### Page 1 of 24 

# Supplementar **y Material** 
**Inv estigation of Waste Incineration of Fluorotelomer**  **- Based**  **Pol ymers as a Potential Source of PFOA**  **in the Env ironment** 

P. H. Taylor a , 

### * , T. Yamada a 

### , R. C. Striebich a 

### , J. L. Graham a 

### , and R. J. Giraud b

a 

### University of Dayton Research Institute, Environmental Engineering Group, 300 College Park, Dayton, OH 45469
b 

### E. I. du Pont de Nemours and Company, Inc. , 1007 Market Street, W ilmington, DE 19898

* Corresponding author. Tel.: +1 937 672 3065 ; fax: +1 937 229 2503 E
- mail address: ptaylor1@udayton.edu
**Table of Contents** 1.0 Stoichiometric Calculations

................................ ................................ ..................... 3 1.1 Establishing Experimental Conditions

................................ ............................. 3 1.1.1 Constraints

................................ ................................ ........................... 3 1.1.2 Calculating Experimental Run Duration

................................ ................ 3 1.1.3 Summary

................................ ................................ .............................. 4 1.2 Setting Combustion Test Air and Methanol Feed Rates

................................ . 4 1.3 References

................................ ................................ ................................ ...... 6 Tables Table A
- 1. Uncontrolled HF Emiss ions from Mass Burn M WC s Table A
- 2. Stoichiometric Calculation of Complete Oxidation of PTFE in the

Presence of Excess Methanol Table A
- 3. Oxidation of Methanol: Stoichiometric Calculations with Refined

Inputs Table A
- 4. Combustion Stoichiometry Calculat ions for Combustion of FTBP

Composite 1 Table A
- 5. Combustion Stoichiometry Calculations for Combustion of FTBP

Composite 2

### Page 2 of 24



### Table S

- 1. Summary of FTBP Composites Elemental Analysis Table S

- 2. PFOA Analysis Method Description Table S

- 3. FTBP Combustio n Test Analytical Results for Impinger Samples Table S

- 4. Fluoride Ion Recovery & Exhaust Gas Hydrogen Fluoride (HF) Concentration Table S

- 5. PFOA Exhaust Gas Concentration Calculations Table S

- 6. 13 

### C

- PFOA Surrogate Spike Recovery for Combustion Test Aqueous Samples Table S

- 7. Typical W aste Incineration Exhaust Gas Oxygen Levels Figure S

- 1. Typical Structure of a Fluorotelomer

- Based Polymer in this Study Figure S

- 2. Thermogravimetric Analysis of FTBP Composites at 25 o 

### C/min Figure S

- 3. Reactor Temperature Profile for FTBP Combustion Testing

### Page 3 of 24



### 1.0 Stoichiometric Calculations

**1.1 Establishing Experimental Conditions**  Prior to conducting Phase I transport testing, planned Phase II combustion testing experimental conditions for certain operating parameters (i.e., duration of experimental run, target exhaust gas oxygen concentration, and target exhaust gas water concentration) were established to assure consistent operating conditions during both phases of the experimental program.
**1.1.1 Constr**  **aints** The Phase II Quality Assurance Project Plan (submitted to EPA prior to conduct of the Phase I transport test) clearly set the following constraints:
 High temperature reactor operation at a temperature of 1000 o 

### C ( ± 10 o 

### C) for a gas residence time of 2 s econds ( ± 0.2 sec),
 Exhaust gas oxygen concentration “greater than 10% throughout the combustion test run following introduction of the methanol fuel”,
 Exhaust gas water concentration (calculated) of approximately 15% (within range of 8% and 20%) resulting primarily from oxidation of methanol fuel,
 Test substance composite weight of 100 ± 10  g, and
 Combustion test run duration between 15 and 75 minutes after pyroprobe insertion. Furthermore, an ABB EL 3020 continuous gas analyzer (CGA) was in place prior to the Phase I transport test and planned for use to provide continuous monitoring of ox ygen, carbon dioxide, and carbon monoxide during Phase II combustion testing. The CGA’s oxygen analyzer has a design flow rate of 30 to 60 liters per hour (ABB, 2005). Thereby, an additional constraint was to maintain a vapor flow rate greater than 30 li ters per hour (i.e., greater than 500 sccm).
**1.1.2 Calculating Experimental Run Duration**  The elemental composition for the expected Phase II test substances were not known because such analyses (required for Phase II) had not been conducted prior to the P hase I transport test. Therefore, polytetrafluoroethylene (PTFE) was used as a model compound in combustion calculations because it is a fluorinated polymer of known molecular composition (76% F, 24% C). Wi thin the constraints above and for PTFE, it was possible to compute a target experimental run duration using a target exhaust gas hydrogen fluoride (HF) concentration and assuming complete oxidation of the PTFE and the methanol fuel. A target HF concentration of 10 mg HF per dry standard cubic meter ( dscm) was used to correspond to the high end of typical uncontrolled (i.e., combustion section exit) HF emission levels from municipal waste combustors (M WC s), considering the range of 2.3 to 7.9 mg/dscm based on available information summarized in Table A

- 1. (Oxidation of

### Page 4 of 24



### a highly fluorinated polymer (i.e., PTFE) would be expected to yield a high end HF emission level.) Information from mass burn M WC s was used because these units represent over 76% of M WC waste capacity in the U.S. (IW SA, 2002). Based o n the design of the 3

- zone furnace in the thermal reactor system, an effective isothermal reactor length of 20 inches (50.8 cm) was originally expected. (Subsequent temperature profile measurements for Phase I provided an effective reactor length of 23 in ches (58.4 cm) at 250 o 

### C for Phase I and of 26 inches (66 cm) at 1000 o 

### C for Fluorotelomers Phase II.) An effective reactor length of 50.8 cm was used with the reactor tube’s inside diameter (14 mm) to compute the reactor volume corresponding to a gas resid ence time of 2 seconds at 1000 o 

### C in the stoichiometric calculations shown in Table A
- 2. The calculated values in Table A
- 2 show run duration as well as corresponding exhaust oxygen concentration (dry basis) and exhaust gas water concentration at different excess air levels for a fixed methanol to PTFE ratio. This ratio was adjusted through iterative calculations until a run duration for complete oxidation of PTFE in the presence of excess methanol clearly greater than 15 minutes was obtained with an exhau st HF concentration close to the target value of 10 mg/dscm (i.e., 1.22 x 10 - 3 

### %) while assuring the other constraints noted above had been met. Therefore, a run duration of 15.97 minutes (rounded to 16 minutes) was computed and the corresponding values for exhaust gas oxygen concentration (dry basis) and exhaust gas water concentration were 13.0% and 10.3%, respectively. Selecting a target exhaust gas oxygen concentration of 13% dry basis (equivalent to 11.6% wet basis) seemed appropriate to assure oxy gen concentration in exhaust gas greater than 10% throughout the combustion test run following introduction of the methanol fuel as this level appeared high enough to compensate for a potential drop in thermal reactor system exhaust oxygen concentration wh en the polymer would be introduced to the reactor system via pyroprobe gasification.
**1.1.3 Summary**  The following target values for Phase II combustion testing were calculated prior to Phase I transport testing:
 Experimental run duration of 16 minutes,
 Ex haust gas oxygen concentration (dry basis) of 13%, and
 Exhaust gas water concentration of 10.3%. These values were established as targets in Phase I testing to assure consistent operating conditions during both phases of the experimental program.
**1.2 Set**  **ting Combustion Test A ir and Methanol Feed Rates**  Once the effective reactor length was experimentally determined prior to Phase II combustion testing, the effective high temperature reactor volume and total exhaust gas flow corresponding to 2 seconds gas r esidence time were set for the 14 mm inside diameter reactor tube. Combustion stoichiometry calculations prior to Phase II testing

### Page 5 of 24



### were used to iteratively evaluate combinations of synthetic air and methanol feed rates yielding this target total exhaust g as flow rate versus the target values for exhaust gas oxygen (O 2 

### ) and water (H 2 

### O) concentrations established prior to Phase I (see section 1.1.3 above), including consideration of the following factors to fine tune the combustion stoichiometry calculations :  methanol liquid density (as function of liquid temperature and pressure),
 more refined values of Universal gas constant and methanol molecular weight,
 same standard temperature used during calibration of the air mass flow controller,
 oxygen level in the synthetic air on hand as noted on its certificate of analysis
 reactor pressure as sum of monitored values for room pressure + back pressure, and
 input setting/display resolution (number of available digits) for both the air mass flow controller and the methanol feed pump. These calculations are based on complete oxidation of CH 3 

### OH according to the following reaction: CH 3 

### OH + 1.5 O 2 

###  CO 2 

### + 2 H 2 

### O Therefore, for each mole of CH 3 

### OH combusted, 1.5 moles of O 2 

### are consumed, 1 mole of CO 2 

### is produced , and 2 moles of H 2 

### O are produced. As the O 2 

### is supplied in synthetic air made up of nominally 21% O 2 

### and 79% nitrogen (N 2 

### ), each mole of CH 3 

### OH combusted is also accompanied by 79/21 moles of N 2 

### as both an inert reactant and a product. The results of the refine d methanol oxidation stoichiometry calculations shown in Table A
- 3 indicate the predicted concentrations for exhaust gas O 2 

### , CO 2 

### , and H 2 

### O. Further calculations including the contribution of each test substance composite are described in Tables A
- 4 and A
- 5 , which make use of the dry basis elemental analysis results provided by the analytical laboratories after normalizing to 100% to account for differences across the analytical techniques used. The “monitor” entries in the first column in Tables A
- 3, A
- 4, and A
- 5 point out the parameters that are monitored in the thermal reactor system; the “analyzed” entries in the first column of Tables A

- 4 and A
- 5 point out the parameters were values from elemental analysis are used. Comparison of the reaction products in Tables A
- 4 and A
- 5 to the reaction products in Table A
- 3 indicates that the oxidation of methanol is controlling. Based on these calculations (i.e., described in Tables A

- 3,A
- 4, and A
- 5), the estimated amount of oxygen needed for Phase II combustion t esting to provide exhaust O 2 

### and H 2 

### O concentrations comparable to those used in Phase I testing is 662 sccm synthetic air when 61.71 μL/min of methanol is fed. The resulting predicted exhaust H 2 

### O concentration of 10. 2% for the Phase II combustion test (Ta bles A
- 3, A
- 4, A
- 5) is very consistent with the 10.3% calculated value used during the Phase I transport test. The resulting predicted exhaust O 2 

### concentration of 13.1% (dry basis) is very consistent with the 13.0% O 2 

### concentration for the Phase I transpo rt test.

### Page 6 of 24



### 1.3 **References** ABB, 2005. EasyLine Continuous Gas Analyzers Model EL3020 , Data Sheet 10/24_4.10 EN

. Environmental Standards, Inc., December 27, 2005, revised June 23, 2006. Quality Assurance Plan for the ECA Incineration Testing Program

— Phase II Fluorotelomer Incineration Testing. IW SA (Integrated Wa ste Services Association), 2002. The 2002 I WSA Directory of Wa ste
- to
- Energy Plants.

### Page 7 of 24



### Table **A -**  **1** . Uncontrolled HF Emissions from Mass Burn M WC s
**Item Value**  **Units Reference and/or Comment**  Low end reference mass burn MW C **uncontrolled** HF emission 0.009 kg HF/metric ton MSW EPA, Locating and Estimating Air

Toxics Emissions from Municipal Waste Combustors , PB89
- 1952226, April 1989. [ Table 4
- 3 for older ma ss burn MW C s ] MW C exhaust gas volume (ty pic al) 5000 Nm 3 

### /m etric ton MSW Environment Agency of Japan in

“Meeting on Measures to Control Dioxin Emission, the second report, 25 June 199 9” as reported by Ogura et al, Chemosphere 2001, 44, 1473
- 1487. ma ss burn M WC **uncontrolled** HF em ission 1.8 mg HF/ Nm 3 

### calculated (=0.0 0 9/5000*1E06mg/kg)

ma ss burn M WC **uncontrolled** HF emission 1.9 Mg HF/ scm calculated (=1.8*293/273)

EPA, Municipal Waste Combustion: Background Information Document for Promulgated Standards and Guidelines , EPA
- 453/R

- 95
- 0136, October 1 995. [scm at 20 o 

### C and Nm 3 

### at 0 o 

### C] MW C exhaust gas moisture (ty pical) 15 % Environmental Standards, Inc. Quality Assurance Project Plan for the ECA Incineration Testing Program

— Phase II Fluorotelomer Incineration Testing , December 27, 2005, revised June 23, 2006. ma ss burn M WC **uncontrolled** HF em ission 2.3 mg HF/ dscm Conc (Dry) =



### High end ty pical mass burn MW C **uncontrolled** (spray dryer inlet) HF emission, corrected to 7% O2 (test average) 7.9 mg HF/ dscm Clean Air Engineering, Rep ort on

Compliance Testing Performed for Covanta of Fairfax, Inc Units 1, 2, 3, and 4 SDA Inlets and FF Outlets (Stacks) I

- 95 Energy/Resource Recovery Facility , Volume I of III, August 7, 2001. [highest across 3 units tested] Conc (W et)



### 100%

- Volume% H 2 

### O 100%

### Page 8 of 24

**Table A -**  **2.** Stoichiometric C alculation of Complete Oxidation of PTFE in Presence of Excess Methanol **Sample:** PTFE [C2F4] Mass (μg) 100 mo l wt (g/m ol) 100 **Constants Me**  **OH : Sample Ratio** (Variable) 19,000 R 0.0821 L
- atm/(mol

- K) standard T 25 o 

### C **Reactor Inside Dia meter**  **Reactor Length T**  (C) **RT** (sec) pressure 1 atm (mm) 14 (in) 20 1000 2 (cm) 50.8

x (xs Air) Effluent O2

(%) Effluent

H2O (%) Effluent CO2

(%) Effluent HF

(%) Air

Vol (L) Me OH Vol (L) Run

duration (min) Me OH

Injection Rate Air Flow

R ate Me OH

Vapor Flow Rate Input

Vapor Flow Rate Variable Target: >10 Target: 15 (8

- 20) Target: 1.22E
- 3 (μL/min) scc/min scc/min wet scc/min



### Dry Basis Dry Basis Dry

Basis 0% 0.0 23.1 15.1 3.17E
- 03 3.32 0.46 6.90 111.5 481.50 67.41 548.91 10 % 2.0 21.4 13.6 2.86E
- 03 3.65 0.46 7.50 102.5 486.94 61.97 548.91 20% 3.7 19.9 12.4 2.61E
- 03 3.98 0.46 8.11 94.8 491.56 57.35 548.91 30% 5.1 18.5 11.4 2.40E
- 03 4.32 0.46 8.71 88.2 495.54 53.36 548.91 40% 6.3 17.4 10.5 2.22E
- 03 4.65 0.46 9.32 82.5 499.01 49.90 548.91 50% 7.3 16.4 9.8 2.06E
- 03 4.98 0.46 9.92 77.5 502.05 46.86 548.91 60% 8.2 15.5 9.2 1.93E
- 03 5.31 0.46 10.53 73.0 504.74 44.16 548.91 70% 9.0 14.7 8.6 1.81E
- 03 5.64 0.46 11.13 69.1 507.14 41.76 548.91 80% 9.7 13.9 8.1 1.70E
- 03 5.98 0.46 11 .74 65.5 509.30 39.61 548.91 90% 10.3 13.3 7.7 1.61E
- 03 6.31 0.46 12.34 62.3 511.24 37.67 548.91 100% 10.9 12.7 7.3 1.53E
- 03 6.64 0.46 12.95 59.4 513.00 35.91 548.91 110% 11.4 12.1 6.9 1.45E
- 03 6.97 0.46 13.55 56.7 514.60 34.31 548.91 120% 11.8 11.6 6. 6 1.38E
- 03 7.31 0.46 14.16 54.3 516.07 32.84 548.91 130% 12.2 11.2 6.3 1.32E
- 03 7.64 0.46 14.76 52.1 517.41 31.49 548.91 140% 12.6 10.7 6.0 1.27E
- 03 7.97 0.46 15.37 50.0 518.65 30.25 548.91 150% 13.0 10.3 5.8 1.21E
- 03 8.30 0.46 15.97 48.1 519.80 29.11 5 48.91 160% 13.3 10.0 5.5 1.17E
- 03 8.63 0.46 16.57 46.4 520.86 28.05 548.91 170% 13.6 9.6 5.3 1.12E
- 03 8.97 0.46 17.18 44.7 521.85 27.06 548.91 180% 13.9 9.3 5.1 1.08E
- 03 9.30 0.46 17.78 43.2 522.77 26.14 548.91 190% 14.1 9.0 4.9 1.04E
- 03 9.63 0.46 18.3 9 41.8 523.63 25.28 548.91 200% 14.3 8.7 4.8 1.01E
- 03 9.96 0.46 18.99 40.5 524.43 24.47 548.91 210% 14.6 8.5 4.6 9.73E
- 04 10.29 0.46 19.60 39.2 525.19 23.72 548.91 220% 14.8 8.2 4.5 9.42E
- 04 10.63 0.46 20.20 38.0 525.90 23.01 548.91

### Page 9 of 24

**Table A -**  **3.** Oxidati on of Methanol: Stoichiometric Calculations with Refined Inputs **Reactant: Methanol Units**  **Value Reference/Comment**  monitor liquid temperature o C 23.8 Feed pump isothermal T: measured with 1/16" calibrated thermocouple with chiller controlling to 24.0 C m onitor liquid pressure psig 2500 Feed pump controller readout: pump discharge pressure (typical value)

liquid pressure psia 2514.7 liquid density g/mL 0.80296 NIST "Isothermal Properties for Methanol", http://webbook.nist.gov/chemistry/fluid/ a monit or injection rate μ L/min 61.71 Feed pump controller readout

injection rate mL/min 0.06171 mass feed rate g/min 0.0496 = density (g/mL) * injection rate (mL/min) molecular weight g/ mole 32.0419 NIST "Methyl Alcohol", http://webbook.nist.gov/cgi/cboo k.cgi?Name=methanol&Units=SI molar feed rate mol/min 0.0015 = mass feed rate / molecular weight **Reactant: Sy nthetic air** 

std temperature o C 21.1 Brooks gas mass flow controller calibration sheet monitor room pressure torr 740 MKS pressure transduce r readout (typical) monitor back pressure in. W. C. 20 Magnehelic reading:back pressure on reactor = impinger liquid level + CGA back pressure

pressure Atm 1.0228 reactor pressure = room pressure + back pressure % oxygen (O2) % 21.06 Airgas Certificate of Analysis, Reference Number 32

- 112669912
- 1 % nitrogen (N2) % 78.94 = 100
- % oxygen [COA says N2 = balance] monitor flow rate scc/min 662 Brooks mass flow controller readout for Synthetic Air

flow rate std L/min 0.662 moles O2 mol/min 0.0059 Cal culated using Ideal Gas Law [n = PV/RT] with Universal Gas Constant (R) of 0.08206 L

- atm/( mol
- K) moles N2 mol/min 0.0221 Calculated using Ideal Gas Law [n = PV/RT] with Universal Gas Constant (R) of 0.08206 L

- atm/( mol
- K) **Product moles** moles CH3OH m ol/min 0.0000 Assuming complete oxidation: all CH3OH converts to CO2 and H20 mole CO2 mol/min 0.0015 Assuming complete oxidation: moles CO2 out = moles CH3OH in moles H2O mol/min 0.0031 Assuming complete oxidation: moles H2O out = 2 * moles CH3OH in moles O2 mol/min 0.0036 Assuming complete oxidation: moles O2 out = moles O2 in

- moles O2 consumed moles N2 mol/min 0.0221 Assuming N2 is unreacted: Moles N2 in = Moles N2 out

total mol/min 0.0304 **Product volumes** CO2 std L/min 0.0365 Calculated using Ideal Gas Law [V = nRT/P] & Universal Gas Constant (R) of 0.08206 L

- atm/(mol

- K) H2O std L/min 0.0730 Calculated using Ideal Gas Law [V = nRT/P] & Universal Gas Constant (R) of 0.08206 L

- atm/(mol

- K) O2 std L/min 0.0847 Calculated using Ideal Gas Law [V = nRT/P] & Universal Gas Constant (R) of 0.08206 L

- atm/(mol

- K) N2 std L/min 0.5226 Calculated using Ideal Gas Law [V = nRT/P] & Universal Gas Constant (R) of 0.08206 L

- atm/(mol

- K)

total std L/min 0.7168 Calculated using Ideal Gas Law [V = nRT/P] & Universal Gas Constant (R) of 0.08206 L

- atm/(mol

- K) total scc/min 716.7602

### Page 10 of 24

**Table A -**  **3.** Oxidation of Methanol: Stoichiometric Calculations with Refined Inputs (continued) **Product composition wet basis**  **dry basis**  (Note: Volume % = Mole %) CO2 vol % 5.09% 5.67% H2O vol % 10.19% O2 vol % 11.81% 13.15% N2 vol % 72.91% 81.18%

total vol % 100.00% 100.00% **Excess Air** Entering moles O2 mol/min 0.0059 Portion of monitored synthetic air flow input that is oxygen, on a molar basis Require d moles O2 mol/min 0.0023 Moles of O2 required for complete oxidation: 1.5 * moles CH3OH in Ex cess air % 154.6%

a E.W . Lemmon, M.O. McLinden and D.G. Friend, "Thermophysical Properties of Fluid Systems" in **NIST Chemistry WebBook,**  NIST Standard R eference Database Number 69, Eds. P.J. Linstrom and W .G. Mallard, June 2005, National Institute of Standards and Technology, Gaithersburg, MD 20899 (http://webbook.nist.gov).

### Page 11 of 24

**Table A-4.** Combustion Stoichiometry Calculations for Combustion of FTBP Composite 1 **Units Value**  **Reference and/or Comment Reactant: FTBP Composite 1**  monitor sample mass μg 100 target value for measured polymer sample mass, as is basis analyzed solids content wt % 72.02% Akron Rubber Development Lab (ARDL) C & H Report, Table 5, average

sample mass μg, dry 72.02 target value for measured polymer sample mass, dry basis normalized C content wt %, dry 57.7% Table S-2 normalized H content wt %, dry 3.73% Table S-2 normalized F content wt %, dry 38.62% Table S-2 total wt %, dry 100.00% mass C in polymer μg, dry 41.52 = normalized dry wt % * sample mass (dry basis) mass H in polymer μg, dry 2.68 = normalized dry wt % * sample mass (dry basis) mass F in polymer μg, dry 27.81 = normalized dry wt % * sample mass (dry basis) moles C in polymer mol 3.46E-06 atomic weight = 12.011 g/mol, ref: Morrison & Boyd, Organic Chemistry , 3rd ed, 1973. moles H in polymer mol 2.66E-06 atomic weight = 1.0080 g/mol, ref: Morrison & Boyd, Organic Chemistry , 3rd ed, 1973 moles F in polymer mol 1.46E-06 atomic weight = 18.9984 g/mol, ref: Morrison & Boyd, Organic Chemistry , 3rd ed, 1973 **Reactant: Methanol** monitor liquid temperature o C 23.8 Feed pump isothermal T, measured with 1/16" calibrated thermocouple with chiller controlling to 24.0 C monitor liquid pressure psig 2500 Feed pump controller readout: pump discharge pressure (typical value)

liquid pressure psia 2514.7 liquid density g/mL 0.80296 NIST "Isothermal Properties for Methanol", http://webbook.nist.gov/chemistry/fluid/ a monitor injection rate μL/min 61.71 Feed pump controller readout

injection rate mL/min 0.06171 mass feed rate g/min 0.049551 = density (g/mL) * injection rate (mL/min) molecular weight g/mole 32.0419 NIST "Methyl Alcohol", http://webbook.nist.gov/cgi/cbook.cgi?Name=methanol&Units=SI molar feed rate mol/min 0.001546 moles = molecular weight / mass **Reactant: Sy nthetic air**  std temperature o C 21.1 Brooks gas mass flow controller calibration sheet monitor room pressure torr 740 MKS pressure transducer readout (typical value) monitor back pressure in. W .C. 20 Magnehelic reading: back pressure on reactor = impinger liquid level + CGA back pressure

reactor pressure atm 1.02283 33.91 ft W .C. = 1 atm; 760 torr = 1 atm; reactor pressure = room pressure + back pressure % oxygen (O2) % 21.06 Airgas Certificate of Analysis, Reference Number 32-112669912-1 % nitrogen (N2) % 78.94 Airgas Certificate of Analysis, Reference Number 32-112669912-1 monitor flow rate scc/min 662 Synthetic air flow rate monitored by Brooks gas mass flow controller

flow rate std L/min 0.662 moles O2 mol/min 0.005906 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mol-K) moles N2 mol/min 0.022137 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mol-K)

### Page 12 of 24

**Table A-4.** Combustion Stoichiometry Calculations for Combustion of FTBP Composite 1 (continued) monitor **Run Duration** min 16 Preset value for combustion test ex perimental run

**H consumption** convert F in polymer to HF mol/min 1.83E-07 1 mole H (i.e., 1/2 mole H2) per mole F to form HF, over run duration excess H from polymer mol/min 1.55E-07 (moles H in polymer - moles of H need to convert F to HF) over run duration; note excess H --> H2O moles H20 from xs polymer H mol/min 7.75E-08 2 moles H (i.e., 1 mole H2) per mole H20, over run duration **O2 consumption** convert C in polymer to CO2 mol/min 3.46E-06 1 mole O2 per mole C for C + O2 --> CO2, over run duration convert H in polymer to H2O mol/min 3.88E-08 for excess H from polymer to H2O; 0.5 mol O2 per mole of H2O formed, over run duration convert C & H in MeOH mol/min 0.0023 1.5 mole of O2 per mole of MeOH: CH 3 OH + 1.5 O 2 --> CO 2 + 2 H 2 O **Product moles** mo les CH3OH mol/min 0.0000 Assuming complete oxidation: all CH3OH converts to CO2 and H20 mo le CO2 mol/min 0.0015 Assuming complete oxidation: moles CO2 out = moles CH3OH in + moles C in (from polymer) mo les H2O mol/min 0.0031 Assuming complete oxidation: moles H2O out = 2 * moles CH3OH in + moles H20 in (from polymer) b mo les O2 mol/min 0.0036 Assuming complete oxidation: moles O2 out = moles O2 in - moles O2 consumed mo les N2 mol/min 0.0221 Assuming N2 is unreacted: Moles N2 in = Moles N2 out total mol/min 0.0304 **Product volumes** CO2 std L/min 0.0366 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mol-K) H2O std L/min 0.0730 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mol-K) O2 std L/min 0.0846 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mol-K) N2 std L/min 0.5226 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mol-K) total std L/min 0.7168 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mol-K) total scc/min 716.7612 **Product composition wet basis**  **dry basis**  (Note: Volume % = Mole %) CO2 vol % 5.10% 5.68% H2O vol % 10.19% O2 vol % 11.80% 13.14% N2 vol % 72.91% 81.18% total vol % 100.00% 100.00% a E.W . Lemmon, M.O. McLinden and D.G. Friend, "Thermophysical Properties of Fluid Systems" in **NIST Chemistry WebBook,**  NIST Standard Reference Database Number 69, Eds. P.J. Linstrom and W .G. Mallard, June 2005, National Institute of Standards and Technology, Gaithersburg MD 20899 (http://webbook.nist.gov). b Consistent with the requirement in Section C.2.2 of ECA Appendix C.2 to first convert weight % values from the labs to molar quantities on a dry basis, the very small amount of water evaporated from the starting polymer sample is not accounted for here.

### Page 13 of 24

**Table A-5.** Combustion Stoichiometry Calculations for Combustion of FTBP Composite 2 **Units Value**  **Reference and/or Comment Reactant: FTBP Composite 2**  monitor sample mass μg 100 target value for measured polymer sample mass, as is basis analyzed solids content wt % 75.70% Akron Rubber Development Lab (ARDL) C & H Report, Table 5, average

sample mass μg, dry 75.70 target value for measured polymer sample mass, dry basis normalized C content wt %, dry 62.80% Table S-2 normalized H content wt %, dry 5.09% Table S-2 normalized F content wt %, dry 32.10% Table S-2 total wt %, dry 100.00% mass C in polymer μg, dry 47.54 = normalized dry wt % * sample mass (dry basis) mass H in polymer μg, dry 3.86 = normalized dry wt % * sample mass (dry basis) mass F in polymer μg, dry 24.30 = normalized dry wt % * sample mass (dry basis) moles C in polymer mol 3.96E-06 atomic weight = 12.011 g/mol, ref: Morrison & Boyd, Organic Chemistry , 3rd ed, 1973. moles H in polymer mol 3.83E-06 atomic weight = 1.0080 g/mol, ref: Morrison & Boyd, Organic Chemistry , 3rd ed, 1973 moles F in polymer mol 1.28E-06 atomic weight = 18.9984 g/mol, ref: Morrison & Boyd, Organic Chemistry , 3rd ed, 1973 **Reactant: Methanol** monitor liquid temperature o C 23.8 Feed pump isothermal T, measured with 1/16" calibrated thermocouple with chiller controlling to 24.0 C monitor liquid pressure psig 2500 Feed pump controller readout: pump discharge pressure (typical value)

liquid pressure psia 2514.7 liquid density g/mL 0.80296 NIST "Isothermal Properties for Methanol", http://webbook.nist.gov/chemistry/fluid/ a monitor injection rate μL/min 61.71 Feed pump controller readout

injection rate mL/min 0.06171 mass feed rate g/min 0.049551 = density (g/mL) * injection rate (mL/min) molecular weight g/mole 32.0419 NIST "Methyl Alcohol", http://webbook.nist.gov/cgi/cbook.cgi?Name=methanol&Units=SI molar feed rate mol/min 0.001546 moles = molecular weight / mass **Reactant: Sy nthetic air**  std temperature o C 21.1 Brooks gas mass flow controller calibration sheet monitor room pressure torr 740 MKS pressure transducer readout (typical value) monitor back pressure in. W .C. 20 Magnehelic reading: back pressure on reactor = impinger liquid level + CGA back pressure

reactor pressure atm 1.02283 33.91 ft W .C. = 1 atm; 760 torr = 1 atm; reactor pressure = room pressure + back pressure % ox ygen (O2) % 21.06 Airgas Certificate of Analysis, Reference Number 32-112669912-1 % nitrogen (N2) % 78.94 Airgas Certificate of Analysis, Reference Number 32-112669912-1 monitor flow rate scc/min 662 Synthetic air flow rate monitored by Brooks gas mass flow controller

flow rate std L/min 0.662 moles O2 mol/min 0.005906 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mole-K) moles N2 mol/min 0.022137 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mole-K)

### Page 14 of 24

**Table A-5.** Combustion Stoichiometry Calculations for Combustion of FTBP Composite 2 (continued) monitor **Run Duration** min 16 Preset value for combustion test run

**H consumption** convert F in polymer to HF mol/min 1.60E-07 1 mole H (i.e., 1/2 mole H2) per mole F to form HF, over run duration excess H from polymer mol/min 2.29E-07 (moles H in polymer - moles of H need to convert F to HF) over run duration; note excess H --> H2O moles H20 from xs polymer H mol/min 1.15E-07 2 moles H (i.e., 1 mole H2) per mole H20, over run duration **O2 consumption** convert C in polymer to CO2 mol/min 3.96E-06 1 mole O2 per mole C for C + O2 --> CO2, over run duration convert H in polymer to H2O mol/min 5.73E-08 for excess H from polymer to H2O; 0.5 mol O2 per mole of H2O formed, over run duration convert C & H in MeOH mol/min 0.0023 1.5 mole of O2 per mole of MeOH: CH 3 OH + 1.5 O 2 --> CO 2 + 2 H 2 O **Product moles** moles CH3OH mol/min 0.0000 Assuming complete oxidation: all CH3OH converts to CO2 and H20 mole CO2 mol/min 0.0016 Assuming complete oxidation: moles CO2 out = moles CH3OH in + moles C in (from polymer) moles H2O mol/min 0.0031 Assuming complete oxidation: moles H2O out = 2 * moles CH3OH in + moles H20 in (from polymer) b moles O2 mol/min 0.0036 Assuming complete oxidation: moles O2 out = moles O2 in - moles O2 consumed moles N2 mol/min 0.0221 Assuming N2 is unreacted: Moles N2 in = Moles N2 out total mol/min 0.0304 **Product volumes** CO2 std L/min 0.0366 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mole-K) H2O std L/min 0.0730 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mole-K) O2 std L/min 0.0846 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mole-K) N2 std L/min 0.5226 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mole-K) total std L/min 0.7168 Calculated using Ideal Gas Law & Universal Gas Constant of 0.08206 L-atm/(mole-K) total scc/min 716.7616 **Product composition wet basis**  **dry basis**  (Note: Volume % = Mole %) CO2 vol % 5.11% 5.69% H2O vol % 10.19% O2 vol % 11.80% 13.14% N2 vol % 72.91% 81.18% total vol % 100.00% 100.00% a E.W. Lemmon, M.O. McLinden and D.G. Friend, "Thermophysical Properties of Fluid Systems" in **NIST Chemistry WebBook,**  NIST Standard Reference Database Number 69, Eds. P.J. Linstrom and W .G. Mallard, June 2005, National Institute of Standards and Technology, Gaithersburg MD 20899 (http://webbook.nist.gov). b Consistent with the requirement in Section C.2.2 of ECA Appendix C.2 to first convert weight % values from the labs to molar quantities on a dry basis, the very small amount of water evaporated from the starting polymer sample is not accounted for here.

### Page 15 of 24



### Table S **- 1**  . Summary of FTBP Composites Elemental Analysis

Sam ple % Solids % Wa ter Carbon (As Is) Hy drogen

(As Is) a 

### Carbon

(Dry Basis) Hy drogen

(Dry Basis) b 

### Fluorine

(Dry Basis) Reported Result Calcul ated Reported Result Reported

Result Normalized

Value Normalized

Value Normalized

Value % % % % % FTBP Composite 1 72.02 27.98 45.80 6.092 57.7 3.7 38.6 FTBP Composite 2 75.70 24.30 47.54 6.575 62.8 5.1 32.1

a 

### Reported value for Hydrogen (H) includes H present due to H 2 

### O in sample. b 

### Corrected to exclude H in H 2 

### O in sample.

### Page 16 of 24



### Table S **- 2** 
**.** PFOA Analysis Method Description Sample Matrix Impinger water (HPLC water with absorbed reactor exhaust gas) Method Su mmary 40 mL of aqueous sample (spiked with surrogate) concentrated via

C 18 

### SPE cartridge eluted with 5 mL of methanol then determined via electrospray liquid chromatography/tandem mass spectrometry (LC/MS/MS) using selected reaction monitoring (SRM) Sensi tivity Limit of Quantitation: 25 ng/L

Limit of Detection: 5 ng/L Calibration Calibration standards prepared in water with final concentrations of

0, 25, 50, 100, 250, 500, and 1000 ng/L. Linear regression calibration curve (using 1/x weighting) with co rrelation coefficient (R) ≥ 0.992 (R 2 

### ≥ 0.985) for initial calibration. QC Criteria Laboratory Control Standard (LCS) recovery: 70

– 130%

Extracted check standard recovery: 85

– 115% Surrogate spike recovery: 70

– 130% Surrogate Phase I transport test : 1 3 

### C

- PFOA : mass - labeled perfluoro

- n - octanoic

acid (m+2) provided by DuPont (custom synthesized by PerkinElmer), i.e., perfluoro

- n - [1,2
- 13 

### C 2 

### ]
- octanoic acid or 1,2
- 13 

### C 2 

### - PFOA Phase II combustion test : 13 

### C

- PFOA: mass

- labeled perfluoro

- n octanoic acid (m+4) purc hased from We llington Laboratories, i.e., perfluoro

- n - [1,2,3,4
- 13 

### C 4 

### ]
- octanoic acid or 1,2,3,4
- 13 

### C 4 

### - PFOA Chromatography Instrument Micromass Quattro Ultima

HPLC Column Genesis C

- 8, 5 cm x 2.1 mm i.d. x 4 μm Mobile Phase A 2 mM ammonium acetate in wat er Mobile Phase B methanol Ions Monitored: Analyte Transition Retention Time

PFOA 41 3  369 ~5 min 1,2
- 13 

### C 2 

### - PFOA 

### 415  370 ~5 min 1,2,3,4
- 13 

### C 4 

### - PFOA 

### 417  372 ~5 min Linear PFOA and branched PFOA are not chromatographically resolved by th is m ethod and thereby cannot be distinguished

. Laboratory MPI Research Inc., State College, PA

### Page 17 of 24



### Table S **- 3**  . FTBP Combustion Test Results for Impinger Samples

Test Substance Sam ple Identification Fluoride (m g/L) PFOA

(ng/L) None Pre
- Test Thermal Blank <0.05 Not analyzed



### Pre
- Test Steam Clean 0.82 Not analyzed 

### Composite 1 Pre
- Run Thermal Blank #1 0.20 ND

Experimental Run #1 0.58 ND Steam Clean #1 0.59 ND Post
- Run Thermal Blank #1 0.19 ND Pre
- Run Thermal Blank #2 <0.05 ND Experimental Ru n # 0.48 ND Steam Clean #2 0.72 ND Post
- Run Thermal Blank #2 <0.05 ND Pre
- Run Thermal Blank #3 <0.05 ND Experimental Run #3 0.28 ND Steam Clean #3 0.78 ND Post
- Run Thermal Blank #3 <0.05 ND HPLC W ater Blank <0.05 ND Composite 2 Pre
- Run Thermal Blank #4 0.16 ND

Experimental Run #4 0.45 ND Steam Clean #4 1.56 ND Post
- Run Thermal Blank #4 0.11 ND Pre
- Run Thermal Blank #5 0.10 ND Experimental Run #5 0.47 ND Steam Clean #5 1.30 ND Post
- Run Thermal Blank #5 0.12 ND Pre
- Run Ther ma l Blank #6 0.12 ND Experimental Run #6 0.29 ND Steam Clean #6 0.98 ND Post
- Run Thermal Blank #6 0.11 ND HPLC W ater Blank 0.05 ND

ND

– Compound not detected. Limit of Detection (LOD) for this matrix is 5 ng/L. As the pre
- test thermal bl ank and pre
- test steam cleaning show, the source of fluoride for the post

- run steam cleaning runs was determined to be thermal degradation of the perfluoroelastomer O

- ring on the exit end of the reactor.

### Page 18 of 24



### Tabl **e S-**  **4. F**  **lu or**  **id e**  **Io n**  **Recover y,**  **E xhaust** 

**Ga s**  **Hy dr**  **ogen Fl**  **uor id**  **e (H**  **F) C**  **oncent ratio**  **n, a**  **nd Fl**  **uor id**  **e Yie**  **ld**ExperimentalRunMeasuredFluorideionconcentrationMassofpolymerFluorineinpolymerWatervolumePredictedFluorideionconcentrationFluorideionRecoveryObservedHFconcentration Run Av g O 2 co ncObservedHFconcentrationat7%O2PredictedHFconcentrationat7%O2ObservedFluorideionYieldObservedHFYield
(m g/ L) (μg) (% ) (m L) (mg/ L) (% ) (mg/ ds cm) (% ) (mg/ ds cm ) (m g/ ds cm) (g F/ k g Po ly me r) (g H F/ kg

Po ly me r) 1 0. 58 102 38. 6 60. 28 0. 65 89 3. 6 13. 32 6. 6 7. 4 343 361 2 0. 48 104 38. 6 60. 51 0. 66 72 3. 0 13. 29 5. 5 7. 5 279 294 3 0. 28 103 38. 6 60. 43 0. 66 43 1. 8 13. 25 3. 2 7. 4 164 173 4 0. 45 108 32. 1 60. 81 0. 57 79 2. 9 13. 20 5. 1 6. 4 253 267 5 0. 47 108 32. 1 60. 69 0. 57 82 3. 0 13. 22 5. 3 6. 4 264 278 6 0. 29 91 32. 1 60. 20 0. 49 60 1. 8 13. 23 3. 3 5. 4 192 202 Meas ured Flu ori de io n co nc ent rat ion from MPI R eport . L ab not es "Q C meas urement s d id n ot me et th e cr it eria sp ec if ie d in th e me th od or QAPP. T he dat a sh oul d be co ns id ered es tima te d va lu es ." Mas s o f poly me r is Sa mple Net We ight

. Conc ent rat ion of Flu ori ne in p oly mer is n orm aliz ed fl uorine co nc ent rat ion on dry b as is. Wa te r vo lume is to ta l wat er vo lu me i n imp in gers f or run, a ssu ming w at er dens ity = 1 g /mL

. Predic te d Flu oride io n co nc ent rat io n = [( ma ss o f pol yme r) * ( % Flu ori ne in p oly mer )/ 100] / ( wat er vo lume) Fluor id e ion Re co ve ry ( %) = ( meas ured Flu or id e ion co nc ent rat ion) / ( predic te d Flu oride ion co nc ent ra tio n) * 100 Obs er ve d HF co nc ent rat io n = ( me as ured F ion co nc ) * (wat er v olum e) / 1 000 * [( Mo lec ular Wt o f HF)/ (A to mic Wt o f F)] / ( dr y g as v olume) Molec ul ar weight o f HF = ( at om ic w eight o f H) + ( at om ic w eight o f F) Ato mic w ei ght o f H = 1. 008 g/ mole Ato mic w ei ght o f F = 18. 998 g/ mole Dry g as v

ol um e is v

olum et ric f

lo w rat e on dry b as is * d urat io n of p yr oprobe heat ing (16 min ) Vo lu me tr ic f

low rat e = 6. 32E -04 ds cm/m in ( fro m sto ic hiom et ri c ca lc ulat ions ) Run Av g O 2 co nc is r un av

erage ox yg en co nc ent rat ion fro m CG A f or run. Obs er ve d HF co nc ent rat io n at 7 % O 2 = ( obs erv ed HF co nc ent rat io n) * (2 1. 1% - 7 %) / ( 21. 1% - [( Run Av g O 2 co nc ) %]) Predic te d HF co nc ent rat io n at 7 % O 2 = ( predic te d HF co nc ent ra tio n) * (21. 1% - 7 %) / ( 21. 1% - [( Run Av g O 2 co nc ) %]) Predic te d HF co nc ent rat io n = ( predic te d F io n co nc ) * (wat er vo lume) / 1 000 * [( Mo lec ular Wt o f HF) / (Ato mic W t o f F)] / ( dry g as v ol um e) F io n Emissio n Fa cto r = ( me as ured F io n co nc )*(wat er v olum e)*1000/ (mas s o f poly me r) HF Emissio n Fa cto r = ( me as ured F io n co nc )*(wat er v olum e)*1000/ (mas s o f poly mer)*(M ol ec W t o f HF)/ (A to mic Wt o f F) Not es :

### Pag e 19 of 24



### Table S **- 5.**  PFOA Exhaust Gas Concentration Cal culations

Experimental Run Measured

PFOA concentration Equivalent

PFOA concentration, assuming ND = LOD Wa ter

volume Equivalent

PFOA exhaust gas concentration Run

Avg O 2 

### conc Equivalent

PFOA exhaust gas concentration at 7% O 2 

### ( ng/L) (ng/L) (m L) (ng/dscm) (%) (ng/dscm) 1 ND 5 60.28 30 13.32 54 2 ND 5 60.51 30 13.29 54 3 ND 5 60.43 30 13.25 54 4 ND 5 60.81 30 13.20 54 5 ND 5 60.69 30 13.22 54 6 ND 5 60.20 30 13.23 53

Notes: Wa ter volum e is t otal water volume in impingers for run, assuming water density = 1 g/mL. Dry gas volume is volumetric flow rate on dry basis * duration of py roprobe heating (16 min) Volumetric flow rate (dry) = 6.3184E
- 04 dscm/min (from stoichiometric calculations) Run Avg O 2 

### conc is run average ox ygen concentration from CGA for run. Exhaust gas concentration at 7% O 2 

### = (exhaust gas concentration) * (21.1%

- 7%) / (21.1%

- [(Run Avg O 2 

### conc) %])

### Page 20 of 24



### Table S **- 6** 

. 13 

### C

- PFOA Surrogate Spike Recovery for Combustion Test Impinger Samples

Sam ple Identification 13 

### C

- PFOA Found (ng/L) Am ount 13 

### C

- PFOA

Added (ng/L) 13 

### C

- PFOA Recovery (%) Pre
- Run Thermal Blank #1 525 500 105 Experimental Run #1 529 500 106 Steam Clean #1 536 500 107 Post
- Run Thermal Blank #1 531 500 106 Pre
- Run Thermal Blank #2 537 500 107 Experimental Run # 527 500 105 Steam Clean #2 468 500 94 Post
- Run Thermal Blank #2 546 500 109 Pre
- Run Thermal Blank #3 536 500 107 Experimental Run #3 527 500 105 Steam Clean #3 524 500 105 Post
- Run Thermal Bl ank #3 556 500 111 HPLC W ater Blank 510 500 102 Pre
- Run Thermal Blank #4 495 500 99 Experimental Run #4 519 500 104 Steam Clean #4 492 500 98 Post
- Run Thermal Blank #4 549 500 110 Pre
- Run Thermal Blank #5 587 500 117 Experimental Run #5 531 500 106 Steam Clean #5 536 500 107 Post
- Run Thermal Blank #5 596 500 119 Pre
- Run Thermal Blank #6 526 500 105 Experimental Run #6 544 500 109 Steam Clean #6 474 500 95 Post
- Run Thermal Blank #6 507 500 101 HPLC W ater Blank 515 500 103

### Page 20 of 24



### Table S **- 7** 
**.** Typical W aste Incineration Exhaust Gas Oxygen Levels Exhaust O 2 

### Level (dry basis) Ty pe of Incinerator Reference 10% (nominal) Mass burn M WC a 

### Blount Energy Resource Corp. Correlation Procedure for Continuously Monitoring Furnace Temperatures (W arren County Resource Recovery Facility) , March 22, 1989. 10.8% (average) Mass burn M WC Clean Air Engineering. Test Report for Covanta of Fairfax, Inc. I

- 95 Energy/Resource Recovery Facility , 1997. 8.4% b 

### (average) Refuse Derived Fuel (RDF) M WC Finklestein, A. and R. D. Klicius. National Incinerator Testing and Evaluation Program: The Environmental Characterization of Refuse

- derived Fuel (RDF) Combustion Technology, Mid

- Connecticut Facility, Hartford, Connecticut , EPA
- 600/R

- 94
- 140 (NTIS PB96
- 153432), December 1 994. 10

– 13% Modular M WC Pace Analytical. Comprehensive Emissions Test Report: MSW Incinerator Unit No. 1 ESP Outlet & MSW Incinerator Unit No. 2 ESP Outlet (Polk County Solid Waste Plant), March 11
- 14, 2003. 13.5% Medical waste incinerator EPA. Medi cal Waste Incineration Emission Test Report: Weeks Memorial Hospital, Lancaster, New Hampshire , EMC Report 96

- MW I
- 11, March 1996. a 

### MW C = municipal waste combustor b 

### Calculated from spray dryer inlet O 2 

### concentrations (basis not specified) across 8 runs o ver range of steam loads during performance test runs indicative of “good combustor operation”.

### Page 2 1 of 24



### Figure S **- 1.**  Typical Structure of a Fluorotelomer

- Based Polymer in this Study



# Hy **drocarbon Side Chain** 

**Crosslinker Monomer**  

# X FC

**R** FC F C

**Fluorotelomer Side Chain** 

**Hy drocarbon**  **Pol ymer**  **Backbone**

### Page 22 of 24



### Figure S **- 2.**  Thermogravimetric Analysis of FTBP Composites at 25 o 

### C/min

### Page 23 of 24



### Figure S **- 3**  . Reactor Temperature Profile for Combustion Testing

100 200 300 400 500 600 700 800 900 1000 1100

0 10 20 30 40 50 60 70 80 90 100 

### Di **st ance**  **fro m F**  **ur nace**  **In le**  **t (c m)** **T e** **m p** **e r** **a t** **u r** **e (** **o C** **)**



### (Target Temperature = 1000°C)

Wi th 600 standard cc/min of synthetic air (21.1% oxygen, balance nitrogen; Airgas) flowing through the reactor, t he reactor temper ature profile was performed by sequentially measuring the reactor internal gas temperature every 2.54 cm along the length of the quartz tube. This profiling was conducted in air (without methanol fuel present) prior to combustion testing due to safety rea sons. The effective reactor length (indicative of gas residence time) at 1000 o 

### C was 66 cm of the 76 cm long section of the quartz tube radiantly heated by the split tube furnace. Supplemental calculations after the completion of the testing program indic ate that oxidation of the methanol fuel feed to the reactor could have resulted in temperature overshoot as high as 1283 o 

### C (adiabatic reaction temperature) at the inlet end of the reactor followed by approximately 0.15 second cool down. Such overshoot wou ld result in the mean gas temperature of the reactor increasing from 1000 o 

### C to 1003 o 

### C during combustion testing.