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MPl 

RESEARCH 

TSCA-HQ-2004-016, RCRA-HQ-2004-0016, TSCA-HQ-2005-5001 

SEP A Fluorotelomer-Based Product Characterization 

Subject: MPI Research Technical Progress Report 

April 01, 2012 to April 27, 2012 

1 Introduction 

This document presents the progress of the technical work for characterization of fluorotelomer-based 

products and corresponding synthesized or purified polymers in support of the Biodegradation Testing 

Supplemental Environmental Project ("Biodegradation SEP"). This progress report is prepared pursuant to 

Characterization Laboratory Exhibit A: Scope of Work, Section 4f This report describes the technical work 

performed from April 1 to April 27, 2012. 

2 Progress Summary 

The study plan to compare A3 polymer (ID #111183-35E) extractions using MTBE to dissolutions with THF 

was approved by the EPA (Appendix A) on March 8, 2012. MPI Research initiated laboratory work April 6, 

2012 and completed the laboratory experimental portion of the project on April 26, 2012. Analysis of 

dilutions for all values above the method of analysis standard curves, compilation of spreadsheets, drafting 

of the report, and the QC review of data, spreadsheets and draft report are in progress. 

A total of 461 hours were directed toward the conduct of this study plan from April 6 to 26, and included 

three and one half full time laboratory equivalents, and one full time administrative equivalent (project 

management and QC oversight). The invoice is attached as Appendix B and the total of $126,000 includes 

the charges for the conduct of this investigation and one hour of participation in a teleconference on April 

18, 2012 by Patricia de Lisio. 

Five (5) experiments were conducted as outlined in the study plan and summarized here: 

1. THF-1: A solution of the A3 polymer was prepared using THF. High and low fortifications and dilutions 

were prepared. This procedure employed the use of vortex mixing. Analysis of the samples for the 17 

analytes was executed using three MPl Research LC-MSMS methods (method numbers V7448, 

V7449, V7450) and one GCMS method (MPI Research method number V7451). No GC-NCI MS 

analysis (method V7452) was conducted for confirmation of the 8-2 FTO analyte for all five 

experiments. Raw data is contained in Appendix C. 

2. THF-2: A solution of the A3 polymer was prepared using THF. High and low fortifications and dilutions 

were prepared. This procedure employed the use of vortex mixing with centrifugation. Analysis of 

samples for the 17 analytes was executed using three MPI Research LC-MSMS methods (method 

numbers V7448, V7449, V7450) and one GCMS method (MPI Research method number V7451). 

Raw data is contained in Appendix D. 

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MTBE-1: Single-step extraction of the A3 polymer was conducted using MTBE. High and low 

fortifications and dilutions were prepared. This procedure employed the use of water-saturated MTBE, 

vortex mixing, rotisserie mixing, and freezing. Analysis of the samples for thel 7 analytes was executed 

using three MPI Research LC-MSMS methods (V7448, V6601, V6602) and one GCMS method (MPI 

Research method number V6603). Raw data for this experiment is contained in Appendix E. 

MTBE-2: Single-step extraction of the A3 polymer was conducted using MTBE. High and low 

fortifications and dilutions were prepared. This procedure employed the use of water-saturated MTBE, 

vortex mixing, rotisserie mixing, centrifugation and freezing. Analysis of the samples for thel 7 analytes 

was performed using three MPI Research LC-MSMS methods (V7448, V6601, V6602) and one 

GCMS method (MPI Research method number V6603). Raw data for this experiment had not yet 

been scanned at the time of completing this monthly progress report, and will be included in the May 

2012 progress report. 

MTBE-3: Sequential extraction of the A3 polymer was conducted using MTBE. High and low 

fortifications and dilutions were prepared. This procedure employed initial addition of one milliliter of 

water and three milliliters of MTBE, three additions of three milliliter quantities of MTBE (all 4 MTBE 

phases were stored and analyzed separately) vortex mixing, rotisserie mixing, centrifugation and 

freezing. Analysis of the samples for the 17 analytes was performed using three MPI Research LCMSMS methods (V7448, V6601, V6602) and one GCMS method (MPI Research method number 

V6603). Raw data for this experiment is contained in Appendix F. 

3 Attachments 

3.1 Appendix A: Approved study plan 

3.2 Appendix B: April 2012 Invoice 

3.3 Appendix C: THF-1 raw data 

3.4 Appendix D: THF-2 raw data 

3.5 Appendix E: MTBE-1 raw data 

3.6 Appendix F: MTBE-3 raw data 

4 Signatures 

I certify under penalty of law that I have examined and am familiar with the information submitted in this 

document and all attachments and that this document and its attachments were prepared either by me 

personally or under my direction for supervision in a manner designed to ensure that qualified and 

knowledgeable personnel property gather and present the information contained therein. I further certify, 

based on my personal knowledge or on my inquiry of those individuals immediately responsible for 

obtaining the information, that the information is true, accurate and complete. I am aware that there are 

significant penalties for submitting false information, including the possibility of fines and imprisonment for 

knowingly and willfully submitting a materially false statement. 

Patricia L. de Lisio, Study Director Date 

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[3.1 Appendix A Approved Study Plan 

MPI Research 03/27/12 Technical Progress Report 
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Proposed Study Plan to Test THF and MTBE Polymer Extractions and Analysis 

' Prepared by: Paul Connolly, Study Director, MPI Research 

Objective: 

Evaluate the differences in preparation techniques of fluorotelomer products (FTPs) for analysis by 

LC/MS/MS and GC/MS. Comparison will be between Tetrahydrofuran (THF) dissolutions and Methyl 

tert-butyl ether (MTBE) extractions. 

This experimental work will occur outside of any existing protocols and not be conducted under GLPs. 

Fluorotelomer Product for testing: 

The sample A3, Group 1 Substance 1, Sample ID 111188-35-E (MPI # C0478715) will be used for testing. 

This is the Lab-scaled synthesized fluorotelomer product (high purity raws). 

Analytes for Testing: 

The following analytes will be tested: 

1 Analyte List 

1 6-2 FTOH 

2 8-2 FTOH 

3 10-2 FTOH 

4 PFOA 

5 PFNA 

6 PFDA 

7 PFUnA 

8 7-3 Acid 

9 8-2 FTCA 

10 8-2 FTUCA 

11 8:2 FTO (GC/PCI/MS) 

12 PFOI 

13 7:2 sFTOH 

14 PFDI 

15 8:2 FTI 

16 8:2 FTAC 

17 10:2 FTI 

18 8:2 FTO (GC/NCI/MS) 

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Analytical Methodology for testing: 

The following analytical methods will be used for THF testing: 

V0007448, "Method of Analysis for the Determination of 6-2 Fluorotelomer Alcohol, 8-2 

Fluorotelomer Alcohol and 10-2 Fluorotelomer alcohol, in Fluorotelomer-based Products and 

Corresponding Synthesized or Purified Polymers by LC/MS/MS" 

V0007449, "Method of Analysis for the Determination of 8-2 Fluorotelomer Saturated Acid in 

Fluorotelomer-based Products and Corresponding Synthesized or Purified Polymers by 

LC/MS/MS" 

VQ007450, "Method of Analysis for the Determination of Perfluorooctanoic Acid, 

Perfluorononanoic Acid, Perfluorodecanoic Acid, Perfluoroundecanoic Acid, 7-3 Fluorotelomer 

Acid, and 8-2 Fluorotelomer unsaturated Acid in Fluorotelomer-based Products and 

Corresponding Synthesized or Purified Polymers by LC/MS/MS" 

V0007451, "Method of Analysis for the Determination of Perfluorooctyl Iodide, Perfluorodecyl 

Iodide, 8-2 Fluorotelomer Iodide, 10-2 Fluorotelomer Iodide, 8-2 Fluorotelomer Acrylate, 7-2 

Fluorotelomer iso-ethanol and 8-2 Fluorotelomer Ethene in Fluorotelomer-based Products and 

Corresponding Synthesized or Purified Polymers by GC/PCI/MS" 

V0007452, "Method of Analysis for the Determination of 8-2 Fluorotelomer Ethene in 

Fluorotelomer-based Products and Corresponding Synthesized or Purified Polymers by 

GC/NCI/MS" 

The following analytical methods will be used for MTBE testing: 

Draft Method, "Method of Analysis for the Determination of 6-2 Fluorotelomer Alcohol, 8-2 

Fluorotelomer Alcohol and 10-2 Fluorotelomer alcohol, in Fluorotelomer-based Products and 

Corresponding Synthesized or Purified Polymers by LC/MS/MS" 

: V0006601, "Method of Analysis for the Determination of 8-2 Fluorotelomer Saturated Acid in 

Fluorotelomer-based Products and Corresponding Synthesized or Purified Polymers by 

LC/MS/MS" 

V0006602, "Method of Analysis for the Determination of Perfluorooctanoic Acid, 

Perfluorononanoic Acid, Perfluorodecanoic Acid, Perfluoroundecanoic Acid, 7-3 Fluorotelomer 

Acid, and 8-2 Fluorotelomer unsaturated Acid in Fluorotelomer-based Products and 

Corresponding Synthesized or Purified Polymers by LC/MS/MS" 

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V0006603, "Method of Analysis for the Determination of Perfluorooctyl Iodide, Perfluorodecyl 

Iodide, 8-2 Fluorotelomer Iodide, 10-2 Fluorotelomer Iodide, 8-2 Fluorotelomer Acrylate, 6-2 

Fluorotelomer Alcohol, 7-2 Fluorotelomer iso-ethanol, 8-2 Fluorotelomer Alcohol, 10-2 

Fluorotelomer alcohol, 8-2 Fluorotelomer Ethene and PFOA telomer 8-2 Ester Fluorotelomer 

Compounds in Fluorotelomer-based Products and Corresponding Synthesized or Purified 

Polymers by GC/PCI/MS" [Note: Fluorotelomer Alcohols will be analyzed by Draft FTOH 

LC/MS/MS procedure.] 

V0006604, "Method of Analysis for the Determination of 8-2 Fluorotelomer Ethene in 

Fluorotelomer-based Products and Corresponding Synthesized or Purified Polymers by 

GC/NCI/MS" 

Procedure for Testing: 

Tetrahydrofuran Procedures 

1. Weigh vial. Add ~ 20 mg of polymer to a vial. Add 1 mL of THF and weigh. Repeat 6 times (total of 7 

vials). Prepare procedural blank by adding 1 mL THF to an empty vial. Add low and high matrix spikes to 

preselected vials. For each vial: 

A. Vortex 15 seconds. 

B. Draw an aliquot from the 3 vials. Draw an aliquot from matrix spikes. 

C. Draw a second aliquot from 3 vials and matrix spikes. Dilute lOx (weighing vials). 

D. Draw a third aliquot from the 3 vials (step B) and matrix spikes (step B). Dilute lOOx dilution (weighing 

vials). 

2. Weigh vial. Add ~ 20 mg of polymer to a vial. Add 1 mL of THF and weigh. Repeat 6 times (total of 7 

vials) and prepare a procedural blank by adding 1 mL THF to an empty vial (including weights as for the 

polymer vials). Add low and high matrix spikes to preselected vials. For each vial: 

• A. Vortex 15 seconds. 

B. Draw an aliquot from 3 vials and from matrix spikes. 

C. Draw a second aliquot from 3 vials and matrix spikes. Dilute lOx (weighing vials). 

D. Draw a third aliquot from the 3 vials (step B) and matrix spikes (step B). Dilute lOOx dilution (weighing 

vials). 

E. Centrifuge all dilutions, matrix spikes, and blanks. 

F. With care to avoid disturbing, draw an aliquot of each vial. 

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; Methyl tert-butyl ether Procedures 

1. Weigh vial. Add ~20 mg of polymer to a vial. Add 3 mL of water-saturated MTBE, and weigh. Repeat 6 

times (total of 7 vials). Prepare a procedural blank by adding 3 mL of water-saturated MTBE to an empty 

vial. Add low and high matrix spikes to preselected vials. For each vial: 

A. Vortex 15 seconds then rotate on a rotisserie for 30 minutes. 

B. Draw an aliquot from the 3 vials and the matrix spikes and freeze. 

C. Draw a second aliquot from 3 vials and matrix spikes. Dilute lOx with water-saturated MTBE 

(weighing vials), rotate 30 minutes, and freeze. 

D. Draw a third aliquot from the 3 vials (step B) and matrix spikes (step B). Dilute lOOx with watersaturated MTBE (weighing vials), rotate 30 minutes, and freeze. 

2. Weigh vial. Add ~20mgL of polymer to a vial. Add 3 mL of water-saturated MTBE, and weigh. Repeat 6 

times (total of 7 vials) and prepare a procedural blank by adding 3 mL of water-saturated MTBE to an 

empty vial (including weights as for the polymer vials). Add low and high matrix spikes to preselected 

vials. For each vial: 

A. Vortex 15 seconds then rotate on a rotisserie for 30 minutes. 

B. Draw an aliquot from the 3 vials and the matrix spikes. 

C. Draw a second aliquot from 3 vials and matrix spikes. Dilute lOx with water-saturated MTBE 

(weighing vials), rotate 30 minutes. 

D. Draw a third aliquot from the 3 vials (step B) and matrix spikes (step B). Dilute lOOx with watersaturated MTBE (weighing vials), rotate 30 minutes. 

E. Centrifuge all dilutions, matrix spikes, and blanks. 

• F. With care to avoid disturbing, draw an aliquot of each dilution and freeze. 

3. Weigh vial. Add ~20 mg of polymer to a vial. Add 3 mL of MTBE and 1 m l H20, and weigh. Repeat 6 

times (total of 7 vials) and prepare a procedural blank by adding 3 mL MTBE and 1 mL of water to an 

empty vial (including weights as for the polymer vials). Add low and high matrix spikes to preselected 

vials. For each vial: 

A. Vortex 15 seconds then rotate on a rotisserie for 30 minutes. 

B. Centrifuge. 

C. With care to avoid disturbing, freeze. Remove MTBE placing it in tared vial and store in freezer. 

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D. Add 3 mL MTBE to frozen water, let thaw to about room temperature. 

E. Repeat steps 3A through 3D to a total of four MTBE extracts, storing each sequential step in separate 

vials from the others. 

F. Following the final MTBE extraction weigh the tube and determine the weight of the sample 

remaining. Taking the remaining sample to be effectively all water, add sufficient acetonitrile to yield a 

composite being at least 60% acetonitrile. Rotate on a rotisserie for 30 minutes, centrifuge and take an 

aliquot of each sample for analysis. 

G. Take an aliquot from step 3F and dilute lOx with 60:40 ACN:H20 and analyze to check for consistence 

with results of 3F. 

Analysis 

1. For THF, 43 samples, matrix spikes, and blank should be frozen. Preselect a random order for all 

samples, placing a solvent blank every 5 samples and running a calibration curve at the beginning and 

end of each batch. Examine calibration curves for shifts. Examine solvent blanks for carryover. Examine 

the sequence for reductions in source strength. Calculate the median and range for triplicate 

extractions. Calculate the matrix spike recovery for each concentration. Record values and observations 

in a data sheet or similar. 

2. For MTBE, 105 samples, matrix spikes, and blank should be frozen. Run as described for THF samples. 

Time and cost: 

It is expected to take no more than 22 working days at a cost not to exceed $125,800. 

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3.2 Appendix B Invoice 

MPI Research 03/27/12 Technical Progress Report 
Original Invoice 

MPI Customized. 

Responsive. 

RESEARCH On-nme.* 

BUI To: 

E.I. DUPONT DE NEMOURS AND COMPANY 

NASHVILLE PAYMENT CENTER 

RE: ROBERT TUCKER 

20 OLD HICKORY BOULEVARD 

OLD HICKORY, TN 37138-3159 

UNITED STATES OF AMERICA 

Purchase Order No.: 

MPI Project Manager: 

MPi Study No.: 

Study Title: 

Invoice No.: 

Invoice Date: 

Due Date: 

Terms: 

INV-076325 

April 30, 2012 

July 29, 2012 

Net 90 

Remit Check To: 

MPI RESEARCH, INC. 

1521 PAYSPHERE CIRCLE 

CHICAGO, IL 60674 

UNITED STATES OF AMERICA 

Project ID: P5682 

Sample ID: 

CW199856 

deLisio, Patricia L 

0125.0144 

A3 STUDY TO TEST THF AND MTBE POLYMER EXTRACTIONS AND ANALYSIS 

Matrix Description Units Unit Price Amount 

* Cumulative total of 461 hours were 

directed towards the conduct of this study, 

and included three and one half full time 

laboratory equivalents, and one full time 

admlnstrative equivalent (project 

management and QC oversight). 

'4/18/12 Call attended by Patricia de Lisio 

LABORATORY TIME 1.00 125,800.00 

CONFERENCE CALL 1.00 200.00 

Total for Invoice INV-076325 USD 

$125,800.00 

$200.00 

$126,000.00 

ACH Instructions: Bank of America 

ACH Routing/ABA: 071000039 Account Number: 1054530762 Tax ID: #38-3400587 

Wire Transfer Instructions: Bank of America 

Wire Routing/ABA: 026009593 Account Number: 1054530762 Swift Code: B0FAUS3N 

Correspondence ONLY: 3058 Research Drive, State College, PA 16801 TELEPHONE: 814-272-1039 FAX: 814-231 -1580 
THIS DOCUMENT DOES NOT CONTAIN CONFIDENTIAL BUSINESS INFORMATION (CBI) 

3.3 Appendix C THF-I Raw Data 

See CD for files. 

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3^4 Appendix D fHF-2 Raw Data 

See CD for files. 

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3.5 Ajp)pendix E MTBE-I Raw Data 

See CD for files. 

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J 

3.6 Appendix F MTBE-3 Raw Data 

See CD for files. 

MPI Research 031/27/12 Technical Progress Report