Document qaw8gqJ5yrv4OmBgDqadDgOxK
:
AR226-3642
ARRRG. 3638
INTERIM REPORT #1 Analysis of Oskdale Water Samples
STUDY TITLE
AnalysisofPerfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS),
Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil,
Sediment, Fish, and Clams Using LC/PMrSo/grMaSmfor the 3M Cottage Grove Monitoring
DRAETAQUIREMENTS
[EPA TSCA Good Laboratory Practice Standards 40 CFR 792
STUDYDIRECTOR
Jaisimha Kesari P.E., DEE
We1s4t0o0nWSeosluitoinonWs,ayInc.
`West Chester, PA 19380 Phone: 610-701-3761
:
INTERIM REPMOaRyT1C9,O2M0P05LETION DATE
PERFORMING LABORATORY
`Exygen Research
St3at0e58CoRlelseegae,rcPhADr1i6ve8:01 Phone: 814-272-1039
STUDY SPONSOR
3M Company
3M Building 0236-01-B-10
PShto.nPea:ul6,5M1-N7335-56134744
PROJECT
Protocol Number: P0001400 Exygen Study Number: P0001400
Total Pages: 110
REED
000024
rimRept1 Anyi OkieWate Seles [----
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT
Exygen Study Number P0001400, entitled "Analysis of Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and
Perfluorooctancsulfonate (PFOS) in Water, Soil, Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by Exygen Research.
foF0ie7r7y
Principe] Investigator
Exygen Research
Weston Seton. oc. Jaisimha Kesari P.E., DEE
`Study Director
TAO. 3
`RSopboenrstorA.RePparsecsheknteative
3M Company
FI
.
Baehs .
D#
ANCES
Date
Page200110
000025
InterimReport #1-AnalysisofOstale Water Spies ExyeenStady No: PO001400
QUALITY ASSURANCE STATEMEN
Exygen Research's Quality Assurance Unit reviewed Exygen StudyNumber P0001400,
entitled, "Analysis of Perfluorooctancic Acid (PFOA), Perfluorobutanesulfonate (PFBS),
Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonste (PFOS) in Water,Soil,
Sediment,
Program."
FAislhl, raenvdieCwleadmpshaUsseinsg'wLeCr/eMiSn/sMpeSctfeodrftoherc3oMnduCoctttaegcecoGrrdoivngeMtooniEtxoyrgiengn
Research's Standard Operating Procedures, the Study Protocol, and all applicable Good
Laboratory Practice Standards. All findings were reported to the Exygen Principal
InvestigatorandManagementand to theStudyDirector.
Phase
1. ProtocolReview
Date
Inspected
0324/05
DatPeriRnecpipoarltetdoDate ERxepyopretnedto.DateReported to
Investigator ~~ Maagement StudyDirector
03/25/05
03/29/05
05/19/05
2 ExmcinReview 0VM05 02505 03905 05905
3.aRnadwoDraita Review 0516105 osnsus osaos. osnons ARneavliyetiwcal Report
Ta Foratner
`Techical Lead, Que
Unit
Bat5elisles
"Note: All inspections will be documented in the QA statement for the final analytical
`report at the conclusionofthe study.
"S000
`Exygen Research
Page3of 110
000026
Interim Report #1-Analysis ofOakdale Water Samples
Exygen Study No.: PO001400
CERTIFICATION OF AUTHENTICITY
This interim report, for Exygen Study Number P0001400, is a true and complete
representation of the raw data.
`Submitted by:
Exygen Research
3058 Research Drive State College, PA 16801
(814) 272-1039
Principal Investigator, Exygen:
< 2d
ohn Flaherty Vice President
Exygen Research
Sess
Date
[Exygen Research Facility Management:
ytu) :
Richard A.
PErxeysgiedennt Rsearch
Study 7 Weston Solution, In.
s-#-05
Date
Jaisimha Kesari P.E., DEE `Weston Solutions, Inc.
Sponsor Representative, 3M Company:
--a eA
Robert A. Paschke Manager, 3M Corporate Environmental Programs
Dad
Joilos
Date
aenad Exygen Research
Page 4 of 110
000027
Interim Report #1-AnalyssofOakdale Water Samples
Exygen Study No. POO0I400
Y IDENTIFICATION
AnalysisofPerflvorooctanoic Acid (PFOA), Perfluorobutanesulforate (PFS), Perfluorohexanesulfonate (PFHS), and Perflucrooctanesulfonate (PFOS) in Water, Soil, Sediment, Fish, end Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring
Program
PROTOCOL NUMBER:
PO0D1400
EXYGEN STUDY NUMBER: ~~ P0001400
TYPE OF STUDY:
Residue
SAMPLE MATRIX:
Water
TEST SUBSTANCE:
Perfluorooctanoic acid (PFOA), Perfluorobutancsulfonate (PFBS), Perfluorohexanesulfonate (PFE), and Perfluorooctanesulfonate (PFOS)
SPONSOR:
33MM CBuoimlpdianngy0236-01-B-10 St Paul, MN 55144
STUDY DIRECTOR: SPONSOR REPRESENTATIVE:
Jaisimha Kesari PE, DEE Weston Solutions, Inc. 1400 Weston Way West Chester, PA 19380 R3oMbeCrotmAp.aPnayschke 3M Building 42-02.E-27 St Paul, MN 55144
PERFORMING LABORATORY: Exygen Research 3058 Research Drive State College, PA 16801
ANALYTICAL PHASE TIMETABLE:
Study Initiation Date:
03/03/05
IInntteerriimm AAnnaallyyttiiccaall STtearrmtiDnaattei:onDate:0043/2211//0055
Interim Report Completion Date: 05/19/05
.
Ning:
Exyeen Research
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Interim Report #1-Analyss ofOskdale Water Samples
Exygen Study No. PO00LA00
PROJECT PERSONNEL
The Study Director following personnel
ffoor mthiEsxypgroejnecRtesiscaJracihsiwmehraeKaesssaorciiaattedWewsitthonvaSroilouutsiopnhse,seInsc.of
The this
interim portionofthe study:
Name John Flaherty Karen Risha. Paul Connolly Chrissy Edwards Mark Ammerman Amy Sheehan Eric Edwards James Miller Edward Kaiser.
Title Vice President
Scientist `Technical Lead LC/MS
Technician Sample Custodian Associate Scientist Sample Custodian
Scientist Scientist
Exygen Research
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Inter Report#1-Analysis ofOskiale Water Samples Exygen Study No. PO01400
TABLE OF CONTENTS
TITLE PAGE rrr sarsmmsapnss A
---- Page
GQOUOADLILTAYBAOSRSAUTROARNYCEPSRTAACTTEICMEECNOTMPvcL.IANCE STATEMENT...
2
CERTIFICATION OF AUTHENTICITY... errs
N STUDYIDENTs IFICATION...
LTIASBTLOEFOTFABCLOESN.T.E. NTS r.oreorrrss rrrrsrmnss esmsssssmssssesis]3
LISTOFFIGURES...
sss)
LIST OFAPPENDICES...
20 3.0
OBJECTIVE... INTRODUCTION...
sss
12 2
40 5.0
RAEFNERAENLCEMYTAETTSETRIISAAMCLPLEAS.L...c . ec nmmmto eim----13
606.1.DEESXCURCIHPOTRIPOYNOCOBFAUAENALr YTICAr L METHr OD...
rcs rrrnees 13 3
6.2. Preparation ofStandards and Fortification SOIUtONS vv 16
6.3. CHIOMMORTEPRY rrr ssn]
66..56..DQescuripationn oatfnLdiCE/XtMASm/aIMSEtCIanilstCrUouBmienOnNtao ndOperat. ing oo Conditons..............1..8.17
7.0 EXPERIMENTAL DESIGN cc
enmity
9A .0 CONCLUSIONS......co. voerarrerrsssn 20
10.0 RETENTIOFN DA ANDT SAMPA LES ccc
20
Exygen Research HOHE
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Interim Report #1-AnalyssofOakdale Water Samples
Exygen Study No: PO01400
LIST OF TABLES
Page Tablel. Summaryof PFBS, PFHS, PFOS and PFOA in Water
TableIl. Matrix Spike Recoveryof PFBSand PFHS in Water Samples..................24
Table Il. Matrix Spike RecoveryofPFOS and PFOA in Water Samples................30
Table IV. Surrogate Spike Recoveryof PC PFOA in Water Samples.................36
HH Fxygen Research
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A
Interim Report #1-AnalysisofOakdale Water Samples
`ExygenStudy No. PO001400
LIST OF FIGURES Page
Figure 1. Typical Calibration Curve for PFinOReagAent Water.......cvvvrcv 43
Figure 2. Extracted Standards ofPFOA in Reagent Water, 25 ng/L and 50 ng/L, RAPD sansgrnmasmmesngponirnriommntigwmnmmmenngrmsndsh
Figure 3. PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent WEtet, RESpECtVely.....rrrvvre 4S
Figure 4. Chromatogram Representing an Oakdale Water Sample: `Analyzed for PFOA, DE=100 (Exygen ID: C0064522, Da Set: 03240CR) corre 46
Figur5e. Typical Calibration Curve for 'C PFOA in Reagent Water .................47
Figure 6.
Figure 7. Figure 8.
Figure 9. Figure 10.
0Extra5c0tNeGdLS,taRndEarSdsPofE"CCHPVFEOALiYn.RreavgerntvWvatrern,n25snsgn/Lssnsnes 88 C PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, RESDECHVEY.....v.... ror 89 Chromatogram Representing an Oakdale Water Sample:
Analyzed for "C PFOA (Exygen ID: C0064522, Data Set: 032405C).........50
Typical Calibration Curve for PFBS in Reagent Waler.......rurvrvvvure51
Extracted Standards ofPBSinReagent Water, 25 ng/L.and 50 ng/L,
Figure 11. PFBS in Reagent Water, 50 ng/LFortified Reagent Water, and
500 ng/L Fortified Reagent Water, RESPEC...
53
Figure 12. Chromatogram Representing an Oakdale Water Sample
Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data Set:
BROCE smn
----
Figure 13. Typical Calibration CurveforPFHS in Reagent Wale ......ovvovurore 55
Figure 14. Extracted Standardsof PFHS in Reagent Water, 25 ng/L and 50 ng/L, RU mmm
Figure 15. PFHS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, RESPECUVeIY.......vvruvvvovsvvonsnST
Figure 16. Chromatogram Representing an Oakdale Water Sample
Analyzed for PFHS, DF=100 (Exygen ID: C0064522, Data Set:
032405CR)......... rn
goons resis
Figure 17. Typical Calibration Curve for PFOS in REGEENt WALET ...rvvvovrrvrsn 59
ExygenResearch
Witain
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Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No: PO001400
LIST OF FIGURES Continued
Figure 18. RExtreactesd StuandmardseofnPFOS in Reagent Water, 25 ng/L and 50 ng/L,
Figure 19.
PFOS in 500 ng/L
Reagent Water, 50 ng/L Fortified Reagent Water, and Fortified Reagent Water, RESPECHVElY.....vrurrvreernn
61
Figure 20. CAhnraloymzaetdogforramPFROeSp,reDsFen=t1i0n0g a(nExOyagkednalIeD:WCa0t0er64S5a2m2p,leData Set: O32405CRY.erronsrsmmsmssmesmsssssssnssnn6
Exygen Research
:
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InterimReport#1-AnalysisofOakdale Water Samples
Exygen Study No. P0001400
LIST OF APPENDICES
Appendix A
Study Protocol P0001400 (Exygen Study No. P0001400) with Analytical Method: V0001780:"MethodofAnalysis for the Determinationof Perfluorooctanoic Acid (PFOA) in Water by
Page
Exygen Research
:
!
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--_--m--m------ Interim Report #1-AnalysisofOskdale Water Samples
Exygen Study No. PO0D1400
1.0 SUMMARY Exygen Research extracted and analyzed water samples for the determination of perfluorooctancic acid (PFOA), perfluotobutancsulfonate (PFS), perfluorohexanesulfonate (PFHS), and perfiuorooctanesulfonate (PFOS) according to Exygen Method 001780 (Appendix A). `The limit of quantitation for PFOA, PBS, PFHS and PFO in water was 50 ng/L and the limitofdetection for PFOA, PFBS, PFHS and PFOS in water was 25 ng/L. Analytical results for the analysis of PFOA, PBS, PFHS and PFOS in water samples are summarized in Table 1. The overall average percent recoveries standard deviations for all fortifications of PFOA, PFBS, PFHS and POS in water samples were 93% + 19, 141% 21, 96% 15 and 109% * 32, respectively. The overall average percent recovery
+ standard deviation for all fortifications of the surrogate field spike compound, PC-
PFOA, in water samples was 3% + 21.
2.0 OBJECTIVE The objective of the analytical part of this study was to determine levels of perfluorooctanoic acid (PFOA), perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFE), and _perfluorooctanesulfonate (PFOS) in water accorditnog Protocol PO001400 (Appendix A).
3.0 INTRODUCTION
TahnidsPreOpoSrtidnetwaaitlesrtuhseirnegsutlhtes aonfaltyhteiacnaallmyseitshfoodr etnhteitdleetde,r"mVin0a0t0i1o7n8o0f:PMFeOtAh,odPFoBfSA,naPlFysHiSs for the Determinationof Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS."
The study was initiated numberPO001400, The
on March 03, analytical start
2005, when date forthis
the study director interim report was
signed protocol March 21, 2005,
and the analytical termination dat for this interim report was April 21, 2005.
Exygen Research,
.
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Interim Report#1-AnalysisofOakdale Water Samples
ExygenStudy No. PO001400
4.0 ANALYTICALTESTS, ES
One hundred and twenty-one water samples, which correspond to twenty-nine sample
sites, were
(Exygen received
atIDamCbOie0n6t44t0e4m-pCe0ra0t6u4r4e3o8n,
MCaOr0c6h441452,.C2O000654f4r6o1m,
TCiDmO6F4r4i6n7k-Ca0t0W6e4s5t3o2n)
Solutions, Inc. The samples were logged in by Exygen' personnel and placed in
refrigerated storage.
Sample log-in and chain of custody information is located in the raw data package associated with this interim report. Storage records wilbekept at Exygen Research.
5.0 REFERENCE MATERIAL
`The analytical standard, PFOA, was purchased from Sigma Aldrich and was received at Exygen on December 03, 2003. The sumogate spiking standard, "C labeled 3peMrfCluocmrpoaocntya.noiTchaeciadna(lytCicaPlFOstAa)n,dawrdass, rPeFcBeiSveaduadtPEFxHySg,enweorne Aspurpiplli1e5d, b2y0034M.froPmFBthSe was received from 3M at Exygen on July, 06, 2000. 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. PFOA was stored. raemfbriiegnetr.ated.PFBS, PFHS and C PFOA were stored frozen and PFOS was stored
CPomFpOoAund PPCFPBFSOA PFHS PFOS
ExvgSePn[0n0v0e3n8to0r0yNo.. -21Lo6tH#B Pur9i7t.y6(4%) Expi1r2a/t0i8o/n05Date
SSPP0O000004215824 350170-1195 996.77 01321/209410069
SP0002401
SEO3S 986 10/1806
SP0002694 401801 1012 04/23/06
`The molecular structuresof
following pages:
PFOA,
"*C
PFOA,
PFBS,
PFHS
and
PFOS
are
given
on
the
Horney Exygen Research
Poge 13 of 110
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InterimReport#1-Analysis of Oakdale WaterSamples
Exygen Study No.: POOOL400
PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight: 414 Transitions Monitored: 413 -- 369 (for quantification) and
413 > 219(forconfirmation)
Structure:
FF
FF F
H
FF F F
CBhCemPiFcaOlAName: 1,2-13C perfluorooctanoic acid Molecular Weight: 416
DOU TSrtaruncstiutrieo:n Monitored: 415 -- 370
:
F
9
E1 ERE
ne" Nou
PChFeBmSical Name: Perfluorobutancsulfonate
Molecular Weight: 338 supplied as the potassium salt (CFsSOyK")
`Transitions Monitored: 299 -- 99 Structure:
[3 F F E 503 .
FlFrE
Tai Exygen Research
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foterimReport#1-AnalysisofOskdale WaterSamples
Exygen Study No: PODO1400
PFHS Chemical Name: Perfluorohexanesulfonate
Molecular Weight: 438 supplied as the potassium salt (CgF1;SO5K")
`Transitions Monitored: 399 -- 80
Structure:
FF
F
F 503 .
F FF
CPhFeOmiScal Name: Perfluorooctancsulfonate
Molecular Weight: 538 supplied as the potassium salt (CyF1;SOyK")
`Transitions Monitored: 499 --> 80 Structure:
F FlF FE]FI]F F 503 .
7F F
FF FF
6.0 DESCRIPTION OF ANALYTICAL METHOD
PTehrefluaonraloyotcitcaanloicmeAtchiodd(P"FVO0A0)01i7n8W0a:teMrebtyhoLdC/oMfS/AMnaSl"yswiass ufosredtfhoer tDheitsesrtmudiyn.ation of
6.1. Extraction Procedure
A 40 mL aliquot of the water sample was used for the extraction procedure. After
fortification of appropriate samples, the samples were loaded onto a Cis SPE cartridge conditioned with 10 mL of methanol and 5 mL of water. The eluate was discarded.
Approximately five millilitersof methanol was added to the cartridge. Five milliliters of cluate was collected into 2 graduated 15mLpolypropylene centrifuge tube. Each sample
was analyzed by LC/MS/MS electrospray.
Bygen Research
EHOna
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InterimReport #1-AnalysisofOakdale Wate Samples
Exygen Study No. P0001400
6.2 Preparation of Standards and Fortification Solutions
Individual stock standard solutions of PFOA, C PFOA, PFBS, PFHS and PFOS were
prepared as specified in Exygen method V0001780. The stock standard solutions were prepared at a concentration of 100 pg/mL by dissolving 10 mgofeachofthe standard (corrected for purity and salt content, ifnecessary) in methanol. From these solutions, LO ug/ml. forification standard solutions were prepared by taking 1 mL of the appropriate stock and bringing the volume up to 100 mL with methanol. By taking 10 mLofthe appropriate 1.0 pg/mL. fortification standard and bringin the volume upto 100 mLwithmethanol, 0.1 pg/mL fortificationstandardswere prepared. By taking 10mL of the appropriate 0.1 pg/mL fortification standard and bringing the volume up to 100 mL with methanol, 0.01 g/ml. fortification standards were prepared.
Sperveepraarledseitns
woaftsetraanndadrpdrsocceosnsteadintihnrgouPgFhOAth,e
C PFOA, PFBS, PFHS and
extraction procedure, identical
PFOS were
to samples.
`The following concentrations were prepared:
Conc.of Fort Fort Volume of
Solution Volume Fortified Sample
(ng/mL)
WL)
(mL)
0
0
"0
10
100
"0
10
200
"0
10
400
40
100
100
0
100 200
"0
! ofPF1O00A, VC PFO4A0,0PFBS, PHS a4n0d PFOS
CFailniablraCtoinocn.Stodf. (ag) 0 25 50 100 250 500 1000
An additional mixed stock solution of PFOA, C PFOA, PFBS, PFHS, and PFOS was
prepered. at 1000 pg/mL and diluted to 100 and 10 pg/mL for bottle spiking purposes. `Complete detcaanbieflousndintherawdatapackage associated with this study.
The stock standard solution and al fortification and calibration standard solutions were stored in a refrigerator (4 + 2C) when not in use. Documentation of standard preparation is located in the raw data package associated with this interim report.
Exygen Research
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Interim Report#1-AnalysisofOskdle Water Samples
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63 Chromatography Quantification of PFOA, PFBS, PFHS and PFOS was accomplished by LOMSIMS electrospray. The retention time of PFOA, PFBS, PHS and PFOS was ~12 min, ~5 mins, ~11 mins, aod ~13 mins, respectively. Peaks above the LOD were not detected in anyofthe reagent blarik samples corresponding to the analyte retention time.
6.4 Instrument Sensitivity The smallest standard amount injected during the chromatographic run had a concentraotfi2o5n ng/LofPFOA, PFBS, PFHS and PFOS.
6.5 Description of LC/MS/MS Instrument and Operating Conditions Instrument: API4000 Biomolecular MessAnalyzer Interface: Turbo lon Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400
Software: Windows NT, Amalyst 14.1 HPLC: Hewlett Packard (HP) Series 1100
HP Quat Pump. HP Vacuum Degasser HP Autosampler HP Column Oven HPLCColumn:ThermoFluophaseRP, 50mam 2.1 mm Column Temp.: 30C MIonbjeiclteioPnhVaosle.:(A1)5: uL2mM Ammonium Acetate in water Mobile Phase (B): Methanol
Time(min) 00
6%5A
%35B
10
65
35
80 25
7s
100 25
7
110 65
35
Totalruntime:~11880min 65
35
Flow Rate: 0.3 mL/min
Shep Tr
Exygen Research
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Interim Report #1-AnalyssofOskcle Water Samples
Exygen Study No. POOI00
Lons monitored:
Analyte
PFOA PFOA Confirmlon
13CPFOA PFBS
PFHS PFOS
Mode
negative negative negative negative negative negative
Transition
Mo4n1i3to3r6e9d 413-5219 4155370 29999 399-580 49980
Approximate
Retention Time
~1(2mimni)n. ~12 min. ~12 min ~5 min. ~11 min ~13 min.
6.6 Quantitation and Example Calculation
Fifteen microliters of sample or calibration standard were injected into the LC/MS/MS. "Thepeakareawas measuredand thestandardcurve wasgenerated(using 1x it weighted linear regression) by Analyst software using six concentrations of standards. The concentration was determined from the equations below.
Equation1 calculated the amountofanalyte found (in ng/L, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program.
Equatio1n: Analyte found(ng/L) =(Peak area -interceptx) DF
Where: DF = Dilution Factor, factor by which the fsilnoaplevolume was diluted, ifnecessary.
pFroirorsatompelxetrsacftoirotnif,iEedquwaittihoknn2owwansaumsoeudnttoscoaflcPuFlaOtAe,thPeFpBeSr,cePntFHreSc,ovPerFyO.S and "'C PFOA
Equation 2: Recovery (4) =
{analytefound (`nagm/oLu)n-taandadleytde(inngc/oLn)trol(ng/L) x100%
An example ofa calculation using an actual sample and resuls from the PFOA analysis
follows: `Water
sample
Exygen
ID
C0064432
Spk
F
(Set:
03210SBR),
fortified
at
50000
nL
with PFOA where: peak area
= uel
intercept
= 26200
slope
=1
dilution factor
=0
ng/L PFOA added (fort level) amt in corresponding sample (ng/L)*
= =
50000 37600
(*The primary sample result was used for all calculations)
Bxygen Research
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Exygen Study No.: PO0O1400
From equation 1: Analyte found (ng/L) = [117130=3021626001] x 100
From equation 2: % Recovery
= 86012ngL* = (86012ng/L--376000g/L) x100%
50000mg/L
= 97% (+values are slightly differeat from raw ata due to rounding)
7.0 EXPERIMENTALDESIGN
s3aCmpPleFcOoAllewcatsionusboetdtlaess ain stuhrelroagbaotreatfoorrybalelfotrheebseaimnpglessh.ippCedPtoFOthAe fwiaelsdfoadrdseadmptlointgh.e For samples designated as field matrix spikes, PFBS, PFHS, PFOS and PFOA were also addeda & known concentration to the bottles in the laboratorybefore being shipped to thefield. The sampleswerefilled to 2 200mLvolumetric filllineinthefield.
The samples were extracted in five sets. Each set consistedof onereagentblank and two reagent blanks fortified at known concentrations. The first set contained six sample sites, the second set contained six samples sites, along with a tip blank and two trip blank spikes. The next two sets contained seven sample sites cach. The fifth set contained three sample sites, along with a second trip blank and two trip blank spikes. For cach sit, 2 sample, a fieldduplicateand two-matrix field spikes were collected. For each site, a laboratory duplicate of the primary sample was extracted and two laboratory matrix spikes were also extracted. Forthe two laboratory marix spikes, two40 mL portions of the primary sample collected for the site was poured from the botile and fortified. Not onlywere PFBS, PFHS, PROS and PFOA addedinthe laboratory prior to extraction, but
also C PFOA was added. The additional "'C PFOA was added because the levels of
PFBS, PFHS, PFOS and PFOA spiked. ino the samples were known to exceed the calibration ranges and were not analyzed without dilution; therefore, C PFOA levels were adjusted to require the same dilution as the other analytes.
For cach primary sample collected, between the field and lab; seven individual QC results
`were reported for "C PFOA. Some samples gave recoveries for "C PFOA outsideofthe `normal acceptance rangeof70-130%. Because laboratory control spikes for 'C PFOA
`PwFerOeAacrceecpotvaebrlyepienretvheersyesveetn, idnosnterufmoerntthewassahmepslewweraes aficcceepotfablCe aPnFdOnAo,eavtidleenastteornroersiCn spiking or extracting could be found, no re-extractions were performed. C PFOA recoveries outsideof 70-130% are deemed indicative of matrix effect.
Exygen Research
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Exygen Study No. PO0L400
8.0 RESULTS Analytical results for the analysis of PFOA, PFBS, PFHS, and PFOS in water samples are summarized in Table I Fortification recoveries for PFOA, PFBS, PFHS and PFOS in the water samples are ddeetvaiialteidonsinfoTraablllefsortIiIficaantdionWs IofPFTOheA,oPveFrBaSll, PavFeHrSageanpdePrcFeOntS riencwoavtereiressam+plsetsanwdearred. 93% 19, 141% 21, 96% = 15 and 109% 32, respectively. Fortification recoveries
for *C PFOA in the watersamplesare detailed in Table IV. The overall average percent
recovery + standard deviation for all fortifications of "C-PFOA in water samples was
83%=21.
9.0 CONCLUSIONS P"TFheOwAataecrcsoarmdpiltensgowaenraleytsiuccaclesmseftuhlloyde0xt0r0a1c7te8d0a.ndTahnearleyzweedrfeonroPFcBirSc,umPsFtHanSc,esPFthOatSmaanyd have affected the data quality or integrity.
10.0 RETENTION OF DATAAND SAMPLES wAilllobreigisnhailpppaepdetrodtahtea sgpeonnesroart.edTbhyisExdoyegsennoRtesienaclrucdhetfhaactiplietryt-aspiencitfoicthriaswindtaetraimsurcehpoarst tihnestirnutmeernitmoarntaelmytpiecraaltruerpeorltogasn.d aElxlacortigcionpailesfoacfiallilt-rsapewcdiafitcs,raaswwdealtal,awsiaslibgeneredtcaoipneydoifn the Exygen Research archives for the period of time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792.
Exygen Research
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Page 200f 110
000043
InterimReport#1-Analysis ofOs WaterSa amples Exysen Study Nog PO0OL400
TRA ExygenResearch
Page 21of 110
000044
InterimReport #1-Analysis ofOakdale Water Samples
[Exygen Study No.: P0001400
Tablel. Summary of PFBS, PFHS, PFOS and PFOA in Water
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Page 2206110 000045
Intern Report#1-Asalysi ofOakdaleWaterSamples
ExygenStudy No: PO0O1400
Tablel.
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Page 23 of 110
000046
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Interim Report #1-Analysis ofOakdale Water Samples.
ExygenStudy No.: P0001400
TableIL. Matrix Spike Recovery of PFBS and PFHS in Water Samples
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Page 24of 110
000047
Tori Report 1 AnalysisofOnl We Ses ExStyyNgo.PeODInA0
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Page 25 of 110
000048
------
Interim Report #1-AraolfyOsskialse Water Samples.
Exygen Study No. P0001400
Table II.
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Matrix Spike Recovery of PFBS and PFHS in Water
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Page 26 of 110
000049"
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Table Il. Matrix Spike Recovery of PFBS and PFHS in Water
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Page 27of 110
000050
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Table Il. Matrix Spike Recovery of PFBS and PFHS in Water
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Page280 110
000051
------
InterimReport #1-AnaolfOyaskdialse WaterSamples
ExygenStudy No.: P0001400
Table Il.
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Page 29.0110
000052
Interim Report #1-AnalysisofOakdale Water Samples
`Exygen Study No.: PO001400.
`Table ITL. Matrix Spike Recovery of PFOS and PFOA in Water
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Interim Report#1-AnaolfyOaskdialse WaterSamples
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Page 31 of 110
000054
Interim Report #1-AnalysisofOakdale Water Samples
ExygenStudyNo.: P0001400
Table IIL. Matrix Spike Recovery of PFOS and PFOA in Water
Samples Continued
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Page 320f 110
G000S5
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InterimReport#1-AnalysisofOakdale Water Samples
ExygenStudy No.: PO001400
Table IIL Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued
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Page 33 of 110
000056
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InterimReport#1-AnalysisofOakdale Water Samples
Exygen Study No.: P0001400
Table III. Matrix Spike Recovery of PFOS and PFOA in Water
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Page 340f 110
000057
--------------------------------------------------------------------------------------------------------------------eeeeeeeeeeeeeeee
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No.: P0001400
Table IIL.
Matrix Spike Recovery of PFOS and PFOA in Water
mregE i e we E_E-- Samples Continued
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Page3601110
000059
InterimReport#1-Analysis ofOskWadtersSalmplees
Exygen StudyNo. POO1400
Table IV. Surrogate Spike Recovery of "C PFOA in Water Samples Continued
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Exygen Rescarch
Page370f 110
000060
F--
Interim Report #1-Anlysis ofOakdale Wate Samples
Exygen Study No.: POOL
Table IV.
Surrogate Spike Recovery of C PFOA in Water Samples
Continued
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Page 3801 110
000061
--
-_----
Interim Report #1-Analysis ofOakdale Water Samples
Exygen Study No.: PO001400
Table IV.
Surrogate
Spike
Recovery of
Continued
C
PFOA
in
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Page 390f 110
000062
--_--
IneriraReport#1-AnalysisofOskdale Water Samples ExygenStudyNo. POOO1400
TableIV. Surrogate Spike Recovery of "C PFOA in Water Samples
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Pag0e04000f016103
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Interim Report #1-Analysisof Oakdale Water Samples
Exygen Study No.: P0001400
Table IV. Surrogate Spike Recovery of C PFOA in Water Samples
Continued
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cQo0o0s4asSa3o1 OKOMNNLOIWTGHR-ITRZIOPZIO0SSI3S1Hk0OeLSopew Sw0o0 1aw C0052 ORLUNGWRFZHiOghS0p0eOMp0n 50000 52000
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Page 410f110
000064
Incr Report #1 AnalysisofOsa Wate Samples Exygen Stdy No: POODIA00
Eaygen Research
Page 4200110 000065
-_--mm----
Interim Report #1-AnalysisofOskdsle Water Samples
Exygen Study No: PO0DI00
Figure I. Typical Calibration Curve for PFOA in Reagent Water
iy
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Exygen Research
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Page 430110
000066
LL
Interim Report #1-AnalysisofOskdale Water Samples
`Exygen Study No.: P0001400
Figure2. Extracted Standards of PFOA in Reagent `Water, 25 ng/L
and 50 ng/L, Respectively
WEE
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Page ator 110 000067
------------------A-------------- ---- ----------
InterimReport 1Acsyss ofOsi Water Sales Exygen Study Nos FUOLAO0
Figure3. aPnFdO5A00innRge/aLgFeonrttiWfaietderR,ea5g0enngt/WLaFtoerrt,ifRieesdpReectaigveenltyWater, NTS roses
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Foo
Note: A linear lot ofPFOA was used to calibrate the instrument. The two peaks shown
in Figur4e are due to different isomerspresentin environmental samples. The area
`counts for all isomers prearse ienclnudted to reportonetotal PFOA value.
Taran, Buys Research
Page dSor110
000068
Ioteim Report #1-Anaolf yOlsailse Water Sap
Exygen Sudy No: POOOI00
Figured. ef
Chromatogram Representing an Oakdale Water Sample Analyzed for PFOA, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)
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Interim Re#p1oAnarlystis ofOlle Water Samples
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Figure 5. Typical Calibration Curve for C PFOA in Reagent Water
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Page 470110
000070
------
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No.: P0001400
Figure 6. Enxgt/rLa2ctnedd5S0tnagn/dLa,rdRsesopfectCivPelFyOA in Reagent Water, 25 BL EE Te
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Page 48 of 110,
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Interim Rep#1oAnarlystisofOskdale Water Samples
Exygen Sudy No. Poo01400
Figure 7. WCatePrF,OaAndin50R0eangge/nLtFWoarttiefri,ed50Renagg/eLntFoWratitfeire,d RReesapgeecnttively WE Teeebent
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Page 4900110 000072
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Interim Report #1-AnalysisofOakdale Water Samples
`Exygen Study No: PO001400
Figure. WC
Chromatogram Representing an Oakdale Water Sample
Analyzed for C PFOA (Exygen ID: C0064522, Data Set:
032405C) ERE
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Page $007 110
000073
------------+--
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Figure. Typical Calibration Curve for PFBS in Reagent Water
g
23 72a
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Page 51 of 110
000074
--------------------------------------------------------e--e----e
Interim Report #1-Analysis ofOakdale Water Samples
ExygenStudy No.: PO001400
Figure 10.
Extracted Standards of PFBS in Reagent Water, 25 ng/L and 50 ng/L, Respectively
WE TT ee
5:
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Bxygen Reseach
Page 5206110
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Exygen Study NosPUOOL400
Figure 11. PanFdBS50i0n nRge/aL.geFnorttWifaiteedrR,e5a0genngt/LWaFtoretri,fiReedspReecatgievnetlyWater, WT --------------"
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Interim Report#1-AnalysisofOskdale Wate Samples ExeStudy No: POOOL400
Figure 12.
Chromatogram Representing an Oakdale Water Sample
Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data
Set: 032405CR)
W AA I A en
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2
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Page S4of110
000077
InterimReport #1-Analysis ofOakdale Water Samples
ExygenStudyNo.: P0001400
Fire geure m13. ---------------- Typical Calibration Curve for PFHS in Reagent Water
i
i
2
:
----
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I
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Figure 14. Extracted Standards of PFHS in Reagent `Water, 25 ng/L
and 50 ng/L, Respectively
WR ER
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IR
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Exygen Research id
Page 560110 000079
--_--_------
Interim Report #1-Anelysis of Oakdale Water Samples
`Exygen Study No. P0001400
Figure 15. PanFdH5S0i0nnRge/aLgeFonrttiWfaiteedrR,e5a0genngt/LWaFtoertri,fRieedspReecatgievenltyWater,
WAS rove poms --------
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Exygen Research Raa
Page 5706110 000080
_
Interim Report #1-Analysis of Oakdale Water Samples
Exygen Study No.: P0001400
Figure 16. Chromatogram Representing an Oakdale Water Sample Analyzed for PFHS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)
BSRRR oe
s:
if:o
Exygen Research Pa
Page S801 110 000081
-
InterimReport#1-AonfaOkldayleWsatser Samples Exygen Study No. P000L400 Figure 17. Typical Calibration Curve for PFOS in Reagent Water
.
1 wl
.
2
Bangg Exygen Research
Page 59of 110
000082
FE
--------
Inter Report #1-AzalysisofOkla Water Sumples Exygen Study No: PO001400
Figure 18. Extracted Standards of PFOS in Reagent Water, 25 ng/L
and 50 ng/L, Respectively
WOR Ar E ee
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Page 600110
000083
InterimReport#1-AnalysisofOakdale Water Samples.
Exygen Study No.: PO001400
Figure 19. aPnFdO5S00innRge/aLgeFonrttiWfaiteedrR,e5a0genngt/LWaFtoertri,fRieedspReecatgievenltyWater,
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Page Sof 110 000084
a.
Interim Report #1-Analysisof Oskdale Water Samples
`Exygen Study Noi: 0001400
Figure 20. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOS, DF=100 (Exygen ID: C0064522, Data
Set: 032405CR)
WC RR STR
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=
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Exygen Research
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Page 620110
000085
i
--_-- nei Re#p1 Aanalrysistof Oakdale Water Samples ExyienStudy Nos PO0O1400
APPENDIX A
Study Protocol
P0001400 (Exygen Study No. P0001400) with Analytical Method: V0001780:"Method of Analysis for the Determination of
Perfluorooctanoic Acid (PFOA) in Water
by LC/MS/MS"
8
Exygen Research
Page 63 of 110
000086