1 

### Response to EPA Review of Fluorotel omers Amended Final Study Report

The text below responds to each of the questi ons raised in the Review of Fluorotelomer Incineration ECA Final Report sent by e -mail on November 17, 2010 from Maj’d ElZoobi to Philip Taylor. Both Phase I and Phase II testing described in the Amended Final Study Report were performed in a ccordance with the r equirements of theEnforceable Consent Agreement (ECA) and TSCA GLPs as embodied in the EPAapproved Quality Assurance Proj ect Plans (QAPPs). Some of the questions seem to go beyond these requirements. It is important to note that the project team established and executed a quality management system to assure conformance with the EPA-approved

QAPPs and documented such conformance in the Final Study Report, as amended on
December 22, 2008.

I. Phase I PFOA Transport Testing

1. Reactor Temperature Profile

How have the authors assured that there is no significa nt difference between the temperature profile of the reactor during the calibration of the reactor heater, and the actual temperature profile occurri ng during the experimental runs?

As described in Section I.A.1 of the Final Study Report, the quartz reactor was housed

in a Thermcraft Model SST-3.00-0-30-3C-D 2155-BE three-zone tem perature controlled split tube furnace. Therefore, based on th e design of this furnace, the temperature of the quartz reactor tube was controlled by external radiant heating supplied by the split-tube furnace. The Reynolds num ber of the gas for the 250 o 

### C case (Phase I) was roughly 100. Under these conditions, heat transfer is dominated by radiation. The addition of water and slightly higher gas flow during tr ansport test runs compared to pre-Phase I temperature profiling does not materially ch ange the heat transfer coefficient which in both cases is dominated by the radiation cont ribution. Hence, the effect of water and higher gas flow during Phase I ex perimental runs is negligible.

II. Phase II Incineration Testing

1. Phase II Reactor Temperature Profile

a. The reactor was held at 1000°C for most of its length, but the heater temperature set-points were in the range of 979°C to 993°C. However, heat transfer from heater to quartz tube requires that the temperature of the earlier be higher than that of the later which is contrary to w hat is reported; is this explained by an erroneous heater temperature controller, such that the actual heater set-point is actually greater than 1000°C?

As described in Section I.A.1 and Section II.F .1 of the Final Study Report, the quartz

reactor was housed in a Thermcraft Model SST-3.00-0-30-3C-D2155-BE three-zone temperature controlled split tube furnace. By design, the furnace temperature controllers operate on feedback from the t hermocouples imbedded in the furnace and were not tied to the calibrated thermocouples used to monitor the surface temperature2 

### of the quartz reactor tube. The thermocouples integral to the furnace and used with the furnace temperature controlle rs do not appear to be calibra ted to the same degree as the Omega “special limits of error” thermo couples used to monito r the quartz reactor tube. Reactor midpoint quartz tube surface temperature T3 was calibrated prior to Phase II testing in accordance with Table B-2 of the EPA-approv ed Phase II QAPP.

b. Why does the reactor’s temperature dr op beginning at length 32 in.? Is that because the heater ends at this length and does not cover the entire reactor? Even if that were the case, it is surp rising that temperature would drop 600°C in the span of only 4 in. due to ambient cooli ng only (ie, without the use of a cooling device.)

The furnace is an SST-3.00-0-30 model, meaning that it is 3 feet long and has a 30 inch heated length. Therefore, the first 3 inches of the furnace and the la st 3 inches of the furnace are not radiantly heat ed. As radiation is the dominant heat transfer mechanism, when the gas stops being heated, the temperature quickl y drops on its own without external cooling.

Pursuant to ECA and QAPP requ irements, the outlet transfer line (on the discharge end of the furnace) was separat ely electrically heated to assure it stayed above 200 o 

### C to prevent potential condensation.

c. How have the report au thors determined whether the reaction heat effects will cause any significant difference between t he temperature profile of the reactor during the calibration of the reactor heat er, and the actual temperature profile occurring during the experimental runs to en sure that the correct effective length was determined and consequently that the desired residence time of 2 sec. was actually established?

In accordance with Table B-2 of the appr oved Phase II QAPP, the temperature calibration prior to Phase II experiments was performed to relate t he external surface temperature of the reactor t ube with internal gas temperatur e as the external surface temperature would be continuously monitoring during the experiments. As described in

Section II.F.1.a of the Final Study Report, the Phase II temper ature profile presented in Figure 3 of the Final Study Report was al so determined prior to actual combustion testing.

In response to this question, we have performed a supplemental in-depth engineering analysis to examine the potentia l effect of the heat of reac tion of methanol oxidation on gas residence time at temperature. This investigation of th e reaction heat effects indicates that the gas temperat ure could have overshot the 1000 o 

### C target temperature by up to 283 o 

### C (to 1283 o 

### C) and cooled to the target te mperature range within less than 0.2 seconds. Hence, these calcul ations confirm operation at 1000±10 o 

### C over a gas

residence time controlled within the range of 1.8 to 2.2 seco nds in conformance with the measurement performance criteria in Sect ion A7.1 of the EPA-approved Phase II QAPP. As the average gas temperature across the 1.98 sec residence time was3 

### 1000.5 o 

### C (see page 38 of Final Study Report), the average gas temperature across the total 2.13 (=1.98 + 0.15) seconds (includi ng the region associ ated with temperature overshoot and cool down) would be 1003.3 o 

### C.

The 1283 o 

### C value is the adiabatic reaction te mperature and thereby the theoretical maximum temperature attainable by the reac tion gas mixture due to the oxidation of

methanol as described in Table R-1.

Calculations to determine the duration of the cool down from this maximum temperature to the target temperature r ange are presented in Table R-2. First, the temperature range between 1283 o 

### C and 1020 o 

### C was divided into incremental segments, and the heat duty for each increment was determined (Q inc 

### = mCp Δ T). (With a wall temperature

of 1008 o 

### C [see Appendix 28 to Final Study Report], an end temperature of 1020 o 

### C was chosen because as the gas temperature appr oaches the wall temperature, the heat transfer asymptotically goes to zero.) Se cond, the heat transfer coefficient (h) and the radiant flux (Q rad 

### /A) for each increment were determined . Third, the surface area (A) for

each increment was determined via heat balance. Next, the incremental lengths were calculated for each cylindrical section, and cumulative length was determined. Similarly, the incremental volumes and re sidence times were computed to yield a cumulative gas residence time for cool down of 0.149 second.

The derivation of the thermal conductivity of the gas mixture using available information on component thermal conductivities is descr ibed in Tables R-3 and R-4. Table R-5

lists the references cited in th is supplemental engineering analysis.

Data on full-scale mass burn municipal waste combustors in Section D.4.2 of Appendix D.4 to the ECA showing time-average (over 2 seconds) temperatures of approximately

1230 o 

### C indicate that a potential s hort-duration peak value of 1283 o 

### C for the lab reactor system is consistent with oper ating data for full-scale com bustors. This comparison

confirms that Phase II test c onditions were representative of typical full-scale municipal waste combustor operations even when the theoretical maximum attainable temperature for the reacting gas is assumed.

2. Consideration of Formation of Other PFC a. According to Table 8, “Pyroprobe Ca rtridge and Sample Weight Measurement for FTBP Composites”, a residue was formed on the pyroprobe in two of the nine experimental runs. A 3 μ g and 4 μ g residue was formed in runs FTBP1-1 and FTBP2-3 respectively. Taking into account balance accuracy of ±2.5 μ g, the

amount of residue is 0.5 μ g and 1.5 μ g for runs FTBP1-1 and FTBP2-3 respectively. However, in the report (F . Combustion Testing / 2. Description of

Test Conditions / a. Test Substance Wei ght Measurements / P. 33) it is stated that the residue reported in Table 8 for these two runs is within the weighing accuracy of the microbalance. Please expl ain this taking into account the above.4 

### The value shown in Table 8 of the Final Study Report for residue was a calculated value. Table 8 of the Final Study Report has 9 such values, 5 of which are negative, 2 of which are zero, and 2 of which are positive. This suggests variability is important to understanding this calculated value.

As PDF page 194 (notebook page 99 of Appendix 4) of the Appendices to the Final Study Report shows, the standard deviation of the reference weight measurements during this project was 2.5 μg. As the second paragraph of Se ction II.F.2.a. of the Final Study Report attempts to explain, if each of the two measurements used to compute the calculated sample residue value in Table 8 wa s accurate to ±2.5 μg, then the resulting residue value would be ±5 μg (=±2.5 μg + ±2 .5 μg). Hence, any calculated residue value less than 5 μg would not have been di stinguishable from measurement error

associated with the use of the microbalance. Hence, Section II.F.2.a. of the Final Study Report stated, “The apparent residue remain ing for weighings denoted FTBP 1-1 and

FTBP 2-3 is an artifact of the sampling weighing process.”

Upon further review, we now see that the measurement error associated with this set of weight measurements was act ually ±7 μg rather than ±5 μg and that our original description of the measurement error asso ciated with the residue calculation was not
robust. From statistics, we know that t he 95% confidence interval for each weight

measurement on this balance during this project was 2 σ = 2 * 2.5 = 5 μg. Hence, each weighing on this balance was actually ±5 μg. Since residue is calculated from two weighings, each of which is ±5 μg, it is neces sary to consider the variance associated with each weighing to determine the expected error in the residue calculation. Residue is effectively calculated as a sum. The vari ance of a sum is the su m of the variances. With a standard deviation of 2.5, the vari ance for the calculated residue value is calculated as (2.5 2 

### + 2.5 2 

### = 6.25 + 6.25) = 12.5. Standar d deviation is the square root of variance. With a variance of 12.5, the standard deviation for the calculated residue value is the square root of 12.5 = 3.5. Hence, the standard deviation associated with the residue calculation is ±3.5 μg. Ther efore the 95% confidence interval for the

calculated residue values is ±7 μg (=2 * 3.5 μg). None of calculated residue values in Table 8 of the Final Study Report are outsi de of ±7 μg. Consequently, no residue was actually observed in any of the ex perimental run pyroprobe cartridges.

b. Another consideration in regard to the possibility that other PFC were formed is

whether a fluorine mass balance closes. Do you have any data on a fluorine

balance?

For the paper we are preparing for submission to a peer-reviewed journal, we have

calculated fluoride recoveries and found that for 2 out of 3 runs for each composite the

fluoride balance closes within 70 to 130%. For example, the calculated fluoride ion recovery for run 1 was 89%. As the journal article will demonstrate, the calculated HF emission concentrations are comparable to municipal waste combustor HF exhaust concentrations prior to air pollution cont rol equipment. Detailed examination of the fluoride analytical data during manuscript prepar ation reveals that there was a low bias in the fluoride ion chromatography results in part due to a negative y-intercept in the5 

### instrument calibration curve used by the laboratory, perhaps due to contamination of

their calibration standards.

Based on our telephone discussion in Dece mber, we have also computed mass of fluoride ion per mass of polymer for each ru n and mass of HF per mass of polymer for

inclusion in the attached table. See the t able titled “Fluoride Ion Recovery, Exhaust Gas Hydrogen Fluoride (HF) Concentration, and Fl uoride Yield”. We plan to provide EPA with a preprint of the j ournal article once it is accepted for publication.Table R-1. Adiabatic Reaction Temperature for Oxidation of MethanolReaction: CH3OH + 1.5 O2 --> CO2 + 2 H2O (g)AB C DHfo298(cal/gmol)Cp/R = A + BT + CT2+ DT-2CH3OH (g)2.211 1.222E-02 -3.450E-060 -48,050 Heat capacity (Cp) constants: Smith & Van Ness 4th ed, Table 4.1O23.639 5.060E-040 -2.270E+04 0Standard Heats of Formation (Hfo298): Smith &Van Ness 3rd ed, Table 4-4N23.280 5.930E-040 4.000E+03 0CO25.457 1.045E-030 -1.157E+05 -94,051H2O (g)3.470 1.450E-030 1.210E+04 -57,798UnitsValueBasisgmol CH3OH1ΔHo298cal -161,597ΔHo298J -676,122RJ/gmol-K 8.314Reference T (Tr)C 25Reference T (Tr)K 298.15Inlet Temp (Ti)C300Inlet Temp (Ti)K 573.15Reactant Mean T (TmR)K 435.65Excess (xs) air % 154.6%Molar quantitiesstoichiometricactualReactant CH3OHgmol 11Reactant O2gmol1.5 3.819Reactant N2gmol 5.643 14.367Product CO2 gmol11Product H2O gmol22Product O2gmol0 2.319Product N2gmol 5.643 14.367CpmeanR,CH3OHJ/gmol-K 57.00CpmeanR,O2J/gmol-K 30.98CpmeanR,N2J/gmol-K 29.61-ΔHoRJ 165,209Final T (Tf)C1283Final T (Tf)K 1556.50PredictedΔHoPJ 841,331Prod Mean T (TmP)K 927.32CpmeanP,CO2J/gmol-K 51.35CpmeanP,H2OJ/gmol-K 40.25CpmeanP,O2J/gmol-K 33.75CpmeanP,N2J/gmol-K 31.91CalculatedΔHoPJ 841,331Iterate until PredictedΔHoP= CalculatedΔHoPΔHoP= (Tf- 298.15)∑products(nCpmeanP)CpmeanP= R [(A + BTmP+ C/3 (4T2mP- TrTf) + D/(TrTf)]ΔHoP= (-ΔHoR) -ΔHo298TmP= (Tr+ Tf)/2Actual moles Reactant O2 = (stoichiometric moles Reactant O2) * (100 + %xs air)/100CH3OH + 1.5 O2--> CO2+ 2 H2O (g)TmR= (Tr+ Ti)/2CpmeanR= R [(A + BTmR+ C/3 (4T2mR- TrTi) + D/(TrTi)]-ΔHoR= (Ti- 298.15)∑reactants(nCpmeanR) where Ti≥298.15Actual moles N2 = (stoichiometric moles N2) * (100 + %xs air)/100standard heat of reaction (calculated)4.184 J / calCommentUniversal Gas Constant; with this R, Cp is in J/gmol-Ktemperature at which CH3OH conc corresponds to lower flammability limit per Bodurtha, Eq. 2-8

### Table R-2. Cool Down from Adiabatic Reaction Temperature

g/min mol/min Vol % g/mol 

### Comment

CO 2 

### 0.068 0.002 5.10% 44.01 mol/min & Vol % from Table 4 of



### H 2 

### O 0.056 0.003 10.19% 18.02 Appendix 7 to Final Study Report



### O 2 

### 0.115 0.004 11.80% 32.00 g/min = mol/min * g/mol



### N 2 

### 0.620 0.022 72.91% 28.01



### total 0.859 0.030



### m mix g/min 0.859 mass flow rate



### MW mix g/mol 28.28 molecular weight of gas mixture



### m mix lb/hr 0.114



### L ft 3.000 reactor tube length (inside furnace)



### D mm 14 reactor tube internal diameter



### D cm 1.4



### D ft 0.046



### L

m ft 0.046 mean beam length = D for cylinder



### P atm 1.023 reactor P (Report, Appendix 7, Table 4)



### P

c atm 0.052 partial pressure of CO 2



### P

c 

### L ft-atm 0.002 P

c L = P

c * L

m



### P

w atm 0.104 partial pressure of H 2 O



### P

w 

### L ft-atm 0.005 P

w L = P

w * L

m



### σ Btu/hr-ft 2

-  ̊ R 4 1.74E-09 Stefan-Boltzmann constant



### T  ̊ C 1300 1283 1250 1200 1150 1100 1050 1020 assympote; stop calcs as T nears T wall 

### Cp CO2 

### /R 7.054 7.035 6.999 6.943 6.887 6.831 6.774 6.739 Cp/R = A + BT + CT 2 + DT -2



### Cp H2O 

### /R 5.756 5.731 5.684 5.612 5.540 5.467 5.395 5.352 where A, B, C, and D from Table R-1



### Cp O2 

### /R 4.424 4.415 4.398 4.372 4.346 4.320 4.294 4.278



### Cp N2 

### /R 4.214 4.204 4.185 4.155 4.126 4.096 4.067 4.049



### Cp mix 

### /R 4.541 4.529 4.506 4.472 4.437 4.402 4.367 4.346



### Cp mix Btu/lbmol-  ̊ F 9.019 8.995 8.950 8.881 8.812 8.743 8.673 8.632 R = 1.986 Btu/lbmole-  ̊ F



### Cp mix Btu/lb-  ̊ F 0.319 0.318 0.316 0.314 0.312 0.309 0.307 0.305 heat capacity of gas mixture



### Δ T  ̊ C 0 17 33 50 50 50 50 30 gas temp change in each segment



### Q inc Btu/hr 0.000 1.105 2.135 3.210 3.185 3.160 3.135 1.872 incremental heat duty = mCp Δ T



### k mix Btu/hr-ft-  ̊ F 0.060 0.059 0.058 0.057 0.055 0.053 0.052 0.051 thermal conductivity of gas mixture



### Gz dimensionless 1.811 1.822 1.846 1.884 1.925 1.969 2.016 2.049 Graetz number = mCpL/ k



### Nu dimensionless 4.017 4.021 4.029 4.041 4.054 4.067 4.082 4.092 HTRI: Nusselt number = C 1 + C 2 Gz 1⁄3



### h Btu/hr-ft 2 -F 5.249 5.206 5.123 4.996 4.867 4.737 4.606 4.522 h = k Nu/D



### T  ̊ F 2372 2341 2282 2192 2102 2012 1922 1868 T(  ̊ F) = T(  ̊ C)*1.8 + 32



### ε CO2 dimensionless 0.0065 0.0067 0.0070 0.0073 0.0080 0.0085 0.0087 0.0090 emissivity, Perry's 5th ed., Fig. 10-55



### ε H2O dimensionless 0.0028 0.0030 0.0031 0.0035 0.0038 0.0042 0.0048 0.0055 emissivity, Perry's 5th ed., Fig. 10-56

### Table R-2. Cool Down from Adiabatic Reaction Temperature (continued)

C

so dimensionless 0.007 0.007 0.007 0.007 0.007 0.007 0.007 0.007 spectral overlap, Perry's 5th ed., Fig. 10-58



### C

w dimensionless 1.1 1.1 1.1 1.1 1.1 1.1 1.1 1.1 P correction factor for H 2 O, Fig. 10-57



### ε gas dimensionless 0.010 0.011 0.011 0.012 0.013 0.014 0.015 0.016 

### ε gas 

### = ( 

### ε CO2 

### + 

### ε H2O )C

w (1-C

so )



### T  ̊ K 1573 1556 1523 1473 1423 1373 1323 1293 T = T (  ̊ C) + 273.15



### T g  ̊ R 2832 2801 2742 2652 2562 2472 2382 2328 T g = T gas (  ̊ R) = [T (  ̊ K) ]*1.8



### T wall  ̊ C 1008 1008 1008 1008 1008 1008 1008 1008 ref Final Study Report (p. 38)



### T wall  ̊ R 2306 2306 2306 2306 2306 2306 2306 2306



### ε CO2,Tw dimensionless 0.0070 0.0073 0.0075 0.0080 0.0085 0.0086 0.0087 0.0090 ref Perry's 5th ed, pp 10-56 - 10-59



### ε H2O,Tw dimensionless 0.0060 0.0058 0.0057 0.0055 0.0054 0.0053 0.0052 0.0050 ref Perry's 5th ed, pp 10-56 - 10-59



### α CO2 dimensionless 0.008 0.008 0.008 0.009 0.009 0.009 0.009 0.009 

### α CO2 

### = ε CO2,Tw 

### * (T gas /T wall ) 0.65



### α H2O dimensionless 0.007 0.007 0.007 0.006 0.006 0.006 0.006 0.006 

### α H2O 

### = ε H2O,Tw 

### * (T gas /T wall ) 0.45 * C

w



### α gas dimensionless 0.015 0.015 0.015 0.015 0.015 0.015 0.015 0.014 

### α gas 

### = ( α CO2 

### + α H2O 

### )(1-C

so 

### )

Q rad 

### /A Btu/hr-ft 2 353 351 309 245 195 151 97 87 Q rad /A =0.9 σ (T g 4 

### ε gas - T

w 4 α gas )



### A ft 2 0 3.8E-04 8.4E-04 1.6E-03 2.2E-03 3.4E-03 7.0E-03 1.0E-02 Q = hA(T g -T

w ) + (Q rad /A)A



### L inc ft 0 2.6E-03 5.8E-03 1.1E-02 1.5E-02 2.3E-02 4.9E-02 7.0E-02 incremental length = A/( π D)



### L inc cm 0.000 0.080 0.178 0.344 0.467 0.714 1.487 2.141 1 ft = 30.48 cm



### L cumul cm 5.411 cumulative length under curve = Σ L inc



### V inc cm 3 0.000 0.123 0.273 0.529 0.720 1.099 2.289 3.296 incremental volume = π (D 2 /4) * L inc

Vol Flo L/sec 0.065 0.065 0.063 0.061 0.059 0.057 0.055 0.054 vol flow rate = (mol flow rate)(RT/P)

Vol Flo cm 3 /sec 65.33 64.62 63.25 61.17 59.10 57.02 54.94 53.70 R = 0.08206 L-atm/(mole-  ̊ K)



### t inc sec 0.000 0.002 0.004 0.009 0.012 0.019 0.042 0.061 incremental res time = V inc /vol flowrate



### t cumul sec 0.000 0.002 0.006 0.015 0.027 0.046 0.088 0.149 cumulative res time = Σ t inc



### AUC sec-  ̊ C 0.00 0.03 0.14 0.43 0.61 0.96 2.08 1.84 area under cool-down curve



### T avg,UC  ̊ C 1040.9 T avg, under curve = Σ AUC / Σ t inc + 1000



### T avg,2s  ̊ C 1000.5 avg T over 2 sec res time per Report (p.38)



### T avg,tot  ̊ C 1003.3 T avg, tot =(t cumul *T avg,UC +2*1000)/(2+t cumul )

Note: using 1.98 sec for "2 sec" per Report (p.38)



### C 1 

### , C 2 

### = Heat Transfer Research Institute (HTRI) proprietary constantsTable R-3. Thermal Conductivity ( k ) of Nitrogen, Carbon Dioxide, Oxygen, Water, & Mixture

Nitrogen a Carbon

Dioxide b Oxygen b Water c Mixture d Mixture e

T T k k k k k k (C) (K) (W/m-K) (W/m-K) (W/m-K) (W/m-K) (W/m-K) (Btu/hr-ft-F)

1020 1293.15 0.08071 0.08256 0.09007 0.13830 0.08786 0.05076

1050 1323.15 0.08214 0.08379 0.09171 0.14373 0.08970 0.05183

1100 1373.15 0.08451 0.08576 0.09442 0.15123 0.09259 0.05350

1150 1423.15 0.08684 0.08761 0.09711 0.15879 0.09545 0.05515

1200 1473.15 0.08914 0.08936 0.09977 0.16640 0.09828 0.05679

1250 1523.15 0.09141 0.09100 0.10241 0.17405 0.10109 0.05841

1283 1556.15 0.09289 0.09204 0.10414 0.17910 0.10292 0.05947

1300 1573.15 0.09365 0.09255 0.10502 0.18174 0.10386 0.06001

a Ref.: NIST Webbook at P = 1 bar* [Lemmon et al, 2011]

b Ref.: DIADEM Professional (The DIPPR Information and Data Evaluation Manager for

the Design Institute for Physical Properties, Version 5.0) at P = 1 bar* [Rowley et al,
2010]

c Ref: NIST REFPROP Version 8.1 Beta at P = 1 bar* [Kestin et al, 1984 in Lemmon et

al, 2010]

d Calculated using Mason and Saxena modification to the Wasiljewa equation [Reid et

al, 1977, pp. 508-509]; see examples in Table R-4

e Conversion factor for W/m-K to Btu/hr-ft-F is 0.57779

* The effect of pressure on thermal conductivity of gas in the range of 1 bar to 1.023 atm

is negligible because thermal conductivity of a gas changes about 1% per atmosphere
in the region below 10 atm. [Reid et al, 1977, pp. 499-500]Table R-4. Sample Calculations: Computing Thermal Conductivity of Actual Mixture at Two TemperaturesT (K)No.SpeciesMolefraction[y]MolecularWeight[M]k(W/m-K)T (K)No.SpeciesMolefraction[y]MolecularWeight[M]k(W/m-K)1556.151N20.729128.01340.092891573.151N20.729128.01340.093651556.152CO20.050944.00950.092041573.152CO20.050944.00950.092551556.153O20.118131.99880.104141573.153O20.118131.99880.105021556.154H200.101918.01530.179101573.154H200.101918.01530.181741556.15mixture0.102921573.15mixture0.10386ijMi/Mjki/kjAijMolefractionj∑yj*AijijMi/Mjki/kjAijMolefractionj∑yj*Aij111.000001.000001.000000.72910.981122111.000001.000001.000000.72910.98096820.636531.009280.897900.050920.636531.011850.898410.050930.875450.892010.941200.118130.875450.891700.941120.118141.554980.518650.933900.101941.554980.515300.932230.1019211.571020.990811.120250.72911.096849211.571020.988291.119450.72911.09588821.000001.000001.000000.050921.000001.000001.000000.050931.375350.883801.049090.118131.375350.881261.048270.118142.442900.513891.033190.101942.442900.509261.030370.1019311.142271.121071.065080.72911.044369311.142271.121451.065180.72911.04429320.727091.131470.951540.050920.727091.134740.952180.050931.000001.000001.000000.118131.000001.000001.000000.118141.776200.581450.993980.101941.776200.577880.992250.1019410.643101.928071.039920.72911.02255410.643101.940631.041440.72911.02389620.409351.945960.922140.050920.409351.963620.923780.050930.563001.719850.978090.118130.563001.730460.979390.118141.000001.000001.000000.101941.000001.000001.000000.1019Table R-5. References

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Environmental Standards, Inc., 2006. Quality Assur ance Project Plan for the ECA Incineration Testing Program – Phase II Fluorotelomer Incineration Testing.

EPA, 2005. Enforceable Consent Agreement for Fluo rotelomer-based Polymers Chemicals (EPA docket No. OPPT-2004-0001).

Kestin, J., Sengers, J. V., Kamgar-Parsi, B. and Levelt Sengers, J. M. H., 1984. Thermophysical Properties of Fluid H 2 O. J. Phys. Chem. Ref. Data. 13(1), 175-183.

Knudsen, J. G., Bell, K. J., Holt, A. D., Hottel, S. M., Sarofim, A. F., Standiford, M. S., Stuhlborg, D., and Uhl, V. W., 1973. Heat Transmission, in: Perry, R. H. and Chilton, C. H. (Eds.), Chemical Engineers’
Handbook, 5 th edition. McGraw-Hill, New York, Section 10.

Lemmon, E. W., Huber, M. L., McLinden, M. O ., 2010. NIST Standard Reference Database 23: Reference Fluid Thermodynamic and Transport Propertie s-REFPROP, Version 9.0, National Institute of Standards and Technology, Standard Refe rence Data Program, Gaithersburg.

Lemmon, E.W., McLinden, M. O. and Friend, D. G, 2 011. Thermophysical Properties of Fluid Systems in: Linstrom, P. J. and Mallard, W. G. (Eds.), NIST C hemistry WebBook, NIST Standard Reference Database Number 69, http://webbook.nist.gov.

Reid, R. C., Prausnitz, J. M., and Sherwood, T. K ., 1977. The Properties of Gases and Liquids, 3 rd

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Taylor, P. H., 2008. ECA Incineration Testing Program: Laboratory-Scale Incineration Testing of Fluorotelomer-based Polymers Amended Final Study Report.Fluoride Ion Recovery, Exhaust Gas Hydrogen Fluoride (HF) Concentration, and Fluoride Yield

Experimental Run Measured Fluoride ion concentration Mass of polymer Fluorine in polymer Water volume Predicted Fluoride ion concentration Fluoride ion Recovery Observed HF concentrationRunAvgO2conc Observed HF concentration at 7% O 2 Predicted HF concentration at 7% O 2 Observed Fluoride ion Yield Observed HF Yield(mg/L) (μg) (%) (mL) (mg/L) (%) (mg/dscm) (%) (mg/dscm) (mg/dscm)(g F/ kgPolymer)(g HF/ kgPolymer)10.58 102 38.6 60.28 0.65 89 3.6 13.32 6.67.4 343 36120.48 104 38.6 60.51 0.66 72 3.0 13.29 5.57.5 279 29430.28 103 38.6 60.43 0.66 43 1.8 13.25 3.27.4 164 17340.45 108 32.1 60.81 0.57 79 2.9 13.20 5.16.4 253 26750.47 108 32.1 60.69 0.57 82 3.0 13.22 5.36.4 264 27860.29 91 32.1 60.20 0.49 60 1.8 13.23 3.35.4 192 202Notes:Measured Fluoride ion concentration from MPI Report. Lab notes "QC measurements did not meet the criteria specified in the method orQAPP. The data should be considered estimated values."Mass of polymer is Sample Net Weight.Concentration of Fluorine in polymer is normalized fluorine concentration on dry basis.Water volume is total water volume in impingers for run, assuming water density = 1 g/mL.Predicted Fluoride ion concentration = [(mass of polymer) * (% Fluorine in polymer)/100] / (water volume)Fluoride ion Recovery (%) = (measured Fluoride ion concentration) / (predicted Fluoride ion concentration) * 100Observed HF concentration = (measured F ion conc) * (water volume) / 1000 * [(Molecular Wt of HF)/(Atomic Wt of F)] / (dry gas volume)Molecular weight of HF = (atomic weight of H) + (atomic weight of F)Atomic weight of H = 1.008 g/moleAtomic weight of F = 18.998 g/moleDry gas volume is volumetric flow rate on dry basis * duration of pyroprobe heating (16 min)Volumetric flow rate = 6.32E-04 dscm/min (from stoichiometric calculations)Run Avg O2conc is run average oxygen concentration from CGA for run.Observed HF concentration at 7% O2= (observed HF concentration) * (21.1% - 7%) / (21.1% - [(Run Avg O2conc) %])Predicted HF concentration at 7% O2 =(predicted HF concentration) * (21.1% - 7%) / (21.1% - [(Run Avg O2conc) %])Predicted HF concentration = (predicted F ion conc) * (water volume) / 1000 * [(Molecular Wt of HF) / (Atomic Wt of F)] / (dry gas volume)F ion Emission Factor = (measured F ion conc)*(water volume)*1000/(mass of polymer)HF Emission Factor = (measured F ion conc)*(water volume)*1000/(mass of polymer)*(Molec Wt of HF)/(Atomic Wt of F)