waste gas through the sampling train. The dry gas meter is used to measure the dry gas flow rate and the total volume of dry inert gas sampled. The two (2) waste gas feed lines were sampled concurrently using two sampling trains, one on each of the waste gas feed lines. The target sampling rate was maintained at approximately 0.50 liters per minute. Waste gas feed lines sampling was also performed concurrently with the stack gas emissions sampling at the thermal oxidizer stack. Dry gas meter flow, pressure, and temperature data were used to determine the total mass of dry gas sampled. Nitrogen is used in the system as the inert sweep gas for the waste gases in the vent header systems. Therefore, the waste gas dry gas composition was assumed to be 100% nitrogen and assigned a molecular weight of 28 amu. Pre- and post- sampling impinger differential weights were used to determine the mass of organic constituent vapors condensed in the sampling train from the sampled waste gases. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 7 Focus Project No. P-001393 2.3.4.2 Stack Gas Modified Method 18 Sampling A Modified Method 18 sampling train was used to sample the stack gas for four (4) of the five (5) target PFAS compounds: HFPO, HFPO-DAF, COF2, and Fluoroether E-1. The Modified Method 18 sampling protocol is similar as described for the waste gas feed lines except use of a vacuum pump equipped metering system was required to draw the sampled stack gas through the sampling train. The target sampling rate was 1.5-2.0 liters per minute. Dry gas meter flow, pressure, and temperature data were used to determine the total volume of dry gas sampled. Dry gas molecular weight was determined via Method 3A analysis of the dry gas meter exhaust. 2.3.4.3 Stack Gas Modified Method 0010 Sampling As previously noted, HFPO-DA is classified as a SVOC by EPA that can potentially condense and/or attach to particulate matter. The HFPO-DA stack emissions are sampled iso-kinetically using a modified SW-846 Method 0010 sampling train as previously described. The Modified Method 0010 sampling train was operated for 180 minutes during each sampling run to sample a minimum volume of three (3) dry standard cubic meters (dscm). The stack sampling location traverse points were determined and performed in accordance with EPA Method 1. Stack velocity and flow rate were determined based on EPA Method 2 (pitot tube) measurements. Dry gas meter flow, pressure, and temperature data were used to determine the total volume of dry gas sampled. Dry gas molecular weight was determined via Method 3A analysis of the dry gas meter exhaust. Impinger moisture gain was used to determine stack gas moisture content per EPA Method 4. 2.3.5 Sample Analyses Waste line and stack gas samples are analyzed as described in the following sections. 2.3.5.1 Waste Gas Line Analyses The characterization of the five (5) target PFAS compounds in the waste gas feed lines was determined via analysis of the Modified Method 18 impinger contents. Please refer to Table 2-2. HFPO, HFPO-DAF, COF2, and Fluoroether E-1 were determined using Method 8260B analysis. HFPO, HFPO-DAF, and COF2 were quantified via analysis for their respective derivative ester compounds and reported respectively as HFPO, HFPO-DA, and COF2 equivalents. Fluoroether E-1 was quantified via direct analysis using Method 8260B. HFPO-DA was quantified via direct analysis using EPA Method 537. Each of the Modified Method 18 impinger samples was recovered and analyzed separately. Analysis results were then used to calculate target analyte feed rates. The sum of the positive analysis results for each target compound was used to determine the waste gas feed line concentration with zero being used for non-detect values. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 8 Focus Project No. P-001393 2.3.5.2 Stack Gas Method 18 Analyses The emissions of the HFPO, HFPO-DAF, COF2, and Fluoroether E-1 were determined via analysis of the Modified Method 18 impinger contents. Please refer to Table 2-2. Like the waste gas feed lines, HFPO, HFPO-DAF, COF2, and Fluoroether E-1 are determined using Method 8260B analysis. HFPO, HFPO- DAF, and COF2 were quantified via analysis for their respective derivative ester compounds and reported respectively as HFPO, HFPO-DA, and COF2 equivalents. Fluoroether E-1 was quantified via direct analysis using Method 8260B. Each of the Modified Method 18 impinger samples was recovered and analyzed separately. In calculating target analyte emission rates, the following approach is used: • For cases where all of the impinger analysis results are non-detect (ND) for a target analyte, the earliest (first) impinger reporting limit (RL) is used as the Modified Method 18 train total catch for that analyte. • For cases where some, but not all of the impinger analysis results are non-detect (ND) for a target analyte, the sum of the positive analysis results and the RL of earliest non-detect impinger is used as the Modified Method 18 train total catch for that analyte. • For cases where all of the impinger analysis results are positive for a target analyte, the sum of the positive analysis results is used as the Modified Method 18 train total catch for that analyte. As discussed later in this report, all stack gas Modified Method 18 analytical results are non-detect values. Therefore, the HFPO, HFPO-DAF, COF2, and Fluoroether E-1 emission rates were based on the methodology noted in the first bullet, above. 2.3.5.3 Stack Gas Method 0010 Analyses The seven (7) fractions from the Modified Method 0010 sampling train components were prepared using SW-846 Method 3542 and analyzed for HFPO-DA via EPA Method 537. Sampling train fractions were combined as noted below and a total of four (4) separate analyses were performed per sampling train: • Front-half composite (probe, nozzle, and filter holder front half solvent rinses, and particulate filter) • Back-half composite (XAD-2 resin, coil condenser and filter holder back half solvent rinses, and impinger solvent rinses) • Condensate and impinger contents, and • Breakthrough XAD-2 resin tube. The sum of the first three (3) sampling train fraction analyses noted above is used for the sampling train total catch. The fourth fraction, the breakthrough XAD-2 resin tube, was analyzed to assess breakthrough and is excluded from the emissions determination calculations. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 9 Focus Project No. P-001393 2.3.6 PFAS Feed and Stack Emission Rates Waste gas feed line sampling and analysis data were reduced and reported as mass of HFPO, HFPO- DA, HFPO-DAF, COF2, and Fluoroether E-1 per total mass of waste gas feed. These data and thermal oxidizer waste gas line mass flow meter data were used to determine the HFPO, HFPO-DA, HFPO-DAF, COF2, and Fluoroether E-1 mass feed rates to the thermal oxidizer. The Modified Method 18 sampled volume data and analysis results were used to determine the HFPO, HFPO-DAF, COF2, and Fluoroether E-1 stack emission concentrations. The Modified Method 0010 sampled volume data and analysis results were used to determine the HFPO-DA stack emission concentration. The Modified Method 0010 stack flow data were used to determine the HFPO, HFPO-DA, HFPO-DAF, COF2, and Fluoroether E-1 stack emission rates. Example equations are presented in Section 4.0 of this test report. 2.3.7 Other Sampling and Analysis In addition to the waste gas feed lines and thermal oxidizer stack emissions, the demineralized water make-up used in the scrubber system, and the HF acid and Stage 4 purge streams from the scrubber system were sampled and analyzed for the same five (5) target PFAS compounds. The purpose of the analysis of the demineralized water make-up samples was to evaluate possible target analyte contamination introduced to the stack gas scrubbing system that could impact the stack gas emissions sampling results. The purpose for the analysis of the acid and purge samples was to demonstrate that the fate of the target analytes was not their removal by the scrubber system after passing through the thermal oxidizer combustion zone. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 10 Focus Project No. P-001393 Table 2-1. Properties and Structures of Target Destruction Efficiency PFAS Compounds Compound Hexafluoropropylene oxide Hexafluoropropylene Dimer Acid or C3-Dimer Hexafluoropropylene Dimer Acid Fluoride Carbonyl Difluoride Heptafluoropropyl-1,2,2,2-tetrafluoroethyl ether Acronym HFPO HFPO-DA HFPO-DAF COF2 Fluoroether E-1 CAS No. 428-59-1 13252-13-6 2062-98-8 353-50-4 3330-15-2 Molecular Formula C3F6O C6HF11O3 C6F12O2 COF2 C5HF11O Mole Weight 166.02 330.05 332.04 66.01 286.04 Molecular Structure O||CF3 -CF2 -CF2 -O -CF -C -OH| CF3 O||CF3 -CF2 -CF2 - O - CF - C - F| CF3 CF3-CF2-CF2-O-CF–F3 Normal B.P., oC @ 760 mmHg -28 151 56 -85 40 V.P. @ 25oC, psia 98.7 (Gas) 0.0224 0.551 Gas 8.1 V.P. @ 25oC, mmHg abs 5,103 (Gas) 1.16 28.5 Gas 419 Note Reacts with methanol to form methyl-2-methoxy-tetrafluoro-propionate (2-MTP), B.P. 41oC. None Reacts with methanol to form HFPO dimer, methyl ester (HFPO-DOCH3), B.P. 116oC.Reacts with methanol to form dimethyl carbonate (DMC), B.P. 90oC. Thermal decarboxylation product of HFPO-DA OCF3 - CF- CF 2 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 11 Focus Project No. P-001393 Table 2-2. Analysis and Reporting Convention for Test Samples Target Analyte Derivative Compound or Target Analyte Actually Measured in the Laboratory Analytical Method Reported Equivalent Compound HFPO Monomer CAS #428-59-1 Methyl 2-methoxytetrafluoropropionate (2-MTP) CAS #10186-63-7 SW-846 Method 8260 HFPO Monomer CAS #428-59-1 HFPO-DAF CAS #2062-98-8 HFPO, Dimer Methyl Ester CAS #13140-34-6 SW-846 Method 8260 HFPO-DAF CAS #2062-98-8 Carbonyl Difluoride CAS #353-50-4 Dimethyl Carbonate CAS #616-38-6 SW-846 Method 8260 Carbonyl Difluoride CAS #353-50-4 Fluoroether E-1 CAS #3330-15-2 Fluoroether E-1 CAS #3330-15-2 SW-846 Method 8260 Fluoroether E-1 CAS #3330-15-2 HFPO-DA (C3-Dimer) CAS #13252-13-6 HFPO-DA (C3-Dimer) CAS #13252-13-6 EPA Method 537 HFPO-DA (C3-Dimer) CAS #13252-13-6 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 12 Focus Project No. P-001393 Natrual Gas Air Stack Thermal Oxidizer Catch Tank Monomer Manufacturing Vents 1st Stage Recycle Polymer Manufacturing Vents 2nd Stage 3rd Stage 4th Stage Recycle Recycle Recycle Demineralized WaterMakup Demineralized WaterMakup Caustic Purge to Offsite Disposal CaF2 Unit Purge to Offsite Disposal To Atmosphere CaF2 to Offsite Disposal Scrubber Gas Stream Water Stream Figure 2-1. Thermal Oxidizer Process Flow Schematic Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 13 Focus Project No. P-001393 Figure 2-2. Modified Method 18 Sampling Train Schematic P:\1_PBB Project Files\Chemours_102017\Handout for Raleigh NC Meeting on December 6 2019\Modified Method 18 Train Schematic for Chemours_3 Compounds_FINAL_112719.vsdCreated by Patti Bales_Last Edited on 3/17/2020 12:40 PM CENTROID OF STACK OR DUCT TO BE SAMPLEDSTACK GAS FLOWMoisture & Condensables Knockout MidgetImpinger #1DRY ICE/ MeOH BATHImpinger #2Impinger #4Schematic of Modified Method 18 Sampling Train for Sampling Waste Gas forHexafluoro Propylene Oxide (HFPO), HFPO-DA and HFPO-DAF and Analytical Assessment by SW-846 Method 8260BImpinger #3UMBILICAL CORDTHERMOCOUPLE OR TEMPERATURE READOUTImpinger #6Impinger #5METER BOX CONTAININGROTAMETER, DRY GAS METER, PUMP, FLOW CONTROLS, AND TEMPERATURE READOUT, AND PROBE HEAT CONTROLSISOLATION VALVESAMPLING MODEVACUUM RELEASE MODELEAK CHECK (VACUUM) MODECHARCOAL TRAPIMPINGERS CHARGED WITH METHANOL (100 mL EACH)TWO-WAY PTFE ISOLATION VALVESTHREE-WAY PTFE ISOLATION VALVE Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 14 Focus Project No. P-001393 Figure 2-3. Modified Method 0010 Sampling Train Schematic Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 15 Focus Project No. P-001393 Figure 2-4. Installed Waste Gas Sampling Point Schematic <------ BALL VALVE <------ BALL VALVE<------ BALL VALVESwagelok® Connection for Sampling Train Connection for Compressed Nitrogen Purge ------------------>GAS FLOW Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 16 Focus Project No. P-001393 3.0 TEST PROGRAM SUMMARY 3.1 PERFORMANCE OBJECTIVE The thermal oxidizer test performance objective was to demonstrate 99.99% DE of PFAS compounds. The test program was designed to characterize and determine the inlet feed rates, and the stack emissions rates of five (5) site-specific target compounds: HFPO, HFPO-DA, HFPO-DAF, COF2, and Fluoroether E-1. The development details of the sampling and analysis methodologies used are presented in the preceding Section 2.0. System DE performance was calculated based on the sum of the system inlet feed rates, and sum of the stack emissions rates of these five (5) compounds. 3.2 TEST IMPLEMENTATION SUMMARY Table 3-1 summarizes the test program sampling and analysis. The thermal oxidizer test program was conducted February 28-29, 2020. Three (3) runs of waste gas feed line sampling and thermal oxidizer emissions sampling were performed. Table 3-2 summarizes the sampling dates and times. The performance test was conducted in substantial conformance with the approved test plan. 3.3 TEST OPERATING OBJECTIVES The thermal oxidizer performance test operating objectives and actual operating data are summarized in Table 3-3. 3.4 DEVIATIONS FROM THE TEST PLAN Three deviations from the approved test plan are noted: • Sampling and analysis for a fifth compound, Fluoroether E-1, was added to the sampling and analysis scope as described in Section 2.3.1. This addition to the test program expanded the amount of target PFAS compounds potentially characterized in the waste gas feed and emissions for DE performance determination. • Sampling of the Stage 1 scrubber purge stream was deleted from the test program. Sampling of this stream was primarily included in the test plan as an option to sampling of the HF acid stream. Sampling of either stream provides similar process information. Deletion of the Stage 1 scrubber purge stream sampling had no impact on test results or determinations. • An additional (7th) impinger was added to the stack gas Modified Method 18 sampling train serving primarily as a moisture knockout trap. This impinger was charged with methanol, and placed in-series as the 1st impinger, preceding the other six (6) impingers described in Section 2.3.3.1. This added 7th impinger was not chilled with dry ice as the other six (6) were, but was maintained in a separate regular ice water bath at approximately 2˚C to knock out moisture vapor while avoiding the freezing of condensed water from the stack gas. Condensed moisture from the stack gas would potentially freeze in the 1st methanol/dry ice bath impinger or connecting tubing possibly plugging up the sampling train. This additional impinger was recovered, analyzed and reported as a separate sample. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 17 Focus Project No. P-001393 Table 3-1. Thermal Oxidizer Performance Test Sampling and Analysis Sample Name Sampling Location/ Access Sampling EquipmentSampling Reference Method 1 Sample Size/Frequency- Target Analyte(s) Analytical Reference Method 2 Monomer Waste Gas Feed Line #1 Specially fabricated sampling port Modified Method 18 Sampling Train EPA Method 18 0.5-1.0 liters per minute concurrent with Method 0010 stack gas sampling HFPO-DAF, HFPO, COF2, & Fluoroether E-1 HFPO-DASW8-46 Method 8260B (Reaction Products) EPA Method 537 2Polymer Waste Gas Feed Line #2 Specially fabricated sampling port Modified Method 18 Sampling Train EPA Method 18 0.5-1.0 liters per minute concurrent with Method 0010 stack gas sampling HFPO-DAF, HFPO, COF2, & Fluoroether E-1 HFPO-DASW-846 Method 8260B (Reaction Products) EPA Method 537 2Stack Gas Stack Port Modified Method 18 Sampling Train EPA Method 18 ~2.0 liters per minute concurrent with Method 0010 stack gas sampling HFPO, HFPO-DAF, COF2, & Fluoroether E-1 SW-846 Method 8260B (Reaction Products) Stack Gas Isokinetic Port Modified Method 0010 Sampling Train SW-846 Method 0010 Minimum sampled volume of 3.0 dry standard cubic meters 3,4 HFPO-DA EPA Method 537 2 Demineralized Makeup Water Tap on line 50-100 mL Plastic Graduated Cylinder; 60 and 1000 mL HDPE Sample Bottles ASTM E-300-86 Sampling Frequency: At the start of the test run and at 60-minute intervals during each test run. Sample Size: Note 5 HFPO, HFPO-DAF, COF2, & Fluoroether E-1 HFPO-DA SW-846 Method 8260B (Reaction Products) EPA Method 537 HF Acid Stream Tap on line 50-100 mL Plastic Graduated Cylinder; 60 and 1000 mL HDPE Sample Bottles ASTM E-300-86 Same as Demineralized Water HFPO, HFPO-DAF, COF2, & Fluoroether E-1 HFPO-DA SW-846 Method 8260B (Reaction Products) EPA Method 537 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 18 Focus Project No. P-001393 Table 3-1. Thermal Oxidizer Performance Test Sampling and Analysis Sample Name Sampling Location/ Access Sampling EquipmentSampling Reference Method 1 Sample Size/Frequency- Target Analyte(s) Analytical Reference Method 2 Stage 4 Purge Tap on line 50-100 mL Plastic Graduated Cylinder; 60 mL HDPE Sample Bottles ASTM E-300-86 Same as Demineralized Water HFPO, HFPO-DAF, COF2, & Fluoroether E-1 HFPO-DA SW846 Method 8260B (Reaction Products) EPA Method 537 Notes: 1 Reference Sampling Method Sources: “ASTM” refers to American Society for Testing Materials, Annual Book of ASTM Standards, Annual Series “SW-846" refers to Test Methods for Evaluating Solid Waste, Third Edition, November 1986, and Updates. “EPA Method" refers to New Source Performance Standards, Test Methods and Procedures, Appendix A, 40 CFR 60. 2 Reference Analysis Methods Sources: • Modified Method 18 – “Measurement of Gaseous Organic Compound Emissions by Gas Chromatography.” EPA 40 CFR Part 60, Appendix A. • Method 0010 – “Modified Method 5 Sampling Train”. Taken from Test Methods for Evaluating Solid Waste: Physical/Chemical Methods Compendium, SW-846, Third Edition, September 1986 and its updates, USEPA, OSWER, Washington, D.C. 20460. • Method 5, Appendix A, Test Methods and Procedures, New Source Performance Standards, 40 CFR 60. • Method 8260B – “Volatile Organic Compounds by Gas Chromatography/Mass Spectrometry (GC/MS)”. Taken from Test Methods for Evaluating Solid Waste: Physical/Chemical Methods Compendium, SW-846, Third Edition, September 1986 and its updates, USEPA, OSWER, Washington, D.C. 20460. • Method 3542A – “Extraction of Semivolatile Analytes Collected Using Method 0010 ("Modified Method 5 Sampling Train")”. Taken from Test Methods for Evaluating Solid Waste: Physical/Chemical Methods Compendium, SW-846, Third Edition, September 1986 and its updates, USEPA, OSWER, Washington, D.C. 20460. • Method 537 – “Determination of Selected Perfluorinated Alkyl Acids In Drinking Water By Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)”, Version 1.1, September 2009, EPA/600/R-08/092. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 19 Focus Project No. P-001393 Table 3-1. Thermal Oxidizer Performance Test Sampling and Analysis 3 The exact volume of gas sampled will depend on the isokinetic sampling rate. 4 Isokinetic sampling trains include: • Sampling traverse points determined in accordance with EPA Method 1. • Performing stack gas velocity, pressure and temperature profile measurement for each sampling location (EPA Method 2) • Oxygen and carbon dioxide concentrations measured to determine stack gas molecular weight (EPA Method 3A) • Determining the moisture content of the stack gas for each sampling train sample (EPA Method 4). 5 Two sample portions of these process streams are collected at each sampling interval: • For samples receiving the HFPO, HFPO-DAF, COF2, and Fluoroether E-1 analyses, a graduated cylinder was used to measure a 40 mL aliquot of the collected material and transfer it to a 60 mL HDPE bottle containing methanol. The lid was placed on the sample bottle and sealed. The methanol reacts with HFPO, HFPO-DAF, and COF2 under these conditions to form derivative products that are evaluated by the laboratory. . The grab portions of these samples were composited in the laboratory to provide a single representative result for each test run. • For the HFPO-DA analysis sample, a 100 ml aliquot of the collected material was placed into a 1000 ml HDPE bottle. The lid was placed on the sample bottle and sealed. Each additional aliquot was added to the bottle to build a field composite of the process sample. The laboratory analyzed the composited sample to provide a single representative result for each test run. The different sample portions are labeled to distinguish between those receiving analysis for the HFPO, HFPO-DAF, COF2, and Fluoroether E-1, and those receiving analysis for HFPO-DA. The final number of discrete sample aliquot portions collected was dependent on the final run duration. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 20 Focus Project No. P-001393 Table 3-2. Thermal Oxidizer Performance Test Sampling Dates and Times Run No.: Run 1 Run 2 Run 3 Date: 28-Feb-20 28-Feb-20 29-Feb-20 Start: 11:15 16:30 9:15 Finish: 14:33 19:43 12:32 Duration: 3:18 3:13 3:17 Table 3-3. Thermal Oxidizer Performance Test Operating Data Parameter Tag No. Units Permit Statistic Run 1 Run 2 Run 3 Average Monomer Waste Gas A41756FC lb/hr NA Average 433.6 401.4 400.4 411.8 Maximum 455.5 447.1 506.5 469.7 Minimum 405.1 354.9 343.5 367.8 Std Dev 13.8 20.7 46.4 27.0 Polymer Waste Gas A41103FC lb/hr NA Average 241.8 240.1 244.3 242.1 Maximum 247.5 248.2 250.4 248.7 Minimum 235.0 233.0 236.5 234.8 Std Dev 2.4 3.1 2.8 2.8 Total Waste Gas Calculated lb/hr <2,200 Average 678.8 641.5 651.2 657.2 Maximum 1291.0 695.3 1991.2 1325.8 Minimum 642.7 597.7 592.8 611.1 Std Dev 46.0 22.0 106.3 58.1 Combustion Temperature A40937TC deg F >1,800 Average 1,922 1,922 1,921 1,922 Maximum 1,924 1,924 1,923 1,924 Minimum 1,920 1,919 1,918 1,919 Std Dev 1 1 1 1 Scrubber Flow Rate Calculated gpm >40 Average 60.5 60.5 60.5 60.5 Maximum 60.8 60.6 60.8 60.8 Minimum 60.2 60.3 60.2 60.3 Std Dev 0.1 0.1 0.1 0.1 Scrubber pH A41261XC SU >7.1 Average 8.15 8.15 8.13 8.14 Maximum 8.18 8.18 8.18 8.18 Minimum 8.13 8.11 8.09 8.11 Std Dev 0.02 0.02 0.02 0.02 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 21 Focus Project No. P-001393 4.0 TEST RESULTS 4.1 TEST DATA REDUCTION BASIS The strategy for the determination of the PFAS target analyte feed rates and their emissions evaluation are conducted to provide the most conservative assessment of the thermal oxidizer performance. Specifically: • Calculation of PFAS target analyte feed rates use zero (0) for laboratory non-detect (ND) values determined from the waste gas line Modified Method 18 sampling and analyses. No feed rate credit or contribution is taken for constituents below the sampling and analysis measurement limits. • The stack gas ND values represent the quantitative limits of the sampling and analytical measurements under the test conditions. Actual emissions are not assumed to be zero (0), but are assigned the reporting limit (RL) value for the method. The Modified Method 18 sampling train includes seven (7) impingers in-series that are recovered and analyzed separately. The calculation of PFAS Modified Method 18 measured stack emission rates is based on the RL for the first in-series impinger when all seven (7) impingers are ND for a target analyte. • The Modified Method M0010 measured stack emission rates are based on separate analysis of three (3) sampling train fractions [front-half composite (FH), back-half composite (BH), and the combined impinger contents and rinses composite]. During this test program, HFPO-DA was detected in all three (3) sampling fractions during all three (3) sampling runs. Therefore, the calculation of HFPO-DA Modified Method 0010 measured stack emission rates is based on the sum of all three (3) analysis fraction detected values. The breakthrough XAD-2 resin analyses serve as quality control (QC) indicators and are excluded from the HFPO-DA emissions determinations. The balance of Section 4.0 details how the test data were reduced to determine thermal oxidizer PFAS DE performance. 4.2 WASTE GAS CHARACTERIZATION AND TARGET PFAS COMPOUND FEED RATES The waste gas feed lines were sampled using the Modified Method 18 sampling train. Tables 4-1 and 4-2 summarize the analyses of the polymer and monomer waste gas feed lines. Tables 4-3 and 4-4 summarize the feed rates of the target PFAS compounds. The detailed waste gas feed line sampling data and laboratory analysis reports are included in Appendixes B and C, respectively of Weston’s Thermal Oxidizer Control Efficiency Test Report, Test Dates 28-29 February 2020 included as an attachment to this test report. Please note that a zero “0” was applied for calculations used for sample fractions that were reported by the laboratory as non-detect (ND). The waste gas feed rates to the thermal oxidizer are measured by mass flow meters. To determine the target compound feed rates, the waste gas feed sampling and analysis data were reduced to yield mass of target compound per total mass feed. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 22 Focus Project No. P-001393 Please refer to Tables 4-1 and 4-2. Each of the waste gas feed line sampling train fraction mass concentrations for a target analyte were added together to provide the total mass of each target compound during a test run. The compound mass totals were determined from sum of the individual impinger analyses: CTOTi = ΣCNi Where: CTOTi = Total mass of individual target compound for a test run, CNi = Individual mass results of each target compound. The total mass of all target PFAS compounds captured during a test run was determined from the sum of the individual target PFAS compounds: CPFAS = ΣCTOTi Where: CPFAS = Total mass of target PFAS compounds CTOTi = Total mass of each target compound. Please refer to Tables 4-3 and 4-4. From the Modified Method 18 sampling train recovery data, the total mass of waste gas vapors condensed was determined from the sum of the changes in the impinger masses: ΔIMTOT = ΣΔIMN Where: ΔIMTOT = Total impinger mass change ΔIMN = Individual impinger mass changes. From the Modified Method 18 sampling train dry gas metering system data, the mass of dry gas sampled was determined: DGM = VM*DGMC*(TS/TM)*[(PB)/(PS)]*MWG/MVSTP Where: DGM = Dry gas mass VM = Dry gas meter measured volume DGMC = Dry gas meter coefficient TS = Standard temperature in oR or oK Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 23 Focus Project No. P-001393 TM = Dry gas meter temperature in oR or oK PB = Barometric pressure PS = Standard pressure MWG = Dry gas molecular weight MV = Molar volume (volume per mole of gas at STP) STP = Standard temperature and pressure. Tables 4-3 and 4-4 show the reduced sampled volumes from the previously referenced Weston report for the waste gas feed line Modified Method 18 sampling trains in dry standard liters. The waste gas feed line dry gas fraction was assumed to be 100% nitrogen and was assigned a molecular weight of 28 amu. The mass of dry gas sampled was determined by multiplying the measured dry gas standard sample volume by the molecular weight of nitrogen and dividing by the molar volume at standard temperature and pressure, 24.055 liter/gram mole. The total mass sampled from the waste gas feed line is the sum of dry gas total mass and the impinger mass gain: MTOT = DGM + ΔIMTOT Where: MTOT = Total organic vapor and dry gas mass sampled ΔIMTOT = Total impinger mass change DGM = Dry gas mass. The mass fraction of the target PFAS compounds per total mass feed was determined dividing total mass of target PFAS compounds captured by the total mass sampled: FCPFAS = CPFAS/MTOT Where: FCPFAS = Feed concentration of target PFAS compounds in mass/total mass sampled CPFAS = Total mass of target compound MTOT = Total mass of organic vapor and dry gas mass sampled. The total PFAS target compound mass feed rate was determined by multiplying the calculated mass fraction of total PFAS target compounds by the mass feed rate measured by the thermal oxidizer mass flow meters: FRPFAS = FCCPFAS ∗ MF Where: FRC = Mass feed rate of target compound FCC = Feed concentration of target compound in mass/total mass MF = Mass feed rate measured by the mass flow meter. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 24 Focus Project No. P-001393 4.3 TARGET PFAS COMPOUND STACK EMISSION RATES Two (2) sampling trains were used to measure the stack emission rates of the target PFAS compounds: • Modified Method 0010 for HFPO-DA, and • Modified Method 18 for HFPO, HFPO-DAF, COF2, and Fluoroether E-1. The detailed stack gas sampling data and laboratory analysis reports are included in Appendixes B and C, respectively of the previously referenced Weston report. 4.3.1 Modified Method 0010 Measured Emissions Please refer to Table 4-5. From the Modified Method 0010 sampling train fraction analysis, the total mass of the target compound was determined from sum of the individual fraction composite analyses: CTOT = CFH + CBH + CIMP Where: CTOT = Total mass of target compound CFH = Mass of target compound in front half fraction (probe, nozzle, and front half solvent rinses and particulate filter) CBH = Mass of target compound in back half fraction (XAD-2 resin, and back half and impinger solvent rinses) CIMP = Mass of target compound in impinger fraction (condensate and impinger liquid). From the Modified Method 0010 sampling train dry gas metering system data, the volume of dry gas sampled was determined: DGV = VM*DGMC*(TS/TM)*[(PB+ΔH)/(PS)] Where: DGV = Dry gas volume sampled at standard temperature and pressure VM = Dry gas meter measured volume DGMC = Dry gas meter coefficient TS = Standard temperature in oR or oK TM = Dry gas meter temperature in oR or oK PB = Barometric pressure ΔH = Delta H sampling pressure (vacuum) PS = Standard pressure. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 25 Focus Project No. P-001393 The details of the stack gas Modified Method 0010 sampled volume determinations are included in the previously referenced Weston report. The sampled stack gas volumes from the Weston report reduced to standard conditions are presented in Table 4-5. The stack gas concentration of the HFPO-DA was determined by dividing the total mass of HFPO-DA by the sampled volume: ECC = CTOT/DGV Where: ECC = Emission concentration of target compound in mass/dry volume CTOT = Total mass of target compound DGV = Dry gas volume sampled at standard temperature and pressure. The stack flow rates from the Weston report reduced to standard conditions are presented in Table 4-5. The emission rate of the HFPO-DA was determined by multiplying the stack gas concentration by the stack flow rate: ERC = ECC ∗ SFDG Where: ERC = Emission rate of target compound ECC = Emission concentration of target compound in mass/dry volume SFDG = Dry gas stack flow rate at standard temperature and pressure (as determined from Method 0010 data) (Method 1, 2, 3A, and 4 data). 4.3.2 Modified Method 18 Measured Emissions Please refer to Table 4-6. From the Modified Method 18 sampling train fraction analysis, the total mass of each target compound was determined from sum of the individual impinger analyses: CTOT = ΣCN Where: CTOT = Total mass of target compound CN = Individual impinger mass analysis results. Analysis results for all four target compounds measured using Modified Method 18 were non-detect (ND). As noted in Section 2.3.5.2, only the reporting limit (RL) for the first impinger was used to calculate PFAS emissions results. From the Modified Method 18 sampling train dry gas metering system data, the volume of dry gas sampled was determined: DGV = VM*DGMC*(TS/TM)*[(PB+ΔH)/(PS)] Where: DGV = Dry gas volume sampled at standard temperature and pressure Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 26 Focus Project No. P-001393 VM = Dry gas meter measured volume DGMC = Dry gas meter coefficient TS = Standard temperature in oR or oK TM = Dry gas meter temperature in oR or oK PB = Barometric pressure ΔH = Delta H sampling pressure (vacuum) PS = Standard pressure. PS = Standard pressure. The details of the stack gas Modified Method 18 sampled volume determinations are included in the previously referenced Weston report. The sampled stack gas volumes from the Weston report reduced to standard conditions are presented in Table 4-6. The stack gas concentration of target compounds was determined by dividing the total mass of the target compounds by the sampled volume: ECC = CTOT/DGV Where: ECC = Emission concentration of target compounds in mass/dry volume CTOT = Total impinger mass of target compounds DGV = Dry gas volume sampled at standard temperature and pressure. Please refer to Table 4-7. The emission rate of the target compounds was determined by multiplying the stack gas concentration by the stack flow rate: ERC = ECC ∗ SFDG Where: ERC = Emission rate of target compound ECC = Emission concentration of target compound in mass/dry volume SFDG = Dry gas stack flow rate at standard temperature and pressure (as determined from Method 0010 data) (Method 1, 2, 3A, and 4 data). 4.4 TOTAL PFAS DESTRUCTION EFFICIENCY Please refer to Table 4-8, “Total PFAS” is the arithmetic sum of HFPO, HFPO-DA, HFPO-DAF, COF2, and Fluoroether E-1. The total PFAS destruction efficiency (DE) was calculated by dividing the difference of the total PFAS feed rate and the total PFAS emission rate by the total PFAS feed rate: DE = (FR-ER)/FR *100% Where: DE = Total PFAS destruction efficiency, percent (%) Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 27 Focus Project No. P-001393 FR = Total PFAS mass feed rate ER = Total PFAS mass emission rate. The total PFAS DE performance results presented in Table 4-8 demonstrate that the thermal oxidizer controls all PFAS at an efficiency greater than 99.99%. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 28 Focus Project No. P-001393 Table 4-1. Thermal Oxidizer Monomer Tank Feed (Line #1) Summary Analyses Target Compound Train Fraction Units Run 1 Run 2 Run 3 COF2 Impinger 1 ug 46,600,000 45,300,000 68,000,000 COF2 Impinger 2 ug 1,570,000 1,180,000 3,420,000 COF2 Impinger 3 ug 124,000 67,400 139,000 COF2 Impinger 4 ug ND ND ND COF2 Impinger 5 ug ND ND ND COF2 Impinger 6 ug ND ND ND COF2 Totalug48,294,000 46,547,400 71,559,000 HFPO-DAF Impinger 1 ug ND ND ND HFPO-DAF Impinger 2 ug ND ND ND HFPO-DAF Impinger 3 ug ND ND ND HFPO-DAF Impinger 4 ug ND ND ND HFPO-DAF Impinger 5 ug ND ND ND HFPO-DAF Impinger 6 ug ND ND ND HFPO-DAF Total ug 00 0 HFPO Impinger 1 ug 180,000 338,000 90,800 HFPO Impinger 2 ug 345,000 285,000 461,000 HFPO Impinger 3 ug 266,000 203,000 365,000 HFPO Impinger 4 ug 208,000 164,000 267,000 HFPO Impinger 5 ug 153,000 102,000 98,700 HFPO Impinger 6 ug 242,000 75,800 205,000 HFPO Total ug 1,394,000 1,167,800 1,486,600 Fluoroether E-1 Impinger 1 ug ND ND ND Fluoroether E-1 Impinger 2 ug ND ND ND Fluoroether E-1 Impinger 3 ug ND ND ND Fluoroether E-1 Impinger 4 ug ND ND ND Fluoroether E-1 Impinger 5 ug ND ND ND Fluoroether E-1 Impinger 6 ug ND ND ND Fluoroether E-1 Total ug 00 0 HFPO-DA Impinger 1 ug 1,410 5,050 6,440 HFPO-DA Impinger 2 ug 156 114 254 HFPO-DA Impinger 3 ug 69.2 57.7 78.8 HFPO-DA Impinger 4 ug 35.6 32.2 43.6 HFPO-DA Impinger 5 ug 66.0 15.8 33.0 HFPO-DA Impinger 6 ug 29.2 6.34 26.8 HFPO-DA Total ug 1,766 5,276 6,876 Total Target PFAS Mass Total grams 49.69 47.72 73.05 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 29 Focus Project No. P-001393 Table 4-2. Thermal Oxidizer Polymer Tank Feed (Line #2) Summary Analyses Target Compound Train Fraction Units Run 1 Run 2 Run 3 COF2 Impinger 1 ug ND ND ND COF2 Impinger 2 ug ND ND ND COF2 Impinger 3 ug ND ND ND COF2 Impinger 4 ug ND ND ND COF2 Impinger 5 ug ND ND ND COF2 Impinger 6 ug ND ND ND COF2 Totalug00 0 HFPO-DAF Impinger 1 ug 235 ND 205 HFPO-DAF Impinger 2 ug 118 110 ND HFPO-DAF Impinger 3 ug 47.5 ND ND HFPO-DAF Impinger 4 ug ND ND ND HFPO-DAF Impinger 5 ug ND ND ND HFPO-DAF Impinger 6 ug ND ND ND HFPO-DAF Total ug 401 110 205 HFPO Impinger 1 ug ND ND ND HFPO Impinger 2 ug ND ND ND HFPO Impinger 3 ug ND ND ND HFPO Impinger 4 ug ND ND ND HFPO Impinger 5 ug ND ND ND HFPO Impinger 6 ug ND ND ND HFPO Total ug 00 0 Fluoroether E-1 Impinger 1 ug 1,010 802 795 Fluoroether E-1 Impinger 2 ug 248 182 134 Fluoroether E-1 Impinger 3 ug 54.7 60.6 91.3 Fluoroether E-1 Impinger 4 ug ND ND ND Fluoroether E-1 Impinger 5 ug ND ND ND Fluoroether E-1 Impinger 6 ug ND ND ND Fluoroether E-1 Total ug 1,313 1,045 1,020 HFPO-DA Impinger 1 ug 44.2 30.8 52 HFPO-DA Impinger 2 ug 18.7 24.1 20 HFPO-DA Impinger 3 ug 8.16 8.29 12 HFPO-DA Impinger 4 ug 2.82 1.59 2.76 HFPO-DA Impinger 5 ug 0.784 0.155 0.263 HFPO-DA Impinger 6 ug ND ND ND HFPO-DA Total ug 75 65 86 Total Target PFAS Mass Total grams 0.00179 0.00122 0.00131 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 30 Focus Project No. P-001393 Table 4-3. Thermal Oxidizer Monomer Tank (Line #1) Sampling Results and Feed Rates Parameter Units Run 1 Run 2 Run 3 Net Inlet Condensed Mass grams 120.8 129.6 189.9 Speciated Compounds in Condensed Mass Total COF2 ug48,294,000 46,547,400 71,559,000 Total HFPO-DAF ug 0 0 0 Total HFPO ug 1,394,000 1,167,800 1,486,600 Total Fluoroether E-1 ug 0 0 0 Total HFPO-DA ug1,766 5,276 6,876 Total Target PFAS Sample Mass grams 49.69 47.72 73.05 Total Dry Gas and Condensed Mass Sampled Sampled Dry Gas Volume (@ 20oC, 1 atm)Liters 100.614 98.903 100.165 Sampled Dry Gas Mass (24.055 L/gmol, MW=28)grams 117.115 115.123 116.592 Total Mass Sampled (Condensed + Dry Gas)grams 237.915 244.723 306.492 Constituent Concentrations in Total Sampled Mass Total COF2 g/g flow 2.0E-01 1.9E-01 2.3E-01 Total HFPO-DAF g/g flow 0.0E+00 0.0E+00 0.0E+00 Total HFPO g/g flow 5.9E-03 4.8E-03 4.9E-03 Total Fluoroether E-1 g/g flow 0.0E+00 0.0E+00 0.0E+00 Total HFPO-DA g/g flow 7.4E-06 2.2E-05 2.2E-05 Total Target PFAS g/g flow 2.1E-01 1.9E-01 2.4E-01 Calculated Constituent Feed Rates Monomer Tank Gas Flow lb/hr 434 401 400 Monomer Tank Gas Flow kg/hr 197 182 182 Total COF2 g/hr 39,927 34,634 42,400 Total HFPO-DAF g/hr 0 0 0 Total HFPO g/hr 1,152 869 881 Total Fluoroether E-1 g/hr 0 0 0 Total HFPO-DA g/hr 1.46 3.93 4.07 Total Target PFAS Feed Rate g/hr 41,807 35,507 43,285 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 31 Focus Project No. P-001393 Table 4-4. Thermal Oxidizer Polymer Tank (Line #2) Sampling Results and Feed Rates Parameter Units Run 1 Run 2 Run 3 Net Inlet Condensed Mass grams 1.5 2.8 4.2 Speciated Compounds in Condensed Mass Total COF2 ug 0 0 0 Total HFPO-DAF ug 401 110 205 Total HFPO ug 0 0 0 Total Fluoroether E-1 ug 1,313 1,045 1,020 Total HFPO-DA ug75 65 86 Target PFAS Sample Mass grams 0.00179 0.00122 0.00131 Total Dry Gas and Condensed Mass Sampled Sampled Dry Gas Volume (@ 20oC, 1 atm)Liters 101.565 101.665 101.301 Sampled Dry Gas Mass (24.055 L/gmol, MW=28)grams 118.222 118.338 117.914 Total Mass Sampled (Condensed + Dry Gas)grams 119.722 121.138 122.114 Constituent Concentrations in Total Sampled Mass Total COF2 g/g flow 0.0E+00 0.0E+00 0.0E+00 Total HFPO-DAF g/g flow 3.3E-06 9.1E-07 1.7E-06 Total HFPO g/g flow 0.0E+00 0.0E+00 0.0E+00 Total Fluoroether E-1 g/g flow 1.1E-05 8.6E-06 8.4E-06 Total HFPO-DA g/g flow 6.2E-07 5.4E-07 7.1E-07 Total Target PFAS g/g flow 1.5E-05 1.1E-05 1.1E-05 Calculated Constituent Feed Rates Polymer Tank Gas Flow lb/hr 242 240 244 Polymer Tank Gas Flow kg/hr 110 109 111 Total COF2 g/hr 0.000 0.000 0.000 Total HFPO-DAF g/hr 0.367 0.0989 0.186 Total HFPO g/hr 0.000 0.000 0.000 Total Fluoroether E-1 g/hr 1.203 0.0939 0.926 Total HFPO-DA g/hr 0.0684 0.0584 0.0782 Total Target PFAS Feed Rate g/hr 1.64 1.10 1.19 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 32 Focus Project No. P-001393 Table 4-5. Thermal Oxidizer Modified Method 0010 Stack Emissions Sampling Results Parameter Units Run 1 Run 2 Run 3 Stack Flow dscfm 5,179 5,058 5,320 Method 0010 Sampled Volume dscf 127.323 122.804 130.162 Method 0010 Front Half HFPO-DA ug 0.0284 0.0279 0.0216 Method 0010 Back Half HFPO-DA ug 0.164 0.0941 0.0716 Method 0010 Impingers HFPO-DA ug 0.0259 0.0376 0.0237 Method 0010 Breakthrough XAD-2 HFPO- DA (Breakthrough Indicator Only) ug 0.00488 0.0167 0.0107 Method 0010 Train Total HFPO-DA (Excludes Breakthrough XAD-2) ug 0.218 0.160 0.117 Method 0010 HFPO-DA Emissions Rate g/hr 0.000533 0.000394 0.000287 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 33 Focus Project No. P-001393 Table 4-6. Thermal Oxidizer Stack Gas Modified Method 18 Sample Summary Analyses Parameter UnitsRun 1 Run 2 Run 3 Speciated Compounds in Impingers COF2, Impinger 1 ug < 1.71 < 2.15 < 1.39 COF2, Impinger 2 ug < 2.40 < 2.25 < 2.19 COF2, Impinger 3 ug < 2.25 < 2.32 < 1.47 COF2, Impinger 4 ug < 1.87 < 2.29 < 1.85 COF2, Impinger 5 ug < 2.42 < 2.48 < 2.13 COF2, Impinger 6 ug < 1.94 < 2.32 < 2.18 COF2, Impinger 7 ug < 2.22 < 2.09 < 1.30 Total COF2 including ND Values ug < 14.8 < 15.9 < 12.5 Total COF2 only Impinger 1 ug < 1.71 < 2.15 < 1.39 Total COF2 only Impinger 1 or Positive Results ug < 1.71 < 2.15 < 1.39 HFPO-DAF, Impinger 1 ug < 0.562 < 0.706 < 0.458 HFPO-DAF, Impinger 2 ug < 0.788 < 0.740 < 0.722 HFPO-DAF, Impinger 3 ug < 0.740 < 0.764 < 0.486 HFPO-DAF, Impinger 4 ug < 0.616 < 0.754 < 0.611 HFPO-DAF, Impinger 5 ug < 0.797 < 0.818 < 0.703 HFPO-DAF, Impinger 6 ug < 0.641 < 0.764 < 0.718 HFPO-DAF, Impinger 7 ug < 0.761 < 0.687 < 0.427 Total HFPO-DAF including ND Values ug < 4.91 < 5.23 < 4.13 Total HFPO-DAF only Impinger 1 ug < 0.562 < 0.706 < 0.458 Total HFPO-DAF only Impinger 1 or Positive Results ug < 0.562 < 0.706 < 0.458 HFPO, Impinger 1 ug < 0.0254 < 0.0320 < 0.0207 HFPO, Impinger 2 ug < 0.0356 < 0.0335 < 0.0327 HFPO, Impinger 3 ug < 0.0335 < 0.0346 < 0.0220 HFPO, Impinger 4 ug < 0.0279 < 0.0341 < 0.0277 HFPO, Impinger 5 ug < 0.0361 < 0.0370 < 0.0318 HFPO, Impinger 6 ug < 0.0290 < 0.0346 < 0.0325 HFPO, Impinger 7 ug < 0.0331 < 0.0311 < 0.0193 Total HFPO including ND Values ug < 0.221 < 0.237 < 0.187 Total HFPO only Impinger 1 ug < 0.0254 < 0.0320 < 0.0207 Total HFPO only Impinger 1 or Positive Results ug < 0.0254 < 0.0320 < 0.0207 Fluoroether E-1, Impinger 1 ug < 0.0291 < 0.0366 < 0.0237 Fluoroether E-1, Impinger 2 ug < 0.0408 < 0.0384 < 0.0374 Fluoroether E-1, Impinger 3 ug < 0.0383 < 0.0396 < 0.0252 Fluoroether E-1, Impinger 4 ug < 0.0319 < 0.0390 < 0.0317 Fluoroether E-1, Impinger 5 ug < 0.0413 < 0.0424 < 0.0364 Fluoroether E-1, Impinger 6 ug < 0.0332 < 0.0396 < 0.0372 Fluoroether E-1, Impinger 7 ug < 0.0379 < 0.0356 < 0.0221 Total Fluoroether E-1 including ND Values ug < 0.253 < 0.271 < 0.214 Total Fluoroether E-1 only Impinger 1 ug < 0.0291 < 0.0366 < 0.0237 Total Fluoroether E-1 only Impinger 1 or Positive Results ug < 0.0291 < 0.0366 < 0.0237 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 34 Focus Project No. P-001393 Table 4-6. Thermal Oxidizer Stack Gas Modified Method 18 Sample Summary Analyses Parameter UnitsRun 1 Run 2 Run 3 Total Target PFAS Compounds Including applicable ND values ug < 20.2 < 21.6 < 17.0 Total Target PFAS Compounds only Impinger 1 ug < 2.33 < 2.92 < 1.89 Total Target PFAS Compounds only Impinger 1 or Positive Results ug < 2.33 < 2.92 < 1.89 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 35 Focus Project No. P-001393 Table 4-7. Thermal Oxidizer Modified Method 18 Stack Emissions Sampling Results Parameter Units Run 1 Run 2 Run 3 Sampled Stack Volume dsl 281.262 278.471 283.048 Sampled Stack Volume dscf 9.931 9.833 9.994 Stack Flow dscfm 5,179 5,058 5,320 Total Target PFAS only Impinger 1 or Positive Results ug < 2.33 < 2.92 < 1.89 Total Target PFAS only Impinger 1 or Positive Rate g/hr < 0.0728 < 0.0903 < 0.0604 Table 4-8. Thermal Oxidizer Total PFAS Destruction Efficiency Parameter Units Run 1 Run 2 Run 3 Monomer Feed Total Target PFAS Inlet by Modified Method 18 (ND=0) g/hr 41,081 35,507 43,285 Polymer Feed Total Target PFAS Inlet by Modified Method 18 (ND=0) g/hr 1.64 1.10 1.19 Total Target PFAS Inlet by Modified Method 18 (ND=0) g/hr 41,082 35,508 43,287 Outlet HFPO-DA by Modified Method 0010 g/hr 0.000533 0.000394 0.000287 Outlet Other Target PFAS by Modified Method 18 g/hr < 0.0728 < 0.0903 < 0.0604 Total Target PFAS Outlet g/hr < 0.0733 < 0.0907 < 0.0607 Total Target PFAS DE % > 99.99982% > 99.99974% > 99.99986% Average Target PFAS DE % > 99.99981% Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 36 Focus Project No. P-001393 5.0 QUALITY CONTROL 5.1 WASTE GAS SAMPLING The waste gas constituents and their concentrations vary based on the product(s) being manufactured at any particular time. Waste gas sampling was performed using the Modified Method 18 sampling train that was developed for the Chemours Fayetteville Works test program. Both waste gas feed lines were sampled independently to determine the concentrations of the five (5) target PFAS compounds. The waste gas sampling was performed at a constant sampling rate for 180 minutes during each test run, and concurrent with the stack gas sampling. The samples obtained represent the average composition during each test run. The sampling and analysis data were reduced to yield mass of target analyte per total mass of waste gas in each feed line. This information and the respective waste gas feed line mass feed rate data were used to determine inlet feed rates of the target PFAS compounds. The following sections examine the quality of the waste gas feed characterization results and their associated impacts on the measurement of the thermal oxidizer DE performance. 5.1.1 Modified Method 18 Capture Efficiency Figures 5-1 and 5-2 graphically show the impinger mass changes for the waste gas Modified Method 18 sampling. The data show the efficiency of the sampling method for capturing entrained condensable organic vapors. The monomer waste gas feed (Line #1) sampling data show a relative high capture efficiency with nominally 90% of the capture occurring in Impinger 1. Based on the target PFAS compound distributions discussed in Section 5.1.3, similar capture performance is occurring for the polymer waste gas feed (Line #2) sampling. The sum of the differential mass changes for the polymer waste gas feed is positive. The negative values for individual impingers reflect “bump over” of impinger liquid from one impinger to another that can occur with the release of vacuum during the pre- and post- test run leak checks of the sampling train. 5.1.2 Monomer Waste Gas Sampling During the test, Vinyl Ethers North (VEN) was producing PSEPVE. COF2, HFPO, and HFPO-DA were present in the monomer waste gas feed (Line #1), while no HFPO-DAF or Fluoroether E-1 were measured in these samples. Figures 5-3, 5-4, and 5-5 graphically show the relative loadings of each of the three (3) detected target compounds in the six (6) Modified Method 18 impingers. COF2 and HFPO-DA are primarily captured in the first two impingers. COF2 readily reacts with methanol. During all three (3) runs, no COF2 is detected after the third impinger. The capture of HFPO-DA is assumed to occur via condensation and dissolution, and HFPO-DA does not react with methanol. The distribution of HFPO-DA was detected in all six (6) impingers with 92-98% of the train total being captured in Impingers 1-3. These data show COF2 and HFPO-DA are being captured with a high degree of efficiency. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 37 Focus Project No. P-001393 HFPO was detected in all six (6) impingers distributed at comparable levels throughout. Capture of HFPO is dependent on both condensation and chemical reaction. These data show HFPO is being detected at a lesser degree of efficiency, thus its measured concentration and actual feed rate is higher than is being measured. A low bias to this concentration translates to a low bias in the DE determination. Therefore, a higher concentration determined for HFPO for this feed line would result in a higher DE demonstration. Despite a low bias in feed rate measurement, all PFAS DE is demonstrated to exceed 99.99% efficiency. 5.1.3 Polymer Waste Gas Sampling During the test, Polymers was running an SR polymer campaign. HFPO-DA, HFPO-DAF, and Fluoroether E-1 were present in the polymer waste gas feed (Line #2), but no COF2 or HFPO were detected. Figures 5-6, 5-7, and 5-8 graphically show the relative loadings of each of the three (3) detected target compounds in the six (6) Modified Method 18 impingers. HFPO-DA was detected in all six (6) impingers with 95-97% of the train total being captured in Impingers 1-3. Fluoroether E-1 is primarily captured in the first two (2) impingers with none detected after the third impinger. Capture of both HFPO-DA and Fluoroether E-1 occurs via dissolution and condensation, and neither compound reacts with methanol. These data show HFPO-DA and Fluoroether E-1 are being captured with a high degree of efficiency. HFPO-DAF was detected in Impinger samples 1-3 during Run 1, and intermittently in Impinger samples 2 and 1 during Runs number 2 and 3, respectively. The data show generally that the polymer manufacturing line was not a significant contributor of PFAS compounds during this test. However, the monomer manufacturing line concentrations and flows were sufficiently high to allow a demonstration of performance greater than 99.99% DE. 5.2 WASTE GAS ANALYSES Tables 5-1 through 5-4 summarize the surrogate spike compound recoveries for the waste gas analyses. 5.2.1 Monomer Waste Gas Analyses Please refer to Table 5-1 for the monomer waste gas (Line # 1) SW-846 Method 8260B analysis surrogate spike recoveries. For the SW-846 Method 8260B (volatile organic) analyses for COF2, HFPO, HFPO-DAF, and Fluoroether E-1, surrogate spike recoveries ranged from 90-107%. Four (4) standard surrogate spike compounds spanning the volatile range were reported. The narrow range and high degree of surrogate recoveries represent a relatively high precision and accuracy with regard to the measurements of these target analytes in the high concentration waste gas samples. Several of these samples required significant dilution prior to analytical processing. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 38 Focus Project No. P-001393 Table 5-2 refers to the monomer waste gas (Line # 1) EPA Method 537 analysis isotope dilution internal standard (IDIS) spike recoveries related to the determination of HFPO-DA. The IDIS spike recoveries of the labeled HFPO-DA (13C3 HFPO-DA) ranged from 14-98%. Four (4) of the 18 total analyses were below the target range of 50-200%, with three (3) of those four (4) being the Impinger 1 for all three runs, the highest loaded impinger in all cases. Even though these samples had IDIS recoveries below the data quality objective (DQO) recovery range, the data is assumed to appropriately accurate, and useable for its intended purposes. 5.2.2 Polymer Waste Gas Analyses The analysis results show the concentrations of target compounds in the polymer gas (Feed Line #2) were nominally four (4) orders of magnitude lower than in Feed Line #1. Please refer to Table 5-3 for the polymer waste gas (Line # 2) SW-846 Method 8260B analysis surrogate spike recoveries. For the SW-846 Method 8260B (volatile organic) analyses for COF2, HFPO, HFPO-DAF, and Fluoroether E-1, surrogate spike recoveries ranged from 90-107%. Four (4) standard surrogate spike compounds spanning the volatile range are reported. The narrow range and high degree of surrogate recoveries represent a relatively high degree of precision and accuracy with regard to the measurements of these target analytes in the high concentration waste gas samples. Table 5-4 displays the polymer waste gas (Line # 2) EPA Method 537 analysis IDIS spike recoveries. The IDIS spike recoveries of the isotopically-labeled HFPO-DA (13C3 HFPO-DA) ranged from 13-107%. Even though these samples had IDIS recoveries below the DQO recovery range, the data is appropriately accurate, and useable for its intended purposes. 5.3 STACK GAS SAMPLING Measurement of the stack gas emission rates of the five (5) target PFAS compounds involved two (2) sampling trains: • Modified Method 18 for COF2, HFPO, HFPO-DAF, and Fluoroether E-1, and • Modified Method 0010 for HFPO-DA. The Modified Method 0010 stack was performed for 180 minutes during each test run to sample a minimum of three (3) dry standard cubic meters (dscm) of stack gas. The Modified Method 18 sampling was performed concurrently. The following sections examine the quality of the thermal oxidizer stack gas emissions sampling and analysis data results, and the associated impacts on the measurement of the thermal oxidizer DE performance. 5.3.1 Stack Gas Modified Method 18 Results Please refer to Table 5-5 for the Modified Method 18 analysis surrogate spike recoveries. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 39 Focus Project No. P-001393 For the SW-846 Method 8260B (volatile organic) analyses for COF2, HFPO, HFPO-DAF, and Fluoroether E-1, surrogate spike recoveries ranged from 85-112% with the target recovery being 50-150%. The stack gas Modified Method 18 samples were analyzed using selected ion monitoring (SIM) technique to reduces the detection (reporting) limits to substantially lower levels. For this reason, recoveries of only the two (2) surrogate compounds associated with the target analytes are reported. Conversely, the previously discussed waste gas line Modified Method 18 analyses were analyzed at normal Method 8260B levels with all four (4) of the standard surrogate spike compounds spanning the volatile range being reported. The narrow range and high degree of surrogate recoveries represent a relatively high degree of both precision and accuracy with regard to the measurements of these target analytes in the stack gas. All of the Modified Method 18 target analytes were “non-detect” in all sample fractions. The analytical data quality indicators display sufficient accuracy of the low measurements, and indicate that the data is reliable for demonstrating that the actual DE of the measured compounds exceeds the reported 99.999%. 5.3.2 Stack Gas Modified Method 0010 Results Please refer to Table 5-6 for the Modified Method 0010 sampling and analysis surrogate spike recoveries. For the EPA Method 537 analyses of the Modified Method 0010 sampling train fractions, two (2) types of surrogate spikes and three (3) isotopically labeled spiking compounds were used: • Two (2) sampling surrogates applied to the XAD-2 resin before field sampling: − Isotopically labeled perfluorooctanoic acid (PFOA) (13C8 PFOA) − Isotopically labeled perfluorooctanesulfonic acid (PFOS) (13C8 PFOS) • One analysis IDIS, isotopically labeled HFPO (13C3 HFPO-DA) applied to each analytical fraction during sample preparation for analysis. The two (2) sampling surrogate compounds applied to the XAD-2 resins provide a comprehensive assessment of the system’s ability to capture and retain the target analyte through all the sampling and analysis processes. The analysis IDIS applied to all analytical fractions provides an assessment of the ability to recover the target analyte through the sample preparation and analysis processes. The Modified Method 0010 fractions were analyzed using high performance precision liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). The recoveries for the two sampling surrogate spike compounds ranged from 102-132% for 13C8 PFOA and 87-94% for 13C8 PFOS. The target range for these compounds was 50-150%. These excellent recoveries demonstrate the ability to capture and retain the target analyte on XAD-2 resin. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 40 Focus Project No. P-001393 The recoveries for the IDIS surrogate spike compound ranged from 79-102% for 13C3 HFPO-DA. The target range was 25-150%. The excellent recoveries demonstrate the ability to recover the target analyte through the sample preparation and analysis processes. Table 5-6 also shows recoveries for the two (2) sampling surrogate spike compounds in the impinger and breakthrough XAD-2 fractions. These surrogate compounds are not actually applied to the sample fractions noted. Analysis data for 13C8 PFOA and 13C8 PFOS in these post XAD-2 resin sample fractions was obtained to assess if the surrogates applied to the XAD-2 resins are being stripped and travel to the impingers or the second XAD-2 trap during the sample flow through the sampling train. The values are all less than 1% which demonstrate the sampling surrogate spikes are not traveling within the sampling train. These analytical data quality indicators for the Modified Method 0010 sampling and analysis indicate that the data are sufficiently accurate for these very low-level stack gas measurements and that the data are usable for their intended purpose. 5.3.3 Positive HFPO-DA Results All of the Modified Method 0010 stack gas train fractions exhibited low level positive results for HFPO-DA. Please refer to Table 5-7. Individual fraction and sampling train total results are all less than one (1) microgram (ug). Similar HFPO-DA levels were exhibited in the blank train (BT) and proof blank (PB) analyses. The reagent blank and XAD-2 resin media checks all displayed “non-detect” levels. These positive results appear to be due to background sources and have no significant impact on the DE performance determinations. The exact source of the low-level positive HFPO-DA results is unclear. The analysis data perhaps point to possible sampling train component artifacts, or background. It is not probable that the HFPO-DA in the samples originated from thermal oxidizer emissions. The potential for HFPO-DA to pass through the combustion system as HFPO-DA is thermodynamically improbable. Fluoroether E-1 is the thermal decarboxylation product of HFPO-DA which occurs at approximately 200-250oF. Incomplete combustion of HFPO-DA could possibly be exhibited as Fluoroether E-1. However, the Modified Method 18 samples all give non-detect results for Fluoroether E-1 which makes the survival hypothesis seem remote. Other low-level background HFPO-DA sources are considered probable. 5.4 PROCESS WATER ANALYSES The demineralized make-up water used in the scrubber system, and the HF acid and Stage 4 purge streams from the scrubber system were sampled and analyzed for the same five (5) target PFAS compounds. The analyses are summarized in Table 5-8. The purpose for the sampling and analyses of the demineralized make-up water samples was to evaluate possible target analyte contamination introduced to the stack gas samples. The purpose of the acid and purge samples was to evaluate the possible fate of the target analytes. There were two positive results for HFPO-DA in the Run 2 and Run 3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 41 Focus Project No. P-001393 HF acid samples, both below the reporting limit (RL). All other process water analyses were negative the five (5) target PFAS compounds. 5.5 OTHER ADDITIONAL TESTING PERFORMED Two additional testing programs were conducted on the thermal oxidizer: • Pretest performed January 3-4, 2020, and • DE performance test conducted February 4-5, 2020. The January 3-4, 2002 pretest was performed as a full-dress rehearsal for the test team to work through all testing logistics, analyses, and reporting. During the January test, only the monomer manufacturing operations (Line #1) were directing PFAS-bearing waste gas to the thermal oxidizer. The polymer manufacturing was not operating at that time. Although all PFAS DE performance exceeded 99.99% during these tests, the results do not reflect the thermal oxidizer standard operations treating both monomer and polymer manufacturing waste gases. The initial attempt at the formal DE test was conducted February 4-5, 2020. Analysis results of the stack gas samples indicated the presence of contamination of the target PFAS compound HFPO in the stack gas Modified Method 18 train samples. Several observations regarding the HFPO contamination imply that the source is not derived from the stack gas sampling: • The concentration profiles are erratic and progressively increase in the successive sampling train impingers, • The blank train had similar background contamination features as are observed for the Run 1-3 trains, • The proof blank for the sampling trains were contaminated at levels comparable to the sampling trains, • The reagent blanks were non-detect. However, the exact source or cause of the contamination was not isolated or determined. All PFAS DE performance exceeded 99.99% inclusive of the HFPO contamination analysis results. In response, Chemours elected to perform additional testing of the thermal oxidizer. To address the suspected HFPO contamination, the stack gas Modified Method 18 sampling train impinger and connecting tubing components were subjected to an aggressive cleaning process involving soaking in a mild caustic solution and baking in an oven to remove any possible contaminants. The cleaning process was followed up with performance of a proof blank analysis to verify the absence of contamination. The DE testing was performed February 28-29, 2020 to prove the source of the positive analytical results was indeed contamination and not from incomplete combustion in the thermal oxidizer. The February 28-29, Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 42 Focus Project No. P-001393 2020 DE testing, as reported herein, did not exhibit positive results for any of the Modified Method 18 sampled compounds including HFPO. The January 3-4 and February 4-5, 2020 test results are reported separately. Below is a summary of the Thermal oxidizer performance from these other tests. Test Date Run 1 Run 2 Run 3 Average January 3-4, 2020 >99.99987% >99.99984% >99.99983% >99.99985 February 4-5, 2020 >99.99918% >99.9986% >99.99981% >99.99921 5.6 OVERALL DATA QUALITY ASSESSMENT A comprehensive review has been conducted of the thermal oxidizer performance test data quality indicators. Quality assurance and quality control (QA/QC) measurements indicate the data sets for this test project are representative of the processes from which they are derived, and that sufficient measurements have been performed to assess the overall precision and accuracy. The conclusion from this assessment is all the data are of sufficient quality to be used for their intended purposes. Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 43 Focus Project No. P-001393 Table 5-1. Monomer Waste Gas (Line #1) Method 8260B Analysis Surrogate Recoveries Method 8260B Analysis Surrogate Recoveries Run Surrogate Recovery Sample Fraction No. 1 2 3 4 Z- 1334 Monomer Feed Line, MM18, Impinger #1 1 102% 97% 93% 95% COF2 Exceeded Range; Re-analysis 103% 97% 95% 96% Z- 1335 Monomer Feed Line, MM18, Impinger #2 1 103% 97% 94% 96% Z- 1336 Monomer Feed Line, MM18, Impinger #3 1 105% 97% 91% 97% Z- 1337 Monomer Feed Line, MM18, Impinger #4 1 105% 97% 94% 95% Z- 1338 Monomer Feed Line, MM18, Impinger #5 1 104% 95% 92% 96% Z- 1339 Monomer Feed Line, MM18, Impinger #6 1 105% 97% 92% 96% HFPO Exceeded Range; Re-analysis 105% 97% 92% 95% Z- 1340 Monomer Feed Line, MM18, Impinger #1 2 105% 95% 95% 97% Z- 1341 Monomer Feed Line, MM18, Impinger #2 2 105% 96% 94% 95% Z- 1342 Monomer Feed Line, MM18, Impinger #3 2 105% 96% 92% 96% Z- 1343 Monomer Feed Line, MM18, Impinger #4 2 102% 95% 93% 97% Z- 1344 Monomer Feed Line, MM18, Impinger #5 2 104% 97% 93% 97% Z- 1345 Monomer Feed Line, MM18, Impinger #6 2 106% 97% 94% 96% Z- 1346 Monomer Feed Line, MM18, Impinger #1 3 106% 98% 95% 94% COF2 Exceeded Range; Re-analysis 107% 96% 94% 95% Z- 1347 Monomer Feed Line, MM18, Impinger #2 3 103% 96% 92% 96% Z- 1348 Monomer Feed Line, MM18, Impinger #3 3 104% 97% 90% 95% Z- 1349 Monomer Feed Line, MM18, Impinger #4 3 105% 97% 92% 95% Z- 1350 Monomer Feed Line, MM18, Impinger #5 3 105% 95% 93% 95% Z- 1351 Monomer Feed Line, MM18, Impinger #6 3 105% 96% 94% 95% No. Surrogate Target 1 1,2-Dichloroethane-d4 70% - 160% 2 4-Bromofluorobenzene 57% - 152% 3 Dibromofluoromethane 62% - 134% 4 Toluene-d8 71% - 139% Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 44 Focus Project No. P-001393 Table 5-2. Monomer Waste Gas (Line #1) Method 537 Analysis IDIS Recoveries EPA Method 537 Analysis Surrogate Recoveries Run 13C3 HFPO- DA Sample Fraction No. 50-200% Z- 1334 Monomer Feed Line, MM18, Impinger #1 1 33% Z- 1335 Monomer Feed Line, MM18, Impinger #2 1 83% Z- 1336 Monomer Feed Line, MM18, Impinger #3 1 77% Z- 1337 Monomer Feed Line, MM18, Impinger #4 1 98% Z- 1338 Monomer Feed Line, MM18, Impinger #5 1 44% Z- 1339 Monomer Feed Line, MM18, Impinger #6 1 57% Z- 1340 Monomer Feed Line, MM18, Impinger #1 2 20% Z- 1341 Monomer Feed Line, MM18, Impinger #2 2 75% Z- 1342 Monomer Feed Line, MM18, Impinger #3 2 64% Z- 1343 Monomer Feed Line, MM18, Impinger #4 2 67% Z- 1344 Monomer Feed Line, MM18, Impinger #5 2 91% Z- 1345 Monomer Feed Line, MM18, Impinger #6 2 93% Z- 1346 Monomer Feed Line, MM18, Impinger #1 3 14% Z- 1347 Monomer Feed Line, MM18, Impinger #2 3 58% Z- 1348 Monomer Feed Line, MM18, Impinger #3 3 56% Z- 1349 Monomer Feed Line, MM18, Impinger #4 3 70% Z- 1350 Monomer Feed Line, MM18, Impinger #5 3 60% Z- 1351 Monomer Feed Line, MM18, Impinger #6 3 67% Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 45 Focus Project No. P-001393 Table 5-3. Polymer Waste Gas (Line #2) Method 8260B Analysis Surrogate Recoveries Method 8260B Analysis Surrogate Recoveries Run Surrogate Recovery Sample Fraction No. 1 2 3 4 E- 1134 Polymer Feed Line, MM18, Impinger #1 1 105% 97% 91% 99% E- 1135 Polymer Feed Line, MM18, Impinger #2 1 103% 97% 93% 100% E- 1136 Polymer Feed Line, MM18, Impinger #3 1 103% 97% 93% 100% E- 1137 Polymer Feed Line, MM18, Impinger #4 1 102% 97% 91% 100% E- 1138 Polymer Feed Line, MM18, Impinger #5 1 103% 97% 91% 100% E- 1139 Polymer Feed Line, MM18, Impinger #6 1 104% 95% 92% 99% E- 1140 Polymer Feed Line, MM18, Impinger #1 2 104% 97% 91% 98% E- 1141 Polymer Feed Line, MM18, Impinger #2 2 103% 97% 91% 99% E- 1142 Polymer Feed Line, MM18, Impinger #3 2 103% 97% 91% 100% E- 1143 Polymer Feed Line, MM18, Impinger #4 2 101% 98% 91% 100% E- 1144 Polymer Feed Line, MM18, Impinger #5 2 102% 97% 90% 98% E- 1145 Polymer Feed Line, MM18, Impinger #6 2 103% 97% 91% 99% E- 1146 Polymer Feed Line, MM18, Impinger #1 2 105% 97% 90% 100% E- 1147 Polymer Feed Line, MM18, Impinger #2 3 106% 98% 93% 99% E- 1148 Polymer Feed Line, MM18, Impinger #3 3 104% 97% 90% 99% E- 1149 Polymer Feed Line, MM18, Impinger #4 3 102% 97% 92% 99% E- 1150 Polymer Feed Line, MM18, Impinger #5 3 104% 97% 91% 99% E- 1151 Polymer Feed Line, MM18, Impinger #6 3 103% 96% 92% 98% No. Surrogate Target 1 1,2-Dichloroethane-d4 70% - 160% 2 4-Bromofluorobenzene 57% - 152% 3 Dibromofluoromethane 62% - 134% 4 Toluene-d8 71% - 139% Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 46 Focus Project No. P-001393 Table 5-4. Polymer Waste Gas (Line #2) EPA Method 537 Analysis IDIS Recoveries EPA Method 537 Analysis Surrogate Recoveries Run 13C3 HFPO- DA Sample Fraction No. 50-200% E- 1134 Polymer Feed Line, MM18, Impinger #1 1 18% E- 1135 Polymer Feed Line, MM18, Impinger #2 1 19% E- 1136 Polymer Feed Line, MM18, Impinger #3 1 33% E- 1137 Polymer Feed Line, MM18, Impinger #4 1 63% E- 1138 Polymer Feed Line, MM18, Impinger #5 1 91% E- 1139 Polymer Feed Line, MM18, Impinger #6 1 102% E- 1140 Polymer Feed Line, MM18, Impinger #1 2 25% E- 1141 Polymer Feed Line, MM18, Impinger #2 2 17% E- 1142 Polymer Feed Line, MM18, Impinger #3 2 37% E- 1143 Polymer Feed Line, MM18, Impinger #4 2 70% E- 1144 Polymer Feed Line, MM18, Impinger #5 2 107% E- 1145 Polymer Feed Line, MM18, Impinger #6 2 107% E- 1146 Polymer Feed Line, MM18, Impinger #1 3 13% E- 1147 Polymer Feed Line, MM18, Impinger #2 3 28% E- 1148 Polymer Feed Line, MM18, Impinger #3 3 34% E- 1149 Polymer Feed Line, MM18, Impinger #4 3 59% E- 1150 Polymer Feed Line, MM18, Impinger #5 3 96% E- 1151 Polymer Feed Line, MM18, Impinger #6 3 106% Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 47 Focus Project No. P-001393 Table 5-5. Stack Gas Modified Method 18 Analysis Surrogate Recoveries Method 8260B Analysis Surrogate Recoveries Run Surrogate Recovery Sample Fraction No. 1 2 G- 2764 Stack Gas, MM18, Impinger #1 1 112% 91% G- 2765 Stack Gas, MM18, Impinger #2 1 112% 88% G- 2766 Stack Gas, MM18, Impinger #3 1 108% 87% G- 2767 Stack Gas, MM18, Impinger #4 1 109% 89% G- 2768 Stack Gas, MM18, Impinger #5 1 106% 85% G- 2769 Stack Gas, MM18, Impinger #6 1 108% 88% G- 2770 Stack Gas, MM18, Impinger #7 1 110% 87% G- 2771 Stack Gas, MM18, Impinger #1 2 111% 87% G- 2772 Stack Gas, MM18, Impinger #2 2 105% 88% G- 2773 Stack Gas, MM18, Impinger #3 2 105% 88% G- 2774 Stack Gas, MM18, Impinger #4 2 111% 89% G- 2775 Stack Gas, MM18, Impinger #5 2 108% 88% G- 2776 Stack Gas, MM18, Impinger #6 2 109% 90% G- 2777 Stack Gas, MM18, Impinger #7 2 110% 89% G- 2778 Stack Gas, MM18, Impinger #1 3 110% 89% G- 2778 Stack Gas, MM18, Impinger #2 3 109% 90% G- 2779 Stack Gas, MM18, Impinger #3 3 110% 90% G- 2780 Stack Gas, MM18, Impinger #4 3 110% 90% G- 2781 Stack Gas, MM18, Impinger #5 3 111% 92% G- 2782 Stack Gas, MM18, Impinger #6 3 110% 90% G- 2783 Stack Gas, MM18, Impinger #7 3 111% 92% No. Surrogate Target 1 1,2-Dichloroethane-d4 50% - 150% 2 Dibromofluoromethane 50% - 150% Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 48 Focus Project No. P-001393 Table 5-6. Stack Gas Modified Method 0010 Analysis IDIS Recoveries EPA Method 537 Analysis Surrogate Recoveries Run Surrogate Recovery Sample Number Sampling Train Fraction No. 1 2 3 M- 1177 Stack Gas, MM0010, Front Half 1 93% NA NA M- 1178 Composite M- 1179 Stack Gas, MM0010, Back Half 1 97% 132% 87% M- 1180 Composite M- 1182 M- 1181 Stack Gas, MM0010, Impingers 1 99% 0.1% 0.05% M- 1183 Stack Gas, MM0010, Breakthrough XAD 1 93% 0.04% 0.03% M- 1184 Stack Gas, MM0010, Front Half 2 79% NA NA M- 1185 Composite M- 1186 Stack Gas, MM0010, Back Half 2 92% 102% 91% M- 1187 Composite M- 1189 M- 1188 Stack Gas, MM0010, Impingers 2 95% 0.9% 0.2% M- 1190 Stack Gas, MM0010, Breakthrough XAD 2 84% 0.06% 0.006% M- 1191 Stack Gas, MM0010, Front Half 3 88% NA NA M- 1192 Composite M- 1193 Stack Gas, MM0010, Back Half 3 92% 104% 94% M- 1194 Composite M- 1196 M- 1195 Stack Gas, MM0010, Impingers 3 102% 0.3% 0.06% M- 1197 Stack Gas, MM0010, Breakthrough XAD 3 89% 0.08% 0.07% No. Surrogate Target 1 13C3 HFPO-DA 25% - 150% 2 13C8 PFOA 50% - 150% 3 13C8 PFOS 50% - 150% Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 49 Focus Project No. P-001393 Table 5-7. Thermal Oxidizer Modified Method 0010 Analysis Results Parameter Units Run 1 Run 2 Run 3 BT PB Method 0010 Front Half ug 0.0284 0.0279 0.0216 0.188 Method 0010 Back Half ug 0.164 0.0941 0.0716 0.0679 Method 0010 Impingers ug 0.0259 0.0376 0.0237 0.0281 Total ug 0.218 0.160 0.117 0.284 0.00267 Method 0010 Breakthrough XAD ug 0.00488 0.0167 0.0107 0.00124 Methanol Reagent Blank HFPO-DA ug< 0.00160 ND Deionized Water Blank HFPO-DA ug< 0.0120 ND XAD-2 Resin Media Check 1 HFPO-DA ug < 0.00160 ND XAD-2 Resin Media Check 2 HFPO-DA ug < 0.00300 ND Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 50 Focus Project No. P-001393 Table 5-8. Thermal Oxidizer Process Water Analyses Demineralized Water Analyses Compound Units Run 1 Run 2 Run 3 Average Compounds Analyzed by EPA 537 HFPO-DA ng/L < 3.92 ND < 4.00 ND < 3.81 ND < 3.91 ND Compounds Analyzed by Method 8260B Carbonyl Difluoride mg/kg < 4.18 ND < 4.21 ND < 4.14 ND < 4.18 ND HFPO-DAF mg/kg < 1.32 ND < 1.33 ND < 1.31 ND < 1.32 ND HFPO mg/kg < 1.20 ND < 1.21 ND < 1.19 ND < 1.20 ND Fluoroether(E-1) mg/kg < 1.37 ND < 1.38 ND < 1.36 ND < 1.37 ND HF Acid Analyses Compound Units Run 1 Run 2 Run 3 Average Compounds Analyzed by EPA Method 537 HFPO-DA ng/L 1.81 J < 4.36 ND 1.57 J 2.58 Compounds by Analyzed Method 8260B Carbonyl Difluoride mg/kg < 4.18 ND < 4.12 ND < 4.07 ND < 4.12 ND HFPO-DAF mg/kg < 1.32 ND < 1.30 ND < 1.28 ND < 1.30 ND HFPO mg/kg < 1.20 ND < 1.18 ND < 1.16 ND < 1.18 ND Fluoroether(E-1) mg/kg < 1.37 ND < 1.35 ND < 1.33 ND < 1.35 ND Stage 4 Purge Analyses Compound Units Run 1 Run 2 Run 3 Average Compounds by Analyzed EPA Method 537 HFPO-DA ng/L < 3.88 ND < 3.84 ND < 3.81 ND < 3.8 ND Compounds Analyzed by Method 8260B Carbonyl Difluoride mg/kg < 3.96 ND < 4.16 ND < 4.04 ND < 4.05 ND HFPO-DAF mg/kg < 1.25 ND < 1.31 ND < 1.28 ND < 1.28 ND HFPO mg/kg < 1.14 ND < 1.19 ND < 1.16 ND < 1.16 ND Fluoroether(E-1) mg/kg < 1.30 ND < 1.36 ND < 1.33 ND < 1.33 ND Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 51 Focus Project No. P-001393 Figure 5-1. Monomer Waste Gas (Line #1) Modified Method 18 Condensable Vapor Capture Efficiency Run No. Impinger #1Impinger #1 (%) Impinger #2Impinger #2 (%) Impinger #3Impinger #3 (%) Impinger #4Impinger #4 (%) Impinger #5Impinger #5 (%) Impinger #6Impinger #6 (%)Net Weight Gain (g)1 101.4 83.9% 6.1 5.0% 2.5 2.1% 2.0 1.7% 7.6 6.3% 1.2 1.0% 120.8 2 116.2 89.7% 9.4 7.3% -4.0 -3.1% 2.8 2.2% 2.4 1.9% 2.8 2.2% 129.6 3 170.1 89.6% 10.5 5.5% 3.0 1.6% 2.3 1.2% 1.6 0.8% 2.3 1.2% 189.8 Impinger Units = gramsChemours - Fayetteville NCModified Method 18 Train Impinger Distribution of PFASTO Performance Test Graph of Feed Line #1 Impinger Weights101.46.12.52.07.61.2116.29.4-4.02.82.42.8170.110.53.02.31.62.3-20.00.020.040.060.080.0100.0120.0140.0160.0180.0Impinger #1 Impinger #2 Impinger #3 Impinger #4 Impinger #5 Impinger #6Net Weight Gain in GramsImpinger NumberDistribution of Weight Gain in Modified Method 18 Train ImpingersRun #1Run #2Run #3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 52 Focus Project No. P-001393 Figure 5-2. Polymer Waste Gas (Line #2) Modified Method 18 Condensable Vapor Capture Efficiency Run No. Impinger #1Impinger #1 (%) Impinger #2Impinger #2 (%) Impinger #3Impinger #3 (%) Impinger #4Impinger #4 (%) Impinger #5Impinger #5 (%) Impinger #6Impinger #6 (%)Net Weight Gain (g)1 0.7 46.7% 0.4 26.7% 0.2 13.3% 0.2 13.3% 0.0 0.0% 0.0 0.0% 1.5 2 15.5 553.6% -10.9 -389.3% -2.4 -85.7% 0.4 14.3% 0.3 10.7% -0.1 -3.6% 2.8 3 2.9 69.0% 0.4 9.5% 0.4 9.5% 0.3 7.1% 0.1 2.4% 0.1 2.4% 4.2 Impinger Units = gramsChemours - Fayetteville NCTO Performance Test Graph of Feed Line #2 Impinger WeightsModified Method 18 Train Impinger Distribution of PFAS0.70.40.20.20.00.015.5-10.9-2.40.40.3-0.12.90.40.40.30.10.1-15.0-10.0-5.00.05.010.015.020.0Impinger #1 Impinger #2 Impinger #3 Impinger #4 Impinger #5 Impinger #6Net Weight Gain in GramsImpinger NumberDistribution of Weight Gain in Modified Method 18 Train ImpingersRun #1Run #2Run #3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 53 Focus Project No. P-001393 Figure 5-3. Monomer Waste Gas (Line #1) Modified Method 18 COF2 Capture Run No.Impinger #1 (µg/Sample)Percent (%) Impinger #1Impinger #2 (µg/Sample)Percent (%) Impinger #2Impinger #3(µg/Sample)Percent (%) Impinger #3Impinger #4(µg/Sample)Percent (%) Impinger #4Impinger #5 (µg/Sample)Percent (%) Impinger #5Impinger #6(µg/Sample)Percent (%) Impinger #6Train Total (µg)1 46,600,000 96% 1,570,000 3% 124,000 0% 0 0% 0 0% 0 0% 48,294,0002 45,300,000 97% 1,180,000 3% 67,400 0% 0 0% 0 0% 0 0% 46,547,4003 68,000,000 95% 3,420,000 5% 139,000 0% 0 0% 0 0% 0 0% 71,559,000Chemours - Fayetteville Works Thermal Oxidizer (TO) February 2020 Performance Test 2Distribution for Modified Method 18 Analytical Results and Train Distribution of Carbonyl DifluorideTO Feed Line #146,600,0001,570,000124,00000045,300,0001,180,00067,40000068,000,0003,420,000139,000000010,000,00020,000,00030,000,00040,000,00050,000,00060,000,00070,000,00080,000,000Impinger #1 (µg/Sample)Impinger #2 (µg/Sample)Impinger #3 (µg/Sample)Impinger #4 (µg/Sample)Impinger #5 (µg/Sample)Impinger #6 (µg/Sample)ug/SampleSampling Train Impinger NumberDistribution of Carbonyl Difluoride in Method 18 Train ComponentsRun #1Run #2Run #3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 54 Focus Project No. P-001393 Figure 5-4. Monomer Waste Gas (Line #1) Modified Method 18 HFPO Capture Run No.Impinger #1 (µg/Sample)Percent (%) Impinger #1Impinger #2 (µg/Sample)Percent (%) Impinger #2Impinger #3(µg/Sample)Percent (%) Impinger #3Impinger #4(µg/Sample)Percent (%) Impinger #4Impinger #5 (µg/Sample)Percent (%) Impinger #5Impinger #6(µg/Sample)Percent (%) Impinger #6Train Total (µg)1 180,000 12.9% 345,000 24.7% 266,000 19.0% 208,000 14.9% 153,000 10.9% 246,000 17.6% 1,398,0002 338,000 28.9% 285,000 24.4% 203,000 17.4% 164,000 14.0% 102,000 8.73% 75,800 6.49% 1,167,8003 90,800 6.11% 461,000 31.0% 365,000 24.6% 267,000 18.0% 97,800 6.58% 205,000 13.8% 1,486,600Chemours - Fayetteville Works Thermal Oxidizer (TO) February 2020 Performance Test 2Distribution for Modified Method 18 Analytical Results and Train Distribution of 2-MTP as HFPO (Monomer)TO Feed Line #1180,000345,000266,000208,000153,000246,000338,000285,000203,000164,000102,00075,80090,800461,000365,000267,00097,800205,000050,000100,000150,000200,000250,000300,000350,000400,000450,000500,000Impinger #1 (µg/Sample)Impinger #2 (µg/Sample)Impinger #3 (µg/Sample)Impinger #4 (µg/Sample)Impinger #5 (µg/Sample)Impinger #6 (µg/Sample)ug/SampleSampling Train Impinger NumberDistribution of 2-MTP as HFPO in Method 18 Train ComponentsRun #1Run #2Run #3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 55 Focus Project No. P-001393 Figure 5-5. Monomer Waste Gas (Line #1) Modified Method 18 HFPO-DA Capture Run No.Impinger #1 (µg/Sample)Percent (%) Impinger #1Impinger #2 (µg/Sample)Percent (%) Impinger #2Impinger #3(µg/Sample)Percent (%) Impinger #3Impinger #4(µg/Sample)Percent (%) Impinger #4Impinger #5 (µg/Sample)Percent (%) Impinger #5Impinger #6(µg/Sample)Percent (%) Impinger #6Train Total (µg)1 1,410 79.8% 156 8.83% 69.2 3.92% 35.6 2.02% 66.0 3.74% 29.2 1.65% 1,7662 5,050 95.7% 114 2.16% 57.7 1.09% 32.2 0.610% 15.8 0.299% 6.34 0.120% 5,2763 6,440 93.7% 254 3.69% 78.8 1.15% 43.6 0.634% 33.0 0.480% 26.8 0.390% 6,876Chemours - Fayetteville Works Thermal Oxidizer (TO) February 2020 Performance Test 2Distribution for Modified Method 18 Analytical Results and Train Distribution of HFPO-DATO Feed Line #11,41015669.235.666.029.25,05011457.732.215.86.346,44025478.843.633.026.801,0002,0003,0004,0005,0006,0007,000Impinger #1 (µg/Sample)Impinger #2 (µg/Sample)Impinger #3 (µg/Sample)Impinger #4 (µg/Sample)Impinger #5 (µg/Sample)Impinger #6 (µg/Sample)ug/SampleSampling Train Impinger NumberDistribution of HFPO-DA in Method 18 Train ComponentsRun #1Run #2Run #3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 56 Focus Project No. P-001393 Figure 5-6. Polymer Waste Gas (Line #2) Modified Method 18 HFPO-DAF Capture Run No.Impinger #1 (µg/Sample)Percent (%) Impinger #1Impinger #2 (µg/Sample)Percent (%) Impinger #2Impinger #3(µg/Sample)Percent (%) Impinger #3Impinger #4(µg/Sample)Percent (%) Impinger #4Impinger #5 (µg/Sample)Percent (%) Impinger #5Impinger #6(µg/Sample)Percent (%) Impinger #6Train Total (µg)1 235 58.7% 118 29.5% 47.5 11.9% 0 0% 0 0% 0 0% 4012 0 0% 110 100% 0 0% 0 0% 0 0% 0 0% 1103 205 100% 0 0% 0 0% 0 0% 0 0% 0 0% 205Chemours - Fayetteville Works Thermal Oxidizer (TO) February 2020 Performance Test 2Distribution for Modified Method 18 Analytical Results and Train Distribution of HFPO Dimer, methyl ester as HFPO-DAFTO Feed Line #223511847.50000110000020500000050100150200250Impinger #1 (µg/Sample)Impinger #2 (µg/Sample)Impinger #3 (µg/Sample)Impinger #4 (µg/Sample)Impinger #5 (µg/Sample)Impinger #6 (µg/Sample)ug/SampleSampling Train Impinger NumberDistribution of HFPO dimer, methyl ester as HFPO-DAF in Method 18 Train ComponentsRun #1Run #2Run #3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 57 Focus Project No. P-001393 Figure 5-7. Polymer Waste Gas (Line #2) Modified Method 18 Fluoroether E-1 Capture Run No.Impinger #1 (µg/Sample)Percent (%) Impinger #1Impinger #2 (µg/Sample)Percent (%) Impinger #2Impinger #3(µg/Sample)Percent (%) Impinger #3Impinger #4(µg/Sample)Percent (%) Impinger #4Impinger #5 (µg/Sample)Percent (%) Impinger #5Impinger #6(µg/Sample)Percent (%) Impinger #6Train Total (µg)11,010 76.9% 248 18.9% 54.7 4.17% 0 0% 0 0% 0 0%1,3132802 76.8% 182 17.4% 60.6 5.80% 0 0% 0 0% 0 0%1,0453795 77.9% 134 13.1% 91.3 8.95% 0 0% 0 0% 0 0%1,020Chemours - Fayetteville Works Thermal Oxidizer (TO) February 2020 Performance Test 2Distribution for Modified Method 18 Analytical Results and Train Distribution of Heptafluoropropyl 1,2,2,2-tetrafluoroethyl etherTO Feed Line #21,01024854.700080218260.600079513491.300002004006008001,0001,200Impinger #1 (µg/Sample)Impinger #2 (µg/Sample)Impinger #3 (µg/Sample)Impinger #4 (µg/Sample)Impinger #5 (µg/Sample)Impinger #6 (µg/Sample)ug/SampleSampling Train Impinger NumberDistribution of Heptafluoropropyl 1,2,2,2-tetrafluoroethyl ether in Method 18 Train ComponentsRun #1Run #2Run #3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 58 Focus Project No. P-001393 Figure 5-8. Polymer Waste Gas (Line #2) Modified Method 18 HFPO-DA Capture Run No.Impinger #1 (µg/Sample)Percent (%) Impinger #1Impinger #2 (µg/Sample)Percent (%) Impinger #2Impinger #3(µg/Sample)Percent (%) Impinger #3Impinger #4(µg/Sample)Percent (%) Impinger #4Impinger #5 (µg/Sample)Percent (%) Impinger #5Impinger #6(µg/Sample)Percent (%) Impinger #6Train Total (µg)144.2 59.2% 18.7 25.0% 8.16 10.9% 2.82 3.78% 0.784 1.05% 0 0%74.7230.8 47.4% 24.1 37.1% 8.29 12.8% 1.59 2.45% 0.155 0.239% 0 0%64.9351.8 60.1% 19.7 22.8% 11.7 13.6% 2.76 3.20% 0.263 0.305% 0 0%86.2Chemours - Fayetteville Works Thermal Oxidizer (TO) February 2020 Performance Test 2Distribution for Modified Method 18 Analytical Results and Train Distribution of HFPO-DATO Feed Line #244.218.78.162.820.784030.824.18.291.590.155051.819.711.72.760.26300.010.020.030.040.050.060.0Impinger #1 (µg/Sample)Impinger #2 (µg/Sample)Impinger #3 (µg/Sample)Impinger #4 (µg/Sample)Impinger #5 (µg/Sample)Impinger #6 (µg/Sample)ug/SampleSampling Train Impinger NumberDistribution of HFPO-DA in Method 18 Train ComponentsRun #1Run #2Run #3 Chemours TO DE Test Report 27-Mar-20 Rev 0.doc 59 Focus Project No. P-001393 6.0 CONCLUSION The Chemours thermal oxidizer is controlling PFAS emissions at an average efficiency exceeding 99.99981%, demonstrating compliance with the Consent Decree requirement to control all PFAS at an efficiency of 99.99%.