PROGRESS REPORT: JULY 2010 

BIODEGRADATION TESTING SUPPLEMENTAL 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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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 Calibration 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 Analytes in Sludge by PCI GC/MS .....................................96 

Appendix J Method Outlines and Sample Preparation Forms...............................................103 

Appendix K Analytical Standard, Stock Solution and Reagent Preparation Information.....121 
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Introduction 

This document presents the progress of the technical work for the Biodegradation Testing 

Supplemental Environmental Project (“Biodegradation 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 adapt EPA Athens soil 

and sludge methodologies to SCAS matrices and preparations for the initial pilot study. 

For LC/MS/MS analysis of the surrogate recovery 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 supernatant SCAS matrices. Procedural losses due 

to volatilization during MTBE evaporation steps 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 were achieved for all seven acid analytes and the 

two surrogate recovery standards when the complete method was applied to untreated 

aqueous supernatant (2 sequential MTBE extractions followed by ion-pairing cleanup of 

residual matrix). Quantitative procedural recoveries were also obtained for all seven acid 

analytes and M+8 PFOA when untreated sludge 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 determination 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 fortified 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. 
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Matrix fortification trials were completed in both the sludge and aqueous supernatant that 

demonstrated quantitative procedural 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 two sequential MTBE extractions. Each MTBE extract was 

cleaned prior to analysis using a back-partition in reagent water. A suitable ion(s) for 

monitoring 8-2 FTO by positive chemical ionization 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 instrumentation. The invoice and an 

allocation of costs with associated tasks are presented in Appendix A. 

Analysis by LC/MS/MS 

Reagent fortification samples prepared in tests conducted early in the current review period 

provided additional evidence for acid analyte 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 nanogram level using appropriate volumes from 

combined acetonitrile stock solutions. Each reagent fortification preparation was originally 

conceived with a unique experimental objective. 

One reagent fortification trial was designed to model partitioning behavior of acid analytes 

between aqueous supernatant and MTBE as function of aqueous solution pH (3, 7 and 9). 

Both the MTBE and aqueous phases were processed for analysis (Appendix B). Although 

bias from volatile losses precluded an unequivocal assessment of the effect of solution pH on 

the partitioning behavior, it was observed that all detectable acid analyte mass was present in 

the MTBE layers under acidic testing conditions. The finding supports potential use of 

matrix acidification in a given sequential extraction as a means of shifting a majority of acid 

analyte mass balance distribution to earlier sequential extraction rounds. Incorporation of the 

procedure into the overall methodologies may eventually be required to meet an acceptable 

mole percentage criterion for defining the endpoint of the sequential extractions. 
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The next experiment employed a reagent fortification sample as a positive control prepared 

concurrently with analyses of acid analytes fortified onto charcoal and styrene traps. The 

trapping media were then subsequently extracted with a single aliquot of MTBE. The 

experiment demonstrated that use of a single MTBE extraction, 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 demonstrate that the presence of aqueous supernatant or 

sludge matrix residue would not adversely affect acid analyte procedural recovery when 

dried MTBE extracts were reconstituted with 1:3 ACN:H2O. MTBE extracts from sludge 

and aqueous supernatant matrix blanks generated in earlier trials were fortified with the acid 

analytes before evaporation to complete dryness and reconstitution with the final solvent. 

Evaporative losses were again evident, especially for the sludge-exposed MTBE 

fortifications. 

Based on the above findings, several alternative nitrogen evaporation procedures were 

investigated. Procedural recoveries of the acid 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) temperature conditions and evaporation to near 

dryness (in-situ) solvent conversion to acetonitrile. Comparison of these approaches showed 

that the in-situ solvent conversion procedure provided the best procedural recoveries 

although all modified methods provided 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 organic solvents due to 

protonation of the carboxylic acid functional group. However, volatile losses in acidified 

matrix trials to this point had also been much greater as compared to those observed with 
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neutral and basic pre-treated matrices (reference to June 2010 Progress Report, pg. 5). With 

the revised evaporation procedure incorporated into the aqueous supernatant method, 

acceptable procedural recoveries were obtained for all acid analytes from an acidified 

aqueous matrix for the first time. 

A sludge matrix experiment was conducted to complete 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 Progress Report, pgs. 5-6 and Appendix F). In 

each of these experiments, MTBE extracts were evaporated under 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 recoveries were obtained for all analytes (suggesting volatile losses 

were minimal) and hydrolysis trends were not detected relative to observations of volatile 

and hydrolytic losses for acidic and basic pre-treatments, respectively. 

As seen in the earlier sludge trials, the M+2 PFHxA surrogate recovery standard, 

characterized by a relatively smaller perfluorinated 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 step, 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 supernatant procedures (two MTBE extractions followed by an 

ion-pairing cleanup of residual aqueous supernatant matrix) had been largely inconclusive 
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due primarily to the MTBE handling issues outlined herein. Using the in-situ solvent 

conversion procedure, an experiment was performed on untreated aqueous supernatant using 

2.5 and 5 milliliters of MTBE for each extraction. The results demonstrate that quantitative 

procedural recoveries for all acid analytes may be obtained using either MTBE extraction 

volume (Appendix D*) For volatile 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 extraction solvents (ACN, MeOH and MeOH) to be 

applied to trapping media subsequent to the initial 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 (Anasorb CSC), the binary solvent system 

ACN:MeOH provided quantitative procedural recoveries for all acid analytes and was 

marginally better than MeOH (Appendix E). None 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 matrix 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. 

Based on unacidified trial results with styrene trapping media, MeOH was selected as the 

solvent for acidification with 0.1 M HNO3 or 0.1 M formic acid. MeOH containing 0.1 M 

HNO3 provided significantly better procedural recoveries compared with MeOH containing 

0.1 M formic acid. LC/MS/MS sequences on processed MeOH:HNO3 extracts were 

characterized by significant suppression 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 available. To date, M+2 8-2 

FTCA has been used as a matrix internal standard for 7-3 Acid given the close proximity of 

7-3 Acid and M+2 8-2 FTCA chromatographic retention 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 high 
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procedural recovery (mean of 214%) with the IS). The use of lower strength nitric or 

hydrochloric acid (less oxidative), or use of an acid with a strength intermediate 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 retention time of 8-2 FTO (approx. 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 standards 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 alternative ion was still not indicated (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 shape/focusing and additional optimization of the 

methane flow rate. For purposes of the initial 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 method for those analytes for which calibration 

standards were not used/available. 

Final calibration standard levels for each of the 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 volatile 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 obtained for the majority of volatile analytes 

fortified into untreated aqueous supernatant (Appendix H) and sludge (Appendix I) SCAS 
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matrices using two MTBE extractions when a back-partition cleanup of each MTBE extract 

with polished reagent water was employed in the 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 method to be used in subsequent trials (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 aqueous 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 analytes (6-2 

FTOH, 7-2 sFTOH, 10-2 FTOH and 8-2 FTAC) required two sequential 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 continues to be seen 

in the data summaries. Evidence that the back-partition MTBE extract clean-up procedure 

was sufficiently robust was suggested by our observation 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 results 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 provided (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 opposed 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. 
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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 underway to perform all of the 

procedures as provided as a prelude to the initial pilot study. An appropriate amount of the 

study analytes will be fortified into SCAS mixed-liquor and trapping media and determined 

by LC/MS/MS or GC/MS as appropriate. In addition 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 standard of 7-2 sFTOH (previous standard was consumed), stock 

and standard preparations and all reagent preparations 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/definitive 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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Appendix A 

Invoice 
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Allocation of Costs 

Month, Year Tasks 

 Design and 

Procurement of 

SCAS Units 

(Task A) 

Acquisition 

of Standards 

(Task B) 

Adaptation of 

Analytical 

Method (Task C) 

Pilot Studies 

Task (D) 

Refinement of 

Methods 

Task (E) 

Method 

Validation

s (Task F) 

Storage 

Stability 

(Task G) 

Biodeg

dation 

Studie

(Task H

Dec 2009 $1,803 $1,085 $42,422 Jan 2010 $29,227 Feb 2010 $1,300 $36,745 Mar 2010 $14,350 Apr 2010 $570 $15,935 May 2010 $760 $71,860 June 2010 $57,870 $35,003 July 2010 $42,430 $15,130 Labor Total $1,803 $3,715 $310,839 $50,133 Materials $6,800 $10,500 $20,644 $1,724 Total Cost $8,603 $14,215 $331,483 $51,857 
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Appendix B 

Reagent Fortification Trials and Investigation of MTBE Evaporative Losses 
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Appendix C 

Analysis of Acid Analytes in Sludge by LC/MS/MS 
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Appendix D 

Analysis of Acid Analytes in Aqueous Supernatant by LC/MS/MS 
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Appendix E 

Analysis of Acid Analytes in Trapping Media by LC/MSMS 
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Appendix F 

Investigation of 802 FTO Response by GC/MS 
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Appendix G 

Representative GC/MS Calibration Curves of the Volatile Analytes 
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Appendix H 

Analysis of Volatile Analytes in Aqueous Supernatant by PCI GC/MS 
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Appendix I 

Analysis of Volatile Analytes in Sludge by PI GC/MS 
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Appendix J 

Method Outlines and Sample Preparation Forms 
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Appendix K 

Analytical Standard, Stock Solution and Reagent Preparation Information 
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