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MPI 

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 

June 26,2010 to July 23,2010 

1 Introduction 

This document presents the progress of the technical work for characterization of ftuorotelonnerbased 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 June 26, 2010 up to the week 

ending July 23, 2010. The following components of the Work Plan have been completed: 

Components 1, 2, 3, 5, 6 and 7. 

2 Progress Summary 

The technical work consisted of method development outlined in Component 7 ofthe Work Plan. 

LC/MS/MS methods were developed and draft methods finalized for the following analytes: 7-3 

Fluorotelomer Acid, 8-2 Fluorotelomer saturated Acid, 8-2 Fluorotelomer unsaturated Acid, 

Perfluorooctanoic Acid, Perfluorononanoic Acid, Peri'luorodecanoic Acid and 

Perfluoroundecanoic Acid. 

GC/MS methods were developed and draft methods finalized for the following analytes: 6-2 

Fluorotelomer Alcohol, 8-2 Fluorotelomer Alcohol, 10-2 Fluorotelomer Alcohol, 8-2 Fluorotelomer 

Ethene, 8-2 Fluorotelomer Iodide, 10-2 Fluorotelomer Iodide, Periluorooctyl Iodide, Perfluorodecyl 

Iodide, 8-2 Fluorotelomer Acrylate, 7-2 Fluorotelomer iso-ethanol and PFOA telomer 8-2 ester. 

A draft protocol for the validation of the GC/MS and LC/MS/MS methods was written and 

reviewed. The protocol was initiated on 07/19/2010. 

The total method development time incurred for the period of time covered by this report was 31 

hours. The associated cost for this method development work is $7750 as identified in 

Component 7 of the Work Plan. The cost is based upon the daily rate of $2,000. The total costs 

associated with the components initiated with respect to this Progress Report are $7750.00. The 

associated invoice is presented in Appendix C. 

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3 Analysis by LC/MS/MS 

Two LC/MS/MS draft methods were prepared and submitted for Quality control review: 

• "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" (V0006601) 

• "Method of Analysis for the Determination of Periluorooctanoic Acid, Periluorononanoic 

Acid, Pertluorodecanoic 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" (V0006602) 

4 Analysis by GC/MS 

The analyses were performed on a Agilent (Formerly Hewlett-Packard) GC/MS system with 

positive chemical ionization using helium carrier gas and methane reagent gas. A HP-IMS 

column was used for the development work for the following analytes: 

Analvtes 

6-2 Fluorotelomer Alcohol 

8-2 Fluorotelomer Alcohol 

10-2 Fluorotelomer Alcohol 

8-2 Fluorotelomer Ethene 

8-2 Fluorotelomer Iodide 

10-2 Fluorotelomer Iodide 

Perfluorooctyl Iodide 

Perfluorodecyl Iodide 

8-2 Fluorotelomer Acrylate 

7-2 Fluorotelomer iso-ethanol 

PFOA telomer 8-2 ester 

lUPAC name 

1 H,1 H,2H,2H-perfluorooctan-1-ol 

1H,1H,2H,2H-perfluorodecan-1-ol 

1H,1H,2H,2H-perfluorododecan-1-ol 

1H,1H,2H-perfluoro-1-decene 

1H,1H,2H,2H-periluorodecyl iodide 

1 H,1 H,2H,2H-perfluorododecyl iodide 

Perfluorooctyl Iodide 

Perfluorodecyl Iodide 

2-propenoicacid, 

3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10.10-

heptadecafluorodecyl ester 

2-nonanol, 

3,3,4.4,5,5,6,6,7,7,8,8,9,9,9-

pentadecafluoroOctanoic acid, pentadecafluoro3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-

heptadecafluorodecyl ester 

CAS# 

647-42-7 

678-39-7 

865-86-1 

21652-58-4 

2043-53-0 

2043-54-1 

507-63-1 

423-62-1 

27905-45-9 

24015-83-6 

Not 

Available 

Calibration standards in MTBE containing all analytes were prepared. The concentrations for 

each analyte were 10, 20, 50, 80, 100, 200, 500 and 1000 ng/mL. Linearity was achieved for 

each analyte from 10 to 200 ng/mL. 

8-2 Fluorotelomer Ethene was analyzed under NCI condition on a DB-624 column (30m x 

0.25mm x 1.40pm df). Linearity was achieved from 10 to 200 ng/mL. 

Draft GC/MS methods for all analytes under PCI condition and for 8-2 Fluorotelomer Ethene 

under NCI condition were finalized. 

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Two GC/MS draft methods were prepared and submitted for Quality control review: 

• "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 in 

Fluorotelomer-based Products and Corresponding Synthesized or Purified Polymers by 

GC/PCl/MS" (V0006603) 

• "Method of Analysis for the Determination of 8-2 Fluorotelomer Ethene in Fluorotelomerbased Products and Corresponding Synthesized or Purified Polymers by GC/NCI/MS" 

(V0006604) 

5 Attachments 

5.1 Appendix A: Draft Methods (LC/MS/MS) 

5.2 Appendix B: Draft Methods and Raw data (GC/MS) 

5.3 Appendix C: Invoice 

6 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 properly gather and present the infonnation 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. 

MPI Research 07/30/2010 Technical Progress Report ^^^ ^ ^^^"^ 
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OJI? ^ W/0 

Amy SheehanjuBtudy Director Date 

MPI Research 07/30/2010 Technical Progress Report PAGE 4 OF 4