TSCA-HQ-2004-0016, et. al. July 20, 2011

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2

nd Quarter 2011 Progress Report

April 1, 2011 – June 30, 2011

Biodegradation Supplemental Environmental Project (SEP A)

A. Pursuant to Section V.l.a. of the SEP, DuPont is required to submit a quarterly report within thirty 

days after the end of each calendar-year quarter. This report which is due July 31, 2011 satisfies 

said requirement.

1. Description of Activities Undertaken

A. Panel Administrator

As reported in the previous Quarterly Report, the SEP Panel submitted its “Preliminary Conclusions and 

Recommendations” report on the biodegradation pilot studies to EPA and DuPont on December 9, 2010. 

In its Preliminary Conclusions and Recommendations Report, the Panel noted that it would need to see 

the Certificates of Analysis for the test materials before it could make specific recommendations on the 

test substance(s) or the analytes to be measured in the long-term study, as required by the SEP (Appendix 

A, Sect. V.A.2.c & d). Shortly thereafter, it was agreed to by EPA and DuPont that the Panel’s Final 

Report on these studies should be deferred until the characterization report from MPI Research was 

received and that the Panel’s Final Report would encompass its assessment of both the biodegradation 

pilot studies and the analytical characterization data. 

In April 2011 a revised draft of the SEP Panel’s Final Report on the biodegradation pilot studies was 

prepared and distributed to the Panel, incorporating Panel member comments on the previous draft. The 

Panel also was informed of modifications to the protocol for the long-term biodegradation studies that had 

been agreed to between EPA and DuPont since submission of the Panel’s “Preliminary Conclusions and 

Recommendations Report” report in December.

During this Quarter, ILSI RF provided monthly updates to the Panel on the status of the analytical 

characterization work and the estimated completion date of the Analytical Characterization Lab’s report, 

based on input received from DuPont. ILSI RF is expecting to receive the report from the Analytical 

Characterization Lab in late August 2011.

B. MPI Research Characterization Work

DuPont continued to host monthly conference calls/webmeetings with MPI and EPA to address technical 

issues and answer any questions EPA may have on the monthly progress reports submitted by the 

laboratory. On March 25, 2011, DuPont submitted a scope of work modification document to EPA for 

review and approval (Email from Robert Tucker 3/25/11 10:28AM). MPI is not realizing the economies 

of scale they had expected when they originally submitted their proposal for the SEP work, as a result of 

the reduced scope of work. They also had not planned for modifications to the extraction procedure and 

the effort associated with it. Their proposed changes were outlined in the document submitted to EPA. 

DuPont sought EPA's approval, so that DuPont may process the changes and allow MPI to be paid for the 

work they are performing. EPA approved the scope of work modifications on June 7, 2011 (Email from 

Mark Garvey 6/7/11 11:43 AM).

MPI’s technical work this quarter focused on characterization of the A3 pilot test group. A proposal to 

conduct testing to determine if an adjustment in sample size would improve the extractability and increase 

the amount of extraction solvent recovered was submitted to EPA for approval on February 9, 2011 

(Email from Paul Connolly 2/9/11 11:48AM). With some modifications proposed by EPA, the proposal 

was approved on March 21, 2011 (Email from Mark Garvey 3/21/11 5:10 PM). This work was carried 

out and indicated there was a lack of separation between the MTBE and the aqueous dispersion in water 

when the volume of water was 15 mL. Following additional discussions with the team, it was decided to 
TSCA-HQ-2004-0016, et. al. July 20, 2011

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change the amount of aqueous dispersion to approximately 1.455 mg and the volume of water to 1 mL. 

The results of this work in conjunction with discussions held with DuPont and WLI led the team to 

suspect that the GC/MS inlet temperature may have caused thermal degradation of the polymer into the 8-

2 FTOH. MPI re-injected the previously generated MTBE extracts at a lower inlet temperature. The 

results provided information on the effect of reducing the GC inlet temperature from 200 to 150 degrees 

C on 8-2 FTOH concentrations in the MTBE extracts. Initial results showed an 80% concentration 

reduction of 8-2 FTOH in the first three MTBE extracts (A, B, C1) from the two polymers in two trials 

(i.e., C0479706 Trial 2 and C0479715 Trial 3). As a result, proposals for additional method development 

work were submitted by MPI to EPA and DuPont.

On May 16, 2011, MPI proposals for additional development work were submitted to EPA for review and 

approval (Email from Bill Berti 5/16/11 4:37 PM). One involved Tetrahydrofuran (THF) dissolutions of 

the two samples from the A3 pilot test group in duplicate and only for the analytes PFOA by LC/MS/MS 

and 8-2 FTOH also by LC/MS/MS. The second involved MTBE Extracts of the two samples from the A3 

pilot test group in duplicate and only for the analytes PFOA by LC/MS/MS and 8-2 FTOH also by 

LC/MS/MS. EPA approved these proposals on May 25, 2011 (Email from Mark Garvey 5/25/11 12:54 

PM). MPI, DuPont, and EPA agreed to evaluate the THF preparations of the A3 pilot test group samples 

rather then perform MTBE extractions. MPI developed preliminary chromatographic and mass spec 

conditions for the 8-2 FTOH compound and presented the data to DuPont and EPA. On June 22, a 

conference call was held to discuss the data. At that time, a request was made to include the 6-2 and 10-2 

FTOH compounds in the analysis. MPI is continuing towards the goal of analyzing A3 samples dissolved 

in THF. As of the end of the quarter, MPI was tasked with constructing a time-line and estimated costs 

for: 1) LC/MS method development for 6:2, 8:2, and 10:2 FTOH 2) validation protocol amendment and 

approval, 3) validation study, 3) new COA protocol or protocol amendment and revised QAPP and 

approvals, 4) perform study, 5) write draft report, 6) QA review and approvals. A complete COA for the 

A3 test substance is expected August 26, 2011.

Additional details regarding MPI’s progress can be found in the three technical progress reports that were 

submitted by MPI directly to EPA on 4/29/2011, 5/27/2011, and 6/29/2011.

C. Wildlife International Biodegradation Work

DuPont continued to host monthly conference calls/webmeetings with WLI and EPA to address technical 

issues and answer any questions EPA may have on the monthly progress reports submitted by the 

laboratory. Work conducted over the period consisted of the review and discussion of data from test 

substance characterization and discussion of Task E items with stakeholders. Technical work also 

consisted of a method installation trial to demonstrate quantitative acid analyte procedural recovery using 

the revised activated sludge mixed-liquor procedure. In addition, revisions of draft method validation 

protocols, and preparation of a Scope of Work to evaluate the analysis of 6-2 FTOH, 8-2 FTOH and 10-2 

FTOH in MTBE extracts of an activated sludge matrix by liquid chromatography mass spectrometry in 

the presence and absence of the Group A1 polymer were started. 

On December 17, 2010, the Wildlife Draft QAPP and Draft Analytical Method Validation Protocol were 

submitted to EPA for review and approval (Email from Robert Tucker 12/17/10 10:26 AM). WLI revised 

the QAPP based on EPA review; however, revisions may be needed based on the need to complete all 

analysis using a LC/MS/MS instead of using GC/MS for alcohols due to potential for polymer 

degradation in the GC inlet at elevated temperature. As of the end of the quarter, WLI was charged with 

outlining an LC/MS/MS method (including cost and timing) to measure FTOH in the SCAS test MTBE 

extracts instead of using GC/MS as a result of the potential for polymer degradation in the GC inlet at 

elevated temperature. Issues such as number of replicates, frequency of draw and fill, analytical method 

and validation, etc. need to be resolved prior to completing final protocol for QAPP. David Lynch of 

EPA and Bill Berti of DuPont were to convene a conference call the week of July 11, 2011, to discuss a 
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SCAS strawman that addresses the number of replicates, frequency of draw and fill, etc. Participants will 

include Wildlife, EPA, and DuPont.

Additional technical details regarding WLI’s progress can be found in the three technical progress reports 

that were submitted by WLI directly to EPA on 4/29/2011, 5/31/2011, and 6/29/11.

D. Submitted Quarterly Progress Report Describing Progress 

Section V.I.a. of the CAFO provides that “Within thirty days after the end of each calendar-year quarter 

(i.e., by April 30, July 31, October 30 and January 30) after execution of this Consent Agreement 

pursuant to Paragraph IX.9., respondent shall submit in writing a quarterly report for the preceding 

quarter that shall include a discussion of the Respondent’s progress in satisfying its obligations in 

connection with each SEP including at a minimum, a narrative description of activities undertaken, 

compliance with the schedules or milestones set forth in the applicable appendix, and a summary of costs 

incurred since the previous report.” 

On April 20, 2011, a 1st Quarter 2011 progress report covering the time period from January 01, 2011 to 

March 31, 2011 was submitted to the EPA (CD-2011-2).

2. Document Reviews 

A. Review and Approval of Wildlife Pilot Study Report

An unaudited draft report for the initial biodegradation pilot study (Group 1, Substance 1) was sent to

EPA, DuPont and the Panel Administrator on October 25, 2010. A revised unaudited draft report for the 

initial pilot study (Group 1, Substance 1) was sent to the EPA, DuPont and the Panel Administrator on 

November 5, 2010. An audited draft report was sent to the EPA, DuPont and the Panel Administrator on 

December 2, 2010 and the raw data was sent on December 13, 2010. Final comments from DuPont and 

EPA were to be submitted by June 17, 2011. WLI will issue the report.

B. Review and Approval of Wildlife Draft QAPP and Analytical Method Validation Protocol

On December 17, 2010, the Wildlife Draft QAPP and Draft Analytical Method Validation Protocol were 

submitted to EPA for review and approval (Email from Robert Tucker 12/17/10 10:26 AM). WLI has 

revised the QAPP based on EPA review. Issues such as number of replicates, frequency of draw and fill, 

analytical method and validation, etc. need to be resolved prior to completing final protocol for QAPP. 

Protocol revisions may now be needed based on the need to complete all analysis using a LC/MS/MS 

instead of using GC/MS for alcohols due to potential for polymer degradation in the GC inlet at elevated 

temperature.

 C. Review and Approval of the ILSI SEP Panel Preliminary Report

On December 9, 2010, the ILSI SEP Panel report was sent to EPA and DuPont; its title is “Preliminary 

Conclusions and Recommendations: Evaluation of the Biodegradation Pilot Studies by the ILSI Research 

Foundation Biodegradation SEP Panel.” On December 16, 2010, EPA accepted it to satisfy the final 

report required under the SEP on the condition that the panel revises the document in light of information 

obtained after the characterization data becomes available (Email from Mark Garvey 12/16/10 5:31 

PM). As of the end of 1Q2011, the Panel is still awaiting characterization data from MPI so they may 

finalize the report.
TSCA-HQ-2004-0016, et. al. July 20, 2011

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3. Compliance with Schedules or Milestones

This section outlines compliance with schedules or milestones as well as requests for extensions granted 

between April 01, 2011 and June 30, 2011. All deadlines in the second quarter were met. Pending 

deadlines and open issues are also described below.

A. Quarterly Progress Reports

On April 20, 2011, a 1st Quarter 2011 progress report covering the time period from January 01, 2011 to 

March 31, 2011 was submitted to the EPA (CD-2011-2). The next quarterly progress report (3Q2011) is 

due October 30, 2011.

B. Pending Deadline Summary

All deadlines were met in the second quarter of 2011. There is one pending deadline at this time: 

1) October 30, 2011 to submit the 3Q2011 progress report

4. Summary of Costs Incurred

The cost of the SEP from April 1, 2011 to June 30, 2011 as it was accounted on cost ledger is shown in 

Attachment A. The table shows the costs from both accounts (SEP Eligible account and the DuPont 

Synthesis account) and breaks the cost distribution down into salaries, overheads, travel, operating 

supplies and analytical costs. The 2

nd quarter 2011 SEP eligible (Biodegradation Main account) costs

were $155,685 and the Total SEP eligible project costs to date are $2,499,981.

5. Attachment

Title Number of Pages

Attachment A SEP Cost Summary for 2Q2011 1
TSCA-HQ-2004-0016, et. al. July 20, 2011

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Attachment A

Cost Summary - 2Q2011 Progress Report

SEP Biodegradation: Synthesis Account - VZ78101073 (DuPont Funded)

January February March

1Q 2011 

Sum April May June

2Q 2011 

Sum July August September

3Q 2011 

Sum October November December

4Q 2011 

Sum YTD 2011

Total Costs 

of Program 

as of Dec 

31, 2010

Salaries 

Chambers Works 0 0 0 0 0 140,428

Barley Mill/Exp Sta 0 0 0 0 0 26,529

Travel 0 0 0 0 0 0

Operating Supplies 0 0 0 0 0 19,071

CCAS Analytical 0 0 0 0 0 135,260

Consultants 0 0 0 0 0 248,247

RAS Analytical 0 0 0 0 0 112,288

R&D Research Serv 0 0 0 0 540

Engg 0 0 0 0 0 6,335

Overheads 0 0 0 0 0 0

Chambers Works 0 0 0 0 0 29,847

Barley Mill/Exp Sta 0 0 0 0 0 3,904

TOTAL 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 722,449

SEP Biodegradation: Main Account - VZ78911724 (SEP Eligible)

January February March

1Q 2011 

Sum April May June

2Q 2011 

Sum July August September

3Q 2011 

Sum October November December

4Q 2011 

Sum YTD 2011

Total Costs 

of Program 

as of Dec 

31, 2010

Salaries 

Chambers Works 0 0 0 0 0 267,148

Barley Mill/Exp Sta 1,774 1,731 2,921 6,426 3,805 1,680 1,545 7,030 0 0 13,456 139,941

Travel 591 591 0 0 0 591 2,558

Operating Supplies 0 0 0 0 0 2,676

Exygen 0 0 0 0 0 124,250

MPI Research Inc. 73,434 73,434 14,074 8,042 22,116 0 0 95,550 153,721

ILSI Research 

Foundation 59,524 59,524 6,986 22,447 29,433 0 0 88,957 163,677

Wildlife International 

LTD 44,086 34,651 21,960 100,697 27,116 24,800 51,916 0 0 152,613 980,775

CAS billings 7,250 14,500 3,480 25,230 11,020 8,120 11,600 30,740 0 0 55,970 142,722

Analytical Lab 0 0 0 0 0 126

R&D Research Serv 7,020 5,460 12,480 5,980 3,120 9,100 0 0 21,580 1,620

Overheads 0 0 0 0 0 0

Contract Admin 1,763 1,040 4770 7,573 2,060 483 1,488 4,031 0 0 11,604 52,061

Barley Mill/Exp Sta 978 552 978 2,508 853 233 233 1,319 0 0 3,827 24,558

TOTAL 56,442 59,494 172,527 288,463 71,894 44,125 39,666 155,685 0 0 0 0 0 0 0 0 444,147 2,055,834