PROGRESS REPORT: JULY 2010

BIODEGRADATION TESTING SUPPLEMEN TAL ENVIRONMENTAL PROJECT

Submitted to

E.I du Pont de Nemours and Company Wilmington, Delaware 19898 U.S.A.

United States Environmental Protection Agency Washington, DC U.S.A. 

# Wildlife International, Ltd.

8598 Commerce Drive Easton, Maryland 21601 USA 1 (410) 822-8600

July 30, 2010

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2010_July_Progress Report 2 Table of Contents

Title Page ..................................................................................................................... ..............1
Table of Contents.............................................................................................................. .........2
Introduction................................................................................................................... .............3 Progress Summary ............................................................................................................... ......3 Analysis by LC/MS/MS........................................................................................................... ..5 Analysis by GC/MS .............................................................................................................. .....8 Appendix A Invoice............................................................................................................. ....11 Appendix B Reagent Fortification Trials and Investigation of MTBE Evaporative
Losses..................................................................................................................13 Appendix C Analysis of Acid Analytes in Sludge by LC/MS/MS..........................................36 Appendix D Analysis of Acid Analytes in Aqueous Supernatant by LC/MS/MS ..................41 Appendix E Analysis of Acid Analytes in Trapping Media by LC/MS/MS ...........................51 Appendix F Investigation of 8-2 FTO Response by GC/MS...................................................74 Appendix G Representative GC/MC Calibrati on Curves of the Volatile Analytes.................77 Appendix H Analysis of Volatile Analytes in Aqueous Supernatant by PCI GC/MS............84 Appendix I Analysis of Volatile An alytes in Sludge by PCI GC/MS .....................................96 Appendix J Method Outlines and Sample Preparation Forms...............................................103 Appendix K Analytical Standard, Stock Solu tion and Reagent Preparation Information.....121Does Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 3 Introduction This document presents the pr ogress of the technical work for the Biodegradation Testing Supplemental Environmental Project (“Biodegr adation SEP”) performed from 28 June 2010 up to the week ending 23 July 2010.

Progress Summary The technical work consisted of continuing method development to ad apt EPA Athens soil and sludge methodologies to SCAS matrices an d preparations for th e initial p ilot study.

For LC/MS/MS analysis of the surrogate re covery standards (M+8 PFOA and M+2 PFHxA) and the acid analytes (PFOA, PFNA, PFDA, PFUA, 7-3 Acid, 8- 2 FTCA and FTUCA), experiments were conducted to further refine procedures when employing all sequential extraction rounds in sludge and aqueous supern atant SCAS matrices. Procedural losses due to volatilization during MTBE evaporation st eps have now been mitigated by using an in-situ solvent conversion procedure where the extract is not allowed to evaporate to complete dryness. Quantitative procedural recoveries we re achieved for all seven acid analytes and the two surrogate recovery standa rds when the complete method was applied to untreated aqueous supernatant (2 sequential MTBE ex tractions followed by ion-pairing cleanup of residual matrix). Quantitative procedural reco veries were also obtained for all seven acid analytes and M+8 PFOA when untreated sl udge was taken through four sequential extractions (2 x MTBE and 2 x ACN:MeOH with ion-pairing cleanup). The sludge results were achieved even though the revised MTBE evaporation procedure had not yet been implemented at the time.

LC/MS/MS methods were established for determin ation of the applicable surrogate recovery standard (M+8 PFOA) and all seven acid analytes fortified onto charcoal trapping media.
The current method for determination of the acid analytes fortifie d onto styrene (Xad-2) trapping media was shown to provide quantitative procedural recoveries for all of the acid analytes with the exception of 7-3 Acid. The method will require further refinement subsequent to the conduct of the initial pilot study.Does Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 4 Matrix fortification trials were completed in both the sludge and aqueous supernatant that demonstrated quantitative procedur al recoveries of the surrogate recovery standard (M+4 8-2 FTOH) and ten of the eleven volatile analytes (PFOI, PFDI, 8-2 FTI, 10-2 FTI, 6-2 FTOH, 8-2 FTOH, 10-2 FTOH, 7-2 sFTOH, 8-2 FTAC and 8-2-8 Ester) by positive chemical ionization (PCI) GC/MS using tw o sequential MTBE extractions. Each MTBE extract was cleaned prior to analysis using a back-partitio n in reagent water. A suitable ion(s) for monitoring 8-2 FTO by positive chemical ionizati on GC/MS at part per billion concentration
levels was not found.

The total costs associated with the project for the period covered in this Progress Report are approximately $56,560 for labor and $18,900 for in strumentation. Th e invoice and an
allocation of costs with associated tasks are presented in Appendix A.

Analysis by LC/MS/MS Reagent fortification samples pr epared in tests conducted early in the current review period provided additional evidence for acid analyt e loss due to volatility associated with evaporation of MTBE extracts to complete dryness. In each reagent fortification preparation, the appropriate reagent(s) was fortified with all acid analytes and acid surrogate recovery standards (as applicable) at the 2-10 nanogr am level using appropriate volumes from
combined acetonitrile stock solutions. Each r eagent fortification preparation was originally conceived with a unique experimental objective.

One reagent fortification trial was designed to model partitioning behavi or of acid analytes between aqueous supernatant and MTBE as func tion of aqueous solution pH (3, 7 and 9). Both the MTBE and aqueous phases were proc essed for analysis (A ppendix B). Although bias from volatile losses preclud ed an unequivocal assessment of the effect of solution pH on the partitioning behavior, it was observed that all detectable ac id analyte mass was present in the MTBE layers under acidic testing conditions. The finding supports potential use of matrix acidification in a given sequential extrac tion as a means of shifting a majority of acid analyte mass balance distribution to earlier sequen tial extraction rounds. Incorporation of the procedure into the overall methodologies may ev entually be required to meet an acceptable mole percentage criterion for defining th e endpoint of the sequential extractions.Does Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 5 The next experiment employed a reagent fortific ation sample as a positive control prepared concurrently with analyses of acid analytes fo rtified onto charcoal a nd styrene traps. The trapping media were then subsequently extr acted with a single aliquot of MTBE. The experiment demonstrated that use of a single MTBE extr action, although appropriate for quantitative procedural recovery of volatile analytes by GC/MS (reference to June 2010 Progress Report), was not suitable for obtaining acceptable procedural recoveries for the acid analytes.

Another experiment was intended to demonstrat e that the presence of aqueous supernatant or sludge matrix residue would not adversely affect acid analyt e procedural recovery when
dried MTBE extracts were reconstituted with 1:3 ACN:H 2 O. MTBE extracts from sludge and aqueous supernatant matrix blanks generated in earlier trials were fortified with the acid analytes before evaporation to complete dryne ss and reconstitution with the final solvent. Evaporative losses were again evident, especially for the sludge-exposed MTBE
fortifications.

Based on the above findings, several alternat ive nitrogen evaporation procedures were investigated. Procedural recoveries of the aci d analytes were determined for fortified MTBE extracts subjected to nitrogen evaporation to complete dryness under ambient, cold (using an ice bath) and ultra-cold (dry ice/acetone) te mperature conditions and evaporation to near dryness ( in-situ ) solvent conversion to acetonitrile. Co mparison of these approaches showed
that the in-situ solvent conversion pro cedure provided the best procedural recoveries although all modified methods pr ovided quantitative procedural recoveries for all acid analytes. The procedural recoveries for the acid analytes with the in-situ solvent conversion procedure ranged from 99.0 to 109% of the nominal fortified mass.

The revised MTBE evaporation procedure was incorporated into a trial with aqueous supernatant sample acidified to pH 3 prior to MTBE extraction. Acidification of the aqueous matrix should promote increased extractability of acid analytes into or ganic solvents due to protonation of the carboxylic ac id functional group. However, volatile losses in acidified matrix trials to this point had also been mu ch greater as compared to those observed withDoes Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 6 neutral and basic pre-treated matr ices (reference to June 2010 Progress Report, pg. 5). With the revised evaporation proce dure incorporated into the aqueous supernatant method, acceptable procedural recoveries were obtaine d for all acid analytes from an acidified aqueous matrix for the first time.

A sludge matrix experiment was conducted to comp lete a set of trials using all four proposed extractions where the sludge was subjected to various forms of pre-treatment (Appendix C). Acid analytes and surrogate recovery standards were fortified into untreated sludge in a closed system followed by four sequential extractions (2 x MTBE and 2 x ACN:MeOH with ion-pairing cleanup) using the same methods as were used in the earlier trials with acidic and basic pre-treatment (reference to June 2010 Pr ogress Report, pgs. 5-6 and Appendix F). In each of these experiments, MTBE extracts were evaporated unde r a gentle flow of nitrogen to complete dryness at ambient temperature. Although in-situ solvent conversion was not used in the cited sludge trials, untreated sludge was clearly the best experimental condition as quantitative procedural recoveri es were obtained for all anal ytes (suggesting volatile losses were minimal) and hydrolysis trends were not detected relative to obs ervations of volatile and hydrolytic losses for acidic and basic pre-treatmen ts, respectively.

As seen in the earlier sludge trials, the M+2 PFHxA surrogate recovery standard, characterized by a relatively smaller perfluorin ated carbon chain length (PFC chain lengths = 6), appeared to bind more to sludge matrix as compared to longer PFC chain-length acid analytes (PFC chain length ranging from 7-10). The mean procedural recovery for M+2 was only 56% of the nominal fortified mass. An analogous trend for telomer alcohol analytes extracted from sludge and determined by GC/MS was noted (e.g. 6-2 FTOH, see Analysis by
GC/MS ). As M+2 PFHxA will be used as a surrogate recovery standard only during the ion-pairing extract clean-up ste p, the low recoveries obtained in these sludge trials had no impact on the development strategy for the sludge SCAS matrix.

In contrast to the SCAS sludge matrix, use of the revised MTBE evaporation procedure was critical in development of a suitable aqueous supernatant method. Until now, results using the entire proposed aqueous supe rnatant procedures (two MTBE extractions followed by an ion-pairing cleanup of residual aqueous supernatant matrix) had been largely inconclusiveDoes Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 7 due primarily to the MTBE handling issues outlined herein. Using the in-situ solvent conversion procedure, an experiment was perf ormed on untreated aqueous supernatant using
2.5 and 5 milliliters of MTBE fo r each extraction. The results demonstrate that quantitative procedural recoveries for all acid analytes may be obtained using ei ther MTBE extraction volume (Appendix D*) For volatil e analyte determinations in aqueous supernatant (detailed below), 2.5 milliliters of MTBE was sufficient to quantitatively extract volatile analytes using two rounds of extraction.

As MTBE alone was not sufficient to extract acid analytes from trapping media, trials were conducted using the candidate sequential extrac tion solvents (ACN, MeOH and MeOH) to be applied to trapping media subsequent to the in itial MTBE extraction. All extracts were processed for LC/MS/MS analyses of the acid analytes and the revised MTBE evaporation procedure was used. For charcoal traps (A nasorb CSC), the binary solvent system ACN:MeOH provided quantitative procedural recoveries for all acid analytes and was marginally better than MeOH (Appendix E). N one of the candidate extraction solvents was suitable for extraction of the acid analytes from styrene-based trapping media. Given the ester linkages associated with adsorption onto styrene-based trapping media such as Xad-2, acidified solvents were investigated for use in extracting the acid analytes from Xad-2 traps.

* Due to a procedural error, only results without the ma trix internal standards applied are presented for the 5- mL test sample. Therefore, the 2.5-mL test results are presented with and without the matrix internal standards applied for comparative purposes only

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Based on unacidified trial results with styrene trapping medi a, MeOH was selected as the
solvent for acidification with 0.1 M HNO 3 or 0.1 M formic acid. MeOH containing 0.1 M
HNO 3 provided significantly better procedural recoveries compared with MeOH containing
0.1 M formic acid. LC/MS/MS sequences on processed MeOH:HNO 3 extracts were characterized by significant supp ression of the matrix internal standard responses, although they did compensate for all but one analyte (7 -3 Acid). A mass labeled equivalent for 7-3
Acid for use as a matrix internal standard is not commercially availabl e. To date, M+2 8-2
FTCA has been used as a matrix internal sta ndard for 7-3 Acid given the close proximity of 7-3 Acid and M+2 8-2 FTCA chromatographic rete ntion times. However in this instance, the mismatched internal standard appeared to overcompensate for the initial, suppressed 7-3 Acid response (approximately 30% recovery without use of the IS and excessively highDoes Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 8 procedural recovery (m ean of 214%) with the IS). The use of lower strength nitric or hydrochloric acid (less oxidative), or use of an acid with a st rength intermed iate between nitric and formic (e.g. acetic acid) may each be investigated subsequent to the conduct of the initial pilot study.

Analysis by GC/MS The PCI GC/MS response for 8-2 FTO at m/ z 427 was specified in the May 2010 Progress Report as the only available quantitation ion for this volatile analyte. Some loss of response at m/z 427 at the expected re tention time of 8-2 FTO (appro x. 2.6 min.) was documented in the June 2010 Progress Report after a new column was installed. When revisiting full scan mode with freshly prepared 8-2 FTO standard s in MTBE, we determined that the loss of response due to stability in MTBE was not a factor. Furthermore, sensitivity remains poor
and a more sensitive alternativ e ion was still not i ndicated (Appendix F). Possible means to improve 8-2 FTO sensitivity that are currently being investigated include use of a lower initial oven temperature for better peak shap e/focusing and additional optimization of the methane flow rate. For purposes of the in itial pilot study, the mass window bracketing m/z 427 response will be included in the SIM method to allow a semi-quantitative assessment of 8-2 FTO concentration if present at high enough levels. The same semi-quantitation approach was used in the EPA Athens met hod for those analytes for which calibration
standards were not used/available.

Final calibration standard levels for each of th e volatile analytes were established for use in the initial pilot study. Calibration standards for PFOI and PFDI will range in concentration from 20.0 to 100 ng/mL. Calibration standards for 8-2 FTI, 10-2 FTI, 6-2 FTOH, 8-2 FTOH, M+4 8-2 FTOH, 10-2 FTOH, 7-2 sFTOH, 8- 2 FTAC and 8-2-8 Ester will range in concentration from 0.400 to 5.00 ng/mL. All vol atile analytes and M+ 4 10-2 FTOH matrix
internal standard at a constant concentration of 5.00 ng/mL are combined in five levels of calibration. Example calibration functions for the volatile analytes are presented in Appendix G.

Quantitative procedural recoveries were obtai ned for the majority of volatile analytes fortified into untreated aqueous supernatan t (Appendix H) and sludge (Appendix I) SCASDoes Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 9 matrices using two MTBE extractions when a back-partition cleanup of each MTBE extract with polished reagent water was employed in th e procedure. The exceptions were 8-2 FTO (quantitation is currently precluded) and 8-2- 8 ester (hydrolysis to 8-2 FTOH). Depending
on the final calculation met hod to be used in subsequent tria ls (see below), several additional analytes may be at or below the acceptable range (mean procedural recovery <70% of nominal) of quantitation (e.g. PFOI in aqueou s supernatant and 8-2 FTI in sludge using combined MTBE extraction and back-partition concentration factors).

For both the aqueous supernatant and sludge SCAS matrices, the majority of volatile analyte
mass was recovered in the first MTBE extraction round. Several of the volatile an alytes (6-2 FTOH, 7-2 sFTOH, 10-2 FTOH and 8-2 FTAC) re quired two sequentia l MTBE extractions (2.5 mL each) to achieve quantitative procedural recoveries from aqueous supernatant or sludge. Evidence for hydrolytic conversion of 8-2- 8 Ester to 8-2 FTOH c ontinues to be seen
in the data summaries. Evidence that the ba ck-partition MTBE extract clean-up procedure was sufficiently robust was suggested by our obse rvation that telomer alcohol responses had not deteriorated following completion of the GC/MS matrix trials described in this Progress Report.

Appropriate calculation of the GC/MS result s will require further evaluation. Three calculation approaches currently under review are presented in Appendices H and I for aqueous supernatant and sludge, respectively. For comparative purposes, three spreadsheets using the same three approaches are also provi ded (in Appendix H) for the original aqueous supernatant back-partition data set (June 2010 Progress Report). The question to be answered is whether or not it is appropriate to assume that volatile analytes reside exclusively in the bulk post-extracted MTBE phase (as oppos ed to being co-dissolved with a portion of MTBE remaining in the aqueous phase) during the original and back-partition steps. The answer may more evident upon accumulation of additional GC/MS data sets. Fortunately, data collected during sample processing in conjunction with the database now being developed for use in the initial pilot study will allow data to be calculated in any of the proposed ways after the fact.Does Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 10 Current versions of the method outlines and bench- sheets to be used for the initial pilot study are presented in Appendix J * . Experiments are currently unde rway to perform all of the procedures as provided as a prel ude to the initial pilot study. An appropriate amount of the study analytes will be fortified into SCAS mi xed-liquor and trapping media and determined by LC/MS/MS or GC/MS as appropriate. In a ddition to assessment of procedural recovery and mass balance, the data generated will be used to refine and test the performance of the database currently under development.

Records of a replacement standa rd of 7-2 sFTOH (previous standard was consumed), stock and standard preparations and all reagent pr eparations since the June 2010 Progress Report are provided in Appendix K.

* The sample preparation sheets contain lightly shaded data entry fields that represent potential data collection that may be added for future trials/pilots/d efinitive SCAS tests to be conducted after the initial pilot study. These fields are not required for calculation of analyte concentration/mass in the original matrix compartments based on the proposed calculation methods to be employed at this time

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2010_July_Progress Report 11 Appendix A
InvoiceDoes Not Contain Confidential Business Information (CBI)2010_July_Progress Report12Allocation of CostsMonth, Year Tasks TotalDesign andProcurement ofSCAS Units(Task A)Acquisitionof Standards(Task B)Adaptation ofAnalyticalMethod (Task C)Pilot StudiesTask (D)Refinement ofMethodsTask (E)MethodValidations (Task F)StorageStability(Task G)BiodegradationStudies(Task H)InstrumentLeaseDec 2009 $1,803 $1,085 $42,422 $45,310Jan 2010 $29,227 $29,227Feb 2010 $1,300 $36,745 $38,045Mar 2010 $14,350 $14,350 $18,900Apr 2010 $570 $15,935 $16,505 $18,900May 2010 $760 $71,860 $72,620 $18,900June 2010 $57,870 $35,003 $92,873 $18,900July 2010 $42,430 $15,130 $57,560 $18,900Labor Total $1,803 $3,715 $310,839 $50,133 $366,490Materials $6,800 $10,500 $20,644 $1,724 $39,669Total Cost $8,603 $14,215 $331,483 $51,857 $406,158 $94,500Does Not Contain Confidential Business Information (CBI)

2010_July_Progress Report 13 Appendix B Reagent Fortification Trials and Investigation of MTBE Evaporative LossesDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 36 Appendix C Analysis of Acid Analytes in Sludge by LC/MS/MSDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 41 Appendix D Analysis of Acid Analytes in Aqueous Supernatant by LC/MS/MSDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 51 Appendix E Analysis of Acid Analytes in Trapping Media by LC/MSMSDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 74 Appendix F Investigation of 802 FTO Response by GC/MSDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 77 Appendix G Representative GC/MS Calibration Curves of the Volatile AnalytesDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 84 Appendix H Analysis of Volatile Analytes in Aqueous Supernatant by PCI GC/MSDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 96 Appendix I Analysis of Volatile Analytes in Sludge by PI GC/MSDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 103 Appendix J Method Outlines and Sample Preparation FormsDoes Not Contain Confidential Business Information (CBI)

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2010_July_Progress Report 121 Appendix K Analytical Standard, Stock Solution and Reagent Preparation InformationDoes Not Contain Confidential Business Information (CBI)

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