Document a4L86apjpwMyzxMdx44XjK1oN
AAR2R2E6--33663364
INTERIM REPORT 61 Analvss ofOakdale Water Samples
STUDYTITLE
Analysis of Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS),
Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil,
Sediment, Fish, and Clams Using a: LC/MS/MS for the 3M Cottage Grove Monitoring
DATA REQUIREMENTS [EPA TSCA Good Laboratory Practice Standards 40 CFR 792
STUDY DIRECTOR
Jaisimha Kesari P.E., DEE `Weston Solutions, Inc.
Wes1t40Ch0eWsteesrt,oAn Wa19y380
Phone: 610-701-3761
INTERIM REPORT COMPLETION DATE
*
May 19, 2005
PERFORMING LABORATORY
`Exygen Research
St3a0te58CoRelseeagrcPhADr[i6v8e01
Phone: 814-272-1039
stuSpMyCsomppoannsyor
3M Building 0236-01-B-10
PSht.onPea:ul6,5M17N35556154744 PROJECT
Protocol Number: P0001400
Exygen Study Number: P0001400
Tout Pages: 110
000024
ir. om
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT
Exygen Study Number P0001400, entitled "Analysis of Perfluorooctanoic Acid (PFOA), Perfiuorobutanesulfonate (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 LaboratoryPractice
Standards 40 CFR 792 by Exygen Research.
/2 [La
Efrz.e Principal Investigator
JaisimhaKesari P.E., DEE `Weston Solutions, Inc.
Robert A. Paschke
`Sponsor Representative
3M Company
_ za Spas
Die Date
paal
S000 600028
InterimReport #1-AualysisofOakdale Water Samples Exygen Stady No: PO0OI400
QUALITY ASSURANCE STATEMENT
Exygen Research's QualityAssurance Unit reviewed Exygen Study Number P0001400,
entitled, "Analysis of Perfluorooctanoic Acid (PFOA), Perfluorobutanesulfonate (PFBS),
Perfluorohexanesulfonate (PFHS), and Perfluorooctanesulfonate (PFOS) in Water, Soil,
Sediment,Fish, and ClamsUsingLC/MS/MSforthe 3MCottageGroveMonitoring
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 InvesantdMiangagaemtenotarndtothe Study Director.
Date DetPrRiencpioparlt|etdoDatRBexpyagrtmed to DitoReporiedto
Phase
Inspected Investigator Management Study Director
1. Protocol Review
03/24/05
03/25/05
03/29/05
05/19/05
2 DmctiooReviow OY2OS OMS0S 0905 0s19NS
andnr 3. Raw Data Review
Analytical Report Review
OsaG1TS
osnsbs
osaons
osiisns
TR haitter
Te ical Lead, Quali surance Unit
Butpe5l17fes
"Note: All inspections will be documented in the QA statement for the final analytical
reportattheconclusionofthe study.
Exygen Research
BUOO@RO0 IG
Page3of 110
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Interim Report#1Analysis ofOakdale WaterSamples Exygen Study Noi PO001400
CERTIFICATION OF AUTHENTICITY
This interim report, for Exygen Study Number P0001400, is a true and complete representationof the raw data.
Submitted by:
Exygen Research
S3t0a5t8e CRoelsleeagrec,hPDAri1v6e801
(814) 272-1039
Principal Investigator, Exygen:
fd
BVixhcynegePFnrleaRsheiedsretenyatrch
Asks
Date.
`Exygen Research Facility Management:
Cu, ]
RBPirxecyshgiaedrendntA. Research Sudy y Weston Solution, Inc.
5-405
Date.
Jaisimha Kesari P.E., DEE `Weston Solutions, Inc.
`Sponsor Representative, 3M Company:
< os
Robert A.
Manager,
Paschke
3M Corporate
Environmental
Programs.
Exygen Research Fo. s
Dad
Joilos
Date
Page 0110
000027
Interim Report #1-AnalysisofOskdale Water Samples
Exygen Study No.: POOOIA00
'UDY IDENTI
TION
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
"PROTOCOL NUMBER:
'P0001400
EXYGEN STUDY NUMBER:
PO001400
TYPE OF STUDY: SAMPLE MATRIX: `TEST SUBSTANCE:
Residue
`Water
Perfluorooctanoic acid (PFOA),
Perfluorobutanesulfonate (PFBS),
PPeerrfflluuoorrooohcetxaanneessuullffoonnaattee((PPFFOHSS)), and
SPONSOR:
33MM BCuoimlpdianngy0236-01-B-10
St. Paul, MN 55144
STUDY DIRECTOR:
aot amon way Jaisimha Kesari P.E., DEE
Weston Solutions, Inc. `West Chester, PA 19380
SPONSOR REPRESENTATIVE:
Robert A. Paschke
SBPoiMnEg LS981827 3M Company
PERFORMING LABORATORY:
Exygen Research
3St0a5t8e RCoelsleeagrec,hPDAri1v6e801
ANALYTICAL PHASE TIMETABLE:
tac Sominaton Date GAZ1108 `Study Initiation Date:
Interim Analytical Start Date:
03/03/05 03/21/05
Interim Report Completion Date: ~~ 05/19/05
Sriya
`Exygen Research
Page Sof 110
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Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No. PO00I400
PROJECT PERSONNEL
The Study Director following personnel
for this project is Jeisimha Kesari at Weston Solutions, Inc. from Exygen Rescarch were associated with various phases of
The this
interim portionof the study:
Name John Flaherty Karen Risha Paul Connolly Chrissy Edwards Mark Ammerman Amy Sheehan Eric Edwards James Miller Edward Kaiser
Tite Vice President
Scientist Technical Lead-LC/MS.
Technician Sample Custodian Associate Scientist Sample Custodian
Scientist Scientist
Exygen Research
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InterimReport#1-AnalysisofOakdale Water Samples
`Exygen Study No.: P0001400
TABLE OF CONTENTS
TITLE PAE dps Ts mdhgummdPeag]e Q`GUOAOLDILTYABAOSRSAUTROARNYCEPRSATCATTICEEMECONMTP.L.I.ANCE STATEMENT ...c.occvvvrrmrrrns2n
PROJECT PERSONNEL......ccorovrr rns orrsnscon sisesssessretrsrsertem messes
EISTOFAPPENDICES cummings]
$0 BOIRODUCHON, fis sarsiagmmemniimonimgmnimmmmmerrmrth 4$.00 BAINRAOLYITINCEALMTAESTT SEAMRPLEwSus.foraragaems mnsmgemmsmmsmmmer1s3h
6.0 DESCRIPTION OF ANALYTICAL METHOD ....coccornmrmnnrismsssssssssssssssssenens 15
6.2. Preparation ofStandards and Fortification SOItONS...........uursssssssssssssrrsenss 16.
CA TRSOIE yr gonna uoaprngpmmmmeminnetd
6.5. Description of LC/MS/MS Instrument and Operating Conditions...
7
6.6.Quantitationand EXAmPle Calculation. .............uwwrvrscemermininnsorecs 18
7.0 EXPERIMENTAL DESIGN .....oocoonomnimmiirmmrsmssrsinssesmssns sss sssssssssssssssne: 19.
9.0 CONCLUSIONS... orem
20
10.0 RETENTION OF DATA AND SAMPLES .....occoreovvocmmnsrnssnsssssssssssssrsssssennn 20
`Exygen Research
EAGT
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Interim Report #1-AnalysisofOakdale Water Samples
ExygenStudy No: POD01400
Table].
TabloTL. Table I.
Table IV.
LIST OF TABLES Page
SummaryofPEBS, PFHS, PFOS and PFOA in Water
Matrix Spike Recovery ofPEBS and PFHSin Water Samples..............24 Matrix Spike Recovery of PFOS and PFOA in Water Samples............30
Surrogate Spike Recoveryof C PFOA in Water Samples ..............w....36
Fxygen Research,
'
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Interim Report #1-AnalyssofOakdale Water Samples
Exygen Study No. PO001400
Figure 1. Figure 2. Figure 3. Figure 4.
Figure S.
Figure 6.
Figure 7. Figure. Figure 9. Figure 10.
LIST OF FIGURES
Page
Typical Calibration Curve for PFOAinReagent Walef........cr.conid
Extracted Standards ofPFOA in Reagent Water, 25 ng/L and 0 ng/L, ROPE -rmnssmmsemmmssmmenesmsrossemsmnerns PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, RESPECHVY rrr Chromatogram Representing an Oakdale WaterSample: Analyzed for PFOA, DF=100 (Exygen ID: C0064522, De Set: BSC immmnniagrmnsmmmesmmstmmmmtnnmtl
TypicalCalibrationCurvefor C PFOA in Reagent Water ...................47
Extracted Standards of "*C PFOA in Reagent Water, 25 ng/L
1 SONL,RESPECHVEY.rrrrnrnrr ncn
88
""CPFOA in Reagent Water, S0 ng/L Fortified Reagent Water, and S00 ng/L Fortified Reagent Water, RESPECHVEY...........orcrcreed)
Chromatogram Representing an Oakdale Water Sample:
Analyzed for "C PFOA (Exygen ID: C0064522, Data Set: 032405C).........50
Typical CalibrationCurvefor PFBS in Reagent Waler....ovvvnoronsS1
Extracted Standards ofPFBSin Reagent Water, 25 ng/L and 50 ng/L,
Figure 11. PFBS in Reagent Water, 0 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, RESPECHVElY......roeurrrvvs 53
Figure 12. Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data Set:
Figure 13. Figure 14. Figure 15. Figure 16.
Figure 17.
Typical Calibration Curve for PFHS in Reagent WAL ......ovevrrr 55
Extracted Standards ofPFHS in Reagent Water, 25 ng/L and 50 ng/L, BADR gmmmmminesmmmmmmmmmssmmamnds
PFHS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 g/L Fortified Reagent Water, RESPECHYElY..r.cvrvovrrarrvsmnns ST
Chromatogram Representianng Oakdale Water Sample AnalyzedforPHS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR).... nigmR------------------"--
Typical Calibration Curve for PFOS in Reagent Water
mma)
Exygen Research
#2
Pags90f110
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Interim Report #1-AnalysisofOakdale Water Samples
ExygenStudyNo.: POOO1400
LIST OF FIGURES Continued
Figure 18.
Extracted Standards RESPECHVE. eros
of
PFOS
in
ResamgeenntssWastsesrs,s2i5onngs /L andm 50 ngn /L,
80
Figure 19. P50F0OnSg/iLnFRoeratigfeinetd WRaetearg,en5t0Wnagl/eL,FoRrteiSfipedERCetaigeVnetlWYaute.rv,vavndvvvnnrn-61
Figure 20. A-CnharloymzaetdofgorraPmFROeSp,reDsFen=t1i0n0g a(nExOyagkednalIeD:WaCt0e06r4S5a2m2p,leData Set:
O340SCR) rrr eerie
Exygen Research
Fatt
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Interim Report#1-Analysisof Oakdale Water Samples
`Exygen Study No. PO001400
LIST OF APPENDICES
Page
Appendix A. Study Protocol P0001400 (Exygen Study No. PO001400) with Analytical Method: V000I780:MethodofAnalysis for the Determination ofPerfluorooctanoic Acid (PFOA) in Water by
Exygen Research
TESONG,
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Interim Report#1-AnalysisofOakdale Water Samples
`Exygen Study No. 0001400
1.0 SUMMARY
Txygen Research perfluorooctancic
cxtracted acid
and analyzed (PFOA),
wateprerfslaumoprloebsutafnocrsutlhfeonadteete~rm~ina(tiPoFnBS)o,f
perfluorohexancsulfonate (PFHS), and perfluorooctancsulfonate. (PFOS) according to
Exygen Method 0001780 (Appendix A).
"LTheiolifmmditetoiefcqttuiaonntfiotratPioFnOfAo,r PPFROBAS,, PPFFBHSS,aPnFdHPSFOaSndinPwOatSerinwawast2e5r wnga/sL.50 ng/L and the A`nsaulmymtairciazlerdesiunlTtsabfloret1h.e TanhaelyosviesraolflPaFvOerAa,gePpFeBrSc,enPtFrHecSovaenrdiePsFOsStiannwdaartdedrevsiaamtpiloenss afroer all fortifications of PFOA, PFBS, PFHS and PROS in water samples were 93% + 19, 141% 21,96% 15 and 109+% 32, respectively.The overall averagepercent recovery
+ standard deviation for all fortifications of the surrogate field spike compound, "*C-
PFOA, in water samples was 83% +21.
2.0 OBJECTIVE
The objective of perfluorooctancic
the analytical part of acid (PFOA),
this study was to determine perfluorobutanesulfonate
levels of (FBS),
perfluorohexancsulfonste (PFHS), and perfluorooctanesulfonate (PFOS) in water
according to Protocol PO0D1400 (Appendix A).
3.0 INTRODUCTION
TahnidsPrFepOoSrtidnetwaaitlesrtuhseirnegsutlhtes aonfatlhyteiecnaallmyseitshfoodr etnhteitdleetde,r"mVi0na0t0i1o7n8o0f:PMFeOtAk,odPFoBfSA,naPlyFsHiSs forthe DeterminationofPerfluorooctanoic Acid (PFOA) in Water by LC/MS/MS."
The study was initiated number PO001400. The
on March 03, analytical star
2005, when date for this
the study director interim report was
signed protocol March 21, 2005,
and the analytical termination dateforthis interim reportwas Apri 21, 2005.
Exygen Research
wg
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InterimReport#1.AnalysisofOskdale Water Samples
Exygen Study No: POOOL400
4.0 ANALYTICAL TEST SAMPLES
One hundred and twenty-one water samples, which correspond to twenty-nine sample
sites, (Exygen ID C0064404-C0064438," C0064442-C0064461, C0064467-C0064532) `were received at ambient temperature on March 15, 2005 from Tim Frinak at Weston
rSeoflruitgieornast,edIsntco.rageT.he samples were logged in by Exygen' personnel and placed in
Sample log-in and chain of custody information is located in the raw data package
`associated with this interim report. Storage records willbekept at Exygen Research.
5.0 REFERENCE MATERIAL
`The analytical standard, PFOA, was purchased from Sigma Aldrich and was received at
Exygen on December 08, 2003.
perflucrooctancic acid (C PFOA),
wasThreeceisvuerdroagtatEexysgpeinkionng
Apsrtialnda1r5d,,20"04C
frloambeltehde
3M Company. The analytical standards, PFBS and PFHS, were supplied by 3M. PFBS.
`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 ExyognAeprnil 23, 2003
"The available information for the reference materials is listed below. PFOA was stored
ambient. PFBS, PFHS and C PFOA were stored frozen and PFOS was stored refrigerated.
PoFmpOoAund ~~ExvgeSnPI0n0v0e3n8t0or0yNo.. 2L3o1tIG#HB
VCPFOA
SP0004184 3507-195
PFBS
SP0000252
101
PFHS
SP0002401
SE036
PFOS
SP0002694
430180-1
Pur9i7t.y64(%)
97
96.7
98.6 101.2
Expi1r2a/t0i8o/n05Date
0329/09
12/04/06
10/18/06 04/23/06
`The molecular structures of PFOA, *C PFOA, PFBS, PFHS and PFOS are given on the
following pages:
ELOHH
Exygen Research
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InterimReport #1-AnalysisofOakdale Water Samples.
`Exygen Study No.: PO001400
PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight: 414 Transitions Monitored: 413 -> 369 (for quantification) and
413 >219(forconfirmation)
Structure:
E F F BF F FlPErTlE F E `OH
C PFOA Chemical Name: 1,2-13C perfluorooctanoic acid
Molecular Weight: 416
Transition Monitored: 415 - 370
Structure:
FFF 0
wll } A we" Nou
peel]F
ChPeFmBiScalName: Perflsorobutanesuifonate MoTlraencsuitliaornsWeMiognihtto:re3d3:8 2s9up9plie9d9as the potassium salt (C:FsSOyK")
Structure:
F flF r F PlFtlr 503"
Exygen Research
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InterimReport#1-AnalyssofOakdale Water Samples
Exygen Study No.: PO0O1400
PFHS
Chemical Name: Perfluorohexanesulfonate
Molecular Weight: 438
Transitions Monitored:
s3u9p9pl--ie8da0s
thepotassium
salt
(CF1;S0yK)
Structure:
F ELEEE F 503 FFlOeEr CF
PFOS Chernical Name: Perfluorooctanesulfonate: Molecular Weight: 538 supplied as the potassium salt (CoF,SO;K") Transitions Monitored: 499 --> 80 Structure:
F- Fle] EF _503 | flFeOFleF CF
6.0 DESCRIPTION OF ANALYTICAL METHOD
`The analytical method "V0001780: Method of Avalysis Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS was
for the Determination used for this study.
of
6.1. Extraction Procedure
A 40 mL aliquot of the water sample fortification of appropriate samples, the
was used for samples were
the extraction loaded onto a
procedure. After Cis SPE carridge
Acopnpdriotxiiomnaetdelwiytfhiv1e0mimllLiliotefrsomefthmaentohlanaonldw5asmaLddoefd wtaottehre. caTrhtreidgcel.uatFeivweamsildliilsictaerrdsedo.f
ewlausataenwalayszecdolblyecLteCd/iMnSto/Ma Sgrealdeucattreosdpr1a5y.mL polypropylene centrifuge tube. Each sample
Esygen Research
pea
amet AY
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InterimReport#1-Analysis ofOakdale Water Samples
Exysen Study No: PO001400
62 PreparationofStandards and Fortification Solutions
pInrdeipvairdeudalasstsopcekcisftiaenddianrdExsoylguetnionmsetohfoPdFVOOA0,017C80P.FOTAh,e PstFoBcSk,stPaFnHdaSrdansdolPutFiOonSs wweerree
prepared at a (corrected for
cpounrcietnytraantdiosnelot fco1n0t0entp,g/ifmnLecbeyssdairsys)olivninmget1h0anmolg.ofFeraochm
of the standard these solutions,
1.0 pgimL. appropriate
fortification standard. stock and bringing the
solutions were prepared by taking volume up to 100 mL with methanol.
1
mL of By taking
the 10
mmLLowiftthhemeaptphraonporli,at0.e11.u0gg//mmlLf.orftoirftiicfaitciaotniosntasntdaanrddasrdwearned pbrreipnagriendg.thBeyvotalkuimneg u1p0mtoL1o0f0
the appropriate 0.1 with methanol, 0.01
g/mL fortification g/m, fortification
standard and bringing the standards were prepared.
volume
up
to
100
mL
pServeepraarledseitnswoaftesrtaannddarpdrsocceosnsteadintihnrgouPgFhOAth,e exCtraPcFtiOoAn,prPoFcBedSu,reP,FiHdeSntaicnadl PtoFOsaSmpwleers.e The following concentrations were prepared:
Conc.of Fort Fort Volumeof
Solution Volume Fortified Sample
(ag/mL)!
0
ul)
0
(mL)
0
10
100
"0
10
200
4
10
400
40
100 100
40
100 100
200 400
40 40
! ofPFOA, "'CPFOA, PFBS, PFHS and PFOS
Final Conc. of Calibration Sid.
(g/L)
0 25 50 100 250 500 1000
pArnepaadrdeidtiaotna1l0m0i0xepdgsmtockansdolduitliuotnedoftoPF1O00A,an"dC10PFpOgA/,mlPBfoSr,boPttFlHeSs,piaknidngPpFuOrSposweass. Complete detailscanbe found in the raw data package associated with tis study.
The stock Stored in
standard solution and a refrigerator (4 +
al fortification 2C) when not
and in
calibration standard solutions were use. Documentation of standard
`preparation is located in the raw data package associated with tis interim report.
Exygen Research a
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term Report #1-Analysisof OakdaleWater Samples
Exygen Study No: PO0OIA00
6.3 Chromatography Quantification of PFOA, PFBS, PFHS and PFOS was accomplished by LC/MS/MS electrospray. The retention time of PFOA, PFBS, PFHS and PFOS was ~12 min, ~5 mins, ~11 mins, and ~13 mins, respectively. Peaks above the LOD were not detected in anyof the reagent blank samples corresponding to the analyte retention time.
6.4 Instrument Sensitivity
-
The smallest standard amount injected during the chromatographic run had a concentration of25 ng/L ofPFOA, PFBS, PFHS and PFOS.
6.5
DescriptionInosftrLuCme/nMt:S/MASPIIn4s0t0r0uBmieonmto
and Operating Condi
lecular Mass Analyzer
t
i
o
n
s
Interface: "Turbo lon Spray Liquid Introduction Interface.
Computer: ~~ DELL OptiPlex GX400
Software: `Windows NT, Analyst 1.4.1
HPLC:
HewlettPackard (HP) Series 1100 HP Quat Pump
HHPP VAuatcousuammpDleegrasser
HP Column Oven
HPLC Column: Thermo Fluophase RP, 50 mm x 2.1 mm
Column Temp.: 30C
IMnojbeictlieonPhVaosl.s:(1A5):pL2. mM Ammonium Acetate in water
Mobile Phase (B): Methanol
Time(nin) %A %B
0.0
65
35
10
65
35
108.00
2255
57s
11810.0
6655
335
T FlowouRantetl :im0e:3~m1L8mmiinn
[Exygen Research
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Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No: PO001400
Tons monitored: Andivte PFOA
PFOAConfimlon 13CPFOA PFBS PFHS. PFOS
Mode negative negative negative negative negative negative
Transifion `Monitored 413 369 4135219 415-5370
299599 399580 49980
Approximate Retention Time
(min) ~12 min. ~12min. ~12min. ~5 min. ~11 min ~13 min
6.6 Quantitation and Example Calculation
`FTihfeicpeenakmiacrreoaliwtearssmoefassuarmepldeanord ctahleisbrtaatnidoanrdstcaunrdvaerdwawsergeenienrjaetcetded(uisnitnogt1h/exLfiCt/wMeSig/hMtSe.d lincar regression) by Analyst software using six concentrations of standrds. The concentration was determined from the equations below.
Equation | 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; `Anslyte found (ng/L) =(Peakarea-interceptx) DF slope.
Where: DF = Dilution Factor, factor by which the final volume was diluted,ifnecessary.
pFroirorsatompelxetrsacftoirotnif,iEedquwaittihoknn2owwansaumsoeudnttosocaflcPuFlaOtAe,thPeFpBeSr,cePntHrSec,ovPerFyO.S and C PFOA
`Equati2o:n Recovery ((%a)na=lyte found (ng/L) -analyte in control (ng/L) 100%
`mount added (og)
An example of a calculation using an actual sample and results from the PFOA analysis
follows: `Water
sample
Exygen
ID
CO064432
Spk
F
(Set:
032105BR),
fortified
at
50000
ng/L
with PFOA where: peak area
- ume
intercept
= 2600
slope
= Bp
dilution factor
= 00
ng/L PFOA added (for level)
= 50000
amt in corresponding sample (ngL)* = 37600
(The primary sample result was used for ll calculations)
Brygen Research
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From equation 1: `Analyte found (ng/L) = [1170161 = 26200] x 100 1330
From equation 2: %Recovery
= s6012ngLe = (86012ngL-- 37600ng/L) x 100%
50000 ng/L
= 97% (+valuss are slightly different fom raw data due to rounding)
7.0 EXPE
CAL DESIGN
saCmpPleFOcoAllewcatsionusboetdtlaess ianstuhrerolgaabtoeratfoorryablleftohree bsaemipnlgess.hippCedPtoFtOhAe fwiaelsd faodrdseadmptlointgh.e For samples designated as fiekl matrix spikes, PFBS, PFHS, PFOSand PFOA were also added at known concentration to the bottles in the laboratory before being shipped to the field. The samples were filled to a 200 mL volumetric il line in the field.
`The samples were extracted in five sets. Each set consistedofonereagentblank and two. reagent blanks fortified at known concentrations. The fist set contained six sample sites, the second set contained six samples sites, along with a trip blank and two rip blank spikes. The next two sets contained seven sample sites each. The fifth set contained three sample sites, along With a second trip blank and two trip blank spikes. For each site, a sample,a field duplicate and 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. For the two laboratory matrix spikes, two 40 mL. portions of the primary sample collected for the site was poured from the bottle and fortified. Not only were PFBS, PFHS, PFOS and PFOA added in the 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. into the samples were known to exceed the cwaelriebraadtjiuosntredantgoerseqaunidrewtehreesanomte adnilaultyizoendaswtihtehootuhtedrilauntailoynt;est.herefore, C PFOA levels
For cachprimarysample collected, between the fieldand lab; seven individual QC results
wnoerrmearlepaocrcteepdtafonrce'rCanPgFeOoAf.70S-o1m3e0%s.ampBleecsaugsaevelarbeocroavteorriyescofnotrr"olCsPpiFkOesAfoourtsCideoPfFtOheA.
`were acceptable in
PFOArecoveryper
every set,
the seven
idnosnterufmoerntthewassahmepslewewraes
farceceeopftablCe
aPnFdOnAo,
eavtidleeanstt
eornroersiCn
srepciokvienrgieosroeuxttsriadcetoifng70c-ou1l3d0%bearefoduenedm,endoinrdei-ceaxttirvaecotfiomnastrwiexreeffpeecrtfs.ormed. 'C PFOA
ExygenResearch
EEE
Pege 19.0 110
000042
-------------------------- e-- e --
InterimReport#1-AnalyssofOakdale Water Samples
Exygen Study No. 0001400
8.0 RESULTS
Analytical results for the analysis ofPFOA, PBS, PFHS, and PFOS in water samples are Summarized in Table
Fortification detailed in
recoveries Tables 11
for and
PFOA, PEBS, PFHS and PFOS in II The overall average percent
the water recoveries
samples are + standard
d9e3vi%at+io1n9s, f1or41a%l f=or2t1i,fi9ca6ti%onso1f5PaFnOdA1,0P9F%BS+,3P2,FrHeSspeacntdivPelFyO. SiFonrtwiafticeartisoanmprelceosvewreirees
for 'C PFOA in the water samplesare detailed in Table IV. The overall average percent
recovery * standard deviation for all fortifications of "C-PFOA in water samples was
8%=21
9.0 CONCLUSIONS "PTFheOwAataecrcsaarmdpiltensogwaenraleytsiuccaclesmseftuhlloydeVxOtr0a0c1t7e8d0a.ndTahnearleyzweedrefonroPcBiSrc,umPsFtHanSc,esPFthOaSt maanyd have affected the data quality or integrity.
10.0 RETENTION OF DATA AND SAMPLES
Awilllobreigisnhailpppaepdetrodtahtea sgpeonnesroart.edTbhyisExdoyegsennoRtesiencalrucdhethfaatcipletty-asipnescitfoicthriaswindtaetraimsurcehporats ithnestirnutmeernitmoarnatleymtpicearlatruerpeorltogas.nd Ealxlacotricgoipniaesfoafclailtl-rsapewidfaitce,raasw wdealtla,awa sbiiegrneletdacilonpedy oinf the Exygen Rescarch archives for the period of (ime specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792.
Exygen Research .
Page 200f 110 1000043
IniReport 1-AnsolfOynies Wee Samples BaysSudyNo: FOOLA0O
EeRn0 [----
Page21 of110 000044
----------------------------------------------------------------e--eeeet
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No.: POOI400
Tablel. Summary of PFBS, PFHS, PFOS and PFOA in Water
Samples
sme cronper conor conudanlirens coronas
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a --
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`Exygen Research
rie
Page 220110
000045: +
Interim Report #1-AnalysisofOakdaleWaterSamples
Exygen Study No. PO001400
Table. Summary of PFBS, PFHS, PFOS and PFOA in Water
`Samples Continued
ene, itis cosas cnn
res curren
cTowmhees oSgmmn EonR s uroS. me 21 wn mo o om mmm m=mw=
cTconhu"m, c SoUcMwocs wwNwEmSo. IsEmEy aw a== P psoroo r,
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so
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cToomEenne oSgduOmeoMuvsEwessoRsosSsn TmRo m mwoooE mowom me
oTwTs EouSmowSwwNsom.e wFemo m3m edmE ammm
ccTuHseEs oSotuoUmeNwmsSmoom.ess eax ==rs = o em wm eEm
mcTunsE.s oSoluammnissuesomonnmeone 0%tM I4x" ==- -5=
J
wo w wo
n-- v onei marteb c ra sven
NBG HG
`Exygen Research
Page 2307 110
000046
-- i -------------- So-- eee----
Interim Report #1-AnalysisofOakdale Water Samples
`ExygenStudyNo.: P0001400
Table IL.
Matrix Spike Recovery of PFBS and PFHS in Water Samples
momen |Z0DOD LIZ]
ore |u| vx www em CmOe Jaa| va ww we]
D md
wwe ow ow mew
wim 000 DTN DD
cumgumosminnieonn| ol go wm ow [ww] 0 www (Sm || pen wc [oe ww wwe
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rit wan| mas von vo won| a mew
wim ||
rr" fn| mes
TEREEEL |
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vw wa woo
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ve mw
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Page 24 of 110
1000047.
---------------------- ee-- see-- eea-- mes------ --
InterimRepart #1-AnslyssofOskdsle Water Samples Exygen Sudy Noi PO0OI400
Table Il. Matrix SpSiakmepRleecsovCeornytoifnPueFdBS and PFHS in Water
or
Ss HaS meer SETTIE NL mer
mpi| 0 STN D0 0
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Exygen Research
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Page 250f110
000048
------------------------------------------ere
Interim Report #1-Analysis of Oskdale Water Samples
`Exygen Study No: P0001400
Table Il.
Matrix Spike Recovery of PFBS and PFHS in Water
Samples Continued
sme
aTo erlEiTMvue Tleen" ATM wep
wim (TDD DID WL
ummm || am we we] ol we ow
ebm
TT
coments| fe we
LIT
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mt || ww
maete || ww
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um
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mime| DT TID
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Exygen Reseach
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Page 2601110
000049
------------------------------------i------------ ------------------------ Interim Ror#1-AnalyssofOskdle Water Samples r--
Table IL.
Matrix Spike Recovery of PFBS and PFHS in Water
Samples Continued
samp
Sans heen Me my Sobat Whe Mes Mees
mim[e 2 0 SD TD
Smee (oo oo CW oo
a Ee
meme(0 2 SHLD
ety*TM (eal aw wn. ww |u| - w
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BE hc zH =
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BxpgenResearch
era
Page2706110
000050
tein Report1Als ful WcSerges
ws s---- EStx ly No: Pe OCOIO0
Table Il.
Matrix Spike Recovery of PFBS and PFHS in Water
`Samples Continued
a AY We my pa hs Reon Remy
Jr rig Eed C ael omd i,
srr.
mem |
a] ww
m wiimm i (|7| T00T T DDDDD
Cena (TIT LIDITD
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==
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owl
we =
SmRens
Co
--
000051
--_--mm----
InterimReport #1-AnaolfOyaskdialse Water Samples
`ExygenStudyNo.: P0001400
Table Il. Matrix Spike Recovery of PFBS and PFHS in Water
Samples Continued
it
rdEE we EE
meme (N00 DIDNT
cmt ul em fem] ewe ow neGlare |] ve wife] ww = ota EE.
i
--
26604 Exygen Research
Page29 of 110
000052
ii--------re ---- ------ ------ ------ ----
Interim Report #1-AnalysisofOakdale Water Samples
`Exygen Study No.: P0001400
Table ITl. Matrix Spike Recovery of PFOS and PFOA in Water Samples
sn
Et pri TH WE mgr
mone || et] umm stint|ol compen| | omental
ge uw ww] em we ow mm [em] wn ow ve vm wm| ww vn ww || www we we mm] ow ww
wim |
cometsom ||
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OD
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mommies| | ey me comonomer
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mm -
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CSTD| ao|
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Exygen Research
Page 3001110 000053
S------------------ A -- -------- -------- ------ ----g-- oes ee-- retea-- sier--
Interim Rep#1-oAnarlystisofOakdale Water Samples
ExygenStudy No.: PO0O1400
Table IIL. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued
J
oe iar we es$a TT mo mn
CERN [ee]
mmm
CUNCTENIIIIE |
oe mow we] ke
Lf
v0 see wo [ww] we
mw ow
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Or arr CUMEITIIIZIT
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we
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DT DDT
wo wo| ] ow
mE. | mm mm
CUNDITITIEII en| cus wore wo ome amo wow
SEINE, wo ba wo we fm) wm we om
weg[m L000m L mW ee
CNCEIDIITIE La | 0 mm ow jw we we ow
Tm eie es
Exygen Research
EEOESO0
Page31 0f 110
000054
------------------------------------
InterimReport#1-Analysisof Ouisle Water Samples ExygenStudy No: PU0OLA0D
Table II. Matrix Spike Recovery of PFOS and PFOA in Water
`Samples Continued
so
emsEL
mC orma nemn || we
merrell am
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cuunmgmeirnont||2|
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ExpResearch
Page 320110 000055
r--m------------------------------------------------------------------------------------------------------------------------------
Interim Report #1-AnaolfOyaskdialse Water Samples
ExygenStudyNo.: PO001400
Table IIL. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued
iit apaEE i Ee wr
eFrr etm , ||ee| 0nme C fenm -- =
ngmzmmimeen| C nm|
ow
mm (nm.
comtapivrw ise|
|
a nn
vn +
|| vo. Num | nw
ele|TT TT TT
somerset |_| en nin] wm w- ow
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ExygenResearch
Figs
Pa 33g of1e 10
000056
------------------------------S----
Interim Report #1-AnalysisofOakdale Water Samples.
Exygen Study No. PO001400
Table Ill.
ia
Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued
atptS SITeT TrEes "EHEE,E
rbd ri Sm tn oke | .
un
a |o|n| wme oeno4 [f om|] mw m w ww we
menses ey wn fm] we
a oSTm Eh Ee L
|| |con|
we
wn
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few| nw wm [so] eww
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ole
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an
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oll.
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STL
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cmorotengethese|I| z oso e m + ||.rm
= om
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|l ww fuo| ww ||ey www fo] wo
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ow
cw umenT er Ee E| ||| ry ww wfonm]] n wm owm ow
Exygen Research
;
Page 340f 110
000057
----------------------------------ein--em ------------
Interim Report #1-Analysis ofOakdale Water Samples
Exygen Study No.: P0001400
TableIIL. + Matrix Spike Recovery of PFOS and PFOA in Water
`Samples Continued
i
Ee i TE ie wa
I Aw ww = fled.
mee (2 2S Sf
SATIRE Lois vot cover 0 Jo] ramen WT | | um i fn] CIEL || to sen vo fimo]
TT Tr anntamed
Smo
= wr ve we ow 0 ww we
=7
Tpit
RED
)
Page 3501110 000058
em reree e ee e r ee
Interim Report #1-AnaolfOyaskdialse Water Samples
EBxygenStudy No.: PO001400
Table IV. Surrogate Spike Recovery of "C PFOA in Water Samples
Ueoron
Egon
TTTSamplT e TT e`Sepked RecoverReeemd Recovery
CaC0osun40e4os5pskk 0 Conscct
OKOLKALLMNGGHWA-NWEE0000%500331100 OKLMNGW-W30050310
smsoo sssww wwno CR
C`oCovnesstecRse.p Coasts
(OKOLKMLNIGNHGWHN0H00550331100Dup OKLWNGWWSOGSIIDLowSpkasiph
w wo aae Sooo 470
=uos
Congas? OKMNGWWSCORIIOHGN SMe SOs S00 U0 6
CCoonoescadacoesssppkk `Conse
OKRMLGAHWGBW0N2B5S0331100 OKLNGW-WB0050310
smmoo sssow so des
we =
`cCooovnss0i8cReep Cobuild
OKLUOONKKOLWINWNGECHOHCANHEBNITITOI0LG3o1Gw01S0w0ipeSpp
Sm F0a0 mS80
or 11
COOGMT OKLMN.GW-WEOGSONO Hoh Spke 50> 50000 300 79
cCoomnssaeesrrzassppkc Consasiz
OOKRLMING-GNH-ZW2B5-00005500331100 SUINGHANZE0020310
xsmoo usswm m0 mm
6@5 v
CCooonsaeutztRaep Congeatd
OKUOKNL-MGNGWHAW2Z5-000.5005301301005. OKLWNGWNVZSOOBIOLmSpleSep
020 5X0
Tseke S210
.. 104
Cmeits ORMNGNWIEORIMOKghSpkeSpe S00 0 58
coCosneaesatssSppkx cConosetastcetroep
OKOLRMNU-GGHW-WASE300.0088013100 O OKLNRIOWO -WE0NGE0O 310
sswoe dwoes9 Fw a m sEtS
oCoospue4a1t7e Ciits
OOKKMONDKOLNWAWG.SGHIW.O-WOWEW3IIGOO0L80oEw3S1S0HpSok00kepeHS.SpOGpP:d
5s 00 t270 50000 42500
255 85
cCoCvoeosmsozasosapeL Kk OOKRKLLEMMIMNNCGGHH.--4#1222000655-000.040555600333111000
0 mo mao0m ws wo am =
CoCvosnae4ezs0zRyep CObHZ2
CKOKLOLVKMNLGGMHNWNVAGZNH0Z5WS-20O005O35R.00M351O003SL1Dao0kpwe Sppb
ww2% S000 6240
5==
COOSHZS OKLNNGW-WZISOISIOHONSpkeSop S000 OOD 78
c`oCnosoasasdzzssSopkh `coneaszs
OO`KROLLRNNI.A-GNGW.-.O2WW12N51Z5.I.S00000G55506G33311H000 ONGI.WZ160050310
ssoo wmwme wo won
xti2em
soa a
coCoosoeseuzctzRsep CCooeoadcizzts
OOLKM(NNONGKGWIWWNWZNZIGISHSOOT2JH1SM5C0OS0NO5GL0No3S1wp0SkpDelpeOspspp
52X0 SOD
34000
53 71
ee ree r
Iohre v.ryigihPFmOaAlrvye hesuhnediodusnamdpl1e ,arecosvweriyhV"ePsFOAreVcaey GHEY
Exygen Research CSIP
Page 36 of 110 000053
--------------
InterimRepert #1-Analysis ofOskisle Water Samples
Exygen Study No: PODO1400
Table IV.
Surrogate
Spike
Recovery of
Continued
C
PFOA
in
Water
Samples
ExDon
DeSsacmrippltieon
ee Spiked RTeCc.oPvTFeOrsA Recovery gl) gl) 0)
CCO0064442288S5p 0 Cooseiza
OKLLMUNN.SGWHWIZ2D001.00.0005500331100 OLMN.CWW20100.080510
mm00 ssmo woms wae w
CaCtos0usc4asn2r0en COOSA
OKLOUKNLOUGKNWLGWHUZWNIZG00IOWD02.0R01S.00.005L.0o035w1003SD1a0bpa Spr
wmoo S000
4as r0 w50
COUBA31 OKLMN.GWWZDTO00SIHNiDnSpb Sogp> 50000 30200 60
CCoo0oso4aasss2 5SppkF Coosasss
OOOLKKmLUNMONNWG..GWPH.N-WPT7?-.-000.0.05085000333111000
wI w w asoo os
coCoosnes4isazzsRep COBH
OKNGCWKKPLLUWNIIGNOWOG.GPHWITPN-O?0L005o00w53S013p01iD0apSped
2wsam S00 4620
oas os
COOBMTS OKLMNGW-PWTOOSGSIOHGh SpRe Shop S000 300 56
coCoOs0BuAiTsTs CO0B4438
OOKKLLUMNONGK-WLG-NWT-R-GITUPR-IPTOIROOI0OP0S110S0.O0HL5oo0hw3SS1pp0kheo SSopppbb.
S2000 60000
Gs0o0 51300
o10z5
cCovasesassz Sike4 Coosassz
OKRLUNIGNWO-PWH-BP.E00005500331100 ORLMNGW-PHEDGSIH0
wsoo smwne wwes wa &
c`oCoasoeaaisszsRsep CoOBU4s
OK(OOLKLLUN.NNGWG.GPHHY-BP--W0PB.-0W50L00B3o51On00S1OOp0kpSeSIp0ro
w wo wa2 && S00 W070
COBH OKLMNGW-PWSOOKSIONGhSphoSOs S000 200 2
CaCnoCo0osinansgidaasssopkt) OOLOrLUINnNOGWWWPoPHHeSE0D000o55e00c33a11r00d
m0o owoe wr wo 5
conCosoissttssir op COMMS
OKLUOONKKGLLHNUN-NGP.HGW-HOP-NLPGOH-TS0.O00L500o53w04S501pD0kipaSpd
m wa a S00 40
&a
COOB4MD OKLUINGH-PHBHONOSSkOeSOIppOo 50000 20 50
Ccoovosanasso sSpKk `Coossizh
OOOKRULLIIANNG.-O6WS1N10100222.:000.0.0505500030541100D
wsow ssao ow0s ae &
Cc`oC0oBnaasasdosren CON
OKOLLUNLNGVSNWWGWEWWBSIIGO02100202500L00o300w1580SD1p00ipk3eS10o
m 2 dewo 5000 080
@50 101
COOnMssa --_--_--
OKLMNGW-WSI0Z00SI0Hgh SpSOom0 50000
2600
68
Naotme:h Sincea isnstu huri s mdanbmn.shaave reunydedresus,recovery vloesmay varysigh
Exygen Research
eugene
Page 370110
000060
--_
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No.: PO001400
Table IV. Surrogate Spike Recovery of C PFOA in Water Samples Continued
"CPEOA
Evifo SE
Dseanign
ooratas Racosd RacGo8wry
cCoCoeonentuessatisssppsutn conmiash op
fOremGaHmNEmmIDe0e05ns10 HWE)
fmwooo oww ww mWdew wo owom
CDTouoRrtiEs SoOIrnuSAwmNaosCIwmBSAmOODoENElLSo1o0uSDMseupemSoCops 002000 SdwHmO owa8
ScooClaoimsusaissssixcs comics ep
OLoOALmRCIaWNnENMEEGDEET1L0000.150550003331100 Simonwarvro0s03D
F mw o Rwwm wom om
CDfososolusescoO miOAM iROiWWN mEINmGI SeouOiSaMDtS s0ciSy WO EMo1 mSCY
fcoooaoitcsbi?oeSrnodc coast Bop
SoSiwimmaoonnnwowwaea0soa0500s55e020s00000 Shinonwzo00000
asw oo mwamw oToam wom ow
CCSoiveosiudtssss OKoOwIMDOMWONNNIOWOCRNOGAIDIIOXHSOL0ghw9SN0pe0e sHso SGma0nom28y0
ou 83
cSoonoemveieaerrsrsssxch covert Top
oSOiainnGownEwzaEos20005es0s300098 LinO25 0.050000
awGooo wawme mom wm o
CCfoommciinctse roeqaOrRorANNeWGERs0 OtIaRXnNt0eSt S1 E Wm O BCwm8TT
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Page 380f 110
000061
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Interim Report #1-AnaolfyOsskdialse Water Samples.
[Exygen Study No.: P0001400
Table IV. ' Surrogate Spike Recovery of C PFOA in Water Samples
Continued
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Page 390f 110
000062
InterimReport#1-AnaoflOaykdsasle Wate Samples ExygenStudy No.PO0DI00
TableIV. Surrogate Spike Recovery of 'C PFOA in Water Samples
Continued
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Page 400f 110
000068=
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InterimReport#1-AnalysisofOskdale Water Samples
Fxygen Study No PODO1400
Table IV. Surrogate Spike Recovery of *C PFOA in Water Samples
Continued
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Page 4207110
000065
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Titer Rep#1-oAnarlystisofOakdale Water Samples
Exygen Stidy No. PO00I400
Figure 1. Typical Calibration Curve for PFOA in Reagent Water
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Page 4307110
000066
-- imi------ Interim Reprt#1-AnalysisofOskdle Water Samples Exysen Stady No: POUOIAD0
Figure 2. Extracted Standards of PFOA in Reagent Water, 25 ng/L
and 50 ng/L, Respectively
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Page dof 110
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Figare3. PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively
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Figured. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOA, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)
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Figure5. Typical Calibration Curve for C PFOA in Reagent Water
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Page 47of110
000079
termReport#1-Analysi ofOakdale Water Samples
Exygen Study Nos: PO0O1400
Figure 6.
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Extracted Standards of C PFOA in Reagent Water, 25
ng/L and 50 ng/L, Respectively
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Page 48of 110
000071
nein Report #1-AnslyisofOkla Wate Samples ExygenStyNo: POOLOD
Figure 7. C PFOA in Reagent Water, 50 ng/L. Fortified Reagent
Water, and 500 ng/L Fortified Reagent Water, Respectively
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Figure8. Chromatogram Representing an Oakdale Water Sample Analyzed for C PFOA (Exygen ID: C0064522, Data Set: 032405C)
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Page $0010
000073
Interim Report#1-AnalysisofOskdale Water Samples
`Exygen Study No. PODO1400
Figure9. Typical Calibration Curve for PBS in Reagent Water
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PageSTof 110
000074
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trim Report #1-Analyss of Oakdale Water Samples Exygen Sudy No: PO00L400 Figure 10. Extracted Standards of PFBS in Reagent Water, 25 ng/L,
and 50 ng/L, Respectively
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Page 520110 000075
trim Report #1-AnalysisofOakes Supe Exygen Study No: POOOL00
Wim om ms a Figure 11. PFBS in Reagent Water, 50 ng/L Fortified Reagent Water,
and 500 ng/L Fortified Reagent Water, Respectively
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Page 530f 110
000076
InterimReport #1-Analyss ofOskdsle Water Samples
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Figure 12. Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)
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InterimRept#1-AnalysisofOskdsleWatce Samples
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Figure 13. Typical Calibration Curve for PFHS in Reagent Water
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Page SSof 110,
000078
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Interiea Report #1-AnalysisofOakdale Weter Samples
Exygen Study No. PO0D1400
Figure 14. Extracted Standardsof PFHS in Reagent Water, 25 ng/L.
and 50 ng/L, Respectively
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Page 56 of 110
000079
----------------------------------------------------------------------
Toteri Report#1-Ansys ofOskdale Weter Samples
Exygen Study No: PU00L00
Figure 15. PHS in Reagent Water, 50 ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, Respectively
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Page 5701110
000080
Interim Report#1-AnalysisofOakdale Water Samples
Exygen Study No. PO001400
Figure 16. Chromatogram Representing an Oakdale Water Sample Analyzed for PFHS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)
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Page S80 110
000081
Inicrim Report #1-AnaysisofOse Water Samples Exon Study No: PO001400 `Figure 17. Typical Calibration Curve for PFOS in Reagent Water
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Page S90110
000082"
Interim Report #1-Analysisof Oakdale Water Samples
`Exygen Study No.: P0001400
Figure 18. Extracted Standards of PFOS in Reagent Water, 25 ng/L and 50 ng/L, Respectively
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Page 00f110
000083
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Figure 19. PFOS in Reagent Water, 50 ng/L Fortified Reagent Water,
and 500 ng/L Fortified Reagent Water, Respectively
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Page 6206110 000085
Intec Report #1-AnsolfOyaksdialse Water Samples ExygenSudy No: POOI4O0
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"
Exygen Rescarch
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Page 6306110
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