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INTERIM REPORT # 10 - Analysis of Fish and Clam Samples
STUDY TITLE Analysis o f Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur
Monitoring Program
DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792
STUDY DIRECTOR Jaisimha Kesari P.E., DEE
Weston Solutions, Inc. 1400 Weston Way
West Chester, PA 19380 Phone: 610-701-3761
INTERIM REPORT COMPLETION PATE May 09, 2006
PERFORMING LABORATORY Exygen Research
3058 Research Drive State College, PA 16801
Phone: 814-272-1039
ro
t-
STUDY SPONSOR 3M Company
3M Building 0236-01-B-10 St. Paul, MN 55144 Phone: 651-733-6374
CO ro
PROJECT Protocol Number: P0001131 Exygen Study Number: P0001131
Total Pages: 132
BEST COPY AVAILABLE
[u )A o /e . D o o u n a if j
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: POQ01131
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT
Exygen Study Number P0001131, entitled "Analysis o f Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by Exygen Research.
/ /T ? Flaherty srincipal Investigator Exygen Research
Weston Solutions, Inc.
Michael A. Santoro Sponsor Reprsentative 3M Company
Exygen Research
Date
Date ' Page 2 of 132
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Interim Report #10-Analysis of Fish and Clam Samples 1 Exygen Study No.: P0001131
QUALITY ASSURANCE STATEMENT
Exygen Research's Quality Assurance Unit reviewed Exygen Study Number P0001131, entitled, "Analysis of Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfhiorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program". All reviewed phases1 were inspected for conduct according to Exygen Research's Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported to the Exygen Principal Investigator and Management and to the Study Director.
Phase
18. Raw Data Review and Interim Analytical Report Review
26. Raw Data Review and Interim Analytical Report Review
Date Inspected
Date Reported to Date Reported to
Principal
Exygen
Investigator Management
Date Reported to
Study D irector
08/01-05/05
09/20/05
09/21/05
09/21/05
05/03/06
05/08/06
05/09/06
05/09/06
Shaffer ical Lead, Quality
ance Unit
Date
'Note: All in-lab inspections will be documented in the QA statement for the final analytical report at the conclusion of the study. This QA statement involves only the review o f the interim report and associated raw data.
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CERTIFICATION OF AUTHENTICITY
This interim report, for Exygen Study Number P0001131, is a true and complete representation o f the raw data.
Submitted by:
Exygen Research 3058 Research Drive State College, PA 16801 (814)272-1039
Principal Investigator, Exygen:
a /m John Flaherty Vice President Exygen Research
'
S '/fM Date
Exygen Research Facility Management:
Date
Study Director, Weston Solutions, Inc
JaisimhaTCesari P.E., DEE Weston Solutions, Inc. Sponsor Representative, 3M Company:
Michael A. Director o f Rdgulatory Affairs
Exygen Research
Date
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Interim Report #IO-Analysis ofFish and Clam Samples
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STUDY IDENTIFICATION
Analysis o f Perfluorobutanesulfonate (PFBS), Perfluorohexancsulfonate (PFHS), and PerQuorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur
Monitoring Program
PROTOCOL NUMBER:
P0001131
EXYGEN STUDY NUMBER: POO01131
TYPE OF STUDY:
Residue
SAMPLE MATRIX:
Fish and Clams
TEST SUBSTANCE:
Perfluorobutanesulfonate (PFBS), Perfluorohexancsulfonate (PFHS), and Perfhiorooctanesulfonate (PFOS)
SPONSOR:
3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144
STUDY DIRECTOR:
Jaisimha Kesari P.E., DEE
Weston Solutions, Inc.
1400 Weston Way
-
West Chester, PA 19380
STUDY MONITOR:
Michael A. Santoro 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144
PERFORMING LABORATORY: Exygen Research 3058 Research Drive State College, PA 16801
ANALYTICAL PHASE TIMETABLE:
Study Initiation Date:
11/05/04
Interim Analytical Start Date:
12/27/04
Interim Analytical Termination Date: 04/17/06
Interim Report Completion Date: 05/09/06
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PROJECT PERSONNEL
The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc. The following personnel from Exygen Research were associated with various phases o f this interim portion o f the study:
Name John Flaherty Karen Risha Paul Connolly Amy Sheehan Christine Edwards Brittany Kravets Mindy Cressley Krista Gallant
Scott Crain Eric Hoover Carlyle Horrell Shawn Robb Mark Ammerman Eric Edwards Edward Cams
Title Vice President Laboratory Supervisor Technical Lead-LC/MS Associate Scientist
Technician Technician Technician Technician Technician Technician Intern Technician Technical Lead - Facilities Sample Custodian Sample Custodian Sample Custodian
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TABLE OF CONTENTS
Pagg
TITLE PAGE.......................................................................................................................... 1
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT........... .................. 2
QUALITY ASSURANCE STATEMENT............................................................................3
CERTIFICATION OF AUTHENTICITY..............................
4
STUDY IDENTIFICATION.................................................................................................. 5
PROJECT PERSONNEL........................................................................................................6
TABLE OF CONTENTS........................................................................................................7
LIST OF TABLES..................................................................................................................8
LIST OF FIGURES..... ...........................................................................................................9
LIST OF APPENDICES.......................................................................................................10
1.0 SUMMARY................................................................................................................... 11
2.0 OBJECTIVE.................................................................................................................. 12
3.0 INTRODUCTION......... ....................................
13
4.0 ANALYTICAL TEST SAMPLES............................................................................. 13
5.0 REFERENCE MATERIAL................................................
13
6.0 DESCRIPTION OF ANALYTICAL METHOD..........................................................15
6.1 Extraction Procedure...................................................................................................15
6.1.1 Sample Preparation...................................................................................... 15
6.1.2 Glassware Preparation............................
15
6.1.3 Column Preparation..................................................................................... 15
6.1.4 Sample Extraction........................................................................................ 15
6.2 Preparation o f Standards and Fortification Solutions................................................ 16
6.3 Chromatography..........................................................................................................17
6.4 Instrument Sensitivity...........................................................
17
6.5 Description o f LC/MS/MS Instrument and Operating Conditions........................... 17
6.6 Quantitation and Example Calculation....................................................................... 18
7.0 EXPERIMENTAL DESIGN........................................................................................ 20
8.0 RESULTS......................................................................................................................20
9.0 CONCLUSIONS.... ..........................................
21
10.0 RETENTION OF DATA AND SAMPLES.............................................................. 21
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LIST OF TABLES
Eg
Table I. Summary o f PFBS, PFHS and PFOS in Fish Samples........................................23 Table II. Summary o f PFOS in Re-extracted Fish Samples...............................................30 Table HI. Summary o f PFBS, PFHS and PFOS in Clam Sam ples....................................32 Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Sam ples................... 33 Table V. Matrix Spike Recovery o f PFOS in Re-extracted Fish Samples........................ 46 Table VI. Matrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples..................49
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LIST OF FIGURES Figure 1. Typical Calibration Curve for PFBS in M ethanol.............................
Page ....51
Figure 2. Non-Extracted Standards o f PFBS in Methanol, 0.0005 pg/mL and 0.001 pg/mL, Respectively.................................. ........................ .....
....52
Figure 3. PFBS in Control Fish Blank, 0.00625 pg/mL Fortified Control Fish Spk A, and 0.025 pg/mL Fortified Control Fish Spk B, Respectively.............................. 53
Figure 4. Chromatogram Representing a Fish Sample Analyzed for PFBS (Exygen ID: C0049478, Data Set:061605E)...................................................54
Figure 5. Typical Calibration Curve for PFHS in M ethanol.......................................... 55
Figure 6. Non-Extracted Standards o fPFHS in Methanol, 0.0005 pg/mL and 0.001 pg/mL, Respectively............................................................................. 56
Figure 7. PFHS in Control Fish Blank, 0.00625 pg/mL Fortified Control Fish Spk A, and 0.025 pg/mL Fortified Control Fish Spk B, Respectively.............................. 57
Figure 8. Chromatogram Representing a Fish Sample Analyzed for PFHS (Exygen ID: C0049478, Data Set: 061605E)................................................ 58
Figure 9. Typical Calibration Curve for PFOS in M ethanol.......................................... 59
Figure 10. Non-Extracted Standards o f PFOS in Methanol, 0.0005 pg/mL and 0.001 pg/mL, Respectively..............................................................................60
Figure 11. PFOS in Control Fish Blank, 0.00625 pg/mL Fortified Control Fish Spk A, and
0.025 pg/mL Fortified Control Fish Spk B, Respectively.............................. 61
Figure 12. Chromatogram Representing a Fish Sample Analyzed for PFOS (Exygen ID: C0049478, Data Set:061605E).................................................. 62
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LIST OF APPENDICES
Page
Appendix A Study Protocol P0001131 (Exygen Study No. P0001131) with Analytical Method V0001783: "Method o f Analysis for the Determination o f Perfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS" Protocol Amendments 1 and 2, and Deviations 2 and 3 .................................. .................................................................................63
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1.0 SUMMARY
Exygen Research extracted and analyzed fish and clam samples for the determination of perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) according to Exygen Method V0001783 (A ppendix A).
The limit o f quantitation (LOQ) for PFBS, PFHS, and PFOS in fish and clams was 0.2 ng/g. For one sample (C0048133) only one gram o f fish was used for extraction, so the limit o f quantitation for PFBS, PFHS, and PFOS in this fish sample was 1.0 ng/g.
The initial analytical results associated with fifty-one fish samples are not reported (NR) in Table I because the endogenous levels of PFOS were too high to calculate accurate matrix spike recoveries. These samples were re-extracted and the results o f the re analyses are summarized in Tables II and V.
Analytical results and assessed accuracies for the analysis o f PFBS, PFHS and PFOS found in fish samples are summarized in Table I. Analytical results and assessed accuracies for the analysis o f PFOS found in the re-extracted fish samples are summarized in Table II. Analytical results and assessed accuracies for the analysis o f PFBS, PFHS and PFOS found in clam samples are summarized in Table III. Laboratory matrix spikes that were in the appropriate concentration range (primary concentration less than three times the spiking level) were used to calculate the assessed accuracies.
The average percent recoveries standard deviations for PFBS, PFHS, PFOS in fish samples were 79% 13%, 94% 12%, and 85% 20%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in fish samples are summarized in T able IV. The average percent recovery standard deviation for PFOS in the re-extracted fish samples was 109% 20%. Fortification recoveries for PFOS in the re-extracted fish samples are summarized in T able V. The average percent recoveries standard deviations for PFBS, PFHS, PFOS in clam samples were 84% 10%, 93% 13%, and 73% 16%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI.
The sample IDs assigned by the client follow this formula: Dxx-xO 1-xxxxxx-x-04xxxx. The first string begins with D for Decatur, Alabama and the xx defines the sampling area within the Wheeler Reservoir o f the Tennessee River where: DL3 = Up river Letter o f Intent (LOI) sampling location LOC-3 DL2 - Cross river LOI sampling location LOC-2 DL1 " Downstream Fox Creek mouth LOI sampling location LOC-1 DBC = Bakers Creek mouth DOU = Cove at 3M WWTP outfall DMC = Downstream Mallard Creek mouth
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The second string defines the general category of the biota sample and the sampling round where: FC1 = Fish sample first round 101 = Invertebrate sample first round
The third string defines the species (first two characters), the sample type (third character), and the sample number (last three characters) within that sampling area and type o f sample where: IP = channel catfish (Ictalurus punctatus) MS = largemouth bass (Micropterus salmoides) CF = Asiatic clam (CorbicuiaJluminea)
F = Filet tissue sample W = Whole body sample
001 through 005 = sample number within the sampling area and sample type
The fourth string (single character) additionally defines the sample type where: 0 Primary field sample 1 = Field duplicate sample 2 - Equipment rinseate blank sample
The fifth, string defines the sample preparation date in YYMMDD format.
Examples o f this sample ID system are:
Sample DBC-F01-EPF004-0-041021 is the filet tissue sample prepared on October 21, 2004 from the fourth channel catfish collected at the Bakers Cheek mouth sampling location.
Sample DLl-FOl -MSW002-0-041104 is the whole body sample prepared on November 4,2004 from the second largemouth bass collected at the Fox Creek mouth sampling location.
2.0 OBJECTIVE
The objective o f the analytical part o f this study was to determine levels o f perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) in fish and clams according to Protocol P0001131 (Appendix A).
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3.0 INTRODUCTION
)
This report details the results o f the analysis for the determination o f PFBS, PFHS, and
PFOS in fish and clams using the analytical methods! entitled, "V0001783: Method o f
Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by
LC/MS/MS."
' ;>?
The study was initiated on November 05, 2004, when the study director signed protocol number P0001131. The analytical start date for this interim report was December 27, 2004, and the analytical termination date for this interim report was April 17,2006.
4.0 ANALYTICAL TEST SAM PLES
Forty fish samples (Exygen ID C0048126-C0048165) were received on dry ice on October 23, 2004 from Tim Frinak at Weston Solutions, Inc. Fifty-six fish samples (Exygen ID C0049450-C0049505) were received on dry ice on November 6, 2004 from Charles Young at Weston Solutions, Inc. Twenty-six fish samples (Exygen ID C0056354-C0056479) were received on dry ice on January 13, 2005 from Tim Frinak at Weston Solutions, Inc. Six clam samples, consisting o f whole clams from each sample site (Exygen ID C0056480-C0056485) were received on dry ice on January 13, 2005 from Tim Frinak at Weston Solutions, Inc. A whole Whiting (Family: Gadidae) was purchased from a local grocer by Ed Cams on December 20, 2004 and was used as the control fish (Exygen ID C0054391). The samples were logged in by Exygen personnel and placed in frozen storage.
Sample login and chain o f custody information is located in the raw data package associated with this interim report. Storage records will be kept at Exygen Research.
5.0 REFERENCE MATERIAL
The analytical standards, PFBS and PFHS, were supplied by 3M. PFBS was received from 3M at Exygen on July 6,2000, and May, 13,2005. PFHS was received from 3M at Exygen on January, 20, 2003. PFOS was purchased from Fluka Corporation and was received at Exygen on April, 23,2003.
The available information for the reference materials is listed below. PFBS and PFHS were stored frozen and PFOS was stored refrigerated.
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Compound PFBS PFBS PFHS PFOS
Exveen Inventory No. SP0000252 SP0005726 SP0002401 SP0002694
L o t# 101 101 SE036 430180-1
Purity (%1 96.7 96.7 98.6 101.2
Expiration P 12/04/06 12/04/06 10/18/06 10/31/07
The molecular structures o f PFBS, PFHS and PFOS are given below:
PFBS Chemical Name: Perfluorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (CiFsSCVK.'1)
Transitions Monitored: 299 99 Structure:
PFHS Chemical Name: Pcrfluoiohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (C6Fi3S03*K+)
Transitions Monitored: 399 -> 80 Structure:
F F
F
FFF FFF
PFOS Chemical Name: Perfluorooctanesulfonate Molecular Weight: 538 supplied as the potassium salt (CgFnSOjTC*) Transitions Monitored: 499 -* 80 Structure:
FFFF
FFFF
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6 0 DESCRIPTION OF ANALYTICAL METHOD
The analytical method "V0001783: Method o f Analysis for the Determination o f Perfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS" was used for the fish and clam samples in this study.
6.1 Extraction Procedure
6.1.1 Sample Preparation
Before the samples could be weighed for the extraction, they had to be processed. To process, the frozen samples were placed into a food processor and homogenized with dry ice. The samples were transferred to one-gallon Ziploc bags and placed in frozen storage with bag left open to allow the dry ice to sublime. After sublimation, the sample bags were sealed and remained in frozen storage until time o f analysis. Sample processing records are located in the Sample Information section o f the raw data package.
6.1.2 Glassware Preparation
The 12S mL pear-shaped flasks were silanized by first rinsing the flask with 30% dimethyidichlorosilane in toluene solution. The flasks were rinsed once with toluene followed by three rinses with methanol. The flasks were allowed to air dry before use.
6.1.3 Column Preparation
The 20 mL columns were packed at Exygen in sequence with 2 grams flo risil, 2 gram s silica gel, 2 gram s o f carbon, and 1 gram LC -N H 2. The columns were conditioned on the day o f extraction with 20 mL o f methanol followed by 20 mL o f acetonitrile. All washes were discarded. These clean-up columns were used to remove matrix interference and not to retain PFBS, PFHS, and PFOS. Additional details about the column packing materials can be found in the raw data package associated with this report.
6.1.4 Sample Extraction
A 5-gram* portion o f fish or clam sample was weighed into a fiftym illiliter centrifuge tube for the extraction. After fortification o f appropriate samples, 30 mL o f acetonitrile was added to the samples. The samples were allowed to shake on a wrist action shaker for ~15 minutes. The samples were placed into a freezer for ~l hour. Freezing o f the
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samples allowed the fats and proteins to precipitate. The samples were centrifuged for ~10 minutes at ~2000 rpm. The supernatant was then loaded onto the conditioned clean-up column fitted inside the silanized pear shaped flask. The eluate was collected in the silanized pear-shaped flask. This process removed the fats and proteins from the extract. Ten milliliters o f acetonitrile was added to the samples left in the centrifuge tube. The remaining sample in the tube was homogenized using a tissumizer for ~30 seconds. The tissumizer was rinsed with ten milliliters o f acetonitrile. The rinse was added to the sample tube. The samples were allowed to shake on a wrist action shaker for another 10 minutes. The samples were placed into a freezer for -1 hour. The samples were centrifuged again for -10 minutes at ~2000 rpm. The supernatant was then loaded onto die same clean-up column. The eluate was collected into the same pear-shaped flask. The column was washed with 20 mL of acetonitrile, collecting the wash in the pear-shaped flask. Approximately 3 or 4 drops o f 1-octanol was added to the extracts in the flasks. The samples were evaporated using a rotary evaporator at reduced pressure. The 1-octanol held the analytes in the pear-shaped flask while the solvent evaporated. Two milliliters o f 2% ascorbic acid in methanol was added to the flasks to make final volume. The flask was swirled to dissolve and mix the sample. The sample was transferred to a HPLC vial using a disposable pipet. Each sample was analyzed by LC/MS/MS electrospray.
"'Due to lack o f sample, a one-gram portion o f sample C0048133 (DMC-F01-MSW001 0-041216) was used. All other samples were weighed out in 5-gram portions.
6.2 Preparation of Standards and Fortification Solutions
Individual stock standard solutions o f PFBS, PFHS and PFOS were prepared as specified in Exygen method V0001783. The stock standard solutions were prepared at a concentration o f 100 pg/mL by dissolving 10 mg of each o f the standards (corrected for purity and salt content) in methanol From these solutions, mixed 1.0 pg/mL fortification standard solutions were prepared by taking 1 mL o f each o f the appropriate stock solutions and bringing the volume up to 100 mL with m ethanol By taking 10 mL o f the mixed 1.0 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, a mixed 0.1 pg/mL fortification standard was prepared.
A mixed stock standard solution of PFBS, PFHS, and PFOS was also prepared. The stock standard solution was prepared at a concentration of 1000 pg/mL by dissolving 100 mg of each o f the standards (corrected for purity and salt content, if necessary) in methanol. From this solution, a 100 pg/mL fortification standard solution was prepared by taking 10 mL o f the stock and bringing the volume up to 100 mL with methanol. By talking 10 mL o f the 100 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, a 10 pg/mL fortification standard was prepared. By taking 10 mL of the 10 pg/rnL fortification standard and bringing the volume up to 100 mL with
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methanol, a 1.0 pg/mL fortification standard were prepared. By taking 10 mL o f the 1.0 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, a 0.1 pg/mL fortification standard was prepared.
A set o f non-extracted standards containing PFBS, PFHS and PFOS was prepared in methanol. The following concentrations were prepared:
Cone, o f Fort Fort
Solution
Volume
Gig/mL)1
(mL)
1.0 5.0
1.0 2.5
1.0 1.0
0.05 10
0.025
10
0.01 10
0.005
10
1o f PFBS, PFHS and PFOS
Volume o f Fortified Sample
(mL) 100 100 . 100 100 10 100 10
Final Cone, of Calibration Std.
Gig/mL)
0.05 0.025 0.01 0.005 0.0025 0.001 0.0005
The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator (4 2) when not in use. Documentation o f standard preparation is located in the raw data package associated with this interim report.
6.3 Chromatography
Quantification o f PFBS, PFHS and PFOS was accomplished by LC/MS/MS electrospray. The retention times o f PFBS, PFHS and PFOS were ~ 4.7 mins, - 10.8 mins, and ~ 12.9 mins, respectively.
6.4 Instrument Sensitivity '\
The smallest standard amount injected during the chromatographic run had a concentration o f0.0005 pg/mL o f PFBS, PFHS and PFOS.-
6.5 Description of LC/MS/MS Instrument and Operating Conditions Instrument: API 4000 Biomlecular Mass Analyzer
Interface: Turbo Ion Spray Liquid Introduction Interface
Computer: DELL OptiPlex 0X400
Software: Windows NT, Analyst 1.4.1
HPLC:
Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler
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HP Column Oven
HPLC Column: Thermo Fluophase RP, 50 mm x 2.1 mm
Column Temp.: -30 C Injection Voi.: 15 pL Mobile Phase (A): 2 mM Ammonium Acetate in water Mobile Phase (B): Methanol
Time (min) 0.0 1.0 8.0 10.0 11.0 18.0
Total run time; -18 min
Flow Rate: 0.3mL/min
%A 65 65 25 25 65 65
%B 35 35 75 75 35 35
Ions monitored:
Analvte
PFBS PFHS PFOS
Mode
negative negative negative
T u itio n M onitored 299 - 99 399-80 499 - 80
Approximate Retention Time
(min) -4.7 min. -10.8 min. -12.9 min.
6.6 Quantitation and Example Calculation
Fifteen microliters o f sample or calibration standard were injected into the LC/MS/MS. The peak area w as m easured and the standard curve w as generated (using 1/x ft w eighted linear regression) by Analyst software using six concentrations o f standards. The concentration was determined from the following equations. Equation 1 calculated the amount o f analyte found (in ng/mL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program.
Equation 1:
Analyte found (ng/mL, wet weight) " (Peak area - intercept) x DF slope
Where: DF = Dilution Factor, factor by which the final volume was diluted, if necessary.
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Equation 2 was used to convert the amount o f PFBS, PFHS and PFOS found in ng/mL to ng'g (ppb).
Equation 2:
Analyte found (ppb, wet weight) =
TAnalyte found (ng/mL) x final volume (2 mL)l sample weight (5 g)
For samples fortified with known amounts o f PFBS, PFHS and PFOS prior to extraction, Equation 3 was used to calculate the percent recovery.
Equation 3:
Recovery (%) = (analvte found (ng/mL) - analyte in control (ng/mL)) xl00% amount added (ng/mL)
Note: For the analyte recovery calculation, the "control" is the unspiked aliquot o f the primary field sample.
An example o f a calculation using an actual sample follows (calculation is for PFBS
only):
Fish sample Exygen ID: C0049478 Spk E (Set: 061605E), fortified at 10 ng/g with
where:
peak area
280750
intercept
3070
slope
13100
dilution factor
1-
ng/g PFBS added (fort level)
10
amt in corresponding sample final volume (mL)
NQ (not quantifiable) 2
sample weight (g)
5:
From equation 1: Analyte found (ng/mL, wet weight)
. = r280750 - 30701 x 1
13100
=* 21.2 ng/mL
From equation 2: Analyte found ng/g (ppb)
= 121.2 ng/mL x 2 roL) 5g
= 8.48 ng/g (ppb)
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From equation 3: % Recovery
= (8.48 ng/g - 0 ne/g) x 100% 10 ng(g
= 85 %
7.0 EXPERIMENTAL DESIGN
For fish and clam samples designated as laboratory matrix spikes, PFBS, PFHS, and PFOS were added at a known concentration to the samples in the laboratory after the samples were weighed for extraction.
The fish samples were extracted in thirty sets, five that were re-extraction sets. The clam samples were extracted in one set. Each fish or clam set included one control fish matrix blank and two control fish matrix blanks fortified at known concentrations. Two sets o f fish contained three samples, one set o f fish contained four samples, one set o f fish contained seven samples, and twenty-one sets o f fish contained five samples. Three sets o f re-extracted fish contained ten samples each. One set o f re-extracted fish contained twelve samples. One set o f re-extracted fish contained nine samples. One set o f clams contained six samples.
Accuracies were assessed for each sample by reviewing the individual QC results obtained for each sample.
8.0 RESULTS
Analytical results and assessed accuracies for the analysis o f PFBS, PFHS and PFOS found in fish samples are summarized in Table I. Please note that the chromatography for PFBS was poor for this matrix. Exygen recognizes this and great care has been taken to integrate each data set consistently. Analytical results and assessed accuracies for the analysis o f PFOS found in the re-extracted fish samples are summarized in Table II. Analytical results and assessed accuracies for the analysis o f PFBS, PFHS and PFOS found in clam samples are summarized in Table III.
The average percent recoveries standard deviations for PFBS, PFHS, PFOS in fish samples were 79% 13%, 94% 12%, and 85% 20%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in fish samples are summarized in Table IV. The average percent recovery standard deviation for PFOS in the re-extracted fish samples was 109% 20%. Fortification recoveries for PFOS in the re-extracted fish samples are summarized in Table V. The average percent recoveries standard deviations for PFBS, PFHS, PFOS in clam samples were 84% 10%, 93% 13%, and 73% 16%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI.
Exygen Research
Page 20 of 132
000263
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
9.0 CONCLUSIONS
The fish and clam samples were successfully extracted and analyzed for PFBS, PFHS and PFOS according to analytical method V0001783.
10.0 RETENTION OF DATA AND SAM PLES
All original paper data generated by Exygen Research that pertains to this interim report will be shipped to the study director. This does not include facility-specific raw data such as instrument or temperature logs. Exact copies o f all raw data, as well as a signed copy o f the final analytical report and all original facility-specific raw data, will be retained in the Exygen Research archives for the period o f time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792.
Exygen Research
Page 21 o f 132
000264
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
TABLES
Exygen Research
Page 22 o f 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS in Fish Samples (continued)
Exvaen ID
C0048144 C0048144 Rep
C0048145 C0048145 Rep
C0048146 C0048146 Rep
C0048147 C004fi147 Rep
C0048148 C0048148 Rep
C0048149 C0048149 Rep
C0048150 C0048150 Rep
CO048151 C0048151 Rep
C0048192 C00481S2 Rep
C0048153 00048153 Rep
C0048154 C0048154 Rep
C0048156 C0048155 Rep
C0048156 C004S168 Rep
C0048157 C0048157 Rep
00048158 C0048158 Rep
C004815 C0048159RSP
C0048100 C0048160 Rep
C 004 8I81 C0048161 Rep
C0048182 C0048182Rep
O ient Samo! ID
C4 Sulfonate PFBS PMdiorotlwten--udonat
Analyte Asseesed Found Accuracy (no} wetm . (+*-%)
C6 Sulfonate PFHS Petllwratiamin aultenrt
A n a lyte Found
Aseessed A ccu ra cy
(rtfliWwetwi ( * - * )
C l Sulfonate PFOS PirHnrooctm--uKonrt*
A n a lyte Found (NMleMWI.
Aueesed Accuracy
(*% >
DL1-F01-IPF001-0-041021
0.432
30
0.201
30
33.4
40
D L1-F01-IP F0014M )41021`
0.428
30
0.2S2
30
32.0
40
O L3-F0M PF0034M UI021
0.448
30
ND
30 3.55 30
DL3-F01-IPF003-0-041021 *
0.440
30
0.226
30
3.36
30
D I3-F 01-IP F 004-04>41021
0.784
40
NO
30 0.362 30
D L3-F 01-IP F 004-0-041021*
O.fiOO
40
ND
30 0.230 30
D L3 -F 0 1 -IP F 0 0 5 0 -0 4 I0 2 1 DL3-F01 -IPF005-0441021 *
DBOF01-PF0014M H1021 DBC-F014PF0014>-041021*
1.63 1.07
1.34 1.30
60 NO 30 60 NO 30
50 0.692 30 50 0.660 30
5.48 40 5.64 40
NR NR NR NR
DBC-F01-tPF002*0"041021
1.43
50
NO
30
110
30
D B C -F 0U P F 0 02-0-O 4 102 1"
0.756
60
ND
30
109
30
DBC-F01-IPFD03-0-041021
0.606
60
0.644
30
NR
NR
D0C-FO1 -IPF003-04M1021 *
0.652
50
0.624
30
NR
NR
P 8C -F01-FW 001-0-041021
0.864
40
2.21
30
NR
NR
DBC-F01-IPWQO1-04)410214 0.508
40
2.20
30
NR
NR
DBC-FO1-IPW 0024)4)41021 DBC-F01-IPW 002-0-041021*
0.700 0.736
40 40
9.12 8.86
30 30
NR NR NR NR
D 6C -F01-PW 00341-041021
0.736
30
6.76
30
NR NR
OBC-F01-IPW 003-0-041021*
0.760
30
7.44
30
NR
NR
D O U -F01-IPF001-04M 1021
4.36
40
1.02 30
NR
NR
D O U -F 01-IP F 0014M )41021*
4.24
40 0.972
30
NR
NR
DO U-F01-IPF002-0-041021
6.76
40 0.792
30
NR
NR
D O U -F 01-IP F 002 -0-0 410 2 1 *
828
40 0.720
30
NR
NR
D O U -F 01-IP F 003 0-04 102 1 DOU-F01-IPF0Q3-O4)41021*
DOU-F01-IPF004-0-041021 D O U -F01-1P F 00 4-0 -041021*
DOL)-F1-lPF00S4)-O41021 DOU-F01 -IPF0054W)41021*
5.88 6.66
6.12 0.28
4.56 4.36
40 1.02 40 1.02
30 2.30 30 2.36
30 0.998 30 0.382
30 30
30 30
30 30
NR NR NR NR
NR NR NR NR
NR NR NR NR
DOU-FOI-IPW 0014)4)41021
2.89
30 0.948
30
NR
NR
DOU-F01-IPW 0014)4)41021 '
2.81
30 0.964 30
NR NR
DOU-FOI-IPW 002-0-041021
16.4
50
3.69
30
NR NR
DO U-F01-IPW 002-C-Q 41021*
16.3
50
3.70 30
NR
NR
D L2-F 01-M SW 001-04)41021
0203
30
NO
30
120 50
D L2-F01-M SW 0014H )4102r
ND
30
NO
30
120
50
D L2-F01-M SW 002-0-041021
NO
30
ND
30
102 30
D L2-F01-M SW 002-04141021*
NO
30
ND
30
100 30
"Laboratory Dupflcste NO 3 Not detected at o r above Lim it o f Quantitation which is 0.2 ng/g (wet weight). NR Not reported due to quality control meult failure.
Exygen Research
Page 24 of 132
000266
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS in Fish Sam ples
ExMwnID
Client Sample ID
C4 Sulfonate PFBS Pa fc i wht e n w fcw li Analyte Ataeased
Found Accuracy
<*/-*>
Cfi Sulfonate PFHS
t e j ua t t e i i i w inM li Analyte Aaaeasad Found Accuracy fhofetnetat. < *-*)
C0048126 C0Q48128 Rep
DL3-F01-IPF001-0-041021 DL3-F01-IPF001-0-041021*
C0048127 C0046127 Rep
DI3^01-IPF002-0041021 DL3-F01-PF002-0-041021*
C004812B
DMC-F01-IPF001-0041021
C0048128Rep DMC-F01-IPF001-0-041021*
C0048129
DMC-F01-IPF002-0-041021
C004612B Rap DMC-F014PF002-0-041021*
C0048130 C0048130 Rap
CD048131 C0048131 Rep
DMC-F01-IPW001-0-041021 OMC-FOUPWOCI-0-041021*
DMC-F014PW0024HM1O21 DMC-F01-IPW002-0-041021`
C0048132
DWC-F01-MSW001-0-041021
C0048132 Rap DMC-F01-M8W001-0-041021*
C0048133* DMC-F91-MSW002-0-041021 C0048133 Rep* DMC-F01-MSW002-0-041021*
C0048134 C0048134ROP
C004813S C0048139 Rap
C0048136 CC048138 Rep
C0O48137 C0046137 Rep
DL2-F01-IPF001-0-041021 DU-F01-IPF001-0-041021*
DL2-F01-IPF002-0-041021 DL2-F01-IPFD02-0-041021*
DL2-FC14PF003-0-041021 DL2-F01-IPF003-0-041021*
DL2-F014PF004-0-041021 DL2-F01-IPF004-0-041021
C0048138 C0048138 Rap
DL2-F01-IPFOOS-0-041021 DL2-F01-IPF005-0-Q41021*
C004813B C004B130 Rep
C0048140 C0Q48140 Rap
DL2-F01-IPW001-0-041021 DL2-F01-IPW001-0-041021*
DL2-F01-MSF001-0-041021 DL2-F01-M8F001-0-041021*
C004B141 C0048141 Rap
C0048142 C0048142 Rep
C0048143 C0048143 Rap
DL2-F01-M6F002-0-0410B1 DL2-F01-MSF002-0-041021*
DL2-F01-MSF003-0-041021 DL2-F01-MSF003-0041021*
DL2-F01-MSF004^041021 DL2-F01-MSF004-0-041021*
0.309 0.316
0.266 0.3B2
0.330 0.366
0.712 0.7B2
1.08 1.06
0.088 1.34
0.218 0.202
HD* . ND*
0.660 1.00
0.816 0-B52
0.247 0.216
0.346 0.330
0.336 0.318
0.326 0.400
0.333 0.348
0.408 0.308
0.416 0.376
0.345 0.349
40 40
40 40
SO 50
30 30
40 40
50 so
30 30
30 30
50 50
50 50
30 30
40 40
40 40
30 30
30
30
40 40
40 40
30 30
ND ND
NO ND
ND ND
ND ND
NO 0.297
ND ND
0.524 0.484
ND* ND*
ND NO
ND ND
ND NO
ND ND
ND ND
ND ND
ND ND
ND ND
ND NO
ND ND
30 30
30 30
SO 50
30 30
30 30
30 30
30 30
30 30
40 40
40 40
30 30
30 30
30 30
30 30
30 30
30 30
40 40
30 30
Ca Sulfonate PFOS Pwtluoffoactein nltenati Analyte Aaaaaaed
Found Accuracy <w-%>
5.16 30 5.64 30
4.16 40 4.S0 40
7.40 50 8.36 50
14.1 50 17.0 50
70.0 40 56.4 40
34.4 30 34.2 30
270 30 280 30
530 30 S48 30
3.45 50 2.86 50
4.72 50 6.04 50
2.01 30 2.08 30
4.52 40 4.12 40
2.45 30 2.80 30
5.88 30
8.12 30 77.2 30
67.6 30
94.8 40 98.4 40
41.6 40 40.0 40
83.6 30 83.2 30
"Laboratory Duplicate *1 .0 of eampte uaad ter traction Inateed of8.0 p.
ND b Not detected at or aoova Limit of Quantitation trtiich la 0.2 ng/g (wat weight).
HD* - Not detected at or above Urn* of Quantltetton which la 1.0 rV Q (w weight).
NR Not reported dua to quteky contra! raauKMuraa.
Exygen Research
Page 23 o f 132
OO0
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS PFHS and PFOS in Fish Sam ples (continued)
Exvoer io
C lient Sample ID
C4 Sulfonate PFBS Faifliiejoeutaaaeulfaiata
Analyte * Aateaaed . Found Accuracy hotel w mm. <+A%)
C6 Sulfenate P F H I P fim o X a iia n -- atonal
Analyte Aieeeeed Found Accuracy
C l Sulfonate PFOS
Partluofoocym--ntoqaU
A n a lyto Found
Am sd Accuracy
(n tfa )w a ittt.
C0046163 C0048163 Rep
C0048164 C0048164 Rep
C0048165 C0048165 Rep
00049450 C0049450 Rep
C0049451 C0049451 Rep
00049452 00049452 Rep
C0049453 C0049453 Rep
C0049454 C0049454 Rep
C0049456 C0048455 Rep
C0049456 00049456 Rep
CC049457 00049457 Rep
C0049458 00049458 Rep
00049459 C00494S9 Rep
C0049460 C0046460 Rep
00049861 C004946I Rep
C0049482 C0049462 Rep
C0049463 C0049453 Rep
C0049484 00049464 Rep
C0049485 C004465 Rep
DL2-F01-M SW 003-0-041Q 21 DL2-F01-MSW 003-0-041021*
DL2-F01-MSW 004-0-041021 DL2-F01-MSW 004-0-041021*
DL2-F01-MSW 005-0-041021 D L2-F01-M SW 005-0-04102r
DBC-F01-MSW 0OI-O-041104 OBC-F01-MSW 001-0-041104*
DBC-F01-MSW 002-0-041104 DBC-F01-M 6W 002-0-041104*
DBC-F01-MSW 003-0-041104 DBC-F01-MSW 003-0-041104*
DBC-F01-USW 004-0-041104 DBC-F01-MSW 004-0-041104*
DBC-F01-MSW 005-0-041104 DBC-F01-M 8W 005-0-041104*
D B C -F01-M S F001-0-041104 DBC-fO1-M SF001-0-041104*
aaC-FOl-MSF002-04)4t104
DC-F01-MS F002-0-041104'
D B C -F 0 1 -IP F 0 0 4 -0 -0 4 1 104 D B C -F 0 1 -P F 0 0 4 -0 -0 4 1 1 0 4 *
DBC-F01-IPF0064H141104 D B C -F 01 -IP F 0 05-0 -04 1104*
D6C-F01IPW004-0-041104
DBC-F01-IPW 004-0-041104*
DBC-F01-IPW 005-0-041104 DBC-F01 - I PWOOS4J-041104*
DOU-F01-IPW 003-0-041104 DOU-F01-IPW 003-0-041104*
DOU-F01-IPW 0040-041104 DOU-F01-IPW 004-0-041104*
DOU-F01-IPW 005-0-041104 D O U -FQ 1-1PW 005-0-041104*
OL2-F01-IPW 002-0-041104 DL2-F01-IPW 002-0-041104*
DL1-F01-MSW 0014MM1104 OL1-F01-M SW 001-0-041104*
ND NO
ND ND
ND ND
0.888 0.852
0.866 0,864
0.880 0.784
0.684 0.880
0.832 0.832
0.820 0.786
0.786 0.780
0.504 0.520
ino
1.84
0.484 ,0 .4 4 4
0.572 0.532
M2 ,3.05
. 3.46
3.11
; 2.97 290
1.04 0.960
190 1.24
30 .
ND.
30
92.4
30 ND 30 91.8
30 NO 30 66.0 30 NO 30 94.8
30 NO 30 168 30 ND 30 174
30 8.32 30 , . 6.32
30 3.43 *>. 3.35
30 . 3.62 30 3.64
30 30
30 30
30 30
NR NR
NR NR
NR NR
30 9.72 30 NR 30 9 9 0 30 NR
30 Z 7 7 30 . 2.66
30 3,58 30 9 4 6
30 30
30 30
NR NR
NR NR
30 1.94 30 .1 .9 0
30 30
NR NR
30
0.584 ,
30
30 0.540 30.
142 152
30 2.16 30 , NR
30 2.18 30
NR
30 30 ,
3.26 3.28
30 , 30
. 2.10 2.10
30 ,, 30 ;
30 30
NR NR
NR NR
30 6.00 30 NR 30 5.92 30 NR
30 7.12 30 NR 30 8.84 30 NR
30 5.12 30 NR 30 5.32 30 NR
30 ND. 30 8.20 30 ND 30 6.60
30 0.896 30 30 0.932 30
NR NR
30 30
30 30
30 30
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
30 30
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
40 40
NR NR
Dupflofh NO * Not O etocM a t o r abova Lim it o f Q uanttationuM ch it 0.2 n g /g(vw t weight). NR NM ipoitad dua to duality control nauK tauraa
Exygen Research *f i
Page 25 of 132
000268
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: POOG1131
Table 1. Summary o f PFBS, PFHS and PFOS in Fish Sam ples (continued)
Exvoen 10
C0049466 C0049468 Rep
C0049487 C0049437 Rap
C0O49466 C004Q488 Rap
00049469 C004B469 Rap
C0049470 C0049470 Rap
C0049471 C0049471 Rep
C0049472 00049472 Rep
C0049473 C0049473 Rep
00049474 C0049474 Rep
C004947S C0049475 Rap
C0049476 00049476 Rep
C0049477 C0049477 Rap
00049478 00049478 Rep
C0049479 C0049479 Rep
C0049480 00049480 Rep
C0049481 C00494G1 Rep
C0049482 C0049482 Rep
C0049483 C0049483Rep
C0049484 C0049484 Rep
C M nt Sam oa 10
C4 Sulfonate PFBS rifluorohyaim im an
A ntiyte Assessed Pound Accuracy ffUArtwatwL M M
DU-F01-M SW O0S4M H1104 DL1-F01-MSW 002-0-041104*
DL1-F01-MSW 003-0-041104 DL1-F01*M 8W 003-0-041104*
DL1-F01-MSW 004-0-041104 DL1-F01 -MSWOO+O-041104*
DL1-F01-MSW 0054HM1104 DL1-F01-MSW 005-0-041104*
DL1-F01-MSFCOt-0-041104 DL1-F 01-M SF001-0-041104*
D L1-F01-M S F002-0-041104 DU-F01-M SF002-0-041104*
OL1-FQ1-MSF003-0-041104 C X .1-F01-M 8F003-04M 1104*
D L1-F01-M S F004-0-041104 D L1-F 0 1 4 4 6 F 0 0 4 -0 -0 4 1 104*
DU -F01-M 8F005<W 41104 D L1-F01-M S F005-0-041104*
0L1 -F01-IPW 001-0-041104 DL1-F01-IPW 001-0-041104*
0(.1*F01*PW 002*0-041104 DL1-F014PW 002-0-041104*
DL1-F01-IPW 003-0-041104 DL1-F01-IPW 0U3-0-041104*
DL1-F01-IPW 004-0-041104 DL1-FOHPW 004-0-041104*
DL1-F01-IPF002-0-041104 D L1-70H PF002-0-041104*
DL-1-F014PF003-0-041104 D L-1-F01-IP F O O M -O 41104*
D L-1*F0M P F004<0-041104 D L-1 -F 0 1 -IP F 0 0 4 -0 -0 4 1 104*
DU-1-F014PF00S-O-O41104 DL-1-F01-IPF005-0-041104*
DL3-F01-M 8W 001-0-04I105 DL3-F01-MSW 001-0-041105*
DL3-F01-MSW 002-0-041105 DL3-F01448W 002-0-041105*
1.30 1.15
0.560 0.528
1.22 1,12
1.22 1.20
ND NO
NO NO
0203 NO
NO NO
NO ND
0.772 0.870
0.468 0.472
ND NO
NO NO
NO ND
ND NO
NO ND
M3 NO
NO ND
ND NO
30 30
30 30
30 30
30 3C
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
CSSuVonat* PFHS Perthnrnh Mrsw uO asols
A nalyte Found
Assessed A c c u ra c y
MMM
C l Sulfonate PFOS Psrils--nnrMn--ultanati
Analyte Assessed Found Accuracy to rt) wetwi. MMW
1.72 1.54
1.13 1.14
0.908 0.880
1.18 1.18
0.315 0.29
0.624 0.804
0.652 0.676
0.532 0.836
0.684 0.544
0.556 0.744
0636 0.616
0209 0.247
0238 0246
0222 0247
0266 0262
ND ND
0273 0.366
ND ND
NO NO
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
NR NR
NR NR
161 166
NR NR
293 307
NR NR
NR NR
NR NR
NR NR
17.4 18.9
15.7 15.6
9.36 9.52
59.6 572
11.1 11.2
20.9 21.4
7.60 7.36
8.72 B.56
136 137
180 162
NR NR
NR NR
30 30
NR NR
30 30
NR NR
NR NR
NR NR
NR NR
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
` Laboratory DupdcMa NO b N ot detected at o r above Lim it o f Q uanltatlon which Is 0.2 ng/g (w et weight). NR Not raprated due to quality control m u lt failures,
Exygen Research
Page 26 o f 132
Interim Report #10-Ana]yis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table 1. Sum m ary o f FFBS, PFHS and PFOS in Fish Sam ples (continued)
E xvoenlD
C lie n t S sm plelD
C4 Sulfonate PFBS Peituoreliutw eultoin l
Analyte Aeeassed Found Accuracy
<+/-*>
CIS Sulfonata PFHS p--a u>ronw urron--
A n a lyla . Found
Aaaaaaad A c c u ra c y
(-% >
CS Sulfonate PF08 PirTHtorooc<xi--Mapmia
Analyte Aaaeawd Found Accuracy (ola)wetil. ( iA l
00040495
DL3-F01-M 8W 003-0-041105
ND
30
ND
30
148 30
00040485 Rap DL3-F01-MSW003-G-041105*
ND
30
ND
30
144 30
C0049469
DL3-F01-M 8W 004-0-04110S
ND
30 0.285 30
198
X
00049486 Rep DL3-F01-MSWC04-0-041105'
ND
30 0.282 30
199
X
CO04O487
DL3-F01-M 5W 005-0-041105
ND
30 0.366 30
173
X
00040487 Rap DL3-F01-M5W 005-0-041106*
ND
30 0.341
30
168
X
C0049488
D L3-F01-M S F001-0-041105
NO
30
ND
30
116 X
C0O49488Rap DL3-F01-MSF001-0-041105*
ND
30
ND
30
115 X
C0049489
DL3-F01-M 8F002-0-441105
ND
30
ND
30
118 X
C0040488 Rap DL3-F01-M 5F002-0-041105*
ND
30
ND
30
in
X
00048490
D LS -F01-M 3F003-0-041105
ND
30
ND
30 75.6 X
C0048490 Rap DU3-F01-MSFQ03-0-0411057
ND
30
ND
30 72.0 X
C0040491
D L3-F01-M S F004-0-041106
ND
30
ND
30 130 X
C0049401 Rap DL3-F01-MSF004-0-041106*
ND
30
ND
30
134 X
C0049492
DL3-F01-W SF005-0-041105
ND
30
ND
30 81.6 X
00048492 Rap DL3-F01-MSF006-0-041105*
NO
30
ND
30 83.6 X
C0049483 C00484B3 Rap
DMC-F01- IPW 003-0-041105 DMC-F01 -tPW 003-0-041105*
ND ND
30 0.386 30 e u
30 0.334 30
63.6
X X
C0049484
DMC-F01-IPW 004-0-041106
0.300
30
0.396
30
88.8
X
C0048484 Rap DMC-F01-IPW 004-0-041105*
0.345
30
0.464
30
696
X
C0048495 CO049405 Rap
DM C-F01-IPW 00M HJ41105 DMC-F01-IPW 005-0-041105*
ND ND
30 0.270 30 30 0-255 30
64.4 82.6
X X
C0049480
DMO-F01-M SW 003-0-041105
ND
30 0.592 30
354
X
C0049406 Rap DMC-F01-MSW 003-0-041105*
ND
30 0.560 30
330
X
C0Q49497
DMC-F01-MSW 004-0-041105 0.318
30
1.90
30
258
X
C0049497Rap DMC-F01-MSWOO4-0-041105* 0.233
30
1.88 30
269
X
C0049488
DM OF01-M SW 005-0-041105
ND
30 0.980
30
NR
NR
C 0040406Rp DMC-F01-MSW 005-0-041105*
ND
30 0.936 30
NR
NR
G0048490 C0049498 Rap
CC04BS00 C0049500 Rap
00048501 C0040501Rap
DMC-FOI-M6F002-0-041 05 OMC-F01-MSF02-0-041105*
DMC-F01-MSFOO3-0-041 05 D M C -F01-M S F003-0-041105*
D M C -F 01-M S F004-0-041105 MC-F01-M SF004-0-041105*
ND ND
ND ND
NO ND
30 NO 30 30 0.367 30
30 ND 30 30 NO 30
30 0.254 30 30 0.228 30
NR NR NR NR
588 40 66.0 40
116 X 119 X
C0048502 C0048502 Rap
00049503 C0049603 Rep
D M C -F 01-M S F005-0-041105 D M C -F01-M S F 005-0-041105*
D M C -F 01-IP F 003-0-041105 UM C-F0W PF003-0-04 105*
ND ND
ND ND
30 0.420 30 30 0.448 30
146 X
147 X
30 ND 30 7.92 X
30 ND 30 7.92 X
'Laboratory DupHcM ND * Not detected a t orabova Lim it o f Q uantitalon which i t 0.2 ng/g (wet weight).
NR Not n p o rM dua k>quaMy oontral nuuK M b)*.
Exygen Research
Page 27 of 132
000270
Interim Report #10-Analysis o f Fish and Clam Samples
Exygcn Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS in Fish Sam ples (continued)
Exvoen ID
C0049504 C0049504 Rep
C0049S05 COM9505 Rep
C0056354 C0056354 RSp
00066466 C005645SRep
COOSA456 C0056466 Rep
C00S64S7 00050457 Rap
C0066458 00050456 Rep
C006645S 00066450 Rep
C00S6460 C0056460Rep
C0056461 C0056461 Rap
COO58402 COO56462 Rep
C0066463 00056463 Rep
00056464 C00564B4 Rap
C005645 COO56465 Rep
COO56406 C0056466 Rep
C0056497 COO58467 Rep
C0056466 C005B466 Rap
C00S64S9 C0056460Rep
C00S6470 COO56470 Rep
C lient Samoie ID
DMC-F01-1PF004-0-041105 DMC-FOHPF004-0-041 IDS*
DM C4=014PF0054W )41105 DM C-F01-IPF005-0-04t 105*
D L2-F01-M 8F005-0-041216 DL2-F01-MSF00&O-041216*
DL2-F01-PW Q06-0-041216 D L2-F014PA0054XM 1215*
DOU-FOI-MSW 002-0-041216 DOU-F01-M6W 002-0-041216*
DL2-F01-IPW 004-0-041215 DU-F01-IPW 004-0-041215`
DOU-F01-MSW 003-0-041216 DOU-FOf-MSW 003-04M1216'
DL3-F01-IPW 004-0-041130 DL3-F01-IPW 004-0-041130*
DOU-F01 -M 6W 001-0-041216 DOU-PD1-MSW001-04)41216*
OOU-FO1-MSWO4-0-041216 DOU-F01-MSW 004-0-W 1216*
OOU-F01-M8W 005-04M1218 DOU-F01 -MSW0054W)41216*
D O U -F01-M SF005-0-041216 D O U -F01-M SF005-0-041216`
DL3-F014PW 002-04H1130 DL3-F014PW 002-04)41130*
D L3-F01-1PW 003-0-041130 DL3-F01-IPW 003-0-041130*
D O U -F014U S F0034KM 1216 D O U -F01-M SF003-0-041216*
D B C -F01-M 8F006-14)41216 D 6C -F 01-M S F005-1-041216*
DBC-FO1-MSF0O&4KI41216 D B C -F01-M S F006-0-041216*
D O U -P 01-M S F002-0-041216 0O U -F01-M S F002-0-041210*
DL3-F014PW 001-04M1130 D L3-FQ 1-IPW 001-0 -041 130 *
C4 Sulfonate PFBS arflyergbutariMiifftwurti Analyte Asooiasd Found Accuracy
ND ND
NO ND
NO ND
NO NO
0.206 0.227
ND ND
ND NO
ND ND
7.08 7.12
4.72 4.66
0.364 0.36
1.41 1.43
ND ND
ND ND
1.72 1.73
0.220 ND
ND ND
0.688 0.872
ND ND
30 30
30 30
30 30
30 30
40 40
30 30
30 30
30 30
30 30
40 40
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
C6 Strifonate PFHS Parfteofoh-- nm iHbnate Analyte Assessed
Found Accuracy
CS Sulfonate PFOS Pyfluorooctta-- tfpnati
A n a lyte Found
Assessed A ccura cy
<no4)alvit < + /-*]
ND 30 44.0 30 ND 30 43.6 30
ND 30 46.4 30 ND 30 46.0 30
ND 30 49.2 30 ND 30 51.6 30
ND 30 13.2 30 ND 30 13.3 30
1.72 30 NR NR 1.70 30 NR NR
ND 30 6.80 30 ND 30 8 80 30
10.4 30 NR NR 10.6 30 NR NR
ND 30 7.02 30 ND 30 7.62 30
15.4 30 NR NR 14.2 30 NR NR
21.7 30 NR NR 22.5 30 NR NR
1.34 30 NR NR 1.41 30 NR NR
8.40 30 NR NR 6.44 30 NR NR
NO 30 12.0 50 ND 30 11.5 SO
ND 30 6.44 40 ND 30 52 8 40
6.56 30 NR NR 6.68 30 NR NR
1.7 1.76
30 30
NR NR NR NR
1.56 1.60
4.56 4.56
0.246 0.21
30 30
30 30
30 30
NR NR
NR NR
0.04 620
NR NR
NR NR
30 30
Labcmtofy Duplicate NO Not detected a t o r above Lim it o f Quantitafon vvtildi Is 0.2 ngfg ("e t weight). NR = Not reported duo to quteky control result tenure.
Exygen Research
Page 28 o f 132
000271
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS in Fish Sam ples (continued)
Exw en 10
C0058471 C0O56471 Rep
C0056472 C0056472 Rep
C0056473 C0056473 Rap
C0056474 C006S474 Rep
C005347B COO56475 Rep
C006647B COO56476 Rep
C0056477 C0Q36477Rep
C0056478 COO56478 Rep
COO56479 C0056479 Rep
C lient Semple ID
C4 Sulfonate PFBB N sflu orobtMan irBanato
Analyte Assessed Found Accuracy (noADtMtwi (/-,)
ce Sulfonate PFtiS
Analyte Assessed Found Accuracy (noUKmlwt.
DOU-FO1-USF002-14M 1218 D O U -F01-M SF002-1-04121S *
0.840 0.830
30 30
4.68 4.72
30 30
D O U -FO I-M S F0Q 4-0-041213 DOU-F01-M SF004-0-041216'
0.792 0.813
30 30
2.35 2.22
40 40
D O U -F01-M SF001-0-041213
Z18
30
10.9
30
D O U -FO 1-M SF001-0-041216*
2.28
30
10.7
30
DBC-F01-MSFOQS-0-O41216 D B C -F01-M S F003-0-041216'
ND ND
30 Z 0 9 30 2.00
30 30
D B C -F01-M S F004-0-041216
ND
30
187
30
DBC-F01-M SF004O-041216*
ND
30
177
30
D M C -F 01-M S F001-0-04I21B DMC-F01-MSF001 -0-041213*
ND ND
30 0.420 30 30 0.456 3 0
DL1-F01-IPW 005-0-041216
0.2S3
30
0.344
30
OL1-F01-IPW 0054J-04I21B*
0.249
30
0.344
SO
DL2-F01-IPW 003-0-041201
ND
30
ND
30
DL2-F01-IPW 033-0-041201*
NO
30
ND
30
DU-F01-IPW 005-0-041201
ND
30
ND
30
DU3-F01-IPW 005-0-041201*
ND
30
ND
30
C l Sulfonate PFOS
Analyta Found
Assosaod Accuracy
</- %i
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
38.8 67.6
7.48 7.44
4.68 4.72
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
30 30
40 40
30 30
`Laboratory Dupiltiato ND Not detected a t o r above Lim it o f Quantitation w hich Is 0.2 ng/g (wot welpht).
NR Not mpoftsd due to quality control rnj failures.
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Page 29 o f 132
000272
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table II. Summary o f PFOS in Re-extracted Fish Samples
E x v m n ID C0048151 C00481S2 C0048153 C0046154 C004815S C0048158 C0048160 C0049450 C0049451 C 0049452 C0049453 C 0049454 C 0049455 C0049456 C 0040456 C 0049459 C 0049460 C0049461 COO49402 C 0049463 C0W 946S C0049466 C0049467 C 0049469 C0049471 C0049472
C lient S am ple 10 D B C -F01-IP W 001-0-041021 D B C -F01-IP W 002-0-041021 D B C -F01-1P W 003-0-041021 D O U -P 01-IP F001-0-041021 D O U -F01-IP F002-0-041021 DO U-F01-IPFQ 05-C -041021 D O U -F01-IPW 0Q 2-0-041021 D B C -F01-M S W G 01-0-041104 0 BC-F01 -M S W 002-0-041104 D B C -F01-M 3W 003-0-041104 D B C -F01-M S W 004-0-041104 D B C -F01-M S W 005-0-041104 D B C -F01-M S F001-0-041104 O B C -F01-M S F002-0-041104 D B C -F 01-IP F 005-0-041104 D B C -F01-IP W 004-0-C 41104 D B C -F 01-IP W 005-0-041104 D O U -F01-IPW G 03-0-041104 D O U -F 01-1PW 004-0-Q 41104 D O U-F01 -IPW GG5-0-041104 D L1-F01-M S W 001-0-041104 D L1-F01-M S W 002-0-041104 D L1-F01-M S W 003-0-041104 D L1-F01-M S W 005-0-041104 D L1-F01-M S F002-0-041104 D L1-F01-M S F003-0-041104
NR Not reported due to quality control result failures.
Exygen Research
CS Sulfonate PFOS
Pr1luorooc*anMiilfo<Mt*
A n a lyte Found
Assessed
(nfliB) WstWalght
A ccu ra cy <+/-% )
2080 3330 1660 506 636 644 1210 0480 7520 12800 3440 5240 5240 4760 808 1230 2620 NR 1740 2130 968 708 QgQ 604 568 432
30 30 90 30 30 30 40 40 30 30 30 30 30 30 30 40 30 NR 30 30 30 30 30 30 30 30
Page 30 of 132
000273
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study N o.: P0001131
Table IL Summary o f FFOS in R e-extracted Fish Sam ples (continued)
Exyoen ID C0049474 C0049498 C0049499 C0056456 COC56458 COO56460 COC56461 COO56462 COC56463 C00564M C0056467 C0056466 CC056469 00056471 C0056472 C0056473 C0056474 CC056475 C0056476 C0O48148 C0048150 C0048156 C0048157 C0048159 C0049473
Client Sample ID DL1-F01-MSF005-0-041104 DMC-F01-MSW005-0-041105 DMC-F01-MSF002-0-041105 DOU-FO1-MSWO02-O-O41216 DOU-F01-MSW003-<WM1216 DOU-F01-M8WQ01-0-041216 DOU-FQ1-MSW004-0-041216 DOU-F01-MSW005-0-041216 OOU-F01-MSF005-0-041216 DOU-F01-MSF003-0-041216 DBC-F01-MSF005-1-041216 DBC-F01-MSF005-0-041216 DOU-F01-MSF002-0-041216 DOU-F01-MSF002-1-041216 DOU-F01-MSF004-0-041216 DOU-F01-MSF001-0-041216 : DBC-F01-MSF003-0-041216 DBC-F01-MSF004-0-041210 DMC-F01-MSF001-0-041216 DBC-F01-IPF001-0-041021 DBC-F01-IPF003-0-041021 DOU-F01-IPF003-0-041021 DO-F01-IPF004-0-041021 DOU-F01-IPW001-0-041021 DL1-F01-MSF004-0-041104
COSulfonate PFOS
Analyte Found ftmfa)WatW alt**
Aseeeeed Accuracy (*/%)
740 30
560 30
620 30
26200
60
4040 30
NR NR
5120 30
496 30
720 30
848 30
NR NR
8960 SO
640 30
692 30
1820 30
2070 30
4640 30
9280 50
840 30
384 30
293 30
359 30
424 30
387 30
348 30
NR * Not reported due to quality oontrol result failures.
Exygen Research
t
Page 31 of 132
000274
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table III. Sum m ary o f PFBS, PFHS and PFOS in Clam Sam ples
Exvoen ID
d a te
Sam ple ID
C4 Sulfonate PFBS `riluoroftiitin--Wann
A nalyte Aeeeecad Found A ccuracy
(natalwet wt. (+/%>
C Sulfonate PFHS Peretforohexanemilfonete
A nalyte Aeasseed
Found
A ccuracy
(natal netwt. <+/-*)
C l Sulfonate PFOS PerfluotpoetnuMbnati
A nalyte A seatead Found A ccuracy
(nota)wet wt. </%)
C0056480
OL3-I01-CFW 001-0-041216
NO
40
ND
40 1.82 50
C0056480 Rap D L3-I01-C FW 001-0-041216*
ND
40
ND
40
1.82
50
C0056481 DMC-101-CFW 001-0 0412 16
ND
30
ND
30 6.18 50
C0066481 Rap O M C -KH -C FW 001-0041216*
ND
30
ND
30 6.12 50
C0056482
DL2-I01-C FW 001-0-041216
ND
30
ND
30
1.81
50
C 00S M 82 Rap D L2-I01-C FW 001-0-041216*
ND
30
ND
30
1.77
SO
C00S6483 D BC -I01-C FW 001-0041215
ND
30
ND
30 4.48 30
COOS6483 Rep D B C -I01-C FW 001-0041215*
NO
30
ND
30 4.44 30
COOS8484
D L1-I01-C FW 001-0-041215
NO
30
NO
30 8.80 40
COOS8484 Rep D L1-I01-C FW 001-0041218*
ND
30
ND
30 8.84 40
C00S6485 DOLM01-CFW 001 -0-041216 C0056485 Rap D O U -W 1-C FW 001-0041216*
ND ND
30 0.202 30 30 0.20S 30
11.4 10.9
50 50
la b o ra to ry Duplicate NO ' N ot de tected a t o f above L im it o f Q uantitation w hich la 0.2 ngAl (w et w eight).
Exygen Research
Page 32 of 132
000275
p. 33
Interim Report #10-Analysis o f Fish and Clam Samples ,
Exygen Study No.: P000I131
Table IV . M atrix Spike Recovery PFBS, PFHS and PFQS in Fish Sam ples
Sanate
D LS*O H PF001-04>41021 (COO--V* 3pkC .H K*)
DL3-F014PF001-0-041021 te n ta i Bpap. tnopp)
DL3-F01-IPF002-0-041021 (000(11275*0. folte)
DI>FO1HPF0C2-O-O41021 (C O N att?** S, lOOptet
DMC-FD1 -IPF001-0-041021 {(aiaaapkeriapp^
DMC-F01 IPFD01-0-041021 |coaai2apiH. iaopte>
DMC-FQ1-IPF002-0-041C01 (oootaizaftuc, latab)
OMC-F01-IPF002-0-041021 {00MH2aQpkH, MODfOI
D M O f01-IPW 001-<W M 1021 (CQM1K 5 *0 ,1 4 *9 )
DMC-F0l-IPW W 1-O<M1O2l tonuiaoapki. iPa
DM C-F01 -fPWOG2-O-O41021 IC0M191 5 *6 ,1 0 *9 )
DMC-F01-IPW 002-004 1021 (Cdo*ai9i ephJ. wa te
O M C-FO f-M SW O O f-0-041021 <oooMiai a * t, ia p * ap*>
DMC-F01-HSW001 -0-041021 <00041198 IpfcP.100*9 $pM)
DMC-F01 -MSW OQS^MMKCI * (cootaisi ateo, aa totBaiai
DMC-F01-MSW 002-0-041021* (OOWai999 * M.00 9 Bpiw)
DL2-F01-IPF0O1-0-041021 (caoMiat a * p,ia paiBaa) DI2-F01-1PF001-0-041021 <oowifM a k. un api pii|
DUSF01-IPF002-0-041021 <couiaa a o .i t e t t e ) DL2-F01 -0^002-0-041021 (CooMia&iteL. ioo ite apfc*)
Amount
C4 Olifante PFB S Amt Found Amount in Sttnpft Rocevm d B itw m y
C6 Sulfonate PFH8
Ami Found Amount In Sample Racouarad Recovery
(naMwrtwL < * ) ..
C6 Sulfonate PFQ8
Aim Found Amount in Sample Recovered Recovery
(%>
10 0.30 &56
63
ND
6.26 63
5.16
12.6 74
100 0.30
02.4
62
ND
732 73
5.1Q
754
73
10 0.265 6.52 63 100 0205 00.5 60
NO 7.40 75 4.16 NO 79.0 60 4.W
10.3 61 60.6 77
10 OMO 4.40 42
ND
5.34 52
7.40
0.96 26
100 0.330 05.4 66 ND 74.0 75 7.40 51.8 74
10 0.712 7.60 70 1 M 0712 76.0 77
NO 0.60 06 NO 06.0 96
14.1 14.1
10 1.00 7.00 65
NO
7.84 76
700
100 1.00 64.0 64 ND 900 60 7 0 0
10 0.866 6.70 56
NO
7.86 60
34.4
100 0.000
600
00
ND
746 75
34.4
10 0216
0.70
96
0.524
944
89
100 0.216
012
81
0.524
032
93
270 270
so NO* 452 90 500 NO* 432 66 10 0.000 S.B0 51 100 0.600 46.4 46
ND*
52JO
104
530
ND 462 66
530
NO 6.68 66 3.45 ND SO J 50 3.45
29.6 104 71.6 131
44.8 101 270 375
470 924 8.36 56.4
166 80 . ai * 67 106 . 78 40 S3
10 0410 504 46
NO 6.40 64 4,72
8.56 36
100 0.01
64JB
64
ND
786 79
4.72
724
68
*SnpN randaa wipia d i ft ipM ng la v i tgaftcardly; wafer. V * acquate raoowfy vate cannot btcafculated
* i.O fl of M iwp a Md fc r o im lw W --d of 1 0 ft. MD Noi datected at or abovt Limit of Quantitation wftich ie 0 2 nflg (*te NO* * Not daiacted at er abova Umtt of Quantitation wNch k 1.0 ng^j(wat weight).
NR H reported dm tequfty ooaUol w a ll faluraa. Ra M inate waulte aw hewn tn Tata I. Noia: Sine* M i summary tab** te o w i round* tw uM i, raeovary valga* nay vary teofc*y from tha waluoo in aw raw date.
Exygen Research
Page 33 of 132
000276
Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Sam ples (continued)
templo Coocrtoon
OU-F01-IPFOC3-0-04121 tC0**m**C, 10petOpOui DL2-f01*IPF00WKK1021 {CflUttt h, IDO Bphs|
L2-F01-1PFOC>4-O<041021 <03040117Optta tOpOOOOM) DU-F01'IPF004-0<041021 (C00M19TSpkKfOOwO M
DU-FOI-JPF0C5-O-O4121 (00040100tfk t.iQ f# pMI OU-F01-IPF00WMM121 (COOMIMSOkJ, 100fft$#e*)
DL2-F01-lPW001'Q-041Q21 |COOM139^KP. 1Depotpn*i
DLWC01-IPW001-0041021 {C0040130%hK. 100ff Opta)
DC2-f01-MSF001-a<M121 fo m t m apkO.Kipphapa) DL2-F01-MSF01-0-041021 (C0040140plil, 100ffb 8pl)
DL2-F01M9F0Q2O4>41021 (C004H418pkC. tOppO* * * ) DL2-F01-MF0G2O041Q21 (C0M14fk M.ICOpotoSpRu)
DL2-F01-M8F003-0-041021 (C0MB14SpfcD.lOppfc SpO*> DL2-F01-MSFOO3-O441OB1 {C0MI14*tp l J.100 * SPD
DL2-F01-MSRXM-0-041021 (OOMOiaapaa, io ppfaapa*) DL^F01-MSFKM*04410Z1 (Q M io apkj. 100ppb *)
D L l-tth -41*041-0-041021 JC00401UIffcF.ICppt apa)
0L1-FOI-IPF001-CM4i 021 (01040144* * K. 100R* Sp04)
DL3-FD1*6>F003-04)41021 (C0MO148Bpko, io peaapa*)
DL3-F01*IPFOG34-O41O21 <cao40i4i* * u o *e apa
C4 Sulfcnnl PfBS
^ CH Sutfofmli PFHS
^ CaSutfonill PFOS
Amount AmtFound Amount
S IS 5 7 Amount
Ami Found Amount
Sp6ted In Sample Recovered Recovery in templa Rnoovanad Rummy In templo Rnoovnrnd Recovery
fcaf mal)wetwt (nowiwtnL (%) MM ) MM). (%> M il * t M W * ( * 1.
10 0.247 7.00 6ft
ND 7.M 80 2.01
030 72
too 0347 B2J 63
NO 733 73 2.01
74.0 72
10 0.346 6.64 66 100 0.34 07.0 7
ND 7.60 76 4.02 NO 70.0 77 4.02
113 00 004 70
10 0.338 0 .
6
NO 7.68 77
2.46
9.00
72
100 0-336
84
66
NO 80 ft 81 2.46
B20 00
10 3326 7.04 67 100 0320 66.0 66
ND 7.60 76 9.8ft ND 112 77 0.00
13.9 80 063 70
10 0S30 736 70 100 0333 64. 64
ND 2 02 772 MD 77.6 78 112
70.0 . 158 81
10 0.40ft 100 0460
6.66 61.0
66 01
ND 740 75 94.8 ND 00.0 00 949
101 * 156 61
10 0 4 ie 6.62 01 ND 6.76 88 41 413
100 041 44 64
ND 70.6 71 41.8
104 62
10 0345 7.06 67 100 0346 71. 71
ND 7.90 78 63.6 ND 012 01 03
91.2 167 S3
10 0.432 7.44 70 0381 8.16 7
334
40.0
-
too 0432
7.2
67
0381
70.4
78
33.4
100
73
10 0448 too 0440
120 603
eo 00
ND 8X6 81 3.00 ND 813 82 3.60
10.0 73 80.0 78
NO Not ttnMelnd t or aboyn Urn ofO urtiK ton h ldi In 0.2 ngfe (Mt Might). Nn'NotnoorMduoloqwItroanMnMtMW um Wo -- )<N BiM amwm InT ib i. II. Note: n o Mo nummaryttMo ohowoi m M ntooto. MaauntyvaliMi mayvaryateMy from valuaa InIt n o data.
Exygen Research
Page 34 of 132
000277
Interim Report # 10-Analysis o f Fish and Claifl Samples
Exygen Study No.: P0001131
Table IV . M atrix Spike R ecovery PFBS, PFH S and PFOS in Fish Sam ples (continued)
. Simple
Dl3*F01*IPf004*<MH1Q21 (00049141*p* C. 10pp*6pl) DUWR)1HPF00WO41021 (cmmM epfcHi no poimk)
OL3-FQ1-IPFOO6-0-0*1021 (00049147Ipk D. 10ppb*6) DL3-F01- r F006-0-041021 (COOU147OfkltlMppb Ipha)
DBC*F01*IPFD01-<K>41021 <00049144tpHE, loppi Opto) D0C-FO1.|PPOO1<MM1Q21 (C0M9140Spi!4|W ppb IpHnl
D0C-FO1-FFDQ2-0-041021 <00049149IpF, 10ppb* * ) D6C-F01- f'FWC-WW1021 (COOM149Ipk K, 190ppOfOw)
D ec^roi-iprooM 4io2i |C004190S|*0,10 pf*9pl) D6C-F014PF003-0441021 (00099190*K L.W PPMpOt)
O0C-FO1-IPWOO1-O-O41O21 . *09040151 9f*C, 1 0 *0 ** )
O0C-POMPWOO1-O-O41O21 <000411016pkHiIpOppQtpOra)
DBC-F0WPWH-<WM1021 (C0H9192OfcftD, 10ppiapO) OBC^OWPWOffiMW)41Q21 1C00491&30|* 1.100ppbIplh)
D0OF01-TW00>0-0410C1 (C00491I3OphC. 10NbOpto) DeC"F01rW0094H)4ia21 (C0049109OpOJ, HOppO8p6e)
OOU-FOI-JPFOOI-0-041031 (00090104Ipk F.10ppO6pl*) D09J*F014PF001-(M)41021 (cm o itt iekKiW poMfiM )
DOU-F01-1PF002-0441021 (C0040160fpkO. lOppOlpI) DOit-F01-tPF002-0*04H)21 |COOt4l$54pkL IQOppOlpOw)
DCMJ-F01-IPF0034-041021 (00099109OpfcC. 10pp0Opl> DOU-F01-1PF003-0-041021 (0004019990kH. 100ppOBpHiOI
Amount AiMFoortt Am>t InBampI*
Amt Found ; Amount
AmiRound Amount
msampi*
Recovery V\Sarupia Recovered Recovery
t%\ ' ina)amai IMWlMtWL l%) a) wt
091
10 0.704 100 0.704
e.4 60.6
61 00
ND ; NO
1010 iw " , ; 382
0.90
1
56.4 ;*/B0
QJ82. ; a i2
10 1.53 5/44 36 100 1.53 60.4 so
ND , 0.16 , r,
5,46 117
NO 032
93 ` . 5.46 ' 86.8
10
1.34
024
49
0.002
106
101 . NR
100 1.34
944
56
0.502
060 . 66
NR,
NR NR
10 143 100 1.43
5.04 44 . ND
9.36
G0.2 56
ND ,
H.O
94 68 ^
110 .110
113 109
10 0.000 100 0.096
6.72 60.6
57 0.644 60 0,644
10.4 , ,96 ", 666 68 !
NR NR
NR NR
10 0.064 7.00 2 2:21 068 75
NR
100 0.004 70.0 60 2.21 eoo 0 6 - NR
NR NR
10 0,700 7.50 68 >8.12
.100 0.700 OSLO 09
0.12
"10 0.73 ' 8-32 100 0736 , 706
76 70
676 676
10 4.30 100 430
10.6 OS 763 72
1.02 102
162 , w
NR
t k , 96.0 67 , NR
\ 16.5 91 ^ j. MR
006 94 NR
0.46 65 00.0 05
NR* NR
NR NR NR NR NR NR
1 10
076
13.1 63 0.782 072
60
NR : NR
100 6.76
78j0
60
0.792
600
79 , nr
NR
10 5.00 ' a * 60
1.02> . 10.6
96
NR:
100 5.00 :
' 7$ i-fc 06.4 97 'NR
NR NR
66 61 82 61 NR NR 70
NR NR NR NR NR NR NR NR NR NR NR NR
NR NR
'la m p i* m atti m o la li w aplUng lavai alanMcanDr. nanfa*.an accurata laoovaiy valua carnaiba c a lc ilita c
ND Mot datadad al or * m v* u m i of Quamtatlon whleh la 0.2 nolg (M woM). MR Noirapotau Oimto quattacantalnatilifaluraa. Ra atalyal i maultaaia attcnn InTable H. Nato: Uno* Ma aummaiytatua itm v rotiodati laaulta,raoaratyvalva* ma)fvaYallB>iyira i. Ih . valva In Ih* a
Exygen Research
Page 35 of 132 000278
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV . M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
D M aM tan
DOU-F01-1PF004-0-041021 ( * * * 7 3 * D, 10pot Iptel 000-f01-IPF004^HM1Q21 (oobmu/ M i. u n * a tm
DOU-F01-IFPOOSO-041021 iCOootlMtp i. lo f* Se*#>
DOU-F1-IPF005*0*041021 (OI041If* J. 100p* Opte)
D U -FD llPW n-04410C1 (COUMMfttek F,10ppt Opte) OOU-FD14PW001-0-041021 (GOMMOttek K.100ff* Opte)
DOU-f01-PWQC2-0-04'tQ21 |C004t100tea, lOpptSOM) DOU-FQ1-IPW002-0-04121 (COMOiteteti. 1 MtOpte)
DL2-F1-MGW001-0-041021 (C0040101 tpkt, 1tpp* Opte)
DL2*f01-M6W001-0-041021 4COOM101 te* J*iooppttete)
DL2-FQ1-M3W0Q2-0-041021 (COMBIU***. M t Bptei DU-F01 -M3W0G2-O-O41021 (OOMOIOtte t L, 100 Opte)
DL2-F01-M8WC0CKHM1021 toooum tekc, m tte te i DU-F01-M8W0034-041021 (C9046M*tph 0 ,100ppt8pte)
DL2-F1-M8W004-0-041021 (C0040104fpkE, p p tte te l DUHF01-MSW004<M41021 <00001144ipk F, 100ppbOpte)
DL2-F01 -M6WOO5-0-41021 tOCOkOHtipk0,10 pp*Opte)
DL2-F01-MSWOOWMM1021 (C0M0109p* H, 100t f t Opte)
DBC-F1-MSW001-MH114 (cm m o spec, 10 pp*ete)
06C-FD1-M3W001-<W>41104 IG0MM006pkP. 1 pptOpte)
Amounl a m Found Amount
And Found Amount
Anil Found Amount
Spked msnmpl# RM0*>d Recxnery In Sample Rocovdnd noeonwy inSMnpl Reoovortd R acom y
fnoAil (MMMlal. (MMMIM. t% \
H
10 6.12 13.2 71 2.30 12.0 7 100 6.12 75.4 70 2.30 B6.0 64
NR NR
NR NR NR NR
10 4,56 100 4M
120 76 0.966 110 102
70.0
71
0.868
650
e
NR NR
NR NR NR NR
10 2M 100 269
100 73 0.040 .7 72.4 70 0.9*8 63.6
90 03
NR NR
NR NR NR NR
10 15.4 100 10.4
04.4 100 04.0 70
3.06 340
10 0203 962 91 100 0203 760 77
ND ND
10 ND 100 ND
9.66 7 66.4 66
ND ND
10 NO 964 9Q 100 ND 616 61
ND ND
10 ND 7.90 70 100 NO 24 02
ND ND
10 NO 7.96 00 too ND 90.8 91
ND HO
13J! 98 192 66 0.M 07 66.2 65
6.12 61 63.6 94 906 91 950 96 706 73 83. 94 0.08 61 100 m
NR NR
120 120
102 102 02A 924 MA MO 1M 1M
NR NR NR NR 120 * 177 57 110 . 105 03 103 * 162 90 7S.0 1M 70 138 234 66
10 0.HS 10.3 4 fi.32 170 93
NR
K 0600 0.4 90 8.32 113 106 NR
NR NR NR NR
reoMuoowcoodotm Mhfcq MnoI NflwWcontly;tenefana. %* oocumiorowm iy value cannot bo calcuteod ND Notdetected at g above UmH of QurnitMUon uftteh 0.2 n ^a Cm*w ight). Nft * Notp o rted Am toquat%aoftM neeulltellure. WoeodyeH reeiito am ehewn InTteto II.
Notes <4oeothlo eununeiytoMo ohowo rounded m eute, reedvwyvcJuo*nwyteiyiioMyfront the valuoo in fee nm dote.
Exygen Research
Page 36 of 132
000279
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P000I131
Table IV . M atrix Spike Recovery PFBS, PFHS aud PFOS in Fish Sam ples (continued)
Swnpto
M&FO 1-MSW002-<K)41104 (OOMMI1Spe, 1p * 6pM)
08C.FD144SW0024441104 tCOMMSI pkP. lOJppPIpta)
DBC'FOI-M8W0CKWH>41104 iCOOSMUCpkQ. 10ppbto n )
ODOFOI443W003-0-041104 <000*9462to H . lO O totoN
O0C-FO1-MSWOO4-O-O41104 tototoss to * to to )
OBC-F01-U8W004-0-041104 IC80SM9St o A 1V to M )
DBC-fO1-MSW00<WM*411Q4 tCOUMHto x. to to w
D0C-F01-M3W006-0-041104
to(coton to u tom ato
06C-F01-M3F001-0-041104
(CitoMsi to *4toto tto ) DtcBcCw-FN01-HtoSFO. 01-0t-o04t1o104l
DB&F01446F002-04M1104
IC80WWtoO,16toto)
OBC-FOI-UHFOat0041104 P M M K tV .W W lM
D0C-FD1-IPF004-0041104
(caototofto c.K)toIp")
DeOF01-IPF004-0-041104 (COMtoTto o . to to l
DBC-FO'WPFOOWHW1104
(OOQ4W66to110to to*}
DBC*FOHPFOO-0-O41104
IC0MM64to f >100to Wto>
08C-F01-IPW004--041104 (OKHtoWto 0.10 to to ) DBC-F01-IPWQ04-&041104 1C66O490to K 1Q0to >*to
BC-F01-IFW005-0-041104 tCOMMflOto I to to rt) DOC-F01'IPW0054M41104 (G0MM46to J . 100t o 1to )
C43uBcnfPFBS
C6 itdtonnf PFBS
C9 8ultbnl PFOS
Amount Amt Found Amount
Amt Found Amount
Amt Found Amount
8 |)M it o m to RpoovtPd R*eou*(y In Smnpto R ioow td Raoovary In Samite Raeouarad Rooovwy
( t u total to. * *< *. (%>
totalto * t*>
10 0JBM 8.98
91
343
129
94
NR
100 0469
049
94
3.43
113 110
NR
NR NR NR NR
10 O.flBO 9.82
91
3.62 13.8 100
NR
100 0.600 96.0 95 3.62 104 100 NR
NR NR NR NR
10 0.084 9.S6 91
9.72 19.5 98
NR
100 0.904
972
98
9.72
124 114
NR
NR NR NR NR
10 0.832 a 20 74 2.77 102 74
NR
100 0.892 91.8 91 2.77 100 106 NR
NR NR NR NR
10 0.820 9.80
89
3.68
13.7 101
1100 0.820 <9.4 99 3.58 109
ia 0.768 o.ee 92 1.94 125 106
100 0.769 0.9 90 1.94 102 100
10 0404 104 100 0494 11.0 110
100 0404
044
94
0.584
108
106
NR NR
NR NR 142 142
NR NR NR NR
NR NR NR NR 152 254 112
10 1JB0 104 88
2.15 122 101
NR
100 100 90.8 89 2.15 105 103 NR
10 0.494 9.72 92 328 13JD 97
NR
100 0.484
87j6
97
328
104 lOf
NR
NR NR NR NR NR NR NR NR
10 0,572 104 98
2.10 132 111
NR
100 C47J
K4
92
2.10
102 100
NR
NR NR NR NR
to ito ra W w -- ds a spiking itto to u to n d y : to to b f, an Bceurt o moovwy v a to c a n t* to calpulato , NO * Not detectedat or abcto UmHof QmaOnUonuMch 0.2 M i N R -N ot (ported duo to ^M lllyooniroirm uK M uraa. R e ^ ra M m aiM i aitMai In Tabla \i, Noto: SingeIhto euiwmafy toWoahaemuuded ceeeHapeoavaiystoee -- yva y sdphKyfeu* to valueto to rawdate.
Exygen Research
Page 37 of 132
000280
Interim Report #10-Analysis o f Fish and G am Samples
Exygen Study No.: P0001131
Table IV . M atrix Spike R ecovery PFBS, PFHS and PFOS in Fish Sam ples (continued)
Semole aotntton
o o u -ro i*ip w o o a -c w )4i w |C Q *4*M OpfcK. 10ppfrtpha) D O U -F01-ir)W OOa>0441104 (0004*441 Spia, 100pf* SpA)
D O U -F 01-IP W 0044M I41104 (C00MM2 SpfcC. 1000* S M
D O U -F01-IP W 004-0-041104
(COC4MI2Spi0, 104 ppb(#)
DOU-R>VIPW0QHH1104 (00MMU *pfct 10*P **M OOU-FOt-lFWOGKMKI 104
(00*4*4*3 fp k F, 900 *0 * tp M )
D L2-F01->W 002-(K K 1 104 (0004*464Apfca fftp p O M
0L2-FO1-IPVVOQ2-O-O41104
(0*04*4*4 tph *106 ppb6pM)
OL1*F01-Maw001<0-41104 (0OM64609pfc>.t* m bM M
DL1-F01-MSW001-0-041104 ICCK4M64tpfcJ, 1606 S M
OU H-MSW0W-9-041104 (O otM tM iK . < 0 f**6 M
DLi*f*01-M8W0024MH1104 (0004*4*1Spki. 160ppt*pM
DU-F01-MSW01&04M1104 (0004*467SfO0,10 (** **M )
D L14sO 144ftW 00 S O -041 l04
(0004*447M D.160M* ***}
DL1-f901`M8W004-0-041104 [C0*4**6ti Spk E. 10p p k*M
DL1*f01*MSW004-0-041104 (0104*46**pkr, 100ppt***)
ix i -Foi-4wpow-04iia4 (00*4*46*Spk<2.KlppbS***) DL1-F01-MSWOOfl-O-041104 (C004M616|*H 100p**S M
IX1-F01-MSF001-0-041104 (0001*470Spk1 ttp p tS M 0L1-F01-MSF001 4 1104 (00*4*470 *pkj, m * * ***)
Amount Ami Pound Amount CfOtd* 1n Semple (nato! M0> V w t MA/BIMWL
Ann Found Amount
Ami Found Amount
In Semple n *o a w *d RKtHwy *8*m pN R dconrad Recovery
ri ' (N ttlM ta t
HH
ri
10 3.12 100 3.12
13.1 68J>
KM
85
6.00 eoa
1 6 .3
103
107 101
NR NR
NR NR NR NR
10 3v49 12.6 93
7 .1 2
1 7 .4
103
NR
100 3A0
St
65
7 .1 2
108 101
NR
NR NR NR NR
10 2.07 10.6 75
100 2.07
83.6 61
S .12
b.12
13.5
to o
84 104
NR NR
NR NR NR NR
10 1.04 ioa 1.04
8 .4 6 8 0 .0
84 78
ND KM 104 6 2 0 NO 87j6 98 8.20
1 4 .3 124
81 116
io 120 100 120
10. 84 0.088 113 104 68.6 88 0.606 112 111
NR NR
NR NR NR NR
10 1.30 0.78 85
too ij o
80.4 78
1.72 12.4 107 1.72 100 98
NR NK
NR NR NR NR
10 0.560 6.62 64 100 0.560 652 86
1.13 10.2 91 1.13 898 96
10 0.800
8,S2
76
0.908
0 .7 8
89
100 0.806
642
84
0 .8 0 8
983
98
10 1.18 100 1.16
8 .8 0
76
82.4 61
1.16 10A 92 1.16 982 98
NR NR
161
181 NR NR
NR NR NR NR 201
286 108
NR NR NR NR
10 NO 100 HD
7.7B 76 0.315 9.52 92 7*A 78 0.315 90S 90
293 293
303 * 394 101
tanplaimUu.uoM i wplUngta l gnlHan^wtom.As o lili mcomymu*cannaibotatevi* ND > Natdatocted<rabwiUmflorQunlil*Uonwhlchlt0.3ngig(*iviaM). NR>Noirapt**dualoqudMycontrainmultMijim. M-4n*ym miraiMn mTMII.
Hm:8I.C tnnumiiwyi*UN>onroi*0di*it.racomryh. m*)(,17 fron"tnP
Exygen Research
Page 38 of 132
000281
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV . M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Sam ples (continued)
Sampla DaacrtoUon
DL1*F01-MSF0Q2-0-0411Q4 **71 0 K,10MhMMI DL1-F01-MSF0Q24K)41104 |C*04Mtt epku lOOppftM e l
DLVFO1-M0FOOWW41104 (CtOWTl tphC.-Hpeta * ( * ]
DL1-FO1-MSF00M3441104 (COOM472ftpkD, tooppb
DL1-F01-M8F00MMM1104 (COMMDSptf. lO ppfttf*) OL1-F01'MSF004-0-041104 <C0W*tt S *F .
DL1-F01-MSF006-0-041104 tcaam tt tg t s. m mb tote)
DL1-FO1-MSF00HW41104 (OOMM746 * H. IDGpp6Ifk ^
DL1-F01-PW001<04)41104 (O0O479tpk I19Mb9pfc*) DL1*F01-JPWO(M-0041104 <000047O J. toopp*6pR|
DLVF014PW002'O^M1104 (0000471 O I t , ppt)
DU -F014PW002-WN1104 (00049470%fkL, 100** MO}
DL1-F914PW003-0441104 <090404770p*C, 990p*j DL1-F01-PW005-0041104 (C0049477Sffc D, lOOppO*>
CX.1-F01-IPW004'0-041104 (C0U7Bpfce, 10pph ft*) DL1'F0WPW0044MJ41104 (C904K70tpiiF, 100pp0M*>
P t l- F O t IFTOCg 0 0 4 1 104 (Q9Q404TO9ll0.10094O M DU-F01 *IPFOt-0-041104
(00040479 p fcH .W p p Opin)
DL-1-F01-IPF003-Q-041104 <C90tMN1(41,19 DL-1-F014PF003-0-041104 <00049490SpkJ. 100 * $ * * )
C4 8ucnto PfBS________ COSuHonataPFHS
Amount Amt Found Arnold
Amt Found Amount
Splkad M Sample ftacoverad Recovary in Sampla Rvcowed Recovery
10 ND 100 ND
6.60
M
0.024
100
99
040 66 0.624 6.4 ` 06
10 02W 0.76 06 0.652 102 95 100 0.203 04.4 04 0.652 95.2 96
10 ND 100 NO
0.00 00 0.532 10.4 99 060 07 0.532 101 100
10 ND 100 ND
0.04 00 0.604 10.1 024 62 0.664 94.0
94 93
10 0.772 0.64
79
0.500
9.72
92
100 0.772
04.0
83
0.558
970
97
10 0.400 t o o
82
0.536
0.06
94
100 0.460
764
76
0.536
00.0
67
10 NO 100 ND
9.06
91
0.20
9.44
92
S0.4 90 0209 106 1
10 ND 100 ND 10 ND 100 ND
0>4B 05 71.6 72 0.00 00 80.4 s o
0.230 0.230 0222 0.222
9.00 840 9.26 8/1
96 65 91
ea
10 ND 10O ND
0.00 06 0J65 100 109
70.6
79
0.206
04
oo
ill
COOdfenataPFOS
Amount Recovered Recovery
i% i
NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR rm NR NR nr NR NR NR NR NR 174 204 90 17.4 113 00 15.7 27A 117 15.7 100 64
9.30 tB.7 n 0.30 109 106
59.
7 2 j0
*
a . 140 80
11.1 164 7 11.1 106 9 7
204 300 90 20.9 109 60
-aamm mutua ancaMi m aptois Ivratunncawy.tornkm, anauuaa racovafyvalacannota* caicniaM ND - Not tMaclad at or aaon U nit cf Ouanaallon wnicti * 02 ntfg (wetwalgH). N Not raporta. tum toquaKTy ctyrtnjt rm uft m ana. R ^analyati nauta ana ahowi ki T a il* a.
N on; Anca M i m um m y M ila ahowa wuadad raauHa, lara tmiy m tuaa may aaiy a ll^ rtty from t o valvaa m tha raw dala.
Exygen Research
Page 39 of 132
000282
p. 40
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike R ecovery PFBS, PFHS and PFOS in Fish Samples (continued)
Swnpla
DL-1- f01-IPF04-0-041104 (C0MMMIfk K, 10ppbVpto) DL-1-FOHPF004-0-041104 icommm ip k tw o fft s m
DL-1-F014PFDWW>41104 (COMM t # C, 10Mslp**> DL-1 FOHPPOOKMWUM (coomw to o. m m * * )
0L3-F01'MSW0C14MM1105 (GOMMO%* ft. 10at* M v) DL4F01-MSW001-0-04110S (COMMISIph 1,to jppbM *)
DLSP01-M8W0G24MI41105 (CCD4Da4H*6,10N*lpl*l DL3fDi-MSW002-0-0i1105 (CtoMM to h,toopppto }
L3-F01-MSWOOW-041105 tCOMMIOSekl, 10B * IUMI
DI4-F1-M4W03-0-0411Q fCocuMisip* j, tippe to to
DL3-FD1-M8W0044KM1105 (GOMMlIto K.10pphIpl) DL3-F01-M3WQ04-C-041105 <Q004Mtpk L. 100ppbSUM)
DLJ-FOt ` MS1NC0S-O41108 <CMM7(>C. toppliipHi) DL3-f01-MW00643-04110S (COMM*?to 0 ,1*0K*>to>
OL5-F1-MSF90t-D441105 (COMMtt^kC. fOppfrlp*) DLJ-FOI-MaFDOl-0041105 (COMMMto F.0 ppeIplM)
DL^Foi-Marooz-o-041 ios OOMMM8pk8,10 M* Ip to DL3-F01-M6PQ02-0441 105 (C004MWtpk . 0 MbMMj
DL3-F1-MSF003-0-04110B ' (COMM* 1*1, (dppbto*)
OL3-F01-M8FQO3-O-Q41105 (COMMtt8dJ.HCff* Spftl)
C4{ PFHS
Amount Amt Found Amowd
AmtFound Amount
Amt Found
Spikod In ftampla Raemarad Raccuwy nSampf# Awovm d Rfcoviry In Snm^tn
(nottwatwt o n
Amount Raommnad RMotwy M riM tu t l%1
10 NO 0.00 80
too HD
84.8 os
NO fl.48 96 7.80 NO 90.6 8 7.80
154 82 102 94
10 NO 100 ND 10 ND 100 NO 10 HD 100 KD
10 NO 100 n o 10 NO 100 ND 10 HD 100 ND 10 NO 100 NO 10 ND 100 HO 10 ND 100 NO
7.44
74
0575
9.00
88
04.6
85
0.373
984
98
6.72 6.72
0.30 M 05.6 86
ND 920 92
138
ND 994 100 139
0.44 84 004 90
ND 9.92 99
180
NO
106 100
100
0.00 08 884 88
NO 0.80 88
146
NO
102 102
146
0.40
86
0.286
8.81
84
198
884 88 0286 102 102 188
9.56 96 0.388 11.1 107 too 100 0.38 108 106
0.48 95 ND 11.4 114 944 6 NO 108 10
0.00 99 ND 104 104
MS
ND 103 f03
173 m
lie 116 116 116
9.32 90 ND 11.0 110 75.6 to o 81 ND 107 107 78
15.9 72 102 93 166 . 258 119 150 . 263 103 164 * 284 108 226 1 103 183 348 73 138 * 234 118 984 * 218 100 92.0 . 190 114
` WWM ramduv a n ) * Iw aplklna Iw n ilg n < c tn llr. n n im m x u n 1 / u ca m * 6 NO - NaUMacM*ler(bamUmllor&MnlMhM<iNd'iN02iiotl(M*<Mi9NQNR>N<*r*Fanad du* U n ualltrcanm l m u tt M ura*. RaanNylU m illm ih u n m T tU a ll. Notas Stag* aw a u m m iy iu l*a ih a m taandad f u ll* . raceawy v tlim rn y u a c y ilK ih iy 8aai H i* v ia -- I t 8ia 11
Exygen Research
Page 40 of 132
000283
p. 41
Interim Report #10-Analysis o fFish and Glam Samples ,
Exygen Study No.: P0001131
Table IV . M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Sam ples (continued)
ampin DaaotolMn
D t^F01-M3F004-D-041105 fCQMMM Ipk K, tO0p6S0ht) DOFP1-MSF004-044110S lCQ04C*ei M L , 1IOppbIpfte)
DL3-FQ1-M3F00WMH1105 tCC0*MK9pkC. tOppbSf**} DL3-F01-MSF006-CM>41106 (G0MMMBffcO, 100ppiM>
DMC-F01-IPWO0&45-O41106 {00041409 * K.10M M e) DMC' F01-IFWOO*0441106 {CooiMta Si* f . iooppbM>
DMC-F01-IPWD04-0-041 K)5 (COMMMpk&IPprt fp*a) DMC-FGWPW004-0-Q41W6 JCOSi M K lO O M M tl
DMC-F01-IPW006-0-0411C6 (COo h im M 'U O M t p i)
DMC-F01-IPW005-04H1*105 (000404M J. 0 p0SP**)
DMC-F014ISW003-0-041105 (C0MMM$pkK,WppfcM *)
DHC-FOI-MSWDOMHWI106 fCoarMMIpkL MOn * Spaa)
DMC-F01-M3W004-0-041106 (COOtMtrM C.10M M e)
DMC>FQ1-M5W004-0-041105 (COMMITM B . MOppblPftt)
OMC-FOI-MSW006-(H>41106 fOOD4MSpkli ID M M lM
DMC-F01-M3W006-0-041106 (COMMM8 * F. IMppb Spttel
DMC-P01-MSFC02-0-0*1106 ' (0004MMM q>1PM M l
OMOFO1'M^0Qfl-0-041106 IC0M4MMH. 100pp0M*l
DMC-P01-MSF0Q3*O-O41106 <000400M >11M M M )
DMC-FO1-MSF00O-O-O41106 (COMM 1 ICOppb6pe)
Amount Amt Found SF*oO InSampta
10 ND 100 ND
0.60 904
10 NO 100 NO
6.92 e&6
10 ND 1W ND
&36 844
10 0.000 100 0.300
6.04 90-4
10 ND 100 ND
8.96 60.4
10 ND 100 ND
R64 924
10 0.316 100 0.316
ftS2 82-4
10 ND w ND 10 ND 100 ND
0.16 so.e 8.36 97.8
10 NO 6.20 100 NO ; 672
H*
hi
Amt Found Amount
Amt Found Amount
in Sample Recovered Htcovery In Sample Recovered Recovery
M lv a tu t. (fatalvatwL (%\ (fataleel4
66
ND ; 11j0
110
130
144
60 NO 104 104 .130 . 239
69
ND ' 1043
3 1 81.6
972
86 ND 08.4 96 61.6 161
63 0.386 ] 9,52 64 0.386 - 966
91 . 61.2 99 81.2
760 158
77 0.396 . 9.28
' 686
90 0.396
10 104
66.6
107 168
109
* 9 95 99
60 0.270 i 10.1 '-99.- ,64.4 68 0.270 106 106 64.4
96 0.692 11 0 104 92 0.592 106 106
354 364
92
1.90
12.1 .1 0 2 .
259
62
190
101 - 09..
250
75,6 . 153 69 369 464 110 259 6 313 94
92 0.960 11.6 109 94 0.960 118 117
NR NR
NR NR NR NR
94 ND 104 104 NR
98
NO
104 104
NR
NR NR NR NR
82 ND 10.4 04 (6.9 109 . 97 ND 110 . 110,, 660, 194 137
*8jnpJemaidmoMceedi toetfMOQlevel tapifaenty; tarefam, anccuieK iwevey vela*cervwtbecMcUMtd
WD Wetdalactnd 1or abovn Urn*d QuanWaHonWell i i 0.2 nglg (walwalgM). .
NR-Notrpcmd4vatoi|uatyoorroliaaMtaiuiaa.
pml* * i. llm * lr TaftH.
Not.: tinea M ( aaaMwy MMtahem muaOaa rnauKa.iaaaai| valuaa mayvary all^nly from 9mvaMaa In tha rM 4ala.
Exygen Research
Page 41 of 132
000284
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Sam ples (continued)
tw u ftt
OMC*F01-MSFOO4*O-O411O5 (COM ig t K. 10MhapM)
OMC-F01-MSF004-0-041106 (CM4MQ1tfk U 100ppepda)
DMC-F01-MSF006-0-C41106 {OOMttOt SpkC.10 ppOOpto) DMC-F01-MSFQ05-0-041106 (CMUM3 SpfcO, IMppMpM
PMC-F01-IPRWHW41106 (CNMB83SpkC,10ppfc8pht) OMC-FOHPFOOO-O-041106 (CauBMtpkf, to o ****)
DMG-FQ1-IPF004-0-041105 (C06M8O4Spk6,10 pptQpRli) OMC-F01*>F004`0>04110$ (OttMSGt 1* K .100pph 8pM
0WC-FD1-IPRX-0-041106 <OODWapl. MppeOp) MC-fOHPFOOS4KKI10ff (coo# tpkj. w d p >ap*)
DL2-F01-Mtf09S44121 KVBoat W in DL2*F0l-IPW0C6-O-04121 (C00MM4 tpft r. 100 h * *#*)
DL2>F01-IPWOGA-6-O41215 {CMB44M*pft0. t* **> L2-POHPW00S-0-O41216 (C006MM 8# 0,10*wo *<>
OOU-f01-MSWGQ2-0-04l216 <00060460 ft* K10ppepi)
DOU-F014ISW0024441216 (C0M460tpkj, 100ppOOp)
OL2-F014PWOG44-04121B <CQ06M r ftpp. Wppfr*) OL2F01 IPW 0C 4-O -O412 1 6
(00066447 Opt Dt MOppOSfMa)
DOU-F01-M3W003-0-04U16
<00060460POK, f t p * * * )
DOU-F01*M8W003-0-041216 <C60M4M ipk L, 160 ppp U m
Amount Spotoa
CBJ
Amt Found AffKNflt
AmlFound Amotf*
Amt Found
w Sima fte o o w rt Recovery in Simple Recovered Recovery hi Sample
M M M tU rnoMmi*. 4%)
(M m u M (%) MM)eut
Amount Recovered
IIMMVMtWt
RKOWy Ml
10 ND 100 NO
&76 68 0254 11.1 106 68.0 00 0254 107 107
11 116
10 ND 100 NO
6.52 65 0.420 12.2 118 03j6 84 0.420 110 110
146 146
10 ND 7.92 79 NO 108 106 7.08
100 ND
82.0 82
NO
108 106 7.82
10 NO 100 NO
7J92 79 632 3
ND 10.7 107 446 ND 107 107 444
10 ND 100 NO
7.86 79 75.0 7
ND 10.3 103 46.4 ND 964 00 4 0 /
10 NO 0.44 64
ND
10jO
100
492
100 NO
03.2 63
ND
102 102 492
10 ND 6.00 60 ND 113 115 112
100 ND
044 05
NO
107 107 132
10 0.206 8.92
67
1.72
10J 92
100 OJM 672 67 1.72 024 91
NR NR
10 ND 6.06 61
ND
10.4 104
0.00
100 NO 704 77 ND K 2 95 040
10 NO 8.12 81
10.4 194 90
NR
100 ND 664 88 10.4 105 95 . HR
123 228 110 193 280 114 162 61 101 93 56.2 . 134 90 54.4 121 75
592 100 142 93 22.7 96 121 108 NR NR NR NR 14.5 90 97.2 90
NR NR
NR NR
*r~r`T i rirfr*- --1-`rr'*--T*-----
----
NO Not iMttctM *t a t/txnUm* orQumKaKn which a 0.? ng (wmwvtght).
NR Nolmoitao uataqjMty ooniral PMiAtMun. *- rus* mTit! I.
No: a m MMimtiyKM*nom imaraiflimuM. ncwmy vataaeny v * / (MM*ft wwtaw mtw r
Exygen Research
Page 42 of 132
000285
p.43
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV . M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Sam ples (continued)
Simpta
OL3<FOHPW004-0441130 tCOMMMI)* (, 1H M DL3-F01-JPW0Q4-0*041130 <00094400aptr, m dp*)
DOU4=01-M8WOO1-0-04121 (cofiMMojane. mm ktHM
DOU-F01-MBW001-04H121B fCOOBMooam n.iso mk Spks)
DOIW1*JHSW004-0-D41218 . icowo*i apta.10* * m * j
DOU-FOI*M$W004-0-04121 (oaosoMf amtK loo mom
DOU-F01-M6W0S-OO41216 (COUS2 Ipk 6,10 0 SpOsI
DOU-FOI-M8W00WW41218 icooeaw amim.1 wo ap)
OOU-FQ14I48F005-0-041216 <00090403cutc. o amt DOU-f01 4M8F006-0-041216 <CwMO>amorreo M *)
DL3-F01-IPW002-0-041130 icnoaoioiamt a. lOpstamh DL3*F014PW002-0041130 (coofioiM amtF.iooppaaaim)
OI3-F01-IPW00WK113O (Coeaewas, mS|*ti 0U-F01 -IPW003-04M1130 ICNM40Stphh,tooa amu)
DOU-F01-MSFOOO-O-041219 (CouMooamiK. loppaam) DOU-FOI-MSF08-0-041216 (Coqsomiam>l no moammj
ddc^ o1MaFOO-i-osi21a ffUBHIT aptC.10psbOp--)
[C-F<I1-MSF*-1-04121 KMH497( D, ,W K * M b)
OBC-FOI-MSF00WWM1218 (C04wm3i* k. ppaam*) DBOF01-MSF0S4-041216 (cooMHoapal. too aoaaano)
C 4S u*onfP fB S
C6SeMont PFH8
0 Sultanate PFQfl
Amount Amt Found Amount
AmtFound Amount
Amt Found Amoinl
Splkad feiaoirpM Rocpwwd Raootmy In Sampla Racovamd Rooovwy In8ampla Rasommd RaooMiy
<miUt*t
<*>
ML
10 HD 7.62 75 100 ND 664 fifi
NO 11.0 1 7.92 ND 118 118 7.92
17.3 94 114 108
10 7.08 14.8 76 100 7.08 892 78
15.4 Z7.5 121
154
122.0
107
NR NR
NR NR NR NR
10 4.72 100 1 21.7 29.3 76 100 4.72 720 88 21.7 104 82
NR NR
NR NR NR NR
10 0.384 7.08 87 1.34 8.62 72
100 0.304
72.0
72
1.94 87.0 68
NR NR
NR NR NR NR
1.41 8.80 72 0.40 170 92 100 141 72.0 71 8.40 940 86
NR NR
NR NR NR NR
10 NO 7.02 79 ND 9.04 90 12.0 166 46
100 HD
81.2 81
ND 110 110 12.0
108 3
10 ND 100 ND
7.08 80 84A 04
NO 8.88 . 89 8.44 NO 102 102 B.44
12.3 <9 92.0 67
10 1.72 9.00 73 8.98 140 77
NR
100 1.72 B9.fi 88 6.56 107 100 NR
10 0.220 8.36 81
1.79 11.6 . 97
100 0.220
63.6
03
1.79
98.0 95
NR NR
NR NR NR NR NR NR NR NR
10 ND a m 04 ' 1.80 11A 97
too ND
eo.fi 81
1.88 .6
98
NR NR
NR NR NR NR
3wnp*s <smeus aacm d i ft spMnp Jay* stcmacsniv; m i* * * , an^ocmala >ctiaryyfcJi e*y>ct 0 csteuhnad
ND Notdoiociod at OfabcwaUrnttoiOunntiWion which k0^no*g(otweight). ,
-
NR * Notreport d o t *0qumUym n M rasuN M ures. Ra-snalym reaukt *r# h*m m TJa H.
Nolo: filn c s M i summary ttM o shew s reundsd mauNs* reoovsry v al-- mayvary s ig M ly M en tbs vat s In Iks saw data.
Exygen Research
Page 43 of 132
000286
Interim Report #10-Analysis of Fish and Oam Samples
Exygen Study No.: P000113)
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
Semple D aoM r
DOU-F01-M3F002-0-041216 rc w 4 e e ii*a . ic m m * ) D0U-F014ISFOOS-CMM1210 tc a m m m h. o p * M *)
t3-F01-tPW00l-0-O4l13O <CmMlQgRC. 11M* *M| DL3-F01-W00HW41130 (COaSKttip t 0. * M t tftk)
DOU*F01-M3F002-1 <041210 fCOMMTl pkUOppfe*)
DOU-F01.MSF02-1-O41218 (0USW71 M J .W n t M a]
DOU-F01-M3F004-CMM1218 (CooMnapkK, OOU-F01445F004-CMM1219 |C00M4ntpk L 1 M tp*a)
DOU-F014ISF001-0441210 <cooawnm t. n M M * ) DOU-RM -MSF001-0-041216 (o ao sam m f. 1 M M i
DBC-F01'MSF003-0-041210 (C0M8474 ipk ft 1 ppbMa) DBC-F01-MSF003-0-041216 (CMS4474 ip* H, iMppb M )
DBC-F01-M8F004-0441210 IOOOM4738pM. 10M i M>
OBC-F01-M8F004-04M1216 IOMM47 tpk J. 10* M M * )
DMC-F01-M8F001-044121* IC0M4M M c, to ppiM )
OMC-F01-M3F001-0-041216 fCOM47S M 0,100M M *)
DL1-F01-JPW006-0-041216 tCM*W77 M 1 . 10M M )
D U 'F014PW O O M M M 121 <CM 4n$pk J, 100 ppfatpH)
Ot2-FOUPW0034441201 (COOQ471M K. 10M M )
DL2-FO1-IPWOOMM>41201 IC0MM7IM L, 1ooppiM M
Amount Ami Found Amount
Ami Rtuntf Amount
AmtFound Amount
Spiked In Semple Recovered Repovny m Semple Rocowmd Racuvary In Semple t o a m i Racovaty
inert)wot* . t%>
10 o a s t 0.24 4 456 14-5 0 100 OJM 01 3 4.S6 104 99
NR NR
NR NR NR NR
10 ND 100 NO
7.10
75
0.246
fi.60
96
82-4 2 0.246 101 101
9.04 944
174 82 102 93
10 0.040
620
84
4j08
14.5 9
100 0.840 82.0 81 4j6B 103 98
NR NR
NR NR NR NR
10 0.792 7.7 70 235 U O <6
100 0.762
812
BO
2.36
86.6
53
NR NR
NR NR NR NR
10 2.10
11.1 69
100 2.1
tit
61
10. 20-6 10.9 104
99 93
NR NR
NR M* NR NR
10 ND 6.46 S
2.09 114 90
NR
100 ND
84.0 64 200
100 104
HR
NR NR NR NR
10 NO 100 ND
7.72 77 75.6 78
JB7 124 387 684
90 98
NR NR
NR NR NR NR
10
NO
9.08
91
0.420
0.M
87
NR
w o ND 88.0 80 0.420 102 102 NR
10 0.253 7.40
71
0.644
9.96
93
100 0 2 5 3
72-4
72
0.644
664
86
664 8.0
NR NR NR NR 83.2 . 148 78
10 ND 744 70 NO 6.04 0 7.46 13.7 62 100 ND 71jB 72 NO S2.0 92 7.46 64.0 77
*6amptwdutawppadjftappAMj JaveMyMeaffBy, la wllw ,iscym ooawaryval--cannotbacalculrtsd HO =* Not detected ai orabove Urn*ofQuanitatlonwhlch It 0.2ng* (walweight). NR-Notrapcrtid but la quplllycontrol rwufltaluii. Ro-nSyM m4bmm thoa InTstta #.
N o t* 8toa da aammaiy ttb ta a tm * rovodM m a t* , laeeveryvakw i nay vary t il# * * boon UN wafaaa ta lh a ra w d m .
Exygen Research
Page 44 of 132
000287
Interim Report #10-Analysis o f Fish and Clam Samples
Exygcn Study No.: P0001131
Table IV . M atrix Spike R ecovery PFBS, PFHS and PFOS in Fish Sam ples (continued)
Sampla
D13-FQ1-IPW005-0-0412Q1 lcowi79 spfci, ioppa Spat) DL3-F01-IPW006-0-041201 (Cauaat7aM i. M pab*ka)
Amount SpOtad inofti)
C 4& ionataF F B ^
^ C t 3 utfonala PFHS
^ ^ ^ Cg S u lle n PFQ6
Amt Found Amount
Amt Found Amount
Amt Found Amount
In Sampla Racovarad Racovaty in Samplt Racovorod Rocouary in Sampla Ftaanvarad Racouary
tiM lo a la t
rnatalwatnt rnatolaaiat (%}
10 ND 100 NO
8.10 2 M.B 85
NO e.w 90 4.00 ND 972 7 4.ae
14.0 91 94,4 90
Am ^ k M dardD avlaaon:
7* 1
Standard Oavtaton:
M 12
S an* iMidu* woMda tin aptkinglawl algiimcany,'tom. antear** neomiy v*to canm*baakutaM
ND m dM w M *lor*lxw lJirM alQ iiaritnaliaiM M ctlltO JllM (M (W (lgni). NRBNot raportaoOut ID q u a coMol raauHtadama- Ra-analyall raaufcara diwm lr Trtrta It. Nato SlacotMa awnawiy M ia adorn raaadad laauMa, iaavary vataaa mayvary aHMlyfta n * wakwal i t a M
data.
Aaangas W tandafdD aalallon: I t
Exygen Research
Page 45 of 132
000288
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P001131
Table V. M atrix Spike Recovery o f PFOS in Re-extracted Fish Samples
Sam pio Deaeria6on
DBC-FO H PW 001-0-041021 (Q004S151SffcC, lODOppb)
D0C-FOHPWOO2-O-O41O2t (00041 Sph D. 6000 ppl>)
DBC-FO1-I PW003-Q-Q41021 tcooeatsa sta c. toon ppb)
DOU-F01-IPF001-0-041021 (COMaiuSpkP, tu n ppb)
DOU-F01-IPF002-0-041021 (CotM usspfco. moou
0O U -FO 1-IP F00KM M 1021 (CO044165SpkH, IMO ppb)
DOIJ-F01-IPW0Q2-0-04 1021 (COOdOtMSpkl. 1000ppb)
D BC-F01-M SW 001-<W 41104 (COG4048QSPU KUXppb|
DBC-FO 1-MSW002-0-041104 (CQOM4S1 Spk K, 10,000 ppb)
DBC-RM -MSW003-0-041104 {COQ4Q462 Spt(L, 10,000 ppb)
DBC-F01-M SW 004-O O 41104 (C00404WSpk Ml SOOOppb)
DBC-F01-M SW 005-0-041104 (COOW454SpkN. 10,000 ppb)
D8C-F01-M SF001-M 41104 (C004M66 SpkC, 10,000 ppb)
OBC-FOI-MS F002-0-041104 (CO04MM Spk0,10,000 ppb)
DBC-F01-IPF005-&041104
(0004M60Spk e. 1000ppb)
OBC-F01-IPW 004-0441104 (C0M94M 8pk F, WOOppb)
DBC-FO1-IPWO05*O-O41104 (C0049450SpkG, 5000ppb)
DOU-F1-IPW 003-0-041104 fOOCMMOl Spk K 1000 ppb)
DOU-F01 -1PWD04-0-041104 {CO04M42Spk>, 1000ppb)
D O U -F01-IPW 006-0-041104 (C004M03 SpkJ, 5000 ppb)
D.1-F01-M SW 001-0-041104 (0004M66 Spk K 1000 ppb)
DL1-F01-M SW 0020-041104 (C00404MSpfcC, 1000ppb)
DL1-F01-M SW 003-0-041104 (0004M67 Spk 0, 1000ppb)
DL1-FO1-MSWO5-0-O411O4 (C004M5BSpk S, 1000ppb)
Amount Spiked (no/a)
1000 SOOO 1000 1000 1000 1000 1000 10000 10000 10000 SOOO 10000 (0000 10000 1000 1000 SOOO 1000 1000 SOOO 1000 1000 1000
1000
e g Sulfonate PFOS
Am t Found in Sample (ng/g) wet w t
Amount Recovered (notai w et w t
Recovery <%> ...
2080
2880
76
3330
8680
107
I8 6 0
3160
150
998
1760
116
836
1740
110
644
1650
111
1210 9480
2610 23200
140 137
7820
16800
91
12800 3440
23200 8520
108 102
5240
16200
100
5240 4780
14400 15200
92 104
80S 1230
1600 2690
99 13
2B20
8620
78
2270
2640
37*
1740
2740
100
2130 968 708 696
7600 1660 1780 1930
109 89 107 123
804
1680
108
Not reportad do* lo quality control raault(allure. Vdftioa are notIncluded m the turenw y etelc
Exygen Research
Page 46 o f 132
000289
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table V. M atrix Spike Recovery o f PFOS in R e-extracted Fish Sam ples (continued)
Sampto D escription
DOU-F01-IPF0O4-(M>41021 (C004S167GpkJ. 1000pfifc)
Q O U -F01-IPW 001-04M 1021 (C004*100S[*K, 1000 ppb)
D L1-F01-M S F004-0-041104 {G0MM73 Spk L W D ppb)
Amount Spiked (no/o)
1000
1000
1000
C8 S u tfo n a f PFOS
Am t Found in Sample
Amount Recovered
(n o ^ )w a tw t (na/o)w atw t.
Recovery [% )
424
1620
110
387
1480
109
348
1400
105
A vang* Standard D n M a w
1M 20
Exygen Research *
- A ' ' ' ' - <
Page 48 of 132
000290
p.48
Interim Report# 10-Analysis of Fish and.Clara Samples
Exygen Study No.: P0001131
Table V. M atrix Spike R ecovery o f PFO S.in R e-extracted Fish Sam ples
Sam pto D aacriotkn.
(continued)
CB S u io w ta PTOS
Amount , S p thad
(0 0
Amt Found In Sample (nota)w etw l
Amount
R ecovered
(note) w e t w t
Recovery (%)
DL1-FO1-MSF0Q2-O-0411O4 (00040471 SpS F, 10S0act!)
DLt-F01*M5F00MK>41104 (0O4M72Sfik G, 1000 ppb)
OL1-F01-MSF006-0-041104 (C004W74Spk H. 1000,Kb)
MC-F01 -MSW 005-0-041105 (C0949496pfc 1,1000 ppb)
;
, 1000
1000
P
1000
1
665 . . . 1690
fy ' 432 _ '
' 70
740 18W> 560 1780 '
112 124 109 122
DMC-F01-MSF0024W>41106 , (0004941Spk J. 1900ppb)
1090 ,
620
' 1500
88
DOU-F01 *MSW002*0-041210 <009994*0SpkK, 10,000ppb)
QOU-FOl-MSW03-0-041216 (COOBMSBSpk L,8000 ppb)
DOU-F01-MSW001-0-Q41216 <00000400SpkC, tOOOOppb)
10000
5000 10000
! I
26200 4040 7600
' 32700 10200 26000
45 123 174*
DOU-F01-MSW004-0-04121 (C000040I Spk D,0000 ppb)
5000
5120
9680
96
DCHJ-FD1-MSW006-0-04121
(C0066462Spk E, 1000ppb]
1000
466
1780
126
DOU-F01-MSFQ05-0-041216
(COO5O4035pk F, 1090 ppb]
1DOO
720
1620
110
OU-F01-MSF003-0-G4121 (00000400 Spk G, 1000 ppb)
DBC-FG1-MSFD05-1-041216 (C0000407Spk H, 10000 ppb)
1000 10000
846 6320
1720 32400
87 230'
DBC-F01-MSFD05-0-041216 (C0060400Spk 1,10000 ppb)
10000
6960
24100
151
DOU-F01-MSF02-0-041216
(C0056409Spk J, 1000ppb)
1000
640
1720
108
DOU-F01-MSF02-1-04121B (00050471 Spk K, 1000 ppb)
DOU-F01-MSF004-0-041216 (00050472 Spk L. 1000ppb)
1000 1000
692 1820
1950 2700
126 88
DOU-F01-M SF001^041216 (C0090473Spk C, 000ppb)
soco
2070
.7 9 6 0
118
OBC-F01-MSFD03-O-O41216 (C0000474Spk 0,10000 ppb)
10000
4640
15500
109
DBC-F01-MSF004-0-041216 {00050478SpkC, 10009PPb)
OMC-F01-MSF001-0-041216 <00000470Spk Ft100Oppb)
10000 1000
9280 840
24500 2040
152 120
OBC-FO1-IPF001-0-041021
(C0040140 Spk G, 1000 ppb)
1000
384
1360
97
DBC-F01-IFF003-0-041021
<CQ049180&phH. 1000 ppb)
1000
203
1340
106
DOU-F01-1PF0050'041021
(C00401MSpk I1000 ppb)
1000
366
1400
104
Not reported dua toquality conantremitfakires. Valasare notincluded fr Iha summary ataMics.
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
FIGURES
Exygen Research *;h . **, h
Page 50 of 132
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table VI. M atrix Spike R ecovery PFBS, PFHS and PFOS in Clam Sam ples
ampte
DLW01-CW 001-0-041216 (COO-OS'* C.ttpM
DU-01-CPWOOHHM1216 lCnwmpQ, looppci)
DM0401-CFW0014KH1216 (Coowin akK, tepyfcj
DMXOI-CFW00MKM131H tCM--411Sc*f, HBppb)
OL2-W1-CFW001-0-041210 (C e a * 8 9 * w ffii
L2-101-CFW001-0-041216 (cm--ig a K wan*)
DBG4Q1-CrW(H1-0441216 (000-- 1 * 1.10*6}
DBC*I01-CFWOQ1-(M)41215 <000M--apkJ, tttH ft)
OL1-W1-CPW001-0441210 (C00--maphK.iopft4
DU4OVCFWOOMMK1210 IQX6M94Sc*L HOn*>
OOU-Wt-CFWOO1-0-041210 (C009-- 3pfcM,10lvU
D0tw0l-CPM0014-04121B (Cn-- spkN, iDoprni
Amount AmiFound
10 NO too ND 10 NO 100 NO 10 ND 100 NO 10 ND 100 ND 10 ND 100 ND 10 ND 100 NO
Am ort
90 2.4 04 2.0 7.20 836 103 044 8l86 802 048 4.4
Am)Found Amount
Ant Found
Rfloonwy InSWttpl* Reooimd R*coy
f t l <*>
00 ND & te 2 1.92
2 ND 6.0 96 1.92
90 ND 44 94 16 03 ND 80.8 9 6.16
n ND 4 ND 103 ND 4 NO
?.w 79 ro t 101 101 1.91 10 100 4.48 97,2 97 4.46
0 ND 08 ND
9.32 93 8.eo 103 M3 8.00
86 0.202 8.92 81 11.4
84 0.202
6.0
96 11.4
Amount
32 86.5 11.8 92-6 7.52 884 130 Ml 16.0 88 17.2 8.0
fW ' 46 83
61 67
87 87 86 82
82 88 88 87
04 10
NO Not(tatecMlor bowUinit ofOuanUMiMwhich to0.2 flir t
Mai. nei WJmflwflim tolflo
mu, rgwi.v>i n yiy igN>r twi.
Manta: 93 9--Mlafd OavMcnt 19 hrll.
A -a a : 7 tta n tM DMstlani 1
H 1
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Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 2. Non-Extracted Standards o f PFBS in M ethanol, 0.0005 (ig/mL and 0.001 fig/mL, Respectively
I sara* p m Arms.-I M cmM
m .* lC n u r -umpl* i n * from Mfs<Mwfflr -/
tntercsity. cps
0.61
300
a' CL
i 200
I
1
so
o-i 1 2 3 4 6 6 7 0 0 10 11 17 13 14 16 16 17
8S727prBcstjnUf42pgjaiaaj9amumpi.2itaainmaeisoBEjNIIi(M. min
M r 1SSS7 aw n* N .ljU -T B r <f> *1.0.515 mta
062
I700
BOO-
Intend^, cps
U
IM 0`
|
I 1300
" 3001P1100
122
3 J 1 AT
3.1^
0-J
123 46
0.27 07
0.10 10.00 ^10.
00
10 11 12 t3
tim e, atin
14 16
10 17
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 1. Typical Calibration Curve for PFBS in M ethanol
M M O S I F la ti.,* (F F M )[ ` U n u f Kis m I m f W w alfM I*g> 1-1X>4x + J.07t*00 3 ( r - 0.M 8)
Area, counts
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Interim Report #10-Analysis ofFish and Gam Samples
Exygen Study No.: P0001131
Figure 3. FFBS in Control Fish Blank, 0.00625 ng/mL Fortified C ontrol Fish Spk A , and 0.025 |ig/m L Fortified Control Fish Spk B, R espectively
I O u g u itCm lOrM / W (tMtirmm)29M O M m ft*offertdP
9 f3ifto w N N K sd r
| Reagent 9pfcA* r F ff (QC)290.0(090 mu-simple 10 liS S im n OOIOOQSjhW *ei:74474eounfc Height 1100. eps *1:4.42 n
AA2
8 9 10 11 12 13 14 10 10 17
Tim, min | Re*ghl 9pfc B. PTO*(OC)200.0000 mu. simple 11 et30 Mm OBIOOBEjmHT
* e j: 330020 VMS HOfght 16000. op *T ` 027 min
Li0.00
a
1.0*4' 1.0*4'
1 0000.0
0.0
2 3 4 0 0 7 8 9 10 11 12 10 14 10 19 17
Time, min
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Interim Report # 10-Analysis o f Fish and G am Samples
Exygen Study No.: P0001131
Figure 4. Chromatogram Representing a Fish Sample Analyzed for PFBS (Exygen ID: C0049478, Data Set:061605E)
MMI
A im 4 V h Ni H tfttb
-im p
K ti M M m ta
NfM SEftflr
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 5. Typical C alibration Curve for PFHS in M ethanol
W1B05E
(PFHt "Lift#' R > |m I ii>f t ' * wlfMl y - 2.M X 004 x + 3JM 0 0 3 ( r - 0M S1)
Area, counts
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 6. Non-Extracted Standards o f PFHS in M ethanol, 0.0005 pg/mL and 0.001 pg/m L, R espectively
Intensity, cps
I B 8 7 m *P fH 9 frm rt) H A M M m -m m pk 1 o M A m itm t rn k H ffi t 74*. cp* RTi M m *
f CNEmflr
700
000 000
400
300
300
100
0
I 887279 HPH( ftjn d * 9 Q G i> * 0 A hui - um 0 2 *188 Item OettOOE^iff
Amt: 3317 MM
1390.00 KT:103 min
10.33
11 12 13 10.33
1300 iOOD 900 eoo400
200
D-
11.16
13.73
10 11 12 13 14 10 10 17
Menait)', cps
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Interim Report #10-Analysis of FiBh and Clam Samples
Exygen Study No.: P0001131
Figure 7. PFHS in Control Fish B lank, 0.00625 pg/m L Fortified C ontrol Fish Spk A , and 0.025 pg/mL Fortified Control Fish Spk B , R espectively
AMpMrt CMtfp t
|U itM w r;7 IU M J in
9 of 39fr*m N fM E w ilf
1151
Intensity, eps
Ai m : 100711 COtwin Jtlfll* 12000. cp> RT: 1 0 3 min
Intensity, cp*
Intensity, cps
Atm: 721071 oeuntt
3X>4' 2X>4` 1jO*4
0.0 J -
30100. c p AT: 10.0 min
10JB
B7
0 0 10 11 12 1 14 16 16 17 Tim, mln
Exygen Research ( ' _\ ! -r\
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 3. Chrom atogram Representing a Fish Sam ple Analyzed for PFHS (Exygen ID: C0049478, Data Set: 061605E)
-M a p * JO fM trom M tfM u fflr
Ami 2McMw(rHtigmt m * ten
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 9. Typical C alibration Curve for PFOS in M ethanol
a e ie o s e F I l> .rik (W O S ):n jn a ir R agrurtcn f t / i f N algM ifl) y - l.1 4 rH M 4 x *3 .3 # *0 0 3 (> -0 0 6 0 9 )
Area, counts
Exygen Research
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interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 10. Non-Extracted Standards o f PFOS in M ethanol, 0.0005 jig/mL and 0,001 pg/m L, Respectively
I n r m -P fo s & **4**)
m m - m ip * #o fa u t * tttm & w n r
Atm?SUcmm* M U g t 4 i l t p * T i t l i m *
12.40
Inlensifer. cps
Irrlensttr. tp s
Am 14B67 mo * H dtfri: 000. m AT: 12a ml
700
000 000
400 300
200 100
Qi -- --r
1
12.40 Thu, mi#
Exygen Research
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Interim Report if10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 11. PFOS in C ontrol Fish Blank, 0.00625 p.g/mL Fortified Control Fish Spk A , and 0.025 pg/m L Fortified Control Fish Spk B , R espectively
Intensity, cos
Intensity, tps
fta f t C uir/ At m ; I M c m iO M iflC S M cp* R7
fofJIO M S OifWSRwW
4P-
2G
0i
0yMv.1*1
4.40
1 A a
34
12.10.
11p*
0 6 10 11 12
TJim , ml
I R u g " * OpkA- P F0*(O C )4M06J.a0O m u-sjm pli 10 of 36 to *0010096 wHf
Ana: 71600 ooun* Haight: 4940. OM RT: 125
13.16 13
1457
,10.00 17>00% 1751 , i . 4k,
14 19
4000 2000 <
0
A12.40
7 0 0 10 11 12 13 14 19 10 17
TMm , mi*
I K ia fin l 6p)r 0 PFOf (QC)40Bjfl0J amu im pk 11 af 30 from O01OD0E.WM Arta: 207141 m u i* Hilght: 10000. c*s RT; 129 mo
1,9*4 14>4 90000
09
12.40
A
0 B 10 11 12 13 14 19 19 17 TIfTM, mi
Intensity, cps
Exygen Research .. i ! J ',3 i *H
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 12. Chromatogram Representing a Fish Sam ple Analyzed for PFOS (Exygen ID: C0049478, Data Set:061605E)
CfM Hn PFOt <tM ww04NHM LM -N a p k H o tM fn m MMMEwttr
M i l M 2 M ff CMNrir M itgtt! O M M l
milI
12.47
Exygen Research
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Interim Report #10-Analysis o f Fish and G am Samples
Exygen Study No.: P0001131
APPENDIX A
Study Protocol P0001131
(Exygen Study No. P0001131) with Analytical Method,
Protocol Amendments 1 and 2 and Deviations 2 and 3
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Exygen Study No.: P0001131
ExygenProtocolNunfer P0001I31
STUDY PROTOCOL
Study Title: Analysis of Perfluorobutauesulfouate (PFBS),
Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) In Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small
Mammal Seram Using LC/MS/MS for the 3M Decatur Monitoring Program
Exygen Protocol Number: P0001131
Put-fanning Laboratory: Exygm Stw tick
3058 Research Drive State College, PA 16801 Phone: (814)272-1039
Sponsor Representative; Michael A . Santoro Director o f Regulatory Affaire 3M Building 0236-01-B-10 S t Paul. MN 55144 Phone: (651) 733-6374
Pnjfc l v j 6S
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Exygen Study No.: P0001131
Exygen Protocol Number: POOD(131
DISTRIBUTION:
1) Jaiaunh* K enri, Study Director, Weston Solution 2) John M- Fliberty, Principal Investigator, Exygen Research 3) Michael A. Sintoro, Sponsor Representative, 3M Company 4) Exygen Research Quality Assurance Unit
Exygen Research
Page 1 o f65
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Interim Report #10-Analysis of Fish tod Clam Samples
Exygen Study No.: P0001131
BxyieaProtocol Number. POMI 111
PROTOCOL APPROVAL
Study Title: Analysis ofPerfluorobutaneiulfonate (PFBS), PerfluorohexaneaulforiMe (PFHS), and Perfluorooctanetulfonato (PFOS) in Water, Soil, Sediment, Fish, dam a, Vegetation, Small Mammal Liven and Small Mammal Scrum Uaiag LCA1SMMS Jbr the 3M Decatur Monitoring Program
Exygen Protocol Number: P0001131
APPROVALS
JaiaimhaQ Weiton Solution
hector
Michael A. S^fitoro, Sponsor Repreacntative 3MComp
>lut M. Flaherty, Principal Inveatigitor / Exygen Reaearch
U .___________
ad. Quality Aaaurance Unit
Date
zt-ccr-id q t
Date
Page 3 o f 65
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Interim Report #10-Analysis o f Fish aodClam Samples
Exygen Study No.: P000131
Exygea Protocol Number P0001131
TABLE OF CONTENTS
TITLE PAOE......... e r s ttu b u tio n .... p r o t o c o l a p p r o v a l .. TABLE OF CONTENTS.... INTRODUCTION....... TEST MATERIALS .... OBJECTIVE............... TESTING FACILITY.. STUDY DIRECTOR.... SPONSOR REPRESENTATIVE... PRINCIPAL INVESTIGATOR.... PROPOSED EXPERIMENTAL START ANDTERMINATION DATES . IDENTIFICATION AND JUSTIFICATION OF THE TEST SYSTEM..... SAMPLE PROCUREMENT, RBCEIPT AND RETENTION__________ SAMPLE IDENTIFICATION.................................................................. ANALYTICALPROCEDURE SUMMARY ---------- ----- ... VERIFICATION OP ANALYTICAL PROCEDURE__ .....___________ METHOD FOR CONTROL OP BIAS................. ......... ........................... STATISTICAL METHODS_____ GLP STATEMENT..... ................. REPORT..................... ................. SAFETY AND HEALTH----------AMENDMENTS TO PROTOCOL. DATA RECORD KEEPING_____ QUALITY ASSURANCE----------RETENTION O f DATAAND ARCWVINO... APPENDIX L ANALYTICAL METHODS......
................................. I
...... ................2
........................ -.3
..... ..............
4
.............-................ S
............................... 7 ............................... 7
....................... 7
.................... 8
...
... ... ...U
...II ...II ...I) ...12
...13
...IJ
...14 ...14 ...IS
Pogc 4 o f Si
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Exygen Study No.: P0001131
Protocol N u n to r P0001131
INTRODUCTION
The purpose of this study it to perform analysis for perfluorobutanesulfonate (PFBS), perfluorohexanesulfonste (PFHS) and perfluorooctancsulfonate (PFQS) in water, soil, sediment, fish, clan, vegetation, small mammal liven and smell mammal aerum using LC7MS/MS for the 3M Decatur Monitoring Program.
The study will be audited for compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by the Quality Assurance Unit o f Exygen Research.
TEST MATERIALS
The test materials are perthrorobutaneauUbnate (PFBS), pcrfluorohexaneaulfonate (PFHS) and perfluorooctansulfonate (PFOS) and are ail aupplied by 3M
PFBS Chemical N am e Pcrfiuorobutin caulfonatc Molecular Weight: 338 supplied as the potassium salt (C<FS0i'lO Lot Number: 101 Purity: 96.7% Transitions Monitored: 299-99 Structure: F- f
PFHS Chemical Name: PerfluorohexanenilfooatB Molecular Weight: 438 supplied as the potassium salt (CsFnSO jTO
Lot Number: SB036 Parity: 9S.6H
Tianaitions Monitored: 399-a 80 Structure:
P sg tio f i
Exygen Research
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000311
interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
ExygcnProfoco] Number: POOOII31
pros
Chemical Name: Perfluarooctanetulfonate Molecular Weight: 538 (applied a t the potaseiiim aatt (CtFnSOjTC*) Lot Number: 217 Purity: 86.9% Transitions -Monitored: 499-* 99 Structure:
f
F- .SO,'
OBJECTIVE
The purport o f th it rtudy ii to perform analyaia for perfluoiobutanciulfonate (PFBS), perfluorohexanesulfonate (PFHS) and perfluorooctanesulfonate (PFOS) in water, toil, sediment, fish, clam , vegetation, amali mammal live and amali mammal aera for the 3M Decatur Monitoring Program using the current versions o f foe following Exygen analytical method:
V000178Q: "Method of Analyaia for foe Determination o f Perfluoroocianoic Acid (PFOA) in Water by LC/MS/MS"
V0001751: "Method o f Analyaiafo r foe Deteoninaiion o f Perfluoroocianoic Arid (PFOA) in Soil by LC/MS/MS"
V00017S2: "Method of Analysis for foe Determination o f Perfluorooctanoic Arid (PFOA) in Sediment by LC/MS/MS"
V0001783: "Method o f Analyaia for foe Determination o f Perfluoroocianoic Arid (PFOA) in Fish and Clama by LC/MS/MS"
V0001784: "Method o f Analyii* for the Determination o f Perfluorooctanoic Acid (PFOA) in Vegetation by LC/MS/MS"
V0001785: "Method of Analytic for foe Determination o f Perfluorooctanoic Acid (PFOA) in fonali Mammal Liver by LC/MS/MS1'
V0001786: "Method of Analysis for foe Determination o f Perfluorooctanoic Acid (PFOA) in Small Mammal Serum by LC/MS/MS"
TESTING FACILITY
Exygen Research 3058 Research Drive ' State College, PA 16801 Phone: (814) 272-1039
Pag* $ o f i f
Exygcn Research
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
B x y j n Protocol Nun*: P000131
STUDY DIRECTOR
Jaiwinha K enri P.E., DEE W eiten Solution, Ine. 1400 Weiten Way W eit Cheiter, PA 19380 Phone: (610) 701-3761 Fax: (610) 701-7401 j.keari@weatonolution*.conj
SPONSOR REPRESENTATIVE
Michael A. Santino 3M Company Director o f Regulatory Affaira 3M Building 0236-01-B-10 St. Paul, MN 33144 Phone: (631) 733-6374
PRINCIPAL INVESTIGATOR
John M. Flaherty Exygen Reaarch 3038 Reaearch Drive Stete Collega. PA 16801 Phone: (814) 272-1039 johnA alierty@ exygen.eoin
PROPOSED EXPERIMENTAL START AND TERMINATION DATES
It ia proposed that the analytical portion o f this study be conducted from October 01, 2004 to December 31, 2005. H ie actual experimental start and termtoatiofMlatw will be included in the final report.
Page
Exygen Research i* ;,
Page 70 of 132
000313
Interim Report #10-Analysis o f Fish and Clam Samples
, Exygen StudyN o.: P0001131
ExygvoProtocol Number P00Q1131
IDENTIFICATION AND JUSTIFICATION OF THE TEST SYSTEM
The following a * foe test system! for foie study: Water (groundwater end surface water) Soil Sediment Fish Clams e Vegetation e Small Mammal Liver a Small Mammal Scrum
The samples will be collected by Weston Solutions. The control samples will be purchased and prepared by foe testing facility. Purchase and processing details for foe control samples w ill be included m foe final report associated w ith this study.
The test systems were chosen to access the environmental impact of PFBS, FFHS snd PFOS in the Decatur, Alabama area.
SAMPLE PROCUREMENT, RECEIPT AND RETENTION
Water, oil, sediment, fish, d u n ,, vegetation, small mammal liver and small
mammal serum sample w ill be received at Exygen directly from Weston
Solution. The details o f sample procurement for this study lie outlined in the
3M work plan entitled "Phase 2 Work Plan for Sampling Environmental
Media." The number and type* o f sample collected w ill vary depending
availability in foe field. The total number o f ample received and analysed
for each matrix will be documented in foe final report associated with this
study.
'
Water, toil, and sediment samples w ill be used at received without further processing at Exygen. These samples will be stored refrigerated at 2C-8"C.
Fish, dam , vegetation and amali mammal liver, samples w ill be processed according to the appropriate analytical method (see Appendix I). These ample* will be stored ttaaxn at s >10*0. Small mammal whole blood ampio will be centrifuged in the field at foe time o f collection and the serum traction will be uaod for foe study. Small mammal serum will be stored
fatten at i -10*C.
The receipt end processing of the samples w ill be documented in the final report and raw data associated with foe study.
ftig*$of6S
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No;: P0001131
Exyfsn Protocol Najrtwr. POMI 131
SAMPLE IDENTIFICATION
Prior to analysis, each ample will be atsigftod a laboratory sample reference number. The reference number will be unique and will distinguish each laboistory sample tin t ia processed throughout the analytical procedure. Chrometogrlphlc data will be identified by the Laboratory sample reference number.
Sample storage conditions u d locations will be documented throughout the study.
ANALYTICAL PROCEDURE SUMMARY
References: V0001780: "Method o f Analysis for the Determination o f Perfluorooctsnoic
Acid (PFOA) in Waturby LCMS/MS" V0001781: "Method o f Analyais fbr the Determination o f Perfluorooctanoic
Acid (PFOA) in Soil by LC/MS/MS" V0001782; "Method o f Analysis for the Determination o f Perfluorooctanoic
Acid (PFOA) in Sediment by LC/MS/MS" V0001783; "Method o f Analyais for die Detenmination o f Perfluorooctanoic
Acid (PFOA) in F iih aid Clams by LC/MS/MS" VOCO1784; "Method o f Analysis for the Determination o f Perfluorooctanoic
Acid (PFOA) in Vegetation by LC/MS/MS" V0OO1783: "Method o f Analysis for the Determination o f Perfluorooctanoic
Acid (PFOA) in Small Mammal Liver by LC/MS/MS" V000178d: "Method o f Analysis fbr the Determination o f Perfluorooctanoic
Acid (PFOA) in Small Mammal Senun by LC/MS/MS"
The above methods use analytical conditions capable o f separating the isomers o f PFBS, PFHS and PFOS. The final report w ill include the isomen summed into total PFBS. total PFHS. and total PFOS found.
VERIFICATION OF ANALYTICAL PROCEDURE
A laboratory control sample will be used for the preparation o f fortified control samples. The test substance w ill be made into solutions as per the method, and added to the matrices via a micropipette.
For water sampling, Bxygcn will supply one bottle per sample collected. The bottles will be 500 mL prodesned Sci/Spec Premier wide mouth KDPS bottles. These bottles have been routinely used fbr fluorochemicat sample
Page 9 o f6$
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Exypeo Protocol Number: P0901131
r * collection i t the to tin g facility and hive been rtwwn to be free o f PFBS, PFHS and PFOS. Samples will be added to each container to a volumetric fill line i t 200 mL. A field duplicate, a low field spike and a high field spike o f each sample will be collected. The low and high field spike bottles will contain PFBS, PFHS and PFOS as well us perfluorooctsnoic acid (PFOA) and
. U -13C pcrfluorooctanoic acid (,3C PFOA). PFOA and ,3C PFOA are included in the solution used to spike the samples. The results for PFOA and l3C PFOA will not be repotted in fins study. Exygen will supply one field blank (control water) and two field blank spikes (control water fortified with PFBS, PFHS and PFOS at a low and high level) for every twenty samples collected. At the testing facility, each water sample (excluding field duplicates and field spikea) w ill be extracted in duplicate and w ill alio be fortified at a low and high concentration with PFBS, PFHS and PFOS and processed throughthe described procedure to determine method accuracy and to check fos bias.
For soil, sediment, clams, and vegetation, Exygen w ill supply one 500 mL proeleaned Sc/Spec Premier wide mouth.HDPE bottle per sample collected or a zip-iesl bag. A ll contaiaers/bag* used for sample collection will be shipped to the sample location. Samples will be added to each container or bag in the field. At the testing facility, each sample will be extracted in duplicate and will alio be fortified at a known concentration with PFBS, PFHS and PFOS at both a low and high level and processed through the described procedure to determine method accuracy and to check for bias.
For sm ill minimal liver, Exygen w ilt supply a 50 mL polypropylene centrifoge tube: For small mammal scrum, Exygen will supply a collection left for each sample containing aerum separator tubes (red top), vaeutaineis,
needle holdera and needles, transfer pipettes, and polypropylene tubes. At the testing facility, each liver and serum sample will be extracted In duplicate and w ill also be fortified at a known concentration with PFBS, PFHS and PFOS at both a lew and high level and processed through the described procedure to determine method accuracy and to check for bias.
Low and high spiking levels for each matrix arc defined below:
M atrix
Law SolU ns Level
High Snikinu Level
W ater
SOOng/L
5000 n e /L
Soil
4m t/it
40 nn/fi
SodtsTM nt
a n a /a
4 0 no/cE
n>h .
10as/g
lOQng/g
Clam*
JLOntfg
lOOnx/x
Vegetation
10 note
lOOtlfita
Small Mammal liv er
lO w tfa
lOOng/g
Small Mammal Serum . 10 nnfaiL
IOOmt/mL
Pagt Oofas
Exygen Research ' :S
Page 73 of 132
000316
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
E*yjen Protocol Number: P0001131
/v Recoveries arc anticipated to be between 70% and 130% o f the fortified levels; however, die exact precision and accuracy w ill tie determined by the analyda o f die quality control samples described above. A statement of accuracy will be included in the final report
METHOD FOR CONTROL OF BIAS
Control o f Mai will be addressed by taking representative sub-samples from a homogeneous mixture o f recti matrix from untreated control samples, and by analyzing at least two levels o f fortifications.
STATISTICAL METHODS
Statistics will be limited to those specified in die subject methods and to the calculation o f avenge recoveries as applicable.
GLP STATEMENT
All aspects o f this study shall be performed and reported in compliance with EPA 7SCA Good Laboratory Practice Standards 40 CFR 792. The final report or data package (supplied to the Sponsor) shall contain a statement that the study was conducted in compliance with current and applicable GLP standards and will outline any deviations la the study from (base standards. This statement will be signed by the Study Director and Sponsor Representative.
REPORT
A final report w ill be prepared by the principal Investigator or their designee at the coadnsioo o f the study. The report w ill include, but will not be limited to, the following: a The name and address o f the Study Director, Sponsor Representative, and
of the testing facility.
A statement o f GLP compHanee (any related documentation, such os chain-of-custody records, must be in the study records).
PUf* U of6S
Exygen Research
Page 74 o f 132
000317
Interim Report ^10-Analysis o f Fish and Clam Samples
Exygen Study No,: P0001131
Exygsn Protosol Number: P0001131
The signed and dated statement by the Exygen Research Quality Assurance Unit regarding dale* o f study inspections and dates findings were rsported to the Study Director and Management.
A deaoription o f the exact analytical conditions employed in the study. I f the subject method was followed exactly, it if necessary to include only a copy of the analytical method. Any modifications to this method will be incotporated into the report. I f the method is photo-reduced, the project number and page number most be included on each page.
Description offoe instrumentation used and operating condition*.
All result* from all seta analyzed Control and fortified samples will be identified and the data table wilt include sample number and fortification Level.
Representative chiumatognms for each analyte in each matrix, including chromatogram* o f a standard and a control sample, and a chromatogram at a fortification level. The location of the analyte peaks w ill be clearly identified in all chromatogram*
All circumstances that may have affected the quality or integrity of the data will be documented in the repost.
Locations where raw data and foo final report are to be archived.
. Additions or corrections to the final report shall be in the form o f an amendment signed by foe Study Director. The amendment shall clearly identity that part o f the report that is being altered and the reasons for the alterations. The amendment w ill be signed and dated by the Study Director and 8m Sponsor Representative.
All applicable requirement! for reporting o f study results u per 40 CFR 792.185.
SAFETY AND HEALTH
Laboratory personnel w ill practice good sanitation end health habits.
Every reasonable precaution shall be taken to prevent inadvertent exposure o f psnonnel and the environment to foe test or reference substsnce(e).
Pagt 17 o f 65
Exygen Research
Page 75 of 132
000318
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Exyjen Protocol Number: POOOI13J
AMENDMENTS TO PROTOCOL
All significant change* to the aaalytieal protocol outlined hero will be eotpnased in writing, signed and dated by the Study Director and Sponsor Representative. Amendments usually will be issued prior to initiation o f study plan change. However, when a chnge is required without sufficient time for the iseue o f a written amendment, that change may be effected verbally with supporting documentation signed and dated by the Study Director and followed with a written amendment a t soon a t possible. In this case, the effective date of the written amendment wilt be the date o f the documented change. Copies o f the signed amendment* will be appended to all distributed study plan copies. The original amendment w ill be maintained with the original study plan. Any deviations from the study plan or from the analytical method a* provided will be documented and reported promptly to the Sponsor Representative.
DATA RECORD KEEPING
Records to be maintained include the following (as appropriate):
3aff.ple tracking sheet(s) Sample receiptrecent*, storage history, and chains o f custody History and preparation of standard* (stock, fortification, calibration) Description o f any modifications to the method hwtiument run sheets, bench-sheets or logs Analytical data tables All chromatographic and instrumental conditions Sample extraction aad analysis date* A complete fisting o fstudy personnel, signatures and initials Chronological presentation of all study correspondence e Any other documentation necessary for the reconstruction o f tho study
Chromatograms- All chromatograms w ill contain the following:
Sample identification, injection date, arrow or other in d icatio n o f the area o f interest, and injection number corresponding to th e run.
Additionally, fortifications w ill include the amount of analyte added aad the sample numbero f the sample that seat fortified.
Analytical standard chromatograms will additionally include the concentration (e.g., pgtoL).
Pm n of
Exygen Research
Page 76 o f 132
000319
Interim Report #10-Analysis o f Fish and CIam Samples
Exygen Study No.: P0001131
Exygen Protocol Number: P0001131
As part o f the documentation the following sheets wilt be included in each analytical set; a run sheet listing the sample* to be n u in the set, and an
instrument conditions sheet describing the instrument type and operating conditions.
QUALITY ASSURANCE
H e QA Unit o f Exygen Research win inspect the study at intervals adequate to assure compliance with GLP's, and w ill report the findings o f audits to the Study Director, Exygen Management, and the Sponsor Representative.
RETENTION OF DATA AND ARCHIVING
, i-
- r
All hard copy raw data, including, but not limited to, the original chromatograms, worksheets, correspondence, and result shall be included
with die data package submitted to the Study Diiector. These will be archived with die original study plan, amendments, {foal report, and all pertinent information from the Sponsor.
The testing facility shall keep all electronic raw data and any instrument, equipment, and storage logs' foe the period o f time specified in 40 CFR 792.195. An exact copy o f the materials submitted to the study director will also be kept at Bxygen Research.-
Exygen w ill obtain permission from the study director before discarding or
returning sample*.
'
Exygen Research
F a g t (4 offiS
Page 77 of 132
000320
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No,: P0001131
Exygn Protocol Number POOOl131
APPENDIX I
ANALYTICAL METHODS
V0001780: "Method o f Analytic for the Determination o f PeriluoroocUnoic A dd (PFOA) in Waterby LC/MS/MS"
V0001781: "Method o f Analyaii for the Determination o f PerfluoroocUnoic Acid (PFOA) ki Soil by LC/MS/MS"
V0001783: `M ethod o f AnalytU for the Determination o f Perfluorooctanoic Acid (PFOA) m Sediment by LC/MS/MS"
V001783: M ethod o f A iulyiia for the Detenninadon o f Perfluorooctanoic Acid (PFOA) in Fleh end Clama by LC/MS/MS"
V0001784: M ethod o f Analyaii for the Determination o f Perfluorooctanoic Acid (PFOA) in Vegetation by LC/MS/MS"
V0001783: "Method o f Analyeis for the Determination o f Perfluorooctanoic Acid (PFOA) in Small Mammal Liver by LC/MS/MS"
V0001786: M ethod of AnalyaU for foe Determination of Perfluorooctanoic Acid (PFOA) in Small Mammal Serum by LC/MS/MS"
Exygen Research
Pag* IS e fts
Page 78 of 132
000321
Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P001131
Exygen Protocol Number: POOOII31
ANALYTICAL METHOD H K W N n b c V 9 0 0 I7
H r I k n m ih i i rfl
l< A (M (P F O A )la W ant
Analytical Tactio* Facility:
l*ySniUwwdt
3099 RoNwvh Drive 3 ttU O tf*f*,? A U IO l
AppaovadBF
"B A c-A L
VP aaotlCCoHmHolItj
'
TmM coI bmw. IC-MS, S ly p e SiMnfc
10111AW
DM*
/TtalFUMV i
' ViooPm ieil. OreH inM,S iy | ta mb
.jgAdi
DM
Exygen Research
ToUIPapo- 7 P e g tl c f6 S
Page 79 of 132
000322
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxygeu PrnlOMl Number: P0001131
' 1 ' J^ALtlTCALMaTWOP
tdtobedefAaajtpbfe rie CMmabw VlWuomoctmefc Acid(PFOA) in Weterby LC /M IAIl
L.O Su m
TUr a u ta i ii ta
fa iMhdaa amifumiiMiB irfp n u M M cao eic
fa d by H fa Nrtiitoenm Liquid Cbnutetodfay cwwtod to imdem Man
2J0 S M 1 , I t Alw)e obeernfab ttim w prmlco. 12 Ccufaifa to|yiltoi 1ITO8blfcw bmdH| ytfamiitil fa pmperlefety
jjO SuvblfabMU
1.1 Atfa il 40d*. fifa duplefa eebfaton. 12 M n a fa ifiM e ifa tU deededfa weareanplM. 1J Saaepfatoend rettputoad fande be allmnd n aqidlfentt < mm
2.4 AM-- p fa -- belbw w ^lylndbefaibfadM W iiitodfaiM ibcliw i 34 Any afaplaetornisiI | padclaemould be ceamlflJiad ai ~}000 rem for-3
faina andfaeapwnaiPd and falb eaiunttioB. 34 a mple tudlwdep iw w b iu wM be epfaOad i fa im fahn fa fa ibi
4.0 Sin fa i md a u badi
4.1 W afa-H flC |nde 4.2 yfamui-HPLC fade O Aamnd-- Afltoaw- A.CJ, 1 inputonde 4A P pfaunnifiaii Atod-Olpa-Aldricb
'
ID he-- nuudfaefa--d
11 A bifb a * m m faeW ibmmiaipipli *Pbln of
pud
leiwWI n afa ndfalb efaible v e to t ajfa ar esibii of iajeaiiip 1-200
pLM uifai dtoetmd-- bfa edpwfa iuilettUVbmbO).
1.2 A dertoatoaliatola datafa peakkmpmleuaodqimilltiliOB.
12 Aatoydfabataaae treble efnedtoj to OOOOOI p
S.4 $ 0sidi4M M |if|ot^N |)ylillM iirU h|ittb4L
13 I Tito iUpnafaapiilyjaapylnaa I-- iilHegeHim
Id Wpitabletalmplpm <2IOOaI. IQOMOat).
I I 125-mLU H i H f a h f a
I t 2ad.(b o HOLCvialUL
Dlapoaadlapiparne
1)0 Atoapfa dai(100.108* aitato 10-ltd pLX wllb dfaeeeble Hpa.
I I I WaunIFakVat 6 <l* I t t i SPEnridpa
Ftge 17 o fSS
Exygen Research
Page 80 o f 132
000323
Interim Report #10-Analysis ofF ish and Clam Samples
Exygen Study No.: P0001131
Oxygen Protocol Number: POOO1131
WillIII
tMMNwWVMOini
I
AkALVWAadiWiAfc -----
I
MrOwdofA--lyd rIb rtfcfrrMrTlImtIwiWTMAnnan-- ofc AciJtfrfcOA) W a rty
LGMVMS
3.12 V l m n t t l L 3.13 C m rllllg r ill r f
30m l pofonopylm*w 3000iq .
M CtxMWrmMclymm
t.l Aurtyttal CWiw r;H uteliM tltf(K tyw tciw U fc> i3.i wurSCwm.). (NN:*23CM>32130)
3 t a w r 30"C 1 M eM iPhm tA): a mU Ammmbwn W i n Worn tA M o M tH w O I): M M M 4.3 O nljm tProgram:
Sniiw ii} 00 1.0 .0 20.0
124
65 43 25 2) 45
IK w IU i*
&A Ib L^ed 21 0.3 22 0.3. 72 0J 73 0.J 22 03
M l^eBorVatua: H nH aobtlncn m t>M aiiidm 30
11..71 QKoamiTlUlraiiorn-:]3ParoigwAirMm -rirt-- 1 ^ 0 1 lihrilinn wry
TtoMiwt im^ i l iim fiiinn dd m r<i --I w y berlu ig iil In orderto p la in W HPLCmam.
7.0 M U S y ria
7.1 Mod Bla ro ru n Huwlr t M W ro le , ia lro ritg 413 -> W aii.
Ht rbrvr Him a talmdod p ill m l moy b* ctmgol w o a r to optiOM Ikr MSMSryria.
10 KomkHdiMm
1.1 MoMoltriW
1.1.1 a2nonaMulaturaailal InmlHtIaHInhili oIrTatorr*ionpropa! by aiding 0134 y of
AHmuMvrimwa a y boy n y a l.
Pot)i
Pag?M*fM
Exygen Research
Page 81 of 132
000324
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
ExjffHi Protocol Number POOOJ13S
C 1ASALYTICAi. M flU O P ___________ ttadaadofAadyala A ril PotoaniaaitoafTwflwwwWB Acid (PFOA)ill Wnrby LC/MMS
t . l n d rt taito/Tnalifltiiiiu Bohtocn *.U rnpaa**m *kntoltosar-l< l'> M M .*frroA byw cl()itoi)O iii> of*oal)tl*aI*taadato (oonatoad lor pulifrf m i thlut* to 100nL wilh M ta U M L LOTSbotta. 9.IJ A 1iifW . k a M ittia baton afTfOA Ipaapand bbrlniim m L o rn * lOOfttaLMM lM to > dad * 0)1*111oMOO<ri(knRliaMi taalUnLLO M boM t, 9 U Al.pit.tortb*iiaa*altol*nofrroAtopr*p*dbybitoiii|tn Lofa 10ppiHiI.bidon to Atoot oohomc i LO*triOt oothonol in tn iM L ID M M llA 0.1. AO.Ip|M.toiiUbadaioMaaarPfOAtoptapiidbytrtotin 10 Laftoa LdpatnLMlaHadtotflB atyalnniaf 100waQuiaih il in S a il U nibank. 9.1.1 A 041 MfAaL ftatlflmto aatadaao fPTOA it pnpwadtv bnfljin* 1* lL of OH 0.1 H U baton u t Hail atom of 100 with nknd toa I t t ad.LDM battit. 9.14 a*iana> aadkadllaaltonnhlbniawlabaalaatdtotnlHiaraaotot qppmdBaMy 4^Clid n aabla kr a rauinuBB period ofbmod k a ta ta ia tfn p a a lia .
M ItttondCalibiadaalaMtoaa
12 .1 LO M U S caUbeatiaa akadaada an paapand to HFIC w a r. Tbt
MpdtilMttipiK.aMnatoa akatbad* a n p i n a d dtretn* dw molloo paacadiiic,
f i 2 l b JfcUmria| ii t cypbal Mmpte: M tm \ immo wbiotw my b
------|Q -----------------------
VbNM4f C--cum iw of Chlibntion ID
114 KM9l
XCmbdy^l
14 40
XC-->*fry }
t*0 NO
Hm_P -M*j--t _
_
XXCCmnnaMf yyr^AS
XCmidyy-6
* Tb*maad aoaaantlrtaaafIN tadboalnntaartord il pul 108 tototoal
liaaiatoaBaa,laala kooaaaaahalmioflb* maidniddtato| lha traction (SPEJ
XC-
n*aa or'
P agt 9 o f63
Exygen Research
Page 82 of 132
000325
Interim Report #I0-Analy6is o f Fish and Clam Samples
Exygen Study No.: P0001131
Bxygfln Protocol Number: P000113fc
I .......... AWAi.Yncjw.wnio
' "'
ltllB jriM ^3nC S T C 3 n n ln afNrtkmuuwiiillio A n i (Woa) in W iw by LC7MMS
. aA3 A --fc M O fd a n \i4 a m ftea^aul Maiiltl mim W aapiW wfth --A Mtofm o te * fretted.
92A lamed P i t t u r a ff tk r d i in IfraLpolypwpjiw uibtt , cl Z"Cto 6"C, p to twoweek.
AHeWtoeYttaotomd eoncmtitoliui offtwderi mcybyepcwd Mftiad.
IW B*diSwOr
10.1 Sechttoehofcamp)* meiedtQyfeelly 19 or leu) anal teM e ltc*i M w u l OMMnl (jnfrltoJ IM * w fet HFLC ttM r) id Iwo rayent M tantte* to racm n--r f f f i r i i i (I cemrol piltej to venly plOCOdwrin m o y fbf Onbotch.
MU IKnl ilfiiaMfi--nMljwrnfcf. <--1mjil--lahbraMaitlaJyiniiajwpIliaalaf ani ipttaa will bpacKlaJ
11.- toaptatotmaioa
r u Mnu i 4n,wtampli arparto ofWHpldifrtoi M u l I talar
' .. irhva2ia * 50 hL pslypMpyliM M M rihi* o k (fcrtiy m w M npboa l.d m l
i l l Cw iliao Cb P I oamldpaa (I i I mL) by y i lint 10 n il malm! , roUoaiidhyJiiiI.orKPLCwim (-2*pfri). D v w htwlwummdry
I I I L--d l i na i.onaiaiihoaii CnEPaarpidpaI>iaciialuala IM D illi aria ni a l I* HithOMl C alici 5 h L o f ablate info paduatad
II mLpotjnmffytea rantrilhgl aiiaa(final volumi - Jm l). I l l AnaJyuspiaiiailf<KIrM|X>yLOMS/M3.
IM ClnamoioMiphy
12.1 apaetfcaamt l i & a ttn ia i. am pli md Ratifiai ampia in ite LOMWMS rateai A calibration m ilia ri mute pianai m i Minor all
IM 2teadteiaofpyQAocwaplaiapta allant Uvaarmar c u m u lig li Iavril I N bnlmtii a m -- lyfV il
IU J Uli of n om i ititndoii andante mint W Included ih
hipimmi and al te m i of a templi tei. E m a n i uandardl miai lai ' ' ' aaw y 2.10 manto- A i aa tema!ve, u imita mi oi
` "i mgr bo l l j teiad al Un tafim liip or a aci
(la mcoact far a in to ofaaBaatad n iilirdai- lo a ih ir eia, Iteteli calibratila a u to ri. amaib i A altet ani te i 0jaeto)daaamkte MI IM Uh mar Maaiaid cavai Da miraliMimi U m r Handn i tanna aia lanawlai fctiteimalylabyliiMmiayiailna nainp i/o araipbtlm alpcat rea
Pajtft }0eJ6S
Exygen Research
Page 83 of 132
000326
Interim Report #10-Analysis o f Fish and G am Samples
Exygen Study No.: P0001131
E*y*ea Protocol Number P00011] I
I ....................................................................I
LCAimHiA *!! fcaiiiliniii
ffid u jjiia w m rty '
12J '
--SIKmtfaIhMpmlweiotmrfntlliOhypikaottotfiiMtMiifwmMBiMlMi im(fttoOmOmMmm4milliatmiMMmdtMdfeA*rlMaMpmotcNLwjwcm.
)J (orquivakm)
Artymptoihai
13.0 AoM ptaM Criteria
13.1 C luii--n n w Wte riwinpwfc a ft to tja m km * H> <aw>(tan *pwwi
o f 4)3 m u H a 413 aau panM i;orrw pw 'iii 10 t o PFOA m ior, white ike
d n tfltriw (3i> mm) Mpnatot to Im foaiboatoKiia.
134 lia to d Marita n u t t o M M h PPOA M kvok m m to n A * LOQ, If
fckpk o to to a PPOA 1ta to fM to to n 30 ^ 1 to n nw Wank m^W
M U N flto iM lte ld to te N to M lflN M b O fM M M IlS r
13.3 fo -T w la Df wan! jito a 4 m to o to tw n w In hitm an Tit n r f nf
tobtoxm vakw . ITa comtMmike f i l l m o i to ocnyooir lirati. to
M M
IMK
M
M
of M n l be
pta toM i ta nvatoial by
n to
wroiMnnjad.10AtonymMaatnoia
ipfk* twiMt 70Vra-unction ii
114 M y ta llb iM i M M b I k w l to M iM M u l oM iM by M M Hu m Boot TM, a ty b tortal tool 0m rilruM iiin of to ctlibnlM cwvi.
i b W MMt oat n w a l MH o f to total mmbm of mrooud runto'da
lii)HIM
tu A toraaMn u MBMim M to oaMoato can l anaiatal Mt e* M M (Jt* M M S ). V e M to M ta iw to M M M * to n to M i. to n
M ro to ife irt o n M w M ( HM pM to M M M M ly M l. IM ta to lto to m Mwaan iM k O rod m w iiIm m a t not d rift n n to n
I 11 n tto -- w ljU iia l on I f iMonrton lima to ft r nonldr din lim it within a analytical m to n ib aaaiaam teN aaatnal.
Ml] U w to to to to ito to iM iM m k tilto to e e e w e fP F O A to n llie n i'L , to a d an yank a n t) naia| to a ta ta i w m near p o ta to yanm atm )
f i raniIVytoManaLuMnotorw y n y :
P K b tfn o d tV U
D F -to w b y *b M i to to a l n ta M w u d iM a l. I f Mtaaaaqt.
tort;
P age 21 v fii
Exygen Research
Page 84 of 132
00032
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
E*y*eaProtocolNumber P0001131
I )Rc7?CTy3nScSp<tCThiAHNqAil^LyYwT<ICUAwLiMDqigllt<f^OitAtc..M....C...P..F...P..A...)...B..WiMtrhy1 LQW8/US For MMpl lortiM vlA toewa mount* of FTOA gaior I v Naciion, um 4m ibipwiag aqudiaii io wlHtlM* da p ua w wn a ity . RnvnyfH)aatbtddBdQiiill|alwriyio*wiid<M g>> oantyt*fcw rfin ooattjifo rt.)! M
Exygen Research
Plff**'
Page 22 o fJ
Page 85 of 132
000328
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: POOOl131
Exygeii Protocol Number: POOOl 1J |
ANALYTICAL METHOD V00017|t
Mebad c fA aatphhr Ile lM m RuNlN mrOMeeettoMto Arft<PTOA) le le ft by
AmlytioJ TtolfefFesiHty:
fijfltwifll
JO* JLm mkHDrive fUfeCriM f* PA 14IQJ
AfprovtoBy:
IS
TvkQ m m A/ T*aM Lw4v, LC-MS,R q a iM an k
k><
DM#
/VtormMm.Qvmta.bom(UmrA
A4 fr
Exygen Research
ToM Fiaw 1 P a ff 21 of6S
Page 86 of 132
0003e9
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
ExygeaProtoco] Number POOOI !31
Nv^wYMOPlI
aHa l v t ic a l m e th o d
Mutu i ofAttojuti h r * nmrai torta fTalwwwtBMte Atid (fPOA) ioSci)by ICMSMS
Ib ifM lto d a Btotoftoiod farIte adatta udqM alitoiM orptotonKUM i mi b)r Hifb M a m m a U411U O mmliy n iliy ooupM N to ta li M iu dMa iw iata Dam ar BCfldMigJ Oliali.
2.0 Sttojr
21 AhngiotoHivvntolitonMyfnBlaa.
2.2 C m ik ta B te to ta la h tS D t t o l to bandllti4 at>ydtoiiictl far propcrufely
paasantaa.
.
3.0 Miopie Raqutnnonl
3.1 Al W 151fHattoajiLi i r aatraclta.
3.2 No m p l* jiiiii--aln| li w e d Jbr *oal tota. 3.3 tH |M maad n tlM M i ibCUM to aUnto w aquilibmie lo roani
3.4 All in f i l i ramito (hamphlyiai*l totootortiqaatolad (or cacarti!. 3.9 liiapla aollaatinn paaoadono wll to apmiflad tu Ito aampbnj fta fin Ih
wto
42 t o iB lM t o M i
4.1 W hto-NnCpada 42 IM nt-H rL C B id 4J 11iitoim fio to l fi n n i|iit T u li 44 ytowwnnli Aci4-Sl#na-Aitaci
$.0 IIImau r if aa4file tta to
5.1 A MJb partbnnanao Dqidd etoMUMpifh c^4bl of pm piaf ) u 1 ia lin a oquiapto hfc i variata ta l Iqjacaat c^aU of Liiloctimt S-2W lil. am iaad M t --dito Mi Opii ncanto (LOMQ43).
92 A dm to*oltoln pr d> bram ii hoymlmitod qnmmocii 52 Am bita! total rItohII o fnata le 00001 5.4 a l d q to h y hto Plt o i w lh li U h 52 15ad.dimombbfolyfacpfkn caanlaji lutea. 52 I>tom *l aaiwilw (50-IWM. 100-2IXW.). 5.3 U^aLLDKMnmMaMditoMM. 5.1 2aO.<toillPLCvtoUi 52 M ijii l l i | l | n i 92 Aitopliu to (104-1000yL a d HM00 n U itti 4iaoaoMolip. 5.11 W a O fa lV a e l (l|)lC l W B e a r a * a i JJ1 3n4HH9IWBl*M. 5st3 Unaaafebalh.
fiat*1*ofdi
Exygen Research
Page 87 of 132
000330
Interim Repart #10-Analysis o f Pish and Clam Samples
Exygen Study No.: P0001131
Exypro Protoc! Number: P000] 131
up*--*
iftitWiMiiirViwnn
^ M^!iii<ofAl)lllte^rn^2a^rpSerartui>cAgjatWAlin^lt' LCMMB
J.14 W ibugtaM w . 9 .0 CimHInCQPMofM m 9*Lpolffnipymii mb u 3000 ipm.
M CaMMmpfellSyrian
5. A m fcPCllCotlu FlucyUa (Eryrida tarm ac). 71 mm 90ran, 5| <WN:(250*4121)0)
42 K i p m i : (P C 4J M M * Plum(A ): 2 mMAmmaliai AcaantnW iur 0.4 MWH-- (B) I M ataa) 4* Ondi--l Pro*TM:
FlowA ttt H A %A 0l0 ts y$ 4M LO 45 35 0.3 t.0 25 15 0,3 MX) 25 IS 0.3 22J 45 25 0.3
4.4 tra tta Vaiami > t (ex blwTM4 * a 90id.). 47 Q m iO a iliK P u t t a i- M n il -- lu * m ftraian anna. 04 (m lta e i -2 ) almaa.
The4bm aoaMam a bandaia rt (rida andaaybadiai|ad in ant*ta aOntatOnKPIC jaau.
7jQ iW ttl; m
7.1 Mod: EiacocaprnyNairiivrMdM modananilqrim 413 - 309m/t for PPOA.
Ik s m am andltlaaaaaia4adadaafaid a id may ba changed in tM v n a r ttO i M IM I a w .
OjO F n rn O M iT M ilH ( I t4c**3ePkaM
( L I 2 MM maiealan aratala la w ri I prepared hy datai 0154 | el mmCMumv*** IO0OmLram.
AAaaaamtameaiybe papered
hnT
Page i f lifts
Exygen Research
Page 88 of 132
000331
Interim Report #!Q*Analysis of Fish and Clam Samples
p. 89
Exygen Study No.: P0001131
ExygeoProtocolNumber: PQ00111)
a m a l v t ic a l r a w
U a tto o ^ a lllia te te a n tewrinatlii offaillaiiiPWlaM g Ani (fFQ>) it to il by LOUIAIS
, O.U
aaaact u lln o f-L O O ^m L o trV O A kr wwjhm* IOn
' ' ' ' ' afaaalylfcal a to to (tw m ri (U unity) m i dilate IOCiL vriQi
m iH iil tea U to U D W to te .
,14 A lQ p ^a t finOflatfiag ioliflioiiorPFOA la pttparad b>biiwymi in
mLafte 100ttaL a o hto tea lina] r e ta i of 100v i* ncM ^i
la*l23d.LD Btala.
9.1.1 A U jiteL faitillatltoatlati tfrTO A 1pupaardky ta li 10
, isL oTIm IDpetal-notato*Ilia final yakmvof 100ulti natante 11
al2JnJ.LD fS tata.
O.W A HI MteLtentehotoMtetioa ofFPOAtepnoniOy M nglnilV
. .often 1.0u ta l taltela i Wt o t wIuhmo f 100ita -->1
a 123m lU n to la .
- 1.3 A M l notati tenltm t o lattano o fffO A te pnopaitel Oytempio
- 10 mL or teo 0.1 pfw, natation to 0 Oliai rotami of 100 with
m4nboI tea 123eoLLCTOto te .
M TkamaktatafetaiteatooaMaoaaraioOaaiondliiiratloinwai
OPIimirliinrl]- OX andan atekte ter a rn ttimm pmiat a r t matt
M MandataCOlltatateotoltaioan
0J .1 U TlW m t Minima Owlante an pan 1 H flC wattr Tut ' ***--< mtaoda an yaoeaaad tem oli teo atollo piatovi.
y M)|sl| jp
9JM TW M anta te QTiteal a l i teUteinool onBioinVciMmaybe pnpandat aaadad.
final
Ctlibmwn
MMmHot
Stinted ID
* * * fin * > ___ (|jJL
10
mi
utn i n i0j r m r
tSSS&t
XCwmwyy-J
so XCmn*Myy2
10 HO
100
J1&00 .
300
JttL
0100 XCMfeyol XCmmyy* 300 XCwm i i ) 1000 XCm ndirr*
JAcCiMCm- igliost)*HmntrtAnt9m*iismmm/Hglik1iIt*nirntoMatfs(&l K).
P v4rt
Pag* 26 o f 65
Exygcn Research f 1
Page 89 of 132
000332
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Eayfen Protocol Number POOOI13I
M M iU M v in n ii
I .........
AW AtnrCALMBIHOP ~
I
Mahodo/Anhalt Jbtia D a aiitaa ta o fPaOaMtiaoUiioicAcid p ro A ] inSoil by
AU AMMMadmlMlubaftfmtmtNlak)MMh. Willinth
tdfhw M iw aaM i
AM I w tt apqw d Mhntlm dtndadt i IL-aL pdflirepylini u b a
AU AB2a*tCaaBtyfofCtu.iAtipa--NIctrrfinndirnoftltodadtnuyhcprepiitda
JA MMt
AI Ia h hoch T a ^ la am cttd (ijpfciKy 20 a Iw ) amt indudia k u i oat mBad aiaaal(nahad bhrii adaf SnL af hmm I) and twt m ftM oaakall M IM m lamm wm alnal-- <Uk antirot Ute) to wWy
M, s b m *,, * ,,tM
im* qulfcy m m n i plat fcrtti p n jK t
11.1 Wfh 5 1 ifiaafta fcfe JOaL palypnpytat oearfftip Mwi (ibrtiy m
m m w ih m M m m ti w lQ .
i n m S w L * w * * m k Md * 4 m i w d * wsAm * a k tr * f -IJ n tiiiM i. in l w * r * lebeiie e u *n m b befliiD* MfoM 6-1) miwiw,
IM BriM titf vbIm m iy t 40 mL ftfc wM r io th* $0 mL poljprapylfttt
ui O lN M ||fei*IO vj|M llA ~ )IW ipiB .
iijs C M M te Cu WB MCttdJN ( l ( ( OIL) by m alm 10 L mtthinol M>mlbr la t fH nC w tr(-2 0 w M i). Donot I oohianrandty
U S Laid it mm) B l laapla amdu M w a a d Cu 8PE ciftridft. Dncinl
t' l l IHSaabLpMajBi ^a5naMLanIWaiKMaiftidiaaioMoliflSCMotafeut 5tatnaLiosfai lIu].k ima gnduMtd
IIJb lU aynaa pla odolanaiiu yLPMMntS.
12.1 Wal thaa u m u a a f ab dadad. aanpii ad M jifd nnpt iao iht [ " * * " ijaaoL A cnMadai adad ao a pneodt nd bnaw ill
1U 3aaiadislaBtddaioarMwaO. AaMaadla(aalaal*iaaaMeaDMmdaal*>li W baM odM b aM ydid a t I U A aia a t t m aead aUkndm Honda* owm W ktelodtd the
a^ooioi a d a Bl a d af 4 tnaptt a t Banead aaaadi a a l a HaSBiindbama tB y d - H H ld a Ajol*aH*a.a>aunalof
ha>ai
PagelTqf6S
Exygen Research
Page 90 of 132
000333
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Exygen P iatom i Number POOOU31
MuM Mutov a n n i I ANALYTICA3.MITHOO
HMMofAjMitoifc^rmtomlMtonofreirtmbociettaeAodffFOAlinSoilby LCM3MS
M u li b f M illi p ito n i lim i l i i l l i m ili i m i eveqr 5-10 im p la (a im m fc r w i m t t m m t u i lim imi ), to ifc a m eeHsnd d to n im M U H I to Ito J M m a to t b jw tta a in > im p h u t. 114 Uto lim a m M mnm fcr tonint>eu U nni m utoHi curva m u m a n i fcrttu todylubgr to a r iu|na iM Mas ita woiMj ii ufpoto r a iu u u eelibaUeu miduvd igni--ia lina u m f M cuLjhm 1 3 (Or aquatair
mtontoqmMk
IU Im ple n a to li ito u ll UMa m i to rn iti* a m u . Anjr ampia Dm mlliiul lim ig li wpm m **1 4 to lto to r lih in l m i numlyiW
134 c im ilin p in -- I tojw p ali t l fluito la ton ir 340mu from l renili M il eau. Tue !3 m u p m muratorti ut m VOA lim a vrlK th te d w liiQ tfiiitn M M tfc ilN iffM b a i a tk lii
134 M oto! Muto*UHMeul ceauiuWOA tool m er toca to LOQ. l i Unfc cernito 3P0A et lunlc MMMrbea90m lL, torn i o r Umk umplc am toitoatoalm i (kceutocicim i bcrc^cnotol.
19J teeueudecefceuMcplitomd ato ril ita i io t be tom en 7IM30lt of tblr kwwu vebeee. Ile eccirnl m ito fcUento lle Ito eoeeptebllila, ihe mtoe m i c f toHie to rn ii be M c4. Auj uuMu epike emide 4). IJOH to rn ii bu eluelel Ij Ike me!?* letamine it oeeueciion li
134 Auy oMeudeu im iim i fcuud to to I etoU leel m irte i t? H ih . Huye fea r Ten, aup to eueliuM (mu ito eeleulea o f tou lUnton mm .
einlileil unto m meed 30M o f toe lutei number d emncied lundeidl
134 li main ile eetoBcieal <R) fcr mrtbntien curva jennim l aw l be M.M1 Ot1 OeUJl ir enfanti recula fall uuUrri* n m U nii, mai
eurnUulBertoenluvm eeleeuiuie touull to nenelyeel. 13.6 toa ertili to a benweu to ltol i m i lim ila aw nel toi* mm finn
i4 K w lfc ie m a l) e m If murtn tonKl eueedith ii Unit witton m milprtc a torn tocaumto membml
aaeef'
P agtlSqfiS
Exygen Research
Page 91 of 132
000334
Interim Report #10-Analysis o f Fish and Ciani Samples
Exygen Study No.: P0001131
Bxy|a Protocol Number POOOt 131
Hqfiifcewdh
MfMIMwVQdaiYIl
' WirhoaMiftog '
MK)dofAad3iifcettoi>tlwM>iitoaof^Kimroocttittic Acld(ffOA)a>Soilby LCMM4S
14j0 CilciitatoM 141 lie* 4a bmmQamustialo cikalAi the mountoTPPOAfim i (mo^L, taaad M pk aa) M ill t e ihiidnd cm * (liana rapante paaamatan] Cananea!kjrPa Man L pn aoUararapragma:
------- " - . f , - ; f f lM M i-- ni ~~ atoft
D F -M o c a y e M d < P a M I c h n wadUaiel. ifintanai)
143 Par n n p ln M M db Inana aoaamaafPFQA piar lo annaffio, uaa taaMkwbif a p a t a la aataMataa panata raaavary.
UaawiyffO
IntalinahtataaK m il) - -- l?nialicaMral(aljj antapuaddadWt)
143 Un na aiawiaaaaaadqto iw m t IfaamOLmt of PPOA found in n^T. IQ
rtCn*).
PPOA lb n a < ^ *)-fm iM |i< fufflTTnlimintwrt(fimii)l
an apk aip n (dp)
4A Uta t > iaOowinj aquatica ta catalina a n canata or PPOA bund ia ppta Cacadm drywalgCI,
PPOAtaad <ppb)dty dpi! PPOA In n i (ppt) (10OH/total aallMW)
an*7'7
Page n o /i l
Exygen Research
Page 92 of 132
000335
Interini Report #10-Analysis of Fish and Clam Samples
Exygen Study No,: P0001131
E xyfcq Protocol N oub tr: POOOl 131
ANALYTICAL METHOD U M W a ta ; VOMITO
A iuJytfestf Tacting F a cility:
tk rL C /W M I
t Add C TPO U I'
BxmmRnwdi '
M S I IU m b b Ii D rive
S tri 0 * 4 , P A 16101
App w w I B y;
C -lL
P w lC w lly
l
Tactefed tm im , LC4, BxnmUmmK
rtkhfol & k
Du
Exygen Research
}< t; i'
T M ilF a p t: 7
Pag* 30af6S
Page 93 of 132
000336
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Exygn Protocol Number: POOO1131
I .... AiUrilCAi.tritt
MUMNwMberV0OOI7U
|
MWdofAndyh tufco Ttrtiml i nlli at Nrtiw eocw wlt Aal(WOA) in Scdinwn by LDMS/MS
1.0 >cpa
TW m M 1WO*w ftq e d fc rta ImM m tmi
fparincgtHtnsfc
aM hy M f t r ih w i UfoM Chwnla|rn>y w fM l* > aWan M i
OpaWawhnaDwataf(U 3M M fi)taidial.
2.0 tav 23..1) MOiwmIluimhmlwiwMurlilWMwlPylMiBfclodl--M.iillhitMtydaoiiMlftrMefiifmy
1.0 SwpielUoibeMMI
33..1t ALt-llH--r)*O~ rf--irM iM nyl.i*.M....t&--M kMn--. *. j.,~
3.1 * --r'~~ M H ifn M abouti he flewe* Io quiUbriu to Mom
3,4 ANewytaMMOthelbeniijy a/a*ibalm M | aamftad fccunion.
4.0 K aatnaw lJtaiM i 4.1 W ar-)*LC f*4 44 ifiOnH-ancp
/ -- J A w U cyd-Ii^W flll
4.4 AmmmOi * r > - .C.I. I f W On4 4J
3j0 haoonal aal Stim m t 3.1 A oiffc f u f l f n i Mould ilw ilip a * f4bh ot f mafin of 2 0lw B lm iw 4l*w fhW i w lw m iM nreyhl of flaco n 1-100 jil. n w n lal l 0W3w Mw |i ib M i Hr(LO M M a).
1.13.2 A 4oW--I ihiil me 4W Ibaf ll lrebwi4 qwiKiwiw. fo^uMlhaW ae pahlaofnadiocM 040001 f.
M14 30L ia fwattayotjQaaf>) aaw H if ai> S3aL llo a M h yelypaanilawewbMiMb,
3.73.4 DlWWbWmknfWw (3O-10M. WMOOuU IM w L LOfS iw w w i* heul. 34 ljaLdaaam C lia i hit 3. 3.10 A llf lf i n (100-1000fL w l MMOOU 40i flafaobblj 3.1) W wn SayfitV ie Soa( l|) C il S l* aaifcif|aa. 3.12 m o m u n waMMl
P14<
Pttft )l e fs i
Exygen Research *?
Page 94 of 132
000337
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Exygen Proloco) Number: POCO) 131
IW lM M
\1
H K lO HlH ! VW1TW
............1
LOMMdS
5.U Veneur.'
5.14 Wileel ea te ter.
' 5.15 C u r t i n
a in l a ia j 50 m l yolypropyknc tab-- WA3300 qim
0 CWtetelpa|dde Syatea
f>I AMlydaalCeliMii: Wnd |ltei Kl*[KayateM tem ane).3.1row 51)mm.5a (TO., 0505452130)
^ ' Tm m o m M*C 4-3 M b l i l M : 2 aM Aammm /uatan Is wmr 4 MrtiUfWw(B); Mutanet
G fiftptPtop m t
Flow Rale %A 9L& bbU b&i 65 39 0.3 1.0 65 39 OJ I. 29 75 0.3 200 25 73 0.3 n s 65 35 03
M i*td e e Votate M |d,(em bebuaaaad Mmicfeae 90aU .7 Q in illtlli: teak Aim - wMiM l adani oaBbniion ewva. J lim ita i: -2 1 U te
Tbeaboa te lim i aia talmdoJai a*ulde andmayla dimmedio ewtaw aatWaaAa WRC ayteo.
70 M&VSIyatam 7.1 Mate WaMaiQiay Wa p iliti MUMmoda.amuloril*>3 - l i| te rro r
7W *e w aateMw w teaedM I |Me wd M arla eteoied h enlarb M u te ta M IM I m m o .
(.1 MebiUrk II.I 2idMI
I icaMa lo Ite I) paepand lx addin 0.154 of etolO tO B L efanU r.
Exygen Research
P at* M Of65
Page 95 of 132
000338
Interim Report # 10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Exyiea Protocol Number; POOOl 13!
VYM0I7K2
1 . .. . . 1 iw*iYncaCTH<)* "
I
M iM afAmtyih fa rt r w tor iaa a f k rflagiaailutai Add (ffOAJ to dima b> LOMJ/M3
U BtrOMfoaSelaliai
1.11 l%TMdei4iniewlipH<MibyddieiemLfwli<to 1000m i afafa.
A>-- ll > wmiiil.
M
9.I l Papa aMali M a il f-100 M in i fpKM ly*ar*luB Wm* fal l ititital um ilili |m i w l Obcpurlty) araida 1 IW nLM ih naOMdtV 1111nl IPTB Mola.
M I A iO M fa L ftn lfcn lia M ia ffTOA la pnpaiaday Intaglila 10 m i a ffa 100iifa l, M a i la aHall Tatuata of 100wilh na tlw l hrU laL U O T M a
9.1.3 A 1.0agitai fa M aaaaaM 'dm iafPPOA il prigatadbrMagra 1 n L a ffa M MtaLaaMaa la Baalavito f NOMiaiMfa< ia iia iL U H M Ia
9.1. A 01 M ta l IMUtoOM annata afM IA I pftpaodl>yrrtigitt| la
L o fi I.O M talaU lgo a Sul tofana af lOOaMtMoiai in 123a L L C n tata. 1.1.3 A M lM taLfalU kntaaM fataafFK M iagngandltrbriagitig 10 aiL af (ha 0.1 m M . M m m * inai volanti af 100 wfa a la ta li la il n tl.L D ri tatti
M A T ka M kaM M M w inn M O am ia baM nO iitinM ia niara t 4 P > *lfa M r*c<af ira moia fa untatimi padod aro manna fa n fa fa a a fp n m fa ii.
1 lio f ili CiBliraina liliiim i
M .1 IaCffaMOM.1jSttmilfLafaatWta iIaWatdaaBdMl anobf.npared ianaO iaw l aia diluita
9 1 2 U n m a n iai il a typical sancir: additi] ciaicanm ian* may ba
CtoMlIfHtol TFadMatoM M utaiftnML)
IH IN IN tO 5
Velane MI 10
t 2 10 IO
ntataiM iL>
-- W ----100 100 100 1
ftta i CaiaMnOae
io!? so 20 10 Q.J
3 __ I l___ 109___ _____ . .
falaft"
Page i i o f 6S
Exygen Research
Page 96 of 132
000339
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygaa Protocol Number: POCO! 131
liip itw it
MtaadNaataavataUR
M J In w a lla illkta isiin add id ilo Illa a L LO ranim w ^nnkM U n
M ri U nn i tatuata m i u atariUM a fataadtari any b f rnjm i n aaadari
l4 Bank M U 10.1 Baafctank * r nafta a m ata (ta ta lly ar Iw ) a * iacMc I tan urn aakaand tanni lari ta * ta aM aotaol* ta llii ) k*on aanaaaliwta<llatanul n ta > n m WMdiiim tny natal. HU ItataaaaaaantaMdta U m aw ytatlkaM n ri ta* *U ta aacUlaO in Ita faaHlyaaaanaa*ylta ta U ftaaet.
I l l 1M(b SI afanatiata SOari. el)faytaa aonilba* aita (fernIV n
ata,laptaa ttd aatfata talBi H.J Md 33a L a fin acati ata, a, vtatax and rinka A a a rili ictioa ritatcr
ta-M tanaan. 11.1 C w e i* e in e * ta e i -ie < l ta t a - M in a ta . IM OtadNae ta Cu I anarid (I n ta l) ky tain* 1 b L atkanel
nitaaadkyW ail. fMTLC ta ta (-Idw ptae). D oaolltioataiaiH idiy 11.1 Load IdaaaaO ta u n ti a ta oondHIiiaad C SPB caatMia. Dlacta
IM Add * ) nL f anrianal ta edtan lall la ta koooai ef ta aL
Itakifcia k ta C f oata tad A lta on a miai aataa atta ta -30
uim m
11.7 CtatiritataW been-riM O ipeta-W ntanaa. IM P iata ta mataaal natata aaaaOToanridta. O diai ta ta.
II. Waatta w lita Mi * nL t f nataaal. CaBaal ta ta n t andaddkta ta
alta*aMaataa a 1M-
11.10 " mW aa 1------**11***
f* i *-TM *T I-- `-g
-- ----- -
M ta ta k y M ari.afUPlCa tari-2taatacL DonotlataolumimiBdry
INwlHpk11.11 M d ta natam i la -300 mlf m n t ad tad a tha aaccndMdtiwmd
11.12 Stan M - I ad. 100N m k a a l CaOaci S nL orataw Imo nduated
|}J.aiilnta>laaarH la nrtta (Bail gUma - 1m l)
11.11 Atalyaataa alta r iiaaaairairLCIMt n W.
Exygen Research
P o g tH c f i
Page 97 o f 132
000340
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exjscn Protocol Number: FOOD1131
MlMMNMrVDNITn
G _ AHu-VnoiLwriBog
,
umanalatadefA ta riib fb e l) a abial iie f Frttaiam ta ia ii AddffTO A) I Sediment by
13-1 A e rila BOB m arni a f ier*t ilmi ne. uro* radftnlflrd IW>|li imo ita v a m i m lyetaa. a Utaniii aderti ama em idi u t Mimi ili
113 l ati tarti ifH O A rnmip ladini a I n I n m XKmCTtion lerelt
IRHVlW feNMWlII M
flit
UIJ Aa arile M ef aam ad irib a d a m eliriti mai ta iaokried a da
taSadaf ari a b l ed ef e w*l> rii b a d a ta m a bc iraT|nell
tamari eaay J-10 empiee. Al m ritamihe. ai mike HI of crataetron
Ba data May la taeeled ri a tayiataf af u t Ibernai by aUmien
amdMdi Bannened eeay 3-1 ama) ( m a Ibr Hceiri tei 1
aailadil le r i t e m a, rii11naie Badata mai be ita Ctit ari lui
lajeeltaaia mnaieeri.
HA UN Mar Barimi cava Ita arikaloB, Linear aariad cime ire
pa ri f itta raefyt r bylimar ruperarararap Wa annuirn ef a ta ine
rana Irilbialni Bariad a m a a lm eilat MiaLym 3 3(or equivitm)
u bami yaBai.
11J ampie leaeMi dedd ari eaeeed Bariad wepeneee Aay aunplei diei
ea rid a ariad inpoaa driiildta Itadar dHaail a d nenelyMd.
13.1 CtaeaaBbm ami ta a a l perii fndaaitaB inaa 3d* M im e penai f*!3 am. Ita *13 aw penal m rapaidi a Ita PFOAad, abile ita dambarlm (3d*ama)lepaeata be lea efeaitaadlMride.
13.1 Madrid Mnla m a ari eaad am M a tarale pem r dm be LOQ. ira btaefe eeaatae (TOA tamii f a n a Bue 0.2 eftaL, dm a n e blink aaptaaaataebwliidinilberidlaiBieaataie iiaaml.
13.3 Kaprala ta n atal i r i ^ a d aribiiia tai a ia letam e 70-1KIHef Itab leu III elm. If e lu tai iflta bill ibride da eooubk limili, Ita a b e ea et a mpia tamii ta a iwiem d. Any etani rie oetirie 70. I30H duna be m ieBid by b* IMlya le demain* if nralractton il
ISA Any eilltaa la i B adai bead ta e atadcri eadtar by mint da Hut laer 7M, m y be aitadid le a be aleatad ef be erilbmlai rarer Hoeemr. Be e r i M iiatar of Traete* oellbretloe aadeeb d a M u ri ta rerbriri m a ari atrial WM el ba atal mutai of directed Bendata
111 2 * * - m m 00 ftv o U b n tim ow* *n*tuo u t be Ml99) 01* M.MJ) V e!UbrU>a teuhe bll ouoJda (hut limile, then itfiepriiw ip* M be t m * >4wt bwmime t epemien. m i ihe neniirte er*e meiieiml i f Mbleeiheuld beieeeelywd.
Page 3S o/tS
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Page 98 o f 132
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No. : P0001131
E x y jtt Protocol Number P0001131
MMMiiNiveono
I
AW ALYTICAI.aTte _____
1
UM4MMM o fto jo fA M frib fe rtl b m m liM lw afTw ftw wowwoic Atu) (FPOA) SodmwiHby
x 4 S U4aa --Ijlifliu
na. g iilH i limArt w e n * Uli limwitliin m itnnliw d.
im 14.1 ' -Uwtt h u rt } 14l n K-)ixJo-l-M-C--*--io u(ufao-fP-F-O-A--fc-im--d-|i--tf-l-m-L
geened fcy* I^iie eftwe
DF- fcalorlBnHJcfcfctlwl whp--'--iAOiaad, if noow ry.
14.2 For iv v iM fcrtUW 4 laow Mtxwat o l FTOA prior U Uraclioe, fl Miming oflMflaal* cdaAM flagon* n m y .
lUcovoryt) -
lW fa fc*< nM J imWM4iiiomKafcL)I
- nl)<ooJiW(n^il)
14.} Uoth llovlm quodonw crnnwi* nnw l o lFFOA femd i nyL IO
oFl(
FTOAfcoo4(|ip) ( S l A j M t a a W U ^ ^ a l n t i l J l L l l
144 Uo *o fcflowi oflooflo (ir MWH}) colonlo lli nom t of PFOA fand ppkbooodoodry rrilU
FfOA feond<p0* y w ol** FFOA toiKffc) ( lim / Mol oolidoWl
M i' 41
P a g t3 6 a f6 S
Exygen Research
Page 99 of 132
000342
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
B in ProkKol Number: P0001 111
ANALYTICAL MBTHOD Mated M obar. V00917
ndCImkjrtOMUM M M a fA te b d ite akaPMim ln W ii dltotearaattaaafe Add (rn M ) la Flak .
AaabdolTaMfaiFanHbr
l^ p lm w l lOMkaaaaaehOrlva
SUM C olliFt, FA I MOI
AP>ad*jP
f --lL
id OmcaMv
I
T<tieieil Leid.LC-kBkB*)pe lU ew
a / v / S ' ' AVViiiMPMaMPfktMaiMaaMtUdbbdra,LOOpaaMndbkaMt.,1fik jtm <uw *
iituM.
Exygen Research
TOp^TT
Page 37 o f tS
Page 100 of 132
000343
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxyjeo Protocol Number: POOOID)
'"""rimni" .....AlWrYflCALMITHM
.M fihrfof Aaatjwlafcrftg Pilwiil--H w rfftrtB ioocunalB A dd [PFQA) in FWiud ClMMhy LC/MB/M9
1.0 Snpc
'
Thww lfcri b w h WiplB) ! far ifai iacbtioB m i y r i lt i n M partucrwcuwic mM ty Hi|b N tn a a i Liquid CWotnioyyfcy coupted t* a tMtdtm Mass fijiw fn a trlr r m n n r im n ^ tr iin m m iik m i
W W*y
1
AlWQIlllllVflllkMMlNypilMiQlfi
Z.Z C M K lltttw m p riaw M 3 D 3 M b n k aaM ifaiirclN n k ilh rp rap iin r !i
9.1 AtiMitZC | /IM
SotC oe.
4M I w ylll * l MbtfW MWr t > 4 W M I t P lw l x Ite m mnplt In
paB oaw of h Hm m ih iIi i vM k A y i t s . M aw
im p lo in
j j (oI M m m n n h w wU ki irHffftf is Ota * irrif"f p in fer this
4.0 fc u |w > iM M ir t 4.1 W ihr-H P lC ffttla 42 AwtodtriW-mCpti
42 C ato* (12*400a u k ) - X a* ptd*
li44 M t0w al'injC ^4i flttca p i 0*300 *)-R n p tf |n d i 44 rU 0 < M M m il) - Rattt*ad
i4.l7 SI-Owmd wI-HLFCL-NCHi-*H*w*l p ^a U043 l ils n irtir riil rM jrU f-M i
DbBMhytfchlamiliH-XMprt F*^4 4.11 Tallin - H u f* y 4 4. AmwiMAwnw-ACJ.lf|iOt*4 4.1 AoM-KyAttrieh
3.0 hemewswdBqwpmim ,1 A M|h pnibrn-- Q fiqrid c^onumrip+i capaMt f pumping up in 3 alvaliafH pp ^M ) a rar iiMa vofcmm d j n w wpabWo f irywong 3-200 jiL MawMdMa ta a ta MM lp94bBw(LCMSM). S2 A M m 44M S nliivr OKIftrp a ttiM p n ttin adOiMiMifliL J A fl4t}ffri1hrtfm rap** ofr--fcjip *00001 j
h|iirt
Png?J4o/6S
Exygen Research
Page 101 of 132
000344
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: F0001131
ExygcuProtocolNiurijer: P0001Ul
S Janalytical MTmOO
mw f A ilj^ f c t iflm niilMrtMoWwfligtow ttndcA cM ffroA ) In Will >< CtawtybCMSMl
JMJ TKittMHjmtHip M l
$ 125 l f m
flwta.
J.7 S0L5b^wfch>poljp<iyj>fc>i--
5J 15L
osN nft|i(Miw.
19 MqmaM.mtaMlpi (KMOM. IW-MOtL).
910 I l M U M m w i M i i .
S.11 IM L d M rim C v M U l.
117 IMpMiMtptptfM.
113 Aplp1 11(100-1000 JL-W lO-WO( ilj, wHIldUpOobU Ht
3,13 M MM.1.14 O l nbw UOmlj(l lw to t . (M17I7T).
m mm
3.1 C nxifcp Jpt*lfl|iimi3 SOmLp*lMNcp)4n.tu3o M2000rm
6.0 ChMMOTfateSymm
6.1 Ajulytlcil ColuMcFl.cphM.ll1< IcknilBc). M nw Onun. in <PM:MS0MMlM)
M T M M J0*C J 3M w H w *(A )! la M M - A W liilW 4.4 IM M PtaM (B): MMtaml 3 O nliM fnvW K
to w fta
*A K l OO ts 55 0.1 m <s 55 0.1 5.0 25 75 0.5 20.0 25 71 OJ J <5 55 0.5
64 l^caonVol-- r H L l f 6 tanin 4 to m uh m 0 u l).
6U.7
ln T -U .Q irili r rM kA m -stln a ria u M a liK M iM m v .
im im
TWl4ovt nwditloM n . In rn li fl Mi fuid nid m y b. ctonpW mHier w wW tC 1>m.
h i> j.r*
Pa%t 9 o f 65
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Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
ExjrgenProtocol Number P000113I
Impalmi ,
AKAlYTICAUfaCIBOP
ClwabylC/MMMMafaodofAofayaia fcnbflwiiiym wiofhrihroatwni< Acid(PPOA) in Filli Kid
TO M S M S lM n T.l Moda: Elatoofaiay NafadvaM IX nodo,nw tvw iuiatlj -v 399 nrt Ibr PTOA.-
I t* aboaoooadMoNm fattadod aat guidaandmaybockanyed in a d ir a> optiodaafaaMSMS JMan.
i.i iiMnw
I.U 2 aiM I
u SoMm i
|Of>fa m a r it papai* by addin 0.194
fa IMP mLofwat*.
111 2%aaoafaaabdia alcalini iapalpatatibydiaaolviag3 |fnacocbtc
112 10H Pi n faiOdhMaioaihnain faaaa ia pnpand by briniini 3 n i ofdbaafagidkUaMallaocfa a ttaaln l n n o mL witd Macna.
Marnavatora nay baytqwad.
.I KandaidHapaMh 9.1 taodard IfaeMMCaalloa Idlatia
9.1.1 Pia l l i i N a t aafalfa (-MIO in f ili o f PTOAby watgdni 10H o ffatlyUcai dmdaadf ianaafaOfcaparityt anddiiota fa lOOmLwKb aaatinaotna lUnaLLOPt botti.
9.I l A I.O lfaM . Italifitatkai aofaMooe t PKM fainfamia >y ariifaiai ; uta ffa i IN M fm l aobaiao fa a flaai ratoiaa of 100widi nanaool fa a 123aU,U3PBbottla.
8.1.3 A fai pffaaL faniUtaPaoaohdfaoafPPOAio pnpand by M ulini lo l i f dia 11 piM laaM od fa a Inai aolumaor 100rifa o*ikanol
attlnLU PBboM a, 9.1 A A 0.91 p fla l Ibtddtodaai aofaMaoo f PPOAla propalali by bfia|ia|
10 m i a f faa fai pjfad. aekaliod fa a Inai volumi of 100 with adula i ina 1MaalLBP8botila.
P.IJ TlRaakaadfanbkaUuuaoOKiadaanboMondina[aOiparnoni appoMlfaaMy4*Cm i aaaaaMa far aaaMlmampanati f mando faomfaadafaofptapnMlon.
fatatati
P agtiofti
Exygen Research
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000346
Interim Report #1-Analysis o f Fish and Clam Samples
E xygen Study N o.: P 0001131
Exygca Protocol Number: P0001131
ASMmitAminfaoo
OtflM byLCAO/MI
VOOOIHJ
i
92 mmirnA Gilftmton jytokm
92,i 9utamimt&a ma tltMra6ligei<*imi rMt i mt .pttpswd in rrw tfifiil vinStak*
922 Ito Wtowim k i tffk t mam^kK dtaiM il MWcnirviMf may bt
TPartfAMtM Vilw
...."JPU frto tM M taL ) I(j4O
wf3111t4004)
41 (0
tI1too0oo01____
iiw0425
aoi
94 04035
-
L00 0401
" 5 jji>1lacI naHtr-oa HW linh l ILi^aL LiygMinuMTOlitll bouk adZ' CloO' C.aptaafKauolhi.
M A AIwn-- --M ac a--oaoa--attorno<i-- daraayaapit>rca u
IM *M htaU|>
UL! E u fe ta lctirf-- laa -- (Wlcally I m J M I a M it l
m --m u l co--si Ml Wo -- m l ooatsh M M * k--
tuaaiiumln--0---- IMW>--Myp'* iilw --gy-- aolmeh.
103 Ke--I T --c Ibr 0 --I li kaia--yM B -- anOqitt-- *l I pccifail
iotka-- ty -- --a * ** M M --.
IU WaM I | o i fc -a i --M e -- L --Iypnyyl--a oafurilja iubi
flllU lia l iifm --a la lliiw W m in * u n lln o M a r lir U m niitn >U na--ONMaalaafraaaarlba-lkgia. IU Pa--M c --U ta M M la l-- M a lM a U w y--4ki--flacki. II.) PasbM 30 oaL S tl M w ta -- w -- L gSofM l 2 g Jlll-- *< 2 I
ofrM . m i 1 1 IC-NKj. Om llli-- M oluniia ii* Lofw ail--d . * -- L a fa t--i--lk . D M dlaakaa. Do --t all-- 0m otaui io
IU iS L te fet I mL im r - Q il Saaha ky itada M h MH i -- y--oMolam--ciaaaloaaa i i laOta, IUoh tu fluk w-- Mine auct, M to a n d ty M --oKM atO oM D ry0W OaM ca-- Indy btlbia uac. -- C yali^yiQ |oi w itk i itraac iofatcro--i.
P a g t4 l vf6 S
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygea Protocol Number POOOlD)
>jpllU li*
M*kui N--Ur VflOIITM
-- ' I
ANALYTICAl. METHO
'|
MiA ad1A * ) ifc4 trto Pi li i uiii>iieantaillt amuilaiiiaAci<(ffOA) in Filli and Cernatyl0M 9/M $
; 11.1 cm ill>m I m l p U m /leia m at c M j | e * la al ~3DOO ipm
. to-IOetoaea.
1]J O w l t o t a l* ta l a d itimad toB w ill-- t i l * i*d a m a n a li of
. . , to m u t u i Da*. C olto to item Id to 119mL aileriaad ptai-ahipa
flit.
I l i Add 1 m l t f H i M i a> Urn umyt I Urn 9 a L P i A y tuba.
Hm itawtia to to m it o |to w ta lldu<toanin-fcc-M taooBdiuidnmt
.. t o diwe l i r until-WmL adam m arili Ima t o lab.
11-10 Ikata tkanandaafai to~]l>
a 7li-ict]aa Alitar
11.11 Flaw f e t t a ta a ta fa -1 tearjaw*.
11.13 CaraU m to 50m i pujrpuyyl--n lutea imadaiaiait lu p i i l *.2000 ipm
to-lieto * .
, 111) Datatati* to n e a * to ama U t ita n e . C atto ite aiuto km to
` ama paar t w l laafc ito ale tta i I l k to aiuto Sum to initial
1 n a to .
U H Fata 30 e L of aealautTila flam ini to 1 )1 aulumu md c a n ta i Ih ito la in
' to aarna| n h t 1 lieta.
11.11 Add 34 t o t 1 * 1 * to to n a ta to p m 4 a to t o and . tutelato e ada* pian toni aMary la p in < I*C1
H it Maliato to ll utuaa. ty addito 3 m i 1 3 m atita acid in n in n i a
lliiliw to p id fla llre d i"tin im T i'iliiir l
11.11 Itauato to kaae ta HFLC itala natatopaaaUaptoN.
1 U I A to y tM to ito tttap to rn ito ti LOMSOO.
1JJ Hata to a * aiu to a fa * m ie i, aeepla ata* fcaalad ampia ima ihe 1 C W M i> t o a mStataiM andati m to i t i l i * fcltaw al
' maltrto aaaapto
111 ' In tin ta a iMQA lutaledta| ta li lato Bucarmota ncaartrnio lauala n u e te ivta d lta in a a lye ca lia t
IM Ab toiat h i 1 w litaelw t e l i l i amai bainctadadaato tacim iaami e to w i fa M *ta a a i tondedt w e to imaiape * b e t * wary 1.10 eeptaa A l m i t tmalu i. a m to au o f caltoetaa a m id i mar te latitatati to tataeaiap u f a M M e n i ky calibrali itaadanlt le inf i rat l tutry ) ainpln (mm a n i to i atcoiid w oftaatla(lll>. ta
to u r wan ntitatatae aleatoll me b l Ite tin i md tali jettnu in a ampia tal. 114 Uw la m m o d * aama to l utatali ! Usa n e l* cunua un pia ioa l to to eelye tiy Ha lli m ie ta li utili Ux aai|titiii| o fpatk aiut aaawetlhttoi laudani newHuHan uatapMmLpaai )) (or cqnivaa<)
apidi
P agi 42 a/6S
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
ExypsP iotocoI N im br P0001UI
wliiiiii \
WrtHwkwVflCOim
twmMMwinoi''TM
... 1
fetlMiiiMafat fPirftaiOartiftfti A ri* (FFQA)in Filh id
Clm byLC/U&M I
1X9 iM fU i f f i i AaiM oot m u ) rnteaad tu paia. Any Hfflpl Oral tu u i anPartnaporiia aluuld baUntardiknad andtaanaiyiid
llJi A aam nC ittab
IJ.i Cbawatega" " b`"lfdyte<|f a d|t a-i< W a r n tema parali atdMaaaa. I t a *13 -- a--at iacaranda tePPOA . tela 11 tm ja m Iaa(M* --a]Huai-- 0u teaa toartat datate.
IU Mated Ite M mat a Mania PMA lavata malar dun da LOO- If a k W aaaWiaaPPOA lavalapm tm te a OSppb. i n a nav UankMmpla
13J kaaaariaiadacnaalai<kaa)arfnaiilxwikaf aatkaMwaaa'M-iJMnf adrlaava ahaat. Ifaaamral hfa awdda te toaaptabla Ihiul. a lldrflIB flllA N H tolM rtM lll.
lid Any aaltebte tedaid toad te a I terai attillar by aain* ite Huaa Eire Tate ay ba kmladad dam te atbrnlaiinn rite ealibntioo aim . Haaaiar, Ite late water of alltewl teadatea dte Mold ba aacbdad Iaten a te W i a fte ta il wnnterafandateMated
1X9 Ite mw iltei oteOahte 9 * r aafflatewi ama m a te naa te M92 (R* bOJU). It Ite te la malia M l aateda teat tedia, then
Madate a rte n te ia l awafaawflaaahaaMbalanalm d. U.d te a l te a t bamaan andate ate aapte aval im art* a w ten
11*1 -------- y 1" 1-- Baalt teadribaaaaada ibla Kara!Miin aawalyllcaliaalbaaiteawaiawbaaaaaaljnad.
Id.) Ubate M itte n I f '111" *a n te lata te aaw nl atPFOA IbundOnpiiaL. bate an paa* iti aaiac te abaidad anna (Naaar aamteon maaMlera) waaaladby te Matal> a i aatem p a o fw
pyQ dam dliW aH .tr! m a . laaaataaitl
te
MX Itetefcteateiam tetlaaaaaM lteam ateafyP Q A fauadlaaB aiL
*-- i >^1 - p t ~.~ir--r-a t . Am i
pi*<rm(i)
nn
DP--telar by addotte teal ratea ria dfMad, ifpreaaaaiy
rwaiara
Page 41 o f6 i
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Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study,No.: P0001131
Bxygon Protocol Number PQ1131
) .......................... Afuxyncu. x u x u o o
Mll>B<fAMl}UfccilPniiinWo(frtUiwoaciwk AcM(TPOA)iriir!?' ChrakyLCMSMS
tO P w w tk * M iM v tti k a m an nuli bTITOA prior minoion, tt Mtowfetquatto*I dM flta pana* im vy.
R iootw ylH )"
Exygen Research 4 '
*>(<
P ag * 44 O f65
Page 107 of 132
000350
Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study N.: P0001131
B xw u Piwoool Number: P0001131
ANALYTICAL METHOD M aM M m btr V000I7M
M rtbei efA--Urk fcr *e n m r lm lM tPertumun M eiA M criP A t le VapMea byLCMMMI
Ambetwl T M b ( FHy:
Ita n lw e M IW IIIm rtO iiti
M e CMbp, FA M M I
Aemani Btr
_^-----------____ _
f i l l Cotn^Jy
1
Tulaawl I n in ; LC-Ufl.Bam I r m i
^ Y lrirn itiin l O ju T lln i.rrrn n rtm w rl
Exygen Research
Tolti Paini 7 P agt 45 q f65
Page 108 of 132 oocgsi
Interim Report #10-Analysis of Fish and Clam Samples
p. 109
Exygen Study No.: P0001131
E*yfcn Protocol Number: P0001131
1*1> i Wllilllfc
VOOITM
1I
ANALYTICAL M THOD~
J
H *J t f A flilyik farto to w w ita i! fTwfluww a note Add <P30A) in Vwuot
___________ ________ tyLCMS/MS
1.0 Stay
TMa-- h ui h a t ta ta ferlta ta ta w rai M ln iiii afpwfluoroocagiwc aatf fey K M n w i Uyrid r h w t f y lv cwpUd 1 a to ta l Man l pnW nW i Itaw nr (LOMMdS)ia w y ttlim
1.0 May
11 Alwpn d i n t a ta w u ijrm t a . 12 C tota to appapriMc M5DS|KMluadli* kny d lto ta j farprop* Itflxy
y awntf-- .
30 tto yla B tatato B l
M A ito a a O | fto iim |li tapBnwOon, 1.1 Ito y ta aoulObprocm id taltaratapota. taca Oit tan roipl in a
t a pm--* ta Ito iip aii i ni* <ty I. fl * to ta 1 la comunin t a fe r* op to tato* tona w l|H id Ha ta ta doaid ta tto rim M t a pto> 0w nuta 1 ta o n Dam* utM lim v t
to ta l.
U Stol ofl t a inotaam wiJI ta ip*cJlld la to amylino pta ta this
tafta
40 D l|ta t a l to to ll
4.1 W iw -IM C in ta M AcakaaiU - HfLC pal 43 Ctaa<110-100o u * )- la to ^ P1 4.4 M li ll - HfLC ff4a 4.1 S ilin | l<ta200 DtolO - R #m p ita 44 naiMKto-lOOiMalO-ltaamtmte 47 l tol4to LC-NHi-ta n ta p ito 41 l-O a to d -m C fta 4 * L-AaaoAicaeld-taiifMpta 4M D toi*|*lirtl1M toi-taapapid 411 T l t a - H i y t n l i 412 AlitoelltoADto-XCS.*44to*Olta 413 Pirllin iMil-- 1Add - ligna AWdb
SO Ita ito to l ta B iy ^ i-- t
1.1 A U|b yaitaw im UpM d u D m to jta ta * !* r pwiy'ta p u> l ta to ta ita * I* n rt lh tana ta a r tabla rtajtany 7-1TM
p i -- to laatin Ito M to H urtatapP IW M ).
12 A t o t a d ita I-- to t a p ! ju n ta Ia qitailaiioa. M AaaJylkaltataiaci4bWrrtaiai to 0.00001 .
Pagt46cf6S
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000352
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxytoa Pm oool Number: 70001131
1... 1Lru ~
kyLOMMCl
3.4 HMQrtnpMtar-
5. I iri. im Ltn|> i M n . i l 30mLihtmiMi iwljpnipyUni n i t r i t o Mit
3.7 I) w Li% nilH| ?ICf)lln Mndfc|l H* M
3.1 r `7 " -V i
(3<M00uL. ](^00L).
3.3 l23L L D na*N inwillilwNIa
3.1 laLttotK M C vW kit.
311 nMiiHaaiHdM.
>13 ^ ^<M(l0.l0l4llWHa).wkli3i3pMMU.
33..1H3 ImMatala(MalK|f l t ilrt c. a. W7177.
3.13 CM riw i<*fM3rH^Ni*L|al3|nnft(Ml*aim <|>m .
3.0 O m m iip^liia ty ra n
.I A^>aiodOolrat:]nwprat(ICyilcratiSfle).Ilm <r!<H}m m.5tj
M*Ji-03SIJ0) u J0*C i3 M M *n < A ): 3mMAmmoniumAmtalo hl Wwor M MrtH W tB ) ] MMmoI .] a lt n lM im n
Ttmafada} L
IA Ml m
&A 5 65
35 25 45
FW* Ra 3 U M /W fal 35 OJ 0,3 7J 0,3
73 0l3 35 0,3
i H W W : 133t(wtliwllton
6.1 Q itiH tiH in N tt A ra - n m l m in im itra ra urv,. i t ta iH w -23m lm ra
Ha * m a tttaH m M aA d pM * <Binq i ic fevart InOlt oprla dtt HFLClytMui
7.0 M iVBtymra 7.1 MdI c BlKMitii|rNMIVtMBUastt.noiilMrint6l]'3 3M ni/lte PFOA.
Pag*4fef6S
Exygen Research
Pagel 10 o fl3 2
000353
Interim Report #10-Analysis of Fish and Clam Samples
p. 111
Exygen Study No.: P0001131
E xygn Protaoot N uoten POOD113 1
H uhrlN ^tii vm m x
____
ANALYTICALM TTHOP
kyLCMMSMahd ^X S 5 3 n 5 cS rK 5 5 n 3 oa n fb rflutMorwaoic Acid(PPOA)>i
H i M m ttadUmm m hm sM aa tetto m * *y to kwdto order optM iteMtMS tymm.
.9 P N fM iH V M te l s.l MoWbrtaot
14.1 2 oM nmonlun m o m in worn 1proporod 9y lOdfeg0.1$41 of w t--nhwiw W i to1000nL ofwoiir.
1,2 BxtrottktoSnlutiooi
1001o f Mini1.2.1 2%eeo*to*6ld jeneOWittl ii pr^m d Vyd wofrini3 |o f ipcwtac
111 30%
fa Mflwa frp np id by trimiwi 3 m l
AMtovftlijgto<--yba ynpud.
1jo M fr*9 n in H n
94 3friw19orlriTnrTllrinnn Morion
9.1.1 PnpaniaookioMtaior-'lOO fifM .v fP fO A fry wti*WRg 10m*
oirufmtMrMiytrhirnitidmaM-iuodl(inwniwimmidi*tot yurily) Md tiU to 100m l wiih
9.1J A1.0|ictaLfcniiBiaQali4ai*fPFOApnfwidbytarin|iii^t L of 6 W0 jiffeL flotation to flotl votano of 100 with m Oum! i# i U3 mLLDFBOools,
94.1 A 0.1QftatL tartiflrtainn flotation ofPPPA y ^ jflred bytrin fjn j ID mLofdw 1.0pfteL w tek io u ftaaloolix of 100with ttfanal in i ttfaLLDPBtoMte.
9.M A M l n>fciil ferit f ctataa lotalifl of 9FOA to pwfwtl 9y bringing 10 ML of t o 0.1 M taL aatadoi to i flail voiun* oi it with w + m d b i 133mL LEVSM k
94.1 TM fltofciodfertiflcfltieoflotvtloai i n la bottom! Joboro ttjM la ru
94 H fflirt C ittifllfii
94.1 LC M W II MtAnflaa MadWb an pnopaod i i w O iw I vis dilution of*1.0 in W fcrttikidea whidia.
Iafr< u*
P a$t 48 o f83
Exygen Research
Page 111 of 132
000354
Intrim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygen Protocol Number POOOHJI
I ANaLYIK^U.MlItlOD I
iiSwd ofAaahS fcttttoB M aaahiltoa a fPwflaaiuiiu-- lia KaA (PPOA) i Vathatwa byLOMSMS
l i : Ite MkJtea* la a Tyy lial tumt&t; ihtioonl Kneantmcm miy lx
tftniu ,. Vataaa m u la e m u
-- w-- w -
u 15 tot 0415
1.0 1.0 m
041
4l09 IP m
4419
0.00
IO
0.1 IO
fl.tW . W
tot tot
......
4P 4411 BJO^
i l i i >aiioaiflaaltna -- -- to t23-alLLDWiianSwronahbaila
atFC la fC , apk>fix mosti.
tX * Atoaoaaavllwnae airi canaantraltni a fatandaria mayba pnpmrmj aa
m BoaLMUr
IQ.) ( -- to-- f aahptoa-- d ttyylatoly M or laaa) mut aa-ltrto m torn -- anteali l a-- al aad mb -- al ooauoto M U M ai known inaiianaliiiin flak i imaaI iiilli) in n itj lim il i ail racoYaryh r ite batch
I0J I a f i l l i -- fca iato ate itearaaiy doyitoMaaand ta te w ill baaaadliad
la M fuaUqraammm |ta i ha Ma aaajatl.
11.0 8-- laTi -- laa
11.1 W-- I | U h a a -- Ma H o f lU l yatyyropylao aatrifliga lutoK
(hrttfyaaoa*d,hptoaalMiitehtawn).
11.S AM tO w lrfaiaiaaM laaM -- icaaaariaUaiaaalialurhr-Hatiiwlaa
il.) 6Citro---t0--(a ha W, n L --
Mae-- i aarac* ai -M00 mi
n i M a o lM d ttftA in iA iia iid la iM lh e H a M b iiililiik i!
I l '] P M kiia lO te IS P t-- a la aananaa w tt 1 ( Itateli. 2 t attica tal. 1 *
te a . m i 1 f LOWIa CaaM aa ha a-- la wtfc M !. ola-- ami.
-- LafaaaM M a, Bla-- a waahaa. Da m alto* ha atonali la
hy. 114 to lta li ha 115 n i. |ia i h a lli Baaka by m ani whb ha m
0-- liy lllh h n illlaa la Ulawaaat haa RMahalaakwhkiahiaMMaa.
hhw te by amtiaaal (hwa Ito *). Day ha Haha aamyliMy baine aie.
tohaiby a M h iw wihaa-- a arnlt-- i. tu r Da-- aaatealaBlaiaaahliaiM Snaal-- SMiaaMahaiMMhar
a y -- ahapad (ah. Collact ha al-- In ha I n L ail--iiaat peeoabape
ra ic iu r-
Page *9 of6 i
Exygen Research
Page 112 of 132
000.355
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygea Protocol Number: P000113)
M ito t o * . . VMM'U
I a n a ly t ic a l m stuo o
I
tifato*ofAaafaaiifcrtb DamalabIm Wam--cnootoAuM(PPOA) inV tftm icT
tyL C M M fi
11J A**10uiLafaaoaMI1BtoaBaalalatoJOuilcaathtalito. l i t Bubotonntli miti t o - l t i t o anoB iutfrl toll* to r n . 11.10 Ctorifta to * L pofrpnpylto *>camini nmplt 1-1000 iy
. fe c ta to to 11.U d m to to m i to * to am i SPI c a lm Colimi to ilu tt inn to
ii.n m--*Miu tombmi mb-
t i l l AM J-4 to* o f I a n d H to am i la to pw-toao* B to and ' aro < n to * | i i i a--utog|i-- 7vp" * t*t < * ,0
11.14 U to to Ito utTtol, ky to m 2 mL o f2% ncortlc a m im toiul n
to p i* tom * I'M ! to tobHa uhM inrtvi. ll.U IVaafe to a to m id HPIv illi itoatopoanili piato. ll.U A tu fr* u npin 1!tlato w IC M W .
Ht ctonaMtUfty
12.1 a*oatoiaan n iniaB fm li mutoli -- pi miIhrttod Mmplt ilo to L Q M M ^ i.o a to A dUknHia at o u t Buia prua* t o M dw 11
; ||*i Inumili irnmrrrftTi r f '--'*----------- --*-1--
, a m ili ito ito k m >al]r>ioatm i.
I2.J A* i t o ila of u c M Ukrajoa to to d i mu* k* to i to d t o
ta tto a t t o a to t o T i laapi to EimoM u t o i* owa b
to n a m i* bto aa oiayt-10 ta i1n. A i m atoaalva. a i il to or
n in n ili n H to ln a to ut unir lo M u to a to koalaaiat or m
M u t o l p utoto* eibbitoi a ia to * laanpeto irey HO wialn
(in ..... al f~ r n rr-* -- -* ------- -
*~T ho4hnnn.olncu*
to n to M lu *i m u li to ito t o Ito lijic to i ia a n a li *
114 Un lato a t o u t ano to Iiiualalr U nir aaatot a m w
auutaai to to u n liw ly Uatowptoliui il| ira to g n n i rpn* m a
vinai --`" " to n a tia * a tto ala i vttac Mm Ljiui 1.3 (n totoU oil
U t l aipli tnpiQM tot** a n u n t o to ndini to p* " " - Aajr u o p ln dui n i n i uhit u *Hip.......... la t o t a fcl m * t o in aalyii*
1J.I f t a n a ty u t o hwa pa naia la ito n loan 3<* aaalkoa paoni 1413 ubi. ti 411 un pula impiiti n to PPOAalmi, toil to *au0ito loa(M ami)n p to ia lito laa o fto ta a to lto .
Pagt SOo f63
Exygen Research
Page 113 of 132
000356
p. 114
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygcn Protocol Number PCOO1131
MRMIMHORBOCnMlIieAcid (PPA)in Vayatalian bpLCMMdS
11J tM n d Mato matt aai aaoAiaPPOA huela fnaM dita Ae bOQ. Ifa Hak iiU e im Mleala |M H r Uua 03 pife, meei na taadt aeipti BM beebeatdad Aerad aatnaatbaieextiiaed.
11J Reamadle eTeiaant milite aadM h raUnaotai be betweraTO-llOhof Aablana tabee. IfaaeaaalapUae AUeeateide Ae aaaeptableUniia, the a t u e r fa ej l i i A iulii b e ii rabaehd.
1M Asjr eallhaden aM aid tum i U ba a etlacal outll by utln iba Muja Raer TbeL ara? be heded ta s EbefadatiBn ef Ae calibraran Peraer. Ae labal m b tt ef eettadea eMdarda A lt emU ba ciudad M I M cateadJOMefAa Mal tambara rfa b a * afectad.
IM tba ccnetaltea eeafficcai (A) Ae aaMaaHee curvea laaartlid anal ba bONl (R.' M.W5X H ulAaMrn rara AU Databa Huta liaba, bien HpWftAa tupe aaat be Aai a agaa laanaaM panden, aot iha afreta le A e ih iM taledeaaelca dicellbetcani lpral
4 Palia n te te baa aea Manteada an acapice mu* an driA tima Ihan 4%wUkiaa*raat]1ieali*c tf ralratinatunabrlft cacti aia liaill rajMit aaaaabtleal laaAaaAa M M tb a naaalymd.
14.1 Ule AeAAaefeg badeaacctheltia ira arapealefPPOA freed fia IciL, baaab aa peak aal aaiaf Aa KaaAia rana (Dea raeraaaMxi p*ameian> gaaraaledbgrAeMaaaL*aa raSaatepiafara:
mARaaadidgAal)
I4 J Orad ABewlagceeeUoaa} coacta dle Hawn o fPPQA AaadianfaaLia a(fbb).
^fb 2fQ^ie^tllUSeU*WiUfll
n r - ActatbpWebA t Aadvataae anaAbad, if atetawy.
MJ Poraatapia fruited wiA beiaa aaaauati cfPTOA pajal le tractne, aaa Aa ADeadalcatea A aalealataAapaaeaal aaeovaay.
laeoaarrOJa
[watl-- ln .lb u .d W it - MlKfcaAtheaatraMi<)l . |fl0 m ly ti mWi Jfo f/j)
P agoJ/ o f 6$
Exygen Research
Page 114 o f 132
000357
p. 115
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygaa Protocol Number POOOIUI
ANALYTICAL METHOD MflkaANutar YWOITO
MrifcMef Aaalpbtar MBmnaludaa i t M t a n M w k AM(THM) b lm * Mi m i U r n kjrLCMMM
Amlytbtl TMfaaFullQn .,
bn>M M k SWIlUManliDdv SttwCofla*. PA I9W1
AppmvadBjr
y t s c-jlL ____
TMcal U M , 1CMS,BqifM >MMKh
/VJgbkmst/FWaiwnnta/yi - i-.
_DmlillfcM -D*m A k
Exygen Research
,f *Wv/
1 W h |i: 7
Pttjf# $2of65
Page 115 of 132
000358
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exytcn Protocol Number PQOO1131
Im a o il
m m Huant veeei>
I ....................AAAiriicALunta
I
K eiedo ffia l X I tM YlHepiliiiiliioefaeJleweeeaeo AejAltTOA) inSaiell Meneel Liverby LCfldS/MS
1,0 Siepe
TWiieMttadienbe MepInjiiS la OleMeleto eedouermaUaerpertlecnacanoic add by H # M b m e n U pU Q naebpplgr ensiled e > tandem M at t pttdin i eBu de(LC/U&IM8?ie wi l l neeneoi liver.
M Jeibty
L I Abnyvleave adekbemaypncifen U Oeeeolltte ypnpiltaeb lip s bdbe heedliepe y chimipel fa properifny
10 Seepli Heptane
}.) AlleMSsefMieepplakrmkMlign. }1 leplnnaldbienodbfcwet oB. Pilo th binn nple m
b a ip ic ie ii eid I w n e ill wfll dry Im . PUm Ibeempiee le ceeieieea m i bee epie hi Uvea v i p ovemltM l ritow te- certe divavii edMenine t a l md piece he ampia bi In a i M onte u td lim e o f neljde A iaeoMly. Iftha le Im ittB lm emoiaaof appii-lon then d |).lla ev|en(HMle| ea May a i da aneli ; e beeeedn iuppliiil ].) tappi a ta t a t andem aW be epeeWed ie Ite a a > l pia (oc d
40 Pi i | pip adStindarde
4.1 Wetac-HFLCmdi 4 J Mettasi-KPLCpel U e a a H b 'H H iC p i 4.4 il menata I l i a i - A.CJ.teepee Pad 4S fa ttu a li oewii A d d -pmAMdeb
J.1 A b p i pirttcronn Ip iit deeneapepk eepeble a t em piei ep a 2 cllvaau eqelpped iti e verittie aelvn bpanr eepebl e i lejecting 5-2011 KMeecMda Medeat in i tpednenarOC/MSAai
i l A deviaa ebeame dea ftr yafc he|ieiiM ed gaeiduuleo 5.3 ApeiyPoeib tooe tpehe qfrmag lo 0.00001 J.
54 14aL dbpeablepeftpwpyMeeponilidipMba. 55 15aL Hbpeietli p rtn e ip jiln i nairifcpo abee
50 DepmUeafeppipe Hfr-IOOeL. IQO-MBeL). i l U aU W B eenew euedbbette. 5J laLeieaHNLCvMbh.
halvf'
finga S S o ftt
Exygen Research
Page 116of 132
000359
Interini Report #10-Analysis of Fish and Clam Samples
p. 117
Exygen Study No.: P0001131
Exygen Protocol Number P000113l
MkhpdNw*VCeenes
C ................
' ' AKA.VT1CAL UWmOP
'
tM U tt/m fy J fctIhDn-- irtw fN ribi i i rm ric Acid (W A ) Smll
H a u l Uneby LCIMSMi
19 PiBUlAIlptaMH 3.10 AMiyamXKB-lOOO |it.n d 10-100*1.).wM ldiipguttc tipt-
5.11 v io f c ( .S k V iin ( l|) lC ll r S a r t ii4 - .
5.12 0 B vacuai-- UtM. 5.15 Tim iiW ar. 5.M W lhhW toB**. 5.15 Ca lr iftii rpyrtli e t lira. IS atpolyyrapyl. lubaa 5000lym.
5.0 CTMoaWP^ejbir
(.1 A uliteti Cul-- ' WwiylMeSI (*ywnn.7-- tigc).5.1 am 50mm. 5*
(M*tWM-OTlSO> U Twin-- 50*C U N M H k |A |: 2nMA-- m il A*-- mW.U
H il
U deAbI dI OJ IJ U MJ zu
U
23
25 53
now k m
SU fa U u d 35 .3 35 0.3 75 0.3 75 0.3 35 Qtf
( 4 ipjittinVelacci 13*L(qnbciccvcJCOttccanchMSOyL).
tK.7 qM--iTtmtai:aK-2r3atdAnMJU.- CMC! ctccocni cilitcirr cere.
Tbilw urtWiw m nr flil Cf>f iWm i f l < c*n 3inria ep M te HPI M l
la MSMS^Ma
7.1 Ma* liriwiyn yW-- MM nul, -- tori 415- MOyfoi WOA.
ybaiMteMMS
h |c 5 .r.
Par5<0/6!
Exygen Research i \\ ?
Page 117 of 132
000360
Interini Report #10-Analysis of Fish and Clam Sandies
Exygen Study No.: P0001131
Exy| Protocol Number: POOOI131
______________________ MtMMmarVOOOntS
c a NuLVTICAI. MrTBOO
T aasnB gnsrrPllfnaraiilfaUiafnaceratyfWLCfaTnCaWocSwteAald(yrOA)ia Snell
I t wayaral oca fSalitesi
LI Mattonaia
L U 3 eM i -- lui me b M r ia pnpvad try M ai 0 154 , of afamtencaaitaa la lOOPmLcfwen.
Ataman nafaaaaamaybe payant.
9.0 P ittite Pi^uallm
9.1 Satete 9t xW9aaaiJl Lfaiiii Solitem 9.1.1 faaptmt Peek MMan e f-100 m M . at PTOA by w*hjn| 10mu f-- 1)1Ul1Mei1iu1(niiilfHit fHpnrlt)1 an! rtltM in 100mL with taaOmalfai !U-LLCPEboa>t. b .l.l A IO in tu fciPfin Pi actable ctPFQA I pnpa l by Hinyot I m l of(be 100mb!, aabelima Opal te a m t f 100ht wiftaaoi faa USmL LDfB balda. 9-1-3 A0.I p |ftB l.laitlPefaba aabpfaea fPPOAfayteaaalbybifagfag 10 td . a fte IO u U aofaPaeM t laal teaa of ICOwbk aalleaol in a 13}a i-U P ! balda. A M Tba Boat aaaltirttOnaPaa ad erteti am fa ba iknW d i lartHoraaor II apfeariaiiilely 9*C cal afabla to a aahnwc pariai c l 6 amata Pomte tea ofpaapanafae.
U l LC/MMU allibito Caa tllbia c f atam i In maOmolviadilulioii aTOe 0.1 M/mL ItaPlacPae aaltPac
I J J 11a felkteaf la a tmieal aimpte addtioiel ooncaanucai may he
Hhtem
ns*1 w -- IN 10 I1N4 10 U 10
w--
IM
IINN
IN
^UNl Caaaaatniian
^ 0 01.04 0.2
M l % > | | itllliiiban i m l a n t 111 ml 1n in n a r li'm in ili tintiln al rcac * C . ay r ia m a titi
4 AllOMO votona o d cw f-- i l w i o f ladiidi my be prepared n
Page a o f tS
Exygen Research
Page 118 of 132
00361
p. 119
Interim Report #10-Analysis of Fish and Clam Samples
Exygein Study No.: P0001131
Exyim Protocol N onber P0001131
__
f ' '" * an o
UrifcBl NuaAdr VttOITti
AN.tLYTK/O.MgTMOD f ttrtm n m nllirlm ofTiffluowomiloli AcM<WOA) in t u l i
M arnili U m ky LGMSM3
l.B B lkS ltU p
10.1 Bock bank of n o t* m onnl (Ijiieolly 20 Of Iw i) n u ll includ* lew
out m M M k l a two iMkMMd Maob M ilM known
' 10.7
rni i in n ip ia
m in aam
<inIMfoflioKtmloilla~i*r)---lo w1ilillyifplirnr--l-i-im-' n-foironn-yffU1*n-tTa
te ~
li. *
J
InMwpoJiOr-- iwoi
IU> I f l i lia iillin
l) .l W ap ] to fm fiiM o tWinLpolyoTCpyXM nrnnhaoM M lferUlyai ' pi l l i l i, union lid nkP t WB). Noli dui lanuti tifili o f liw maybe ' m M w M M y iiiifa lilM n a p liiliiiillM iliiiriiii.
A ll waw M l* i f l i fcr hS ootaai <W n L
IMO 15 m l.
idTmL ifiM M Ado~mihdn far- minotu i wriwlion M r . o iM n ip -- im a-joa ^ m .5 w h . Du m i m rntta m m Imo 1 30 m l MmchMom nAfc M o m> MO 35 L ofvtM(< 11.1 f i l i l i m * Cu s n Mia ilp i (I $. i *L> ty ihi Mim N ml. natami W n n lyll.ofH P LC w >a(-l nylMC). Do loiu lu li ranilfy
' 11.1 l i t i tkoM*flooa<gaMliMOICu SM om U|A Diicud an .
11.11 Eta M 4 l f Mattami. CMM 1 Ml. of Ululo imo I M lyU lpuiyylM i n-kim o Mkl (Anil witam 2tnU
11.11 Am Um aaila M ini H iiipnj LOMatMl.
1M
M M i m i i it ofash tO M M S nM
M M ampi into the fallow l l
|3 M u d ili pffFQAof m dil lo K lu t iw ornonoeoomlnlloci )vll HMtW lHtaMlBW italyfciliit.
1X1 Al iMmo1 of i i HiuUm -- Milli l i n o lnchwlad il II bollinoli wnl Al in i oCi tm ajk mi. im part m i ta t a f f d t a n n i w ry S-ll imqiIii Al > U ta ita. a Dii in of a lM I o n Mcnfciii n> t* MNt * Mi MpnMot of i m IkHowOd kjr ctliOnuoo mnSrti. lin m p u il lYMyHO im p ili (lo ibcoiiihIm l wcond m ofWMdiinJH in
Ma MlhMIIon u m ilili am i ko I n Eni m i lm in jm ii in
in a i m i 13.4 Um (m e m im i im o Mr im M U t*. Uno* M udai m vm fa
M M W Ai Moti ta IIm v M unitili M ix Unw*i|bfci|ofynk im
Pag* S f a f f i
Exygen Research
Page 119 of 132
000362
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygm Protocol Nvmrfcet: POOOl131
MMad to r to VOOHH
a k a lv t ic a i. iw m o y ' 3dltoda<Aaal)'0l C ato Drirm laII rfprrflanrriilitooiArid(WA)in Borii
" UvatbybOM/MS
romoaato a lh a M in t um uniilluii aatnp M M Ljini 3.3 (orrqaivalinil oaMB4QfMMI.
1 U t a p i r '**' O m it 0 n u r d aondud mpoBota. Any ampler Out f t r rria d <a f ran t o li ba t o lto dMaiadandatooliiied.
13.0 n n rip ta m rtllrli
13.1 Olimo n y i mini * 1 port QtaOaa^iIrr OO1369 m u to rt pm
T413 an. H e 413 -- n o r m n io m ti <oOn fFOA irto, mil to
da rM * loo(340 homi) upwim li Hiloro<onW diario
131 Hiked Mrab M il lo t eecaaa WOA a Inoli p u m ton Kir 10Q. If a
M toaialalniPPOA la tto apramitoa 10Bp'l, to r a n biadi iim pli
Otetotod m i feoaito artohmbon n aia4 .
133 M arnato ofroaaalipaneoadiaaa!]i ito a m la tow 70.130k of
M r k m n i If a aoanllka talk MM* dieaaaapUMa Uniti, (hr
alto m of 0)000 okaaH ba
Arp nutrjr rpft* aauidr 70.
I30H to il* la rrotoid Ijr fee aaaiyat daunntar if raaMncdett 1
134 Aagr coModai nadaiJ toad ti to a OMtofal amdlm byuofaf ibr Hapt Boar Tool, ooavla an M rt Boa Mo aoieaMoa of toe eatitotoa earn. Hoatoar. to Miai aato* of ailbrdtea Metodo to! aeM 1a oelodad MMaaioaeood MKoftoiniol toalmafatodaoda ln|aaat
I3J Ika ooowlodto Holto 01) to mlUmrtoa a m a ptondrd am ba
M il (Rf MJU). If eattadlaa n a to Ml adda Ikoee b ate ton # 10 1 ape m m la M m a adfaoi laoaimot opawfan. and to OM to* 00to Memota* ofoaooptotoald la rioaalyaal. 13.6 Mototta Mao M arnai atotM o aad a a p to a m ael drt* mai toa d 4 k rube aaaUyteoltar. UMmaiaadamdrift raparOrthia baili within
aaanalyticalaaatoeato eata m la nmhoad.
14. CohatoliM I4J Ito to PtiWrlni na tlje 3cricefaartip atteraofffOA fonditi eytrL. Mod ra pact 1 0 aoia to madori aaw (Him ropreoioa pompeiani (aaaOrdbyto IdOMLyaaatom pnpnat:
PROA lhiad(i|U L3 - (BMsMdiotoBOBlX DP tom tolar
o r- tourbytrito to Dualaiutaranadiluatd. raaoooaafy.
k p ia io r
Pago 37 o f6S
Exygen Research
Page 120 o f 132
000363
Interim Report # 10-Analysis of Fish and Clam Samples
p. 121
Exygen Study No.: P0001131
E jty itn Protocol Number POOO] 131
MattedNwefcarVttOI** a k a ly 'iic 'a l M jem on Maftgl pfAM M ity to * Diliin littiin fPeriliiwuigHPori AoM(WQA)toM ill Mmmm) U m by LCMSMS
t i l ffbeerfwolkivwIimtttiMottHMrtnootobhooblwrwttti l>De|ewttsttgfwffeOevAryp.rior to wtreciio. ac
lnlM i4bii4aiH nL) n fri ia a 4 l c l IM m .)) n m
14.) U w *iM bwim r|iiliM <giinm *nwuo<TFO A fo x ) in imfmL w urtipp*).
Exygen Research
K tlltfT Post S o fts
Page 121 of 132
000364
p. 122
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E xypo Pwmcot Nwribor P0001131
AitlyttulTw fcif
ANALYTICAL METHOD M a M M rtc VM0IM<
MmwmI ( o n ly LO M tM t
In n a K in m l 30W fcm rth Pmn (utaOMbiAPA i m
3~vA c- aL___
PflriCj iw B y
'
I
Tw W nl Imfue, LC-MI.b n n RnNiCh
--ttlxfcfar
D in
Exygen Research
TMP^v, 7 Pag }9 a f4$
Page 122 of 132
000365
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
B xyjen Pnioeol Nuiabcr POOOI131
I M U LYnC A LM tTItO D
i U it i t i lliyk i tlU b m m m iiliimofrm Im i lmaic Acid (WOA) in SmiU W-- il horn VyLCtoWMS
1MBcfeta It w bmpli yHl ferfe iB ltaw ad qinta twineo f p n rfto iw w iw k M 4y Bita IwI iimpc Ufcid Ctcwnoin phy h ^ M to tnadon Mnw i Mcwnm te o tm m jfjq tta M i}! m i -- i m m .
10 laMy
M Cww ill dw^ywpriwcllUPI tafewhicdllni my ntataic l fo ptcpwMln'y
3 limpln ftnquaw
1.1 MtaulBl.(IMiMylifcfeMliM.
Sx] J N a w n y to n im w itl k w M
M M E u n p i n - H e w c v o f. Om m ru m
liai k im d M cm plm lyttnr Mnon H y n a a ld R <iw.
atM S w y te w a w o e p r o id w B n t a # k I M b w a p t a i p la n * r U iii
ynJiB.
U ) il| wllltaaiwfepll
4.1 W aM r-H fljC piia 4 J 1M n)I-H ]TC |M 4i 4 J A M ta U l-in C fl*
u M M -lipuoU feiak
5X1 In W --I wit llqiita--*
1.1 A V * p4ribOMM* taN* it-- Wafe0*i oapaNo o f powpiei w w 2 w lnoti aifpta wife t Mrifek talaiw ta Mp *l of taowtal S-2>
| i l tomiPCPt a ip p lwW-- Mwp EpisPwwQPr (LCtMS/MS). !J AM ntoM llM ItiM M oferyM ikktafeilionM dtaantIM taL
5.1 AMW ilta li iiiriptalio fi ta l |i ftW ` i5A 14bL ita ` " Mipil)pnpylw i H t p i i t a iJ n il liopPitalpoljy i uy/lww iBiHifc y tutap. s.4 wipMiw B ta ^ ip i (iM o a a . innaL> 3.1 ll5taLm >M nowIBIIfetaM lH. 11 2b L daw HTLCy ill Idt. j j pli^ipiaHiphMM. 5.N Altapipitai flCO-HWDplnod IM W p lj. wife dKpoMkkdpi. 1.11 W M n S ta ta kV M lM {1 0 tfllS ra a n ld |M .
55..1133 lVyMBimwwa-- w iliM
P a p tO e fU
Exygen Research
Page 123 of 132
000366
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E xyfm Protocol Number! PCOOI 13t
~~
,______
Mato* Mato VMM?
wriHOp
"
_________
MaieiM torvi by LC/M$lVS
5.1+ 1--r|--I ihbhr.
1-U eMkthtocpade<r*pleniat 15m bH irnpytaH M e M3000 (pm
1.1 Ael)Ma*m iitor F lnrehtolIIP(KayowSriondflo), .l mm !0mm. iu (i/itbw eV JU O
t* T a rm a i: XPC 63 Mit ili r a n W ! ZbM Ain s ilili t o M m Wmb
4 M o tO *rto M (B }i -- ---------
5.1 O nm tnpm n
T u ffa i
w I jO a.o 20.0
au
49 OS
OS
Plow Ita & ImLAninl 92 0.3 35 0.3
71 0J 75 0J 35 OJ
M Isfiam Volos* 13Z.(cm bobm snU n nudi m 30 iiU 7 O n d a ta ; M c A m -m n B liM M a M n lla ia im . i t R a s lW -U n to la
Ito tan M dM osimlM M to4*spt3l tod m y bo dan|sd m ortorio M to a lliH H jC tM
7.0
T.l IM c Elwtre*pr*yNi|i<>v*MBM meto, a m o ri IJ - M b im i Ibr PFOA.
Ik* abewi laoMtlaaa w Is* I M M 1 1aide Ad m y be tosato io orda io
I. tapHMiMeUto
1.1 IMO Dess
1.1.1 1 eiM a m a to * m m to m u r io pnytieb by adding 0.134* of s s iin e f cottoio 1000 L o fWr
Asseto voltoloMiyb i posporsi
haw
Pagr 6 ta f6 i
Exygen Research
Page 124 of 132
003G7
Interim Report #10-Analysis of Fish and Clam Samples
p. 125
Exygen Study No.; P0001131
Sxysm frotoeol Nimber: POOOU31
...............
ANALYTtCAl. METHOD
_____
|
Maafl t f Aaalyiltfa ifla-D-m--a-b*ia-lt-a-i t/'rSa'f*la'*ta'"a*e"tlanaio AtH (WOA) In Small
1 .1.1 rm >H artcO: astata f-100 UAlmL DfPTOAby wviphini 10m. atim tytcai m in i latin it Ibcywity) id Hurt id 100 ail. wiiii
* aatttaaliaiaR M .LD K kH . 9 .IJ A 1.0p |M . fcniflaafla* tohlfloa ofPPOA IdyttpatN ky tr!nm I .. iL ofIk t 100n*anL wM m M t Imtl vslann of IDOwitk m Udmi : . IstU S niLL D n tatfa . 91.3 A M HQHLOrtile tllt ll aahritn afffO A Ity wpi J ty b>nn I
. a t. CDlJ0MtaLMhMigO IDt flirti voIm m o f100wMidwAuidi in aU S iLU O T bsifl*
0.1.4 HrtrtacfcaafllhilWlartlaa anim a i nato to wandBia nW (niiint
: wwalaalyO'CaarfaaartMa fta a in Hmm pariaiftin m l
M
111 L O M M lt ofArt01 pfm L fta rifc a lii aaMaa.
9Z2 TI M a ia la a o ffa d ia n ifla : additional ) p n p jn d tt omM .
~PST
v dihiiim iow raty N
IsW*
;a e
g -----2I1H.J00
W111000000-------
100
1ES U-- 10 1.0 00.SJ
411 a alt atUwlaa m m it ia 1U-<*1. LOTOM rnm -nM li boni ' iaZ 'C ta f' C.iVlotfiaoaafea. 9.Z* *Ut il i d u n md Mocaw ib iii o<andanammfb. jXpyod a
10.0 BaKtSalUr
101 lath teak afa
Oyfiaaly 10 or laaa) auiaa iniliifla al Ita*
' oaaarol* fenttlad know
aan n i ant flab iaaaia1i fca) la vtdftrQiaaaOinal iwowry brOfbWh.
101 HiiilniaaMa Or BtU and lateiaaHy distort and
wiltbeapacifinJ
ia Ibt quality t a n ta planOp(Man iaci.
Pt4r^
P qgt 62 o f 65
Exygen Research
Page 125 of 132
000368
Interim Report #1-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygtn Protocol Number POOOl 131
M Ktot NunMl VW9I?
c I Add (FFOA>h SoaM Mi m iI lo w by IC W IC
ll . l Mu m 1mL af
Mioa a t
canuiAint in to (ftniiy
MaaadaiL Nplaaa bd and nfct to. nm* dun afctmMn vobunaa of aetuni
nmybo maaoMddaymdinaon I lit awllobln (bran.
U J A d lm rta A o a ta v la A rifa a ln n la in to rK iiil. CaptfaMv
li<9 Vartgr* j
r7
IM ItaflUk t ! of fci
w t * t M tpirtte ^ mo* (mo I f mL
tfdpaNbli owlri&ti t i t a lid AM J a finnenlollt andiM m Ibr-M otaa lii an t o iio-artlM thtUr-
lid C naattifilitaA aiM -M O O w nte-yailuiiat. II.? Enetw A t H i l l Il> a S t mLdiy ahlc oeaaifin lube lad idd 3}
LaTM ar.
IU OwdMan A t Cp t n m tstoim (1 a 1 wU by pinalin 10 aL meHanal
AUawadbyJal.on<niCvata<-ldNA'tM>. Dapal 1damnrundry
11J> U tdA tta*loatoiidM aattC Hin tM M n DiacaMahiw. il.M Hata WM -1 aL afaatAtnal. Cailant 3 lal. of oKratl into gndutwi]
H tLinVpwpylm n HUm [Ml (fa it elonw- 1 LX
11.11 / A ir aaaiglM a ia i tar t an U A O M
li.0 O n W fifh y
U1 IniaaMbt lamaaMtaatofnacbnandaiA inapt and M illBd m p b into 9k I f M I M tfm m . A calbntno ataudaid m ai ptaeada and Star* ad
IU tiw l adaodffOA n r at|iartingw atlaaai tan tan cancaiunuianlevait nwttd* iniW ail iaan atiijalaal taL
12.1 Aa aadktMafaallhralian naadanltmuabnlaatndtd at IM h a p t.it; id m
Ataidafaaanplaaai. tltaadardanatal bt iaam tn nid baiwtoa atry 1-H>
_ i f l la Allonad by
Iniw pil ltd aaaty -I ita |l it (to intntni fta a Bal'dm e faandmdt)' la
~'
i nuat b t Aa Ural and lit I ' `
ISA
lArdoioiatytaby NnaarraMntaloit aaM| l<y wainmintofaaakana ` aatandaid aanatabatlan **m$ MmaLyn 3.3 (ar at*nvalent]
IU . .
.
M udM obO lw ^M M ifcooldbf h te d A M iid MMlyiMi.
(La:
^ tuff
Page 63 qf'43
Exygen Research
Page 126 of 132
000369
Interim Report #10-Analysis of Fish and Clam Samples
p. 127
Exygen Study No.: P0001131
Bxygm Protocol Number: POOOt 131
lo in lin iiil
M ufeiN iro* vawirM
1 A JtAiVtlC ALM ItTM oit
M iC to C tfAjulytbfcrtkt f l o w iro lfce qTPlrilMOlPOftincar Aci<l(ypOA)ifttinaJl Mu h m I Suuh by LC/M&IM3
13.1 O m unuiu we U w )u*
on Mb u n i 6oifeii
of413 mu. I to 413m |w lc c n u e u id >lto PP(Manion. wMnlw
dMgfotr m b (M 9 M ia) npnm to Hit It
Aatidi.
13.3 MmM .M m* * n w w ( onto PPOA m icvtta p m tr Um t it LOQ. if
Uflflk M in rrO A M to ri* r m * f t * 10 itriiL , rtm b m w tank
MOpilAftW iN M l Md MilttM IN tt I f M-MWMttd.
1 Pi ti'inM atttriw i --1--Mi Mila BMOb -- 70-130H of
Anir know* nhw . V i M rin l tpfln Am i ritta Am f t t l l i Uhim, Am
--Mt u t f f -- j Im foouWMtit d iia M A u r-- U v k * onuta 70
130* Am M At wAwm for AM mt&y* 1 4-- -- If m n t- c i-- a
IM Any thhm tif ito ri * found to be n ic y ouAwr Ay w tof Aw Huy Shot T it, may to fto feM fo-- Am p>kni>ttifm o f fto cttftaiioA w m
H w m r, Ak im i n n b tr t f t if c r t a r t * * Am ml* At w totto mnHnnt n m ri Tim ^ Ito HiM ^ mIim ('iMlnili ifowfoi. P J Dm Borrrirfot t t iOciMt (R) for w fo w in tw v tt p-- *tJ mult be
. A0.M2 (EJ K X K ft I f aaBfanbm nm k$ M l ouMdi dme Haiu. then
jppWflUlt MfM AMU I t tifeM 1 * -- foM-- l O p-titA, tod the tariatoerltocttor-- m ttfaaiplaMimW to --nly*A 13.6 Rilwriwi A m t tA w iiH OiritoOi in i m m 1* nun net drift noar (Nil A<* wild m m iljAw l rm. If Mt*dee dm#drift acw di M i lisw wiHim
ICO ftortafinn*
VM UmA t W tow li u n iA f to tita U --Am -- umt f FFQAI`am i (in ngfaii. total m M k m i) utfao Am m l Ml rv * (Iw v n p -- lo* powtwi*) gHMMtty An Mw Lyim otw ptopim:
PFOAfonai(ftf/tol) (EtyunidfclBBQRL * OF* rivuoi deter Mope
J f * Am ^ vAA fot Asti tr illic i m i dlimCif MMNOr. AfiqnotfoMM20
i l i Far --Mplti AkAIM Ah ta r n mommi AFTOX prior to unction. me Am fotttwtop fu r ia i to ctkufa*#Am p-- mcowry.
R-- ?(% )-
l l t wAanbtofoMMUniifoiD - MMlytofoori ipooMroJCfrinL)] _____________ IdtfolMdfodfMMfotU
h | lir7
Fogy 64o ft)
Exygen Research
l i : V : ,1 i 'M :
Page 127 of 132
000370
Interim Report #10-Analysis of Fish arid Clam Samples
Exygen Study No.: P0001131
Bxyfeo Protocol Number: P001 15]
APU4YTICAI. M E^O P ............ .....................1
MnhX tf^n riyrh fcrfte Pamnb irinnofN tflincpfW wic Add (PPOi in Smell _____________I f w i l tw a ly IOMS/MS__________________
143 Ub**e JMovtac n^riae io avert * t twiM o fPPOA(bund ui tfmL w
' 99*
MR^tovohiMt (mlp)
Exygen Research
.1 P*g* d i o ftS
Page 128 of 132
000371
JWW% Interim Report #10-Analysis ofFish and Clam Samples
p. 129 Exygen Study No.: POOOH31
ir
RESEARCH
3058 RtMMdi Drive Phone: 814-272-1039 State CoUet. PA16801 Fax: 814-231-1580
PROTOCOL AMENDMENT
AmendmentNumber 1 Effective Date-, 01/1W05____ Bnmen StuA Number PC001131 Ctienl Study Number___Mp
Pagai cM
m
1) Anetyticel Procedure Summery V0001780;Section 8.1 2) Verification of Analytical Procedure
1) Add to Section 9.j: Section 9.1.8, Alternate weighfe of standard* may be uaed to
prepare ritornale concentrations of stock solutions a s naoeeeary. Alternate levels of forttilcetlon eolutior may ateo be prepared. 2) Low and high spfcrig lavata of me analytes lor each matrix may be altered depending on sample fee evitable far extraction and/or to cover analyte ooncenbalione anq>ectod in the samples.
--------------------------------------------- RAftNU
1) Itigher concentratone of atandarda need to be prepared In order to prie th ampie
botte itN Q h irlM b . 2 )The ampie ab velatile for amali mamma! (ver andaerumwas mailerthan Kpacfed. Splkrig ri tire predetermlned levrieri rie protooolputs rie eplrsd ooncanbetion tonerthanria detection Irntt. Also, rie anaiyte levale Intha groundwater aamplee eoe eogreoted lo greelly axceed rie predetenrtned spUdng tavoli Isted ri th protocol. Whenrie levala ri rie tampiesgraatlyexceed th apidnglevefe.an accurate
recovery varia cantra be caloulaledforria OC ampie. Hlghar spMng levai Inrie
boriewU coverrie analyle concentnriona aapsded inrie water aan^lee.
IMPACT ON STUDY
The LOQIs 100 ng/g fra O.1 g sample of amai mammalliverand is 1000 ngAnLfor a
0.01 mLempie cf smal memmatserum.
.
Higher levale of spiking for rie wafer samplee wit ensure that more QC recovery data
can tre used.
F
UBRARY>:W00012JM*
J52
^ L - j j a f i i --------
Btyffan QAU Review 1 .11 o titi I f
ADWINISTRATFVE FORM
t
Exygen Research
Page 129 of 132
000372
p. 130
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
3091 toward) Drive Phone: 814*272*1039 State College, PA16801 Fax: 814-231-1980
PROTOCOLAMENDMENT
Amendment N u m b e r :_____ 2
Effective Dote:
03/07/06
Exygen Study Number P0001131 Oient Study Number
r ~ DESCRIPTION OF AMENDED SECTION
1) Report, page 11 o res
2) Test Materials, page 6 of 6S:PFO$ transition monitored 499 90.
P ageloll Nene
1) fnetoed of one final report. Interim reports m be twued.
2) PFOSbansMon monitored may aho be 496*80.
RATIONALE
1) Due to ft oaceea.vo atae ofw date sets, Interimreportswtl be tesuad to aflow the
cileni to receta dla Ine timeliermanen
cifm f*r 4 * s
2) The API 4000 LCMS/MSsytname detect the 480 *>80 PFOS imneHonwith greater
eeneldvhytoan the 480->99 transition.
' ' MFAgT~SaTCa
1) The dent mM be able to receive and review the dala moraqUddy.
2} The 469 *>80 transWon can be detected eWh greeter aenaMvIty, belter rhrometography.
giving
M & zL
5
V w qS ra^-
o
LJBRARVD: V0C012ta-t-
I
TSC"
Of
kt
BtygenQAU Review. L u a U e
ADMINtaTRATTVE FORM
Exygcn Research
Page 130 o fl3 2
00373
p. 131
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
W-1C-W05 VMSpa
F ro a -IK T SOUiriOR
n
RESEARCH
T-314 MOI/J04 F-4J7
3058 Research prive
Phone: 814-272-103
State Collage, PA16801 Fax: 814-231-1580
*.t '
DEVIATION FORM
-EMtlSLL-- _
X Project Soedflc DevleBon ___ FocHtyOeytattcn Dale cf Occurrence: 08/29/05
Exygen Project*: P7W H W
. Deviation#: _ 2 _
Client Project#:
Reference#:
^ DevilatfainJwfei flndutft \d to'r n 8"n jitia n d 5 0 P )
GMP GUP Other
None
X Protocol
____ Method
VfrNA Notebook reference: NA
_____ so p
L o g in # :
i4 2 6 4 A 4 a s 6 Container#: O OQ4BO-a6 L ot#:
M.
^ n a ^ r S b ^ ^ S ^ ^ e a n to t and fortified control ample feach matrix w# be analyzed; however,
control dam w as not obtolrwd. Hah waq w ed ae the contrat for the anayP aeftoaea six dam
Can*:
Preparation___ Analyste____ m stnnwnt __ __CUent Request X Other
No napathflt impact on this atuCy.
Exygen Research
Page 131 of 132 O O illh
p. 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
M -JM K :3)m
free-WSTQN SOLUTIONS
n
RESEARCH
t T-314 F.M4/D04 M 37
35S Reeewch Drive Phone: 814-272*1039 state College, PA 16801 Fax: 814*231*1580
DEVIATION FORM
RBW.lgfJ-
X ProtectScorihc Deviation
Facility Deviation , Oats of Occurrence: T2/Z7AM
Exygen Project#: P780/P1131
Deviation#:
30 .
CftantProject#:
HA
R e A m n e e # : O S'-f i Y fa-x'
Rw iw o t v f t r lS T
QMP OLP Other None
Sawrte Description:
Deviationfype: /incue VHihrmeffMtfJ and SPT
_ _ _ _ _ B ra t c t
_ Method
X SOP
VA 208*20 Section 5A3
Notebook reference: NA
Logrie: ........HA
Container#;
NA Lot#:
NA
SritMsmnrneeSS^chtaraaNane ri Toluene)wee ghwlheiKpImllon date of 02ri3M. but RE544 (Toluene) uaed to melee SL2114expired on 081288). U 1U was ueed to artteed gteseware preparedforthe fleh extractionrimi 1227RM (hrough 017/0S.
Cause: ____Preparation___ _ Analyxi*___ Instrument ___ Client Request X_. Other
lonegative impacton the study. Toluene wee used only a solvent forthe gtassware preparation, DimethyWIchloreelfene. which lathe coating agent waa notexpired.
Deviation blued.
Study
(Q yJt. SkL& & K
QualityAssurance
tfa/cf.
Date
Sponsor Representative Sponsor Management
Date
Exygen Research
Page 132 of 132
000375
