Document 0qrqDR6KLmbjg610E1XnzyeBd
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A K S .A 6 - U U-
INTERIM REPORT # 10 - Analysis of Fish and Clam Sample
STUDY TITLE Analysis of Perfluorobutancsulfonate (PFBS), Pcrfluorohcxancsulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal liv e r 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 DATE May 09, 2006
PERFORMING LABORATORY Exygen Research
3058 Research Drive State College, PA 16801
Phone: 814-272-1039
STUDY SPONSOR 3M Company
3M Building 0236-01-B-10 St. Paul, MN 55144 Phone: 651-733-6374
P R O JE C T Protocol Number P0001131 Exygen Study Number P0001131
Total Pages: 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT
Exygen Study Number P0001131, entitled "Analysis o f Perfhiorobutanesulfonate (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.
-tananiiFl laheirtfyA j ' . .
/TPrirnincciipal Investigator Exygen Research
Weston Solutions, Inc.
Michael A. 5ro
Sponsor
ntative
3M Company
Exygen Research
Date
Date Page 2 of 132
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Interim Report# 10-Analysis of Fish and Clam Samples
Exygen Study No.: P000I131
QUALITY ASSURANCE STATEMENT
Exygen Research's Quality Assurance Unit reviewed Exygen Study Number P0001131, entitled, "Analysis of Perfluoiobutanesulfonate (PFBS), Perfluorohexancsulfonatc (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". All reviewed phases' 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 bisoected
Date Reported to Date Reported to
Principal
Exygen
Investiestor Manaeement
Date Reported to
StadxPirwtpr
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
'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:
S '/? /* Date
Exygen Research Facility Management:
Date
Study Director, Weston Solutions, Inc.
Jaisimha Kesari P.E., DEE Weston Solutions, Inc.
Sponsor Representative, 3M Company:
* Michael A. Santoro Director o f Rdgulatory Affairs
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Interim Report #10-Analysis o fFish and Clam Samples
Exygen Study No.: P0001131
STUDY IDENTIFICATION
Analysis ofPerfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Pertluorooctanesulfonate (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: P0001131
TYPE OF STUDY:
Residue
SAMPLE MATRIX:
Fish and Clams
TEST SUBSTANCE-
Periluorobutanesulfonate (PFBS),
Perfluorohexanesulfonate (PFHS), and Perftuorooctanesulfonate (PFOS)
SPONSOR:
3M Company 3M Building 0236-01 -B-10 St. Paul, MN 55144
STUDY DIRECTOR:
Jaisimha (Cesari 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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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
PROJECT PERSONNEL
The Study Director for this project is Jaisitnha Kesari at Weston Solutions, Inc. The following personnel from Exygen Research were associated with various phases of 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
Page
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
Eag
Tabic I. Summary o f PFBS, PFHS and PFOS in Fish Samples...................................... 23 Table H 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. Matrix 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 VL Matrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples................. 49
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Figure I .
LIST OF FIGURES
Paae Typical Calibration Curve for PFBS in Methanol.......................................... 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 Methanol.......................................... 55
Figure 6. Non-Extracted Standards of PFHS 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 Methanol..........................................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 l 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 (Appendix 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 of 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 L Analytical results and assessed accuracies for the analysis of PFOS found in the re-extracted fish samples are summarized in Table II. Analytical results and assessed accuracies for the analysis of 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 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.
The sample IDs assigned by the client follow this formula: Dxx-x01-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 die 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 (Corbiculafluminea)
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 die 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-F01-1PF004-0-041021 is the filet tissue sample prepared on October 21, 2004 from the fourth channel catfish collected at the Bakers Creek mouth sam pling location.
Sample DL1-F01-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 perfluorobutancsulfonate (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 of 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 P000U31. 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 SAMPLES
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 C00564SO-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
pxyRfflfovntoryNo. SP0000252 SP0005726 SP0002401 SP0002694
L o t# 101 101 SE036 430180-1
Purity (%) 96.7 96.7 98.6 101.2
Expiration Date 12/04/06 12/04/06 10/18/06 10/31/07
The molecular structures of PFBS, PFHS and PFOS are given below:
PFBS Chemical Name: Perfhiorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (C*Fc>S03'K+)
Transitions Monitored: 299 - 99 Structure:
O s'
FF
PFHS Chemical Name: Perfluorohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (CsFnSO'K*) Transitions Monitored: 399 -> 80 Structure:
S 0 3' FFF
PFOS Chemical Name: Perfluorooctanesulfonate Molecular Weight: S38 supplied as the potassium salt (C tF n S O jlf) Transitions Monitored: 499 - 80 Structure:
F F
F F
3
FF F F FF
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6.9 DESCRIPTION OF ANALYTICAL METHOD
The analytical method "V0001783: Method o f Analysis for die Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS" was used for die 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, die 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. A ft 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 125 mL pear-shaped flasks were silanized by first rinsing the flask with 30% dimethyldichloiosilane in toluene solution. The findTM were rinsed Mice 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
florisil, 2 grams silica gel, 2 grams o f carbon, and 1 gram LC-NH2 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 this report.
package associated with
6.1.4 Sample Extraction
A 5-gram* portion o f fish or clam sample was weighed into a fifty-
milliliter 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 -1 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 ipm. 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 die 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 tax milliliters o f acetonitrile. The rinse was added to the sample tube. The samples w oe 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 the same clean-up column. The eluate was collected into the same pear-shaped flask. The column was washed with 20 m L 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 flask s 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-MSW0010-041216) was used. All other samples were weighed out in 5-gram portions.
6.2 Preparation o f 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 of 100 pgftnL 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 of each o f the appropriate stock solutions and bringing the volume up to 100 mL with methanol. By taking 10 mL of the mixed 1.0 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, a mixed 0.1 pgfrnL 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 of 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 taking 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/mL 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, of Fort Fort
Solution
Volume
(ng/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 of Fortified Sample
(mL)
100 100 . 100 100 100 100 100
Final Cone, of Calibration Std.
(jig/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 2C) when not in use. Documentation o f standard preparation is located in the raw data package associated with this interim report
6 J 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 o f LC/MS/MS Instrument and Operating Conditions Instrument: API 4000 Biomolecular Mass Analyzer
Interface: Turbo Ion Spray Liquid Introduction Interface
Computer DELL OptiPlex GX400
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 Vol.: 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
%A 65 65 25 25 65 65
%B 35 35 75 75 35 35
Flow Rate: 0.3 mL/min
Ions monitored:
Analyte
PFBS PFHS PFOS
M?de
negative negative negative
Tfip$ition Monitored 299-^99 399-)-80 499 -+ 80
Approximate Retention Time
(mini -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 was measured and the standard curve was generated (using 1/x fit weighted 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 ofPFBS, PFHS and PFOS found in ng/mL to ng/g (ppb).
Equation 2:
Analyte found (ppb, wet weight) =
fAftriYte found (ng/mL) x final volume (2 mLM sample weight (5 g)
For samples fortified with known amounts ofPFBS, PFHS and PFOS prior to extraction, Equation 3 was used to calculate the percent recovery.
Equation 3:
Recovery (%) -lanalytc found fag/mL) - analvte in control fag/mT)) x 100% 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 only):
Fish sample Exygen ID: C0049478 1 where:
peak area intercept slope dilution factor
ng/g PFBS added (fort level) amt in corresponding sample final volume (mL) sample weight (g)
tal sample follows (calculation is for PFBS
: E (Set: 061605E), fortified at 10 ng/g with
* 280750 - 3070 - 13100 = 1= 10 = NQ (not quantifiable) -2 =5
From equation 1: Analyte found (ng/mL, wet weight)
- f2807SO - 30701 x 1 13100
From equation 2: Analyte found ng/g (ppb)
- 21.2 ng/mL
= 121.2 ng/mL x 2 ml.^ Sg
= 8.48 ng/g (ppb)
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From quation 3: % Recovery
- (8.48 n g /g - Ong/g) x 100% lOng/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 of fish contained three samples, one set o f fish contained four samples, one set of 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 L 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 11. Analytical results and assessed accuracies for the analysis of PFBS, PFHS and PFOS found in clam samples are summarized in Table ID.
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
Interim Report #10-Analysis of Pish and Gam 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 SAMPLES
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 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen StudyNo.: P0001131
TABLES
Exygen Research
Page 22 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS tn Fish Samples
ExvoenJO
0*8(4 Samla IO
C4 SuHonate P P M
N>6mtmb^amrnmtwtei
Analyte AlM S M d
Found Accuracy fM W m tw t <**>
C6 S ulfonate PFHS
Mhwnhniw<iM
Analyte N ttttS Found Accuracy ante m i at. ( * - )
C SuHonote PFOS
PtOuoroMteiMiaiMte
Analyte A lta n a d Found Accuracy
(*-% >
C004812B
DL3-F01-IPF01-0-041021
0.300
40
ND
30 9.16 30
C0048126 Rap DLS-P014PF001-0-041021*
0.318
40
NO
30 id *
30
C0048127
DL3-P01-IPP002-0-041021
0.28S
40
NO
30
4.16 40
C0046127 Rap DL3-F01-IPF002-0-041021*
0.382
40
NO
30
4.96 40
C004813B
DMC-F01-IPF001-0-041021
0.330
90
NO
50 7.40 50
00046128 RSp DMC-F01-IPF001-0041021*
0.366
50
NO
so 8.3 60
C0048129
DMC-F01-IPF002-0-041021
0.712
30
ND
30
14.1 SO
C004612BRop DMC^014PPO04Mk41O21 * a rm 30 ND 30 17.0 50
C0048130
DMC-F0MPW001-0-O4121
1.08
40
NO
30
70.0 40
C0046130 Rap OMC-F014PW001-0-041021*
1.06
40 0297
30
56.4
40
C0048131
OMC-F01-*N002-0041021
0.068
90
ND
30 34.4 30
C00481S1 Rep DMC-F01-IPW002-0-041021*
1.34
90
ND
30 34.2 30
C0048132
DMC-F01-MSW001-0041021 0.218
30
0.524
30
270
30
C0048132 Rap DMC-F01-M8W001-0041021* 0.202 30 0.484 30 280 30
C00481JJ*
DMC-f01 -M6W002-0041021
ND*
30
ND*
30
530
30
C0O48133R*p* DMC-F01-MSW0020041021* NO*
NO* 30 848 30
C0048134
DC2-F01.IPF001-0041021
0.660
90
f*>
40 3.48 so
00048134 Rap DL2-F01-PF001-0-041021*
1.00
90
NO
40
2.86 50
C0048135
DL2-F01-IPFOQ2-0-041021
0.616
90
NO
40 4.72 50
00048135 Rap DL2*F01-PF002--041021*
oses
50
ND
40
5.04 50
C004S135
DL2-P01-IPP003-0-041Q21
0.247
30
ND
30 2.01
30
C0048138 Rep DL2-F01-PF003-0-041021*
0.218
30
ND
30 2.08 30
C0048137
DL2-F01-IPF004-0441021
0.3*0
40
ND
30
452
40
C0048137Rap DL2-F01-PF004-0-041C21*
0.330
40
NO
30 4.12 40
00048136
0L2-F014PF00S-O041021
0-330
40
ND
30 2.48 30
C004813B Rep DL2-F01-IPF0050-04102r
0.318
40
ND
30 2.90 30
C004813B
DL2-F01-FW 001-0041021
0.328
30
ND
30
5.88
30
co o w ia B R a p L2PF014PW001-0-041021*
0.400
30
ND
30 6.12 30
C0048140
OL2-F01-MSF001-0-041021
0.333
30
ND
30 772
X
C0048140Rp DL2-F01-MSF001-0-041021 * 0.348
30
NO
30 67.6 30
C004B141
DL2-F01-M5F0020-041021
0.408
40
hC
30 94.6 40
C004B141 Rap DU-F01-MSF002-0-041021* 0.308
40
ND
30 06.4 40
C0048142
DC2-F01-M SF0030041021
0.418
40
ND
40 41.6 40
C0048142 Rap DL2-F01-MSF0000041021*
0.378
40
ND
40 40.0 40
C0046143
OL2-F01-MSF004-0041C21
0.343
30
ND
30 83.6
30
C0048143 Rap DC2-F01-MSF004-0-041021' 0.349
30
ND
30 832
30
TjtnM oiy OupUcMi * 1.0 g af M irft* u n d fcr m e d ia n tom ad ofao g. NO Not datadas) I or oowb Urn* o f Quantitation * * * Is a 2 n g (wetwelgM) NO* Not detected at or above U m l o<Quantitation which a 1.0rl9<w tw eltt).
NR Not reportad du kxaiaKy conM ra m iM u m .
Exygen Research
Page 23 of 132
Intrim Report #10-Analysia of Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS in Fish Samples (continued)
Exyoan ID
Ctiant Samoa ID
C046144 C0048144 Rap
DL1-F014PF001-&041021 CK.1-F0l-FR)01-ftC41021*
C04814S C0048145 Rp
DL*F1)1-IPFOOM-O4t021 OL3-F014PF0034HM1021*
00046148 C0048148 Rap
OL3-F014PF004-0041021 0U -F 01.IP F 0 44H H 1021*
C0048147 C0048147 Rap
O LS^014PFO O S4M M ioe i DLS^OI 4PF0OS4M41O21 *
C0048148 00049148 Rep
OBC^014PF0014V041021 D8C-F014PF0014M41021*
C0048148 00048140 Rap
C0048160 C0048190 Rap
0BOF01-IPF002-0-041021 OBC-F014PF0024W)41021*
M O F014PF00W W 41021 O0C-FO14PFOO3-M41O21*
C0048151 C0048151 Rp
080F01^W 0014W 41021 DSC^CHPW 0014Mm021`
C00481S2 C0048152 Rap
DBC4=01-PW002<MM1021 06OF0HPW 0024M41021*
C00481S3 00048183 Rap
0604=014PW00S4W141021 0 8 0 4 0 1 -lPWOOO<W)4102r
C0048154 C0048184 Rap
DOU-FC1JPF001-04)41021 DOU-F014PF001-0-04MJ21*
00048156 C00481SSftap
OOU4014PF0024K>41021 OOU-FOl-iPF0024H>41021*
00048158 C00481G6 Rap
C0048157 C0048157 Rap
DOU-F014PF00340041021 DOU-F014PHK<MMHH1*
DOU-F0HPF004-O4341021 OOUPQ14PP0044M41021*
C0O46158 C0048158Rap
D O U4014PF0084W 41021 DOU-F014PF008-04)41021*
C0048150 C0048158 Rap
DOOFOI-IPWO01*0-041021 000-F01-IPW 001-0-04102r
00048100 C0048180 Rap
D0U-F014PW002-0-041021 D O U -H>1.IPW 002-0-04102r
C0048181 C0048161Rap
C0048182 C0048182 Rap
OL2-HM-MSW0O1-O-O41M1 (X2-P01-MSW 001-04M102r
OL2-F01-MSW002-04)41021 D L2-F0144SW 0024M 41021 *
C4 SuNwm PFBS
Analyte Found
4 n a ia a d Accuracy
(**-
0.432 0.428
0.448 0.440
0.784 0.000
1.63 1.07
1.34 1.38
1.43 0.786
0.608 0.082
0.864 0.808
0.700 0.736
0.738 0.780
4.36 4.24
878 398
588 606
612 028
4 58 4.36
2.89 2.81
18.4 19.3
0203 ND
NO NO
30 30
30 30
40 40
60 60
SO 50
50 50
50 50
40 40
40 40
30 30
40 40
C 40
40 40
30 30
30 30
30 30
53 50
30 30
30 30
C eSutfonataPFHS
Anaiyto Found
Aaaaaaad Accuracy
(*-% )
0.201 C.2S2
NO 0.229
NO ND
NO NO
0.602 0.580
NO ND
0-644 0.824
2.21 220
0.12 698
6.76 744
1.02 0.972
0.702 0 .7
1.02 1.02
2.30 2.38
0.096 C.3S2
0.948 0964
3.99 3.70
NO NO
ND 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
CS S ulfonate PPOS
Anaiyto Aaaaaaad Found Accuracy
Ml 32.0
3-59 3.36
0362 0930
946 6.64
N ft NR
110 109
NR NR
NR NR
NO NR
NR NR
NR NR
NR NR
NR NR
NR NR hfB NR
N8 NR
NR NR
120
100
40 30 30
30
40
NR
30 NR NR
NR
NR
NR
NR
NR
NR NR NR
NR
NR
NR
50
30
l a boratory Pt ir an
NO * Nc< detected al or abova U nit ofQuantitation which b 0.2 ng/g(wot weight). NR Not raponad du* to quNRyoonM raw * triton*.
Exygen Research
Page 24 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued)
ExvoanD
Clan SandaD
C 4 u lto n a liP F M
Nrfl--wuta--Pawn
A naya A n t ad Found Aoouraoy
moMwaat <*%)
C ( Suffanata FFMS
NrWmOTh----uUbwl
Analyla A M ttM d
Found Accuracy
Out m i w
(*-% )
C8 Oudonala PF09
FwfccwwawMfciiai
Anaya Found
Aaaaatad Aocuracy
MOM)M l M- <**>
C0048163 C0046163 Rap
C0048164 C0048164Rap
C0048165 C004S1WRap
G004MS0 C004O4S0 Rap
00049451 C0040451Rap
000494 00049452 Rap
C0049453 CQ049453Rap
0004949* C0049454 Rap
00049499 C004945S Rap
0 0 0 *9 4 CQ0494Rap
COO*9*67 C00494S7 Rap
000494 000494 Rap
000494 000494 Rap
C0049480 000494 Rap
00049*81 C0049491 Rap
C0049462 C0049492 Rap
000*9483 000*9*83 Rap
C0049484 00049484 Rap
000*9489 0 0 0494 Rap
DL2-F01-MSW00344M1021 D L2-F01-N B 1N 001004102I*
DL2-F01445W004-0-041021 O L2-F01-M SW 004-0041021*
DL2-F01-MSW006-0-041021 DI2-F01-M5W009-0-041021 *
OaC-FOI-MSWOOI-0441104 DBC-F01-MSWQ01-0-041104*
MC-F01-MSW0024MI4 10* OBC-F01446W 002-04W 110*'
OBC-F014RW 0034MH1104 DBC-F01-M8W003-0-041104*
D6C-F01-MSW004-0-041104 DBC-F01-MSW0044MM1104*
0SOF01-MSW00S4MM1104 DBC-F01-M8W009-0-041104*
06C-F01-M8F001-0-0*1104 DBC-F01-MSF001-0-041104*
QR&FO 1-MSF002-04M1104 06C-F01-M SKW 2-0-041104*
D 6C - l1 *P F 0 0 4 -0 -0 *1 104 D B C -F01-FF0044M 41104*
D6C-F014PF006-0-041104 D B C -F01-P F0094M 41104*
06C-F01-PW 004-0-041104 D8C-FOWPW0 0 *0 0 *1 1 0 *"
D BC -F014P W 0060041104 D 6C-F0HPW 005-0-O 41104*
DOU-HJ1-4PW03-0O4110* K5U-F01-PW 003-0041104*
DOO-FOI-PW 004-0-041104 DOU-F01-IPW004-0-041104*
D00-F01-PW006-0-O*110 DO U-F01-PW 0050-041104*
D L2-F01-PW 002-0-041104 DL2-F01-IPW002-0-041104*
DL1-F01-M8W001-0-0*1104 OL1-F01-M8W1-0-041104*
NO NO
NO NO
NO NO
oa 0.492
0-988 0.88*
00 0.784
0884 0.880
0.832 0-832
0.820 a 788
0.788 0 .7
0.504 0.520
1jM 1.84
0.484 , D.444
0.572 0.532
3.12 .3
3.4 3.11
2.97 2.90
1.04 0.960
1.20 124
30 NO 30 9Z4 U NO 91.8
30 NO 30 M .0 30 NO 30 94.8
30 NO 30 1 NO 30 174
30 8.32 30 . . 8.32
30 30
NR NR
30 3.43 30
NR
80
3.39
30 .
NR
30 582 30 NR 30 164 30 NR
30 9.72 30
30 9
30
NR NR
30 Z77 30 . 2.66
30 30
NR NR
30 1
30 NR
30 148 X
NR
30 1.94 30 .1 .9 0
X X
NR NR
30
0.584 ,
X
30 0.54Q X
142 152
30 2.16 X , NR
30 Z16 X
NR
30 128
X
30 128 , 30 .
30 . 210 30 2.10
X X
NR NR
NR NR
6.00 X
30 992
X
NR NR
30 7.12 X 30 8.84 X
NR NR
30 9.12 X 30 5,32 X
NR NR
30 NO X 82 0 30 NO X 8 .
30 0.596 X 30 0-932 X
NR NR
X X
X X
X X
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
X X
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
40 40
NR NR
` Lanoraaxy D u p in * NO N oldalaclad a lo ra b e ra Um*o< Quandtaiton vrftich 0 .2 ng/p (vrat sight). NR Not iapoi*d du* 10QiiMfy Oman* mmM Mura*.
Exygen Research
Page 2S of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued)
ExvoanlO
C le n t 8amd* IO
COO4S408
DL1-F01-MSW002-0-041104
C0048486 Rap DL1-f014SW <2-O54t104*
C0040487
OL1-F0144SW003-OO41104
C0049487 Rap OL1-F01-MSW0030-341104*
C0049488 C0040468 Rap
OL1-TO1-MSW004-0041104 D L1-F0144SW 004-0041104*
C0049489 cao4BaaRap
DL1-F01-MSW008-0-041104 DL1-F01-MSVW003-0-041104*
C0040470 C004S70Rap
DL1 -F01-MSF001-0-041104 DL1-F01-MSF001-0-041104*
C0049471 C0049471 R ail
0L1-F01-MSF002-0-041104 DU-F01-MSFOQ2-0-041104*
C0049472 00044472 Rap
0L1-F01-M SF00304M 1104 OL1-F01-MSTO34W 41104*
C0049473 C0O49473 Nap
DL1-F0144S7004-0-041104 OL1-RM-M8F004-0-041104*
C0040474 C0049474 Rap
OL1-FC1-MSF0060-041104 0L1-F0144SFOOWWM1104*
0004*475 C0049475 Rap
OL1-F014PW001-0-041104 DL1-F014PW001-0-041104*
00040478 C0O49478 Rap
0004*477 0004*477 Rap
D L1-F014P W 002-0041104 OL1-RH4PWOOMMM1104*
D L1-F01-PW 003-0-041104 L1-F01-IPW003-0-041104*
0004*478 0004*478 Rap
0004*47* 0004*47# Rap
OL1-F014PW 004C041104 D L1-FO HPW 004-0-041104*
D U -F01-1PF002-0-041104 DL1-F01-1P7002-0-041104*
C0049480 C0049480Rap
C004S481 00049481 Rap
OL-1-FDHPf003-0-041104 DL-1-F01-IPFO0M-O4I14*
DL-1-F01.im )04-0-041104 X.-1-F01-tPR4-04>41104*
0004*462 C0O49482Rap
DL-1-F01-IPRXS-0-041104 tX-1-7Q1-tPF005-0-041104-
C0044483 0004*483 Rap
00049464 00040484 Rap
DL3-701-4ISW01-0-041103 DL3-F01-M6W001-0-041105*
DL3-F01-MSW002-0-04110S D t3-701-MSW002-C-041103*
C 4> ulf0 aate l> F U
Analyte Found
Aaaaaaed Accuracy
(4-1
1.30 1.15
0.580 0.528
1.22 1.12
1.22 1.20
ND NO
NO NO
0.203 NO
NO NO
NO NO
0.772 0570
0.468 0.472
ND NO
NO NO
NO NO
NO NO
NO ND
NO NO
NO ND
ND NO
30 30
30 30
30 30
30 ac
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
C aS itfQ M M P F H *
ftte lyto Found
Aaaea--d Accuracy
<*/%)
1.72 154
1.13 1.14
0.908 0.880
1.16 1.16
0.315 0 2*9
0.024 0.804
0.832 OjSTO
0532 0536
0584 0.844
0.568 0.744
0530 0516
0-209 0-247
0-238 0248
0*222 0.247
0565 0262
ND NO
0573 0588
NO 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
*1uUntmyDuplcuti
NO Not dalacted at or abova limit of QuanttaOoriwftlctt la 0.2 ng/(j (mat weight). NR - Not portad du* to quality cortrd vmuI Mums.
CM Sulfonate PFOS
Analyte Aaaaaaad Found Accuracy
NR NR
NR NR
161 188
NR NR
293 307
NR NR
NR NR
NR NR
NR NR
17.4 18.9
13.7 15.6
56 9.52
50.6 57.2
11.1 11.2
20* 21.4
7.80 7.38
8.72 8.58
138 137
160 162
NR NR
NR NR
30 30
NR NR
30 30
NR NR
NR NR
NR NR
NR NR
30 30
30 X
30 30
30 X
90 30
X X
X X
X X
30 30
30 30
Exygen Research
Page 26 of 132
Interim Report #10*Anslysis-ofFish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued)
C48u4fMataPFB8
____ S h s J 2 _
C line 8 a m p iilD
Analyla
Found Accuracy fnafelw*wt W-%)
00049485 G0040486 Rap
0.3-701-MSW 003-0041105 DL3-F01-MSW0OSC-04110S*
CC049488 C004S466 Rap
C0049487 00044487 Rap
DL3-F01-M8W004-0-041106 DL3-F01-MSWC044WM1105*
OL3-FO1-A43WOO5-O-04 f 106 DL3-W1-MSWC06-0-041106*
C0048488 C0044488 Rap
C0044488 00044484 Rap
DL3-F01-M8F001-4HH1106 DLS-F01-44SF001-0041106*
DL3-H)1-MS7002-(H)41106 DL3-701-*487002-0041105*
00044490 00044440 Rap
DL3-F01-M3FC03-0-041106 OL34KM-MSF003-0041106*
00044401 C0044401 Rap
D U -F01-M 87004-0-041106 DL3-F01-*487004-0041106*
C0049492 00044492 Rap
OL3-F0144S700S4-041106 OL3-F01-MSF0064M41106*
C0049493 C0044493Rap
OMC-F01-IPW0084MH1106 DMC-F01-4PW003-0-041109*
00049494
0*40-7014PW 004-0041106
00049404 Rap 0*40701 -4PW004-0-041109*
0004949$ C004949SRap
OMC-F01-IPW0064MM1105 DMC-F01-1PW006-0-041106*
C0049490
OMC-F01-MSW003-0-041106
00049496 Rap D*4C-F01448W003-0-041106*
C0049497 C0049497 Rap
C0049496 C0049498Rap
0*4OF01-44SW004-0041106 DM C -F01448W 004-0041105*
OMOFOI-M 8W 0060041106 M4C-F914MSW005-0-041106*
C0049499
DMC-F01-M6F002-0041108
00049449 Rap OMC-F01-MSF002-0-041106*
00040800
OMC-F0144SF0034KW1106
C0049600Rap 0MOF01-MSFQ0S4O41106*
00049901
OMC-F01-MSF004-0041106
C0049S01 Rap 0*4C -f01-*4S7004004f 105*
C00496Q2
DMC-70144SF005-0041106
C0049S02 Rap D*4C-f01-*48F006-0-041105*
C00499O3 C0049603 Rap
DMC-F014PP0034V041109 O M C -701-IP F0060041109*
NO NO
NO NO
NO NO
NO NO
NO NO
NO NO
NO NO
NO NO
NO ND
0.800 0.346
ND NO
ND ND
0.318 0.233
ND ND
ND NO
ND NO
NO ND
NO ND
NO ND
30 X
X X
X X
X X
30 30
X X
X X
X X
X X
X X
X X
30 30
X X
30 30
X X
30 30
X X
30 30
X X
Ct SuKonata PFKS
Analyla . Found
AMMMd Accuracy
(*-%>
NO ND
0.286 0282
0.368 0.341
ND ND
ND ND
ND NO
NO NO
ND ND
0268 0.334
0X0 0.484
0270 C2S9
0X2 0.560
1.90 1.88
0X0 0.036
NO 0 .X 7
NO NO
0254 0228
0.420 0.448
ND ND
X X
X X
X X
30 30
30 30
X X
X X
X X
X X
X X
X X
X 30
X X
X X
X X
X X
X X
X X
30 30
CtSuifoiurt PFOS
Analyla Found
Aaaeaaed Accuracy
140 144
198 100
173 IX
no 115
116 111
75.0 72.0
1X 134
81.0 83.8
812 63.0
688 698
844 62.8
354 3X
254 269
NR NR
NR NR
56.8 S6.C
110 110
148 147
7.92 7.92
X X
X X
X X
X X
X X
X X
X X
X X
X X
X X
X X
X X
X X
NR NR
NR NR
40 40
30 30
X X
X X
Not datacted at or atova Urn o l Q uantalo r vWchia 0.2 np/g (wat wrtghtv * Notmpcme tom to quaMy comm nuua M u m .
list
Exygen Research
Page 27 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: POOOI131
Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued)
Jjxjgen_rO_
dam
Sample O
C4 tu tfo a tta P F n
Found . ttlS L .
------ i
Accuracy (4-H i
0 SuOonata PFHS NtiNawihmm n O a a Anatyla Aaaaaaad Pound Accuracy
<N->
C0048804 C0049904 Rap
DMC-F01-IPF004-0-041105 DMC-P01-1PF004-0-041106`
C004060S C004BS06 Rep
OMC-F014PF0064M41109 D M C -F 01-IP F 0060-04t105'
C0058354 coosojsaR ap
0L2-F01-M8F0054KM1216 DL2-F01-A4SF006-0-041216*
C0066456 G0099498 Rap
C0088498 C0068466 Rap
C00S6457 00090497 Rap
Dt2-F014PW0064)-041216 0L2^01-BW 0094>941215*
* DL2-F01-IPW0044)-041215 O L24R H 4PW 004-M 41219*
C0069458
CXXJ-F01-MSWOC3-0-041216
C009949BRap
00099490 C00S645QRap
D L8FO HPW 0044W M 11X DL3-F31-IPW004-WM1130*
C0056490
OOU-F01-M6W0C1-0-041210
C0099460 Rap D04I-F0144SW001-0-041215*
00099491
OOU-F01-MSW004-CM>41219
C0099491 Rap DCHJ-F01-MSW004-0-041219*
C0059462
DOU-F01-M8W00S-O041216
C0090492 Rap DOU-F01-MSW006-0-041210'
C0066493
OOU-F01-04SF0004MJ41219
00090493 Rap OOU-F01-M8F00MWM1216`
00096484 00090494 Rap
DL3-F01-IPW002-0-041130 DL3-F01-IPW002-0-041130*
C0096465 00090409 Rap
DL3-F0<-IPW003-0-O41130 DL3-F01-IPW00J-0-041130*
C0090406 C0056486Rap
C0090497 COO50497 Rap
OOU-F01-MSF0034-0412I6 OOU-F01-M8F003-0-041219*
O0C-FO1-MSFOO5-1-O41216 O B C -ni-M S nM )S -1-041216*
00090499 C0099400 Rap
00090490 C0099469 Rap
C0090470 00099470 Rap
OBC-FO1-MSF0OMMJ41210 DBC-F01-fcl8F006-04>41216*
OOU-P01-M8F002-8O41218 OOU-F01-MSF002-0041216*
DL3-F01-IPW001-0-041130 OL3-F01-IPW0014V041 30*
NO NO
NO NO
NO HD
NO NO
0.206 0.227
NO NO
NO NO
NO ND
798 T.12
4.72 499
0.304 0.36
1.41 1.43
NO ND
ND ND
1.72 1.73
0.220 ND
NO ND
0.899 0972
NO ND
30 ND 30 ND
30 ND X ND
30 ND 30 ND
30 ND 30 ND
40 1.72 40 1.70
30 ND 30 ND
30 10.4 30 109
30 NO X ND
X 13.4 X 14.2
40 21.7 40 22.5
X 1.34 X 1.41
X 8.40 X 3.44
X NO X NO
X NO X NO
X 8.99 X 1 8.88
X 1.7 X 1.78
X 1.98 X 1.5
X 4 .X X 4.56
X 0.248 X 0.210
X X
X X
X X
X X
X X
X 30
X X
X X
X X
X X
X X
30 30
X X
X X
X X
X X
X X
X X
X X
COCuHonataPFOS
Anayta Aamaaed P ^jnd Accuracy
44.0 499
49.4 469
409 519
13.2 133
NR NR
6.80 690
NR NR
7 82 7.52
NR NR
NR NR
NR NR
NR NR
120 118
6.44 5-28
NR NR
NR NR
NR NR
NR NR
.04 8.80
X X
X X
X X
X X
NR NR
X X
NR NR
X X
NR NR
NR NR
NR NR
NR NR
X
X X
NR NR
NR NR
NR NR
NR NR
X X
"1-aPoraaxy Dup4ea
NO - Not deleted at or abovaUmft of Quanltaion 4lcM*0.2 nota (wetwaiohtV NR * Nol raported dua to quA y central laauk M im a.
Exygen Research
Page 28 of 132
Interim Report #10-Analysis of Fish and Gam Samples
Exygen Study No.: P0001131
Table I. Summary ofPFBS, PFHS and PFOS in Fish Samples (continued)
- Exyaw"
C0056471 COOSM71 Rap
00096472 C0066472 Rap
C0096473 C0056473 Rap
C0096474 C0066474 Rap
C0096475 C009647S Rap
C00S647S COO56478 Rap
C0096477 C0059477 Rap
C0066478 C0036478Rap
C0096479 C0056479Rap
C aart _______ Sampte P
DOU4HM-U8F002-1441216 DOU-F01-MSFOO2-1-O41218'
DOU-F01-M6F004-0-041218 DOU-F01-MSF004-0-041216*
DOU-F01-MSF001-0041218 DOU-RJ1-MSF001-0-041218*
D6C-F0144SF009-0041216 OBC-FO1-MSFO0M-O41216"
DBC-F01-MSF0040041216 OBC-F01-MSF004-0-041216*
DMC-F01-MSF001-0041216 DMC-F01-MSF001-0-041216"
D L1-F01-IPW 006-0041216 OL1-F01-IPW005-0-041216*
CX^F01HPW0034>041201 DL2-R01-)PW003-0-04f201*
DOF0HFW 0050041201 OU-POHPW 0060041201
C4 Sutfoaate PfM
Found
*w ia d Accuracy
(/- %\
0.640 0.860
0.782 0.816
Z18 138
NO NO
ND ND
NO NO
0.253 0 .2 X
NO NO
ND NO
30 30
30 30
30 30
X X
X X
X X
X X
X X
X X
C6 SuHonat* PFMS
- - - - 1 i 111i j i i n
Analyte Found
Aaaaaaad Accuracy
<*-% !
4.68 4.72
2 .X 2.22
10.0 10.7
ZOO 2.00
187 177
0420 0 .4
0644 0 644
NO NO
ND NO
X X
X X
30 X
X 30
X X
X X
X X
X X
X X
C tftu tfo M t* PFOS
Analyte Found
Aaaaaaad Accuracy
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
88.8 67.8
7 .X 7 .X
4.88 4.72
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
X X
X X
X X
l aboratory PupUcMa
NO - NotdatacladalorabovaUmlt ofOuanlltatkMiw**ii i*o.2 note (^watotni.
NR Wot wportad to quaRy a w maut b tu n i.
Exygen Research
Page 29 of 132
Interim Report #10-Analysis of Fish and Gam Samples
Exygen Study No.: P0001131
Table II. Summary of PFOS in Re-extracted Fish Samples
Ex v q m ID C0048151 C0048152 C0048153 CQ048154 C0048155 C0048158 C0046180 C0049450 C0049451 C0049452 C0049433 C0049454 C0049455 C0049456 C0040458 C0049459 C0049460 C0049461 C0049462 C0049463 C004946S C0049466 C0049467 C0049469 C0049471 C0049472
C te o t Sam otalO D8C-F01-IPW 001-04)41021 DBC-FO I-IPW 002-0-041021 D 8C -F01-IPW 0034-041021 D O U -F 0l-IP F0G 1-O 'O 41021 O O U -F 0H P F0Q 2-0-041021 D O U -F 01-IP F 005-C -041021 D O U-F01-IPW 002-0041021 DBC-F01-MSW G01-0-04110 0BC-F01-M SW Q G 2-Q -Q 4110 DBG -F01-M 3W 003-0-04110 D BC -F01-M 5W 9040-041104 DBC-F01-M SW 0054F04110 D B C -F01-M S F001-0- 4110 OBC-FQ1-MS-O02-0-CVH10 OBC-F014 PF006-0-04110 DB&F01-4PW 004-0-G41104 DBC-FQ1-PW 006-9-041134 IXXJ-F014PW G03-0-041104 DO U -F014PW 04~!>041104 DOU-F01 -IPW CO^O-04110* DL1-F01-M SW C01-0441104 DL1-F01-MSWGC2-CWA1104 D L1-F01-USW 003-0-041104 DL1-F01-M SW 005-0-041104 OL1-F01-M SF002-0041104 DL1-F01-M SF003-0-041104
N R * Not itp o n ttf due la quality controlretuK foflums
Exygen Research
C S u lfo n a te PFOS
frWuo>o<rtin n ilfiM ti
A n a tjte Found (ngfe)W W W t
A asew ed A ccuracy <+-%)
2080 3330 1680 506 636 S44 1210 9480 7520 12600 3440
30 30 50 30 30 30 40 40 30 30 30
5240 5240 4760 60S 1230
30 30 30 30 40
2620 HR 1740 2130 068 708 696 604 568 432
30 NR 30 30 30 30 30 30 30 30
Page 30 of 132
Interim Report #10-AnalyBs of Fish and Gam Samples
Exygen Study No.: P0001131
Table II. Summary of PFOS in Re-extracted Fish Samples (continued)
Exyuan 10 C0049474 C0049496 C0049499 C00564S6 00058458 C0056480 C0056461 C0056462 CO056463 C00S8486 C00S6487 C0056488 C0056489 00056471 C0056472 COO56473 C0056474 C0056475 C0056476 C0048148 C0048150 C0048156 C0048157 C0048159 C0049473
COant Sam la ID DL1-F01-M SF005-0-041104 DM C-F01-M SW 005-0-041105 D M C -F 01-M S F002-0-0411Q 5 D O U -F01-M SV Y 002-0-041216 DOU-F01-MSW 003-<M)41216 DO U -F01-M 8W 001-0-041216 DOU-FOI-M SW 004-0-041216 DO U-F01-M SW 005-0-041216 D 0U -F01-M SF005-O 041216 DOU-F01-M SF003-0-041216 DSC-F01-M SF005-1-041216 DBC-F01-M SF00M W H 1216 DOU-F01-M SF002-0-041216 OOU-F01-M SF002-1-041218 DOU-F01-M SF004-0-041218 DOU-F01-M SF001-0-041216 ; DBC-F01-M SF003-0-041218 D8C-FO1-MSFOO4-O-O41210 D M C -F 01-M S F 001-0-041216 D B C -F 0 1 -IP F 0 0 1 -0-041 021 O B C -F 0 14P F 0 03-0-0 4102 1 D O U -F 01-IP F 003-0-041021 D O U -F 014P F 004-0-041021 DOU-F01-F*W 001-0041021 OL1-F01-M SF004-0-041104
NR Not raportM due to qualty control m u lt U k n a .
C S S u tfooa taP F O S
A nalyta Found
A a a a a a a tf
740 580 620 28200 4040 NR 5120 496 720 848 NR 8960 640 692 1620 2070 4640 9280 840 384 293 359 424 387 348
30 30 30 60 30 NR 30 30 30 30 NR 50 30 30 30 30 30 50 30 30 30 30 30 30 30
Exygen Research
Page 3 1 of 132
Interim Report #1G-Analysis of Fish and G am Samples
Exygen Study No.: P0001131
Table III. Summary of PFBS, PFHS and PFOS in Clam Samples
ExuoantO
dam Sam otolD
C4 S ulfonate PFBS Putuanatew-- aaiil
Analyte Awaaaad Found Accuracy (notaint 4 <*/-%>
C t S ulfonate PFHS Pnrtitcr n h r r w itlnwi
Analyte Aataaaad Found Accuracy M a t m t vt. < *'-*>
C8 S ulfonate PFOS temuoroartui--uMtt--u
Analyte A w aaiad Found Accuracy (notaint 4 (M M
00066480 0L3-I01-CFW 001-0-041218
NO
40
ND
40
1.82 SO
C0096480 Rap OLM01-CFW 001-0041216*
NO
40
NO
40
1.82 50
C00S6481 DMCH01-CFW001 0041218
NO
30
ND
30 6.16 50
00066481 Rap 0M C 401-C P W 001O 0412ir
NO
30
NO
30 6.12 50
C0066462 D LM 01-C FW 0010041216
NO
30
ND
30
1.81
50
C0096482 Rap 0LM 01-0FW 00tO 041216*
NO
30
NO
30
1.77 50
C0096483 o e c -w i-C F W o o io < m 2 is
ND
30
NO
30 4.48 30
C00S6483 Rap D8C401-CPW 0010041215*
NO
30
ND
30 4.44 30
C0066484 CH.1-I01-CFW0010041219
NO
30
ND
30
8.80 40
C0036464RSP DL1-I01-CFW 0010041219*
NO
30
NO
30 8.84 40
COOS6485 0OU-W1-CFW0010041216 00066489 Rap DOU-M1-CFW 0010041216*
NO NO
30 0.202 30 30 0.205 30
11.4 SO 10.9 50
laboratory P i* * * NO N otdatettad at Of abova Uro> o f Quanttation w tiich I 0.2 n g fr (wet waight).
Exygen Research
Page 32 of 132
Interim Report ^10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples
M P PopaMon
DC3^014FTOH*0-O*1ft21 to o o io m M C
DLWH)14W)01^0*^<C1 *000*0901*' . m tm
Oi3-FOHPPOCH4KN12l (Coinz7SffeD. tapp)
DU-FOl<m 02^01<01
IC-H M -*>W 1-0041021 {GSMOIM * .* *
0MC*fHPF001-0O410ai |C D 0*O lM 100M )
DMC-m*IPF002^0410S1 <cooam*fcc. fmm
OUC-f51-*fMB-<W41021 o u o m h , mo gm
D M & fO I-tf'W W I-tHM KQI 1000*01 Opa0.101001
DMC-fOI-^WQOI-OOOKSl fOBttUOMl. Ipp
DMC-fOl.O^VOQ2->M1021 looomii o>oi. toiooi
DMC-FOI-iPWW-CMMKtt fCootipai.tooat
0M D*0M ISW -0*4tC21 {000*01* 0 8.10OPOM>
DMOfOl-KSW0-0<(Ml021 <00*091 M ' 1 *N *M o )
DMC-F01MSWOQ2^XMK)21* 1000*09) f l , 00M *0)
DMC-F01-NSWO2-0-04W21* <000*090OM.MOo M
DL2-FQ1-OTOD1-0-041G21 (0M*03* Opfert9 PPOM*> DL2^01-IPF001-0-041(S1 <omofm m * ioom m m
O L*m 4m & O 441021 {03099* M O . 10*000) OL2-f91HPFOQ2*<MlOtf <000*01*M L < M
AirounJ SpMd
C4a m nH PFM Ait* Found Amount In M ap fllOOMOfOd Nowory
{ M IM (1
O S S '** PfHS
C *B Jton$*9fO *
AM Fwnd Amowd
"XmTogrtd" A m M
In la * H w d iid Racovay msofflp NoaoiioroJ NdCduay
n*l-- - t___ 1
< n o -** <%>
10 0JM
4M
S3
ND
1.24 3
41
124 74
100 0.30
02.4
02
ND 742 73 5.1
74
7
10 0J05 100 0.206
432 006
03 a
ND 740 75 4.16 NO 704 00 4 *
10.3 1 MO 77
10 0.330 4.40 42 ND 534 52 740 9.99 2 100 0.330 004 00 NO 744 75 7.40 svo 74
10 0.712 740 70 100 0.712 740 77
ND 4 M ND osa M
14.1 14.1
10 1.00 7
86
100 140
044 4
ND 7 04 78 ND 0 K
700 700
10 0406 074 100 O.OOQ 004
a a
NO 745
344
NO 744 76 44
10 0210
470
m
0.924
444
8
100 0218 12 i 0424 2
93
270 270
so ND*
452
90
NO-
52JO
104
30
900 wo- 432 a
ND* 492 0 $30
10 0400 8 00 51 100 0400 444 a
NO a M 346 ND 684 9 X43
204 196 104 SO 714 . 131 1
444 ,
101 07
270 .
375 106
470 %
924 79
.a 49 56.4 53
10 041 404 49 NO 40 M 4.72 8 . a
100 041
44
M
ND 784 ? 4.72 72-4 ss
tT iiinHii 0>iipMnpludiynMWrwotwo.awro--nmoawjniaiawialbnahm
M O gdiiw fH wn0fcr0w
NP NotM m m at orabove Um ofOuarfloaM tookis 02 ng (mlwoM*).
NNfOt*WotNioogotNrt4fr4taudotlooOrai>bmoyvotUWnNmtotiQUyrunIritl.DQwanwWuMtlif*cw10JntmEwMosthvoww<nBnhTQ.l.
Nota: tu a O -- mmy M N w mon w te,
M a a wqj n r> -- Ml 1mm 0 M -- h ln n a M n.
Exygen Research
Page 33 o f 132
Interim Report #IO-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
OL2-R)1-<PFOCB-O44ia21
(oaM iM txcK ntV M
OLM w-rpooo<ta2i < m u a t *<. no a * m i
C2-f1-*>c+<K>41021
cnM urananpM N w )
0U-F91->F04444I021
C o tu .v aK L rat M M
D U -F o i-jp w o s^W UKd i 0MMUI M (. H t M M
ou-F0i-wmM44i<Bi
CCM 4M M .J.iakM
DL2^014W00104taZ1
k sim ijim f. io m M OUFO1.VW001 0*1421
ic a u a m ii. m ***>
o u w + is w o i-<m iio * i
01FOIWSFM1-O44ia21
K * m u t m i, im m m m
o u * o i-m s f n * o 4 i <8i (ooiaut ipt c. B n * M
UMi-MaFOK-044102
(COOWMt M . IWk* M M
DU-KVMaF00441K1
(COM IUM O.IIM M M
0U-FA14MFMV0441031
W M M tM l. MOM 1 * 4
[xFouaF ow -< M M ian lc M u > M i.'ii* tM DL2-FOVSFO>MWM1D21 (Cw m i **.). w )* e M t
<CW M U4M F.M M
OLl-fOUPF001^04toei
(OntMtt SM1CMl K* M >)
OU-FOI>l>Fa<Hia2i
(COMM n k a M M . )
IDCLMVMF<1MMM^Ptf,KM(KlKMMnI<*ni
* * * <d
nS^p*
Amt Found Amount
Aiut Found
O am ui# Rm n o r *9npi OioM ivd Raoowr 1 NSnm0o
JS O L2L___ S L -
NiaNiwUut
Amount
ta n s
10 034T
too 3347
10 0340 0 0340 10 0439 100 0339 10 03M 100 0320
10 0333 100 0333 10 0.400 100 CA08 10 0410 100 0410 10 QMS 100 0340 10 0.432
too 0432
10 0449
M0 0440
7.00 624 6.94 07.6
4 6 694 744 80.0 73 4 6
049 14 42 44 7,00 714 7.44 73
730
002
96 NO 3 NO
6 NO
7 NO
6 NO
09 NO
7 NO
0 NO
70 NO 64 in
6 NO
61 NO
1 NO
4 NO
07 NO 71 NO
70 0391 67 0381
6 m
60 NO
746 733
740 764 746 0 4 7.00 773
630 774
749 664 6.76 704 7.90 913
8.1
78.4
846 614
m 73
76 77
77 91 TO 77 62 70
75 06
66
71 7 79 ni
61 82
241
201
4.52 442 2.40 2.46 340 546
772 772
S4.6 044 414 414 634 834 334 334
346 i
630 72 740 73
113 66
60.4 76
046 72
20 60
134 90 653 7 760 . 166 91
Ml 196
413 104
13 167 400 106.0
. 61 *
02
* 83 73
104 73 0.0 78
NO NotMnMMarikMUnMiti __ _:*heFi*r%* imwm now ului cannot atol
Exygen Research
Page 34 of 132
Interim Report #10-Analysis of Fish and Gam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
. anvn
A/nounl AMF o rt 4mowi
MMFount AneuM
MMPound Amount
ap M biOanp* RaooaKotf PlSMfy 'in3AFio Weoid A ataiy feSan** Aooowed INeowry
/natal lmfctacL <jmp * t%l MM talta
Ot3*F01*m04^HMl021 (COMIWMO. 10fp6paa)
10 0.7*4 J4
1
DL3^O1HPF0O*HHHUOl p s m tu * pt ft *8Bibas*e)
100 0.7*4
66.0
06
NO \ NO
1016 . 106 0482 ..
t. 66.4 -66 . . 0.362.
8.96 614
0OF01'*F00ft-644rt21 <ceom47**D 10aM m)
10 1.53 & M
30 NO . 9.16
82
a.
117
96 61 62
G M tM l ip* u m 00M a)
100
DBC-f01*#H1-4041021 4O0Mtwep*x * * * *
DVOFOI-mOHMMlOZI tewMwaapej , n o p m
10 100
doc-fm -ffooxo-cmiozi eoaano m * m **>
D6C-F014PFW2-0441021 <ceMtt4t%ptK.teapMd*)
10 100
o e c-ro i-# ro i* o * io 2i tcoostMOHka, dpaspto
DeC4M)1^P0OS^O41021 to m m Mm t . no***!
10 100
oec-Fo-wpwcoi-tMMioei tosi0i tpke. amaMn)
oec^om pw ooi^4ioei teoBteiMo* h. m p + m *
10 100
OeC^UPWOO&tMMlCBI <caueiexa*D ,ff*% e.)
06C^OMPW<M4MM1Q21 <Cie3a 1.10***)
10 > 100
Dac-Foi-*wooxfr04i 1 (c a u ra . * pp***}
ooc-n>i-rw ooooiiozi iceetam j. Kappap*>
~w 100
OOU*01*1s0014KiaZ1 (OOMM64%kf , 16ppdSpaa)
DOU*F0Hm1-CKJ41O2l (DI0I6W ipkK.WeaMpia)
10 ' 100
DOO-R)MPFQ03stM41Q21 icaawea o. 1#pea|pae)
ooow pw -fr04io2i iQ pannfpauiaippM pM
10 100
DOU-FOI-H^OOMKMIOZI (OOMOIMftp*C ie pph+ m
OOU^Q1-W)034MM1021 (CMisa apkit ionpeatpnai
10 100
143 604 50
NO 6X2 83 46
M8
14* *34 49 0.6Q2 104 101 . NR
NR
1J4 9&4 56 0.662 664 . 66
m r' NR
1.43 5*4 44 . NO 36 4
no
1.43 503 56
NO , NO ' 66 ' 110
113 169
0*00 6.72 57 0.644 10.4 96 . HR
ojos
U
60 0444 W4 68 . NR
NR NR
0.064
706 62
2-21
948
74
NR
0494 704 66 X21 864 66 * NR
NR NR
0.700 0.700
7.56 oao
66 *XI2 60 .12
164 91 964 67
NR NA
NR NR
' 32
7
6.7
164
07 . NR
\
0.736 . 706 70 .7 604 4
NR
NR NR
446 103 66 1.02 9.46 K
NR- NR
436 763 73
1j02 964 65
NR
NR
6.76 1X1 63 0.792 .72 6
NR : NR
6.76 764 6ft 0.792 600 79 . NR
NR
SJ6 123
6ft
142 ' 10.5
96
NR.
NR
946.
? M ' 75"
lie
86.4 7
NR
MR
1 NR NR 7ft
NR NR
NR HR NR NR NR NR NR NR NR NR NR NR
MD NotMdwKMBdeaadtcsrtafeo*unWwwfl*rQeiounaSraetwaetirQ.inw1a*lw16a*.*an0a2eenwtfo<*wtighQ.
MMMotnaonad** toqaa*pantralmai*Mima. *> onMyeM< n d a n mTeWeh.
Exygen Research
Page 35 o f 132
Interim Report ^10-Analysis o f Fish and Clam Samples
Exygen Study No.: P000113I
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
tflfflp l
O O U -fO l-=0044^041021 tcm m ty m d. pp* b w D o u *o i-# *o o 4 4 4 4 io 2 i M m m ? m I. mbam i m
O O U -fO 1-*PO O M W 41021 tC 0 M t*4 p * . o M M ri DOU-FdHPFOOSO-041021 ^ornilo M .10Q pah
DU-F01-*"*001-0-041021
<oaof
M l
O O U fO l4PW0W -0-041021 (C BDM M K.tflO M M o>
D i*f0 i-i*M x & -0 -0 4 itti M IM M I *nM > DCM>f01-IPWOOM4>41021 M t M l1 4 8 ft8 *a )
D L2-F01486W 001-0~04t02l (CBMM1 M Ln ppt M o l tXJW -MW OC1-0-0*1Q21 M it i m J. i m 0iM
OU-F01-UBWOCCM)-041021 ic am m oM k. op* M M 0U -P014 *9 *0 0 2 4 4 4 1021 fOMOHtm U *M M M
DiOL2B-OF0M1io4i4M8 *06 09 4M4 4M1 0M2 1 L2-F0148fWOd4MM1OC21 icnm too m b. mo ppnM )
0L2-F0140 *0 084 441 021 4C0MtM*p*l. M 0 M M OL2"FO1-M9WO044441OS1
0L1MR0H18MM8W00.0180p0po0M410M21 0!2f01M 9*0064441<01 (C M K % kK 1M W M
0eC -F0l-M 6W lti1-O 441104 (C00MM0optC. 10 * M M 06C-P0144SW 0014181104 m m M ft MoM M *>
. 6>A;nolP*B9
" Sulltytaa P fHS
^
PUPS
ASpmMadi
AtSn loFmO aUlaItf
MfWAHCmDoMuMnUMt
fae ow t) <%i
AMmMt Fnopntti M u ta i
Amount RncowM
A n t Found Anol%o>woiy m><Saa)molo
A fflO tf* fMa M mM a l
R ttc w y <%>
10 .12 112 71 2.30 12.0 7 100 .12 714 TO 230 810 64
m
NR
NR NR NR NR
10 4 M 100 *
112 78 0J86 112 102 710 71 m m 818 88
NR NR
NR NR NR NR
10 2JO 102 73 0J48 .? 88 100 2hb 72.4 70 0J48 818 83
NR NR
NR NR NR m
10 10.4 24.4 10Q 3-88 112 86
100 18.*
78 188 883 86
NR NR
NR NR NR NR
10 o jtn 932 01
NO 8J8 17
120
HO CUM 788 77
HO 863 85
120
10 NO 16 87
NO 112 1
102
100 NO 04 88 ND 816 84 102
126 in 87
110 *
185 83
10 NO 634 03
NO 8.08 81 oa>4
103
1O ND 613 81 NO 853 86 82A 182 80
1Q NO TJ8 76 NO 728 73 8BO 718
100 HO
82-0 82
NO 93-6 M
880
188 78
to NO 7.88 80 ND 108 81 188 too MO 80.8 81 MO 100 10 188
13 234 88
10 baa 103 94 032 17J 83
NR
100 0J8B 00.4 00 832
113 106
NR
NR NR NR NR
fu i IH >>.< ta 0* 0 I n i t in t i m,; l lt o . M m in M i t i .a il M I a , n ta JIm i
NO Not u tM atorabout Limi*of QuanUtakonxtadi HOJnjiC* tagmv
HtaBtataaHwioM<taMOnilaBairuWa%ci ntaittaalaitanuailitMtuiamt.a Mul*a.oMMitwamyauAliiamiaramfto,Mait*orTtaMhialya.ln a a
ta ta * d ta .
Exygen Research
Page 36 o f!3 2
Interim Report #10-Anatysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS aud PFOS in Fish Samples (continued)
aampto
DBC-FOt-MSWQCZ+WKM low spal mMiito}
O(OB0CM4MWS14O4SpWe*0I0COW*W*4*11O*4
06C4W44SYWOW3041K4
OBC-F91443W0O34HMI164
(ogoiim iw h.iaawed m
O0OfO1-M8WOO4-(M>411O4
icw am aai. toppaM>
OBC-FQ14I0WOO44-M1104
tcsowwiamj. mb* **)
DOC*ft>^*M8WQ0B>0aO41104
(caaotaspax. tospaaRmi
D*C-F01-M8W006<0-041104
icaiiwi*u totoatototo
OBOFCI-MSFOQMMNIIOI (CMaotMipaM, toppOM)
MC-F91-tf8F0OM>441104
icaBtotoMaam. to
OeC-#01-M6FO<&*041104
icantitoi pao, itppeOpe)
DBG*Qt.*i0a2-O041t04
IQBDiwwawRmowa*t
ec-Fourfoo4- ^ 4it<K
<on*Mrpao. to apMpaa)
D8C-F01-*00*4M>41104
M f ttik R isopsaMto
OBC-FPMffOOfrO-QOI10*
tCeOaeaMpkft, to w tO M
OOC^OUTPOO^O-Wl104 NWMNIp*7.1000P0<to>
o(oieootwotoofswpaew, ipapfoc3a*mie)t
OBC-FOI-PWOOtftOMKM icw w psR teepto epto
09C-F01-PWWWWM110
icoaiiiwopn #*>
D6C-f01-W0054K>41104
eonsnu. toi wopeal
Antounl AmFan) hr****
AntFound Amount
Art*Four*
%*ed I'M .
KiSanpW
Om m tiI
Rwamy
Intern**
flMWKfd IW n r/
A**--1 mi
toiwmn torn***
10 DJ63 0*0 1 343 12* 4 HR 100 QMS 04 94 3.43 m 110 NR
10 0*00 0.92 91 s c 130 100 NR 100 OJOO 06.0 06 3.62 104 100 NR
0.004 9.M 01 0.72 106 06 NR 100 QMS 972 BO 0.72 124 114 NR
IQ 0.032 &20 74 2.77 102 74 NR 100 0.002 01.0 01 2.77 106 106 NR
10 OUBO BOO 00 3*0 117 W
HR
100 0.020 004 00 390 100 102 NR
10 0.700 002 B2 104 12fi 100 NR 100 0.700 0 00 1*4 KB 100 NR
10 JM too too 0.504 11* 110 142 wo Qi04 040 04 0*04 106 106 142
10 1JB0 104 00 2.16 122 101 NR
too 10Q 00 BO 215 105 wa
NR
10 0.404 972 92 320 100 0.404 87 V 320
13* 97 104 lOt
HA NR
10 0J 72 104 90 2.10 132 111 NR
too QJST7 K*
n
2.10 102 100 NR
Amount
NR NR NR NR NR NR NR NR NR NR NR NR
1 254
NR NR NR NR NR NR
nsnowiy (%)
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
, 1
NR NR NR NR
NR NR
mcQvsrywtoacamotHeafcwuaetf
NNNO-NeNtotatpOoittooectueotoo<rMabtoo|re*e|nJrnr*lnotofNQMuanuOmM. oMfimwwNNomfttm0m2OrtiQototNtomtoTMtol,
Mato: Olnqe tot awwewy totoe aOmw w a a to d fiaalto, n e a m y w fciaa w y m >
Owe 0 M um to too war data.
Exygen Research
Page 37 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
fiamph Dmatahon
DOU-F0HPW008*041104 tom m m * * K m + *> D0U-W-tPW0C*041104 fCOWHHt* L . (90|pO9pta)
DOU-F01-JPWOO4*O41104 to a m m * * c to op* a*j D0O-F01-lPW004*041104 (CsoMia>cuocppoMu)
000#01*<PWOQ8*41 104 iC W lH h fc U M h M 0OO-W-IPW0CA*0411<>4 (C80MMaptF.tto PMI
D|>fC1-#*W003*04110* anom u a*a OL2-FC1-IPW002-0-41104 IC *** h h. mbtvM
OU*O1<M0WOO1*041104 (000<0461|*l,fSw68W
1311401-MSWOW*041104 comm mu4.in m
OL1*=01-Mew0t*041104 fe m m tM i+ K * m * DU<rOt-M3W002*041104 CM4MM8 * U14*p * M M
DLt-F01-MSW002*041104 lonniKirafSC. tnn*pa) DL1<F01-llMMl00*041104 i c m ama.hhoau
Otl-POl M8W004-0-041104 (OOMhtnnipk i. MpuahpAu} DL1<F01*M8W004*041104
lOBppOtffeo)
OM-RQl MgWOOd0 00104 IcflKnuM pnq.iowtM oi OU<FD1-MSWOOft*H11M iCOOiSPS^fcliHOwO^
DLl-fOI-MGFOOl*041104 (COMMWaptt Mpk 0U-F01*taF0O1*041104 (c a M M ***j. 0 **V ta )
C A W krm P W
C$dfcnaH=H8
CEUWnaPfO
Amount Ami Pound Amaunt
AmtFound Amount
AmtFound Amount
SpMtOd hSampN bacaam naeoimy in Ovnpte AuookOTd nacoKury in Sump** Racowud Racov*y
im m M kriP U .
m
10 3.13 13.1 too 820 100 3.12 02 05 8J00
12 103 W 101
NR NR
MR NR NR NR
10 349 12.3 3 7.12 17.4 103 NR 100 1A9 A 86 7.12 100 101 NR
NR NR NR NR
10 227 10.3 73 $.12 110 84
NR
100 2.07
m
1 b.12 too 104 NR
NR NR NR NR
10 104 3.43 04 100 1.04 0 0 79
ND 104 104 820 NO 072 98 8.20
142 01 124 116
10 120 100 120
10.0 04 0.800 112 10 0. 03 0208 112 111
NR NR
NR NR NR NR
10 120 0.73 tfi
1.72 12.4 107
NR
too 120 0.4 79 1.72 100 08
NR
NR NR NR NR
10 0250 0.02 04
100 0.500
32
33
1.13 102 91 1.13 082 08
10 0.000 022 70 o.aoa 78 89
100 0.90
MJ
4 0.008 092
99
NK NR
181 181
NR NR NR MR
201 #
2M 108
10 1.10 0.30 70 100 1.10 2.4 81
1.18 104 82
1.18 4
88
NR NR
HR NR HR NR
10 ND 100 HO
7.70 7 0215 822 00 734 7 0.315 802 so
293 293
303 394 101
NO NBO NeMdta r a b a U N I O OmriHIlloiihlJifc<IJiiB^tlMl(^H. NK. Nt.nacrtAm>p ctyaqi rtmMtwktmt. a . may. rMjtaM W M. mra. a.
NalK^aalaw awiyHaaliaaiwimnimia>.iaaw^anmimaaBaaaiaiawlaalBaNiaafc.
Exygen Research
P a g e 3 8 o fl3 2
Interim Report #10-Analysis o f Fish and Clam Samples
Exygcn Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
to n p f
DL)'F014Sf002-<hO1104
KOMMnan . toppaM
n.1-F01-M 8FM M *0411M (Cantin a n i m a n t
OI1-F01-MSPOOMM41104
m o w n a c.M m a n
DU-FOI-MSFOOMMM1104
(C404MM 4 I04nk (14
n.1 -F 0 l.i K X > frO O * 1 1 0
IC0*u*af. M U M
0U -F01-M ara04-O 441104
loeMosna^p. MDfnoaM
OU-fOVM5FOOKW11M <C4Mr41(4 . Mpptpkp)
O .1 -F 0 1 4 IS F 0 0 a * 0 4 1 1 0 4 (noo4iinaptM .ioan.ipu)
n .i-F o i m n 0 4 iio 4 sa n o w n a p a m ppa a m )
OU-FOI^PWOOt-MailM
(OooMsnapfejpMOfpta^ai
OLI-fW4PW0IB4M41104 (O004t*iaoat a. io ppt apow) OL1-F01W002041104
(O O On.nonm copptO pt^
DLi-aoi^Pweo*o4iio4 (CHOMTTlptC, MaptOPO.1 DL1^01-PW00O41104
(coouon apt d. p p a p u )
DLI-FCVPWOM^KXI(04
(Ooo*aaaai, lopptapat)
1'OWPW0O44M)41(O* (CutP(70apt P.100pptOpMP)
-Foi nroaa o aoiioo (O toootnatt . loapa opaa) Ol1-F01F00O4H110 (O0O400T0on H.no ppt Opa.)
OL-1-FOUPFOOKW41104 (en ta* opt uo **u m
4OL-1 -FOI-IP fW VO OO IIO*
iouoioo a n . no n o *)
I **ad
J ja tt. 1
10 100 10 100
10 too
10
100
10
100
10
100
10
100
10
100
10
too
10 100
maMnpi W tc u tn Raoman
M l vatL
ND 8J0 NO 4Z 8
0.200 0.78 86 0.203 04.4 84
NO 8.00 09 NO M J 87
NO 8.04 00 ND 134 82
0.772 864 n 0.772 84.0 83
0.400
too
82
0.400 78.4 78
NO a os 01 ND 00.4 90
NO 840 05 NO 710 72
NO t o o 00 ND 88.4 86
ND too 08 NO 780 70
Amount in ampin ftKOM d Rotow) to Sont*
0.024 0024
1 05 09 964 98
0.062
0.003
103 968
95
86
0032 10.4 88 0837 101 100
0.004 101 94 0.604 940 93
OJM 8.72 93
0.566
970
97
OSM 0.530
9.96 84 800 . 97
0800 944 92
0800
106 106
0839 0830
080 848
90 89
0822 086
91
0822 08*4 98
0805 108 109
0805
904
90
NR NR NR NR NR NR
nr
NR
174
174 15.7 16.7 930 0.30 59
a te
ii.i
11.1
200
20.9
5 ______ Amount Roeommo Wtcwpijr
NR NR NR NR NR NR NR MR NR NR NR NR NR NR NR NR 2 0 4 90 113 99
2 7 4 117 100 04
10.7 109 100
72j0 140 80 199 108 97 5 90 109 0
Not M tocM at or
u n i cf O uM M cn
k 0.2 (M l M * m
-- * " * "f r n r i.nMi , t . . m . , t n t ) t u, , tk M M t l . 4
Exygen Research
Page 39 of 132
p. 40
Interim Report #1^-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
tempi OMortpten
(X-1-F01*m0t041104 (C09WM1ipbK. Wpptlpkel DL-1-FOMPFO044W41104 <00*4*1 % * 1.no m um
OL-1-F0HPFWO4M1104 c.* m tm
DL-1F01-**R)06^WH1104 <caMOMV%i>0. tw **)
004014W V 001-0-041106 <C00W<O4ptt.WpM) DLSTO-M0VMO14-041106 ieoo4ipkr. MOamm >
DtM01-M8Wfi<B46411Q6 fOBBW Uk|NlhM tX>FCmW0Ca4-O*110fl IC--IIIOI a * K 140*<*
DOP01-MSW0094441103 tcwiM N*i towb*M
tx>foi-M awoo^M iioe tenmmi+j, woiuotfnt
OU-FW-MSV000WM118S 0O4WM4** . #* m ) (X3*F91`40WOO44-4611OS <00044**k U< H*MM
004=01-**0034-041106 toeomwyIF c. to Ipiwi OQFP1 MgWOOC0 04110 tcamotop o. 1 9 tm
OC3-FO1440FOOI-44411O5 tcooew^pa. to****} OU-FO1-M0FOO1-44411O6 tceuew r.i e wo
o o r o i Maroon n n i l 100 poom w^an, ww>Mw DOFomaPooa 0 041too <0H40MtIpfctt. tBWOU*M
D*.mi-MfiPttW>641H)0 <000404W M )wo%*> DUM^OVMBKJOMHMUOS COO I I A MO woSUM)
PFH8
Amount mSTSHT ArtM*
AmtFgurt Anoint
H r* f o n t
a p M fcttenpi RmmwM RaooMry taSanuto AooraO nwimnry ntenpl
___51__
*> N i
10 NO 100 NO
OOO 80 M l 66
NO 6.46 66 7.60 NO 68.6 9Q 730
10 MO 7.44 74 0.373 6.00 88 100 HD M i 86 0-373 984 98
672 8.72
10 HO 0.36 M 100 HO 09.6 88
NO JO 62
136
NO M i 100 136
10 HD 6.44 04 wo NO 004 00
NO 6.63 66
160
NO 106 108 160
10 NO wo NO
6.00 86 604 80
NO 9M 98 NO 102 102
146 146
10 HD 6.48 66 03K 6.6 94 196 wo NO 804 80 0386 102 102 186
10 NO 0.96 06 0J86 11.1 10? 173
wo NO
100 100 0366 106 106
173
10 HD 6.46 86
NQ
11.4 114
116
wo NO 40 60
NO
10* 106
116
10 NO 0J6 BB
NO 104 104 116
100 NO 69 60 NO 103 f03 116
10 NO 0.32 93 wo NO 0Qj6 1
HD 110 110 73.6 NO 107 107 734
Antont Rm y 0
164 2 102 94
16.6 72 102 83 166 * 2S6 11 150 . 203 103 164 , 264 106 239 . 1 103 WO 346 73 138 . 204 116 668 * 21 100
920 160 114
NO H a rtlan l N or m ow UnntK* Qui n n
NNS 4 iv iiW ii i(iM % * o liw U n i.
iffi.nuw r>TffiH.
WNcW-- iMi iiyW *iir'oiin<<iMO.nr >wlfwlm .n n a y aw ay In n n .ii-- n o -- 4.
Exygen Research
Page 40 of 132
p. 41
Interim Report #10-Analysis ofFish and Clam Samples .
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
Semple D n iiim
OI^FOl-MSPOM-CMMIIOS k n w m k. m m m OLwn-M apw^o-M fios
0L8F9Miil3M06^>4>411C icmaae*c.& ****> OU-F0144SFOO6-441tO6 tc**nw m ia leopps
OMC*F91'tPWO08<O-O411O6 icoowwo* ii, io m m OMC^OHPWOOVW41*w (CBtoemM *. ico**Me>
0MC-F0WPWW4-0-M1 5 (Ommm m i a to pm m m DMC*F01-(PW004-0-04110S (CMiNII MK 1l0jp6N*vl
Oft4C-F01HRW006<HH1l06 (C K M M ilpulfP IM OMC-F91-VWOQUMM11GB p n m m tm j, *Ope*M*)
DMC4W44SW003444I106 (C M ixH aK .nnM M
DMC-F91-M9MUMOI1106 PM <IM #U tflPnH M
DUC-fW-lt3>V004Ot1l06 (CtMnrm*c. to * tpMi
DMC'FW4i$M0Dt*A41106 icaiBUfTMaa *mMto)
OMC-RH-MSWOOfiKKMlIOS (OOMMtpit. 1NMW
OMC<F01<M3W00BO-O41106 (CMMMMif. 1N 1*m
DMC-n0t*48r92*O4il08 {OnpnaOUffc> **-- ) OMC-PQ1IA8F0080Q41106 lOOMHMMH. MOiMiMM
DMC-F01-M8F0094041106 {OQOMMOMi, '*%*>
DMC-FOVM6FOO^41106 tCMIMBiMatOOMMol
Amount M od
AmtFound toSemple
nm oin Rm n iM Asoewy
Amt Found totempte
n- Ammwou-vnto Reoou--y
JllM^OUAd u se r* *
Amount Iboow d
Rncou--y
(natal
**fr>Mtwt m i M l
mi
to NO MO 96 100 NO OU 90
NO 11jO NO 104
110 104
1 130
144 238 108
10 NO 6JS 69
ND ' 10.3 143 814
74
100 NO MB 96 NO 944 94 61.6 161 96
10 NO flJO 83 0J66 ; 942 91 . 612 784 #
100 NO M A 94 0.366 994 96 12
158 95
10 0.300 404
77 0396 - 9J8
m . 664
100 a 300
90A
90 0.396 104 104 664
107 # 168 99
10 NO 496 90 0.270 10.1 n . .644 100 NO 944 68 0^70 106 166 644
to NO 464 96 0.602 110 -104 354 too NO 92.4 92 0.992 109 106 364
10 0.316 9 ja
1.90
12.1 . 102.
269
100 0.316 844
62
190
101 . 99
294
10 NO 416 92 0J60 114 106 NR 100 NO 9M 4 0.960 118 117 NR
10 NO 436 64
NO 104 104
NR
100 NO 97. 98 NO 104 , 104 MR
10 NO 430 62 ND 104 104 644
100 NO , V 3
7
NO
110 . 110
684
754 153 B
389 484 110
259 13 54
NR NR NR NR NR NR NR NR
108 %
184 1V
W-Ma<pwl*.lii)*i wniwluMX--i
WQlKloo.tm . -- My1. <IKCT1M<I<
MM.
Exygen Research
P8ge41 of 132
p. 42
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
tam p*
OMC-FOI-MSPOD+CMMIIOS tceneeoi m o * w n) 0MC-FO1-M8POO4-O-M1106 tfim tm t m u tDi**M>
DMC-F01-MBP0050041106 (OOOMMBM C.MM 0M) OMC401-MSFOO644411O6 IcaaMMaMO. 100MOiM
0MC-F01-TFOOfrO41105 E M inM C H w M oM OMC-F0l<raa*O41 too (CaeamOMP. M8MW
DMOF0HPF0W-0-04H06 (CMW0IMO.14M-- ) DMC-F014PF004-0-041104 {OOOMK4M K M OpM
auc-m ^pnosooiiQ 6 tOOC*ML WMM) DMC^or-ipfoo6<oo<noo (COOMSOBM J. tOOMlM)
CX2-FOVM6PO06-O41210 (OaoMSMM C. 0L&F014PW0C4OO41215 (OOOMM4M F.taaM Ml
0L2-F014PW0C4OO41215 (CMm ti c .a M L2-P01HPW00^0041215 (GOOMMiMO.
tXHJ-1-MSW0a2-W>4l218 toooMaet m s a m u i
DOlFf0l4tSW0a2-04M12l0 lCe*44l4M * 1* M e#)
OL2-F01IPW004404t3Mfi < O M > artacw m M i 0U-F014M0C4-4O4121S (OOOM4S7M *N 0M M b)
D0l>f01-4SW003^04121 QMBMaMK. ttN th M
0OU-f0144SW0(O-(MH121fi {G00MA1OM Ut>M SSM
aMma.ffW___ __ .M WaagM______ Wxww.rro
Ami Found Aimm
AmlfounO AffOtf*
AmtFound Amount
MSftnow IM mM ftacoMry toSamo* RbqmM Raceway kisntpln iUcowrul IfeOMry
M tlw tui
tnMMM.
r>
Hi
10 NO 8.76 88 0284 11.1 104 11 100 NO 880 88 0254 107 107 11
123 228 110
10 NO 8.92 86 0.420 122 118 148 100 NO 834 84 0.430 110 110 148
193 280 114
10 NO 7.02 78 too NO 820 62
NO 104 106 7.92 HD 106 106 7 93
IftO 61 101 83
10 NO 7JB n 100 HD 832
w ND 7.68 79 100 NO 750 7
NO 107 1C7 440 NO 107 107 44.0
ND 10.3 103 484
NO 9 M
88 484
552 134 90 54.4 121 75
10 NO 8.44 84 100 NO 32 83
ND 104 100 492 ND 102 182 482
982 100 142 83
10 ND 6.00 80 [*> 114 i t i 132 72 7 AS
100 NO 844 88 NO 107 107 132
121 106
10 0206 802 67 1J2 104 92
100 020
ST2
<7
1.72
824
91
NR NR
10 NO 808 81
ND 10.4 10 40
too ND 764 77
HD 882 96
40
NR NR NR NR 144 80 872 w
10 NO 8.t2 81
100 ND
88
10.4 194 80 ia4 108 96
NR HR
NR NR NR MR
I1 *X
Sf ltoin f .
camtwoimyiniu.matt
NO Mol dalnctnd or earn Un* & (X M aM n wMcX 0.1 n6*tt Cwr. i.Jrl
M e. nm c m t n . w n n m nonminnBam i--. . m m y v n i i -- y j r / i u m fpm**<ran if
Exygen Research
Page 42 of 132
p. 43
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
Sm s*
C4 Sutoal Pf88
C* H onf PFHB
CatHBnWI>fOa
Amount Amt found Amount
AimPoimO Amount
Mat Found Amotnt
Sf*ad fetor** fbepmnd Riomvy feitensm Raenerid neoffmry namnmto Rnoovemd K m a y
r%> <**** MM m4 (%) M M *** M lamaP Ml..
0OFWHPW004-0041130
tc a m m cm o. pw
10 HD 732 75
OLM1-VW0O4AO41130 <009*414IW' .m****> WO NO MA 88
NO 11.0 110 7.92 NO 118 118 7.M
17.3 9 114 IX
DQW 1 MBW001frQ41219
i r f in u p aq mmieew
19 7.00 14 75
15.4 275 121
NR
O0tmi-MBW001-*041219
iCMaomap*h. momo i m
100 7.09
2
75
`5 4 22.0 107
NR
NR NR NR NR
OOW91-MSW004-0-0412)V
. |CMMiHRiH.mpp8p--l
1 4.72 10 1 213 203 75
ooaroi-M *Roo4-o-04i2i9
(OWW HfcF.meWO#aio)
100 4.73
n*
X
21-7
104 X
NR NR
NR HR NR NR
DOO-FO1-M8WOOS4O412I0 ioeew e^eo, mwoapbN 10 0394 7.09 7 134 582 72
OOU^D1-MSW0064O4t219
KenpMenwM.mepwiW)
100 0X 4
72.0
72
134
87
NR NR
NR NR NR NR
OOt[01'*t8R)06-0-WI2t9
oemem)am& ****)
10 1.41 9.00 72 8.40 17 X
NR
NR NR
OOt7*HlP005$-0412ia tcaommiewo,me***> 100 1.41 720 71 540 94jO X NR NR NR
otm i-iPwoo8-o4M iiao
icnmemom *. *!)
10 NO 7.02 79
NO 9.04 X
12.0
186 X
0OF014PW0Q2-04M1130 o o M t mar. iemoiaa) 100 NO 813 81
NO 110 110 123
109
W >f01-rW tV 0M 11
<Gmeam4m*.ttimewi
10 NO
DU-P01-mV009<M>41130
fceeaomewh>meppoaeon) 100 NO
7J6 80 94 84
NO 9 X 00 544 NO 103 102 944
12 X X 97
DOU-F01-MSF00&0441216
tceeeeme * * * * ipim
10 1.72 .00 75 9.98 143 77
NR
00U-fQ1'M8FDQ34HIM1216 (CKiemiiwu name Spool 100 1.73 90.9 88 556 107 100 NR
NR NR NR NR
0eC#O1*MSrQO`V941219 Bnim itsw c. * -- > 10 0X9 9JO 91 1.79 11 X NR NR NR
DRC-F91-MSF008-1-04131*
ew m r Spao, teepooW
100 0X 0 8X6 83 f.79 x e
X
NR NR NR
D8C*F01-4UttF006*0>041218 ic n in e sw * . mem earn 10 NO 839 84 ' I X h a X NR NR NR
OnC^5l-M8FOOfrO-M121*
loewemoipfcu w wow >
100 NO
80.0 9t
IX
X X
NR
NR NR
S--W**wXoowcmdtospldnjmmHpaNcaN;fcamtbrfcwBMgi--corny--hiocum*sataWM
NNRONoNttaoptodieWWdd^uMnmoirpoiWbtwyr#oUunrdwdONuRWiWMtoRw>hichio0 2 ngfleN*weiiwghTt)P. Mi.
.
Mam:OfcwpWo ---- myMooliw o mwWM--mm. ---- yaai--o amps PigM *> Mm Nm -- dW.
Exygen Research
Page 43 of 132
Interim Report #10-Analysis of Fish and Gam Samples
Exygen Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
9wnpM n irlis b a i
DOU-fO1*443FOO2-0-O4l21d fOMM***. *c***#} DOU-P914fltf002^4M1316 fcoosMa* n.m m *)
COOR01-IPWOOI*041130 fCOMMtti*C,i t !%*! DC3-W4PWQ014MH1130 (OPWOttlH P. twMpawi
oou-foi-wswaa-i <04121* |C4MH71 tfk k.t0{*49pM)
000^01 MSRKD-1`04121* mms* anj.seam %]
OOU-FO1'M8fOO4-O>O41210 icoa*MnkK, *p4Mi OOOfO144SHXM-O4Ml210 icNMm m l m m Mj
DOU-FO14i36O01-frO4l210 <ooo*4n*Lii*aM j DOU-F014U*fQ01-WHl21* to o m m 9+ 9. m m M *i
D8C-F014MF003-0-441216 p o o m n + k * . ***) N C-f01-M if00O 4l2l lew H tT faH ,
DC-F01-M*F004-<HH12l ooeewTiSpat, to**!> MC-F01-MSF004-<M>41216
10
OMC-FO1-MSFQ01-O44121*
OMC-FDI-MtFOOl-0-04121* (caoM4Tta* 0.m * t Mi
pui-fot iw w e ott*i*
ic m n tn m i
OU-FOi4PW00MO4121 <caosMyr$pki, imh* m o
O t*l4*W 0*O 4l30i
ic a n w ita p a K .
DL2-f014PW0034-0419l iCM M ftfrkM ****
M o n t tan Found Amovt
An*Fountf Amount
Amtfound Amount
9*M4 toSwrvte RuctnvrtO K n a y *i SompM Anoowod NXO'IWK
flouoiwd Racovary
M o i MUMat
-- 1*1....
tnoMuRut r*>
10 0.060 024 4 4.56 14* 96
10O 0*68
806
3
4J6
104 9*
NR NR
NR NR NR NR
to NO 7*0 78 0244 4*0 94 004 to o NO 81 2 024* 101 101 004
172 62 102 03
10 0LJ40 20
*4
4*6
14*
99
100 0.040 82.0 *1 4*8 103 66
NR NR
NR NR NR NR
10 0.792 7.78 70 326 4*0 6
100 0.792
*12
60
2*6
86.6
63
NR NR
NR NR NR NR
10 11
11.1 69
100 2.1* 2 1
10.0 20* 6 1 0 * 104 3
NR NR
NR m NR HR
10 ND 0 4 66 2 jO0 11* 6 1 ND *4* 64 2*0 106 4
MR NR
NR NR HR NR
10 NO 7 3 7 77 3*7 12* 00 100 NO 7Sj6 7* 3*7 98* 06
NR NR
NR NR NR NR
10 NO 00 1 0.420 9 * 6 67 NR 400 NO 600 66 0.420 102 102 NR
NR NR NR NR
10 0283
7.40
71 0.644 9.96 3
86*
802
100 0283 714 72 0.644 6 6 * 66 B.S
145 76
10 ND 7.04 70 NO 004 0 7.4* 107 42 100 ND 71* 72 NO 920 2 7.4* 64* 77
iiw iiffc
. . nt
tiwAcn.m ino u n
wnmi>m cvniM
MD HaidMciMalorak<*UiiiKarOuMallBiNckli0^i%tMt<M<gh0.
1< w> . !--*. HB.W>Hum
*w m -- n > * ,
Exygen Research
Page 44 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
Table IV. Matrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
nmTil n lus
nemfciaoamci ha eateimad
NO N aidW eedaier shew UwifllOuartibilniifiiioiNlUiWpW weigno. . NMaHfNemm*amNigmMa7m<wl.
Mmjmcate*a-- ww iyteMa d a w awdadmatem, mm f r ten waymry
>!-- dam.
Exygen Research
Page 45 of 132
p. 46
Interim Report #10-Ana1ysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table V. Matrix Spike Recovery of PFOS in Re-extracted Fish Samples
Sample OaaeKaHon
D B C -F01-(PW 001-(W 41021 (QOoaisiSptG low ppb)
DeC-F01-B3W 002^ K H t02t IC 9M 1 pt 0. IMO ppb)
OBC-F01-IPW 003-0041021 (CD0MIS3 34* E 10 opt)
D O U -FO H Pf001-0-041021 (COOU144apt P. 1000ppb)
D O U -F 9H P F 0024F 041021 (CooMiasapto. loooppt)
DOL'-FOI -1PF0090-041021 (coM ioaapkKiM Oppb)
DCMJ-F01-IPWOQ2-0-041021 (C0M81W Spt 1.10Mppd)
OBC-F01-MSWOOHM5411O4 (00040490 4 * j , KWOOPPM
D9C-F01-MSW 002-0-041104 (00040401 Spt K. 10,000 ppb)
D 8C -F01-M SW 003-Q -041104 (C04MO462*K 1, 10,000 ppb)
D6C-F01-M SW 004-0-041104 (00040406 t f k M MOOppb)
DBC-F01-M$W 003-0-041104 (00040441 3pt N. 10.000 ppb)
D8C-F01-M SF001-0-041104 (00040464 apkC. 10(000 ppb)
08C-P01-MSFOC2-0-041104 (C00404M a p ta ioooo ppb>
D eC ^O l.FR M W W M 1104 (00040400 apt E. 1000ppb)
06C -W 1-IPW 004-0-041104 tcoM * a * r , ioeo rpb)
O B C -F014PW 00S4M H1104 <coo404aoapt a w o ppb)
DOU-F01HPW003-0-W1 (04 (00040401 Opt K <000ppb)
OOOF01-IPW D04-0-041104 <0004*402 apkt, tooopet
D O U -F014PW 006-0-041104 (00040403 3 J. 4000 ppb)
D t 1-F01-MSWOOWW41104 (00040400 apkK, 1000ppb)
DL1-F01-M SW 0024M 41104 (00040400 aptc. loooppb)
OLI -F01-MSVWC3-OO41104 (C004O4t apto, wooppt)
O t 1-F0144SW00S-0-041104 (Coo440oapt a. loooppt)
Amount Spkad - - W flJ
1000 MOO 1000 1000 1000 1000 1000 10000 10000 10000 5000 10000 10000 10000 1000 1000 5000 1000 1000 sooo 1000 1000 1000
1000
Amt Found InSampto hotatw btw f
20M 3330 1060 508 636 644 1210 94W 7820 12800 3440 3240 3240 4780 60 1230 2B20 2270 1740 2130 96 706 8
804
Amount A acow ad
2880 680 3180 1780 1740 16S0 2610 23200 16600 23200 520 16200 14400 13200 1600 2800 6520 2640 2740 7600 160 1760 1630
1660
(portad Ata id quality <m m n u t U m V tM a a n not Included in dw w m y natica.
Exygen Research
R ac o v ity (% ) 76 107 150 118 110 111 140 137 81 108
102 100 92 104 96 136 78 37* 100 106 8 107 123 106
Page 46 of 132
p. 47
Interim Report #10-Ana]ysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table V. Matrix Spike Recovery o f PFOS in Re-extracted Fish Samples
Sarmp* Oncftodon
(continued)
Amount Splkad (nota)
C * SuionaiB PFOS
Amt Found In Sampia
Amount Racovarad
(nota) wot w i (n a to lw a t* .
Racovary (*)
DL1-F01-M3F002-04M1104
(0004*171Se F. toac WO]
1000
566
1080
> 112
D LI-F01-M 3F0030041104 (C fiO 4M 72S0Q .ia00ppb)
woo
432
1670
124
DL1-F01-MSF006^MM1104 (00040474 tph H. toee M*>
,1000
1
740
1830
10
MC-F01-MSW00S-OO41105 . (CO040490 Spta 1.1 OOOppt)
1000
$60
1780
122
D M C-F01-M 3F002-0-041106
(C O M M A S |* J. 1000 ppb)
1000
620
1500
08
DOO-F01-MSW002-0-04121 (00080400 3JHK. 10.000 POO)
OU^OI-M SW OOM M M I 21 (C00064fiesp i L.WO Wb)
D O U -FO I-M SW 001-0-041216 (C00S0400 Spk C, 10000 ppO)
DOU-F01-M8W 004-0-041216 (C0080401 8pfc 0,8000 ppb)
1
10000 5000 : IOOOO sooo
20000
4040
7000 $120
'
32700
10200
25000 ' 8880
46 123 174' 86
OOU-P01-MSW006-O-O41216 {COOOMB 9pk E. 1000 ppo)
D<X>-F01-MSF005^)-012ia (O 00SM 8I 3pk F. 1000 ppb)
OOU-F01-MSF003-0-041216 (C 00O M 00f*O >1000ppb)
OBC-FC1-MSF006-1-041216 (C00B0447 6 01 H, 1M 00 pb)
D B C -F01-M S F005-0041216 <C0066464 Spt 1. fOOOO* * )
DOU-F0144SF002-0-041216 (COO BM BSf* J. 1 0 0 0(4*)
DOU-F01-MSF002-1-041216 (O00S4471 Ig k K, 1000 |W>)
D O U -F01-M 6F004-0-041216 (00064472 a m U 1000 m b)
DOU-F01-MSF001-0-041216 (00056475 Spk C, 8000 (4* )
OBC-FC1-MSFD03-0041218 (CO00S4MSpfe D. 10000ft * *
DSC-FG1-MSF004-0-041216 (OOOHMT8SfOtE, 10000ppb)
0M C -FD 1-M S H H 1-0O 41216 (COOS6470 8pk F, 1000 ppb)
o e c-F o i-iP F o o i-< w m o 2 i (C0M4144 Bph . 1000 ppb)
06& FQ 1-IPF003-04M 1021 (C 0M 61M Spfc H. 1000 ppb]
DOU-F01-IPF003-0-041021 (C*046ia*Spk I. MOO I )
1000 1000 1000 10000 10000 1000 1000 1000 5000 10000 10000 1000 1000 1000 1000
486 730 646 620 6960 040 082 1620 3070 4040 9280 640 384 293 666
1780 1820 1720 32400 24100 1720 1050 2700 7960 15500 24500 2040 1360 1340 1400
128 110 87 230* 151 108 126 88 118 108 152 120 87 106 104
Ne*npoitad 4M to fty oonM r a u t W u n t. VWum am not M udM * lw u m a y a u a
Exygen Research
Page 47 of 132
p. 48
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table VI. Matrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples
ta r* * toatpdoft tii6 iR io o rw i2 ie <0000*00* * a * a t
OMC401-CFW00V64412W <onrw iiitae.iw *
DMC^i-CWOOI-OOOQIB Ic-- iwOofF.wow
0L24O1-CFWOOl-<HMT21f teno* *******
CU4D1'CRMB1<04l41Zie romms OmKwo*)
pO40t-CFVWH-044121
D6C401-CFWOQ1-O-41215 (caomeapfcA*eppe)
0LH01-Cm0(M4>^4l216 (COMMUta*.***
DL1401-CHNCDUMM1Z1S D eew tau w w
OOiM0l-CPMQOt-O-O4121S eeoaiawtaiMdww
OOUJO1-CF*M01444t218 ici-- in t a h o p*)
Amoual A M fC U ti intu M ad * U n p i t o u
10 ND 100 W
824
10 ND wo NO
004 9
10 NO 100 NO
7-28 5
10 NO 100 NO
103 084
10 NO wo NO
&N 002
10 NO 10D NO
0*0 044
AmiFound Amort
AndFound A n c u
nco--i) kitatyN noopumd tocevy hO m fli tU c o m i WacfNury
) <*>
60 ND *18 03 103 *32 4
02 NO 96A 86 1.82 802 81
00 NO
8,44 84 8.16
11.8 $1
63 ND G6.8 98 61 828 87
73 NO 7.84 78 %1 7 52 87
84 ND
W1 KM 1J1
884 87
103 ND
W4 WO 4.48
130 80
64 NO 872 or 4.48 884 82
00 ND 832 3 0.80 160 2
06 NO
103 103 880 886 81
06 0202
832
01 11.4
172
81
4 0202 960 88 11.4 06.0 87
iI
84 10
d I or utMrmUn* of QuaataKM wNdt H 02ngfe (*t wofcM. rtfMyvmyrtfcNNto* 4ww
03 M O nM m 11
73 If
H
i
Exygen Research
Page 49 of 132
p. 49
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.i P0001131
FIGURES
Exygen Research
Page 50 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 1. Typical Calibration Curve for PFBS in Methanol
O O W O M n *.> *< rrM *" L ii W R M i*a lM f1 /a ra' a< |M i.a T . 1.*1CD 4a 1 07 ^ 0 0 (r O.CSS)
Ana, counts
Exygen Research
Page 51 o f 132
Interim Report #10-Analysis ofFish and Clam Samples
Exygen Study No.: P0001131
Figure 2. Non-Extracted Standards of PFBS in Methanol, 0.0005 jjg/mL and 0.001 fig/mL, Respectively
tm i*b m c y *J> I W n / l 0.1
Ate: 10*57 ** M*JMr7*1. <# RT.-O^V aM OA
Exygen Research
Page 52 of I32
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 3. PFBS in Control Fish Blank, 0.00625 fig/mL Fortified Control Fish Spk A, and 0.025 pg/mL Fortified Control Fish Spk B, Respectively
wwtOtm+tf.W f
' M M 9 H 3U n m MNMCMW
1 234
* 7 * ii a n
I
11RMfMI C|k t - PFM<PC)M0.(MB0 ta il . U K fl. .1M fern OBWSEjMT
AnJ 33M20 m all HaM- MSDO. ap KT Offir Ml
14 M - w
it
Exygen Research
Page 53 of 132
Interim Report #10-Analysis of Fish and Gam Samples
Exygen Study No.: P0001131
Figure 4. Chromatogram Representing a Fish Sample Analyzed for PFBS (Exygen ID: C0049478, Data Set:061605E)
I OMffgl-prat
Anm4MJi
f mfH
Exygen Research
Page 54 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 5. Typical Calibration Curve for PFHS in Methanol
0108( rh.rfk<PFHS>
>** f 1 / * ***> Y-
x 14009 (f- 04M1)
Exygen Research
Page 55 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 6. Non-Extracted Standards of PFHS in Methanol, 0.0005 [ig/mT, and 0.001 |ig/mL, Respectively
li^irwHir, cps
wrwwwi Af%ss f M i i l i l h
w nifm
*7i f U n h
000 000 400'
300 300
100
| nVOPFHt(MMda*<OOXMMAaM-smal3*130lMfliOei06Eriff As m : 331TO eu>H H a lM * 1300. m *T . 1 03 m o
KitanMr, cp
Exygen Research
Page 56 of 132
Interim Report #10-Analysis of Fish and Clam Sandies
Exygen Study No.: P0001131
Figure 7. PFHS in Control Fish Blank, 0.00625 pg/mL Fortified Control Fish Spk A, and 0.025 Hg/mL Fortified Control Fish Spk B, Respectively
(Urlfftm;91MMIH.MV*9TrnfnmNfMMT p M lM tllia ^
A09 X
_ 3.SZ
iC i,
ft 10
Tim , mht
I Rea* 0 * A . W HS (OC) 300 0 *0 .0 *mm a n *l 10 *O a tan* 0M 6Q 6E.*
M m : 1M 711 OMM0 m i i * 13000. m OT: 1 0 mim
12 J4 f
0
7
0
0
10 11
12 10
14 1fl 1ft 17
Tim , M a
Exygen Research
Page 57 of 132
Interim Report #10-Analysis o f Fish and G am Samples
Exygen Study No.: P0001131
Figure 3. Chromatogram Representing a Fish Sample Analy2ed for PFHS (Exygen ID: C0049478, Data Set: 061605E)
ilm e IW W t w HtUm i
MtSMCnMT
Exygen Research
Page 58 of 132
Interim Report #10-Analysis o f Fish and Clam Samples -
Exygen Study No.: P0001131
Figure 9. Typical Calibration Curve for PFOS in Methanol
OBWOO
(yf Ot% u f
f / < Ii WIiiU y - l.KH)OxX90*4O03(r-0M00)
qurHn'MJV
Exygen Research
Page 59 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure IC. Non-Extracted Standards of PFOS in Methanol, 0.0005 jig/mL and 0.001 pg/mL, Respectively
% m ; t M I c m Ih lg k t d H
-M fh
MTi ilim i*
OtrWfceflF
1 3 .
1294
I twnttoroo (lt*r4)4Mj040.Q*mnmnU
Am 14W7
HalfM; 0 * *T: 1 2 * nl
7
0 10 11 12 13 44 16 10 17
Tw, mim
001000CmW
Exygen Research
Page 60 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 11. PFOS In Control Fish Blank, 0.00625 Hg/mL Fortified Control Fish Spk A, and 0.025 pg/mL Fortified Control Fish Spk B, Respectively
I *-- I-- M W -P FO t * w M n n W M M SM#* B i f t M
'W m p W M i *
intorat. c*s
A2 " ,- 4
A
i-^*i u j i*' S>!944*7-
9
11 12 19 14 16 16 17
TIm . (I
| PfD9*t((OOCQ)44M0M94OO m^h>*-urnP1*10 *9 9 061906947
t a i 71090 Munir MO. M T: 13 m
Infcrotr. cp
M n n itr.cn
1. M
1J>*4
60000
04
12.49
r*l
2 4 6 0 7 9 9 10 11 12 19 14 16 16 17 Tim. nl*
Exygen Research
Page 61 o f 132
Interim Report #IO-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 12. Chromatogram Representing a Fish Sample Analyzed for PFOS (Exygen ID: C0049478, Data Set:061605E)
cmmnmt mW WttmHMwJ*tm*w*m*m*}**nlltmMmi.N^9iumnmnspmHtM*sT IIA m i M IN C bW
Exygen Research
Page 62 of 132
Interim Report #10-Analysis of Fish and Gam 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
Exygen Research
Page 63 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygen Protocol N u n c r. P 000I131
STUDY PROTOCOL
Study Title: Analysis of Perflaorobutanesnlfoaate (PFBS),
Perflaorohexaneauifonate (PFHS), god Perflaorooctanesulfonate (PROS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small
Mammal Seram Using LC/MS/MS far the 3M Decatur Monitoring Program
Exygen Protocol Number: P0001131
Performing laboratory; Oxygen Roeearofc 3058 Research Drive State College, PA 16801 Phone: (814) 272-1039
Spotuor Rcprcseittative:
M ic h a e l A . S a n to ro
DirectX*of Regulatory Attain 3M Bunding 0236-01-B-10 S t Paul, MN 55144 Phone: (651) 733-6374
Page t aj6S
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
BxyfM Protocol Ntaaber P0001 131
DISTRIBUTION: 1)JaiMBhaKenii. StudyDirector, Waton Solatio 2)JohnM.Fliberiy. PrinopolInveorifMcr,ExygeRowarch
3) M ichael A . Santoro. Spontor R cpretentttiv, 3M C onpm y
4) ExyganRaewohQoilityAMuranceUmt
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Exygen Study No.: P0001131
fixyi*Protocol Nssaber. P000I Ul
PROTOCOL APPROVAL
Stady Titles Analyst ofPerfborobutaneeaUbnaae (PFBS), Perfluoichexaneaulfarace (FFHS), and Perfluoroocimeaulfanato (PPOS) in Water. Soil, Sediment, Fuh, Clama, Vegetation, Small Mammal Liven and Small Mammal Serum Uaing LCMS/MS tar the 3M Decatur Monitoring Program
Exygen Protocol Number. P0001131
APPROVALS
Exygen Research
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
BxyftcaProtocolNwobei: P0001131
TABLE OF CONTENTS
TITLE PACE--------------------------------------------------------------------------------- -------M s n u B u n o N ------------------------------------------------------------ ------------------------PROTOCOL APPROVAL-------------------------------------- ---------------------------------TABLE OP CONTENTS------------------------------------------------------------------ ----INTRODUCTION-- ------------------------------------------------------------------------------TEST M ATERIALS..---------------- ------------------------------------------------- ------------OBJECTIVE-------------------------------------------- ----- ----------------------- -------------- TESTING FAC ILITY----------------------------------------------------- ---------- -------STUDY D UtBCIUR.------------- -----------------------------------------------------------------SPONSOR REPRESENTATIVE-------------------------------------- --------------------------PRINCIPAL in v e s t ig a t o r ------------------------------------------------------------------PROPOSED EXPERIMENTAL START AND TERMINATION DATES-------------IDENTIFICATION AND JUSTIFICATION OF THE TBST SYSTEM SAMPLE PROCUREMENT, RECEIPT AND RETENTION. SAMPLE IDENTTFICATION----------------------------------------
ANALYTICALPROCEDURESUMMARY---------------
VERIFICATION OP ANALYTICAL PROCEDURE----------METHOD FOR CONTROL OP BIAS . STATISTICAL METHODS----OLP STATEMENT---------- --------------------------------REPORT-------------------- ---- -------------------------------SAFETY A M ) HEALTH-----------------------------------AMENDMENTS TO PROTOOOL-----------------------DATA RECORD KEEP1NO-------------------------------QUALITY ASSURANCE-------------------- ---- ---------RETENTION OF DATA AND A BO O VIN O ----------AFPENDK l a n a l y t ic a l METHODS--------------
........1
................ .3 ................ . . 4 ....................5
____ 3 ........... .
_________ 7 ______ ___7 _________ 7
............... S
_____ __ ________
.... .. II
.... I I ...II .... 11 .... 17 ....13 .... 13 ..... 14 ..... 14
. IS
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Exygen Study No.: P0001131
E*yp*ProtocolNuotar MOO!131
INTRODUCTION
The purpose of ttu study is to perfoon malytia for pecSuorobutanesulfooeie (PFBS), perfluorohexunesulfooatc (PFHS) sod perfluorooctanesulfonalc (PFOS) in " to . toil, sediment, 9th, clam , vegetation, small mammal liven and small mammal strum using LC/MS/MS for the 3M Decatur Monitoring Program.
Thj study rill be audited for compliance vith EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by the Quality Assurance Unit of Exygen X oasch.
TEST MATERIALS
Tbe test malarial are petfluorobutanosulfonate (PFBS). pcrtuonlwxaiMulfooatt (PFHS) and perfluorooctanesulfbaate (PFOS) and are all supplied by 3M.
PFBS
ChemicalName: Pcrftuorobutmeeullbnjte Molecular Weight: 338 supplied aa the potasaium salt (GtFS0)'lO Lot Number 101 Purity: 96.7% Ttancooca Monitored: 299-99 Structure:
PFHS
Chemical Name: PerfluorohnxtnaatilfimatB Molecular Weight: 4311supplied ai die potettium salt (CiFijSQjTC*) LotNumber. SE036 Purity: M.6%
TiunsilionsMonitored: 399-SO Structure:
Pafiafil
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E xyfra Protocol NkMobv P90CII3I
p ro a Chemical Name: Perflunrooctanemlfrimtc MolecularWeight 538 inppUed m the potasaiura tilt (CiFirSOjX*) Lot Number. 317 Parity: S6.9K Timiiriww Monitored: 499-99 Stricture
OBJECTIVE
T lx purpose of dut rtudy it to perform xaityaii tor perftuorobuJanceuifontre (PFBS), parfluorohexanesulfcnai* (PFHS) and perfluorooctaneiulfonatc (PFOS) in wold, oil, sediment. fish, ehms, vogMation, until mammal liven n d n u ll mammal aenan far tlu 3M Decatur Monitoring Program using the curent veraioMofdie fallowing Exygen analytical methods:
V0001780: -Method of Analysis for the Oatamtination of Perfluorooetanoic Add (PFOA) in Water by LC/MS/MS"
V00017S1: -Method of Analysis 6 the LMerminatkn of Perfluoroocunaic Add (PFOA) In Soil by LC/MS/MS"
V0001782: "Method of Analytic fix the Determination of Perfluorooetanoic Add (PFOA) in Sediment by LC/MS/MS"
V0001783: -Method of Amlyrii Ar tho Determination o f PedluoroocUooic Add (PFOA) in Piih a d C in e by LC/MS/MS"
V0001784: -Method of Analyst* for the Determination o f Poriluorooctnnoic Add (PPOA) in Vegetation by LC/MS/MS"
V0001785: "Method of Analyse Sat the Determination of Perfluorooetanoic Add (PFOA) in Small Mammal Liver by LC/MS/MS"
V0001786: "Method of Analyst* fat du Patarmindinn of Perfluorooetanoic Add (PFOA) in Snail Mammal Seram by LC/MS/MS"
TESTING FACILITY
Exygcn Research 3058 Rematch Drive ' State College, PA 16801 Phone: (814) 272-1039
PoftafiS
Exygcn Research
P a g e 6 9 o fl3 2
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
BayfeaPraocot Number r a tti U t
STUDYDIRECTOR
laianaha Kaaari P.E.. DEE Weaton Solution, Inc. 1400 Weston Way West Cheetar, PA 19380 Phone: (610) 70t-3T61 Fax:(610)701-7401 j.keMri@weatoaaoltition*.coni
SPONSORREPRESENTATIVE
Michael A. Santoro 3M Company Dinstor ofRegulatory Affli 3M Building 0236-01-B-10 St. Pud, MN 33144 Phone: (651) 733-6374
PRINCIPAL INVESTIGATOR
Jo ta M. Flaherty E ry y a Remateti JQ8 Rewarcfa Drive State College, PA 16TO1 Phone: (814) 272-1039 johnJUberty@exygLcoin
PROPOSEDEXPERIMENTAL STARTANDTERMINATION DATES
It la propoeod that the aoalytlcai patriot of Uria acudy be conducted from October 01, 3004 to December 3(, 2003. The actual experimental atari and Mnainatioa <UtMwill he iocladed ta the fimi report.
P trjpr 7 o f 6 5
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Exygen Study No.: P0001131
Exygro Protocol Nuocer P9001231
IDENTIFICATION ANDJUSTIFICATION OF THE TEST SYSTEM
The following s a the teeteyttemi for tbit atody:
W eier (groundwater ead eurfece water)
Soil Sortiment
Ffeh
C la n
Vegetation Small Mammal Liver e Small Mammal Scrum
The tampice will be ooilectod by Weetoa Solution. The eontrol a m p ia will be pnrdueed Bid prepared by tko la tin i facility. Purchuc end procaeing details Ibr (he control ample* will be included in the final reper aaociaied with Ibia Judy.
The tcet eyetane were cboeen to nceeu die environm ental im pact of PFBS.
PFHS B id PFOS in the Decatur, Alabama area.
SAMPLEPROCUREMENT, RECEIPTANDRETENTION
W ater, to il, eettiment, fish , clem , vegetarian, em ail mam m al liv e r and email
m anm al ecram eam pk* w ill be received at Baygea d ire c tly from Weeton
S o lu tio n . The detaila o f a m p le procurancnt fix t iii* atudy are: outlined in the
3 M w a rit plan entitled T haae 2 W o rt Plan for Sam pling Environm enui
M edia." Tbo mindset and typee o f a m p ta collected w ill va ry depending
a v a ila b ility in the fie ld . The total number o f te m p le t received tmd analyzed
Ib r each m atrix w ill be documented in the fin a l report ueocialed w ith this
atudy.
.
W ater, to il, ta d eedanect ewnplot w ill bo ueod a t received w ith o u t Anther proceeaing i t Kxyge*. Tbeoo om piea w ill be etored refh g e n usd at 2 *C -t*C . P ith , d e n i, vegetation end email m an n a ! liv e r am plee w ill be proceaed according to the appropriate analytical method (to o Appendix I). There aamplaa w ill be aerad Ikoeen at s -UPC. Sm all mammal w hole blood tam plee w ill bo centrifUged in the fie ld i t d a tun o f collection end the re ru n fraction w ill be ueod fo r the atudy. Sm all mammal return w ill be etored frozen t S -KTC .
The receipt a id proceeaing o f the tem plet w ilt be documented in the fin a l report end taw data aoaodated w itii the atudy.
P af4 t u f t s
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SAMPLE IDENTIFICATION
E i y g a Protocol Wwfct r . POOL131
Prior to analyaii, each sample wilt be Mgncd laboratory sample reference namber. The reference number will be tmlqe m l will distinguish each labaratney am ple dot is processed throughout the siulyltcsl procedure. Ctirrenstogriphic data will be ideatiired by the laboratory sample reference number.
Sample storage conditions sad locations will be documented throughout die study.
ANALYTICALPROCEDURE SUMMARY
References: V0001780: "M ated of Analyte for the Detamiliation o f Perftuorooctanoic
Acid (PFOA) in Waterby LOMS/MS" V0TO1781: "M elted o f Analysis for foe Detemtnatiaa o f Perfluarooctanoic
Add (PFOA) in Sod by LOMS/MS" V0001782: "Method of Analyte for the Detenniaatioa of PerOuoroocUnoic
Add (PFOA) ia Sediment by LCMS/MS" VOO1783: "Method of Analysis for die Determination of Periluorooctanoic
Add (PFOA) in Fish m l Gams by LOMS/MS" V09017S4: "Method o f A aslyte for the Dctcnmaatioa of Perfluorooctanoie
Acid (PFOA) in Vegetation by LOMSMS" V900I78: "M elted o f Analyte for foe Detemriaation of Perfluorooctanoie
Add (PFOA) in Small Mammal Liverby LC/MS/MS" Y0001786: "Method of Analysis for the Determination o f Perfluorooctanoie
Acid (PFOA) la Small Mammal Serum by LC/MS/MS"
The above methods we analytical ctmditioas capable of seperatiitg the iaonten o f PFBS, PFHS and PFOS. The teal report will include the isomen w an ed ieUototal PFBS, total PFHS, end total PFOS found.
VERIFICATION OF ANALYTICALPROCEDURE
A laboratory control simple will be wed for the preparation of fortified control am plea. The test whetance will be made into eolutioaa as per the method, sod added to the matrices via a micropipette.
For water oapfiag, Exygen will supply one bottle par sample collected. The battle* will be 500 mL pr e leaned Sci/Spec Premier wide mouth HDPS botdae. These botda have been routinely used for fluorochsmscai sample
Pat'9ofti
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E xyjro Protocol N w nbrr POMI 131
collection it the tatting facility id have been iberwn to be flee of PFBS, PFHS and PFOS. Sample wiB be added to oacb gentainer to a votanctric 811
floe tt 200 oL . A Held duplicate, a Vow field tpOce md t high field pike of each ampie wOl be collected. The low and Ugh field (pike bottle will contain PFBS. PFHS aod PFOS a well M perfluorooctisoic acid (PFOA) u d
U-13C pmfluorooctaooic add (*JC PFOA). PFOA nd ,JC PFOA m t included in tite otado usM to qpike the ample*. The result for PFOA and MC PFOA will not be nponed in fid itudy. Exygen will upply ene field
blade (control water) and two field blank pike (control water fortified with PFBS, PFHS and PFOS et e tow and high level) for every twenty ample collected. At the Mating facility, each water ampie (excluding field duplicate and field spikes) will be extracted in delicate and will Iso be fortified at a tow and high cancewnaticn with PFBS, PFHS and PFOS and proceatod through the described procedure to determine method accuracy md to check for biaa.
Far soil, wilmeot. clams, md vegetation, Exygen will supply one 500 n>L prccleaned Sci/Spec Prettier wide mouth HDPE bottle per cample collected or
a zip-eealbeg. An comaiBen/bcgiued for ample collection will be Upped to the ample location. Sample will be added to each container or bag in the field. At the leitiag (hcUity, each cample will be extracted in duplicate and win abobe fortified el a known canceuMtion with PFBS, PFHS and PFOS at both a tow and Ugh level md poeeacd through the described procedure to determine method accuracy and IQcheck for bias.
For m ull maacmal fiver, Exygen will (apply t 50 mL polypropylene eormtfoge tube. For m ull mmtmal lerum, Exygen will upply t collection kit for each am ple cementing c a n a separator tabs (rod lop), vecuteinere. needle bolder and needle. transfer pipette, and polypropylene tube At the testing focHty, each liver and sarum ample will be extracted in duplicate and will ateo be fortified at a known concentration with PFBS, PFHS and PFOS at both a tow and high level and proooecad through t i t described procedure to determino method icm ncy and to check for bias.
Low and high miking levtU for pact matrix ate defined below:
Matrix
Law SotUac U val H U Soteclac U vei
Water
50011*0.
5000 ng/L
Soil Sertimwt
m
C iana
mi/* 4nfo
lOnc/g 10 nate
40 ante
40 na/s
lOOogte 100 uste
Vegetation
10 aste
lOOngte
Small Mammal Uvet
10 ani*
100 ante
Small Mammal Senna
lOnsfaiL
IOOni/mL
fugulOufti
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Exygen Study No.: P0001131
Bxfjcn Pwtocol WioBbcr POOOtOl
Recoveries we anticipated to be betwem 70% and 130% of the fortified levels; however, the exact predaioa and accuracy will be determined by the analysis of h e quality control lamplea described above. A statement of accuracy will be includod in Ihe final report.
METHODTOR CONTROL OF BIAS
Control o f biaa will be addressed by taking rapreaentative sub-samples from a homogeneous mixture of each matrix from untreated control terapica, and by analyzing at leaat two lewalaof brtificatieM.
STATISTICAL METHODS
Statistics will be limited to thoae specified hi b e subject methoda and to the calculation of avenge recoveries, ae apptfcaole.
GLF STATEMENT
AH sspccta of fids atudy eball be petfixmed and repotted in compliance with EPA TSCA deed Labo.nory Practice Staadtrda 40 CFR 792. Tb final report or data package (aupplied to b e Sponaor) ihall contain a atatement that b e atudy waa conducted in compliance with current and applicable CLP sondant and will outline any deviatioca in tbe atudy from thoae standards. Thia atatement anil be ngned by b e Study Director and Sponaor Reprsentative.
RETORT
A final report will be peepaaed by the principal tavettiptor or their designer at Checooctailoo o f the atudy. The report will include, but will not be limited to, the following; a The name and adtfrem of b e Study Director, Sponaor Representative, and
of b e tearing fheiSty.
A atrtt meffl of CLP compliance (any related documentation, euch u chain-of-ouatody records, must be io b e study records).
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Exyam PtXKOod Num ber POOOl 13)
Tho aigped and dated (tatemeot by the Exygen Rcaearch QuaJity Aaauranco Unit regarding data o f atndy inapectiona and d ata findings w oe reported to t o Study Director and Management. A demriptioa of die exact analytical condition employed In the study. If the object method wai fitllowad exactly, it it neceaaary to include only a copy of the analytical method. Any modification to dua method will be incorporated into t o repot. If t o m eted ia photo-reduced, the project number and pageam ber moat be metoded on each page.
Dvecripfcce offee instrumentation used and operating condition.
AO reeuks fiom all M b analyzed. Control and fortified aamplea will be identified end to data table will include ample number and fortification level.
Repeeeenutlve chromatograms to each analyte In each matrix, including chramatopama of a standard and a control ample, and a chromatogram at a fortification level The location of t o analyte peaks will be clearly identified in afl chromatograma.
AO circumatancee that may have affected the quality or integrity of t o data will be documented ia t o report.
Location where raw data and tile final report are to be archived. Additions or correction to t o final report to l l be in t o tom of in
amendment B f l by t o Study Dimeter. The amendment to ll clearly identify to t part of t o report to t ia being altered and t o reasons to to attention. The amendment will be signed and dated by t o Study Director and the Sponsor Representative. AS applicable requirement* to reporting of study results si per 40 CFR 792.183.
SAFETY AND HEALTH
Laboratory paraonnel w ill poetic pxxt zulxjion nd health habit. Every m taw bi precaution (ball be taken to prevent inadvertent
export of penonnd and the eovinauoent to the teet or reference
jub*ttnce(i).
_____
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Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
E x y tn r m s o o l Number POOUI13]
AMENDMENTS TO PROTOCOL
AH iigndflc*nt change to Am aaalytlcal protocol outlined het will be ocpniMd in writing, rigned tod doted by the Study Director and Spoiuor RrpniMitilive. Amendment! usually will be inued prior to initiation of tudy plan change. However, when a change a required withoul auificiem time for the iaaue of a written amendment. Out change may be effected verbally with atqipoitiag documentation ligned and dated by die Study Director id followed with a written ladm ent ae toon at poatible. In thin case, the effective daae of the written amendment will be the dale of the documented change. Copioa o f the signed amendment! will be appended to ill diatnbuled etudy plan eopiet. The original amendment will be maimainad with the original atady plus. Any deviation farm tha atudy plan or from the wialydoal method a* provided will be documented and reported proogttly to the Sponaor
DATARECORD KEEPING
Raconte to be maintained include the following (aa apptopi iale):
Sample d rin g dwells)
Sample recb* ricorda, aloings hiatory, and chana o f cuatody H irto ry and preparation 0/ rian daid i (rto ck, fo rtific a tio n , calibration )
a DeroriptionofanymodiGcatioutothemethod
fo e tn m M w r a b o rti, bench-aheeta o r logs
Analytical data tabica
A ll chromatographic and inatrum aotal conddona
Sample entrammo and n a ly iii datai
A cotn pirtn Meting o fatudy penoaneL rigoatincs and in itia l! C hronological oraaentalinn o f a ll study nrr^wvVt . nT f
Anyotherdoctanatlrtjonnecessaryfortherwonatructionofdwatudy
C h ro nu tO fram e- All chromatograms wilt aw i the following: .
Sample idealifleadon, injection date, arrow or other indication of the area ofinterest, aod injection nambercorreapoaviing to the run.
Additionally, fortification will include the amount of analyte added and the am ple numberofthe ample that waa fortified.
Analytical atandard chromatogrami will additionally include the oonoentrahon (e g , pg/mL).
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Exygen Study No.: P0001131
t x y f m PtmocoI Number fOOOllJ 1
At part ofthe documentation the following heet will be included in each analytical let; t run beet Hiring tbo nmplM to betuniniiw set,iD din fcwBumcnt oonrtiriona iheet describing the instrument type end operating conditio.
QUALITY ASSURANCE
Tbc QA Unit of Exygen Research will impeci the study intervals adequate to assure contprimce with GLP'i, md will report tbe Sotting! of u d iti to die Study Dimctor, Exygen Management, end die Sponsor Repreeenurive.
RETENTION OF DATAANDARCHIVING
All hard copy raw data, including, but not limited to, the origins! chromatograms, worksheets, oom spondenoc, end result! shall be included
with the dais package submitted to the Study Director. These will be archived with the original study plan, amendment!, (Inal report, and all pertinent information from tbe Sponsor.
Tbs tasting ftdHly rail keep all electronic raw data and any instrument,
equipment, and stooge log! for the period of time specified in 40 CFR
792.195. An exact copy of tbe tnateriola anbmittod to the study director will
also be kept it Bxygea Research.
.
Exygen w&l obtain permisnoo from the atndy director before discarding or returning (ample*.
Exygen Research
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Exygen Study No.: P000I131
Bxyfni Protocol Number POOOl131
APPENDIX I
ANALYTICAL METHODS
VQ0017SO: D M hiI o f Andyn* for the Detenniaatioa o f Perfluoroocunoic Add (PFOA) in Water by LC/MS/MS"
V0001781: *Mcthnd of Aadyaii for the Detennination of Perfluoroocunoic Add (PFOA) in Soil by LC/MS/MS"
V0001782: "Method of AaelytU for the Detenniiution o f Perfluoroocunoic Add (PFOA) n Sadsnent by LC/MS/MS"
V0001783: "Method of A)wl)afa for die Determination of Perfluoroocunoic Add (PFOA) m Fith od Clane by LCA1S/MS"
V0001784: "Method o f Analyeii for foe Determination of Perfluorooctwoic Arid (PFOA) in Vegetation by LC/MS/MS"
V0001785: "Method ofA etlyw for the Determination of Perfluoroocunoic Arid (PFOA) m Small Mattonai Liverby LC/MS/MS"
V0001786: "Method of Aaelydi for foe Deteaninetion of Perfluoroocunoic Arid (PFOA) in Small Mammal Seram by LC/MS/MS"
Exygen Research
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Interim Report #10-Analysis ofFish and Clam Samples
Exygen Study No.: P0001131
E x y in PrmiKot Nub^mt poooi I} I
ANALYTICAL METHOD M W N M c VM0I79D
AM (T fO A J h m r
MtfiMlTMkvriall;
1*19RnMCJI 309 Driw
hriCtXDBy
ThOpM L a d * IC-hO,
I
7 rt/ f________
/ta M m s
Wlh MI.0t l I l l O ll p l M l l
Dm
Exygen Research
TmlPmK 7
P *#ttaf6S
Page 79 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
P ra tm l Nuoibw: POOOI131
I mu-inciu.wrrwun icamna
lit k M TM aM kkkai U Si H I _____.________ 9fMa*faDa>r<lCMAa)iBwar.
u MHr
Li <iw m i > i i . a a -- t a i i.
m tiiiipiw I
U1.1 HfIlMmMHiriifilMnaaa^<kKkmiiairaii^iii
,J * *< * " *< aO Unu laom
34 -- f lu -- M i > 1 iIm O ak I K cr a S i'p / l i l i a 'S r -1
**IN to kpoaua *MranOMO.
J l a n i k i w
4.1 - L e a k .
4.1 u ^ M i-a P L C p a a <J A a M i 4M a - 4 . a l a p a ana*
M
LI
1
LI L4 L5 L4 LI
LI
L L it
. ` P-V^t f k l
I 4 a l^ ltHHmin1-M0
>La-- H n.4 . H u -- >(L O m a o i.
**--*--h1*------i->---!- --a>*--rfn-<I --at 'imiajaouoli t.Ill
. . . (N M .ItU tM L
U W I W w . ..-------
^
iaLdwIVLCaWljL
. . 04>-UM|iLaM10-t44|lU.nk4jaMWatlfL Wwnt v hk Vk. < (1|) m i * <and4M.
fegt Hefts
Exygen Research
Page 80 of 132
Interim Report #10-Analysis ofPish and Clam Samples
Exygen Study No.: P0001131
BiygeaProtocol Nwfccr POOI131
^ -------------
IOMVMS
lia
1 U C-- im
*jnniag >0sal polypopylona t+m m3000tfm.
40 O nH H |nvfekl)M i
41 FliwwKKK> y tc i rfk ), U --s u kwm.3.
CMtosaMsn)
4 2 T m illi W C 43 IfcW iW w U ): la U M B A iM iiD W a M r
44 MnMiflBMB): IM ml
43 (M iw N vB a:
2M iH 40 !4
40 340 2J
&A 03 03
23
03
T*m*m
3U )S 41 31 42 73 42 73 0.1 33 41
4* fc^ifllM VafcMM: 1 5 |iL ^ * b ii * w 4 l e * a w d ie 5 0 n L k 4? uaiaMC )takA f*-tanlataM saA M lfaam rv 41 -O wkmn
70 7.1 Mod* a*ee<piiyH iew hrtl*W B 0de.w **iM i3- W e o .
to
14
41
MsU oMm*
4M
B0.154 y of
AlHnMvolwninaybo
Exygen Research
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Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygeo Protocol N--b*i: POOOl13!
I .................
iM M
tfULmCALMmiOl
I
Acad(PPA)i i Waw Sy
10MM49
M ta0w6fc*p--M
t l % U f ep fMm ^M^MM--* WMlJCa^MH OMO h&rmp Liiy*)RMfOdAilM*ywM<ICh<OHwWl
#U AlmOnib^iltUtiMliMlliMiilwMfiBWi WOAfa*mn4ybrfaynW
fU 9 '4
AAiai>LLBLtlprtltSffujfftttaiao*a*LLl1lIJO0AUUMDp--fMMafiJNL*mat*f--.Malt.MhiMlifecMecttM*ItMenaefft^ami*OduOAwaAhfKawfparweprpteaO'[*frOe*1tdO0Vlwtyywfffeceid--nfMretftwi*ra^ndMwtilntwwo
f.J.J tAtOVAtipU^ ML to fMa faia ii MfartU t f PPQA i pnpand hy tnafiag
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Page 82 of 132
Interim Report #10-Analysis of Fish arid Clam Samples
Exygra Study No.: P0001131
Ey(BPiotoe(Nuabcr:T000U)I
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Page 83 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exy(t> Piotocol Number POOOl 131
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Pogr 21 o f6S
Page 84 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exytc* Protocol Numb MOO1131
nfim .it
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I ............................... h ih . o l i B P ~ ' 11
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P <*f*22of6)
Page 85 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxypea Protocol N um ber POCOJ1J 1
AuNA+LYiiT\I\C^ArLMvoEoToHwOiD
lomud f A a y * S r * I W r e f c s * * m r f l w m i e w i AW < f f O A) S e i b
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7 Pat*2iaf6S
Page 86 of 132
Interim Report #10-Analysts of Fish and Clam Samples
Exygen Study No.: P0001131
Exyfea Protocol>#afnNr P0001 1)1
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7.
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Mwto^WAUjXhrto&afcttoatoroahiiM mu....... A^(WOA)S&,ity '
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L I to ft?
21 Vay ilwai<| Hn-wryjrmtaai
22 Cw--fctoM fjflw IffflftoM H M aM tofftyrfw ralfcrw oporiafcir
21
29 im$m mm* n*mm4 *mmto mum ^wiNwa ie m
24 AMI^hiwin
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fmI S I -- f i t w t o atiw i y w o i -- r J t o q p w tf M t o i m b I m h a to *
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22
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24 W 0 .lh f M 4 i> itj* n ijtoia ii MM* tow ,
25 ttw L atow H aH lftoM w >iitofcMtoa
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25 DMpwtotopipWM.
214 4to|M -- (1021W tf. 4 12IC0 U to* Hito tola %
211 * t o M >afcVac! w (10 i t t l s n i-- lfrai
212 W w w w rtill
213 U M t o
Exygen Research
Page 87 of 132
Interim Report #10-Analysis of Fish and Ckm Samples
Exygen Study No.: P0001131
E xyfto Protocol Nuaober P000U3)
iQMM^ l i e aiiSyUoffirli~hrtie Ddwwiliii^eita^
AoQ(Pfflaj w od T
1.34 vtotmimm+m.
US 0--
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Page S o fS
Page SS of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exj|60P itte d N w ter PQ00111)
I *mLwmurooi
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t.M A ftl pg--L t e i d t e -- w--i--d ffO A d p ------ Oyhrw-- t 10
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14 f 4 1.1 iqtaL n W m o Bad m ICC w*h
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Page 89 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
h y y n Protocol Num ber: P001 131
faMakM*
MftoCMMtoVOMtiai
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)
ktoMofAMlsiebirteDMntotoIRCaAfPttMvdSnaMCtmaieA^caTOAlBSoilbjr
l2 J A a m amtoad t o t o i haapat Maafc) a m M jn B a c ii wto arfl
4 2 4 2>aaaltoaaaaiaafc to a ft haototoa to 1^-mL
fto a
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U i Ahaamaamto-- im aaatotoiaaa Waaaotoiia m y to praynad a*
14 to * * 5 * 1 *
141 aafc NM W aplaa M k iM <lypfcOy t t or loaa) m e nefcto katu
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ta n a aaM tottoa 0 * : ul i j to vanty
142 l i V * a m to latf m i katonarym tatm m i ta r ill to maciAto
totoa |a illi]i na maini p in to to o p w to x
114 l -- li C-- aalii a
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1U MMllattoa(haaat at mi<tfiaaflt*toQi.i
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Exygen Research
Page 90 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E x y fcsP v aK M o lN w n b er POOOU31
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Page 91 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxyfeo Protocol Nunbon P0001131
i.'mTTioaittnw
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Page 92 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P00Q1131
fa U C tft--MoOl--*IT W00II31
ANALYTICALMETHOD
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PanMofM Page 93 of 132
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E*y|CB Ptatocol Nunbcr MOO) 131
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Page 94 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Cnytca Protocol Nudbcr POOO!151
e 7 M ^ k ^ k n u M^ iy u MidkA<u(iP&u:. v s n a /m
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Page 95 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: POOOl 131
E x y in Protocol Nurobcr. POOOl!3I
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Page 96 of 132
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
b y * Pmoeoi N ttnber MOO) 111
M itori a fA a tliritte rit 3 -- a ria ria a c ito lto ia -- ao k AtIOTOA)la Spinat o iy
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Exygen Research
Page 97 of 132
Intend Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
1Exyte* fiotocol Number FOOD1 3 1
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m to m tim a fto to fM to m m * * * . to t m m * tfto
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i t o d t o i W N l i r to wia* <w Kuri
Tto aar to atoM tow to aatodtotoR of to >dferiiLn
iMtoMMdtoatoRHtoifi to` wad --tow af irtRRil tototto * tto to * to m to
m lklH!OMil9ii<i yaS*j*M ^*~* gtoBftttwwlli.--a4w1i ftcoSnim a u iia m . art da
aatotoa* toRiatoir afaatoplHtoiaU to aiM lynd
tolin
Exygen Research
Page 98 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exyjea Protocol N arcber P00011} |
lamna
iin momnun
ll thitan* witfuA
Ki
mmiMiMt*
MM cfffO A tM l (
IM ri^iyM LfwN vwnpNfn: (Mn rapnata pcnmmraj
m**m(wh**-(H*
ET - h r k r t M l a Ml
IfM M TL
,t3 *? **"***1*1--I--"**f*to*m>m--lt t*m**0ip* p.riar to U M , m
>winm r(M)-
........... ***' * 1tofcto<towimt<MtolUt
144 VtdPVfc *****>-
WMharfto^Li. torto#>(si>
M4 V** toiyiagf--ni l wkatotodtoi--tfpro* b m l m ip k h m im * y w & t *M * * |a* > > * )* y --^ W O t to(|tot ) i[IIIOHHiitoliltoM|
riwr
Exygen Research
Page 99 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
PratooslNunfacr. P000I1)1
AlNAMLYITMICAcL mvtbotshuond
ACbMkjrLGMMW*A t a M * t A M t * W* D M n b * a r f M k H M u H l AaM f f POA) la H *
/nrfyn l T fa FitiBly.
> w l-- ll
tMtKMCX mAinHMi OWlvM I
A>pmn<S)c
Tm^crjmH*wh>.LCC-4tlt.L>p*i>wwrt
/
vQ_
2J& '
&
L
Exygen Research
P < w 3 7 a fii
Page 100 of 132
p. 100
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bx>aea Protocol Nwnbcr F0 0 0 I ) ) l
I
im u rtia lig n w
........................... "I
. OntbrUSUMa
iMnrlUUUaiiiUalil
I imitmMau
U * *<7
'
I2t2 CA*latonn>i >flWnalpiitlMMaMn--TO) M|tfMiwfctaMfc^<iiycMftKlfcrprayia<ty
3j0
ttte y ie . ffceteeiaeptecui * U a few ter c e te e * *
^ I m mp tei lima f
iiUfitWidliteiMfc||te fetki
co
Cl w *r-V L C te e O > m iiW i-P IC te 4J --- -) C4 Hifea.l-lLCi*
PlpWI(PMMnMlO-fteeei|
C7 M t e i l M I I i - K N f M H 41 1 P-- il-H F L C *fe
10
J.t A M * afen m feJ t e l U Cf t e capate te p m * * ep 2
cteMMfrippte te li ateUMa MkM tef*1*1tebte te tteateM 5-20U jrf.*a e tw e *fc a M M S pem e* (L C M lfel).
3U1 aptetete ntetep e COOOO] #
/*rt|fp J4 t/OJ
Exygen Research
Page 101 of 132
p. 101
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
B w n Proooi feafecr P000U3I
m ncA iittT M tt
llium iiuk l
OMlylOMMi
<lh!&A}k Attk mu
UM 151.497 ftUllHNl r im jb m (SQ.KP*, U300IA
1111.1 li M U T l M M t a t l 3 aLtar WtC vWUl
ITT
113
H1I 1K1I
^^*^06^U(S^*eML*.N637171). fWfc|>H| <Il mLrUyfm+ytm.a*m2000nm.
40 CkmMOTMsSMB
U 7M9MME *c
M M aHw(A)t laM A aw M A M i i i W w AMwmI
O nim tofiK ;
D hlM I
ObO
14 40 KJ
fli
TU e
49 29 a
49
JWvftMi
*1 SI 1 SI 11 TJ O 7J i l 39 1 )
1 1 m**y*km* li$U'm\m)aammi+mw*+nul).
IT QmmM mk *------- ----- -- ...................
U Km T* -21 mm.
Ib*aMab**4*waaWtitLiMC*imanm
Itiidewieeybse*ee|^*ei*rle
Exygen Research
Page 39 o/63
Page 102 of 132
p. 102
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygm FiMacol N u o ta r P00011] l
I Mamau. nST ______ ItaoTM* e/b*ftinn.iwau Ai tm W > M u ' mcM wn
rt
7.1 1-- T J Ilf ' i n u i -- Hi.
tfO K
tH tm ntK
LI hlobOaRtM
aiwgof
L3.I L2J
3M* --fcaJttttaLMtffMca *X
iifeptoarMr4Mto*to|2|Mmk mmmM*mnmtmkmpfn10*"m*Lfry Mtomm,.3n i
*?togato.
M 94
144 P lf M ll
r f M t a L af P P M by i # 10 a i
** g ig . 1
**" l 100at. w o
t.tj A
H M m lw n M Im f PPM a m n >n^H :
L U Ah iLUI MlaML.lLoftnifcMa iwi. M n rfryO A It w to to , 1
i W mL U M M iWW W IP to n mton oflOOwto wtoa giin
L M A LOI ffeL t ir t i lw fa ti W MQA b p n y M \ y br**
LU
"WnaIrri`kflIVLnILMUteML MMinLian m u* flan
w h w f IOo TaA
ta
*"" I***"<
Exygen Research
P af*O o{ti
Page 103 o f!3 2
p. 103
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exyt** Protocol Nuabor XX)1131
c WaMafXaoMfeftaMamaaiMaaMHoTUfMICST M atyLCM M a
12 --irnJOiiOi lim n I
9ZI LOMMSaMn
9JJ DiMMiimipUi
My k
JMItf
14
"
lu"
gU
------W-----Itt
0413
14 14 100
041
11
It M
11100
00440033
0401
2ac'c,** J W u M E 'CaooClbNl
X d r t r t i nay to anyone
IM M k t ) Iftl EtAkldiofa
Of Of k n ) B M k c k k at laon
w i l c M M M teen
*M m U y yoooofaal n o am y ko bo k d t
ik b lC Mr M . m m a i k au > -
JU 53U
I- A H X alX M lM lk M
11U3 t m dkMi kKi k. ti .kWw lki ' l l
It ,. C U t a k a l H i X t a i l a f M M . t a K a l X M c k k Dloanf onkoo. Do m i Mo Cm M in t a.
1 1U
M k M > y M aa.iqkiM a), Dty kc Mfca conylacty hobn t a M W **> kl e M i w m ofaiwef
Siiai
H f Al e f t s
Exygen Research
Page 104 of 132
p. 104
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E*ygm Frotooei Neraber POOOU3J
I ____
MALTTICaI MJCTHO
|
IWftftftAftnftfci35ftMMnfttftfftmmiiiiuAcft(fFOA)>criitd
CftnabyLOIOrMS
1 -I1.T CftWft-- ft ip mLpftftw)<n i *mftftftM ft -- l*i -30Q0 ifm .. W - M o f i w
U J PiiftftnftH lM dK oftfftftJnlH 4i^dftnkft
fcw-. . ftpOTtaH* M t COM ftIH loft 139 ML W M M n tfu ft 1I.J ,AM 4 mL f MftwWft ft ft H ^to ftimftbr5'tQMnl iIm--+MwiifAi ituWm.
.. ftft-- fta ftft II! ftunoftofliftflwM. IMO > W f t H | l f t f t * l l i f t w i o i W r t a i f t W IMI n w f t f t l h l f t l H f t * t W f M N . IU I Cnariftf ft f t m i ftfeynyyWn Wh aftftaft npft --3000 ipw>
te-ltPHM.
IMJ 0 l M l M I M O t O M l ) l o f t f t CtlMl ft MU ifll 9 h m f N N b H if tk ft nWbiM W ft ft Wmm fron ft muM
UJI h o W li< M ftftftftM ^ ftin h w W n H M l ftiiii
IIJJ A M M ftw f t M W ft ft H M ft * iHTftfti* lk ul . iH ftU W iftIfW IlM ifttiftq fWOiif t i (P <rO .
IU I IM ftft ftftj H ftftft ly A f t | I ftL f t 3 i--w til icft CTu ftH l ft li| W f t f tf tllf t -- ftftM lI'l.
l U t tW nlftftHft H ftCftftM ftgtfftanl>*pipili l u t n--f]n -- pi w n ii u m iin m n
!#*
ft f t ft iftM L wfth ft fcftft u n fit iw ft* A ftftmiM Hftnd n i w l ft ttfev a
113 l4MlMAift'PfO A am ftW ftcisiU lfr vn eH o w n H n M ilm U ftftftM ftilO M W ftM .
113 An n n i ftftW --i --ftrft-- iftftb ftJ u ftk p w iH f ts a f t f t n j4 n i f to f t n f tn W f tt--p i H f t t a m mrnryS-I0 # ! A f t n f t i m f t m f t M ftratin i m m w m t w
f t n hntfta W ftnft m i b ft* H f t M i f t j n t m in
JU ftr* e ft|n ly le n enftfce ft n IA f t * l ftpw k em ftftnfcnftift--mmtiMac nfcf M n ly M fcrnow*)
TviTF
fiag r 42 0 f6 i
Exygen Research
Page 105 of 132
p. 105
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E u y tia Protocol N um ber POOO1131
*
c
MtetOfeaWteoCIvt)
A tu L tn o a ta m o k
ICrwOiin-HMHAad(rFQA)^Ftfh^
OatebyLCMIfta
A*ylamyMi **
t teAflterbObiteMdnmtytte
JSJ ,M iynCM W >
IU ChMMBfMimiAntfttk.f*fca^avto34*antow*pttmi
i f 4 U M Ito 413 i |iw t i i r m i r t > ffQA m m . wfch to
(12 MItMeMslktUelrItaMMi*ni0iMi4mlliMmlaiMa)imlMM/mmilmaiM9laMNtlloMhllhwrtMaiiMf(Bt9eityKMopaM>ktor,*twef*eiw.i*LMOQw.vVi
111 lkMVtllM y><--
Minute mnnbli ftntoto
ftotoC H i*toM teii iteiail.
134 A ay m t o tm m M tm ti m te M to M Mr by <M tbs Hu*
torn TMi ar te M M Am to to n to to f to iibtoiM wvr
D m , t o M l M r W te U M te tew to te t o i omU te tctadte
UJ ateteMtettbTteMlateHi*I tJe$ 3 i(pKiI*iHttiJiUm)t.t Vd m <fc> t e
1M *4%
HnMdmMmdhbcMcudiM<Cm iuii
ICI
PM*hm t MMI.)-
Ri OrMMnbiMaMlrMMbimiMaiNAfcMrbMklo
m u w m .iM u --
DP-SeWbyNfl*MMvMfwwaiMd.rm uq
Put*<J efi
Exygen Research
Page 106 of 132
p. 106
Interim Report #10-Analysis ofFish and Clam Samples
Exygcn Study No.: P0001131
Baygm Protocol Number POOOllll
___ AK*LyTlG%i.JttTUPP
toPwootobwaftoOMwoetooicAt*(TPbAJiePifeMrt
" ofcylCMMtft
lO tNo(iaoptotett*ot*lMwto*eiOOeMdoa^MeeQeirimeee)Avwpyf.crMncngK.M
iM o w yM
<(*!> iagi!WBlir)
Exygcn Research
to**
F*S'44of65
Page 107 of 132
p. 107
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxfto Pnrtoool Noaiber: P0OO 131
ANALYTICAL METHOD M M N n t r VO0OI7S4
V ipM iity4irthmniwitta a i t m # AcM(rn M l ii
Im nlM iA
mI--iHICtmllrinf+>Ar*K*KM
A* ***4Br
C -iL
MCniiJy
1
Lm*.L04O, tmmak
j Og ^
Exygen Research
Tmva: ?
P a g t 45 a f05
Page 108 of 132
p. 108
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Eftypft Protocol Number P0001131
analyticalKcroo
j
Xmhaid Amfrtortor4 flu -to mtriAio/ia
Ad4(FyOA) V f *
t* life--MJitota 0tomtomi--<L1C1MUM*UO)kOv^nMMioaf ^ M pM to 4 --tom 1
1112 A-in)MlMnHbMe-M--g-nip
it fcrpttpwMtoiy
II K>f mwlll
13 t --ftoatomid top*--4 toto--oto. Ptototor lw > wmu
to4totpoan--<tomtiotot--o mtototoM--tpototo*--ytoJ*p iPttooMalttoot*Nttoorftcoka%fmeiMtouohcaito
`" ` - - - - -
i to ftm n m m m m ii tin of
U
11 Wtoto-VtCpMto
42 AMMto-ifflCfyi
43 Ctoton{l30>409Mitot-lM^tp4to
44 Mto--a l-IM C *
u45 W m p k j m m m * * - -
-
i t a to m toaito p to p f l to to i -- to w to m totoM v # to
1iw i--f in to-- Urn wtg.0O4tf).
911) AA--toatotocttototoml----i----totototOo*r--|iiliitobi|dnloiiuintuito<
Pag046n{6S
Exygen Research
Page 109 of 132
p. 109
Interim Report #10-Analysis ofFish and Clam Samples
Exygen Study No.: P0001131
HxneaFiMBOol N u a d x r P0001131
l inm-imaa.
' H n o(lNflL wnrn. nir >Jl|pyO *| *ytCM M
3.4 RflM yfM paw. l i L iiw M U lb ta. 54 JQ aL4i*a>*to>oljpvon4aB ea****"*. 3.? 34 fli p Hi ibIi i|i|i > (3MBL WMOO^L), S 3 U3m LLW1mbii i m u + k u * m
3.10 i^ te x n c v w u L S.H PfagniMi pppirfi.
SA2 tlM SJ3 OPtlOnOft f ) ffcp il o*.-37177V 114 3.13 C * lfc eiaF eH ld (v * ^ B < * t.0 eh iP * P l* w "* * M 0 0 iP *
trRMptaa*t f <K#yaaomScianMc), l.l Mr t SCmm. V JMfc 33034831303
44 T a p a M E 30*0 13 1 aM AanMkM Am m fa wmt
----- :
Tl
03 14 14 304 84
Flawfcaa
&A u (aLUfti 43 33 04 <3 3$ 04 8 73 04 8 73 04 43 33 04
7.3 M W SlyftM
7.1 Ma4ac ffiKBB^n) M^nhK kB44 coda. ooiM ftn 13 - 309 a rt ft PFOA.
?mt*47cf6S
Exygen Research
Page 110 of 132
p. 110
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
C x y jn PreMeot Nwnbar P0OOI131
I
W il t
i l i *bU.YTICAL>nrniOO
I
a r > 0 -- i--I w
i A4 (PPQA)ic V tm uhaT
jrLCMIMI
a * b a a M a m <w ]
la hh b
PHpnteWliWHi
8.1 IWbM
4.1 2 Mi
U
lOMBLrfwaMr.
0.154 I r
44 l%iee*teMi8imdMeliipNpOT68y*ewMaf2|efwwbir
aMfclOOaLafMtaal.
i l l --<ntmm--ytey^--1 10
94 lari iliOnrtlllMn till! Iii
9lf*l00HW ,#fm>A9ywiieNmlOmg
Mnnaad iat parity) wri e 100 mi w >
lik llttc L L D M M k
44 Al0|^W .fcnHaUi U l i i o f f f O A . ^ ^ b y ^ ^ t
mL*f O* 110&m L a U a M
eflOO vi* m M
hilK aL U fllaM i.
945 A I I ps M M C 6 *M w M aafP K > A ayR |M vdfcy triaging 19 -- -------------------- ------M o llili
( L U ftM i.
944 A101 pgM, M A mcm aaMaa af HRQA mpNgwd %ybnajpog
10 1 TO* 11 j# * L iihitM it a final vatana < 100 vt*
ta ik u lS im P IM fc
94.5 naM fcafifatfia*fefiiaM fiM a n * * Mai fcarafttianaflru
n MMs * r m i m ftrtU *f I u n k i
94
at11.0ftoLMS M ,hm n h94.1 IQ IC H a l i o f i l a W h id -- p w y W b m W ria rito n
P *tt4iofU
Exygen Research
Page 111 of 132
p. 111
Interim Report #10-Analysis ofFish and Clam Samples
Exygen Study No.: P0001131
Exypea Protocol Number P0001 111
[ 4VU,YliUtmnMft
ht o adof *aafr3r 4 g to to M a a t o rfH f c n w c te o ii AcM(PfQA) fa OyLCAttMS
fZ. |(1
tommyte
LC L9 4tS MM .I
-- m ____
TT--
IS 14 14 10
10
TIT------ -- Ha Ml m Ml Ml
T 8 "-- MU Ml Mas
MBS OBI
___ . . - ____ 9H____
nytopnpm dat
m M*
IH M k
1 QjfifMfiOyto20M at toto) mMm Mrndm mtotwoann
. ilapto* >rl f i t o wl wpawryfcrdwb-O
fat_o tortoftowti t e iato t o t o -- i bifliiaaaa ato toa til te to d M
11.0 M ito te
11 1 T P # I f * t o * M tola JO mLM M * aaaattto toot
(M iy aam M , M m V i t o t o MQ.
I U A d>0La#ftw toW totoM gfteeftw neiftetoi*etirr'15
I J C.MftSto toi IQ t o patete )*-- M aao o aM to amate -*2000 rm
A r^M M -a.
1M ! M to a M to t o M t o M t o M t o p a m M ^ M ti .
11J ftafc to t o m a to fa
wte 1 ^ fltol. 1 1 toft t o 2 I
atto t o 1 1 ICOtfc. Cr ullf to t o -- M i IQLof a to -- I
aa 20t o ramatola, Bt o r t w t a Da -- fate to tornita
to ll* M a a to 121 t o y t o y a * Aaaka ty rawaf wife to Km
*HfeiMiaUaaaallMtoaatotoM. Rumto Jhafcwtonatoa m. t o n n i ty atoaat (Ma tern). Pay t o flato nia^ltoy M m -a.
to r ky* * * e e wi*s a b * aftoagm.
U.7 O a a w to to al a a aM tia M W aM b taa to to ftto n M ttb a ('
a y a top to Catea to atoia Into I2SaL tontea* paartop*
fin g t 49 afS
Exygen Research
Page 112 of 132
p. 112
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
BxygeaProtocol NvjobcrPOOOl 13)
I
U n til!
A \ti vtW'aj m m n
I
tffL---irnnrtirtT T i Ifru flu n m -iu n li r i l l fff*T rii in " n iia in i
11* Nd30taicfiUicMtata4ta--|taataiMtaUtairttattan
IIJ N W ta t-- t a s t a t a min m fw datar.
11.
Hit
NCI -**t*a.
L
tata tacitai t--pta n WOOiy
U11..l0l .I mIMn^atplutaftNacoim11.i11u** ta
tata m i
MOU-- -- IIW q fW ||IM lt ( M r O
11.14 I
II.U
wl-- H a taLofa uctata ctadio tanni a MudioMtatataMtaMtac.
It.14 lNtatapc)rtCM*MB
12.1 lL|CMMMl|w9a
Il
03 ItaltadirftFOAwtatapdtaftaCitaMtfotaB
12 -- TW ta tU ti ta *tc tly o il i l
,
J Aft mm m cf rum i o M m uwU mm U taihtaotf tw
MI Mtla4nmsmmmyHfO aammpplleiliMAL fuBcittuamtMi t--otai inmtimcmmahrt
d atatatataa mattata m U Notai ta ta Ngtatai *f m
(tao i N ktaOtatad tahNitcafimmitmanmWtiatdattatdatatariiwXphm lmi-mmym3 -1.0w1 inwta
la tac tata mdtataNetta ta ampia m
134 UN I vtamrtaa*itatalytalpNtari
citai l/i --Igtatat afpota a--
m a g n a ti y 13 (ta a y tinn
a d tata teak de dtaNaar ta ta Ml a m Acni i parati 1413 > . I ta 41J a MBVfsa ta tac FPOA taon, Ita * tastar ta{MlaaNvoftanotaIta tafta
PagiSOqfS
Exygen Research
Page 113 of 132
p. 113
Interim Report **10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
ExytProtocolNumber POOOI13 1
kfLOMMO
UJ t W i M M l n a a la m 3A * kvii p x a k o UXJ. u .
IJJ
Mb*iMvWiOAlmwttai wmm to0J I, m* H)tnipM
atnooto i(M W * mimmm
m m to h i iv i x% f
aakM antat
fcUanl> <4. . . . ^ ii>Ii 1W .a
IJ4
rnhmm rfI--pi a>a 4 m Tl 4*1111 A tj l M a M W M t ! 1 |1 |1 I o u t e t y * U4 Ha*
.>.n..t.T..W..,.m..t.t.k..t...A.rMfU"m tm IwAiiai rfOa th a ia i o t
IM rnmmmmmt W r tiwl iMtrrf
a s m (K* a N s ' i i l M
1J4 *kMMM M a*4 mmln M m t drift dm 4m
4 K * a a ia * * M > * . Ifm u a Ka i drift am *ft*itk li4i0! - 4 < W a Am At M am tta a a to ta .
I4J IftA*a w n . .. nl4ai fc.ia i.im l PfQA faa* tk a>l.
(miMtmMmb*rfe*aaMmataLAft-a M am (Am*> an paaaaatj
142 UnmoAm -
m xrnm itrrt-Q
14J apta M ita IA ta rn aaaA A 'fF 'O A pw m u * , . * HOmrnt OfOim M h A . pao al M M>r.
way(41)
taal^AaAArtt - aata,A4 i.-- lMMl
aart)CMMfi*g)
Exygen Research
Page 114 of 132
p. 114
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxygra Protocol Number P000U31
ANALYTICAL M BJHO D iim n iw tr vom )
H inilUnriyIQMMi<>>!*> + tm m w im tm td pydf c w n f a h a m .(TTOa ) 1 -- ii
im
Anafoliri Tw df Fuilqr
.
S qiM teM l
nim >apiN
Stw Cttbp. PA lJ
I M M 1 * 1 * 1X40, B rrtm Kmnfc
gA 4L -----------
I'tlnlM taiO iata.taiilaiM l
illuM .
-D*mA A
Exygen Research
1W ?VK ?
ft| J2t/dj Page 115 o fl3 2
p. 115
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E l)te Protocol Number: POOOmt
t ._. . _
14
x--* n m * vmim
j+uMcALmtitebo
a'
(vbjLCftW M l
----- ---------------------------- - - - ini
i* %*r iui *> hanktlfcrpropn *W*y
*J-1l ............................ ...
PUk i W
M M pv4kna|H iM iA ]rbi Nm ^
Ud m i 9km *
W rnm km
JJ
tkmmmjmikmmmmk IW w iM itiH
fl
pUp
for dM
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Page 116 of 132
p. 116
Interim Report #10-Analy$is ofFish and Clam Samples
Exygen Study No.: P0001131
Enyyao Protocol Nuatoer. P0001 )31
mito il
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Exygen Research
Pagt}49f6i Page 117 of 132
p. 117
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygea Protocol NmfcerPOOoi !3 i
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Page 118 of 132
p. 118
Interim Report #10-Analysis ofFish and Cam Samples
Exygen Study No.: P0001131
t a r p o Protocol N nab tr W 001131
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Page 119 of 132
p. 119
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exygeo Protocol Number: POOOI131
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Page 120 of 132
p. 120
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exy|n >mcoot Number POOOU31
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p. 121
I n t e r i m Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P000U31
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p. 122
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
B x y ic a Pvococol N t a b s r . POOOl l i !
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Page 123 o fl3 2
p. 123
Interim Report # 10-Analysis of Fish end Clam Supples
Exygen Study No.: P0001131
Exyjea Protect* Number P0001 131
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Exygen Research
Page 124 of 132
p. 124
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No,; P0001131
S X f t Protocol N u s * : P 0 0 0 1 U I
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Exygen Research
Page 12S o fl3 2
p. 125
Interim Report #1U-Analysis ofFish and Clam Samples
Exygen Study No.: P0001131
ExygM Protocol Number P0001I3J
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Exygen Research
Page 126 o f 132
p. 126
interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
Exypra Protocol Nttebcr POOOl 131
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Exygen Research
Page 127 of 132
Interim Report #10-Analysis of Fidi id Gam Samples
Exygen Study No.: P0001131
Bxypts Protocol Kimbcr: P00UJI
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Exygen Research
p * t* U o f65
Page 128 of 132
p. 128
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: POOOU31
Ewgen RESEARCH
3058 Rawareh Drive Phone: 814-272-1039 5to CoUatt. PA16101 Fa 814-231-1580
PBOTflCftAWENWEIfr
Amendment Number 1
EWecdve Date:. 01/1WW
Ewnon Study Number P0001131 Ctani Study Number. 10(1
.tea.
DESCR^flQN OFAMENDED SECTHST 1) Analytical Procedure Summary VOO0 1780;Section 0.1
2) VtrMcalon ofAnalytical Prooadure
AAgwhin'ro
1
1) Addto Secdon 9.}: Section 9.1.8, Aftamele weights of atonttonto may be w ed to
prepare altomala conoantnalone cfatoch aotudona m naoaaaary. Alternate levels of
torfl8ca8on aoMkme may toao be prepared.
2) U re a * high ipMng terete or the analytaatoreach m atte may be M end dependtog
on sam p to ^ mwfabla tor extreotlonandtor to corer analyte ooncanaredone expected in toe aampiaa.
----------- -----------------------RAfifriAH----------------------------------
1) Htfror ooncaatralona ofstandards naad to b t prepared to order to spice tha sample bottles at NghartoMta.
2) The eample aha arelable for amau mammal Kw and aerumwaa amaSerthan a^actod. Spfangattoepre datamdnad terete Intha protocol puts toesptoed eoncarerelw i lowerthan the detictlon In. Aha, tha analyte levels In tha ground wafer sampise me enpactadtogresdy seemed toe prmdstamtnad spiking fevefe fated In the protocol, toman toe terete totoe samples greedy tw eed toe spWngtewfe. an accurate reoerery value oamolbe catotitatad tor toe QC sample. HgharapM ig terete to toe bodfee*41 corer toe analyto concentrator expected in the
~7~~r~rr thsessesje
TheLOQtolOOngffgferaO.1 g s ta lls of smalmammalb a r and to 1000 ngtmL tor a 0.01 m l aanpto of amal mammalarum. Hghar lewis of tpldng tor toe vwtoraampiaa wtdansure toat more QC reoorery data
O IA b9 U M d.
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Exygen Research
Page 129 of 132
p. 129
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
3031 Rateare* D rt*
P tnar 014-273-1039
State College, M 1(001 Fee 014-231 -13
Amendment Number EflecOveOrtK Exygen StudyNumber
PROTOCOLAMENDMENT 2
(&07/06 P0001131 Ciani StudyNumber
H e e le d None
BESCBgIKNOFAMENPH?SECTION
1) Aiport, page 11 a t 6S 2) TactMateriato, pape Oaf68: PFOSkaneiOon monitored 400-> 90.
A M EN D S} TO 1) Inetoad ofone Inni report, Merton repartee* be lecued. 2) PFOSkaneiton monRoted may alio be 4 M ->0Q.
RATIONALE
1) Due to toe enoeeiMwabae a fire M e ante. Interim report wT be fecund to te m the denltoreoaNadele In e tonelermeireri'<* W r W
2 ) The A P I 4000 LC M S A B ayam m e dateci toe 4M *00 P F fl* rrrm rtto n with greater
eerwMMVtoan the 400 > 00 toaneMen
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2) The1400 00 ttaneWon can be detected with ] .................. bettor d n ra to y n d i|f>
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Exygcn Research
Page 130 o f 132
p. 130
Interim Report #I0-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
n-nu (2:Hn
FtwHcrroHmurum
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RESEARCH
MM P.091/104 M t
3058Research Drive Phono; 514-272-1034 State Codage, FA 16801 Fax: 14-231-1580
DEVIATION FORM
-EjatULL
X Piataci SpediteCavitatoli ___ ftadkyOovtaflon
D atacfO acurrenea: 0606415
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controldam was not obtolnafl. flati waa uied aathaooneta for thaanalpfeefdWMtakctarn
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Exygen Research
Page 131 of 132
Interim Report #10-Analysis of Fish and Gam Samples
Exygen Study N o .: P 00 01131
M-tO-tIH :Mpt F(or4CSTW SOLUTIONS
+ MM P.N4/1M MJT
I T 358 temrch Drive Phone: 814-272*1039 State College, PA 16801 Fate 114-231-1580
RESEARCH
D E V IA T IO N F O R M -S R L L S L L
X Pmhnt Spesate PoMetlon ___ FecJIty Deviation Data oi Occuranca: t2/Z7AM
Exygsn Project#: P78tW1131
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tumniarv a t bavtaMen?
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SUH14 (30% OlrneeiyMchloioa>ane In Toluene) was glean the aeptredon deh et 02/13X16. but
RES44 (Tatuane) used to malesSL2114 mqiirsd an 038804. 8L2114 was uend to esntod
glassware prepared for the fleh a rtaeflun from 12878 through 0187/05.
Cause: ____Preparation____ _ Analysis___ Inetrumant _ _ _ Client Request X Other
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