Document RjOpNv34MY6mO6OD758ZY7JDv
tsi enters ------------Grpaee{emesis
226-36AR4R8AE _ 364-2
INT]
AT #1
le Water Sam)
STUDY TITLE
AnalysisofPerfluorooctanoic 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
DRAETAQUIREMENTS
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 19, 2005
PERFORMING LABORATORY
`Exygen Research
3058 Research Drive State College, PA 16801
Phone: 814-272-1039
STU3DMYCosmppoannsyor
3M Building 0236-01-B-10
PShto.nPea:ul6,31M-N7353-56134744
PROJECT Protocol Number: P0001400 Exygen Study Number: P0001400
"Total Pages: 110
FABRA
000024
inRptArorSa ages ayn Sy No:PRIA
`GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT
Exygen Study Number P0001400, entitled "Analysis of Perfluorooctanoic Acid (PFOA),
Perfluorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), and
Perfluorooctanesulfonate
LC/MS/MS for the 3M
(PFOS)
Cottage
in Water
Grove
,
M
Soil,
onito
r
Sediment, Fish,
ing Program,"
and Clams Us
conducted for
ing
3M
Company, is being performed in compliance with EPA TSCA Good Laboratory Practice
`Standards 40 CFR 792by Exygen Research.
Z27 hn Flaherty Principal Investigator Exygen Research
JaisimhaKesari P.E., DEE Study Director `Weston Solutions, Inc.
To ad
Sooo Repti Robert A. Paschke
3M Company
. ExygenRescarch
Fasting
his : Date
lilos
Date.
Page 207110
000025
InterimReport#1-Acalysisof OakdaleWaterSamples SURANCE '
ExygenStudy No.PO0O1400 NT
Exygen Research'sQualityAssurance Unit reviewed Exygen Study Number P0001400,
ePnetriitlluedo,ro"hAenxaelnycssiuslfoofnaPetref(luPoHrSoo)c,taanncidcPAecrifldu(orPoFoOcAt)an,ePseulrffolnuactreob(utPaFneOs)ulifnonWaatte(ePrF,BSSoi)l,,
SPerdoimgeanmt.,"FisAhl,l arnedvCielwaemdspUhsaisensg' LwCe/rMeSi/nMsSpefctoerd tfhoer 3cMonCdoutcttagacecGorrdoivneg MtooniEtxoyrginegn
Research'sStandardOperatingProcedures,theStudyProtocol, andallapplicable Good
Laboratory Practice Standards. All findings were reported
InvestigatorandManagementand totheStudy Director.
fo
the
Exygen
Principal
Date ReportedtoDateReported to
onse
IDuapetceted Plroivnecsiipganlor MEanxayggeemne.nt DSattuedyReDpiorretsetdorto
1. ProtocolReview
03/24/05 0325/05
03/29/05
05/19/05
2 ExmctioaReview 032405 032505 032905 [A
3. 2R0adwInDtaertiamReview
Asalytical Report
Review
snes
osnsns
0519s
05119005
Ie om
Te
Lead, Quali surance Unit
But5e/13/05
r"eNpootret:atAlhleincsopneccltuisoinosnwoifltl ebestduodcy.umentedinthe QA statement for the finalanalytical
SAAN
Exygen Research
Page30f110
000026
oer Rep#1 oAnarlystisoflal Wate Samples Exygen Sty No: P0001400
CERTIFICATION OF AUTHENTICITY
"This interim report, for Exygen Study Number P0001400, is a true and complete representation ofthe raw data.
Submitted by:
Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-1039
Principal Investigator, Exygen:
A
ViewFPlraehseirdteynt
Exygen Research
Safes
Date
Exygen Research Facility Management:
Atd) ,
Richard A.
PBrxeysgiedennt Rseach
1-18-05
Date.
`Study Directgr, Weston Solutions, Inc.
Jaisimha fr P.E, DEE `Weston Solutions, Inc.
Sponsor Representative, 3M Company:
Zax We RobertA. Paschke Manager, 3M Corporate Environmental Programs
[-- wu
Dad
ales
Date
Page 4110 000027
Interim Report #1-AnalysisofOakdale Water Sarapes
Exygen Study No.: PO0O1400
STUDY IDENTIFI [O!
PerflAunoarloyhseixsoafnePseurlfflounoartoeoc(tPaHnSo)ic,AacniddP(erPfFlOuAo)r,ooPcetrafnleusoarlofbountaatnee(sPulFfOoSn)atien (WPaFtBeSr),,Soil, `Sediment, Fish, and Clams Using LC/MS/MS for the 3M Cottage Grove Monitoring
Program
PROTOCOL NUMBER:
P0001400
EXYGEN STUDY NUMBER: ~~ PO001400
TYPE OF STUDY:
Residue
SAMPLE MATRIX:
Water
TEST SUBSTANCE:
Perfluorooctancic acid (PFOA), Perfluorobutanesulfonate (PBS), Perfluorohexanesulfonate (PFS), and Perfluorooctanesulfonate (PFOS)
SPONSOR:
33MM BCuoimlpdianngy0236-01-B-10 St Paul, MN 55144
STUDY DIRECTOR:
Jaisimha Kesari P.E., DEE Weston Solutions, Inc. 1400 Weston Way `West Chester, PA 19380
`SPONSOR REPRESENTATIVE: Robert A. Paschke 3M Company 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
Interim Analytical Sart Date: 03/21/05
Interim Analytical Termination Date: 04/21/05
Interim Report Completion Date: 05/19/05
A, Exygen Research
Page Sof 110 000028
Interim Report #1-AnalysisofOakdale Water Samples.
Exygen Study No.: PO001400.
PR
PERSONNEL
`The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc. The following personnel from Exygen Research were associated with various phasesofthis 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
-
Page6of 110
000029
InterimReport#1-AnalyssofOaks Water Sles ExygenStudy No: POOO1400
TAOFB COL NTEE NTS Page
GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT ......ocvvvvvrrsnrnn2 QUALITY ASSURANCE STATEMENT .....coourvrsmimmisemssmssssssssssssmsssmssssssssssssssssnsd
CERTIFICATION OF AUTHENTICITY coovvvvevsionsssnesssnssssmssssssssssssssssssssssssssssnni
4.0 ANALYTT ESI TSAC MPLA ES.L .........
rrceseemmssersrssssssmrss isomer 13
6.0 DESCRIPTION OF ANALYTICAL METHOD.....ccooumummmmmsrsmsmssmssrsssssssssess 1S.
6.2. PreparationofStandaradnsd FOrtification SOIONS........evevesrererrrrs16
6.5. Description of LC/MS/MS InstrumentandOperating Conditions........................17
7.0 EXPERIMENTAL DESIGN ccs cesses 6.6.Quantitationand Example Caloulation...............usssmsssmsssssssssmssssssrsns 1189
9.0 CONCLUSIONS...
20
10.0 RETENTION OF DA ANDST AMPLA ES .......cocccommsmmmmmsmsssmsssssssrssrsssrsssnons2Q
ExpoenReseach
an
Paogf1e10
000030
Interim Report #1-AnalyssofOakdale Water Samples
Exygen Study No: PO001400
LIST OF TABLES
Page Tablel. Summaryof PFBS, PFHS, PFOS and PFOA in Water
TableIl.
Table II. Table IV.
Matrix Spike Recovery of PFBSand PFHS in Water Samples...................24.
Matrix Spike RecoveryofPFOS and PFOA in Water Samples.............30 Surrogate Spike Recoveryof 'C PFOA in Water Samples... 36
Fxygen Research.
|
Page 8of 110
000031
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InterimReport#1-Analysisof OakdaleWaterSamples
ExSty udy Ng o.: PeOOInA00
Figure 1. Figure 2. Figure 3. Figure 4.
Figure S.
Figure 6.
Figure 7. Figure 8. Figure 9. Figure 10.
LIST OF FIGURES
Ty
pical
Calibration
C
urv
e
fo
r
PFinO ReagAent
Wa
Page
ter....vcceneid3
J Extracted Standards ofPFOA in ReagE ent Water, 25 ng/L and 50 ng/L, 7
PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and. 500 ng/L Fortified Reageat Water, RESPECHYElY... wove 8S
Chromatogram Representing an Oakdale Water Semple Analyzed for PFOA, DF=100 (Exygen ID: C0064522, Data Set: 03405CR) ccs
Typical CalibrationCurvefor 'C PFOA in Reagent Water ..................47
E0xtr5ac0tNeGdLS,taRndEaSrPdsEoCfHV'ECLPYF-OcvAoirnrRoeangs ent Wato er, 25 n ng/L. ra8 "'C PFOA in Reagent Water, 50 ng/L Fortified Reagent Water, and 500ng/LFortified Reagent Watef, RESDECHVeY.....r..... oor d9 Chromatogram Representing an Oakdale Water Sample:
Analyzedfor "C PFOA (Exygen ID: C0064522, Data Set: 032405C).........50
Typical CalibrationCurve for PFBS in Reagent Watef.........cvcvsnS1
Extracted StandardsofPFBSin ReagentWater, 25ng/Land 50ng/L,
Figure 11. Figure 12.
Figure 13. Figure 14. Figure 15. Figure 16.
PFBS in Reagent Water, 50ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, RESPECHVELY.......covrrrcrens53 Chromatogram Representing an Oakdale Water Sample Analyzed for PBS, DF=100 (Exygen ID: C0064522, Data Set: OTHERSccumrmssmmmmmsmmmmmengrmmmm--_t Typical Calibration Curvefor PFHS in Reagent Water .....ovverunnn55 Extracted Standards of PFHS in Reagent Water, 25 ng/L and 50 ng/L, REO sciommsmmmmmimamrmmsmsemapmnn 36 PFHS in Reagent Water, 50ng/L Fortified Reagent Water, and 500 ng/L Fortified Reagent Water, RESPECHVElY.....rnvovsvrsnen ST Chromatogram Representing an Oakdale Water Sample Analyzed for PFHS, DF=100 (Exygen ID: C0064522, Data Set:
Figure 17. Typical Calibration Curve for PFOS in Reagent Water .......ococcvue 59
tan
i
Exygen Research
Page 9.0f110
000032
------------------------------------------------r--------
lori Report #1.Aslysiof Onkle Water Samples Eye SNoa:200y 01400
LIST OF FIGURES Continued
Figure 18. Extracted Standardsof PFOSin Reagent Water, 25ng/Land 50 ng/L,
Figure 19.
PROS in
500 ng/L
FRoeratgiefnitedWRaetearg,en5t0 Wnagt/eLr,FoRrtEiSfiDeEd CRteaigveentlyWa.tne.r,onanrd.rmsmersc
SL
Figure 20. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOS, DF=100 (Exygen ID: C0064522, Data Set:
Trg nt Cr
Page 1000110 000033
_--_--
InterimReport #1-AnofaOalkdyalseWi atser Samples.
[ExygenStudy No.: 0001400
LIST OF APPENDICES
Appendix A
Study Protocol P0001400 (Exygen Study No. P0001400) with Analytical Method: V0001780:"MethodofAnalysis for the Determination of Perfluorooctanoic Acid (PFOA) in Water by
Page
ExygenResearch
ENE
Pa 11g of1e 10
000034
Interim Report #1-AnalysisofOakdale Water Sarrples
Exygen Study No: PO0OI400
1.0 SUMMARY Exygen Research extracted and analyzed water samples for the determination of perfluorooctanoic acid (PFOA), perfluorobutencsulfonate~~(PFBS), perfluorohexanesulfonate (PEK), and perfluorooctanesulfonate (PFOS) according to Exygen Method V0001780 (Appendix A). `The limitof quantitation for PFOA, PFBS, PFHS and PFOS in water was 50 ng/L and the limitof detection for PFOA, PFBS, PFHS and PFOS in water was 25 ng/L. Analytical resultsfortheanalysis of PFOA, PFBS, PFHS and PFOS inwatersamplesarc `summarizedin Table 1. The overall average percent recoverics standard deviations for all fortifications of PFOA, PBS, PFHS and PFOS in water samples were 93% + 19, 141% 21, 96% + 15 and 109% = 32, respectively.Theoverallaveragepercentrecovery
+ 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 (PBS),
perfluorohexanesulfonate (PFHS), and _perfluorooctanesulfonate (PFOS) in water
according to Protocol 0001400 (Appendix A).
3.0 INTRODUCTION
a"TnhdisPrFepOoSrtidnetwaaitlesrtuhseinregsutlhtesoafnatlhyetiacnaallmyseitshfoodr etnhteitdleetde,r"mVi0na0t0i1o7n8o0f:PMFeOtAh,odPoFfBASn,aPlyFsHiSs for the Determination of Perfluorooctanoic Acid (PFOA) in Water by LC/MS/MS." TuhmebestrudPyO0w1a4s00in.itiTatheed aonnalyMtaircaclhst0a3r,t d2a0t0e5,forwhtheins itnhteersitmardeypodritrewcatosrMsairgcnehd2p1r,o2t0o0c5o,l and the analytical termination date for this interim report was April 21, 2005.
ExygenResearch
tnd
Page 120f 110
000035
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Interim Report#1.AnalysisofOskcale Water Samples
Exygen Study No. PO001400
4.0 ANALYTICALTEST SAMPLES
One sites,
hundred and (Bxygen ID
twenty-one water samples, which correspond CO064404-C0064438, CO064442-CO064461,
to twenty-nine sample CO064467-00064532)
were received Solutions, Inc.
at
ambient temperature The samples were
on March logged in
15, by
2005 from Tim Frinak Exygen personnel and
at Weston placed in
refrigerated storage.
aSsasmopcliaeteldogw-iitnh athnids icnhtaeirnimorfepcoruts.toSdtyoriangfeorrmeacotridosnwiisllboecakteepdtiant EtxheygreanwRedsaetaarcpha.ckage
5.0 REFERENCE MATERIAL
The analytical standard, PFOA, was purchased from Sigma Aldrich and was received at
Exygen on December 08, 2003. The surrogate spiking standard, "C labeled
p3eMrflCuoomrpoaocntya.noiTchaeciadna(lytCicPalFOstAa)n,dawrdass, rPeFcBeiSveadnadtPEFxHySg,enweorne Aspurpiplli1e5d, b2y0034M.froPmFtBhSe was received fom 3M at Exygen on July, 06, 2000. PFHS was received from 3M at Exygen on January 20, 2003. PFOS was purchased fiom Fluka Corporation and was receaitEvxyegedn on April 23, 2003. `The available information for the reference materials is listed below. PFOA was stored raemfbriiegnetra.ted.PFBS, PFHS and C PFOA were stored frozen and. PFOS was stored
CoPmFpOoAund CPPBFSOA PFHS PFOS
ExvgSePnl0n0v0e3n8t0o0tyNo.=2BLUotG#HB Pur9i7t.y6(4%) Expi1r2a/t0i8o/n05Date
SPO004184 3507-195 97
03/29/09
SP0000252
10
9.7 12/0406
$P0002401 SP0002694
SEIS 986 40801 1012
10/18/06 04/23/06
`fTohlelomwoilnegcuplagaerss:tructures of PFOA, *C PFOA, PFBS, PFHS and PFOS are given on the
Exygen Research
aT
Page 130110
000036
Interim Report#1-Analysis ofOakWadtear Salmplees
Exygen Study No.: PO0O1400
PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight: 414
Transitions Monitored:
413 -- 369 (for quantification) and
413 > 219 (for confirmation)
Structure:
Por F F. F F
F F Prt F et F
OH
BC PFOA Chemical Name: 1,2-13C perfluorooctanoic acid
Molecular Weight: 416
`Transition Monitored: 415 -- 370
Structure:
WN E
0
oc" Now
feet]F
PCFheBmSis! Name: Perfuorobutaneslfonie
MolecularWeight: 338 supplied as the potassium salt (C/FsSOyK")
TSrtaansciatrioens Monitored: 299 --> 99
Tt F F
F
F
.
F
503
FOF
Exygen Research
:
nr
Page 14of 110
000037
--
Interim Report #1-AnalysisofOakdale Water Samples
ExygenStudy No. PO0O1400
PFHS Chemical Name: Perfluorohexanesulfonate: Molecular Weight: 438 supplied as the potassium salt (CeF1nSO5K') Transitions Monitored: 399 -- 80 Structure:
FEEFQE]LF F _
F
505
FlFrOFle
PFOS Chemical Name: Perfluorooctanesulfonate Molecular Weight: 538 supplied as the potassium salt (CyF1;SO5K") Transitions Monitored: 499 -> 80 Structure:
- EFFIFFE] F 505 FlFOeFlelFeF
6.0 DESCRIPTION OF ANALYTICAL METHOD
PTehrefluaonraloyotcitcaanloimceAtchiodd(P"FVO0A0)01i7n8W0a:teMrebtyhoLdC/oMfS/AMnaSl"yswiass
for the used for
Determination this study.
of
6.1. Extraction Procedure
A 40 mL aliquotofthe water sample was used for the extraction procedure. After
fortification conditioned
of appropriate samples, the samples with 10 mL of methanol and 5 mL
were loaded onto a Cis SPE cartridge of water. The eluate was discarded.
Aelpupartoexwiamsatceollylefcitveedmiinltloilaitgerrsaodfuamteedth1a5nomlLwapsolaydpdroepdytloentehececnatrtrriifduggee. tuFbie.ve Emialclhilistaemrsploef
was analyzed by LC/MS/MS electrospray.
Exygen Research
harddizin
Page 15 of110
000038
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Interim Report #1-AnalysisofOakdale Water Sarpies
Exygen Study No: PO0D1400
62 Preparationof Standards and Fortification Solutions
pInrdeipvairdeudalasstsopcekcisftiaenddianrdExsoylguetinonmsetohfoPdFVOOA0,O17C80P.FOTAh,e sPtFoBcSk,stPaFnHdaSrdansdoluPtFioOnSs wweerree 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, 1.0 pg/mL fortification standard solutions were prepared by taking 1 mL of the a`pmpLroofprtihaetaepsptroocpkraiantdeb1.0rpg/imLt.nhefovgrotilfuiicmaetniuonpgsttoand1a0r0d manLdwbirtihngmientghathneovlo.luBmyetuapkitnog10100 `mLwith methanol, 0.1 pg/mL fortification standards were prepered. 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. Several sets of standards containing PFOA, C PFOA, PFBS, PFHS and PFOS were prepared in water and processed through the extraction procedure, identical to samples. The following concentrations were prepared:
Conc. of Fort Font Volumeof
Solution Volume Fortified Sample
(ng/mL)" (BL)
(ml)
0
0
Fo
10
100
"0
10
200
4
10
400
Py
100 100
"0
100 200
Pp
! of1PF0O0A, 'C PFO4A0,0PFBS, PFHS a4n0d PFOS
Final Conc. of Calibration Std.
(g/L)
0 25 50 100 250 500 1000
Aprnepaedrdeidtiaotna1l0m0i0xpegd/smtLockansdolduitliuotnedoftoPF1O00A,andC10PFpOgA/,mLPFfBoSr,boPttFlHeSs,piaknidngPpFuOrpSosweass. Complete detcaanbieflousndintherawdata package associated with this 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 this interim report.
Exygen Research,
wb
Page 160 110
000039
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Taterim Report#1AnalysisofOakdale Water Samples
Exygen Study No. PO001400
63 Chromatography
Quantification of PFOA, PFBS, PFHS and PFOS was accomplished by LC/MS/MS
meliencst,ro~s1p1raym.insT,haendre~te1n3timoinnst,imreesopefctPiFvOelAy,.
PFBS, Peaks
PFHS above
and PFOS was ~12 min, ~5 the LOD were not detected in
anyof thereagent blank samples corresponding to the analyte retention time.
6.4 Instrument Seasitiviy The smallest standard amount injected during the chromatographic run had a concentrationof25 ng/L ofPFOA, PFBS, PFHS and PFOS.
6.5 Description of LC/MS/MS Instrument and Operating Conditions Instrument: API4000 BiomolecularMessAnalyzer Interface: Turbo fon Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 Software: Windows NT, Analyst 1.4.1 HPLC: HewletPackard (HP) Series 1100 HHPP QVuaactuPuummDpegasser HP Autosampler HP Column Oven HPLC Colum: Thermo Fluophase RP, 50 mm x 2.1 mm Column Temp.: 30C MInojbeicltieonPhVaosl.e:(1A)5:pL2 mM Ammonium Acetate in water Mobile Phase (B): Methanol
Time(min 00
6%5A
%35B
10
65
3s
80
25
7s
100 25
7
110
6
3s
Tortuntaimle; ~11880min 65
35
Flow Rate: 0.3 mLimin
oF
Exygen Research
50000
Page 170f 110 000040
--
.
Interim Rep#1-oAnarlystisofOakdale Water Samples
Exygen Study No: POD01400
Ions monitored: Analyte PFOA
PFOAConfirnlon 13CPFOA PFBS PFHS PFOS
Mode negative negative negative negative negative negative
Approximate,
Transifion ~~RetentionTime
M4on1i3to3r6ed9 ~1(2mmiin)n.
413219 ~12min.
415370 ~12 min.
29999
5 min.
39980
~11 min.
49980
~13 min.
6.6 Quantitation and Example Calculation
`FTihfetpeeenakmaicrreoalwitaesrsmoefassuarmpeldeanodrtchaelsitbraantdiaonrdsctuarndvaerdwawsegreeneirnajtecetded(uisnitnog1thxe LiCtw/eMiSg/hMtSe.d
linear regression) concentration was
dbeyterAmnianleydstfrsoomfttwhaereequuastiinognssbiexlocwo.ncentrations
of
standards.
The
Estqaunadtairodnc1urcvaelc(uJlianteeadr trehgeraemssoiuonntpoafraanmaeltyertse)fgoeunnedra(tinedngb/yL,thbeaAsneadloysntpseoafktwaarreea)upsroignrgatmh.e
Analyte found (ng/L) =(Peak aresal-oipneterceptx) DF Where: DF =Dilution Factor, factorbywhich the fina! volume was diluted, ifnecessary.
pFroirorsatompelxetrsacftoritoinf,ieEdquwaittihoknn2owwansaumsoeudnttoscoaflcPuFlaOtAe,thPeFpBeSr,cePntFHrSec,ovPeFryO.S and 'C PFOA
`REecqouvaetriyo2(n:4) = {analytefound(nagm/oLu)n-taanadldyetde(inngc/oLn)trol(ng/L) x100%
An example ofa calculation using an actual sample and results from the PFOA analysis
follows: `Water
sample
Exygen
ID
0064432
Spk
F
(Set:
03210SBR),
fortified
at
50000
ng/L
with PFOA where: peak area
= noel
intercept slope.
= 200 - B30
dilution factor ng/L PFOA added (fort level)
a) = 50000
(+The primaarymtsianmpcloerrreessuplotnwdiansgussaemdpfloer(anllg/cLa)l*culat=ions) 37600
ExygenResearch
len
Page 180f110
000041
_--_--mmm
InterimReport #1-Analysisof Onkeale WaterSamples
ExygenStudy No.P0001400
From equation 1: Analyte found (ng/L) = [1170161 = 26200] x 100 1330
From equation 2: % Recovery
= s6012ngL* = (36012037g60/0Lng./L--) x 100%
50000 ng/L
= 97% (+values are slightly differeat from raw data due to rounding)
7.0 EXPERIMENTALDESIGN
s'aCmpPleFOcoAllewcatsionusboetdtlaess
a
in
surrogate for all the
the laboratory before
samples. 'C
being shipped
PFOA
to the
was
field
added to the
for sampling.
aFodrdesdamaptlaeskndeoswingncaotnecdenatsrafitcilodnmtaotrtihxesbpoitktelse,s PinFBtSh,e lPaFbHoSra,toPrFyObSefoarned bPeFinOgAswheiprpeeadlstoo -
the field. The samples were filled to a 200 mL volumetric ill line in the field.
`The samples were extracted in five scts. Each set consisted ofone reagent blank and two
reagent blanksfortifiedat known concentrations. The fist set contained six sample sites,
the second set contained six samples sites, along with a trip blank and two trip 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, 2 sample,a field duplicate and two-matixfieldspikes were collected. For each site,
a laboratory duplicate of the primary sample was extracted and two laboratory matrix
tshpeikpersiwmearrye salasmopleextrcaocltleedc.teFdofrotrhtehetwsiotelawbaosraptooruyremdatfrrioxmsptihkeesb,otttwleo a4n0dmfLortpifoiretd.ionsNootf
only were PFBS, PFHS, PFOS and PFOA addedinthe laboratorypriorto extraction, but
PalFsBoS, CPFPHFSO,APwFaOsSadadnedd.PFTOheA
additional C PFOA was
spiked. into the samples
added because
were known t
o
the levels of
excesd the
`cwaelriebraadtjiuosnterdantgoerseqaunidrewtehreesanomte adnilaultyizoendaswitthheooutthedrilauntailoynt;est.herefore, 'C PFOA levels
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 range of 70-130%. Because laboratory control spikes for "C PFOA
PweFrOeAacrceecpotvaebrlye
in
per
every set,
the seven
instrument washes were
done for the sample was
free of "'C
acceptable
PFOA,
and no
at least
evident
ane C
errors in
rsepciokvienrgieosroeuxttsriadcetoifng70c-o1ul3d0%bearefoduened,mendoinrdei-ceaxttirvaecotfiomnastrwiexreeffpeecrtfso.rmed. C PFOA
Exygen Research
Adyprmng
Page 190 110
000042
----
InterimReport #1-AnalysisofOakWadtearSalmplees
ExygenStudy No:PO001400
8.0 RESULTS
Analytical results for the analysis of PFOA, PFS, PFHS, and PFOS inwater samples are summarized in Table I.
Fortification recoveries detailed in Tables Il
for and
PFOA, PFBS, PFHS and PFOS in IL The overall average percent
the water recoveries
samples are + standard
d9e3vi%at+io1n9s, f1or41al%l for2t1i,fi9ca6ti%ons o1f5PaFnOdA1,0P9F%BS+,3P2,FrHeSspeacntdivPelFyO.SFionriwfaitceartsiaonmprleceosvweerirees
for 'C PFOA in the water samples are 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 "PTFheOwAataecrcosradmipnlgetsowaenraleytsiuccaclesmseftuhlloydeVx0tr0a0c1t7e8d0a.ndTahnearleyzweedrefonroPFciBrSc,umPsFtHanSc,esPtOhaSt maanyd _ have affected the data qualityor integrity.
10.0 RETENTION OF DATAAND SAMPLES wAillllobriegisnhailpppaepdetrodtahtea sgpeonnesroart.edTbhyisExdoyegsennoRtesienacrlucdhethfaactiplietryt-asipnescitfoicthriaswindtaetraimsurcehporats ithnestirnutmeernitmoarnatleymtpiecarlatruerpeorltogesn.d Ealxlacortigcionpailesfoacfialltly-rsapewcdiaftiac,raaswwdealtla,awsialsbiegnreedtcaoipneydoifn 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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Page200f 110
000043
p i ---------- ies-- tee-- ter-- epee--e
InterimReport#1-AnalysisofOakdale Water Samples
Exygen Study No.: P0001400
ExygenResearch
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Page20 of110 000044
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Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No.: P0001400
Table]. Summary of PFBS, PFHS, PFOS and PFOA in Water
E me m Gmcemss ser,
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Interim Report#1-AnalysisofOakdaleWaterSamples
`ExygenStudyNo.:P0001400
Tablel. Summary of PFBS, PFHS, PFOS and PFOA in Water
sore Cosiphn Sampcleus CtonstincuendetraSmipsros cusses
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HAG
Pa23gof1e10
000046
---- e -- e
Interim Report #1-AnalysisofOakdale Water Samples.
`Exygen Study No.: 0001400
Table Il. Matrix Spike ReScaomveprlyesof PFBS and PFHS in Water
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Page 24o0f01100 047
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InterimReport#1-AnalysisofOakdale Water Samples
`Exygen Study No.: PO001400
Table IL.
Matrix Spike Recovery of PFBS and PFHS in Water
Samples Continued
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Exygen Research ae18
Page 2501110 000048
Interim Report #1-Analysisof Oskdale Water Samples
Exygen Study No.: P0001400
Table II.
Matrix Spike Recovery of PFBS and PFHS in Water
Samples Continued
see
me reer 35 THR EL
siemens (0 00 00 DWT
comen|t| ve am ve mm] 0 ww
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Page 2606110
000049
----
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No.: P0001400
Table Il.
-_
Matrix Spike Recovery of PFBS and PFHS in Water
Samples Continued
PBOEEl pe var 5l 8 SE ee
meee TIT per i] ow SAID, |] we pn Stn | | ow wn
IlZ|Don ol
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Page 2706110
000050
Inter Report #1.Analysisof Oakdale Water Samples [p----
Table ll.
Matrix Spike Recovery of PFBS and PFHS in Water
SamplesContinued
A
B a E BEE
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Jerri od I
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mmmssmtiriemt || cng (| or
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Page 280110
000051:
--------------------a-- tim-- e -- ees-- eee---- ---- --
InterimReport#1-Anslyss ofOakdale WaterSamples
ExStyudyNgo.Pe001n0)
Table IL. Matrix Spike Recovery of PFBS and PFHS in Water Samples Continued
emp
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mmm
te
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wwe wm fem) ow
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Page 290f 110
000052
--------------ee-- r e-- eri-- e
Interim Report #1-Analysis of Oakdale Water Samples
`ExygenStudyNo.: PO001400
Table III. Matrix Spike Recovery of PFOS and PFOA in Water
Samples
i. B a E reLwierlEiyEa
SEINE, Lum] vn wn mio] = wm
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Page 300f 110
000053
--------------------------------------ttnteoremeeeeesemeo--e--sa--rns
Interim Report#1-Analysis ofOelcale Water Saaples
Exygen Study No. PO001400
Table IIL. Matrix Spike Recovery of PFOS and PFOA in Water SamplesContinued
see
huAnR hTIetWasmtoc+meerpret hUetsRons A"hot
Semi IDI I)ZIOIC
my [um| osm we ww wm ow HCE | 0 wer wo |ww| da wwe ow
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Page 31 0110
000054
eeirereree------------ reer Ine Report #1 AnalysisofOse Wte Saries ESrlyNy o:FO0n 01400
Table IIL. Matrix Spike Recovery of PFOS and PFOA in Water
Samples Continued
-
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ExygenResearch
Pge2or0 000055
----
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No.: PO001400
Table IIL. Matrix Spike Recovery of PFOS and PFOA in Water
Samples Continued
i
Og ge BE 15 EE
cgomempma imit nem |||) 0ODT ZpErEiE eal we wm
hwa omeantg | |woo | en wwe zwo
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Page 330f 110
000056
----------------------------------------------
Interim Report #1-AnalysisofOskdale Water Samples ExygenStudyNo.: POOOLA00
Table III. Matrix Spike Recovery of PFOS and PFOA in Water Samples Continued
i. i Sre EE eeen "TEEEE SEmemoimes ||]ImTe om eDm] T oe mme . cmommmm en|7(| TTDT TID T ITTT mn || om am em] me ne
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Exygen Research
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Page 34 of 110
000057
------------------------------------------------e--mm--a--------a
Interim Report #1-Analysis of Oakdale Water Samples
Exygen Study No.: P0001400
Table IIL. Matrix Spike Recoveryof PFOS and PFOA in Water
Samples Continued
wttEn o nny tent
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BxygenReseach
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Pa3sgar 1e10
000058
termReport#1-Analysis of OakdaleWaterSamples
ExygenStudyNo: POOO1400
Table IV. Surrogate Spike Recovery of C PFOA in Water Samples
eE-- ager----------s-- urie--------T-- Sosoa--R-- ecO o-- rd -- Re eco-- vey
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Page 360110
000059
--------
InterimReport#1-AnaolfOysskdialse Water Samples
`Exygen Study No.: PO001400
Table IV. Surrogate Spike Recovery of C PFOA in Water Samples
Continued
---------------------- SCPrO-- A --
Engen
OSenacrmipptioon
Spmipkle)d Recgotve)rsd Rec0o)very
C0o0o6s4i4s2z8n sSonkd ILLUMNGGWHW1Z0D10C0050050331100
sson ssowm 0@s
caCoosoasstaaszRneo OIRLLUUNNGGWHWWZZ0D1T0C0000S600381100
w wa ar e 5
CCooOsuMsaAo OKLUONKGLMHNW-IGIIWDWO2O01K0S0I.O05L0o3v10SDHuApS S000 4s0 ow80
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CCooonsatsa2a ssppkk E OOKKLLAANN..GOHW.-2PWW77..00..005800351100
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cCuooesaron OOKKLLUANN-.GGHW-.P2WTW-7000.50500331100
mwow ms aa
C0O0084G6M232 OMMONKGLHUANWGIH-OPOYK7S-I0O0L60o3w1S0piDuapSppd 5m00o0 4w2s0 0o6s
COOBMIS OKLMNGW-PATO0N3I0 HEN Spike 0p. 50000 33200 88
CC0OO00O6GG4HM4AS3ST8 cCouoesemszsesoSonk CCovossosanzsRep CCoonosuassss
CO0B4445.
Soovossatsuddes ssooxk CoCvosvesasseodRsep CCoOosOaBaAiHrO ooo CCooC0ooBnn4st5az0iss5o3kk KL ooosBauss0sRtep CCoo0noussz
OCKKLLMMNONGK.HLGMTWNR--IGTPWRT-POTRL0IORFOS1IS-OO0-LH0oG5wH0S3Sp1p0ieeS5p0sds O`OKRLALN.G:W.PPWWES000.50500331100 OOLLUINNGNG-WP-PSN.B00S05I05311D0
OKLOULNNGWGPHW.SPOWDBEOS0SOILSoHw0SpDhpeSp0
OKLMN-GW-PW8-0-050310HighSpike 50ppb
SOKiLUtN-oGwW--oPWwDo000c5a0c3a1i0d OLLUINN GOVN--PPWWOO000055005311DD OKLUCNHGUWMPNW-SGO-DPSWIDSI0.O0L5o0w1S0piia.bped OKLMN.GW-WOOUSOHOHGHSphe Soom OOOKKHLIUANINNNG.GHGHNNNN1GG011200.220.00000655000503111000 OKKLULNAGNHGANSNIGG120.Z0.005005301301D0p OKOLKMLNMGNWG-WWWESI2I000Z8O003S1I0OHLGohwSSapkkeaSSOedD
55S000000000 SS51010000 11000232
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Sw 00 wW078
50000 25800
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Exysen Research
Page 3701110
000060
Interim Report #1-AnalysisofOskdale Water Samples
Exygen Study No.: POOOL400
Table IV. Surrogate Spike Recovery of C PFOA in Water Samples
Continued
-- Euae n m r sumo Te Soorrecso faTecmoomuenetAd Racor
orton
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OSOLLLMIIN-N-GGGHHH--WWW8BB1110008440-00000556000535111000
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ExygenResearch
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Pa 38g of1e 10
000061
Interim Report #1-AnaolfOyaskdialse Water Samples
Exygen Study No.: PO001400
Table IV. Surrogate Spike Recovery of C PFOA in Water Samples
Continued
--E-- ngen --_--
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Page 390f 110
000062
Interim Report#1-AnaolfyOaskdialseWaterSamples
Exygen StudyNo: POOO1400
Table IV. Surrogate Spike Recovery of "C PFOA in Water Samples
Continued
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Page 4001110 000063
-------------- ER------ ------ ------ ------ -- --
InterimReport #1 AnalysisofOakdale Water Sacrpes
ExSty udyNgo. PeODO1n40D
Table IV. Surrogate Spike Recovery of 'C PFOA in Water Samples
Continued
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Interim Report #1-AnaolfOyaskdialse Water Samples.
Exygen Study No.: PO001400
Exygen Research
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Page 4207110
000065
------------
Interim Report #1-AnalysisofOakdale Water Samples
`Exygen Study No.: PO001400
Figure 1. Typical Calibration Curve for PFOA in Reagent Water
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Paged3of 110
000066
------------------------------
Interim Report #1-Analysis of Oakdale Water Samples
Exygen Study No.: 0001400
Figure2.
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Extracted Standards of PFOA in Reagent Water, 25 ng/L. and 50 ng/L, Respectively
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InterimReport #1Analysis ofOncale Water Samples
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Figure3. PFOA in Reagent Water, 50 ng/L Fortified Reagent Water,
and 500 ng/L Fortified Reagent Water, Respectively
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Note: A linear lot ofPFOA was used to calibrate the instrument. Thetwo peaks shown
in Figure 4 are due to different isomers present in environmental samples. The area
counts for all isomers present are included to report one total PFOA value.
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Interim Report #1-Analyss ofOskdale Water Samples
Exygen Study No. PO0OI00
Figured. Chromatogram Representing an Oakdale Water Sample Analyzed for PFOA, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)
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Page4601110, 000069
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InterimReport#1-AnalysisofOskdaleWaterSamples
`Exygen Study No.: P0001400
Figure5. Typical Calibration Curve for C PFOA in Reagent Water
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Page 4701110
000070
Interim Report #1-Ansyss of Ole Water Samples Exygen Study Nos: PO0OLI0O
Figure 6. Extracted Standards of 3C PFOA in Reagent Water, 25
ng/L and 50 ng/L, Respectively
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Page 48of101000071
----------------------------------------------------------------------
teri Report #1-Analyss ofOskdale Water Samples
Exygen Study No: PO0O1400
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Page 4901110
000072
----------------------
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No: POO1400
Figure 8. Chromatogram Representing an Oakdale Water Sample
Analyzed for 'C PFOA (Exygen ID: C0064522, Data Set:
032405C)
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Page 500110
000073
------------ Ine Report #1 Analysis of Ocal Water Smplos Erygen Study No: 20001400
Figure9. Typical Calibration Curve for PFBS in Reagent Water
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Page stor110
000074
Interim Report #1-Analysis ofOakdale Water Samples
Exygen Study No.: PO001400
Figure 10. Extracted Standards of PFBS in Reagent Water, 25 ng/L
and 50 ng/L, Respectively
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Page 206110
000075
--------------------------------------------------------
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study No.: PO001400
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
---------------------------------------------- Interim Report #1-Analysis of Oskale Wate Samples Exygen StyNo: POOOADD
Figure 12.
Chromatogram Representing an Oakdale Water Sample Analyzed for PFBS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)
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Figure 13. Typical Calibration Curve for PFHS in Reagent Water
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Page 5507110 000078
----------------------------------------------------
InterimReport#1-AnaolfyOaskdialse Water Samples
ExygenStudy No.: P0001400
Figure 14. Extracted Standards of PFHS in Reagent Water, 25 ng/L and 50 ng/L, Respectively
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Exygen Research
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Page 56.0 110
000079
------------
Teri Report 41-AnaloyfOsakidalse Water Samples Exygen Study No. PU0DLA0O
Figure 15.
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and 500 ng/L Fortified Reagent Water, Respectively
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Page 5701110
000080
----------------------
Interim Report#1-AnalysisofOakdale Water Samples
Exygen Study No. POODI400
Figure 16. Chromatogram Representing an Oakdale Water Sample
Analyzed for PFHS, DF=100 (Exygen ID: C0064522, Data
Set: 032405CR)
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Exygen Research
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Page 58 of 110
000081
S----------------------------------------es--te--e--m --n ner Report1s ofOnin Water Semple Boysen StyNo: POLIO
Figure 17. Typical Calibration Curve for PFOS in Reagent Water
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000082
InterimReport #1AnaloyfOsakidasle Water Samples Exyaen StudyNo:PO00L400
Figure 18. Extracted Standards of PFOS in Reagent Water, 25 ng/L and 50 ng/L, Respectively
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PageGDor 110 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 61 of 110
000084
------ er --------------
Interim Report #1-AnalysisofOakdale Water Samples
Exygen Study Noi PO001400
Figure 20. WC
Chromatogram Representing an Oakdale Water Sample Analyzed for PFOS, DF=100 (Exygen ID: C0064522, Data Set: 032405CR)
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Exygen Research
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Page 6201110
000085
---- =>..-- .J <-- <<~t ------
_--_ Interim Report #1-Anslysis of Oskdale Water Samples Exygen SucyNo.PO001400
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 Research oo
Page 6307110 000086
