Document dEdm0NVoQexj9Enb9na4zOGB
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AR R 9 .6 - 562*1.
INTERIM REPORT # 10 - Analysis o f Fish and 0 m Samples
STUDY TITLE Analysis o f Pcrfluorobutancsulfonate (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
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
PROJECT Protocol Num ber P0001131 Exygen Study N um ber P0001131
Total Pages: 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT
Exygen Study Number P0001131, entitled "Analysis o f Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, d am s, 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,
Flaherty Principal Investigator Exygen Research
Weston Solutions, Inc.
Michael A. & 5ro
Sponsor
ntative
3M Company
Exygen Research
Date
Daw' Page 2 o f 132
Interim Report # 10-Analysis o f Fish and C!am Samples
Exygen Study No.: P0001131
QUALITY ASSURANCE STATEMENT
Exygen Research's Quality Assurance Unit reviewed Exygen Study Number POOOl 131 entitled, "Analysis o f Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program". 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 Inspected
Date Reported to Date Reported to
Principal Investigator
Exygen M anaeeroent
Date Reported to
Study Director
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
L ydiilShafFer Tecnmcal Lead, Quality
D ate
Note: All in-lab inspections will be documented in the QA statement for the final
analytical report at the conclusion o f the study. This QA statement involves only the review o f the interim report and associated raw data
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: POOOi131
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.
Date
Exygen Research Facility Management:
Z6 Date
Study Director, Weston Solutions, Inc
Jaisimha Kesari P.E., DEE Weston Solutions, Inc. Sponsor Representative, 3M Company:
Michael A. Santoro Director o f Regulatory Affairs
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Interim Report #10-Ana1ysi$ ofFish and Clam Samples
Exygen Study No.: POOO1131
STUDY IDENTIFICATION
Analysis o f Perfluorobutanesulfonate (PFBS), Periluorohexanesulfonate (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
.
PROTOCOL NUMBER:
P0001131
EXYGEN STUDY NUMBER: P0001131
TYPE OF STUDY:
Residue
SAMPLE MATRIX:
Fish and Clams
TEST SUBSTANCE: SPONSOR: STUDY DIRECTOR: STUDY MONITOR:
Perfluorobutanesulfonate (PFBS), Perfluorohcxancsulfonate (PFHS), and
Perfluorooctanesulfonate (PFOS)
3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144
Jaisimha ICesari P.E., DEE
Weston Solutions, Inc.
1400 Weston Way
.
West Chester, PA 19380
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 #1Q-Analysis ofFish and Clam Samples
Exygen Study No.: P0001131
PROJECT PERSONNEL
The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc. The
following personnel from Exygen Research were associated with various phases o f this interim portion o f the study:
Name John Flaherty Karen Risha Paul Connolly Amy Sheehan Christine Edwards Brittany Kravets Mindy Cressley Krista Gallant Scott Crain Eric Hoover Carlyle Horrell Shawn Robb Mark Ammerman Eric Edwards Edward Cams
Title Vice President Laboratory Supervisor Technical Lead-LC/MS Associate Scientist
Technician Technician Technician Technician Technician Technician Intern Technician Technical Lead - Facilities Sample Custodian Sample Custodian Sample Custodian
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Interim Report #10-Analy$is of Fish and Clam Samples '
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TABLE OF CONTENTS
Page TITLE PAGE........................................................................................................................... .
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.....................................................................................
" \0
1.0 SUMMARY..............................................................................
n
2.0 OBJECTIVE.............................................................................................
12
3.0 INTRODUCTION..................................................................................
13
4.0 ANALYTICAL TEST SAMPLES................................................
...............13
5.0 REFERENCE MATERIAL..................................................................... "Z Z Z Z l 3
6.0 DESCRIPTION OF ANALYTICAL METHOD............................................Z Z Z l 5
6.1 Extraction Procedure................................................................................................... .
6.1.1 Sample Preparation........................................................................................
6.1.2 Glassware Preparation....................................................................................
6.1.3 Column Preparation........................................................................................
6.1.4 Sample Extraction..........................................................................................
6.2 Preparation o f Standards and Fortification Solutions................................................. 16
6.3 Chromatography.......................................................................................................... .
6.4 Instrument Sensitivity.................................................................................................. .
6.5 Description o f LC/MS/MS Instrument and Operating Conditions............................17
6.6 Quantitation and Example Calculation.................................
1g
7.0 EXPERIMENTAL DESIGN............................... 8.0 RESULTS....................................................................
20 20
9.0 CONCLUSIONS............................................................................
21
10.0 RETENTION OF DATA AND SAMPLES................................
21
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LIST OF TABLES
Page
Table L Summary o f PFBS, PFHS and PFOS in Fish Samples........................................ 23 Table E Summary o f PFOS in Re-extracted Fish Samples................................................30 M e Iff. Summary o f PFBS, PFHS and PFOS in G am Sam ples.................................... 32 Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Sam ples................... 33 Table V. Matrix Spike Recovery o f PFOS in Re-extracted Fish Samples........................ 46 Table VI. Matrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples.................. 49
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Figure 1.
LIST OF FIGURES
Page Typical Calibration Curve for PFBS in M ethanol........................................... 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 pgfaiL 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 ED: C0049478, Data Set:061605E)...................................................54
Figure 5. Typical Calibration Curve for PFHS in M ethanol.......................................... 55
Figure 6. Non-Extracted Standards o fPFHS in Methanol, 0.0005 pg/mL and 0.001 pg/mL, Respectively............................................................................... ..
Figure 7. PFHS in Control Fish Blank, 0.00625 pg/mL Fortified Control Fish Spk A, and
0.025 pg/mL Fortified Control Fish Spk B, Respectively...............................57
Figure 8. Chromatogram Representing a Fish Sample Analyzed for PFHS (Exygen ID: C0049478, Data Set: 061605E).................................................. 58
Figure 9. Typical Calibration Curve for PFOS in M ethanol........................................... 59
Figure 10. Non-Extracted Standards o f PFOS in Methanol, 0.0005 pg/mL and 0.001 pg/mL, Respectively............................................................................... ..
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 ED: C0049478, Data Set:061605E)................................................... 62
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LIST OF APPENDICES
Page
A ppendix A Study Protocol P0001131 (Exygen Study No. P0001131) with Analytical Method V0001783: "Method o f Analysts 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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Interini Report #10-Analysis of Fish and Clam Samples
Exygen Study No,: P0001131
1-0 SUMMARY
Exygen Research extracted and analyzed fish and clam samples for the determination o f perfluorobutanesulfonate (PFBS), perfiuorohexanesulfonate (PFHS), and perfluorooctanesulfonate (PFOS) according to Exygen Method V0001783 (A ppendix A).
The limit o f quantitation (LOQ) for PFBS, PFHS, and PFOS in fid i and clams was 0,2 ng/g. For one sample (C0048133) only mie gram o f fish was used for extraction, so the limit o f quantitation for PFBS, PFHS, and PFOS in this fish sample was 1.0 ng/g.
The initial analytical results associated with fifty-one fish samples are not reported (NR) in Table I because the endogenous levels of PFOS were too high to calculate accurate matrix spike recoveries. These samples were re-extracted and the results o f the re analyses are summarized in Tables II and V.
Analytical results and assessed accuracies for the analysis o f PFBS, PFHS and PFOS found in fish samples are summarized in Table I. Analytical results and assessed accuracies for the analysis o f PFOS found in the re-extracted fish samples are summarized in T able II. Analytical results and assessed accuracies for the analysis o f PFBS, PFHS and PFOS found in clam samples are summarized in T able III. Laboratory matrix spikes that were in the appropriate concentration range (primary concentration less than three times the spiking level) were used to calculate the assessed accuracies.
The average percent recoveries standard deviations for PFBS, PFHS, PFOS in fish samples were 79% 13%, 94% 12%, and 85% 20%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in fish samples are summarized in T able IV. The average percent recovery standard deviation for PFOS in the re-extracted fish samples was 109% 20%. Fortification recoveries for PFOS in the re-extracted fish samples are sum m arized in T able V. The average percent recoveries standard deviations for PFBS, PFHS, PFOS in clam samples were 84% 10%, 93% 13%, and 73% 16%, respectively. Fortification recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI.
The sample IDs assigned by the client follow this formula: Dxx-x01-xxxxxx-x-04xxxx. The first string begins with D for Decatur, Alabama and the xx defines the sampling area within the W heeler Reservoir o f the Tennessee River where: DL3 = Up river Letter o f Intent (LOI) sampling location LOC-3 DL2 - Cross river LOI sampling location LOC-2 DL1 - Downstream Fox Creek mouth LOI sampling location LOC-1 DBC = Bakers Creek mouth DOU - Cove at 3M WWTP outfall DMC = Downstream Mallard Creek mouth
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The second string defines the general category of the biota sample and the sampling round where: FC1 = Fish sample first round 101 - Invertebrate sample first round
The third string defines the species (first two characters), the sample type (third character), and die 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 the sample type where: 0 * Primary field sample 1 = Field duplicate sample 2 - Equipment rinseate blank sample
The fifth string defines the sample preparation date in YYMMDD format.
Examples o f this sample ID system are:
Sample DBC-F01-IPF004-0-041021 is die filet tissue sample prepared on October 21, 2004 from the fourth channel catfish collected at the Bakers Creek mouth sampling location.
Sample DLI-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 parfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHS), and perfhiorooctanesulfonate (PFOS) in fish and clams according to Protocol P0001I31 (Appendix A).
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Interim Report #10-Aralysis of Fish and Clam Samples
. .Exygen Study No.: P0001131
3.0 INTRODUCTION
This report details the results o f the analysis for the determination o f PFBS, PFHS, and
PFOS in fish and clams using the analytical methods entitled, "V0001783: Method o f
Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Fish and Clams by
LC/MS/MS."
' , ?
The study was initiated on November 05, 2004, when the study director signed protocol number P0001131. The analytical start date for this interim report was December 27, 2004, and the analytical termination date for this interim report was April 17,2006.
4.0 ANALYTICAL TEST 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 C0056480-C0056485) were received on dry ice on January 13, 2005 from Tim Frinak at Weston Solutions, Inc. A whole Whiting (Family: Gadidae) was purchased from a local grocer by Ed Cams on December 20, 2004 and was used as the control fish (Exygen ID C0054391). The samples were logged in by Exygen personnel and placed in frozen storage.
Sample login and chain o f custody information is located in the raw data package associated with this interim report Storage records will be kept at Exygen Research.
5.0 REFERENCE MATERIAL
"Die 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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Exygen Study No.: P0001131
CaB P tt4 PFBS PFBS PFHS PFOS
Exygsn Inventory No. SP0000252 SP0005726 SP0002401 SP0002694
L&J 101 101 SE036 430180-1
PuntY (%) 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 o f PFBS, PFHS and PFOS are given below:
PFBS Chemical Name: Perfluorobutanesulfonate Molecular Weight: 338 supplied as the potassium salt (CiFSOjTC*) Transitions Monitored: 299 - 99 Structure:
PFHS Chemical Name: Perfluorohexanesulfonate Molecular Weight: 438 supplied as the potassium salt (CFnSOjTC4) Transitions Monitored: 399 -> 80 Structure:
PFOS Chemical Name: Periluorooctanesulfonate Molecular Weight: 538 supplied as the potassium salt (CiFl7S 0 3'K +) Transitions Monitored: 4 9 9 - 8 0 Structure:
F F
F F
F F FF FFFF
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6.0 DESCRIPTION OF ANALYTICAL METHOD
i
The analytical method "V0001783: Method o f Analysis for the Determination o f Perfluorooctanoic Acid (PFOA) in Fish and Clams by LC/MS/MS" was used for the fish and dam samples in this study.
6.1 Extraction Procedure
6.1.1 Sample Preparation
Before the samples could be weighed for the extraction, they had to be processed. To process, the frozen samples w o e placed into a food processor and homogenized with dry ice. The samples were transferred to one-gallon Ziploc bags and placed in frozen storage with bag left open to allow the dry ice to sublime. After sublimation, the sample bags were sealed and remained in frozen storage until time o f analysis. Sample processing records are located in the Sample Information section o f the raw data package.
6.1.2 Glassware Preparation
The 125 mL pear-shaped flasks were ailanized by first rinsing the flask with 30% dimethyldichlorosilane in toluene solution. The flasks were rinsed once with toluene followed by three rinses w ith 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 gram s o f carbon, and 1 gram LC -N H 2. The columns were conditioned on the day o f extraction with 20 mL o f methanol followed by 20 mL o f acetonitrile. All washes were discarded. These clean-up columns were used to remove matrix interference and not to retain PFBS, PFHS, and PFOS. Additional details about the column packing materials can be found in foe raw data package associated with this report.
6.1.4 Sample Extraction
A 5-gram* portion o f fish or clam sample was weighed into a fiftym illiliter centrifuge tube for foe extraction. After fortification o f appropriate samples, 30 mL o f acetonitrile was added to foe 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 foe
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samples allowed the fats and proteins to precipitate. The samples were
centrifuged for -10 minutes at -2000 rpm. The supernatant was then
loaded onto the conditioned clean-up column fitted inside the siianized
pear shaped flask. The eluate was collected in the siianized pear-shaped
flask. This process removed the flits and proteins from the extract Ten
milliliters o f acetonitrile was added to the samples left in the centrifuge
tube. The remaining sample in the tube was homogenized using a
tissumizer for ~30 seconds. The tissumizer was rinsed with ten milliliters
o f acetonitrile. The rinse was added to the sample tube. The samples were
allowed to shake on a wrist action shaker for another 10 minutes. The
samples were placed into a freezer for ~1 hour. The samples were
centrifuged agaui 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 mL of
acetonitrile, collecting the wash in the pear-shaped flask. Approximately 3
or 4 drops o f 1-octanol was added to the extracts in he 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
to
the flasks to make final volume. The flask was swirled to dissolve and
mix the sample. The sample was transferred to a HPLC vial using a
disposable pipet. Each sample was analyzed by LC/MS/MS electrospray.
Due to lack o f sample, a one-gram portion o f sample C0048133 (DMC-F01-MSW0010-041216) was used. All other samples were weighed out in 5-gram portions.
6.2 Preparation of Standards and Fortification Solutions
Individual stock standard solutions o f PFBS, PFHS and PFOS were prepared as specified in Exygen method V0001783. The stock standard solutions were prepared at a concentration o f 100 pg/mL by dissolving 10 mg of each o f the standards (corrected for purity and salt contait) in methanol From these solutions, mixed 1.0 pg/mL fortification standard solutions were prepared by taking 1 mL o f each o f the appropriate stock solutions and bringing the volume up to 100 mL with methanol. By taking 10 mL o f the mixed 1,0 pg/tnL fortification standard and bringing the volume up to 100 mL with methanol, a mixed 0.1 pg/mL fortification standard was prepared,
A mixed stock standard solution of PFBS, PFHS, and PFOS was also prepared. The stock standard solution was prepared at a concentration of 1000 pg/mL by dissolving 100 mg o f each o f the standards (corrected for purity and salt content, if necessary) in methanol. From this solution, a 100 pg/mL fortification standard solution was prepared by taking 10 mL o f the stock and bringing the volume up to 100 mL with methanol. By 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 tairing iq mL o f the 10 pgfaiL fortification standard and bringing the volume up to 100 m i. with
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methanol, a 1.0 pg/mL fortification standard were prepared. By taking 10 mL o f the 1.0 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, a 0.1 pg/mL fortification standard was prepared.
A set o f non-extracted standards containing PFBS, PFHS and PFOS was prepared in methanol. The following concentrations were prepared:
Cone, o f Fort Fort
Solution
Volume
(pg/m L) 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
o f PFBS, PFHS and PFOS
Volume o f
Fortified Sample (mL)
100 100 . 100 100 10 100 100
Final Cone, o f Calibration Std.
(pg/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
6.3 Chromatography
Quantification o f PFBS, PFHS and PFOS was accomplished by LC/MS/MS electrospray. The retention times o f PFBS, PFHS and PFOS were ~ 4.7 mins, - 10,8 mins, and ~ 12.9 mins, respectively.
6.4 Instrum ent Sensitivity
The smallest standard amount injected during the chromatographic run had a concentration o f 0.0005 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 0X400
Software: Windows NT, Analyst 1.4.1
HPLC:
Hewlett Packard (HP) Series 1100 HP Quat Pump
HP Vacuum Degasser HP Autosampler
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HP Column Oven
HPLC Column: Thermo Fluophase RP, 50 mm x 2.1 mm Column Temp.: -30 C Injection Voi.: 15 pL
Mobile Phase (A): 2 mM Ammonium Acetate in water Mobile Phase (B): Methanol
Time (mini 0.0 1.0 8.0 10.0 11.0 18.0
Total run time: ~18 min
Plow Rate: 0.3 mL/min
%A 65 65 25 25 65 65
%B 35 35 75 75 35 35
Ions monitored:
Analyte
Mode
PFBS PFHS PFOS
negative negative negative
6.6 Quantitation and Example Calculation
TlMSitipn Monitored 299 -y 99 399 -> 80 499 --80
Approximate Retention Time
(P in ) -4 .7 min. - 10.8 min. -12.9 min.
Fifteen microliters o f sample or calibration standard were injected into the LC/MS/MS. T he peak area w as m easured and the standard curve w as generated (using 1/x fit w eighted
linear regression) by Analyst software using six concentrations o f standards. The concentration was determined from the following equations.
Equation 1 calculated the amount o f analyte found (in ng/mL, based on peak area) using
the standard curve (linear regression parameters) generated by the Analyst software program.
Equation 1:
Analyte found (ng/mL, wet weight) - (Peak area - intercept x DF slope
Where: DF = Dilution Factor, factor by which the final volume was diluted, if necessary.
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Equation 2 was used to convert the amount o f PFBS, PFHS and PFOS found in ng/mL to ng/g (ppb).
Equation 2:
Analyte found (ppb, wet weight) =
fAnalyte found fna/mL) x final volume f2 mLY| sample weight (5 g)
For samples fortified with known amounts o f PFBS, PFHS and PFOS prior to extraction, Equation 3 was used to calculate the percent recovery.
Equation 3:
Recovery (%) - (analvte found fag/mLl *analyte in control fag /m n ) x!00% amount added (ng/mL)
Note: For the analyte recovery calculation, the "control" is the unspiked aliquot o f the primary field sample.
An example o f a calculation using an actual sample follows (calculation is for PFBS only):
Fish sample Exygen ID: C0049478 Spk 1 (Set: 061605E), fortified at 10 ng/g with where:
peak area intercept
slope dilution factor ng/g PFBS added (fort level) amt in corresponding sample final volume (mL) sample weight (g)
= =
*= = = = = =
280750 3070 13100
1 '
10 NQ (not quantifiable) 2
5
From equation 1: Analyte found (ng/mL, wet weight)
-- 1280750 - 30701 x 1 13100
From equation 2: Analyte found ng/g (ppb)
= 21.2 ng/mL
- (21.2 ng/mL x 2 m O 5g
= 8.48 ng/g (ppb)
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From equation 3: % Recovery
- (8.48 n a /g - Ongfel x 100% iO ngfg
= 85%
7.0 EXPERIMENTAL DESIGN
For fish and clam samples designated as laboratory matrix spikes, PFBS, PFH3, and PFOS were added at a known concentration to the samples in the laboratory after the samples were weighed for extraction.
The fish samples were extracted in thirty sets, five that were re-extraction sets. The clam samples were extracted in one set. Each fish or clam set included one control fish matrix blank and two control fish matrix blanks fortified at known concentrations. Two sets o f fish contained three samples, one set o f fish contained four samples, one set o f fish contained seven samples, and twenty-one sets o f fish contained five samples. Three sets o f re-extracted fish contained ten samples each. One set o f re-extracted fish contained twelve samples. One set o f re-extracted fish contained nine samples. One set o f clams contained six samples.
Accuracies were assessed for each sample by reviewing the individual QC results obtained for each sample.
8.0 RESULTS
Analytical results and assessed accuracies for the analysis o f PFBS, PFHS and PFOS found in fish samples are summarized in Table 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 U. Analytical results and assessed accuracies for the analysis o f 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 T able V. The average percent recoveries standard deviations foe PFBS, PFHS, PFOS in clam samples were 84% 10%, 93% 13%, and 73% 16%, respectively. Fortificatimi recoveries for PFBS, PFHS, and PFOS in clam samples are summarized in Table VI.
Exygen Research
Page 20 o f 132
Interim Report #10-Analysis o f Fish and a am 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 docs 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, w ill be retained in the Exygen Research archives for the period o f tune specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792.
Exygen Research
Page 21 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
TABLES
Exygen Research
Page 22 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS in Fish Samples
& "
Ctont Samte IO
C4 autom ate P P M
NHImnibiMM--
Anafyta A m t lid Found Accuracy NOWMtMt <*>-*>
C0048129 C0048126 R(>
DL3-F014PF001-0-041021 D O F014PF0014K *t021*
C0048127 C0048127 Rap
DU^FOW PP002-0-041021 D t3-F01-FRX-0-041021*
C0048120 C0040128 Rep
DM C-F01-IPF001-0-041021 DM C-F01-PF001-0041021'
C0048129 C0048129 Rap
DM C-FO HPF002-0-041321 DM C-F01-1PP002-0-041021*
CQ048130 C0048130 Rap
DM C-FOM PW O01-0-041021 OMC-F01-tPVW 01-0441021`
00048131 C0048131 Rap
DM C-F014PWQ024HH1021 DMC-F01-PW002-0-041Q21*
C0048132
OMC-FO1-MSWOO1-O-O41021
c o o 4 a m a p DM C-F01-M 8W 001-0441021*
C0048133*
DM C-F01-44SW 002-0-041021
C0048133 Rap* OMC-F01-MSW002-04M1021'
C004S134 C0048134Rep
DU-tFOI-tPFOOl4MJ41021 O L2-F01-PF001-0-041021*
C0048135 C0048135 Rap
OU-F01-JPF002-0-041021 D C 2-F01-PF002-0-041021'
C0048136 CQQ4813SRp
CD048137 C0048137 Rap
DC2-F01-JPF003-0-041021 D L2-F01-Pf0034-041021*
DU-W 1-1PF004-0-041021 D L2-F01-*>F004-0-041Q21*
C0048138 C0Q43138 Rap
D I2-F01-IPF00S-O -041021 OL2-F01-FFOOW W N1021'
00048130 C004130 Rap
C0048140 C004140 Rap
DL2-F01-FW 0 0 1-0-041021 DL2-F014PW 001-0-041021-
DL2-F01-M SF001-0-041Q 21 O U-FQ 1-M 8HW 1-O 441021*
C0048141 C0048141Rp
DU-F01-M SF002-0-04KS1 DL2-F01-M 8F002-0041021*
COO48142 C0048142 Rep
OL2-F01-M 6F0030-041Q21 D L2-F01-M SF003-0-041021-
C0048143 C0048143 Rap
O U2-F01-M SF0044V041021 D U -F0144SF004-0-04102T
0.300 0.310
0.206 0.382
0.330 0.306
0.712 am
1.08 1.0
0.968 1.34
0.210 0.202
NO* NO*
0.060 1.00
0.816 0-952
0 .2 * 7 0.210
0.346 0.330
0 330 0.310
0328 0.400
0.333 0.340
0.400 0.398
0.418 0370
0.340 0.349
40 40
40 40
SO 50
30 30
40 40
so so
30 30
30 30
SO SO
SO SO
30 30
40 40
40 40
30 30
30 30
40 40
40 40
30 30
COSuWonate P FH S
>rfcMhamiimb
Analyte Found
Aaaaaaad A ccu racy
N -W
C aSu H o n al* PFO S
PMafi>MWI-- i
Analyte Aaaaaaad Found Accuracy r a -- * </-%>
NO NO
NO ND
NO NO
ND NO
NO 0297
ND NO
0.524 0.484
ND* ND*
ND NO
NO ND
NO NO
ND ND
go NO
NO ND
ND ND
NO NO
ND NO
ND NO
30 30
30 30
60 SO
30 30
30 30
30 30
30 30
30 30
40 40
40 40
30 30
30 30
30 30
30 30
30 30
30 30
40 40
30 30
HO 3.84
4.10 4,56
7.40 0.30
14.1 17.0
70.0 98.4
34.4 34.2
270 290
530 948
3.48 2.86
4.72 9.04
2.01 2.06
4 52 4.12
2.40 2.80
5.86 fi.12
772 87.6
94.6 6 .4
41.0 40.0
B18 032
30 30
40 40
SO so
so so
40 40
30
SO 30
30 30
SO so
so 30
30 30
40 40
30 30
90 30
30 30
40 40
40 40
30 30
"Utoratety OupOcate * 1. o o f M r a te U M d S ir a n ta c f k m ln ttM tf o f 6 . 0 <l NO Not datectedal or aob* Um * c* Quantitation wNcit bi 0.2ng/g (wat Vbaiglit) NO* Not detected M or abova Um * o<Quanitetlon which 1.0 r& 9 (-- * NR Not taponad du toquM yaonm l mau* M u ra .
Exygen Research
Page 23 o f 132
interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table L Summary o f PFBS, PFHS and PFOS in Fish Samples
(c o n tin u e d )
C8ant
Serna a ID
COCOO4O04104144R4ap OOtL11--FF001144PPFr0o0Q114-<)4M))4411002211*
CQC004084184154R5ap ODLL3M-F0D1144PPFF00003M4H4MVU1002211*
C0C004084184164R6ap DDLL5>Ff0011-4IPPfF000044-0-0004411002211*
CQC004084184174R7ap 1XOL3S4=F001144PPRFX0I05S44>K45M411002S11
C0C0040841S4184R8ep DDeBCC--RF>01144PPKFW001144MKH411002211*
C0C004084184194R8ap DOBBCC-4F=0011-4PPFF000022-4(M)4))4411002211*
C0C004084185105R0ap 0D8B0C^-F001144PPFFO0O0S3441W4MM11002211*
C0C00406418511SR1ap DDBBCC--FF001144PPWW0000114-0)443)4411002211*
C0C004084185128R2ap 0O8BCC--FF00114-PFWW00002244WM4H11002211*
00C04080418613SR3ap O0B8C044==0011-4IP^W00003344D4)0M411002211-
C0C004084188145R4ap DDOOUU4-F=001144PPFW000114-0)44>Mat1002211*
000C40801458165R6ap ODOOUU--FF001144PPFF00002244WK>M411002211
C0C00408418G165R8ap C0C004084185175R7ap
DOOOUU44=F001144PPRFW003344W)04m1o0a2i1* DDOOOU-FF001144PPTFO0004444)W04X11002211*
C0048158
C0O4815BRap
DDOOUU4-=F001144PPFF00005544))44V)4411002211*
C00004064185195R8ap ODOOUU--FF0011--IIPPWW000011-04V-0044110022V1
C0C004084186100R0ap ODOOUU-*FF001144PPWW000Q2244)W4)54411002211*
C0C004084188118R1ap COOL24'Ft0Dt144i4MSSWW00001144HMM>4lt002211'
C00004084186126R2ap 0(1X224-=F0C1M4-4MSSWW0000224-0W-0H411002211*
C4 Sul*MatM=M
Prtemi)hren a ....
Found
00..442382 00..444408 00..070804 11..0673 11..3384 01.7.4536 00..006S62 00..866048 00..773080 00..776306 44..3264 86..2738 56.8886 08..2182 44..3568 21.8810 1180..43 5203
ND
NO NO
Accuracy (*#-%)
3300 3300 4400 8600
5SO0 50
SO
5SO0 4400 4400 3300 4400 4400 4400 3300 3300 3300 5500 3300 3300
C8 Sulfonate PFH8
oo
Analyte Found
00..228S12
0N.2O29
NO ND
NO NO
00..85082C
NO NO
2.21 220 88..8162 67.4746 01.8.0722 00..772002 11..0022 22..3380 00..386528 003.8)4684 33.8780
NO NO
NO ND
Aaaeasad Accuracy
(-%>
3300 3300 3300 3300 3300 3300 3300 3300 3300 3300 3300 3300 3300 3300 3300 3300
30 3300 3300
C8 8uHtonata PFOS
Analyla Found
3323..64 33..5356 00..233802 55..6448
NR NR
110180
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
112200 110020
Aaaasaad
Act+cuf.rKaciy
4400 3300 3300 4400
NR Ml
3300 m
NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
5500 3300
"laboratory Dupauna
NO Net detected at or above Limit of Quantitation aWeh a 0.2 nota (wet weiahtt. NR Noreported <kre to quafly oontat raw * M in a .
Exygen Research
Page 24 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS in Fish Samples (continued)
Exw anD
Otent Sm noteC
C4 SuNonatePF*
N<flnf atiiaMwMowia
Analyte - A U M M 4 Pound Aooureoy (noOlM M l (*A *>
C8 Sulfonate P fX t C* M o n t PF08 Nrthinrohiiaaidfcwli Partharaolan--uitwt
Analyte Found
Aaaaasad t s p t A tm s+ d
A ccu ra cy
Found
Aocur&cy
<*-% !
!*% )
00048183 C0Q48183 Rap
C0048164 C0048164 Rap
C004818S C0046165Rep
00040490 CQ049450 Rap
C00494S1 C0040461 Rep
00048492 00049452 Rep
C00494S3 C0Q49453Rep
C0040494 C0049454 Rep
C0048496 C0049455Rep
C0O49458 C0C49458 Rap
CC049457 C0049457 Rep
00049458 C0049458 Rap
C0048458 C00*9459Rep
C0049460 C0049480 Rep
00040461 . C0049481 Rap
C0049462 C0049482 Rap
C0049483 C004&463 Rep
C0049484 00049484 R*p
C0048485 0004848$ Rap
0U-FD1-M SW 003O-041081 DU-TO 144SW 003-0-& 41021"
O U -FO I-MSW0044W4121 DU2-f01-M SW 004-04)41021*
DL2-F01-M SW 006-0-041021 DL2-FO144SVWJO9-O-O41021*
DeC-f01-M 3W O Q t4W 5411(H D8C-F01-MSW0Q1-O-Q411Q4*
D 80F01-M SW 002-04H 1104 DBC-F01446W 002-0-041104'
D8C-F01 -MSWOO3-0-041104 D eO F01-M SW 00$0-04t104*
D BC#01-M SW 004-(XH 1104 D0& FO1-USW 0044W )41104*
DBC-FQ1-MSW05-O4341104 D S& F01448W 00SO 441104*
O BC-F01-M 6FC01-0-041104 DBC-PO1-MSFQ01-0-041104*
OBC-FO ! -M SF004M H 1104 08C-F01-M SF002-0041104*
D BC-H IIJPP004-04M 1104 DBC-F01.PF004^W )41104*
06C-F014PF0064H J41104 0BC-F01-PF00SW -041104*
0BC< F0I-PW 0044XM 1104 D0C-FC1-IPW 004-0041104*
DeC-8014PW 00804)41104 D BC-FO H PW 0080041104*
DOU-F014PW 003-0041104 DOU-RI1-PW 0034HM 1104*
DO O F01-IPW 004-0041104 OOU-W1-IPW044W41 104*
D CKW )1-< PW 005004I104 DOU-F01-f*W 0050-041104*
O UH P01-FW 0024M 41104 DC2-FOHPW 002-0-041104*
DL1-F01-J4SW001 -0-041104 DL1-F01-M SW O 01-0-041104*
NO ND
NO NO
ND NO
0.888 0.882
0.888 0.884
0880 0.784
0.884 0.880
0.832 0.632
0.820 L788
0.786 0.780
0.504 0.520
190 1.84
0.484 ,0 .4 4 4
0.572 0.532
3.12 .3 .0 5
3.49 3.11
2.97 2.90
1.04 0.960
120 1.24
30 NO 90 ND
30 NO 30 NO
30 NO 30 NO
30 30 .
8.32 8.32
30 .
30 . 30
143 3.35
. 3.62 3.64
.
30 9.72 30 0.80
. 30 30
277 . 288
30 3.68 30 3.46
30 1.94
190
30 0.584 , 30 0.540 '
30 2 15 30 218
30 30 .
128 128
30 . 2.10 , 30 210
,
30 6,00 30 5.92
30 7.12 30 8.84
30 8.12 30 5.32
30 : 30
NO NO
30 0.806 30 0.932
30 92.4 30 91.9
30 88.0 30 9 49
30 168 30 174
30 NR 30 NR
30 NR *> N R
30 NR 30 NR
30 NR 30 NR
30 NR 30 NR
30 NR 30 NR
30 NR 30 NR
30 142 30 152
30 , 1
30 NR
30 .
30 .. 30
NR NR
NR NR
30 NR 30 NR
30 NR 30 NR
30 NR 30 NR
30 820 30 8.50
30 NR 30 NR
30 30
30 30
X 30
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
30 30
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
40 40
NR NR
*mtondMyDuptota
NO Noldetected* or abov*Umo<Quantiteton ***! 0.2 no/s(watwaight).
NR Notnportwl 4M qm ny eonra) m w R M ura*.
Exygen Research
Page 25 of 132
Interim Report it10-Analysis o f Fish and Clam Samples
Exygen Study No.: POOO! 131
Table I. Summary of PFBS, PFHS and PFOS in Fisb Samples (continued)
C4 luffMMta PFBS CS lutfanaM PFHS C l 8u4font* FF06
Exvoen ID
dent Sam oa 10
Analyte Aaaaawd Found Accuracy M at) 4 (MM
Analyte Found
ASMNHMd A ccu racy
Analyte Aataaaad Found Accuracy (nofelwatwi. (*/%)
C0049400
DL1-F01-MSW002-0-<M1104
1.30
30
1.72
30
00049486 Rap OLt -fO I -MSW0024WJ41104*
1.1
30
144
30
C0Q49487
L1-F01-M SW 003-0441104 0.860
30
1.13
30
C049407 Rap DL1-F01-M SW 003-0-341104" 0.829
30
1.14
30
C004M 06 C00494B8 Rap
DL1-r01-USW 004-04>41104 D L1-F01-M SW 004-0-041104*
1.22 1.12
30 0.908 30
30 0.880
30
C0049489
DL1-RJ1-MSW 006-0-041104
1.22
30
1.16
30
C30494S0Rap DL1-F01-MSW004-CM141104*
1.20
30
1.18
30
C0049470 C0049470Rap
DL1-F01-M 3FKH-0-041104 DL1-F01-44SF001-0-041104*
ND NO
30 0.31S 30 30 029 30
C0040471 C0049471 Rap
O L1-F01-M SF0024-041104 OL1-FQ1-MSF0Q2-0-O41104*
NO NO
30 0.624 30
30 0.904
30
C0049472 C0044472RSP
0L1-FQ1-MSF00345-O41104 OL1-FOf-M 3X]3-0-041104*
0.203 NO
30 0.662 30 0479
30 30
C0040473 C049473 Rap
OL 1-F0 1-4457004-0-041104 O L1-F01-W 6F004-0-041104*
NO NO
30 0832 30 0.536
30 30
C0046474 C0049474 Rap
DL1-FC1-M SF005-0-041104 D L1-F01-M SF005-0-641104*
NO NO
30 0.984 30 30 0.644 30
C0049479 C004947$Rap
Otl-FOI-ffW OOI-O-041104 D L1-F01-4PW 001-0041104*
0.772 0.670
30 0.566 30 0.744
30 30
C0049476
OL 1-F01-JPW002-0-41104
0.468
30
0436
C0049476 Rap DL1-FC14PW 002-0-041104*
0.472
30
0416
30 30
C0049477 CO049477Rap
DL1-F01-PW 003-0-041104 DL1-F01-1FW 003-0041104*
ND NO
30 0209 30 0.247
30 30
CQ04947B C0049478 Rap
C004L47V C0049479 Nap
O L1-F0HPW O 44W 411O 4 DLVF01-IPW 004-0-041104*
O U -RJ1-1PF0Q2-O-O41104 OL 1-701 -#7002-0-041104-
ND KO
NO NO
30 0238 30 0246
30 0222 30 0247
30 30
30 30
c o w sia o C0049480 Rap
OL-1-F014Pf003-CW Hl104 DL-1-FO1-IPFOO4O-0411O4*
NO NO
30 029 30
30 0262
30
C0049481
DL-1-F01-1PF0040-041104
NO
30
ND
CQ049461 Rap D L-1-FO H PF0044H H I104*
ND
30
ND
30 30
C0049482 C0O49482 Rap
C0049483 C0049463Rep
CO049484 C0049484 Rap
DL-1-F014PFOOS-CMM11O4 DL-1-F01-IPF00M -O41104*
DL3-F01-MSWOO1-0-041103 DU-FOI-M 6W 001-0-041106*
D L4-F01-M SW 002-0-04110S DL3F70144SW 002-0-041105*
ND NO
NO NO
ND NO
30 0373 30 30 0466 30
30 NO 30 30 NO 30
30 NO 30 30 NO 30
NR NR
NR NR
1 166
NR NR
263 307
NR NR
NR NR
NR NR
NR NR
17.4 18.9
15.7 154
46 942
96.6 572
11.1 11.2
20.9 21.4
7.60 7 30
6.72 6.56
138 137
190 162
NR NR
NR NR
30 30
NR NR
30 30
NR NR
NR NR
NR NR
NR NR
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
30 30
*labaoUoiy Dupteate NO N otd atectedalorabovuU m ilof Quanltetton w N chl*02ng/g(tealm ioN ). NR Nat laportad du ta audlly oortrol m u t M u m .
Exygen Research
Page 26 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS, PFHS and PFOS in Fish Samples (continued)
C4 Sulfonate 7FBS CeSuWonMaPTHS CS Sulfonate FOB
Bw n
G iant Sam ptolO
Analyte Aaaaaaad Found Accuracy
MMDaMat t*b%)
Analyta Aaaaaaad
.F omm Accuracy Antalmi 4. <**%)
Analyte
Found
(natal
Aaaaaaad Aocuracy
W-%1
C0049M 5
D L3-70f-M SW Q O XH *1(05
ND
30
ND
X
COO40486Rap DC3-F01-MSW003-0-041105*
NO
30
ND
X
00040488 C0049488 Rep
D L3-F01-M 6W 004-0-04110S DC3-F01-M SW C04-0-041105'
NO ND
30 0.286 30 0 X 2
X X
C0049487 CC048487 Rap
tX.3-701-M 3W 005-0-041106 0U-F01-M SW 00W W 41106'
ND NO
30 0.366 X
30 0.341
X
C0049438
DL3-701448F001-C-041105
NO
30
NO
X
COO40466Rap DUF701-M S7001-0-041105*
NO
X
NO X
COO4043O CQO40480Rap
OL3-701-M8F0C2-0-O41106 DL5-F01-M 3F002-0041105*
ND NO
X X
ND X NO X
COO4049O C0049490 Rap
D LS -7 0 14437003-0-041106 0L3-F01-M SFQ Q 3-04M 11067
NO ND
X X
ND X ND X
C00494Q1 C0049491 Rap
DL3-F01 -M8F004-0-041106 DL3-F014457004-0-041105*
ND NO
X X
ND X NT) X
COO49402 00048402 Rp
034= 0144 3 7 0 0 5 -0 0 4 1 1 0 5 0.34= 01 4157006-04)4 1105*
NO NO
X X
ND X
ND X
C0048493
DMC-701-1PW0034MM1106
NO
X
0X6
X
00048483 Rap DMC-7014PW0034MM1105*
ND
X
0.334
X
C0040484 C0048464 Rap
DMC4=01-tPW0044M)41106 DM C-7014PW 004-0-041105*
0.300 0.345
X X
0.305 0.464
X
X
C0Q48496
DMC-701 -IPW 0054W H1105
ND
X
0.270
X
C 0 0484sn tp DMC-701-IPW006-04M1105*
NO
X
0X5
X
C004848S
DMC -7 0 1-M SW 0C3-0-041106
C0049406 Rap DM C-F0144SW 0034KM 1106*
NO NO
X
0502
X
30 0360 X
COO40487
DM C-F01445W 004-0-041106
CQ048497 Rap DMC-F01-MSW0Q4-0-G41105'
0.31 0333
X
X
1.00 X
1.88 X
C0Q49496
OMC-FC1-MSW005-0-041106
ND
X
0.960
X
C004i4 8 6 Rap DMC-70144SW005-0-041106*
ND
X
0X6
X
C0048498 C0048498 Rap
OMC-70M46FOO2-0-041106 DM C-70144SF002-0-041106*
ND NO
X NO X 0 .X 7
X X
C0040600 C0049500Rap
O M C-701-M S70034H M 1105 04404=01 -MSF0034MM1106*
ND ND
X X
ND X NO X
C0048501
OM C4F0144S70044HH1105
COO405OIRap M C-7014487004-04M1105*
ND ND
X 0X4 X X 0.228 X
C0048602 C0048S02 Rap
DM C-70144SF00647041109 DM C-7C1-M SF006-0-041105*
ND NO
X 0.420 X X 0.446 X
CO0406O3 C0040603 Rap
D M C-7014P7003-0-041109 DMC-701-177003-0-041105*
NO ND
X X
ND X ND X
146 144
198 190
173 168
116 115
110 111
75.6 72.0
1X 134
81.6 83.8
6U
838
88.8 696
64.4 82.8
364 330
259 260
NR NR
NR
NR
8 66.0
116
118
146 147
7.82 7.02
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
X
X X
X X
X X
*UAortoiyDuptesto
NO * Not detected at or afcova Urn# ofQ uantitelonw tifchte 0.2 na/fl(wntwnlght).
NR Not ported dun t> qwMy ooxiol n u l W kn*.
Exygen Research
Page 27 o f 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygcn Study No.: P0001131
Table I. Summary of PFBS, PFHS and PFOS in Fish Samples (continued)
Exvoen to
CBwit S ttfflO l
COO406O4 C0049904 Rap
DM C-F01-IPF004-0-041108 DMC-P01-HRF004-0-041106*
C0O4950S C0048506 Rap
DM C4R314PM 054W 41105 DMC-F01-i f 005-0-041105"
COOH3S4 C0056354 Rap
OL2-R31 -M8F005-0-041218 D L2-F01-M SF006-0-041216*
C006S4SS C0056450Rap
012-F014PW 006-04M 1215 DU-701 -iFYV00547-041215*
C00864S8
DOO-F01-M8W002-0-041216
C0OS6466 Rap DOU-F01-M6W002-0-C41216*
C00S64S7 CO056457 Rap
DL2-F014PW 004-0-041215 DUF014PW 0044V041215*
C0068458 CCC56456 Rap
coooMaa
0)0564SO Rap
DO U-F01-M SW 003-0-041216 DOU-FO f-M $W 003-(M )41216'
DL1-F01-IPW 004-0-041130 DL3-FtH*iPW 004-0-041130*
C0056480
DOIWF01-M6W001-04W1215
C0086480 Rap DOU-F01-MSW001-0-041218*
03056461 C0056461Rap
C0058462 C0056462 Rap
C0066483 00056463 Rap
C0058464 C005645* Rap
C0056496 C005646S R ip
CQ056466 00056466 Rap
OO U-F01-M SW 004-0-041216 DOU-F01-M 3W 0044HH1216'
O O U-F01-M SW 005-0441Z16 DO U-F01-M SW 0054V041216*
D04J-F01-M SF005-0041218 DO U-F01-M 3F0054W M 1216-
DL3-F01-IPW 002-04H1130 DL3F01-IPW 002-0-041 130*
DL3-F01-IPW 0030-041130 DL3-F01-IPW 003-0-041130*
DOU-F0144SF0034W J41216 DOU-F01-M 6F003-0-04I216*
00050467 C0050467 Rap
00066466 C0056466 Rap
C0050400 C0056460 Rap
C0056470 C0056470 Rep
O0C-FO1-M3FOO6-1-O41216 DeCFOM ISflOOS-1-041216*
DBC-FO1-MSF0OWMJ41216 O BC-RM -M 3F006-0-041216*
DOU-F014MSF002-0-G41216 DO U-F01-M SF002-0-041216*
DL3-F01-IPW 001-0-041130 DLVF01-IPW 001-0-041130*
C4 SU foaata PFB 8
Found
Fa ao--id Accuracy
(44-H )
C6 Sutfonata PFH S
PwtNiiinhM u iiiW iim i
Analyte found
A ateaaad A ccu racy
{AIM
HD ND
NO ND
ND NO
NO NO
0l206 0.227
NO NO
ND NO
NO NO
7.08 7.12
4.72 4.66
0.364 0.36
f.41 1.43
NO ND
ND ND
1.72 1.73
0.220 NO
NO ND
0.666 0.372
ND ND
30 NO 30 ND
30 ND 30 ND
30 NO 30 ND
30 ND 30 ND
40 1.72 40 1.70
30 ND 30 ND
30 10.4 30 10.6
30 ND 30 ND
30 15.4 30 14.2
40 21.7 40 22.5
30 (.34 30 1.41
30 &40 30 6.44
30 NO 30 ND
30 NO 30 ND
30 156
30 1 aw
30 1,76 30 1.76
30 1.66 30 1.50
30 4.56 30 4.66
30 0.246 30 0219
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
C8 S uitonita PFOS
A ntyta A aw aod
Found Accuracy
<"*> W-%\
44.0 30 456 30
46.4 4641
492 S I.6
13.2 13.3
NR NR
6.80 880
NR NR
30 30
30 30
30 30
NR NR
30 30
NR
m
7.92 7.52
NR NR
NR NR
m
NR
NR NR
12.0 11.5
5.44 5.28
NR NR
30 30
NR NR
NR NR
NR NR
NR NR
50 80
40 40
NR NR
NR NR NR NR
NR NR NR NR
NR NR NR NR
9.04 30 8.80 30
T-atraoiy Duplea*
MO* Not (M tctad at or bov* LtaiH of OuanttafoA imWdi I* 0.2 ng/g (wot weight). NR Notnportad duato qurfty eanW imuh MMm .
Exygcn Research
Page 28 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table I. Summary o f PFBS, FFHS aud PFOS in Fish Samples (continued)
Exvoan IO
C0056471 C0056471 Rap
C0056472 C0066472 Rep
00050473 C0056473Rap
C0O66474 C006474 Rap
COOS6475 C0056475 Rap
C0066476 COO56478 Rap
C0056477 C0056477 Rap
00058478 COOS6478 Rap
C00S6478 C0056479 Rap
CSart 8arn M K>
C4 Suifoaata P f B l M H fciiia
Analyte Found
Aaaaand Accuracy
M UM M
C 6 3u*onetaPF11S
Anelyto Found tnudUM w
Aaaaaaad A ccu ra cy
<*%)
D O U -F01-M SF002-14)41218 D O tA TO l-M SFO O a-H M *
0.840 0860
30 30
4.68 4.72
DOU-FOt -U S F0 0 4 -0 -0 4 1216 DO U-F01-M SF00441-041216'
0.792 a a ie
30 30
2.35 2.22
DOU-F01-M SF001-0-04I21B
218
30
10.
DOU-FO1-8ASF001-O-O41216*
2 J8
30
10.7
D BC-TO 144SF0054H M 1210
NO
30
2.09
DeC-F01-M SF003-0-041216`
NO
30
2.00
DBC-F91-M SF004-0-041218 O BC-F01-M SF0044H M 1216*
DM C-F01-M SF001-0041218 DM C-F01-M SF001-0-041216*
ND ND
NO ND
30 3.87 30 3.77
30 0420 30 0.456
DL1-F01-IPW 005-0-041216
0.253
30
0.944
0U -m -li> W 0(O -04t216`
0.249
30
0.644
D L2-F014PW 003-0-041201
NO
30
NO
0L2-F01-IPW 0034W H1201*
NO
30
ND
DU-F01-IPW 006<W M 1201
ND
30
ND
OL3-POHPW 0060-041201*
NO
30
NO
30 30
40 40
30 30
30 30
30 30
30 30
30 30
30 30
30 30
CS SuM oaataFFO
Analyte Found
NR NR
NR NR
NR NR
NR NR
NR NR
NR NR
68.8 67.6
7.48 7.44
4.68 4.72
Aaaaaaad A ccu racy
<*-%!
NR Mt
NR NR
NR NR
NR NR
NR NR
NR NR
30 30
40 40
30 30
tatou Oofy Dupdcata NO - Not d*tectad X or dbO'ra Lim it of OutnSlafion Atlch ia 0.2 ng/g (wet w e ijh i).
NR >Not wponM du* toqw%corM imu*WIutm.
Exygen Research
Page 29 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table II. Summary of PFOS In Re-extracted Fish Samples
ExyoenlD C0048151 C0048192 C0048153 C0046154 C0048156 C0048158 C0048180 C0049450 C0O49451 C0049452 C0049453 C0049454 C0049456 C00494S6 C004458 C0O49459 C0049460 C0049461 C0049482 C0049463 C004B46S C0049466 C0049467 C0049469 C0049471 C0049472
Client Sam ple 10 DBC-F01-JPW001-0-041021 O BC-F01-IPW 002-0-041021 D8C4=01-1PW0034W41021 DOU-F1.IPF0014M41021 DOU-F01-IPF0Q2-0-041021 DOU-F01-IPF00545-041021 DOU*F01-IPW0Q2-0-04102t DBC-F01-MSW001-<M>41104 OBC-F01-MSW002-0-041104 DBC-F01-M3W003-0-041104 DBC-F01-MSW004-0-041104 DBC-F01-MSW005-0-041104 DBC-F01-MSF001 -0041104 08C-F01-M SF002-0-04110+ OBC-F01-IPF005-G-041104 DBC-F014F/V004-0-G41104 D BC-F014PW 008-0-0411-34 D O U -F014PW 003-0-041104 DOU-F01-IPW 004-0041104 DOU-F01-IPWC05-0-041104 DL1-F01-MSW001-0-C41104 DL1-F01-MSW002-0-041104 DU-F01-USW 003-0-041104 D L1-F01-M SW 005-0-041104 D L1-F01-M SF002-0-041104 DL1-F01-MSRXJ3-0-041104
NR - Not ported due to quality corn** rt*u*fadur
Exygen Research
C t S ulfonate PFOS
^w H urnnorN .ittiiiem .u
Analyte Found (afoi w * wefaht
Aaeeeaed Accuracy <+/-%>
2080 3330 1800 586 638 644 1210 9480 7520 12600 3440 5240 5240 4780 808 1230 2620 NR 1740 2130 868 708 896 804 968 432
30 30 90 30 30 30 40 40 30 30 30 30 30 30 30 40 30 NR 30 30 30 30 30 30 30 30
Page 30 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table II. Summary of PFOS in Re-extracted Fish Samples (continued)
<30049*74 C0049496 (30049*96 <30056*56 <30056456 <30056*60 C0056461 <30056462 C0G56463 (30056*66 <30056467 <30056*68 <30056469 <30066471 <30056*72 C0056473 (30056*7* C0056475 <30056476 (30048148 (300*8150 (300*8156 (30048157 C0048159 <300*8*73
Otent Sampis ID DL1-F01-MSF0OJHVO41104 DMC-P01-MSW005-0-041105 DMC-F01-MSF002-0-041105 DOU-F01-M3W002-0-041218 DOU-F01-MSW003-0-041216 DOU-F01-M8W001-0-0*1218 DOU-F01-MSW004-0-0*1216 DOU-F01-MSW005-0-041216 DOU-F01-MSF005-0-041216 DOU-F01-MSF003-0-W1216 D9C-F01-MSF005-1-041216 D8C-F01-HSF006-0-041216 DOU-F01-MSF002-0041218 DOU-F01-MSF002-1-041216 DOU-F01-MSF004-0-041216 DOU-F01-MSF001-0-041216 DBC-F01-MSF003-0-041216 DQC-F01-MSF004-0-0*1218 DMC-F01-MSF001-0-041216 DBC-F01-IPF001-0-0*1021 DBC-F01-IPF003-0-041021. DOU-F014PF003-0-041021 DOU-F014PF004-0-041021 DO-F01-W0014WM1021 DL1-FO1-MSF004-0-04110*
NR * Not mportad dua to quaSty oonm i rm itt failures.
CSSiJtfonat PFO S
Ps itHmnoocI
Analyte Found
AMMMd
(hlttDWMWMN Accuracy(*
7*0 30 560 30
0 30
28200
60
*040 30 NR NR 5120 30 *98 30 720 30
848 30
NR NR
8860 50 640 30 892 30 1820 30 2070 30
46*0 30 9280 50
840 30 384 30 293 30 359 30
424 30 387 30 348 30
Exygen Research
Page 31 o f 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table III. Summary o f PFBS, PFHS and PFOS in Clam Samples
C4 Sulfonate PFB8
E xK w n ID
dont Sam otolD
Analyte Found
A taataad A ccu ra cy
... t * _
C0Q56480 DC3-I01-CFW 001-0-04121# C0056480 Rap DC3-I01-CFW 001-0-0412161
NO NO
40 40
00058481 DM CH01-CFW 001-0-041216 COOS6481 Rap DMC-K)1-CFW 001-04H 1218*
NO ND
30 30
C0066482
DL2-I01-CFW 001-0-041218
C0058482 Rap D t2401-CFW 001-0-04121(F
NO NO
30 30
CQ096483 D8C401-CFW 001-0-041215 COOS6463 Rap D8C~)01-CFW 001-0-0*1215*
ND ND
30 30
C0056484
DL1-I01-CFW 0014M 41215
C00S6464Rep DU-W -CFW 001-004121S"
NO NO
30 30
C0056485 DOU-W 1-CFW 001-0-041216 C00S6485 Rap D00401-OFW 001-0-041216*
ND ND
30 30
C * Sutfonata PFH8
A na* Found
A taataad A ccuracy
( /-it)
ND NO
ND ND
ND ND
ND ND
ND ND
0 .2 0 2 0.205
40 40
30 30
30 30
30 ao
30 30
30 30
C l Sulfonate P f08
A n a lyte Found
1.82 1.82
8 .1 8 6 .1 2
1.81 1.77
4 .4 8 4 .4 4
6.ao 884
11.4 10.9
A aaataad A ccuracy
(/%)
50 50
50 50
50 50
30 30
40 40
50 50
*la bootory Du4cte NO * Not detected at or ab ate Um4 of Quanltabon which I 0 .2 nota (w tew aight).
Exygen Research
Page 32 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples
6*npte QtemiXitin
DL514FF001-{M>41M1 < * * .& M M
OL3#O14P01-*O4W1 fcmauaigitp. mapm
Di>F0l-rfOG2<Ht02l KwuizrSftD. tappai
tcm * n rtfi a. toopm*
OMC-RM-lWW-Wloai {oaoatimaptti.iepM
DMC-f01-lPF001-WH1CCn
MC-P014PF902*C4131 (cooteia*tene tite)
C3MC-F0!-Vf002-0^41021 (OtMdUtBmK.WdM
DMC-FC1-PW0014441021 (COMtH*O.M|p
PMC-f01-tfWQ014HMK121 [Qooso%i,ipiiaM
Oft4C-FOl*rwoaz44M1Q21 tem ili* * new *)
DMC-F014PW00t-<M>41021
OMC^ot-Miwaw-WMioai {Ottttltt *#*(.****>
DMC-FW-MSVWOI4-041021 (cotHtm ipk#.loo* **)
DMC>F0l-M3WQ2<O-O4ia2tA te r n ra tata, to m n h i
DMC-F014I3W0024HM1021* tOOMIpM.MOmMpM
Ott#01')FF001 -0441031 tCKMm M '.-w ***>
DL2-F01*4>f0014441001 tax n tfMapt K. ionppbpa*}
D U ^W PfflW -0441021
(COMO*
apte)
D12-F01-0*0024441 oet (COOMiaftlpkL Ite pptOpte)
"C S S ^prited
10 100
10 100 10 100 10 100
10 100
10 100 10 100 flO at 10 100
10 100
ill
C4 a x o r u r m Amami
Bdcamud K M )
...A )
AmiFound Amount in W y hCW Md KM 7
AmiFound moompu
Ammiri
Nicpvnrnd M ) Mlte
RocoMoiy f%>
OJM
6.56
w
0.300
024
02
NO U l 3 5.14
ND 732 n
5.1
12.6 74 794 73
0265 1.92 93 0206 00.0 60
ND 7.40 75 4.16 NO 7M 00 4.1
10.3 61 eo j 77
00 4.40 42 NO 534 740 00 26 0.330 004 09 NO 74 75 7.40 81 74
0.712 7.60 70 0.712 76.0 77
NO 660 06 14.1 NO 9933 09 14.1
26. 196 164 00
1.00 7 96 1.00 94. 64
NO 7.84 75 700 ND m o 00 700
71.6 131 91
0.M0 9.70 59 NO r jo 90 34.4 44.
0400 900 90 NO 746 75 544
101 67
0216 0.79 0.04 9M M 270 0218 12 91 0924 032 03 270
270 375 106
NO* 52 NO* 452 89
NO* 520 104 NO* 4C2 M
930 550
470 924 70
0-MO
S tt
51
ND 960 06 5.48
0.36 40
0.600 49.4 49 NO A S 90 545 56.4 55
041 9.04 46 NO 6.40 64 4.72 SJS 39
0.01
040
9
m
78J 7 4.72 72.4 SO
*5Umn(t4.<MmW)mfHm. n nl m>HwMmH>nfctmiH*iHH (.tc>mti':'UU4om.n4 iMotwr4Mmm*k*mfcutaM
ND Wot m im i .1 or4w Umd of Qunr mmonwuu i u O Jr y g
NO*- NmdMucMNwaixmUn'tfdfOumiUMonaMcfthl.Onrtl'***).
(M.NonttrMAutlBtuMtiaMMinkMMKm h M W ) * n i t a < W i l .
* * **"**
N* *-->--* * * .m w n Numim ,, m ry Unum,lumiamtmmm<
Exygen Research
Page 33 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.; POOOU31
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
ample
OU4W 1W8-0-041M1
QU^m-IPFO034MMtd21 (CantatM*.now****** 01M2-^t0S1TS'F*OfCt4-0*0*410*21) DU<f0t4PF004OO4tQ21
0tcia2M-PiOtMPFOaC.64m444tMO21 OL2-F01-1PR)CMM>4iaai (CWM419***J,MO um C(CI3OJNSUOHMSinWjKP0.i1o0**0s4p1e0e2>1 tX2*01-rWQ01-0-041021 (com*k hum%*i) DU-fC44*SF0014WM1Q21 tamin*m,* mbMi DtCt3M-FCt41-0iAH9aFt0,1J1-0-6*41*0*2*1 D<0U0-4F*Q141144pSfeFC0.01200pp-4M**iaK>1 D<0L02*-1TC4V1M18*FM0.Q1240-0*O441*021) D<LC2^M0t4Wa4maFo00.3p0a04alp0t21} DtcUo4-4F#0i1-aMp8UF0u03o0*04s1*0w21 CL2^01449F<U*0041Q21 (caamvatpfci, topp&spn) D<0Lo2HoF*Qi*l-Mi*aSFj0. m)i*of*r6*4a1Q*2*1 DU00-P*104144P*fO?C,.1-*04*>41*021) <0CLI61*-R14H<-$IPpF*K00,11tOtg0*4S1p0*21} DU0-F*D*M*PfeFfOcfOta-0*0441M02U1 tOomU^ol0a14P*Fu00m3s0m0o4atap2tl*
Amount SpBtsd
AmtFouCnd4 S tnSample
ftif W M
RAamawowurK! i rkmt)
C6SuM nH ffH S
Am<Found Amount toSanyo* Atf*afoctouitrNadt Raoowry
C6Sulfan-i PPOS
AMmStaFmoupnlpd RAMm0oWun0t6 Ntoowty m i*
10 024? 7.00 8 NO 7M 0 241 820 72 mo 3247 624 3 NO 732 73 2.01 74.0 72
10 0340 644 63 NO 740 re 4.32 113 6 100 0346 074 w NO 704 77 4.32 80.4 7
10 *33* *. 06 NO 7.0 77 2.48 846 72 100 0330 064 08 NO 0.6 61 2.48 82.0 80
10 0320 7.04 or NO 7.60 re 3.86 13.9 80 100 0320 46.0 68 NO 772 rr 166 52 7
10 0330 730 TO NO *20 2 772 TOO * 100 0333 44 64 UD 774 78 772 158 81
10 0.400 8JC 65 NO 74 re 644 101 100 0406 014 01 ND 68.0 68 044 188 61
10 0416 6.62 61 NO 6.7(1 06 41/. 412 100 0416 44 4 ND 704 71 414 104 62
10 0343 7.0 67 NO 746 78 34 12 100 0348 714 71 NO 61J 81 834 167 63 10 0.432 7.44 70 0381 8.16 7 334 400 m too 0432 873 07 0381 78.4 re 334 106.0 73
10 0448 720 68 NO 846 61 346 104 73 100 0444 u 68 NO 814 82 166 MO 78
W Kn ... i . mI M*pMlp turn. > >6uw6 iu<iMU>>.it iy.ulu< W|| w|)lfci
ND Not J w a 0 l bom U rtt </OunWMo(i
1 o a ntfg (wl
'M i w iw t a K w w m M a M n * *. < *
-- --<<m ***. m ~ *,*+ m .w *,*v 1mt , tn m * * * * * * N t f n H
Exygen Research
Page 34 of 132
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
. tend*
.Amount Spfod
Aim Foard msampia
Amount
AMFound Amount
Aw m M P*CMMry InSnmM ftaoovamtf ngcaMty
AM POund bSampa
Amount RnooMuad
Racouary
1%) fi
M3'F614PfO0*aO4N1Q21 tooomsaOffeO. **6*)
00-F01-1PF004-04H1021 M W * n. m p + tm i
to too
Ott-F01-*F00644M1021 icoosour* * d.ioaasm)
DL3-F0HPF006-O541021 fO mur a * i m m* lain)
10 too
D eo F 9 i* m o i-ao i 1021 tOMHeipfct. **%*
MC-ronimoi<MMi02i vrnm m w m * mopwvmj
10 too
O0C^914PRX124^M1O21 K xm vm m * M M )
DeC-FOl4PF002-0541021 <C*0M14Sflpl K,<S6fp*M*)
10 100
D0C-WHPFW3*-041C21 MOttMO* a. 10m *H *)
D0C-fO1*#POO3>d^M1O21 (Gmm m m l a m
10 100
0OC-FCWPW00HWM1021 C004IH1%kC. 101*0%*)
DBC-fOWPWOOl-CMMIflai tcoo*mt # h.1*0*aOp*i
10 100
CeC-fOMPWfX&O-IMItttl MU*tu %D. tOppo%*nl
Oec-WPW002-<W>41Q21 CDMuaaapaMeomfeioiM)
10 - .100
0BC-FOHPW0Q3O041021 p m *. **% *)
D oopoi*rw xxw x> 4ia2i MOMWIftpkJ. MOpi*Op*}
to 100
000-f014PTOHHM t1
DOU-F014FF00147-041021 MMU okK.HOMlUMI
10 100
DOU-F0MPF0a2-(W41021 P M % a a p iM a )
DOU-f0HPF002-0^41021 X * tm *u loop t %*)
10 100
DOU-F014PF003^HM1021 (C0M91Nm C.1*m RM>
DOU-FDl-)Pr00WHm021 fcm ous aoKh. toono *>aN
10 100
0J*4 A4 01 0.704 L> 00
NO | NO
105 . I - . 0562. -, 896 1
01.4 ;Voo .. .. 0502, . 012
153
30 NO
0.16 82
a ,
117
153 804 SO NO 035 63 6.40 ' 005
154 654 40 0.662 105 101 . MR
154 8M 90 0.9 065 . 06
MR.
NR NR
1.43 5.04 44 NO : 056 *' 94 1.43 b2 SB NO , 80.0 ' 80
no 110
113 1M
0.000 0.72 57 0.644 10.4 96
MR
OJOO 05 00 0544 505 06 ! MR
MR MR
0.864
7.0 < 02
2.21
050
78
MR
0.004 70.0 60 251 MO M . HR
NR NR
0.700
7.9#
66 jO.12
165
01
MR
NR
0.700
OSLO 66
6.12
96.0 - or
HR
NR
0.736 ' 8.32 78 6.76 165 w . ' MR
0.730 . 705 70 .7* 005 54
m
458 to. 66 1 * 0.4ft 06 456 705 72 152 065
HR NR
NR NR
NR NR
0.78 13.1 3 0762 0.72 09 MR NR 0.71 785 6 0.702 ' BOO 79 MR NR
S Jt
it* 80
1M - 10A
96
HR, , NR
9.H
,71 ^ iJx
86.4 *7 ` 'NR
NR
M 01 62 1 NR NR
79 NR NR NR NR NR NR NR HR m NR NR NR NR NR
M-- . . a ^ .-a.-- ^ .......,
-- ------ ,--. ----------------|t|||||
NO NrtM gM crM OM UrNrfQuanNrtQnar*ftli<Un0t(M lwgM ).
N R .N > w a rM M M % < a n lra liW i M Lm fc R .n ly iR iM M fc M .N ia n th T lM .H .
Naaa: SlraglMataaMMayMIggAwg M M m uliiN M iyM lM M aMywyaRgM.fr
Exygen Research
Page 35 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
Snmptv
DOO-FOHPFO&MWM10CM cosmwipaD, N n U M DO-FClHf'FOW-CMiiOl (caMBurioki. mapa spans
OOU-fOHRMX>MW4102l csMflrttMpfti topassaM DOU-F1-IPF0054-04121 (OSMSiitati, moppbOpa)
OCHMQMPWOOt-C-O4101 W*HOip*r.1AppOlpM) OOU-FO1dPWOO1-C-041G21 (Cotai**tpkk.im cc*opa
D0U-F0l-tPWO-0--04ia21 C0**4iao%*a. 10pp*Sana) oocwh-ipvvo-o^>4icai tcaoMtOp*c 1*0rn m )
CX2-F0M4SWO1-0-041021 ICflWOWfpfcl, t*pp4*0*a)
DL2-fC1*MSW001-0-041021 tca*ai*i amj. inpptM )
OU^14A8VW2-0-4121 tcm m m m c w pp*apa DU#0144SW0G2-0-O41021 (CS>MemptiL.iaS(ppai*t
DU-FtHOtaWOCGO-Wf021 I00*ta*tpkc, ppaOpan DL2-FO1-U8WOO10441O21 caoasmam o. m*pp*tpfl)
0U-F0l.ftfl8W0Dt4d41021 ic tm m spkl n anmm DU*f01-tW0OWM)41021 tOSMIOi tpP, 1Mpp*Splnl
OL*1 -MtWQQfrO-O1021 (OKMOHSapk0.10 Sa**i OU+Ot^ithWOWKMtCOl t a u r u t K.im m m pui
D0OFO1-tMSWOO1-<MM11O4 (caMMflotma lo n k t ^ oac-roi-M swooi-oo4i im 100*4*40tpk Ol tM ppafl*i>
SpM JSO L
CsSufontmFFBS AmtFond Amount in Sm p NflCmnmo 4aoont)
.,,,B l
s _____
Amt Found Amount
Amt Found
NSnmp Rommmd Aapavwy inSampln
M U M t.*
(%>
16 Amount
(%\ '
10 0.12 112 71 2.30 120 7 100 112 70.4 70 2.30 MO 04
NR NR
NR NR NR NR
10 4 100 4J0
112
70
0.000
1U
toa
784
71
0.95
MJ
M
NR m
NR NR NR NR
10 34 10J 73 QJ40 10.7 8
too 2 ta
72.4 70 0.048 63.0 83
m m
NR MR NR NR
to 10.4 34.4 100 340 112 OS 100 10.4 4 7* MO OflJ K
m NR
NR NR NR NR
10 0403 0.32 S1
100 0.20S
764
77
ND 0.00 87 HO 66.2 M
120 120
120 177 07
to ND to o ir
100 NO
00.4 08
NO .12 n ND 03.0 M
102 102
110 189 03
10 NO fiJ4 02 100 ND 612 01
ND JO 01 MO 002 fi
U WA
103 * 182 10
10 ND 7J0 70
ND 720 73 80J
710
K NO 2.0 02 M> 93. M H jO 188 7
10 ND 7.00 00
ND 8.00 81
180
100 NO 013 01
HO
100 103
100
138 334 0
"I10 oaas 10.3 04 M3
100 OIN
0.4
122
17.0 3 113 106
NR MR
NR NB KR NR
NO NMR w M iH M n iy m * H im M M A ,M w y
Exygen Research
Page 36 o fl 32
Interim Report #10-Analysis of Fidi and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
Exygen Research
Page 37 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
St*N
OOU4WHPWOOM441104 icm mm ipak. 9 0 !) OOU^OI*(PW00MMM1104 icooiiin Mil M m *a**)
0OU#O1-IPWOO44WW11(M to o m m MCtoaoh*ai DOU*F01-iPWOO4*O*411<M (Caomts M 0 1MpooM*j
0OU-FO1*IPWOO8-<MM1104 tOBMMaIpfcC. 10* ipna) OOO-FOI-VWOGHWItt* 10QMMOOpKF,Its jpfc>pM)
Di>f0t-JPWC02-O-O4t104 (0800111 to*Q. ApOMlu) JX2-f01->W002^-04t 104 PH4MMtpkM.IOCm* If*)
011*01*19*0014-041104 <00904880*1,1 * * * )
DLt"F01-MSW001-0441104 01*1103 #}
OLI-F01-M8W002-0-041104 toowMiSaMt. 0Li-PQ1*W8W0Q2<<HHl104 *504*MiL 40m MM
PU^O1-MSW0ftl4M>411(M |OOOlH7C 14M40*) Ol1-F01-MSW00^Q^41104
Dt1*O1*M8WOO4-0'O411O4 {CO>o*fM. an*) CX1*01-MSW004-0-<>41104 pHXum r n r. toppphMU)
0U*01-W00*O-<*1104 (0PNWWSpfc6,sphS^ 0t1 *01-MSW0084M1104 (CaMNMMH. 0 *<}
DL1~f01-MSF001-0041104 (00004Tfl*t MfpfcMM OU*P0144SF001-<WH11W (CBMWIitphJ, HB*8 M a)
Amount AmiPound Amount
AmtFound ^nount
AmtFound Amount
SpMtf
tnRompN U N IM lt
Roco*r4 Wcomory hi Sonpto floonwornd 0> cu) CAM)4. NaMMlWL f%)
*8mpN
1Uco*ord R tcooy
10 112 100 112
10 34 190 349
10 3ST 100 2,97 10 144 100 104
10 U20 100 1-
10 1.30 100 u o 10 0960 100 0.500 10 090 190 OfiOO 10 1.1 100 1.18 10 ND 100 NO
m M.O 12.8 HA 10.3 3.0 1.40 K.O
10. ta t 0.7 00.4 0.82 012 0.62 4 0.00 *2.4 7.7 794
100 0.00 K OjQO 03 M2 96 M2 75 S.12 Ot b.12 04 ND w NO 4 0.008 M OHO 06 1.73 70 1.72 04 1.13 tf 1.13 7 0.900 04 0.90 7 1.10 01 1.10 7 0.31S w 0.310
18J 7
1M W9 IIS too 104 tra 111 112 12.1 100 191 98* 0.78 966 104 964 043 090
103 101 103 101 84 104 104 96 104 111 107 08 91 98 89 89 93 * 92 0
NR NR
NR NR NR NR e io 0.20 NR NR NR NR NK NR 141 111 HR m 293 383
NR NR NR NR NR NR M3 134 NR NR NR NR NR NR 201 266 NR HR 303 364
NR NR NR NR NR NR 91 116 NR NR NR NR NR HR
106 NR NR
101
-- *
m irrnrrti rnnurr r<ns fm ct he a 1" --'
NO NNd*dnNrbtMibffNfCNoNMllonaAlrf>N01p'|frMwoU|ht).
* * * * * * * fucrtod A to o u *ty contort to * toi uwc .
rwuHi am m a m * Tart* S.
Exygen Research
Page 38 o fl3 2
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P000U31
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
ta t*
DL1-P014ISF002-0041104 & m * n tm .* m DLl-F01-MW=0a*OO41104 (ON4MV1*U
PU-f01-MeRXKMKM1104 (C*#TiepC.-WwM*iw) DL1^144SF(W*)411<K {C0aM739kD>tQappl#M
DL1-F01-44SPQO44HM114 K m m n 8* f. 10ppa 0L1-f0l4ttr00<-O441104 geoinn M.#. *****}
ai-fOVMSTOMMMH1104 M . K NOM1
0L1>f01448F00SO41104 (OOWMM%#K *08m PM
DL1-f01JPN001<0041104 icowwTi** un m **> DL1-fCHPW001-Wt104 (ooNtm * j, mom m *
DL1-F01-JPW02-O-O411D4 <0064*10<pift,1Cp 0 6*w) DL1-F014PWOO2-OO4MO4 (OOOmNtpkL, t N M a )
DU-F0WPW003-OO41104 tcaoswirrsNc. **} DL1*TOHPWOOWW>41104 'CMM7I*D. * * *
OL1-FC1-VW0044441104 lO U M ll.tl.iliW M .I DL1>FC14PW00M>-04110* iNMT44|fcP. <*%*>
.-FOI-tmOfeO-MI104 toaoNsratpk. asaopRu OU-FOHPFOOa-WHI104 tO0ON4fONN.fft ft* 6p*
DI.-1-FO1-PF0WM41104 laM M lIH U lR k)
(CMMun^t j,
AnnFound Amount
A rt Found Amount
Art^ound Atrouni
* * r t mSMwm Rc.wrt Hmxrmy in lan d * NkowwI A ncnrj m sn w h
J S ttL 0WWM4*
M l at*
1*1
Rooovwd Rwurtor (%
10 ND 9.60 66 0.624 106 88
m
m NR
wo NO 4.6 66 0.624 864 ' 86
NO
m
NR
10 0204 8.78 66 0.652 102 05
100 0 4
4.4
64
0.652
862
86
HR NR
NR NR NR NR
10 NO 8.88 6 O.SM 10.4 86
NR
wo NO 6.0 67 0432 101 100 HR
NR NR NR NR
10 NO 844 66 0.064 10.1 64
100
NO
2.4
<2
0.164
646
83
m m
NR NR NR NR
10 0.772 9.64 7 045 8.72 86 17A 284 0
100 o m
4.0
0566
676
67
17.4
113 M
10 0.466 I N 2 0.SM 668 64 117 27.4 117
wo 0.46# 76-4 76 0536 66 , 87
1ST
100 64
10 NO 06
0406
644
82
6l38
100 ND 10.4 90 0200 108 108 36
t*.7 73 108 100
10 ND 100 NO 10 NO 10O NO
9,46 65 0230 OOQ 88 711 72 0.236 64 8 83
600 80 0222 648 61
86.4 61
0.222
884
88
SM 884
11.1 11.1
724 140 to 164 7* 108 8?
10 NO 660 m 0445 104 103 204 304 98
100 NO 766 79 D2K 804 M 20.8
108 88
NO taM K M *tt< tM < rfQ w tta< m < iM ak2nrti(M iM V t). W < N IW M M IW H llri M iaitM m 1^ -- n. iw J wMipwiMTK-I.
Exygen Research
Page 39 of 132
p. 40
Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
tenpte
Dc-i-f0i-rroo4*4iio4 (C0MMO1ipkX,Wppt)M
[(XC-O1M*W*)1HpiPtCF910*4aWpt4+11m04
Dt-1-I=01-IPR)OM>4>41104 ICON** C.14pi*pM
DtoLp-o1MFM0vHaPpRtWp.6m-Om-Q411n04i
OO-FOI-MOWOCI-0-041105 Wwnipfc6.iippMp4)
DfCLSW-FMOIt-tMIpSkW9.0m01-p0p-b041*10)6
DI3491-M8M0Q3MMM1100 |0BB4MM4^liC,mfpOOplM
ttXc3mHrFt0in1i-al6p6pWH0.0v2K-m-0*4*1*1+0\5
CX3^O1-MSWOOVO-041105 fCOOIMWOpal. tippMpM
0tCc3*x-f$Q*1m-M*8*W-r.0m00-<mHNm11n08
DUM^-MSWW-tKHUOS temmm** k. p* m i (X3-FO1-l4SWtXM-O-d41105 <OOOW468pkLO arilMM)
OOfD1`M$*0064MM1108 tOMriWd1|BC.PMMhii DOr01-M8W006<-04110S W*4W 8ptO.416ppM l)
00-F0144SPOOI-4WM1105
Dt3-'FQ1-448F0O1-0041105 (caotMaaamr.m ppMM)
PO-FQ1 MBPOOl0oil10ft WWWMts. 10peaSpew DC5-FO1-MBPOQ2-OO4110S (OriMMt*ift K.40ppaMM
D(tO3O-FOQW14-M0MfiF0MO$0-Om-OM411MO8
DL3-F01-MBF0t4M)4l105 BooewioM i moppeSaw
ABmfikosudnt t APuHniM*tP-Po-Iu-fnUd
Amount Row anal
ftnoovory
AmtPoinl nStmtio
Amount /laciwraJ H w fy
AmiFound *>Bom0
NMlM Ftooanond RMWWy
(W5rit f%)
D M * ("INI" OM
10 MO a.oo 80
too NO MJ m
NO 8.46 86 TM
NO OM 86 740
164 82 102 04
10 NO 7.44 74 0375 6.00 88 8.72 15.8 72
100 ND 54.6 80 0375 664 88 8.72
102 3
10 NO 100 NO
M 85.6 as
10 CO 8.44 84
100 KO
604 60
NO JO 2
138
NO 86.6 100 13
NO 6.92 88
180
NO 106 108 160
186
2 119
150 m
263 106
10 NO 6.80 86 100 MO 664 86
NO 0.56 98
146
NO 102 102 146
10 NO 6.46 86 0366 OJ* 94 m
100 NO 684 88 0286 102 102 186
10 NO I.M 88 0366 11.1 107 173
100 NO
100 100 0.3*0 106 106
m
10
NO 6.46 6
HO
11.4 114
116
XX) KO 64.8 60
NO
1M 1M
in
10 NO .M 90 ND 104 104 m
too NO to* 60
MO
103 103
11
10 NO 100 NO
32 83 106 81
NO 1 1 j0 110 75.8 ND 107 107 7U
154
354 m
225
301 10 13 m 248 n
138 * 234 114
MS 21 100
820 .
180 114
----r /'T ------- ktil rtfqrtt Xil
NNOft-N- tNfoiWtOMafretdwM*oaruWri*voaUrtrrtNw^Q*Muuir6M. RuaiwiM#^f6ci&ma2AiaraeMkfc>TWeH.
Wo>k jfcxa tw>inn-- y NUNthaw mn4ti w aftt. r w r vriu tt .aay*syrilM*yNw Uww -- m1 i-- 4.
Exygen Research
Page 40 o f 132
p. 41
Interim Report #10-Analysis ofFish and Clam Samples .
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
m p* Dmcrcdcn
Dt*F0l-4*3F0OMM>41105 (CBMMMm K, Qa90m DO#91-*ttfW<W*4f105 fOOMHOI L lta|
DL3F9l-M3r00O0-04110S lOeoixwa--c. toppaip--> DU-F01-M5F006-0-041106 tOMAOMMagao, taopaaM)
DMC-701-1PW00O0-041106 y x m m m o * m * OMC-FOI-rWOOVO-041X* ffO iam ip.
C64C-F0WPWDO4-Q-041>05 icaotom ipaaiO psbfaN i DMC*F01lPW0O*-O-O41KXS tem m m * hh iio**ipM
WHC^O1-lPW00<WW4l10fl toaniai--O panappatat^
OMC-m-*>wooo<W4iiC5 |OQ0MMnipkJ. tOOpaatfia)
DMOfOMiSWOCXMXn (COMMM** K. ** Ifki)
PWC-FQ1-M3WOB-04M1106
OMC*HH443W004*O411<)6 lceoMMri*c.ioapa9pMi)
DMC^OI4ISWOOMMMt1O0 comm* m a 4***)
OMC-f^4ttW0064HM1100 iCooweseai, tappa***
DMC-F014WWOCKWM1106 n w m kf. icofoa i m
DMC-W1-hrOGtt^-0411M {0BMMMpk0 ppkptof OMC-P01-M3F002-0-041106 |0tt**lpfcH ,tt0p|*6pll
DMC/C1-MSFQ09OO411 {OQUMOO*. .
DMC-fOV-MfiF003-0-041106 (COMMa6k4 MOsaoipa>
Araovni AmtFcund Amount
AmtFound Amount
AmNund Amount
SplMNt tiSampta Aaocwarad ftnoovw) n w n p i AmmwmmI OMMV) inlam e* liioow id Racovtry
MM.
- (%1
tna/ilwwwi (a)wt (%>
10 ND 6.60 w 100 MO 904 60
ND ' 1U> .. 110 NO 104 104
130 m
144 * 236 100
10 NO O tt 60
100 NO
006 06
ND ' ND
10.3 04
w* ' 01J 9 14
10 NO oae 63 C.396 ; 9JK2 01 . 612 100 NO 644 64 0.366 990 90 815
10 C.#X> 6.04
77 euee . 956
q' i 60
100 0.300
90/4
90 0396
104
104
66.6
72 161 9 7*JQ . 1$6 6
107 16 m
10
NO
066
BO 370
10.1
96 .64.4
100 NO 604 m 0270 106 106 64.4
79. mm
10 NO 064 96 0602 110 104 354 100 NO 92.4 62 0902 10 106 364
36 * 404 110
10 0.316 &S2 HZ 1.90 121 . 102 209
100 0.316
624
62
1.90
101 . w , ' 296
260 . 313 94
10 ND 016 92 Mao 11 M* ' NR
1<W NO
806 W MW
116 117
HR
Nft NR NR NR
10 NO 036 4
NO 104 104 NR
NR NR
1 NO 67.6 6 NO 104 104 NR . NR NR
10 NO 020 62 NO 10.4 104 66.9 100 NO V 3 67 NO 1W . n o , . 66J
101 104 137
I t i J 1
i
a w a M ) u * tMtfttn g M ritMtoMK
an KOrnMm r e n d in
NO Notdmnctndnt or*xu UrrttelQunnMMcnNoft I. 02 rV j !nt< 4 .
1*1-H a n m m t* m toa w t),o o n u a l Itm M M M M iiiM tiT O M .
la fe a r* * to .
Exygen Research
Page 41 o f 132
p. 42
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
mpls D*c rt*qn
OMC-f01'M8HXM4MM11Q6 K *om u MK. m mmi OMC-fOI-aWOMM1 IDS (CM40MtffcU 00*%*.)
DMC-W1-MSPD05-MJ41 06 H M DMC-rai-MSR*4WMt MS tcauaaa ipao, i0ea**M
0MC~F01HPFM3O411OS iceeuMilet t. * * ) OMC-R4PF003-<>01!06 IcrwimMpap, m m m m
DMC^9mpf0+<MH11* fOMlWt9pta,MiM M a) DM&F014PFM444MK0S {ooMtacam h. m m m m
0MC-r01-PFOO^MKI 1OS <O0MMa.*ai.aM.) C3MC-HPfa<W<I105 (COOM MtX WDf*t MM)
Dl*f0144aPaJ5-412M " M t. I M M OL2-ramnoc<M)4i2is leoowBM f.tean* ape*)
OL5F01-4FWOC84MM1215 leaasMM4aec. taae^*) OU-MHPWOO<K>4t21 (comeasepad, ieiea m m
DQU-WI-*ISW002<WM1218 (OOWMMI. M H tlM
DOU-F01-MSW002-084121* trIIIM *(X m *tal
OL2-fO1-IPW004-O*<t?18 tOMSMirae^ * * * * ) OU*FOt4F>WOOMM>412ia (oonaw *** nom rn)
DOIMWI-MSWCaMMUttM to * * * M r* WMkMM
DOU-M1XI8W003-WM121 < caaaM tjpki.iaie*iaaat
______ W M w i f f w ____________coopjorM oPng___________ coajM M .P F os
M tFcuM ISMKM
faoow ic R*cwo
A rt Found Amount to ta w * ftaccsMrad Racmaq
AmtFaun IntaW *
Amount ftamwrart
<nota)
arttwat.
>
(%) '
10 NO 8.76 n
0554
11.1 108
11
1M NO m o 08 0584 107 107 118
123 228 HO
10 ND too NO
0.52 85 9.428 122 118 83 *4 0.420 110 110
148 148
193 * 280 114
10 NO 7M2 ra NO 10 108 7.02
too NO 82 K
ND 108 108 7 .8
180 81 101 83
10 ND 7.BB 7
ND 107 107 44.0
552
100 NO 032 S3 NO 107 107 44
134 0
10 NO ioo NO
7.90 79 75. 70
NO 103 103 484 NO 064 8ft 404
54.4 121 75
10 NO 0.44 84 100 NO 115 3
NO 1O0 IOO 485 NO 102 102 40
0 100 142 93
10 NO 100 ND
*00 80 04JO 08
ND 11 11 112 NO 107 107 135
22.7 96 121 108
10 OJM
.e
87
172
108 82
NR
m
NH
100 0508
72
07
1.72 02
ot
NR
NR NR
10 ND 8.08 81 NO 10.4 108 0.80 14.8 80 IOO ND 750 77 HO M 2 85 5AO 875 00
10 NO t.i a 1 10.4 i9 4 80 NR Nft NR
100 NO 884 88 10.4 IDS 98
m
MR NR
nSoam-pleNmoetMdmiMaecBWceaiiritytMahaitrwtioatUa rmt ee4ceiQrteu*w4 w9 ;i^i*wrty*Aaenoa.cltmurAaawieciaaWneyiteLeiiie'O rtw in
*0t<xraeQrtM *wiQU0% ao n M im Jite b ra *. emyetew--a i i a r e i n re n ta l.
Exygen Research
Page 42 of 132
p. 43
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Tabic IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
Sampfc
DO*P14PW004-<H>41130 to a m m apo,RM t DL2f014PWQO44M>411 <0*ww eoia. hmwSo*)
CXXWJVM8W001-0>0*1?15 tpam tm ** 4, * oooaaM
OOOPOl-MfiWOOI-004121 tcooioaooMi* loom arto*)
DOU*91-MSWO04.(HK92I6 . icoiiiiiM>.iioaaioo}
OOU*O1'MSWO04-frO*l2l6 fQMBOMM1*00.1 MObOBo)
000*91-M6Wa06<0441216 (ceenoii %ee, w jiii*ei
DOUPD1MSW006-044121 MOMMI*> * HO*|| i)
oou#oiam 5^M M i iCcomin B*&, ***) OOU-701OtSFWMKMttli (COOWMNIpl 0,00000ObpO>*>
tX3-F0HPWW<W>41130 icnw m p1, poo **> DL3-FOWW0W4W1130 oowiet ueM ia mnioeii
O O f01*#WOOHXK1130 iciM im to aw o * M t OU-FOHPW0060-041130 (CMMMOIiife H, MOppaB0M}
D tx w i-M sro o w x u ie lOHIHMmiHO *I DOUHFO1-MSF90^0412ie MOMMIIH L 1 IbMpNa
DOC#01-3FOOO-S-01210 (CammoriokC, toppooMi)
DC-FOHM8FOOO*1*<M121 MOMMT4*0,1 * * !* )
D8C*01-*FQMWmi6 *!)
OBC*D143FOO4441216 Mommim u w 10010*01
SiSugonrttPPBS
C$$*MonoPFH6
CMuMamto PF08
Amount Mot Fount Amount
AmtFound Amount
Amt Found Amoirt
So m m an^t* Raoowamd RMMiy InSmpln R io n m n to o m y InSampla Rowrd Rnoomy
(" iti--
1%)
I
10 HD 7.62 75 NO 11.0 110 7.V 100 NO 604 66 NO 118 116 7.K
172 04 114 m
10 7 . 142 75 154 2/S 121 m
100 7.00 SS2 76
154 122.0 107
NR
KK m mm
10 4.72
ton 1
m
292 76
100 4.72 722 66 217
104 2
HR m
mm NR m
10 0.30 7.08 67 12* 667 72
too 0264 7Z0 n
w * 07.0 48
m
NR
NR NR NR NR
10 1.41 6.60 n
a.40 172 2
wo 1.41 72-0 71 640 94fl 6
HR m
HR NR NR NR
10 NO 7.02 76 NO 8.04 80 13-0 166 48
100 NO 12 61
NO 1K 110 1X0
106 W
10 HD 7.86 4D NO VJ8 . 80 0.44
122
100 NO 6M *4 NO 103 12 6.44 02.0 67
10 1.72 00 73 4M
100 i j
1M 06
ss
142 77 1 100
m m
10 0220 128 SI 100 220 3.
1.78 115 . 9? f.78 886 85
m m
NR m NR m NR NR m NR
10 NO 426 64 ' 1J8 114 97
100 HO
60.4 81
1.06 6
88
m m
m NR NR NR
Swiiyw M o si* IhoapMripjeweleigNicwn^ iw<br%e-eoM*iwpy miuoewnotbo
NO Not<i^ecdotorabowUmKdQuaritiloikinwNchiBa2n^g(wotw*flN). .
turn** HmmMN NotraaortM duo to aty oanoolmHNMvfot. No mot) m
wo Qi To a.
..
Noiot dtnoo mto ooouoasytib ia oNoaooomodod fooadlo^ noooo^y%ulmo v^opababt^ boau tbo oataoo to ibo moo
Exygen Research
Page 43 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
sw wa
OOU-f01-M8fO3-0-04l2t* teowMwspfci. K w tv> DOU-POI4USF002-0.041318 (CMB444*lpt1K np* %*}
W01JPWO0I-WM11* <C00M<x>c. i4m1Mo| DI3R014PW001.04M1I tc**04nm o.t*tsj
DOtJ-FOl-M3F0CB-1<041210 ica m tu i*auopp*M)
OOU-F014kf002-i>04l21 (CMBW7I tVkJ.10R|Mfa]
OOU-FOI-MafWfcMMttlS ICMMnR*K.W%la| OOU^01.SF0044M41?I ICMM471* L m m Mnj
00U-F1.M VW 1444iaie n * * 114 ***) 0004=01KFOOI44M121 (oeoMma* r. m m M
W&Ffrl-MaMOKMHMU (OotMinI* a m Mo) 0>f014K*F0034W>t121i IC1MIWI#M, <Mwt0)
MOFO1-MFO0MM4121 xO M ni*i.wot*.>
oa& foi4wsroo444i2i W M iU i*to>|
DMC-F01-M8RXI1-0-04121 iaoia<*c. **>) OMCAN-MtFOOl-044121 tm u 7 9 i+ a ,m i9+9+*)
0L1-f01-*W0t*4W>l 12'# |COWOI77t>,'OwOM~) 0L1-F01-VWKHMM4121#
<0#M#|#M)
OL2^014PWO4-Wl20t I#R 1*
OU-F014PWOOM441! K 3 n t^L .iain*aM )
9PM thafa)
O im -- OOfM____________0Su*onoloPfH8 AmtFound Anounl
ninwdpm Oh m t n NtCOMWIf OtSomoN Wnanond ItaeoMH) (MtlMtHL
C s& 4 t t.P r0 8 In Same* Ok o iiw I INoowy
Ml
10 0.684 0.24 84 488 14 98
100 a m
810 83 4.50
104 *
MR MR
10 NO 7.10 70 024 020 00 8.04 too NO 82J 4S ai4 101 101 024
10 0.840 20
84
480
142
00
100 0.840 820 81 488 103 08
NR NR
10 0,782 7.7 70 225 <20 0
100 Q.T92
812
80
226
062
83
NR NR
10 3.(0
11.1 80
102 302 0
100 3.11 2 1 102 104 3
m NR
10 NO 100 NO
8.4 86 4.0 M
2.00 112 M 2jOO 108 104
NR NR
10 NO 7.72 77 187 122 n 100 NO 75.4 78 327 082 os
NR NR
10
NO
ftoe
fl
0.430
8.08
07
NR
100 NO 88.0 M 0.420 102 102 NR
10 0.253 7.40 71 0.844 0.98 13
82
100 0253
72A
73 0.644 882
80
082
10 NO 7M 70
NO 8.04 0
7.48
100 NO
71j
73
NO 02.0 2
7.48
NR NA 172 103 NR NR NR NR
NR MR
NR NR NR NR NR NR 832 145 117 842
m m 82 83 MR NR NR NR
NR NR NR NR NR
NR
76 2 77
NO - Not *l#etd Nor60* UmofQuwKntinnMe*#
I * * *
M w ll* l> W * k
Exygen Research
Page 44 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
Table IV. M atrix Spike Recovery PFBS, PFHS and PFOS in Fish Samples (continued)
Snrapld
S0M
C tSuttrtM PFU
ktam pl Naoowand ftneovary OoMwlat
kl Vtfnkt
AlNMlt Qrorad Racomry
r%)
et
.... tittm t n ta m m i
m ii-- f%\ '
CO^01<rW00MHM1201
fC H r?nat, DU1-8W00W-O41201
19 NO a.io 82
NO 1.96
4.m 14.0 81
K m m tnim r a maM m
100 NO
M
80 NO 97.2 Vf 4.69 M.4 U
Aaarapu Tf OtandandOaatadaii4 19
in * t
o
NO r** 3MCM orboxa U n ) O QuantMan wen (u am ( * p a ).
NK>NMi*palM4MI>ia0MMMUKWl>W. WilM cil>n iy W rtia. . row^da
M im ifc l,
rrtr,m. M
O nW w it
a
UndafdDM imt:
Exygen Research
Page 45 of 132
p. 46
Interna Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table V. Matrix Spike Recovery of PFOS in Re-extracted Fish Samples
Sample Deecnption
D B C -F 01-IP W 001-0041021 <0004*101S (* C , lO M ppb)
0 021D e C - F O H P W Q Z -(W H t pfb)(C0040102 $pfcP , 6000
1 003 21D B O F f l -IP W ^ W M in 40 3<coo t s s < * f c (o o o w b )
T C(0U00-F400116-4IP6F9k00a,11-<0H00)4p1p0b)21
D 0! j- F 0t-( P F 002-0-O41021
(C o o M ia s a p ta leoopp)
10?1O O t'- F O t -IP F O O M M M (00046166OpO*. IM O feb)
D O U -F 0M P W C 02-O4M 1021
lcaMaiaSii. t o o o m o
O
B(CC0-0F4O041-0M04S *WJO.
OH W
M X 1104
OO**!
O flC -F O l-M S W O O 2-0041104
(C Q O aai s p k K, i b a o ppti)
O 0C -F O 1-M S W O O W W J41104 004946(C flpK L, IPpOO ppb)
D B C -F 01-M S W 004-0441104 (Coo***ifk MlJOOO ppb)
D B C -F01-M S W 0050041104 <0004446* S o . N. 10,000ppb)
D S C -F 01-M S F 001-0041104
(COM akc. io o d o m b )
4O B C W 44S F 002-0-041104 1000*4464SpkO. 10000ppt>>
D B C -F 01-IF R X 0041104 (000444686)* E. (000)eb)
104D e C - P O W P W O O W M t 004 m)fO *att git tt, w o o
DBOF0 1 4 PW0 0 S4 MH1 1 0 4 (CO O *** 6 (4 a 3000 ppt)
100044*41 1000D O lW 'O U P W O O S -O -O O IlO O
S p tH
mb)
O O U -F 014P W O O *4W )41104 tx&maaak). im o *
0O 0-F0H P W 00W W H 1104 (000494033p k J. 4000m b)
D U - F 01-M S W 001-0041104 (00044406Spk )C 1000ppb)
O L 1J=01-M S W 002-<W141104 (00044400e * * C 100094b)
D L 1-F 01-M S W 0014WV4110 (00044401ak 0,1000ppb)
0. 1-F 01-M S W 008-0041104 (C0044400Opb a . IMO 9P b )
Amount Spiked ( n fr'fl)
1000
sooo
1000 1000 1000 1000 1000 10000 10000 10000
sooo
10000 10000 10000 1000 1000 5000 1000 1000 5000 1000 1000 1000
1000
c a Su<onata P f OS
Ami Found ki Sample ( i o t a ) **el 4
Amouni Recowarad (notai welwt
20 2880
3330 8880
IM O
808 838 644 1210 480 7820 12800 3440 5240 5240 4780 608 1230 2620 2270 1740 21
BOO
706 868
3180 1780 1740 1650 2010 23200 18800 23200 8520 16200 14400 15200 1600 2500 6520 2840 2740 7800 1880 1780 130
004 1680
NoinspoflK)dMloquatkyto rtiti re** Mura.VlfcMan no(ladudMIn aunmaryabate.
Recemwy (%>
78 107 150 11S 110 111 140 137 81 100 102 100 82 104 88 135 78 37* 100 108
SS
107 123
108
Exygen Research
Page 46 of 132
p. 47
Interim Report# 10-Analysis of Fish and Clara Samples
Exygen Study No,: P0001131
Table V. M atrix Spike Recovery o f PFOS in Re-extracted Fish Samples
Sampn 0 --citation
(continued)
c a sunowia p ro s
Amount Spikod
Amt Found In Sampt*
(nota) m l wl
Amount Racovond
Recovery <>
DH-RM-MSRXH^HKIKH
(C004KT13|*r, m ppd)
1000
G0 - . 1890
112
DL1>F01<MSFOOMMM11M (cao4ams)*Q.WMp)M
X
432 '
1570
124
CH ,1W 44SF006^041104
(COMMTitpft H, *00 ftft>
,1000
740
1#30'
109
MC-P01-M3W005-0-041105 ,
(COMweeapM.ioooflph)
'
1000
seo
1730 '
122
DMOF01-M3F00MMM1106
(G*Mft03|*.i. 1000ppb)
1000 620 1500 88
DOU-F01*t5W0024H>4l210 * tCt*60**3e*K. 10,000000)
10000
28200
32700
48
OOU-FOI-MSW03-0-04121 (CMMKSpkL.KMOpobI
5000 :
4040
10200
123
DOU-F01-MSW001-0-041216
(C00M440 toil C, 10000poh)
10000
7800 25000 174*
DOU-fO1-MSWOO4-0-O41216 <0006*16*0,6000**)
5000
5120 8660
96
DOU-f01-MSW006-0-041216
(COOM82Spft E. 100QppO]
1000 48 1760 126
DOU-f01-M5F005-0-0412l6
(0006*463ScfcF. 1000 R*)
1000 720 1820 110
OOU-F01-MSF003-(V04121
(OOOOMOOOfdt Ck1000 ppb)
1000 48 1720 87
D6C*F01-MSF005-1-041214
(C00MW07SpkH, 10000ppb)
10000
9320
32400
230*
DBC-F01-MSFDOWHM1216
(C006440*$pk 1.10000ppb)
10000
SIMO
24100
151
OOU-F01-MSF002'C-041210
$700964*0SpkJ, 1000ppb)
1000 40 1720 108
DOU-F01-MSF002-1-041218
(0005*4711(* K,1000m)
1000 92 1960 126
XWtal-WSKXM-O-MtSia
(Coatwn st u iooonb)
1000 1S20 2700 38
DOU-F01-MSF001-0-041216
(C0O9M73 9pk C, 6000H*}
5000 2070 7980 116
OBC-F01-MSF003-0-041216 (0000*474 Sf* D, 1*000pp*
10000
4640
15500
109
D6C-F01-MSF0M-O04121
IC0Q604S8* 8 . 0000HKD
10000 8280 24500 152
DMC-FD1-MSRX31-0-041216
(C006047BOpt F, 1000ppb)
1000 40 20*0 120
D8OF01-IPR>0MWH1021
(COOM14*Bp*Q, 1000 ppb)
1000 304 1360 97
09C-F014PF003-0-041021
(C0040180Spit H, 1000ppb)
1000 209 1340 106
DOU-RM-iPF005-<K041021
(Ca04B1fl*pk t, 1000ppk)
1000 359 1400 104
*Not report! A n H><|ui*ycnnMmaut Mum*. Vafcnt an notM udad in I n K inm y m u te .
Exygen Research
Page 47 of 132
p. 48
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Table VI. M atrix Spike Recovery PFBS, PFHS and PFOS in Clam Samples
fternpb
XJ^1^FWW1-tM*121ft tooomiQ-- c. f--
DOM1-CPW001-<M1Z16 |0Pi-- ft 10--)
DMC-XM-CfW00l-W>*12ie <c-- m -- t, --
DM^*>1-CRfWI^O*t31B a -- ia* 7 .-- i
OU-W1-CPWQD14M4121* ccn--t t -- *)
CL2-1-CFWtDHW*1?16 KO-- HTfciHWOff
OW1-CPW001-0-84121 tOBCM-- K * m
DOC-C1-CfWCC1-<WW12l5 IP--im -- 4 -- flpbl
OLUQ1-CPWO01-O-841218 (COO--M -M , * *
o u m & w W 'W m 0-- lUKOpp>)
OOU4Ot'Cfl*Q01`O-Ot121ft (C-- MM.1O0--
OOUJOl-CFWOOl^Olt2l6 (TP-- lS<*KW--)
Amount AfftFOi-- ftoftad
ND
Aummm
Amt Found
R-- i Rapp--y hSumf*
IN 0 NO
Amount
And Found
HdOWW) N*ctwy H8dmot
i*>
lift 2 1
Amoud Huwnmd IlMouwy
132 a
100 NO 2* 2 NO 8 ft 182 982 83
10 ND ft04 0 NO ft44 M 8.19 11.8 81 too ND 29 S3 ND 88.9 m M 2.8 *7
10 NO 1 ND
7.29 73 NO 90 * ND
784 7 i t W 101 1*1
7-84 ST a * AT
10 NO 10 3 m ND 10ft 108 4.4ft 130 1 too ND M4 ft* NO *7.2 7 4.48 * 82
10 NO f t m NO f t 3 8.90 160 5 100 ND 92 NO 103 m 880 m t 08
NO
140 & 0202 # .
1 11.4
172 4
100 ND M4 ft* 0202 BOO ft 11.4 80 7
f1t0* 131 >9* 7n1
NNOote*--Nold-- cMuatnoitr--ab>m>NawU--i0M0nf4Qu4amn--m.artviN chl9.2 flQvffyt(iMftgtwNafVr--*).4<--ttn--4--.
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Page 49 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
FIGURES
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Page 50 o f 132
Interini Report #IO-Analysis of Fish and Clam Samples
Exygen Study No,: P0001131
Figure 1. Typical Calibration Curve for PFBS in Methanol
0910001 rkfc.rit(PFM)c*UooaPftfr"**ft /VwelfMNigyy 1.3 1 *4 0 0 4 *>jr?**4m(r O.OOOQ)
A na, m unti
Exygen Research
Page 51 o f 132
Interim Report #10-Analysis of Fish and Qam Samples
Exygen Study No,: PQ001131
Figure 2. Non-Extracted Standards o f PFBS in Methanol, 0.0005 lig/mL and 0.001 ng/mL, Respectively
I
nArnatt:-MpflwutaMuiMmMofMwr*
mm
M>.
lit
im
mninm
DJ1
0
tntere*.cp
IntanMf, cp t
Exygen Research
Page 52 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 3. PFBS in Control Fish Blank, 0.00625 |ig/m L Fortified Control Fish Spk A, and 0.025 pg/mL Fortified Control Fish Spk B, Respectively
MW*
MV* f M x w f M H M l ' M M f t f M l n m MNMCMHr
Exygen Research
Page 53 o f 132
Interim Report# 10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 4. Chromatogram Representing a Fish Sample Analyzed for PFBS (Exygen ID: C0049478, Data Set:061605E)
zn .IM .ta m * -*m v
M
fMSEari r
Exygen Research
Page 54 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 5. Typical Calibration Curve for PFHS in M ethanol
Ama. m unti
Exygen Research
Page 55 o f 132
'i^ u v -'l
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Figure 6. Non-Extracted Standards of PFHS in M ethanol, 0.0005 pg/mL and 0.001 jxg/niL, Respectively
w m n - fifM
Anm
fitm i iQ
HH&t 141
*7 ftJ 4
M tm s L wm
TOO
eoo 000
400
300
300
100
| *1727 P fU t ( t W * * ) e D 0 * MM. U -H * *
* u : 3 3 ir t mm*
13*0. m *T: 10J M R
Tim. nUn fc*mO61O066*W
1033
14
it
04v
'0 1 u ie u
Tim , min
ccb 'sutiui
Exygen Research
Page 56 o f 132
tm w tift.cps
Interim Report #10-Analysis of Fish and Clara Samples
Exygen Study No.: P0001131
Figure 7. PFHS in Control Fish Blank, 0.00625 pg/mL Fortified Control Fish Spk A, and 0.025 jig/mL Fortified Control Fish Spk B, Respectively
CM** * P fm MtfflNNNQ
-mm* *
NfM C
* * 7 2 1 * 1 Mills HHaMJ0100.eps AT: 10.4 m *
12*4
9 10 11 1 14 10 1C 17
Tim.
intanr, cps
MwwUr.tps
Exygen Research
Page 57 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P00Q1131
Figure 8. Chromatogram Representing a Fish Sample Analyzed for PFHS (Exygen ID: C0049478, Data Set: 061605E)
m n m t t m a imm W f t r a k t t * tm m m tr
Exygen Research
Page 58 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 9. Typical Calibration Curve for PFOS in M ethanol
OMOOSC F *h.i* ( n o t ) *UM>r > H M ln ( " I /i f
- l.1 C 0 0 4 s t 33tHXO (> OMSS)
A na, count
Exygen Research
Page 59 of 132
In K fta fe .cp *
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Figure 10. Non-Extracted Standards of PFOS in M ethanol, 0.0005 jig/mL and 0.001 pg/rnL, Respectively
I ffjm -A R *
* * * * * * MM -m m *
ATM? M H ti w O AWfl*fe 4 n * n tlim im
H f$MfiMT
1 2 .
un
ta rn aro t
2 tat fr* otitoac.*#
Am #- 4 4M 7 M V * H cIflM r 000 * * *T: 12 J m\m
700
too 000
400
300
300
100'
< Jts>
e 7 t t 10 11
Tn. *la
124 12 3
^ 1.....war......
14 1 18 7
114 10 17
I'rtenW , tp _
Exygen Research
Page 60 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: F0001131
Figure 11. PFOS in Control Fish Blank, 0.00625 |ig/m L Fortified Control Fish Spk A, and 0.025 pg/mL Fortified Control Fish Spk B, Respectively
drM flM N w M
K ft 72.3Ar
12BO
1 23
40
*7
00
I ftM fant I p 9 . PF0 9 (OC).0*0.0 s * w . wmpN 11 of **m OO1*O0E9
Art: 207141 omi* NaipMr 10000. ** 07; 12-0
10 11 12 1 1 1 4 1 0 1 9
17
1 2 0 4 0 0 7 0 9 10 11 12 13 14 10 10 17
T lr w .n l*
Exygen Research
Page 61 o f 132
Interim Report #IO-Analysis of Fish and Clam Samples
Exygen Study No.: POOO1131
Figure 12. Chromatogram Representing a Fish Sample Analyzed for PFOS (Exygen ID: C0049478, Data Set:061605E)
I c n mm -fifo t (M a m *) t lW w -mwJt nanafm m MNMF.aMr A n t i m W t iM k Jfc fe M r Q I M lw > M l i n t m t *
Exygen Research
Page 62 o f 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
E*y*ra ProtocolN uni*r P0001I31
STUDY PROTOCOL
Study Title: Analysh of Ferfluorobutanesulfoute (PFBS),
Perfluorohexanesalienate (PFHS), and Perfluorooctauesulfonate (PFOS) io W at1, Soil, Sediment, Fkh, Clams, Vegetation, Small Mammal Liver and Small
Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program
Exygen Protocol Number: POO0H31
Perfotming Lahnn.tnrv Exygan Rggeanh 305S Research Drive State College, PA 16901 Phone: (814)272-1039
Snonaor Remeaeatativc: Michgel A. Santoro Director o f Regulatory Affairs 3M Building 0236-01-B-10 S t Paul, MN SSI44 Phone: (dSI) 733*6374
Aigr t *4 6$
Exygen Research
Page 64 of 132
Interim Report #10-Analysis of Fish and Glam Samples
Exygcn Study No.: P0001131
Exygca Protocol Number: FOOD! Ill
DISTRIBUTION: 1) laiaiinha Ketari, Study Director, Weaton Solution* 2) Join M. Fliherty, Principal Inveatijator, Exygta Raaeareb 3) Michael A. Santoro, Sponaor Repreaentativa, 3M Company 4) Exygcn Rocwcb Quality AaaurinceUnit
Exygcn Research
Pagi le ft s
Page 65 o f 132
Interim Report #10-Analysis o f Fish to d Clam Samples
Exygen Study No.: P0001131
K xy|ea Protocol Number POCO113 1
PROTOCOL APPROVAL
Stady Title: Analym oiParfluorobutanefulfonaie (PFBS), Perfluoroliexmeeulfbnaie (PFHS), end Perfluorooctoe*ulfctute (PPOS) in Water, Soil, Sediment, Fidi. Qem t, Vegetation, Smell Mammal Liven and Small Mammal Serum Uaing LOMS/MS for the 3M Decatur Monitoring Program
Exygen Protocol Number: P0001131
Exygen Research
Page) oftS
Page 66 o f 132
Interim Report #10-Analysis of Fish andClam Samples
Exygen Study No.: P0001131
ProtocolNumber. P0001131
TABLE OF CONTENTS
TITLEFACIE----- -----------------------------------------------------D tsniB unoN ---------------------------------------------------------PROTOCOLAPPROVAL.,______________________ _______ TABU OFCONTENTS......__ _____ _______________________ INTRODUCTION____ _____________________ _________ TESTMATERIALS_______ ____________________________ OBJECTIVE_____ ______________ ___ _________________ TESTINGFACILITY_____ __________________ __ _ _______ STUDYDUtBCRM._____ _______________,,______________ SPONSORREPRESENTATIVE.__________________ ________ PRINCIPAL INVESTIGATOR_____________________________ PROPOSED EXPERIMENTAL START ANDTERMINATION DATESEDENTTPICATIONANDJUSTIFICATIONOTTOETESTSYSTEM..... SAMPLEPROCUREMENT, RECEIPTANDRETENTION_________ SAMPLEtDENTOnCATlUN______________________ _______ ANALYTICALPROCEDURE SUMMARY____________________ VERIFICATION OPANALYTICAL PROCEDURE___________ ...... METHOD FORCONTROL OPBIAS________________________ STATISTICAL METHODS_____________________ OLPSTATEMENT___ ___________ ___ _______ REPORT__________ __ ____________________ SAFETY AND HEALTH----------------------------------AMENDMENTSTO PROTOCOL_________________ DATARECORD REEPINO_____________________ QUALITYASSURANCE____________________ _ RETENTION OPDATAANDARCHIVING. .. __ _____ APPENDIX LANALYTICALMETHODS__________ _
...............2
..... ...... .......... ...*
............................ 3
-------------- J
..... ...........
--------------- I
-------- --- > ___________ *
-,............... II .......... II
______ 13
..............-- ...13
.................I
.......................... ...1 3
Pair i a f i i
Exygen Research
Page 67 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Ey**a Franco! Nun*rl>0MU31
INTRODUCTION
The putpoae of thia etudy i to perform intlyei* for perfluorobutenesulfooale (PFBS), periluocofaeMneeulibnetc (PFHS) and periluorooctencaalfonate (PFOS) in water, toil, sediment, fish, clam , vegetation, (m ill mammal liven and mail mammal aarum using LC/MSiWS for the 3M Decatur Monitoring Program.
Thr study will be audited for compliance with EPA TSCA Good Liborstoty Practice Standaida 40 CFR 792 by the Quality Assurance Unit o f Exygen
Rmadi
TEST MATERIALS
The teat material are perfluorobuUneiulfonate (PFBS), pa-fluorohexsnesul(boats (PFHS) and perfluoraoctanesulfonata (PFOS) and am all supplied by 3M.
pros
Chemical N an e PcrihaorabutaaewlfoMte Molecular Weight: 334 supplied aa the pomatiurn salt (CFSOj'K*) Lot Number 101 Purity; 96.7% Tmncitiona Monitored: 299-a 99 Structure:
PFHS Chemical Name: Petfluorarimcaiumilfooate
Molecular Weight: 434 supplied aa the potassium salt (CtFijSOjTC*) Lot Number SEU36 Parity; 9I.6H
Transitions Monitored: 399 - 80 Structure:
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Exyyra Protocol Number: POOOI I] I
pros
Chemical N m e: Periluoreoctanagulliornlc MolecularWeijfit: S3S tupplied at the potauiuin tait (CiFitSOjX*) Lot Number. 217 Polity; M.9H Tnmaitionr Mornred; 499-*99 Structure:
OBJECTIVE
The purpoee ofthi* itudy ie to perform aoaiye for perfluorobumnctulfonatc (PFBS), perfluorohexiaewlforut (PFHS) and pcrfluorooctumulforuiK: (PPOS) in water, toil, aedacoi; ibh, c b m , 'nguaoa, m ull mammal liven Mod m ull mammal aenim for the 3M Decetur Monitoring Program using the current veniona o f the (bllowing Exygtn analytical methoda:
V0001780: "Method of Aaelyrie far the Doterminetion o f Periluorooctanoic Acid (PFOA) in Waterby LC/MS/MS"
V00017SI: "M*hod of Analyst tor the Determination ofPerfluorooctanoic Acid (PFOA) in SoU by LC/MS/MS"
V00017S2: "Method of Analyste for tho Dctcraunation o f Perfluorooctanoic Acid (PFOA) in Sediment by LCMS/MS"
VOOOI783: "Method of Analyait for tho Determination of Perfluorooctanoic Acid (PFOA) in Fiah and Clama by LC/MS/MS"
V0001784: "Method of Analyaia for tho Determination o f Perfluorooctanoic Acid (PFOA) in Vegetation by LC/MS/MS"
V0001785: "Method ofAnalyaia for the Determination o f Perfluotooctanoic Acid (PFOA) in Small Mammal Liver by LC/MS/MS"
VOOOI7S6: "Method of Analyste for the Detemiinaaon o f Perfluorooctanoic Acid (PFOA) b Small Mammal Scrum by LC/MS/MS"
TESTING FACILITY
Exygen ReacaiGh ' 3038 Research Drive ' State College, PA 16801 Phono: (814) 272-1039
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STUDY DIRECTOR
Jatsm ht Ksaari P.E., DEE W*!oo Solutions, he. 1400 WeMon Way Watt Chester, PA 19380 Phone: (610) 701-37! Pax: (010) 701-7401 jJMMKi@weit!atioM.coa
Bxytm Proemi NumberPOOOim
SPONSOR REPRESENTATIVE
Michael A. Santoro 3M Company Director ofRegulatory Affair 3M Building 0236-Q1-B-10 St Paul, MN 55144 Phono: (651) 733-6374
PRINCIPAL INVESTIGATOR
John M. Flaherty Exyym Reaaatch JOSSReaearcti Drive State College, PA 16801 Phone: (814) 272-1039 johaJU herty@ exygom
PROPOSED EXPERIMENTAL START AND TERMINATION DATES
b la proposed (hat the analytical portion o f (Jut study be conducted from
October O', 2004 to Deceither 31, 2005. The actual experimental atan and
Nrmfnl iofiditw will be included io the final report.
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B zyye Protocol NnnAcr PeOOIDl
IDENTIFICATION AND JUSTIFICATION OF THE TEST SYSTEM
The following art lb* last ayrtw u for (hi* tudy: Water (groundwater ad aurfhcc water) Soil Sediment
FWl
Clara Vegetation Smalt Mammal Liver Small Mammal Scrum
The ample will be oollected by Weeton Sedation. The control ample will be purchaaed and prepared by Die teeting facility. Purchase and procening detaik for the control ample will be included in the final report auocialed with thla tudy.
The tet lyitena were choeen to ecceu the environmental impact of PFBS, PFHS and FFOS in the Decatur, Alabama area.
SAM PLE PROCUREMENT, RECEIPT AND RETENTION
Water, aoil, edimant, fiafi, dam , vegetation, mall mammal fiver and mall
mammal actum lamplei will be received et Exygcn directly from Weeton
Solution. The detaile ofample procurement fix ihia study are outlined in the
3M woifc pies entitled "Flure 2 Wodc Plan for Sampling Environmental
Media." The umber and typae of tem pi collected will vary depending
availability la the field. The total number of ample received end analyzed
fcr each matrix will be documented in the final report uaodated with thi
atudy.
.
Water, aoil, aad aeduneol ampfes will be uaed received without ftuiher proceeaing at Bxygea. Tbeae ample* will be arored refrigerated at 2 'C J T
Pith, dam , vegetation and amall mammal fiver aampl will be proceeeed acconliiig to the appropriate analytical method (tee Appendix I). There aem p l w ill be eeorad taean at s -U T C . Small mammal w hole blood sample* will be centrifuged in the field tu b e tune o f collection rod the reram fraction will be used far die ready. Small mammal icrum will be stored frozen at S -10*C.
The receipt and pencoaemg of tbe tem pi will be documented in die final report and raw data aeeociatod with the tudy.
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SAMPLE IDENTIFICATION
E cran Pnxneol Nurtatr. POM!U I
Prior to analysis, each temple will be assigned a laboratory simple reference iwmber. The rahm e number will be unique rad will dittinguish each Jubowtwy am ple tbit ii pmeened throughout the analytical procedure. O m autognphic data will be idaaified by the laboratory simple reference number.
Sim pk (tonge canditioni iud b a to n s will be documented Uroughou! foe study.
ANALYTICAL PROCEDURE SUMMARY
Retcmocre: Y000178: "W etbai o f Analysis fee ihe Detamination o f Perfluorooctinoic
Add (PFOA) in W sterby LC M SM ST VOOO781: -Method of Analyau for the Determination o f P(*flt*xooctanoic
Add (PFOA) in Soil by LC/MS/MS" V0C01782; "Method o f Analysis for the D utennnitioii o f Perfluorooctinoic
Acid (PFQA) tn Sediment by LC/MS/MS"
V00017S3: "Method of Andyiie for the Detetminutioa of Perfluorooctinoic
Acid (PFOA) in Fish rod d im s by LC/MS/MS" V000I7M: "Method o f Anutym for tho Detenniuitioa o f Perfluorooctinoic
Acid (PFOA) in Vegetation by LC/MS/MS" VQ00178J: '-Method o f Analytic for die Detetmiaation o f Perfluorooctinoic , Add (PFOA) m Small Mammal Liverby LC/MS/MS" V0001710: "Method of Analyiii for the Delenmaation o i Perfluoroociamxc
A dd (PFOA) in Small Mammal Saum by LC/MS/MS"
The above methods m e analytical oondilioaa capable o f reparation the iaonaen of PFBS, PFHS and PFOS. The final report will indade the honten sumued into total PFBS. total PFHS, end total PFOS found.
VERIFICATION OF ANALYTICAL PROCEDURE
A laboratory control simple will be used for foe preparation o f fortified oontrol auspice. The test rebalance will be made mh> solutioas as per the method, uod added to the matrioea via a micropipette.
For water sampling, Exygen will supply cue bottle per sample oollecied. Tho boMea aril) be 500 mL pedeaned Sci/Spec Premier wide mouth HDPE botdea There bottlae hive been routinely used far fluorochonicat sample
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Exygen Study No.: P0001131
Exypn Protocol Number: P0001131
collection t t the testing facility m l have been shown to be flee o f PFBS,
PFHS iodPFOS. Samples wiD be added to ecb oootaioer to volumetric Oil tine tt 200 mL A field dupliette, a low Add spike and high field spike of caeb sample will be ooDewed. The low tad high field spike bottle* will eontain PFBS, PFHS end PFOS e* well as pcriluorooctaaoic acid (PFOA) end
U -I3C perfiborooctanoic add (*JC PFOA). PFOA and ,JC PFOA mx included in the aotaiora used to spike the (ample*. The ro u te for PFOA and
JC PFOA will not be nponed fa this study. Exygen will supply one field
blank (control w tter) and two Add blank apfltce (control water fortified with PFBS, PFHS ttx1 PFOS at a low and Ugh level) for every twenty temples oolleeted. At foe testing facility, each water sample (excluding field
duplicates and Add tpikee) will be extracted in d elicate and will also be fortified at a low and h i# concentration with PFBS, PPHS and PFOS and prooeased throughthe described procedure In determine method accuracy nd to check for bias.
For soil, aediment, elama, and vegetation, Exygen will supply one J00 mL preckaued Sd/Spec Premier wide mouth HDPE bottle per sample collected or a rtp-eesl bag. AO containenfotg* used for m nple collection will be shipped
to the sample location. Smaplce will be added to each eootainer or bag in the field. At the testing facility, each atopic will be extracted in duplicate ind wiB also be fortified ai a known coaceutntioo wifo PFBS, PFHS and PFOS at both s low and high level sod processed through the described procedure to
determine method accuracy and fa abeck for biaa.
F w tm all mammal fiver. Exygen wilt supply a 50 mL polypropylene
eoarifli|e tube; Forsm ill mamma! serum, Exygen will supply a collection kit for each sample containing serum separator tubes (rad lop), vneutainen, needle holders snd needles, transfer prpettos, tod polypropylene tubes At the testing facility, each liver and serum sample will be extracted In duplicate and
will abo be fortified a known eoocastration with PFBS, PFHS and PFOS at both s low end ugh kvol and processed through foe dcecribed procedure to determine method accuracy and to check for bias.
WinWlAintWVIran w a mamxnoocmsettbelow:
M atch
Low SolktaiLevel HiahSnikior Level
Water
Soil
Sodiroant
Flail . dams
500ns/L 4n*/g
-- 4 l te_______
lOngfe 10ne/i
5000ns/L 40na/a 40na/e IQOngfa lOOnxie
-------
W .m '.i U .i i l T S
f SmallMatnmi! Scrum
|__. _____JOnsf'aL______
i
100n^u lOOnafa 100ni/mL
Putt 10a fii
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
b u n Protocol Hunter MOO11 I
/ n. Rocovuriea are anticipated to be betw m 70W and 130% o f the fortified Icvelr, however, the exact preeiatn* and aocuracy wiU be determined by the aiuUpie o f fce quality control um pire deacribed above. A ttatement of accuracy will be included in the final report.
METHOD FOR CONTROL OF BIAS
Control o f biaa will be addreaaod by taking repreaentative reb-iamplet from a botnogeaaooa mixture of euch matrix from untreated oontrol sample, and by analyzing at lentt two lavola o f fortification.
STATISTICAL METHODS
Slatiatic will be limited to Shore apecified in the anbject method and to the calculation of average recover*, a> applicable.
GLP STATEMENT
All upecta o f thia tody ihall be perforated and reported in eomphance with ERA TSCA Good Laboratory Practice Standard 40 CFR 792. The final report or data package (aiqjplicd to the Sprmaor) ihall contain a atatemem that the atudy w m conducted in compliance with current and applicable GIP ataadarda and will outline any deviation in the trudy Hum (fcoae ttandarda Thia Moment will be ngned by the Study Director and Sponaor Keprmoniative.
REPORT
A final report will be prepared by the principal inveatigator or their deatgnee at the coochiakn o f the rtudy, lire report will chide, but will not be limited to, the following: a The name and addreaa o f the Study Director, Spooecr Reprcaeottrivi, and
of the bating facility.
A atatemem o f GLP compMance (any related documentation, euch at chain-of-cuetody rectxda, mnat be in the atudy record).
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E x P tM e w i N u m b er. P C O O l1 3!
The eigned and dated Utamcot by the Exygen Reaearch Quality Aaauranca Unit re in in g dale* o f atudy inipoctiona and date* finding wew reported to the Study Director and Management.
A dcecriptkxi o f the exict analytical condition* employed in the ttudy. If the aubjeet method m i followed exactly, it ii neceeaary to include only a copy of the analytical method. Any modification* to thia method will be incorporated into the report. If the method it photo-reduced, the project numb and page member muat be included on each page.
Daecriptioc of the inatrumentation ueed and operating condition*.
AO leenlta from aO aata analyzed. Control and fortified tamplea will be identified and the data table wilt include (ample number and fortification level.
Repreeentatlve dm m atofm tt for end) analyte in each matrix, including ehioinatofnrM o f a rtandaid and a control aample, id a chromatogram at a fortification level The location of the analyte peak* will be clearly identified in tO chromatogram*
AU ctreumatancea that may have affected fit* quality or integrity of the data will be documented In die report.
Locetione where taw data and the final report are to be archived.
Addition* or oorreetioo* to the final report hall be in the form o f an amendmart rijned by the Study M eet . The amendment iheU cleatiy identify that pert o fthe report that Li being altered and the reaeon* for the alteration*. The amendment will be ligned end hwH by the Study Director and the Sponaor Repreeectarive.
AH applicable requirement* for reporting of ady reaulu i* per 40 CFR 792.185.
SAFETY AND HEALTH
Laboratory personnel will practice good eanitation end health habit*.
E very reeaanabl* precaution ahall b e taken to p rev en t inadvertent
expoeure o f penomtel and foe environment to foe tett or reference
iitbiU nM ($).
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Exygen Study No.: POOO1131
B i y j m N o to o o l N um ber: POOUI1u
AMENDMENTS TO PROTOCOL
All aigniflcint changes to 0 aaaiytical protocol outfitted her will be fncased in writing, signed end dated by the Study Director end Sponsor Rqtrtiaanlalive. Amendment* usually will be muod prior to initiation of tiudy plan change. However, when t dung i* required without sufficient time for the iieue o f a written amendment, due change may be effected verbally with eopportins documentation signed and dated by the Study Director and followed with a written amatdmea* aa toon aa poaaiMe. In thia case, the effective date of the written amendment will be the data of the documented change. Copiea o f the aigned amotxknenl* will be appended to all distributed tmdy plan copiea. The original amendment will be maintained with the original rtudy phr_ Any daviaticra from the itudy plan or ftom the analytical method ae provided will be documented and reported promptly to the Sponsor RepfMcntadvc.
DATA RECORD KEEPING
Record to bo maintained include the following (a* appropriate):
Sample tracking sheetfe) Sample ncei|* records, stooge htetory, and cfaaine o f cuatody History and preparation of andarda (stock, fortification, calibration) Demriptim of artymodification to die method Unrinutimt ran sheets, bench-sheets or logs Analytical data tables All chromatographic and iaamimental conditions Sample extraction and analyst date A complets tilin g o fstudy porsoonsl. tignati** and initials Chronologicalpresentation of 11study correspondence Any other documentation neceesary for the reconstruction o f the study
ChromatOfnm a- All ohrocnatogr** will eaotam the foUowing:
Sample identification, injection date, row or other indication of the area ofmteraat, and injection number correspottoing to the run.
Additionally, fortifications will include the amount of analyte added and the sample numberof the ample thal waa fortified.
* Analytical andarti chromatogram# will additionally include foe concentrition (e g , pg/mh).
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Ex>m PrMoco) Number: fOOOl |J l
Ai pert ofthe documestitioo the fallowing hoet will be included in c*ch
nytical et i run beet listing ite samp! to be run in ih* Mt, ad ta inatnnatt oooditjan heel deecribmg the tattniment type and operatine condition.
QUALITY ASSURANCE
The QA Unii of Exygen Reaeerch wiil impeci Ite tudy et interviia adequate to saure complUnce with GLP'. and will report th (fading of uditi to th
Study Director, ExygcttManagement, and th Spenaor Repreeentative.
RETENTION OF DATA AND ARCHIVING
Ail hard copy raw dala, chiding, bul not limited to. the original
chromatogram, worksheets, corrtepondeooe, and result hall be included
with the data package uhmitted Ore Study Director. these will be archived with the original tudy plan, meodment, {foal report, end all pertinent information fio die Sponsor.
The Mating facility hall keep all electronic raw data and any instrument,
equipment, and tongo log fee the period o f tune perilled in 40 CFR
792.19S. An atari copy ofthe materia! intautted to the study director will leo te kept it Bxygen Research.
Exygen will obtain permission from the atady director before returning impk*.
,,
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Exygen Study No,: P0001131
Rays PteMcol Nkariber P0001131
APPENDIX I
ANALYTICAL METHODS
V00Q17S0: "MKhod of Analydj foe the Determination o f Perfluoroocunoic A dd (PFOA) in Waterby LC/MS/MS"
VOOO!781: tM b a d o f Analyaii Em tha Determination o f Perfluorooctanoic Add (PFOA) in Soil by LC/MS/MS"
V0001782: "Method of Analyau for the Determination o f Perfluorooctanoic Add (PFOA) in Sediment by LC/MS/MS"
V0001783: "Method of Auatyaii fbr the Determination o f Perfluorooctanoic Acid (PFOA) in Fiab and Clam* by LC/MS/MS"
V0001784: "Mdhod o f Asalyaia for die Determination of Perfluorooctanoic Add (PFOA) in Vgtation by LC/MS/MS"
V0001785: "Method o f A iulytit foe the Determination o f Perfluorooctanoic A dd (PFOA) in Small Mammal Liverby LC/MS/MS"
V0001786: "Method of A aaly for the Dettnninalinn of Perfluorooctanoic A dd (PFOA) in Sanatl Mammal Seram by LC/MS/MS"
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exyg PiomuI Nunter POOOII3I
ANALYTICALMETHOD
M M N M c vmoitw
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Exyjjen Research
T m ifw 7
p>f l e e t s
Page 79 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Interim Report #10-Analysia of Fish and Clam Samples
Exygen Study No.: P0001131
Protocol H w ito rP O O Q lU J
UMM
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P cgtH efU
Page 81 o f l3 2
Interim Report# 10-Analysis of Fish and Clam Samples
Exygen Study No.: POOOI131
E x n s a Protocol N u o b ft: W 001131
*A L Y T >G U .M rniO >
UVMUMS
I
M *tM.U1M rSwMMM"M--iiAa iIalMiMwM la-t 1 0 0 WPPOAfeyw*Si*g10mt o fw frrtffrf M M ( iim lii far p M y M tfaw le 103 L * M k lU M U H IM l
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Page 82 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Page 83 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Page 85 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: POOG1131
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Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: POOOU31
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Page 87 o f 132
Interim Report #10-Analysis of Fish and Ckm Samples
Exygen Study No.: P0001131
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Page 88 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
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Page 89 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Page 90 of 132
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
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Page 91 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: POOO1131
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Page 92 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Page 94 of 132
Interini Report #10-Analysis o f Fish and Clam Samples
Exygcn Study No.: P0001131
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Page 95 o f 132
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Page 96 of 132
Interim Report # 10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
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Page 97 of 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
CxyfCftfnKocoi Nucober. P0001131
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Exygen Research
Page 98 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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Page 99 of 132
Interim Report #1-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
E ProtocolNadar: P0001131
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Page 100 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
p. 100 Exygcn Study No.: P0001131
tx y fm Protocol Number. POOOIDl
inn n w >
>tm m m vtwiui
I . . . ***iJrnoU.gnioD
i
. CMotrLOMMU.M M * ofA a tfrtltM M frlim to tlio
ro ..l.iM U fy P O A )i.P O i. )
1.0 '
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M I*)
"
SI AAmpttOomwAltPtflMiQipoMiQMi
U C>--it M n n plm MT001iitt IwMlm my cMoMl fcrpnrm pftt)
10 JJ tool*)OtbtpMMtaOk^r PhilwMuoimpltIni
M t p tt liter < t--wgwtn tO try I. H i 1 -- p i t w iolun
I J l o l i i l > M ) M i i l l l l t T till r t l * t i i in)> i ) l a M iiii
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aj w m t-m c * * *
4 i AM M tofl~HK m il
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art*
4445 wIft>oiii|wl-WiiitiCiMm Mm*)"i ^ < |t o
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4471 |4i^*0lC piii
49 i i--Wimto^Kigsagmi
4M DlNft|4MMh~lmalp*'
4U Tdw-Bwipelme*
441U1 AMMmhstiiomtioiilIMi -A.C1ItoiMOmit
iO
i.i a t o * m t o M H i kmM iicw
<m*N r n w pii %* 2
alvasla amtoptoMl vwtaMavatoattIqjMl apabta efiipeett^5*Mo
jLwswiii iM iiito Mmi Ipw-- o itC M M a ).
I J itoiljiloltolwiWMWirfwftymaOOOPl
ft |f 14 o f C i
Exygcn Research
Page 101 o f 132
p. 101
Interim Report #10-Analysis o f Fish end Clam Samples
Exygen Study No.: P0001131
ftotwol Number MOOl Ul
c ... u
ANtLvncALmxmoo
Minirhaiii vmim
'
u IMayv
uxs TVmkU 1U L>wt nm ta b .
i l HMt-
19 o15igmiManBim^LnxMqomi.irlOtlMn iaoMtuir
9.10 D M U H I a m n '
IMI 7I
MS
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1U149 Wmn^h ^tau
w (MftHf094saiwi
* >* i '*uuia U am a 90am5n
iUU rmM"i^mMnnitlo`mlwctmMir-ei ...............tumim***
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Exygen Research
Page 102 of 132
p. 102
Interim Report #10-Analysis o f Fish and Clam Samples
Exygcn Study No.: P0001131
E in e n P n M o c o j N u n te r PO O O II3J
iktirnCAi. wereo
MW^Aaa^iaMnttMOiBiaMitkarfUWWMSMoiot^jWiattTAiafat
ft M M Iim T.l MaM 1I I | | J Mu Min t a x f c -- H m i t l ) H I H
tm*tmMlimiMatylMrtlnt.llMC
la wiiqinlaninfiaum
I I IM A Run
Ila M r il
(MWI of
u innliiV W iM
-*-1
til pmtntM ttf c l a L rf i_____ la o l w b
fey feria#* J I
* t a l M i t 1 mL mm M m
aatyfetimn* / 4 M t a M a
* .l t aait a lM Iwlt a t a I . Wi l
I.U ft M a n k a M in rf-W O Mind. of n o A by a # .? * 10
' ` 'T***? -- *" * (!_' I M ay ) M l Mm 100a t. w o M a lia IS J-a L U H M l
*.U AlljwaltMMlllMaPKMaMMIvMM.:
m i t t * IN H l l ( M a I ta l M a il 109wMu m la i Us t u n fetal*.
R,J T*"**imo*aan* ai>
1U.S(aMLUUaCMfefalaMla.M ta M M m on W at aafeaM fe.M
IV 1 f e r ii
M a ta a a t a l w feai af 100 ok
tari la a U J a l I B I fe rn
.14 `n * * *M iUMlta t a t a t m at aana la a itMaora
faa*4fl
Pegt40oft!
Exygcn Research
Page 103 o f 132
p. 103
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exy|ta Protocol Ntuaban W001131
MaaitMmvtiinwu
I m tim iC T M WaMal^^tetelMaiaMaf>BU<twlaBcl. AM(H'OA)lnla
O a D g rlO H lM
*i ButennaManliMn. AI l M M aaM M M M aatp iM B i4 aaaln a0 iM a< i
J- aTf*aMISt'maaMt,. M. lyMplMala aahttiaaM. ataMW, mayta
< i rn * N iMy>) ii>irH ii
IM M ifaaU
ill EukMab afaM i aaakaeM(OftaaU? Iw) km tieMa atlaw
m' * M M l M l M M r n k M I M
IM
tu
4M M i l a) <#>M a l aaaawatyte te tatet.
a M a te y M e a ta a ae* f h eriu k t M M
!!! )1ihrtet|Mp.
IU Vak I | aTM a aaa*ie M M bL M iM tM aaayitiie tatet
;uu !MM XteaaltSetMImSteIaitaMcSt*-I MM M M t M i * i b - l l i iu >
IM * * m i M M 4a 0 t tatet M A M te M M M i.
tMMef)tufSB`ataSl`*a1ti`*i mtOMM-K-*kf--ftMat taMatei
lWtill
ilhi wMilt
Da *m
IluMi lfIItellUtetll.
tH e* t e M im
IM
am liiBi laM n . U a a t a l U a l t M i m .
SMQrMMmriMOuMaiteMaaaalrtMDayiMt eiM a M ta te t tat.
NftlWa
Pag*41 o fti
Exygen Research
Page 104 of 132
p. 104
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No,: P0001131
Exyfin Protoeat Namier POOOIDI
I ..........AWAi.mc*iMrnw
|
M iri a fX ir i) A rin V a P ia iiiiii n n ia frii n i in iw A a riii O A )w ftili ri
OactyUVUUMS
11.J OaMrip Brilo ni. p D p p jm i uria iwnnlPa riapri -VX p i . rii-iriiria. I J Dmrilfci m a ri ri iiiadkiaaaiM arila* ItMt ririiri ria BMri>ri
, ritpuwriaaOafc. capa a ri-- a e m wl m--m pw xuf.
II* M i 1 aL r i aariaiaUa a atipia la ria 9# ari. naalrip tabi. . . , I w p t i a > l li f c > > i n i t | i il i li tr -l< w < . < ii . . . . riariapI-- airi ! ! ria-- la riari Ma. 11.1 fc ti --t lln iiii r - ll* im m ii mria ritta 11.11 ' f i r n ** ! -- * -!! ih. Iti) Citairip r i a d .y rilfa|u>rim *niaarilNU rit|ria-00in
tU ) Omo rii m a a*a rii ria* D I -- ria. COMI rii M Uri Ho m m fari-ripa tari m i paMat atri ria aria* fina rii taito m ortat
ItJ lw t l( llllll l l ^ iW u ln a m i imWn ri*-- riam m fHMbpal fiari.
IU I M i M p Of tritai* M *ril ri panari* h t uri , riurip fri-- >ri>Mwliiy n paaai (ri< P f l
tu MPri fc* prie. ly Hip l i n i t u eri m w n i
t u r TmZi5 mmmmWtC
<wbl p9tn
IU I m ty m M ftw wm$ m tr^wp 1nVTUff
IU pivcitomunifit#t*i
U J > n w>i t f M tfnribB t i ln#t fr m u m r i w t i l i i i Im ii
I-- >illriillI il ri WlljrififUt IU M ritiri a*afii1ri*lia ria tanti anarii*ii*aitilnri|naia
m m dm ft api Mi tm rnm m m W r i n f i l i t ri-- nm > U t
m m frn itm r-IO im rM tB m m m im ri marni m t/m aU M t) ri *riar i r i aririwria aria* im i bt tri fini a * la* ip*tt*a in i Ila Uri alar ariariri lama rii paritarie Uanr aula canai m p a * a* aaalyiiyep a mwrika wins1/amiilaiaifprium wmariariririerieMwiicaiariailw ariaMm typ U |ar-- ai)
TsSTTf
H fU ltfii
Exygen Research
Page 105 o f 132
p. 105
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E a y a n P m c o l Nuratwr POMI 1} I
c
_______
XiOiihi iiivwim AWAtmcu.M7noS~
______cumm^ icmsah
I t ) im fk w y a M A m U mm m im mmm w p a tw M y i i w flw mm
m m * M * M i rmtm m mm ii H M im U M ti m i m tm ytm
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--XnXiinflx--ln i--Um- iinmiiiii
J WM i t i p t m t u s ta trim ma* w M o n a r -im * ( h a . V > M lv UaHbM aM >itoaMpaU>min.*
n i W n i j l m i u H W! min .
fcwt T< f >-- m t lamini at x iXiXmiimV
m m m trnm *X )% attnm m m lm atndw *tm t< nL
D J *7**nwj>nieli*ilMn Srnia.tUImMg. mtu nlIVHiiiina itwk--l .mfmemai. 1mm1m.
. . ^ a r t ^ f r n i hii>n M X iiiW)i> t U. I M k i M l M M M r i i a d M i l i i M M i l n n i , ,
*m4a^ripliWal?u*m"h *aWh*i*`M"*n- *t "te * * * KmMin
RI *"*" !* >**hi * *** ama (S tar h rnmu m o g a n i l M V r M ia t y v a rtn ra f n v w
**rk**-- '*>*-'t~ ifh t y Ii i i iii
Ma Ua M iki n a i a u marni h . m i rfn0A in ai InntoL c
MMMUMIi! Or-Mrir M k a l l a |n |WHalMml.iriaMMt.
Paft 4J e ft}
Exygen Research
Page 106 o f 132
p. 106
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001I3I
BxyfsaPRMocolKuRiherPOtDt
I ...
~~jika.wicu.Mem
/
O m m h U S tm a ______________________
lJ INvibMnMUMwlft]bmwdwMMiorn*OApitar0ntrwiM.M
1AfleiMleiwMW 6^Eiw ieeww7. Iwwwy^
**<(i*ty
Exygen Research
Fagw 44 o fAJ
Page 107 o f 132
p. 107
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
B x n m Fraterni mmbcr: fOOOt l i 1
AMNAMLYTIIMCALr MV0EMTHIMO4D
< 7 < i i i i B m n i > i n i -- m m i r w w i i
VapMM tyLCMlMI
AMt>awiT(xrMWir
MM I
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VIM M . GpMla, Bo h t m *
-iflJiAlli
Jtjd.
Exygen Research
Ttulhf 7
F a g t4 S a fti
Page 108 of 132
p. 108
Interim Report #! 0-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
E*re= Protocol N u n fe r ?0001131
I .ccavT iou. >iir6Q
Atjj<yKM7
U kH
2? 7*5^ 3
ftM i i i TTDmn >(ICMMei) k
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Mj EWl l m.
ft----
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fUamilpftnmM*Nw**att*hMi *MmmOHt4rwtinift*nyiirMt.uyinwmiMAwt itpotnwtmoi*oww
i m m Cfn m 9mm 1
U wfllheyeWleSeewylmiyURfcr tlw
41 Wm -OKC** 4 3 Amman-- WICmM
4443 Oy^awksi<-1W30L4Cnir*^i-la
43 SUwsH<*elU4 4 PWiMN-Im 40|K
4 7 S e e d * fcC M Ii S * e * p ile 4 1 I-Om m I - K T I X * .* 4
410
411
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3.0
3.1
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uhj
.......................OW nwM^toftOMOl
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Exygen Research
Page 109 of 132
p. 109
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxratn Franco! Nuraber; P0001131
I Aim-vncAL
lto<w u lAmi j t h r $m jtom rm m So^ byLC/M&MS
i
fFEQAJ m VnawnoB
11 mai
3.4 30aL
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in
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in c n i ni n Mir#>it^nt.ra^p<niMiiii>nu>ni-
40 CmMigiAMlyMi
41 A a^iM O ahM rPhaplM vK f (toyalM SaMifleMt tm x SOami. V
'MtttMMaUQ) 42 TfcMHftn: 20*C
42 1 aM Am um km MMki In W a#
M H)WHiml)i KUtei iS M m SNp m
S b i GhW 0* 14 14
241
215
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25 25 45
rWwfca*
i l feU oi) 35 <U 55 45 TS 45
73 45 51 45
4 hj a f Vo<--k l 3 |0 . ( * b e i e a i w l l e m ^ i * S 0 ^
42 OuMiate Piafcito-aaariaadalafffctfkMar*.
41 llaiT lar S a tM K
Ttem M ^teim M daafM iBlam tclaM rtkoM pMiMialffLCoiM.
7.0
7.1 PHTGA*.OIKOWWIJNmdvMflmfi8to.al>1^S3-Wirtto
Exygen Research
P i * 47 f6S
Page 110 of 132
p. 110
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exypa fn meoHNumber P0001131
i AWALtncALinnn^o
m wmtT ii ife m mmMm* h M n M m a pM a m i fcaJnbomI fa a r t *
apiM a * a MKMl i ) w a
. hniinrfuWliNIwi 1.1 IM h llM i
144 I aM m n l a o m m vIb m w b pnparfd >y i M r i 0414 j * f
12.1
112 JO*DiaMftkjMkMwaaMaMAmtmmi byWwtgft)nt
a f4 4 m ^ 4 id 4 k m U m t to a Bm I valaaM a f 10 L w f* alnt.
I f i IttariM i fafM ttte* 94 I mmM OtoaMtetfltMtaaNhUM
ij.i ))imkrMni^ i>iw.rpfM^
fw u ty m d slBNfcv*( m m m t 4wparity)>1tfU* H lOOml wi*>
MiMMf h ftI1SL LON IM k.
9.11 A
MiniIfm mil afnii afHOA
Nay^ f
*Latf fca(.1u10r|s|tUot.faaM. aa a AmIn Ii m afl 00vi* wCmmI
111 Atallt*mMll.fficitaflLWaii--WwBtaifataaatUfgfwPAlatfotyf^taarrattdty>iWiwaMyt*iR0
U$LtCfCVaflfeft.
1 U A l l nffcaLiKiflftiiaa M i afHPA pywaa 9y Wyyaf
10 1 ftf * W IfW , M M ft Ml VttMMMaf >00 Wft*
aA M itelalUnM ft
14.1 Tfc*ila<fc*ifciA^iftaNlki*alaW<a^iftftfAl^Mi{
yp--u--ariy 4PCm i m m kk Aft *niftiaw y f t i af 1 awct*
91 ItaiaiC M ialH ilaM ai
91.1 LaOfAHa91M0iyafMtaMlAaatUWbai<iiMwfdtafltaMtftBp>B^Ba9liaM akaBo(vfftaiii^an
Hff*<M'
f t f i 44 o f45
Exygen Research
Page 111 o f 132
p. 111
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exyfea ProtocolNuwfeen POCO! !JI
| ...
M M n i l > i i r t ni W O B K M
ferMfr-nnUiblynUjffPtfnifftttS ~ Aeii (PPOA)ftVi| --tim
9X TUtataflw*M * <l W ^ ttttnnl in w i g p i ia iy te
flW fate Vrf
4uUMP M41M
IS
1mJ$ M
to to
MU Ml MM
M44O1M1
i
JMSMMaitimt oMt om M
il
I2
i^
MlMQU U H ***-ontani
9X4 AtfiVNCKanvaln*aMntoi Mmc8mntooMinnfMutalinaybapnparnlaft
1M SfctMTJp
141 lOg8nOu8H*>Mm8Mtu8vfl8M(MlwAMpmll8i*mftlml8--IldWHiflty?WtadMayliMypdMillMorMWunBlW)lmHfemlMfinM^at^al>8itkMJlOovw'rt
I0J tm rim m m t o l t o m i Marno 4Mfn m i y k m otti U +mirm n Munitananna* pila >wIII pnjn t
IU0 imjhlMmrntm
M i \ t * Ma nappa Ma IO tata. yntjynpytana w trtti Mai (ftilliy IM M , tapinaM m nfea.
tl.3 AMMaLafnnoMaaiiMalaiitaftW'iiiiAiaaifcafcarlIr-'if aMin U C aMM t o n w L pH)FWU-- 1 8 naanintag ama -OOO tpm
far-llnim i !1.4 ?nfcaalm M m M gBM naaltaM aift<HO *m Mflnfci IIJ h * 30 L M ntan li aaqaaan Mi 1 f fiorini. t %mito p i 2 |
ntaata.nl 1 1 IC-NK Cnmim to I n M I n i ot a m im i
am M w L m tm m m to lm . W a n rlta l o to n . 0 a n ttia * m Km m *
V, 114 SUoriai in US nL pntMapai fintai fejf n a n t viti ttn W
daMtatTUMtatanaitaMtantaaaaaafaaa. JtuMttn fiatar rintoiMi**. M a n i y M l w l {Una Pana}. fty Un Untai (Mptuily M n <m, MnrU*iM )4af m wtafcatoni fnJnpai. U.7 Dann * * aanMitfcaal SPIMan* fitaaliaaiit itaamatan ' UnpnM^ai la*. OiflKl * Milafattaa U5 nL iflatunUphmI*p
PG&*9of6S
Exygen Research
Page 112 o f 132
p. 112
Interim Report #10-Analysis of Fish and Clam Samples
Exygcn Study No.: P0001131
b n e m Protocol Num ber: P 00011J 1
H p Iw ri
IM W oW IU
I
a r a u t k *. -reru n
...............
i
M itel a^4)ateDiianalaaiiaa'7TCinui]ln Ajii(OX) j Vt|in<w
OyLCMtM
Jl.fr M i 10 imL af
ft -- pta m A t JOLrwtHfi| ttfc*
I1J >w*--f*^ i f c f Mh--w a iu t o wd w h ifcw
ll.M CrtA0i Im SOmL pd) tyjlMi *km ottMm Mnptt m -JtCO ijm
11.0 >ipidpimwtjb1U1
tU ) MU M I p l^HMt it I ohm to pr dupH M m i
11.14 UIMmMmM+i mM*tmki*m^tmm,b*yUMmMtoMg1MLmtf*". CMttotei* to tomai
11.U
1X0 OVMHtlMfOy
1X1 ltfctttoMtMMiff*4iMMMpfejMdfriiflp*aMplttoaM
ICM1M M& A M t a m i m i MI p m m tri K b di
' tttlmdtMMtot
i I U t e i l t e i atHOA Mi Mlfc loit h te tapar a ii i ii i Mala
. -- |W te te a i atra in.
' ( J J A f m tm m t f m i m i o M n Uo t t e * am ai te t e t n ii l tw
/* "*
l'n M H i imil a t e r a l r f i m ia u t h n M u t e t a I .
j-- OtteO teteam 1 >10 --II. A * * * . * * ! r
t M te a l i m i aaMmioa H a te * Im i* * r m r H O ho Im
(iM M iliriw tem ifaiteteM O lu te tm n
.alteartea t e t e * a a l t e t e Imi 4 laa lia ja ctia o * * ? 1****
1IA Itea Ite alte aoaoa t e |aaMltMlte K4oaar rateai ni a
w M teteamlriateteMrapaMteiatai
ama
p p u M m i i t e M ataa-- t e arti M an i ria 3 J (a i lo ia . ilm i
tema. arac. IM ln l mm-- l teauki am mmmi I H m<n.ai. Aay a mali. te i
lim i 0 li ........Mili te E te r n iate miamal)4.
DO UMftmm Otete IM Cimai piai aa am aaafcmfa apamt e al rat aia. tram l p w al 413aaa. Tte 411 mm para laraf aate t e PPQAka>. tela t e tea|ter te(M* l i M a a t i la afaatealteite.
3*3
P o fiS O o f i
Exygen Research
Page 113 of 132
p. 113
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
ExymPnwcot Nuafecr nxm i
M a ftlf MiwMr VM|H4
'auim.33SB B CM(PfOA)i>Vmfm*** taLCMMO
te PP*a trati p * tm to WO-
MOA IPMtl |m w M M pyk, Un>t m. Man, MtjM
IJJ _ . ,
ik * ta < M l* to b U M lP im ,!
m iM >
w s m m M* Aa MhMplaWUnuio. Pw
M R lttllllM p IllA N M k V IM lIV lM .
IM to r wliktaia m m toi to to ta < n a ta l m to t > M m u m a
* r " H i M .-- > u fa r ttw g fU r tahnm n ca
i * t m itotom m taaki to i amU ta arcMal
IM HMaMamialtkanlWmWffic'kiawpIta| mi rW
K K ' M M * If I
km Uhu. km
M irim a m m a ta t m a i ___________ _
^ a k to a to m m ttr n m to * m Mta M tr * . IU M a ta ta a lk a tta M ni m la ma m *Mam *
lia i kMaawd k a ta * ta aaitk ilta ia ta a a a ta iitaim.
14.1 Ik u ta k lW ig apmfr-- a in ik a p mOAfcata<lai*'*L.
**r>* *-- 1li `~ 't - H at ini ira i a
flW1 Utak kiat a | a tta^ t a k w a rn TITO ta rn m a l a
m U kaaK fet)-
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Bf - k a ark p alM k i W ta ta m a M . Umtommr
MJ Pw MMpin fatfcSt4v*Mi h m a H a i l K U | n . n K . ka Mbawg m a ta a M m a pacad awwy
ImwarPU
[aalm lia.kakWMt a a ty a k u ta k o m a M ^ l whweWNdWD
Exygen Research
Page 114 of 132
p. 114
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Sxyfaa Protocol Number POOQltJi
ANALYTICAL METHOD At Y m m
* * * * * * * yH far INHm la ii T
ill A H (TTOA) h --i
I M U n r feyIC M M H
wlliM TiA
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I
ftOxiMl Ule.lC*0. IMnw l m i
Exygen Research
n w 52 HZ'55
Page 115 o f l3 2
p. 115
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
CxygcaProtocol umber POOO1131
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Page 116 of 132
p. 116
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Eiyfen Protocol Number PCOOIUI
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Page 117 of 132
interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
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Page 118 o f 132
Interim Report #10-Analysis of Fish and Gam Samples
Exygen Study No.: P0001131
ftsygn Protocol n r t t r P0Q01131
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Exygen Research
Page U 9 of 132
p. 119
Interim Report # 10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
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P m p ilefii
Page 120 o f 132
p. 120
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
EatypnhoKiool Number P0001I31
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Page 121 o f 132
p. 121
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
Euygn P M I Nuo*nr MOOI 131
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Page 122 of 132
Interim Report #I0-Analy3is of Fish and Clam Samples
Exygen Study No.: P0001131
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Page 123 o f 132
p. 123
Interim Report # 10-Analysis of Fish and G am Samples
Exygen Study No.: P0001131
Exy(et Protocol Number MOO1131
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Pagw6tof65 Page 124 o f l 32
p. 124
Interim R eport# 10-Analysis o f Fish and Clam Samples
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Exygen Research
Page 125 o f 132
p. 125
Interim Report ^10-Analysis of Fish and Qam Samples
Exygen Study No.: P0001131
E x)f|a Protocol Number: P0001131
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Page 126 o f 132
p. 126
Interim Report #10Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Exypo Protocol Nmbtr: POOOl 131
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Exygen Research
Page 127 o f 132
Interim Report #10-Analysis of Fish and Clam Samples
Exygen Study No.: P0001131
Bxy/n Protocol Nimber POOl 131
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Page 129 of 132
p. 129
Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
3051 fiaeardi Drhe Phene: 14-272-10 StateCollege, PA16801 Fax: 814-231>1580
PROTOCOLAMENDMENT
Amendment N u m b er:____ 2___ _
Effactve Oete:
03107106
Exygen Study Number P0001131 Client Study Number
DESCRIPTIONOFAMENDEDSECTION
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Interim Report #10-Analysis o f Fish and Clam Samples
Exygen Study No.: P0001131
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Stale College, FA 16401
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