# Appendix C



# Draft Facility Report on Emissions

October 2010 Submission

APFN

NONCBI 

# Company Sanitized

## 2010/15 PFOA Stewardship Program



# Draft Facility Report on Emissions

I . CHEMICAL IDENTIFICATION Identify the chemical for which you are submitting information:

Chemical name: APFN CAS number : 77623-77-9

II . COMPANY IDENTIFICATION Identify the company and location of the facility submitting information:

Company name : SOLVAY SOLEXIS, INC. Site location : THOROFARE, NJ Identify a company technical contact who can respond to inquiries about the information submitted : Technical contact : VIRGINIA HUBERT

Phone: (713)525-6051 Address:_ 10 LEONARD LANE

THOROFARE, NJ

### III . ON-SITE ACTIVITIES Calendar year for which you are reporting: Jan 1, 2009 to Dec 31, 2009

Provide the amount of chemical identified above for the reporting year at specific site:

Imported (virgin) Imported (externally recycled) Manufactured

Estimate the amount of subject chemical distributed off-site: % of manufacture/import kgs/yrkgs/yr

- kgs/yr

Provide the amount used (including any that was manufactured, imported [virgin or externally recycled], or internally recycled) of the subject chemical for the reporting year at specific site :

Narrative Description and Process Flow Schematic: Provide overall material balance of the chemical being reported, showing releases and products (kgs/year) . Use the following page to provide a narrative description and process flow

schematic of on-site activities, and include information that gives an understanding of the nature and extent of potential exposures to the subject chemical . Attach additional pages if desired. The narrative and process flow schematic should cover major unit operations and chemical conversions for manufacturing and on-site uses, if applicable. The narrative should provide insight into why and how releases are caused by the process. The schematic should show the points of release of the subject chemical in the workplace and to the environment. In the event the subject chemical is used in many different processes, provide information on each major process instead of each individual process.

### Narrative Description and Process FlowSchematic:p. 6

### IV. SITE RELEASE ANDTRANSFER INFORMATION (For manufacturing and on-site processing/use if applicable) In this section, estimate the total media-specific releases after on-site treatment of the chemical from

your facility. You may estimate the releases by using monitoring data or any other method you believe appropriate. Estimates should be reported in kgs per year for the reporting period. Enter the values as whole numbers to no more than two significant figures. For example, if your annual releases are estimated to be 12,360 kgs, an estimate of 12,000 kgs should be reported . Estimate the number of days per year the release occurs. Enter a whole number with a maximum

of 2 significant figures. Insert "NA" for release activities not associated with the chemical or "0" for releases of less than 0

.5 kgs per year . For all releases, the source of data and/or basis for determination should be described in detail . Suggested information about the possible sources/basis includes : 1 . If the source/basis is an analytical measurement, then " Describe the method (including analytical standards used, sampling, sample treatment, analysis) . " Describe the uncertainties and assumptions made. " Give the Level of Detection (LOD)/Level of Quantification (LOQ) . 2. If the source/basis is a mass balance, then " Show

the mass balance calculation. " Show

that the mass balance closes . " If the mass balance does not close, then report the fraction of total feedstock that is not accounted for and the assumptions you made to correct the balance. Describe the uncertainties . 3. If the source/basis is other than measurement or mass balance, then " Describe the method used. For example, if engineering calculations are used, give a general description and state your assumptions. Describe the uncertainties.Part IV (cont .) 

### A . ON-SITE AIR RELEASES Estimate the total fugitive or non-point releases to air and the number of days per year the releases occur. These releases include equipment leaks from valves, pump seals, flanges, compressors, sampling connections, and open-ended lines; evaporative losses fromsurface impoundments and spills; releases frombuilding ventilation systems; and, any other fugitive or non-point air emission. In addition, estimate the total releases that occur through stacks, vents, pipes, or other confined air streams as stack or point source releases. Include storage tank emissions and releases frompollution control equipment . If desired, you can provide estimates of the accuracies of your release estimates.

Fugitive (non-point) Stack (point) Estimated Total Estimated % # Days/year Annual Releases Accuracy Release Occurs (kgs) (Optional)



### Basis for each release estimate : (See discussion on source/basis in beginning of Section IV.) 365

MASS BALANCE - CALCULATED BY DIFFERENCE content in the wash water and

in the solids were measured 0

Comments : (This section is available to clarify your responses. Attach additional pages if desired.)

### Part IV (cont .) B . WATER RELEASES FROM SITE N/A Estimate the total releases of the chemical leaving the fence line of your facility fromall discharge points to all streams or water bodies. Include all discharges from process outfalls such as pipes, open trenches, releases fromon-site wastewater treatment, and contribution fromstorm water runoff, if applicable. Do not include discharges to a POTW or other off-site wastewater treatment facilities. If desired, you can provide an estimate of the accuracy of your release estimate. Estimated Total Estimated % # Days/year Annual Releases Accuracy Release Occurs (kgs) (Optional) 

### Water releases : 365

Enter the names of the streams or water bodies to which the facility directly discharges the chemical . Also, enter the NPDES permit number for the facility. If more than one number is assigned to the facility, list each number for the appropriate discharge quantity and receiving water identified. Receiving Water Name(s) : NPDES number(s) :

Basis for each release estimate : (See discussion on source/basis in beginning of Section IV.)

Comments: (This section is available to clarify your responses. Attach additional pages if desired.)Part IV (cont .) 

### C . ON-SITE LAND RELEASES N/A Estimate the total releases of the chemical for each category of land disposal, if applicable. Estimate only on-site releases. Do not estimate leaks fromlandfills separately. This should be accounted for in your estimate of total landfill release. Releases to land treatment/land amendment include all waste containing the chemical that is applied or incorporated into soil on-site. Do not include waste that is landfilled. Surface impoundments are natural topographic depressions, man-made excavations, or diked areas formed primarily of earthen materials designed to hold an accumulation of the chemical . Underground injection is the technology of placing fluids underground, in porous formations of rocks, through wells or other similar conveyance systems. Other releases include any amount of the chemical that is released to land other than those listed. An example is the accidental release of the chemical froman underground pipeline or storage tank. Estimated Total Estimated % Annual Releases Accuracy (kgs) (Optional) 

### Landfill Land Treatment/Land Amendment Surface Impoundments Underground Injection Other (specify) : 

# C ~J



# r

Basis for each release estimate: (See discussion on source/basis in beginning of Section IV.)

### Comments: (This section is available to clarify your responses. Attach additional pages if desired.) Part IV (cont .) D . OFF-SITE TRANSFERS Estimates of off-site transfers should be similar in accuracy and precision to previous release estimates. Dl . Transfer to Publicly Owned Treatment Works (POTW) Number of days/year the release occurs: 365 Estimate the total quantity of the subject chemical , not the waste stream, transferred to the POTW . Complete section below for each POTW

to which your facility discharges wastewater containing the chemical . Enter the POTW's NPDES permit number, if known. Annual Transfer (kgs) : Estimated %

Accuracy of Transfer Estimate (optional) POTW Name: GLOUCESTER COUNTY UTILITY AUTHORITY Street Address: 2 PARADISE ROAD City: WEST DEPTFORD County: GLOUCESTER State: NJ Zip Code: 08066 NPDES number : NJ0024686 Basis for each release estimate: (See discussion on source/basis in beginning of Section IV.) The surfactant content in the wash water was measured per the attached method PF 89/110 WAS E - Perfluorooctanoate and Higher Homologues in Wastewater and Surface Water - Concentration on Porapack Qand Esterification Comments : This is the method that was used in 2009 to obtain the data for the mass

balance .

# ; ; AusimonT., :

APPROVED-COPY N° 

### AUSIMONT S.P.A

. Centro Ricerche e Sviluppo

Bollate Analytical Method PF 89/110 WAS E Perfluorooctanoate and higher homologues 

### in wastewater and surface water Concentration on Porapack Q 

### and esterification This document is composed by: N° pages: 6 N° tables: N° figures : N° attachments: Edition: 3 Date : June 2001 Laboratory: GC Author : Oriani I Verification: Morandi Approval : Pace 1 Scope and application 1 .1 This method is for the extraction of perfluorooctanoate (APFO) and related homologues fromwastewater and surface water. 1 .2 Applicable compounds are: perfluorooctanoate (APFO) [C7FjSCOO-], perfluorononanoate [C8Fi7C00], perfluorodecanoate [C9F,9C00-], perfluoroundecanoate [C,oFz]C00-], perfluorododecanoate [Cl,F23C00-] and higher homologues. 1 .3 Matrices: waste water and aqueous matrixes with APFO concentration lower than 5ppm

. 2 Summary 2 .1 Transfer about 70ml of acidic water in a 100ml dreschel bottle . Connect to gas dispersion side tube a cartridge packed with about 700mg of Porapack Q 60-80 PF 89/110 WAS E Page 1 of 6

# ; ; ausimonT, . mesh . Connect the second line of dreschel bottle to a Nitrogen supply and pressurise at about 20-50 kPa allowing a liquid flow rate through the cartridge of about 1 ml/min. Collect effluent water in a cylinder and stop flowafter collection of about 50m1 . Connect the cartridge directly to Nitrogen supply for 5 minutes to remove the most part of water. Elutes with 6ml of ethanol in a lOml vial . Add 0.4m1 NaOH 0.1% in ethanol and allow drying at room temperature under Nitrogen flow

. Add 2ml of methanol containing 1 % Sulphuric acid. Close carefully the vial with a PTFE capped septum, then allowPFOA esterification at 70°C over night . At room temperature add 0.5ml of CFC 113. Wash out acidic methanol with 6ml water . Remove water layer then wash again with 3m1 water . Allow phases separation at roomtemperature for 15 minutes. Inject 1 pl of lower liquid layer . Analyse using method PF 89/110 GC E . 3 Definitions 3.1 APFO

: perfluorooctanoate. 4 Safety precautions 4.1 When handling samples or solvents and hot vials wear appropriate protective gloves, eyewear, clothing and any other protective devices mandatory in your working area. 5 Interferences 5.1 To minimise interferences when analysing samples PTFE vials and tubing should not be used for sample storage or handling. 6 Equipment 

### 6.1 Balance (+/- 1 mg) 7 Supplies and materials 7.1 Gloves 7.2 Timer 7.3 Syringes glass 1 cc, 5 cc 7.4 Micro-syringes glass 10 V1, 250 pl 7.5 Pasteur pipette 8x6mmdiameter 7.6 Centrifuge tubes glass lOml 7.7 Vials 10m1 7.8 Glass bottles nominal 100m1 7.9 Volumetric flasks 100ml, 500ml volume 7.10 Athermic gloves 7.11 Dreschel bottle 100ml and 500m] PF 89/110 WAS E Page 2 of 6

# VpusimonT.~. 7.12 Glass graduated cylinder 100ml and 500ml 8 Reagents and standards 8.1 Concentrated sulphuric acid R.P.E . Carlo Erba or equivalent 8.2 Methanol R.S. Carlo Erba or equivalent 8.3 Ethanol anhydrous R.S. Carlo Erba or equivalent 8.4 Acetone R.S. Carlo Erba or equivalent 8.5 CHZC12 R.S . Carlo Erba or equivalent 8.6 CFC 113 Fluka for IR or equivalent 8.7 Ammonia 30%R.P .E. Carlo Erba or equivalent 8.8 NaOH R.P.E. Carlo Erba or equivalent 8.9 Nitrogen GCgrade 8.10 Porapack Q60-80 mesh 8.11 Reagent preparation 1% sulphuric acid in methanol : in a bottle of nominal 100ml (true volume 116ml) weigh 49.5g of methanol then add slowly 0.5 g concentrated sulphuric acid. 1%NaOH in ethanol : in a 500ml volumetric flask weigh 0.5g of NaOH then add 500ml ethanol . 8.12 Standard preparation SoI .A: weigh 100mg of solid ammonium salt of perfluoro-acid, dissolve in 100ml methanol in volumetric flask. 

### S200ppm : transfer 100[1 of SoI .A in a lOm] vial, add 1 .9ml of methanol 1% sulphuric acid and followthe esterification procedure. S100ppm

: transfer 50p1 of SoI .A in a 10ml vial, add 2ml of methanol 1% sulphuric acid and followthe esterification procedure . S50ppm : transfer 25p1 of Sol .A in a 10m1 vial, add 2ml of methanol 1% sulphuric acid and followthe esterification procedure. S20ppm : transfer 10~t1 of SoI .A in a l Oml vial, add 2ml of methanol 1 % sulphuric acid and followthe esterification procedure. S10ppm : transfer 5~t1 of SoI .A in a lOml vial, add 2ml of methanol 1%sulphuric acid and followthe esterification procedure. 8.13 Cartridge preparation Weigh about 700mg Porapack Q . Introduce a small plug of glass wool in a Pasteur pipette down to diameter restriction. Transfer to the pipette the Porapack Qthen insert a second small plug of glass wool to keep polymer bed in place . Wash with 15ml Acetone, 15ml Ethanol and 15ml CHZCI2. Keep cartridge under Ethanol until use. PF 89/110 WAS E Page 3 of 6

# VAusimonr,

Before use let ethanol flowing out then wash with lOml distilled water . Connect moist cartridge to the sampling line. 8.14 Sample preparation Transfer 70ml of water sample, measured in a graduated cylinder, into dreschel bottle. Add, slowly 0.3ml sulphuric acid. 8.15 Water spike preparation Sp500- In a volumetric flask measure 100ml drinking water . Add 50~t1 So1 .A, shake for few

minutes then follow8.14 Sample preparation . Sp250- In a volumetric flask measure 100ml drinking water . Add 25u1 Sol .A, shake for few

minutes then follow8.14 Sample preparation . Sp100- In a volumetric flask measure 100ml drinking water . Add 10u1 SoI .A, shake for few

minutes then follow8.14 Sample preparation . Sp50- In a volumetric flask measure 100ml drinking water . Add 5pl Sol .A, shake for few minutes then follow8.14 Sample preparation. 9 Quality control 9.1 Method and matrix blank Use drinking water and apply sample preparation, as in 8.14, recovery and esterification procedure. 9.2 Matrix spike Prepare spiked samples as in 8.15 and apply recovery and esterification procedure. 9.3 Continuing calibration check 9.3 .1 With each batch of samples prepare S20ppm calibration solution . 9.3.2 Analyse S20ppm sample first to assure the accuracy of initial calibration curve. 

### 9 .3.3 Analyse S20ppmsample per group of 10 samples. 9.3.4 Analyse S20ppmsample last to assure the accuracy ofdata. 10 Calibration and standardisation 10.1 APFOresponse line 10.1 .1 Prepare calibration standards PF 89/110 WAS E Page 4 of 6

# VAusimonT>.6

10.1 .2 Inject 1 ViI each at least in duplicate 10.1 .3 Calculate concentration of APFO in solution assuming that Sol .A contains l ~tg APFO/pl solution . Correct concentration only if weighed APFO differs from nominal 100mg more that + / - 10% (namely less than 90mg or more than 110mg) . 10.2 Calibration line 10.2.1 Prepare spiked samples as in 8.15 10.2 .2 Apply each the recovery procedure 10.2 .3 Inject 1 pl each at least in triplicate 10.2 .4 Calculate concentration of APFO in water fromAPFO concentration in spiked samples assuming that So1 .A contains 1 pg APFO/pl solution. Correct concentration only if weighed APFO differs fromnominal 100mg more that + / - 10%(namely less than 90mg or more than 1 I Omg) . 11 Procedures 11 .1 Prepare samples as in 8.14 or 8.15 for spiked samples and label flasks with sample ID

. 11 .2 Connect to gas dispersion side tube the cartridge prepared as in 8.13. 11 .3 Connect the second line of dreschel bottle to a Nitrogen supply and pressurise at about 20-50 kPa allowing a liquid flow rate through the cartridge of about 1 ml/min. 11 .4 Collect effluent water in a cylinder and stop flowafter collection of about 50ml . 11 .5 Connect the cartridge directly to Nitrogen supply for 5 minutes to remove the most part of water . 11 .6 Elutes with 6m1 of ethanol in a l Oml vial . Add 0.4ml NaOH 1 %in ethanol and allowdrying at roomtemperature under Nitrogen flow . 11 .7 Add 2ml of methanol containing 1 % Sulphuric acid . Close carefully the vial with a PTFE capped septum, then allowPFOA esterification at 70°C over night . 11 .8 At roomtemperature add 0.5ml of CFC 113. Wash out acidic methanol with 6m1 water . Remove water layer then wash again with 3ml water . 11 .9 Allowphases separation at roomtemperature for 15 minutes. 11 .10 At roomtemperature, inject 1 pl of lower liquid layer . Analyse using method PF 89/110 GC E. 12 Data analysis and calculations Calculate actual concentration of APFO, or other applicable compounds, from calibration line (10.2) using an external standard method . 13 Method performances

PF 89/110 WAS E Page 5 of 6

# VausimonT.I . Method detection limit is 50ppb APFO in water . Method quantitation limit is 100ppb in water . Precision and accuracy are calculated from data of calibration line ; precision is percent standard deviation at each point, accuracy is percent ratio of average calculated amount to nominal concentration at each point . Recovery at each point is percent ratio of average area of calibration line to average area of APFO response line calculated at same nominal concentration . 14 Pollution prevention and waste management Samples in CFC are disposed in dedicated container . Samples in water / methanol are disposed in dedicated container Solvents are disposed in dedicated container Disposable glass vials are disposed in broken glass containers located in laboratory. 15 Records None

PF 89/110 WAS E Page 6 of 6

### D2. Transfers to other off-site locations In this section, estimate the quantity of the subject chemical , not the waste stream, transferred and the accuracy of the estimate for each category listed. If your facility sends the subject chemical in waste to an off-site location where some of the chemical will be recycled and the remainder will be treated, estimate each amount separately (i .e ., waste treatment and recycling activities) . Estimated Annual Estimated % Transfers (kgs) accuracy (Optional) 

### Incineration Wastewater Treatment (Excluding POTW) Underground Injection Hazardous Waste (RCRA Subtitle C) Landfill Other Landfill Recycle or Recovery (Does not include internally recycled) Internally Recycled Unknown or Other Basis for each release estimate : `" The surfactant content in the polymer was measured per the attached method PF 89/110 GC E - Perfluorooctanoate and Higher Homologues in Algoflon Matrices - Analysis using GC-FID

Comments:_ . ;= 

### APPROVED -COPY N° AUSIMONT S.P.A. Centro Ricerche e Sviluppo

Bollate Analytical Method PF 89/110 GC E Perfluorooctanoate and higher homologues

in Algoflon matrices Analysis using GC-FID ,

This document is composed by: 

### N° pages: 4 N° tables: N° figures: N° attachments: 

### Edition: 4 Date: Oct 2001 Laboratory : GC Author : Oriani I Verification: Morandi Approval : Pace 1 Scope and application 

### 1 .1 This method is for the analysis of extracts of perfluorooctanoate (APFO) and related homologues. 1 .2 Applicable compounds are: perfluorooctanoate (APFO) [C7F15C00-], perfluorononanoate [C8F»COO], perfluorodecanoate [C9F19C00-], perfluoroundecanoate [CJoF2,C00-], perfluorododecanoate [C>>F23C00-] and higher homologues. 1 .3 Matrices: Algoflon based formulations and environmental samples compatible with esterification and GC-FID determination . 2 Summary 2.1 Analysis of APFO and homologues extracted matrices is performed by injection in a packed column, glass, 2m long, 6mmo.d., 3mm i .d ., packed with metylPF 89/110 GC E Page 1 of 4siloxane rubber SE 30 20% on Chromosorb W AW DMCS 80-100 mesh, isothermal run at 80°C, flame ionisation (FID) detector . 3 Definitions 3.1 APFO

: perfluorooctanoate. 3.2 Gaschromatograph (GC) with flame ionisation detector (FID) : model 8000 top fromFisons equipped with standard packed column injector . 3.3 Data system

: Electronic integrator mod. Chromjett from Fisons or PC based acquisition systemmod. Chromcard fromFisons. 4 Safety precautions 4.1 Use caution with temperatures of GC injector and detector . When running temperatures are of about 250°C. 4.2 When handling samples or solvents wear appropriate protective gloves, eyewear, clothing and any other protective devices mandatory in your working area. 5 Interferences 5.1 To minimise interferences when analysing samples PTFE vials and tubing should not be used for sample storage or handling. 6 Equipment 6.1 GC FID mod. 8000 fromFisons 6.2 Electronic recording integrator mod. Chromjett from Fisons or PC running Chromcard software fromFisons 7 Supplies and materials 7.1 GCgrade Nitrogen used as carrier gas 7.2 GC grade Hydrogen used for FID 7.3 GC grade Air used for FID 7.4 Micro-syringes glass 10 pl 7.5 Centrifuge tubes glass l Oml 7.6 Vials lOml 8 Reagents and standards 

### 8.1 CFC 113 Fluka for IR or equivalent

PF 89/110 GC E Page 2 of 4

## u5! 6T1 onT_ . 8.2 Standard Typically one method and matrix blank and one continuing calibration standard S20ppmare prepared with each group of samples. 9 Quality control 9.1 Method and matrix blank Analyse a method and matrix blank prior to each group of samples. 9.2 Matrix spike 

### Analyse a matrix spike prior to standard calibration curve. 9.3 Continuing calibration check 9.3.1 Analyse S20ppm sample first to assure the accuracy of initial calibration curve. 9.3.2 Analyse S20ppm every tenth samples. 9.3.3 If a significant change (i .e . >25%) in peak area occurs, relative to the initial calibration curve, subsequent analysis will be invalid. 10 Calibration and standardisation 10.1 Prepare and analyse a standard calibration curve after each maintenance intervention 

### 10.2 The r2 value for linear regression of data should be 0.98 or greater 10.3 If curve does not meet requirements change analytical column or re-prepare calibration standards. 11 Procedures 11 .1 Use a packed column, , glass, 2mlong, 6mm o .d., 3mm

i .d., packed with metylsiloxane rubber SE 30 20%on Chromosorb W AW DMCS 80-100 mesh 11 .2 Carrier : Nitrogen, flowrate : 40ml/min measured at roomtemperature connecting flowmeter to detector outlet . 11 .3 Injector : standard packed at 250°C 11 .4 Detector : FID at 250°C, Hydrogen flowrate: 30m1/min, Air flowrate 500m1/min 11 .5 Oven temperature: isothermal at 80°C 11 .6 Injection volume: liquid measured 1 W 11 .7 APFO retention time: 3 minutes

PF 89/110 GC E Page 3 of 4

# RU5lCfl1Df1T

12 Data analysis and calculations Calculate actual concentration of APFO, or other applicable compounds, from calibration line using an external standard method. 13 Method performances Method detection limit and method quantitation limit are referred to each matrix and reported in specific methods. 14 Pollution prevention and waste management Samples in CFC are disposed in dedicated container . 

### Samples in water / methanol are disposed in dedicated container Solid polymer residuals are disposed in dedicated container Disposable glass vials are disposed in broken glass containers located in laboratory. 15 Records None

PF 89/110 GC E Page 4 of 4

# Appendix D



# Draft Facility Report on Product Content APFN

NONCBI 

# Company Sanitized

## 2010/15 PFOA Stewardship Program



# Draft Facility Report on Product Content

I . CHEMICAL IDENTIFICATION Identify the product (e.g fluoropolymer dispersion) for which you are submitting information:

Product name: FLUOROPOLYMER Product description (including concentrations of perfluoroalkyl chemicals identified in Section IV below and year ofproduction) : ~ ~ APFN

_ CAS number : 77623-779

II . COMPANY IDENTIFICATION Identify the company and location of the facility submitting information:

Company name : SOLVAY SOLEXIS, INC Site location: THOROFARE, NJ Identify a company technical contact who can respond to inquiries about the information submitted: Technical contact: VIRGINIA HUBERT

Phone: ( 713) 525-6051 Address: 10 Leonard Lane, Thorofare, NJ III . PRODUCTION Calendar year for which you are reporting: Jan l, 2009 to Dec 31, 2009 Provide the amount of the product for the reporting year at each specific site :

Imported Manufactured L-- kgs/yr kgs/yr

### IV. PRODUCT CONTENT

A . CONCENTRATIONS OF RELEVANT PERFLUOROALKYL CHEMICALS Please provide the concentrations (ppb) of various perfluoroalkyl chemicals in your product . For chemicals for which you do not have actual data, please provide range estimates. 

## CAS # 77623-77-9 The following is a nonexhaustive list of chemicals that should be included: PFOA and its salts " Octanoic acid, pentadecafluoro- (CAS 335-67-1) " Octanoic acid, pentadecafluoro- ammoniumsalt (CAS 3825-26-1) PFOA precursors " Octane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7, 8,8-heptadecafluoro-8-iodo- (CAS 507-63-1 ;1 " 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- (CAS 678-39-7) " 1-Decene, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- (CAS 21652-58-4) " 2-Propenoic acid, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl ester (CAS 27905-45-9) " 2-Propenoic acid, 2-methyl-, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl ester (CAS 1996-88-9) " 2-Decenoic acid, 3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-hexadecafluoro- (CAS 70887-84-2) " Decanoic acid, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- (CAS 27854-31-5) Higher homologues " Dodecane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12-pentacosafluoro-12-iodo- (CAS 307-60-8) " Decane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10-heneicosafluoro-10-iodo- (CAS 423-62- 1) " Nonanoic acid, heptadecafluoro- (CAS 375-95-1) " Decanoic acid, nonadecafluoro- (CAS 335-76-2) " 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- (CAS 678-39-7) " Decane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-heptadecafluoro-10-iodo- (CAS 2043-53-0) " Dodecane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10-heneicosafluoro-12-iodo- (CAS 2043-54-1) " 2-Propenoic acid, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl ester (CAS 4980-53-4) " 2-Propenoic acid, 2-methyl-, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12- heneicosafluorododecyl ester (CAS 17741-60-5)

### Part IV (cont .)

B. ANALYTICAL METHODS The surfactant content in the polymer was measured per the attached method PF 89/110 POW E - Perfluorooctanoate and Higher Homologues in Polymer Bulk or Sintered - Extraction and Esterification. Comments:

# RUSimon-r .-_r-~ APPROVED -COPY N° 

### AUSIMONT S.P.A

. Centro Ricerche e Sviluppo

Bollate Analytical Method 

### PF 89/110 POW

E Perfluorooctanoate and higher homologues in polymer bulk or sintered 

### Extraction and esterification

This document is composed by: N° pages: 5 N° tables: N° figures: N° attachments: Edition : 3 Date: June 2001 Laboratory: GC Author : Oriani I Verification: Morandi Approval : Pace 1 Scope and application 

### 1 .1 This method is for the extraction of perfluorooctanoate (APFO) and related homologues fromAlgoflon (PTFE) polymer bulk or sintered. 1 .2 Applicable compounds are : perfluorooctanoate (APFO) [C7F,SCOO-], perfluorononanoate [CgF»COO], perfluorodecanoate [C9F19C00-], perfluoroundecanoate [C,oFZ]C00-], perfluorododecanoate [C,1F23C00-] and higher homologues. 1 .3 Matrices: Algoflon polymer, bulk or sintered, dry (humidity lower than 5% by weight) . 2 Summary 2 .1 About 500mg (I g if sintered) of Algoflon is weighed in a 10 ml vial . Add 2ml of methanol containing 1%Sulphuric acid. Close carefully the vial with a PTFE

PF 89/110 POW

E Page 1 of 5

# usimon-r_P_- capped septum, then allow APFO esterification at 70°C over night . At room temperature add l ml of CFC 113, centrifuge then transfer 2 ml of clear solution in a lOml vial . Wash out acidic methanol with 4ml water . Close vial and allow phases separation at 40°C for 15 minutes. Inject 1~d of lower liquid layer . Analyse using method PF 89/110 GC E. 3 Definitions 3.1 APFO

: perfluorooctanoate . 4 Safety precautions 4.1 When handling samples or solvents and hot vials wear appropriate protective gloves, eyewear, clothing and any other protective devices mandatory in your working area. 5 Interferences 5.1 To minimise interferences when analysing samples PTFE vials and tubing should not be used for sample storage or handling. 6 Equipment 

### 6.1 Centrifuge ALC CENTRIFUGETTE 4236 6.2 Shaker IKA-VIBRAX-VXR 6.3 Balance (+/- lmg) 7 Supplies and materials 7.1 Gloves 7.2 Timer 7.3 Syringes glass 1 cc, 5 cc 7.4 Micro-syringes glass 10 ~tl, 250 41, 7.5 Centrifuge tubes glass lOml 

### 7.6 Vials lOml 7.7 Glass bottles nominal 100m1 7.8 Glass volumetric flasks 100ml volume 7.9 Athermic gloves 8 Reagents and standards 8.1 Concentrated sulphuric acid R.P.E . Carlo Erba or equivalent 8.2 Methanol R.S . Carlo Erba or equivalent 

### 8.3 CFC 113 Fluka for IR or equivalent 8.4 Ammonia 30%R.P.E . Carlo Erba or equivalent PF 89/110 POW

E Page 2 of 5

# RU5I tT'1 onT .,

8.5 Reagent preparation 1 %sulphuric acid in methanol : in a bottle of nominal l 00m1 (true volume 116m1) weigh 49.5g of methanol then add slowly 0.5 g concentrated sulphuric acid. 8.6 Standard preparation So1 .A: weigh 100mg of solid ammonium salt of perfluoro-acid, dissolve in 100ml methanol in volumetric flask. S200ppm

: transfer 100~1 of So1 .A in a 10m1 vial, add 1 .6ml of methanol 1% sulphuric acid and followthe esterification procedure. S 100ppm

: transfer 50~1 of So1 .A in a l Oml vial, add 1 .8m1 of methanol 1 % sulphuric acid and followthe esterification procedure. S50ppm : transfer 25p1 of So1 .A in a lOml vial, add 1 .9m1 of methanol 1% sulphuric acid and followthe esterification procedure. 

### S20ppm : transfer 10p1 of So1 .A in a l Oml vial, add 2m1 of methanol 1 % sulphuric acid and followthe esterification procedure. S10ppm : transfer 5~1 of So1 .A in a l0ml vial, add 2ml of methanol 1%sulphuric acid and followthe esterification procedure. 9 Quality control 9.1 Method and matrix blank In a lOml vial weigh 500mg of Hyflon' MFA powder, follow esterification procedure. 

### Note: Hyflon polymers are free fromAPFO and Surflon surfactants With each batch of samples prepare and analyse a blank as first sample. 9.2 Matrix spike In a lOml vial weigh 500mg of Hyflon' MFA powder, add 5 pl of So1 .A then followesterification procedure. Note : Hyflon polymers are free fromAPFO and Surflon surfactants . With each complete calibration prepare a matrix spike and a blank. As last samples after calibration inject in triplicate blank and matrix spike. 9.3 Continuing calibration check 9.3.1 With each batch of samples prepare S20ppmcalibration solution.

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## U51monTa~-

9.3.2 Analyse S20ppm sample first to assure the accuracy of initial calibration curve . 9.3.3 Analyse S20ppmsample per group of 10 samples, followed by a blank (9.1) . 9.3.4 Analyse S20ppmsample last to assure the accuracy of data. 10 Calibration and standardisation 10.1 Prepare calibration standards 10.2 Inject 1 pl each at least in triplicate 10.3 Calculate concentration of APFO in dispersion from APFO concentration in solution assuming that So1 .A contains about 1 pg APFO/pl solution and Algoflon weight is 500mg. Correct concentration only if weighed APFO differs from nominal 100mg more that + / - 10% (namely less than 90mg or more than 110mg) . 11 Procedures 11 .1 Weigh about 500mg (I g if sintered) Algoflon in a l Oml vial 11 .2 Record weight and label vial with sample ID 11 .3 Prepare S20ppmsolution and label accordingly 11 .4 At roomtemperature, add 2ml of methanol containing 1 %Sulphuric acid. 11 .5 Close carefully the vial with a PTFE capped septum . 11 .6 Allow

APFOesterification at 70°C over night . 11 .7 At roomtemperature add 1 ml of CFC 113, centrifuge then transfer 2 ml of clear solution in a lOml vial . 11 .8 Wash out acidic methanol with 4ml water . Close vial and allow phases separation at 40°C for 15 minutes. 11 .9 Using a syringe take out the aqueous layer . Wash a second time with 4ml water . Close vial and allowphases separation at 40°C for 15 minutes. 11 .10 At roomtemperature, inject lpl of lower liquid layer . Analyse using method PF 89/110 GC E. 12 Data analysis and calculations Calculate actual concentration of APFO, or other applicable compounds, from calibration line using an external standard method. Correct data calculated from calibration line only if the amount of polymer used differ from500mg by a quote higher than +/- 5%

using the formula: Conpp,n = Calpp,T, * (Trueamt/500) Where: Conppm = Concentration in ppmof surfactant corrected for polymer weight Calppm = Concentration in ppmof surfactant fromcalibration line Trueamt = Weight in mg of polymer used PF 89/110 POW

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# monT

13 Method performances Method detection limit is 4ppmAPFO in Algoflon . Method quantitation limit is l Oppm . For sintered Algoflon method detection limit is 2ppm APFO . Method quantitation limit is 6ppm . Precision and accuracy are calculated from data of calibration line; precision is percent standard deviation at each point, accuracy is percent ratio of average calculated amount to nominal concentration at each point . Recovery is percent ratio of average area of matrix spike to average area of S l Oppmcalibration point . 14 Pollution prevention and waste management Samples in CFC are disposed in dedicated container . Samples in water / methanol are disposed in dedicated container Solid polymer residuals are disposed in dedicated container Disposable glass vials are disposed in broken glass containers located in laboratory. 15 Records None

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