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Incineration of Fluoropolymers Project presentation "III<s Karlsruhe Institute of Technology (KIT) com BEEP Taylor & Associates, LLC 15th June 2023 2966620 Incineration of fluoropolymers: PFAS analysis along the flue gas pathway A pilot scale trial at conditions similar to household and industrial waste-to-energy incineration plants that typically burn products containing fluoropolymers was conducted to assess the potential generation of any statistically significant uncontrolled emissions of Per- and Polyfluorinated Alkyl Substances (PFAS) at levels that might present a risk nN 2966620 Research partner Sampling partner Laboratory partner Feed sampling Incineration Advisor Academic Consultant Data quality review (under process) Observer Project partners Institute for Technical Chemistry (ITC) at Karlsruhe Institute of Technology (KIT) SGS Institut Fresenius GmbH, Industries & Environment SGS Belgium NV, Institute for Applied Chromatography Pro-K, Fluoropolymer processing and downstream user association, Germany EE Taylor & Associates, LLC, USA I I Environmental Standards Inc., USA = <ity of Montpelier France UBA, Umweltbundesamt (German Federal Environment Agency) 2966620 Test facility BRENDA / Sampling locations Fuel 3 Oil Rotary Kiln Combustion Chamber Air 8Q Waste Heat Boiler Spray Drier Process Steam 40 bar, 250 C Fabric Filter (rl| Adsorbent Flue Gas Scrubber Scrubber 1 Scrubber2 L H,0 SCR Stack Catalyst Thermal power nN 1 Ammonia Liquor Rotary kiln 1.5 MW Salts, Flue Dust Loaded Adsorben O Slag Boiler Ash PFAS sampling fluegas SGS | PFAS Sampling residues & liquids (SGS) Gas Burner = Induced NaOH Draught Flue gas cleaning 17 BImSchv The BRENDA plant is a large facility that is a good representation of commercial waste-to-energy plants in Europe 2966620 Test facility BRENDA/ Post-combustion chamber -Triple T PFAS Start post combustion zone [m] 1 meter above the burners Project, Level setting 7,65 E1b 1 Temperature in the post combustion chamber 860 (PCC) [C] 3 Volume flow Vpce [my/h wet] after boiler 3947 Cross section PCC [m?] Volume flow Vpcc [m*/h] Height h [m] level E1b Residence time from start PCC zone to level E1b [s] 2,82 16.382 10,88 200 setting 2 7,65 1100 3057 2,82 16.382 10,88 2,00 Wood chips / oil / gas burner PFAS, gas measurement, HF (SICK-laser) (+10.88 m) Start post-combustion zone om 2966620 Experimental Setup test | parameters number of HF and ooo samplin start-up with natural gas and oil " : " starting solid feeding (wood chips) background of rotary kiln / combustion chamber with 3 oil, natural gas and 100 kg/h wood chips locations | ' Ha ath solid fuel: woodchip (100 no Top of post- kg/h) + 320 g/h FP together TrFocec:: 860 C;: mbusti with oil and natural 9 gas 20s chanmer s 3 after boiler, stack background of rotary kiln / no combustion chamber with oil, natural gas and 100 kg/h wood chips 3 Change of temperature post combustion chamber background of rotary kiln / combustion chamber with 2 oil, natural gas and wood chips solid fuel: woodchip (100 no kg/h) + 320 g/h FP together Tecc: 1100 } C; with th oil oil and and natnuartuarlal gas 20s 3 Top of postcombustion chamber (E1b), after boiler, stack background of rotary kiln / Wo combustion chamber with oil, natural gas and 100 kg/h wood chips 3 shut down duration [hrs] 24 24 11 9 1" 13 1 12 hn 9 1 13 11 24 RUN date / remarks 25.2.23; 10 a.m. 26.2.23; 10 a.m. day 1 and 2 day 1 27.2.2023: 9 am day 3 Monday feeding of fluoropolymers vennio2ht 2 28.2.2023; 9 am day 4 - stop feeding the flouropolymers in evening Tuesday 3 01.03.2023; 9 am day 5 [Wednesday over night 2 02.03.2028:3 9:am day 6 | Thursday go a feeding of fluoropolviymers 5 03.03.2023; 9 am - flouropolymers stop feeding in the evening day 7 Friday 6 04.03.2023; 9 am day 8 Saturday day 9 Material PTFE tubes Mass fraction [Wt.-%] 63,00 PTFE tape PVDF 7,00 18,00 PFA 6,00 FKM rubber 6,00 mass flow = 320 g/h Basis of fluoropolymer feed mixture: 1. Feed mixture comprises of4 largest volume fluoropolymers - PTFE, PVDF, PFA, FKM. Together these represent 80% of commercial fluoropolymer production 2. Pro-K supplied fluoropolymer samples of major applications that were grinded and mixed 2966620 Main Operational Parameters, Setting 1 and 2 mass flow wood chips main air 13 mass flow heating oil X |volume flow natural gas volume flow combustion air 2E inclination rotation speed temperature flue gas outlet thermal power unit kg/h my'/h kg/h my'/h my*/h rev p.m C MW setting S1 RUN1,2,3 98 setting S2 | RUN4,5,6 98 418 423 61 46 4 4 872 753 0.2 0.4 800 - 900 1.1 0.9 Increase of rotation speed to avoid slagging - 200 kW, shift thermal power to the PCC volume flow natural gas to burner D4.1 " 2 sum of volume flow combustion air to burner D4.1 volume flow natural gas to burner D4.2 sum of volume flow combustion air to burner D4.2 [residence time 22 temperature flue gas post-combustion chamber outlet (with control) [CO (level E2) 8 |0, (level E2) thermal power total thermal power rotary kiln and post combustion chamber -- |volume flow HS] > 0, 52 [co water vapour my'/h my/h my'/h my'/h s C mg/m' Vol.-% dry MW MW my'/h Vol.-% dry mg/m Vol.-% wet 22 671 22 671 860 0.2 1.2 0.46 1.59 3958 11.9 1.35 6.20 35 429 35 428 1095 1.2 7.0 0.72 1.67 3238 9.0 1.64 8.49 Increase of temperature by reduction of stochiometric ratio + 260 kW = constant 2966620 PFAS analysis Modified OTM-45 for sampling train Combustion lon Chromatography (CIC) for Adsorbable Organic Fluorine (AOF) Ultrahigh-Performance Liquid Chromatography coupled to tandem Mass Spectrometer (UPLC-MS/MS) for targeted long chain PFAS Gas chromatography coupled to mass spectrometry (GC-MS) for volatile Fluorocarbons lon chromatography (IC) for Trifluoroacetic Acid (TFA) lon Selective Electrode (ISE) for Inorganic Fluoride Tunable Diode laser for Hydrogen fluoride 2966620 Modified OTM-45 sampling train Thermocouple Temperature Readout canister slot for volatile C1-C4 compunds failsafe XAD-2 Tv) Fitot Tube Ice Bat ol 35380: V . Manome! ter condensate impinger water impinger Stack Gas Flow SGS modified PFAS sampling train 2966620 Testing methodology 24 samples analyzed per setting 3 samples were collected and analyzed at each sampling point per setting (triplicate sampling) PFAS analyzed at Pre-run, Run and Post-run conditions Ash samples were analyzed for target PFAS content Blank media and solutions were analyzed for their respective parameters Blank sample train were analyzed after every run at relevant sample locations 10 2966620 HF measurement after the boiler (Tunable Diode Laser) 30 25 nN o wet*] [mg/m? -[4,} HF -o test of fluoropolymer feeder & LJ Ld N HF-SICK-Laser profile Lad < Pode % om. io a Ld LJ LJ LJ LK av J > $ 1) id eo LJ RUN 1 Fi RUN 2 RUN 3 $ : s RUN 4 LJ RUN 5 3 * RUN 6 0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 *with operational conditions: temperature boiler outlet 270 C, w, = 6,2 Vol.-% (setting 1) and w, = 8,5 Vol.-% (setting 2) Hours of operation 11 2966620 Fluorine balance (based on HF-Laser) Preliminary results based on in-situ measuremnt of HF-concentration in flue gas by the means of HF-laser F -input = 0,230 kg/h 0,200 Setting 1: T=860C, t = 2s 0,182 RR = Recovery Rate [wt.-%] Setting 2: T=1100C, t= 2s [kg/h] 0,150 0,160 output Total Fluorine 79,03% = RR 1,09% 0,69% = RR = RR 0,000 0,002 0,000 I=] I<] ~ Set1/Runl/noF Set 1/ Run 2 / F-feeding Set1/Run3/noF Set2/Run4/noF Setting / Run / Condition Set2/Run5/F-feeding Set2/Run6/noF 12 2966620 Summary of analytical results (860C) Post combustion Avg. Total Fluorine (mg/m') 2 (LOQ (gas) = 27 ug/m'), (LoQ (part) -- 1.7 pg/m') 36.5 Avg. AOF , (LOQ- 27 pg/m') 31.5 After Boiler 17.3 Non-detectable Stack Non-detectable Non-detectable Sum of PFAS (ng/m") 4.5 0.3 TFA ; (LOQ-14 pg/m') Non-detectable Non-detectable Non-detectable 13 2966620 Results from GC-MS analysis (50 samples) Short chain fluorocarbons Tetrafluoromethane Hexafluoroethane Trifluoromethane Hexafluoropropylene Pentafluoroethane Octafluorocyclobutane LOQ (pg/m3) 20 30 20 5 25 25 Results (Stack) Non detectable except 2 values in separate runs near detection limits (20, 27 ug/m3) Non detectable Non detectable Non detectable Non detectable Non detectable 14 2966620 Total expected PFAS emissions from EU incineration plants Total waste incinerated in the EU = 62 million tons per year* Maximum sum of PFAS released (stack) at 860C/1100C with 0.3 % FP feed = 18.4 ng/m3 ,., assuming PFAS <LOQ=0 Specific Flue gas amount released per ton of waste** Total load of PFAS emitted in the EU But, Actual fluoropolymer waste incinerated (85% of 52,000 tons) = 4060 m3 4, = 4.63 kilograms per year for 0.3% FP feed = 44,200 tons per year (0.07% of total waste) Therefore, total PFAS emissions in the EU should be lower than 4.63 kilograms per year 2966620 Results Fluorine Recovery: Fluorine recoveries ranged from 69 to 84% using Tunable Diode Laser - provides strong evidence for mineralization of the Fluoropolymer feed mixture Trifluoroacetic acid: TFA was not detected for all samples at a reporting limit of 14 ug/m? Targeted PFAS analysis: A large majority of samples (> 99% of samples associated with 860C condition and > 98% of samples associated with 1100C condition) indicated that long-chain PFAS were non-detectable at levels of < 1 ng/m3 PFAS analysis of wastewater and ash residue: A large majority of the samples were non-detectable with reporting limits of 0.02 pg/I GC-MS analysis for short chain fluorocarbons: Non-detectable at a reporting limit of 5-30 pg/m? levels 2966620 Conclusions Fluoropolymers are converted to inorganic fluorides (hydrogen fluoride) and carbon dioxide The absence of organic fluorides and PFAS confirms complete mineralization of fluoropolymers Therefore, fluoropolymers do not generate any measurable levels of small molecule PFAS of concern Standard waste-to-energy incineration operating conditions are sufficient for mineralization of fluoropolymers Fluoropolymers pose no risk to human health and the environment at their end of life when incinerated 17 2966620 Thhaannkk yyoouu 296662200