Document 5DQYd2dR8mNQQnk49J572Vere
RESEARCH .Precise Research.
Provai Results.
/ 2 -2 6 - / W J
RECEIVED
O PPI P -r
05APR 25 AH ih 11
_______________________
AZf7?7
Analytical Report
3M Company
A nalysis o f PFOA and PFOS In W ater Sam ples from O akdale M unicipality
E05-0243
\ Exygen Report No. L0004933
Testing Laboratory \ Exygen Research
3058 Research Drive State College, PA 16801
Requester Gary A Hohenstein Manager, Environmental Operations
E H S O perations 3M Company
Building 42-2E-27 St. Paul, MN 55106
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^ ^ 3 0 5 8 Research Drive State Colleeggee, PA 16801, USA
% TT:: 800288113219 m FF;; 614.272.1019 exygen.com
1 Introduction
Results are reported for the analysis of perfhjorooctanoate (PFOA) and perfluorooctaneeulfonate (PFOS) in water samples received at Exygen as requested by Gary Hohenetein of 3M Company. The Exygen project number assigned to the samples Is LQ004933. Table I lists the target analytes quantitated for the samples.
Table I. Target Analytes for Quantitation
Parameter
Acronym
Formula
Perfluorooctanoate
PFOA or C8 add
C7P16COO'
PerfluoraoctanesuWonate
PFOS or C8 sulfonate
CbFitSOs
2 Sample Receipt
Twenty-one samples were received at Exygen In 500 mL white plastic narrow-mouth bottles. At the request of 3M, an samples wore analyzed. A copy of all sample log-in information is presented In Attachment A.
The samples were reoetved on 03/30/05. The samples were shipped ambient via UPS. The samples were stored refrigerated from time of receipt untl analysis.
3 Methods - Analytical and Preparatory
The Exygen method V0001780 was used to prepare and analyze the samples. A summary of the sample preparation can be found in Section 3.1 and a summary of the analysis concRtions can be found in Section 3.2.
3.1 W ater Sam ple Preparation
Solid phase extraction (SPE) was used to prepare the water samples for LG/MS/MS analysis. Forty milliliters of the water sample was transferred to a C18SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. A portion of the extract was transferred to autosampler vials aid analyzed using electrospray LG/MS/MS.
PAQE2QF5
3 2 Sam ple Analysis by LC/MS/MS
in High Pressure Liquid Chromatography (HPLC), an eiquot of extract Is Injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in ihe column relative to the liquid moble phase, the analyte Is retained for a characteristic amount of time. Following HPLC separation, mass spectrometry provides a rapid and accurate means for analyzing a Wide range of organic compounds. Molecules are ionized, fragmented, and detected. The ions characteristic of the compounds are observed and quantitated against extracted standards.
An HP1100 system Interfaced to an Applied Biosystems API 4000 was used to analyze the sample extracts fa quantitation.
Isomer separation was obtained using a gradient elution through a Thermo Ruophase RP, 50 x 2.1 mm x 5pm column. The sum of the Isomers Is reported as a single value fa each of the analytes.
The following gradient was performed:
Moble Phase (A): Mobfle Phase (8):
l0a1111k...018o00n...000
2mM Ammonium Acetate In Water Methanol
622866555555 733733555555
The following parameters were used for operation of the mess spectrometer
Parameter Ionization Mode Polarity Transitions Monitored
Gas Temperature Drying Gas (N2)
Setting Bectroepray Negative 413->369 PFOA), 499->80 (PFOS), 415->370 (13C-PFOA, surrogate spike)
350C 7.0 L/mln
4 Analysis
4.1 C alibration A 7-point calibration curve was analyzed Initlafy and throughout the analytical sequence for PFOA, PFOS and WC PFOA. The calibration points were prepared at 0,25,60,100,250,500, and 1000 ng/L (ppt) for LC/MS/MS analysis. Calibration standards are prepared using the same SPE procedure used fa samples. The instrument response versus the concentration was plotted fa each point. Using linear regression with 1/x weighting, the slope, y-lntercept
PAGE3 OF5
7
and coefficient of determination (r2) were determined. A calibration curve is acceptable if r2 > 0.985. For the results reported here, calibration criteria were m et The calibration curves are Included in the raw data in Attachment C.
4 2 Surrogates
,3C PFOA (C6Fl5[13qF2I13CpOH) Is used as a surrogate tor the water samples. nC PFOA
was added to the empty sample containers before the bottles were sent to the field tor sampling. In the field, all sample and quality control battles were filled to a volumetric fill line with the sample. ,3C PFOA recoveries can be found In Attachment B. 4.3 Laboratory C ontrol Spikes
PFOA, PFOA, PFOSLaboratory control spikes in the analytical set were prepared by adding a known concentration
of ,aC and to laboratory reagents. Laboratory control spikes are used to assess method accuracy. The laboratory control spikes must show recoveries between 70130% or the data is rejected. For the results reported here, the laboratory control spikes were within the acceptable range.
4.4 Field M atrix Spikes One matrix spike was prepared tor every water sample in the field. Compounds were added to the empty sample containers before the bottles were sent to the field for sampling. Matrix spikes are used to assess method accuracy In the matrix. The matrix spikes should show recoveries between 70-130%. For the results reported here, the matrix spikes were within the acceptable range.
4.5 Sam ple R elated Com m ents ARwater samples were collected in duplicate, Duplicate sample results are reported along with the sample results In Attachment B.
5 Data Summary
Please see Attachment B far a detailed listing of the analytical results. The results are reported In parts per billion (ng/ml) for PFOAand PFOS.
2 5PAQE40F5
6 Statem ent o f A ccuracy
Based on results of laboratory control spikes, field matrix spikes, and surrogate spikes, the analytical accuracy for PFOS and PFOA results for all samples is 30%. Ail laboratory control spikes, surrogate spikes and field matrix spikes showed recoveries within these ranges. Specific sample recoveries are given in Attachment B.
7 Data/Sample Retention
Samples will be returned to 3M 60 days after final reporting. M electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. Hardcopy data Is stored for a minimum of five years. The client will be notified 30 days prior to the disposal of hardcopy data.
8 Attachments
8.1 Attachment A: Analytical Results 8.2 AttachmentB: Spike Recovery Data 8.3 Attachment C: Chain of Custody Forms 8.4 Attachment D: Raw Analytical Data
9 Signatures
M f h o f fbhn M. Flaherty, Vlo^Presidenl
Data
PAGE3 OF3
Section A
1
. Provn Resute.
Exygen ID
L4933-1 L4933-2 L4933-4 L4933-5 L4933-7 L4933-8 L4933-10 L4933-11 L4933-13 L4933-14 L4933-16 L4933-17 L4933-19
Sum m ary o f PFO A and PFOS in W ater Sam ples EG5-0243
Sample ID
O-WS-127287 . O-WS-127287 Dup \ O-W1-208462
O-W1-208462 Dup -W 2-208463
O-W2-208463 Dup 0-W 8-572608
O-W8-572608 Dup 0-W9-.151575
O-W9-151&75 Dup O-W3-208464
O-W3-208454 Dup Field Blank.
Analyte Found (ng/mL)
C8 A dd PFOA
C8 Sulfonate PFOS
Perftuofooctanoste
PwfluarooetaMsulFonate
0.779
1.14
0.710
0.941
0.0887
0.0619
0.0939
0.0609
0.0823
NQ
0.0817
NQ
0.503
0.704
0.457
0.561
0.813
0.580
0.763
0.502
ND ND
ND ND
ND ND
NO = Not detected at or above 0.025 ng/mL. NQ Not quantifiable = Measured concentrated between 0.025 ng/mL and the lim it of
Quantitation (LOQ) which is 0.050 ng/m L \
3/0 6
J ^ 3 0 5 8 Research Drive ^ VkState Collie, FA 16B01, USA
% TJ: 814.272.1039 I F F: : 814.2231.1580 exygen.com
Section B
32-
Field M atrix Spike Recovery Summary for PFOA and PFOS In W ater E05-0243
Sample Description 0-W5-127287 Spike (L4S33-3,1 ppb.Sptke)
0-W1-208482 pike (US33-S, 0.1 ppb Spike)
0-W2*208463 Spike (L4S33-B, 0.1 ppb Sptke]
O-W8-572608 Spike (L4933-12, 03 ppb Spike)
0-WSM51575 Spike (L4833.15,1ppb Spike)
O-W3-208454 Spike (L4933-10, 0.1 ppb Spike)
Field Blank Low Spike <L4ro40.0.1 ppb Spike)
Field Blank High Spike (L4e33*1,1ppb Space)
CS Acid PFOA_______________ Cg Sulfonate PFOS
Amount Amt Found Amount
Amt Found Amount
Spiked In Sample Recovered Recovery In Sample Recovered Recovery
(ng/mL) (ng/mL) (ng/mL) (%)
(ng/mL) - to g s V ) ____ <*>.
1
0.779
1.74
96
1.140
2.11
97
0.1 0.0887 0.174
85
0.0619
0.134
72
0.1
0.0823
0.178
96
0.0296
0.124
94
0.5 \1
0.503 0.813
1.05 109 0.704 1.80 108 0.580
1.26 111 1.53 95
0:1
ND
0.106
106
ND
0.111
111
0.1 ' ND
0.0987
99
ND
0.0983
98
1
ND
0.953
95
ND
0.839
84
`Sample residue exceeds the spiking level significantly; therefore, ah accurate reoovery value cannot be calculated ND * Not detected at or above 0.026 ng/mL NQ = Not quantifiable = Measured concentration between 0.025 ng/mL and the Limit of
Quantitation (LOQ) which is 0.060 ng/mL.
. . i /! <> L< t> !
33
3058 Research Drive State College, PA 16801, USA
x T: 8002813219
F: 014.272.1019 etygen.com
Surrogate Spike Recovery Summary for n C-PFOA in W ater EO5-0243
Exygen ID
Sample D e s c rip tio n
Amount Spiked (ng/m L)
C-PFOA
Amount Recovered
[ng/m L)
Recovery (%)
L4933-1 \ L4933-2 \ 14933-3
O-WS-127287 0-W 5-127287 Dup 0-W 5-127287 1.0 ppb Spk
0.5 0.430 0.5 0.411 1.0 1.03
86 82 103
L4933-4 L4933-5 L4933-6
O-W 1-208462 O-W1-208482 Dup -W 1-208462 0.1 ppb Spk
0.5 0.460 0.5 0.494 0.1 0.0966
92 99 97
L4933-7 L433-8 L4933-9
\ O-W2-208463 O-W2-208463 Dup
O-W2?208463 0.1 ppb Spk
0.5 0.436 0.5 0.422 0.1 0.0991
87 84 99
L4933-10 L4933-11 L4933-12
dW 8-572608 O-W0r572608 Dup O-W8-572608 0.5 ppb Spk
0.5 0.424 0.5 0.416 0.5 0.476
85 83 95
L4933-13 L4933-14 L4933-15
0-W9-151575 0-W9-15175 Dup 0-W 9-151575 1.Q ppb Spk
0.5 0.460 0.5 0.394 1.0 1.02
92 79 102
L4833-16 W933-17 L4933-1B
O-W3-208454 O-W3-208464 Dp O-W3-208454 0.1 ppb' Spk
0.5 0.450 0,5 0.437 0.1 0.104
90 87 104
L4933-19 L4933-20 L4933-21
Field Blank
Field Blank 0.1 ppb Spk \ Field Blank 1.0 ppb Spk \
0.5 0.489
0.1 0.0991 1.0 0.964
98 99 96
34
J L 3 O5 8 Research Drive ^ ^ S ta te Cbilege, PA 16801, USA
^ T : 000.28t.3219 m F r 614272.1019 exygen.com
Section C
35
3068 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1680
Loain
Login Group: L0004933
Login#: P ro je c t
Company Name: Submitted By:
5043 P0000990
3M Kent Lindstrom
C o n fo rm O C S a m p le :
Conform COC: Conform Sample: Conform Request:
T rue
True True True
Login Type: Started: Date Start Due Date:
immediate Receipt of Samples True 03/30/2005 04/09/2005
Received Date: 03/30/2005
Received By: Ammerman, Mark
Spread Sample:
Label: Exygen SD/PI: Risha, Karen Project Title/Type: Analysis of Fluorochemicals by LCMSMS for NRG Sampling of Oakdafe Site / ROUTINE Login Notes:
Conform Notes:
Rachat Carton PKOOQSm
Package / Containers
P 4 tt./ g M tillU n Received Data: 3/30/2005 12:00:00AM Package & Contents Uncompiomiaed
fltlB B H 'U P
UPS 1Z57955E0141403528
T te tip ^ n n p fflfttn g t
None 23.2
D irection/H andled Bv
RECEIVED Ammerman, Mark
Container # C0066673 CQ088674 C0066675 C0066676 C0Q8S677 00055875 C0066679 C0066680 C0066881 C00B6682 C0066683 C0068684 C0066685 C0066686
O m uM /M aht .
g P d e in g rT yp q
278.20 g
500 ml Clear Pteetic
Narrow
288,30 g
600 rn Clear Plastic Narrow
257.30 g
500 ml Clear Plaattc Narrow
266.00 g
800 ml Clear Plastic Narrow
248,50 g
500 ml Clear Plastic Narrow
252.00 g
500 ml Clear Plastic Narrow
243.10 g
500 ml Clear Plastic Narrow
248.10 g
500 ml Clear Plastic Narrow
245.90 g
500 ml Clear Plastic Narrow
254.80Q
500 mt Clear PlaeUc Narrow
243.70 g
500 ml Clear Plastic Narrow
247.00 g
500 ml Clear Plastic Narrow
240.90 g
500 ml Clear Plastic Narrow
251.20 g
500 ml Clear Plastic Narrow
P re se rva tive NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE
Miti IO
3/30/2005 Login,rpt
Report Version: Mar 2 2005 10.50AM Page 1 of 4
Instance:
R0166202 n iR n im n iii
Loqin
Login Group: L0004933
Login#: Project:
5043 P0000990
Conform COC Sample: True
Conform COC:
True
Company Name: 3M
Conform Sample:
True
Submitted By: Kent Lindstrom
Conform Request
True
Login Type:
immediate Receipt of Samples
Started:
True
Date Start
03/30/2005
Due Date:
04/00/2005
Received Date: 03/30/2005
Received By: Ammerman, Mark
Spread Sample:
Label:
Exygen SD/PI: Rlsha, Karen
Project Title/Type: Analysis of Fiuorochemicals by LCMSMS for NRG Sampling of Oakdale Site / ROUTINE
Login Notes:
Conform Notes:
Eastern Carton
PK00Q5818
Package / Contain!-
P lie /C o n d itio n
Received Date: 3/30/2006 12:00QAM Package & Contents Uncompromleed
SNPtttf/ IS
UPS 1Z575501414D3528
Temp. ControWTemo.
None 23.2
C ontainer# C0066887 C0066688 C0O66689 CO066690 C0066691 C0096692 C0066693
Grow W eight f it i
243.70 g
C ontainer Tvoe
500 ml d e a r Plastic Narrow
267.80 g
500 ml Clear Plastic Narrow
243-50 g
500 ml Clear Plastic Narrow
232.60 g
600 ml Clear Plastic Narrow
255.30 g
500 ml Clear Plastic Narrow
237.20 g
500 ml Clear Plastic Narrow
257-60 g
500 ml Clear Plastic Narrow
Preservative NONE NONE NONE NONE NONE NONE NONE
Mfa. Lot
Direction / Hsm ted 8v RECEIVED
Ammerman, Mark
MfaJB
3/30/2005 Logln.rpt
yb 0 Report Version: Mar 2 2005 10:50AM
Page 2 of 4
31
Instance:
R0156202 M iin u n ii
Login
Sample ID L0004933-0001 LOOO4933-O0Q2 LOOO4933-0OC3 L0004933-Q004 L0004933-0005 L0004933-0006 L0004933-0007 L0004933-0008 L0Q04933-0009 L0004933-0010 LOO04933-0011 LOO04933-0012 L0004933-0013 L0004933-0014 L0004933-0013 L0004933-0016 L0004933-0017 LOO04933-0018 L0004933-0019 L0004933-0020 L0004933-0021
Container C0066673 C0063674 C0066675 CO065676 C0066S77 C0066678 C0066679 C0065680 C0066681 C0066Q82 C0066683 CO066684 CO066685 COO66686 C0066687 C0086688 C0066689 C0066690 C0066691 C0066692 00068693
Matfto LIQUID LIQUID
liq u id
LIQUID LIQUID LIQUID LIQUID UQUID LIQUID LIQUID UQUID LIQUID UQUID UQUID UQUID UQUID UQUID LIQUID UQUID UQUID UQUID
Fraction Water
Sam ples
Sample 0-W5-127287
Water
0-W5-127287 Dup
Water
O-WS-127287 1.0 spike
Water
O-W1-208462
Water
0-W1-208462 Dup
Water
0-W1-208462 0.1 tpike
Water
O-W2-208463
Water O-W2-206483 Dup
Water O-W2-20B463 0.1 spike
Water O-WB-572608
Water
0-W8-572608 Dup
Water
O-WB-57280B 0 5 ppb spike
Water
0-W9-151575
Water
Q-W9-151575 Dup
Water 0-W9-1S1S75 1.0 ppb spike
Water
O-W3-208454
Water
O-W3-208454 Dup
Water
O-W3-208454 0.1 ppb spike
Water field Sank
Water
Field Blank 0.1 ppb apfce
Water
Field Blank 1.0 ppb splice
Dpto aptnow 03/29/2005 03/2972003 03/29/2005 03/29/2005 03/29/2005 03/26/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005 03/29/2005
a n t Cue 04/06/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2006 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/09/2005 04/06/2005 04/09/2005 04/09/2005
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3/30/2005 bogin.rpt
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instance:
R0156202
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Environmental Laboratory
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3/29/2005
Project: E05-0243
CONTRA3CMT ELNAVBIORROANTMOERNYTWALORLAKBOORRDAETROBRYYSAMPLE Contract Lab(s): EXYGEN
Page 1 o f 3
Requester: Hohenstein, Gary A (0042-02E-27) PPDDrreaooptjjeaeerRcctttmeNDceeuenismvtc:ebr5diep3:rt0:3i7o/021n081:2/O2260a70k54d4a4le9Municipal Well FCs IV
PPEChrmooomajneipelcltAeNLtduioedmanrdebD:sesorK;;teek6n:r5Ut1Lt'u7ifn7sd8trs-ot5rm3o5@m2mmm.com
Ship Date:
Comments: Pace field sampling.
3M Sample Number E0S-0243-81103 AnalribCode PFOA PFOS
Sampled Date Sample Description
3/29/2005 Analytical
Method
O-W
l-2084C6o2mponents
PFOA PFOA
PFOS by ESMS
PFOS
E05-0243-8U04 Asatoito PFOA PFOS
3/29/2005 Analytical
MethodO-W1-2084C6M2 MDHupBBrtg
PFOA PFOA
PFOSbyESMS
PFOS
E05-0243-81I05 PFOA PFOS
3/29/2005
O-Wl-2084C62om0p.1onPePnBt! Spike
PFOA PFOA
PFOS by ESMS
PFOS
E5-0243-8I106 AnalviltCqdy PFOA PFOS
3/29/2005 O-W2-208463
Analytical Method
Component!
PFOA PFOA
PFOS by ESMS
PFOS
E05-0243-8H07 AaiiYiliCts PFOA PFOS
3/29/2005 O-W2-208463 Dup
A t t i r a i Method
PFOA PFOA
PFOS by ESMS
PFOS
E05-0243-81108 Analysis Code PFOA PFOS
3/29/2005 O-W2-208463 0,1 PPB Spike
figSBgfflttttl
PFOA PFOA
PFOS by ESMS
PFOS
y O i f`
*3
4A/2n0a/b20fl0R5toiPitc 4/20/2005 A M lttfrPgjPfte 4/20/2005 4/20/200$ 4A/2M0/f2r0rt0i5P w P f ff t 4/20/2005 AnaiYiliPif-Prts 4/20/2005 4/20/2005
4/20/2005 4/20/2005
4/20/2005 4/20/2005
3/29/2005
CONTRA3CMT ELNAVBOIRROANTMOERNYTWAOLRLAKBOORRDAETROBRYYSAMPLE
Page 2 of3
Project: E05-0243 (coat.)
Contract Lab(s): EXYGEN
3M Sample Number Sampled Date Sample Description
E05-0243-81109 AoahaliCode PFOA PFOS
3/29/2005 O-W3-208454
Analytical Method
Component
PFOA PFOA
PFOS by ESMS
PFOS
Amlvtis Due Date 4/20/2005 4/20/2005
E5-0243-81110 Analvab-Code PFOA PFOS
3/29/2005 O-W3-208454 Dup
Analytical Method
- fpnpoaea|
PFOA PFOA
PFOS by ESMS
PFOS
4A/a2r0t/2y0i0i5iPwPita 4/20/2005
E05-0243-81 t i l PFOA PFOS
3/29/2005 O-W3-208454 <U PPB Spike
Camwiwno
PFOA PFOA
PFOS byESMS
PFOS
4/20/2005 Pau 4/20/2005
E05-0243-81112 PAFnOiAlrtia M i PFOS
3/29/2005 0-W5-127287
Component
PFOA PFOA
PFOS by ESMS
PFOS
AnalvfU Doc Date 4/20/2005 4/20/2005
E05-0243-8I113 Analysis Code PFOA PFOS
3/29/2005 0-W5-127287 Dup
Analytical Method
CgmpQnsflfr
PFOA PFOA
PFOS by ESMS
PFOS
Aaalval! Due Data 4/20/2005 4/20/2005
E05-0243-&1114 Analysis Code PFOA PFOS
3/29/2005 0-W3-127287 1.0 PPB Spike .
PFOA CPFffOmAiMflrt*
PFOS by ESMS
PFOS
4A/2w0d/y2i0ie05 Pate 4/20/2005
E05-0243-81118 APFftO8lYAfte.Co4fi PFOS
3/29/2005 O-W8-572608
Analytical Method
PFOA PFOA
PFOS by ESMS
PFOS
AMlYlbPKDltP 4/20/2005 4/20/2005
E05-0243-81119 PFOA PFOS
3/29/2005
iO-W8-5726C08omDnuopaenti
PFOA PFOA
PFOS by ESMS
PFOS
Analysis Due Date 4/20/2005 . 4/20/2005
E05-0243-81120 AnilYd? Code PFOA PFOS
3/29/2005 O-W8-572608 0.5 PPB Spike
AmlYttoal. Mrtlrcill
CttBiBtfimrta
PFOA PFOA
PFOS byESMS
PFOS
Annlviis DueDate 4/20/2005 4/20/2005
D 0i7
3/29/2005
CONTRA3CMT ELNAVBOIRROANTMOERNYTWALORLKABOORRDAETROBRYYSAMPLE
Page 3 of 3
Project; E05-0243 (cont.)
3M Sample Number
E05-0243-S1121 Anilyib Code PFOA PFOS
Sampled Date Sample Deicription
3/29/2005 0-W9451575
Analytical Method
Component!
PFOA PFOA
PFOS byESMS
PFOS
E05-0243-81L22 Analvifa Code PFOA PFOS
3/29/2005 Aaalytiyal
M
rtM
0-W9-1515C75omDpuonnent!
PFOA PFOA
PFOS byESMS
PFOS
Contract Lab(s): EXYGEN _______________
ABMlYltl Put Pate 4/20/2005 4/20/2005
Aflitob Due Date 4/20/2005 4/20/2005
E05-0243-81123 ApMyjIi PFOA PFOS
3/29/2005 Analytical
MethedO-WP-1515C7o5m1p.0onPePnBt!
Spike
PFOA PFOA
PFOS byESMS
PFOS
Anafriia Due Date 4/20/2005 4/20/2005
E05-0243-81127 Anatole Cod PFOA PFOS
3/29/2005 Field Blank
Analytical Method
gOTMBftrtl
PFOA PFOA
PFOS byESMS
PFOS
4A/2m0M/20?05P ie Pate 4/20/2005
E05-0243-8112S Analyst Code PFOA PFOS
3/29/2005 Field Blank 0.1 PPB Spike
Aaslyttori
Component
PFOA PFOA
PFOS byESMS
PFOS
4A/20|y/2i0r0ii5p f P a a 4/20/2005
E05-0243-81129 APFnOafArikCtttfi PFOS
3/29/2005 Field Blank 1.0 PPB Spike
Analytical M fW PFOA
PCFoOmAiwnffltt
PFOS byESMS
PFOS
Anatok Due Pate 4/20/2005 4/20/2005
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>HIF TO: JOHN FLARHERTY/SRMRLE CHECK-1N (814) 231*6832 EXYGEN RESEARCH 117 RESEARCH DR
TATE COLLEGE PA 16801-2752
PA 1888-10
420168012752
UPS NEXT OAY AIR
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RESEARCH Precise Research.
Proven Results.
RECEIVED
r.pPT C"'C 05APR 26 AH IIvll
j% r ? 7 F_____________________
Analytical Report
3M Company
A nalysis o f PFO A and PFO S In W ater Sam ples from H astings M u n icip ality
E O S -0186
Exygen Report No. L0Q04709
Testing Laboratory Exygen Research
3058 Research Drive State College, PA 16801
Requester Gary A. Hohenstein Manager, Environmental Operations
EHS Operations 3M Company
B u ild in g 4 2 -2 E -2 7 St. Paul, MN 55106
2005HAY-3 PH 2*51*
PAGE 10 F 5
3 ^ 3 0 5 8 Researdti Drive m ^L S ta ie Cofege PA 16801, USA
T: 800.28811.3219 m `FF:: 814.272.1019
exygen.com
1 Introduction
Results are reported for the analysis of perfiuorooctanoate fPFOA) and perfluorooctanesulfonate (PFOS) In water samples received at Exygen as requested by Gary Hohensteh of 3M Company,
The Exygen project number assigned to the samples is L0004709. Table I lists the target analytes quantitated for the samples.
Table I. Target Analytes for Quantitation
P aram eter
Acronym
Formula
Perfluorooctenoate Perfluorooctanesulfonate
PFOA or C8 acid PFOS or C8 sulfonate
CyFuCOO'
C5F 17S 0 1
2 Sample Receipt
Four samples were received at Exygen in 500 mL white plastic narrow-mouth bottles. At the request of 3M, all samples were analyzed. A copy of a l sample log-in Information is presented in Attachment A.
The samples were received on 03/01/05. The samples were shipped ambient via UPS. The samples were stored refrigerated from time of receipt until analysis.
3 Methods - Analytical and Preparatory
The Exygen method entitled, "Method o f Analysis for the Determination o f Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonyfamkte (PFOSA), and Perfiuorooctanoate (POAA) in Water/' modified for isomer separation, was used to prepare and analyze the samples. A summary of foe sample preparation can be found in Section 3.1 and foe modified analysis conditions for isomer separation can be found in Section 3.2.
3.1 W ater Sam ple Preparation
Solid phase extraction (SPE) was used to prepare the water samples for LC/MS/MS analysis. Forty milliliters of the water sample was transferred to a C18 SPE cartridge. The cartridge was washed with 5 mL of a 40% methanol: 60% water wash. The cartridge was eluted with 5 mL of 100% methanol. A portion of the extract was transferred to autosampler vials and analyzed using electrosprey LC/MS/MS.
PAGE 2 OF5
3.2 Sam ple Analysis by LC/MS/MS
In High Pressure Liquid Chromatography (HPLC), an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid moble phase, the analyte Is retained for a characteristic amount of time. Following HPLC separation, mass spectrometry provides a rapid and accurate means for analyzing a wide range of organic compounds. Molecules are ionized, fragmented, and detected. The ions characteristic of the compounds are observed and quantitated against extracted standards.
An HP1100 system interfaced to an Applied Biosystems API 4000 was used to analyze the sample extracts for quantitation.
Isomer separation was obtained using a gradient elution through a Thermo Fiuophase RP, 50 x 2.1 mm x 5pm column. The sum of the isomers is reported as a single value for each of the analytes.
The following gradient was performed:
Mobile Phase (A): Mobile Phase (B):
Time 0.0 1.0 8.0 10,0 11.0 18.0
2mM Ammonium Acetate in Water Methanol
M 2fc 65 35 65 35 25 75 25 75 65 35 65 35
The following parameters were used for operation of the mass spectrometer:
Parameter Ionization Mode Polarity Transitions Monitored
Gas Temperature Drying Gas <N2)
Setting Electrospray Negative 413->369 (PFOA), 499->80 (PFOS). 415->370 (13C-PFOA, surrogate spike) 350flC 7.0 L/min
4 Analysis
4.1 C alibration
A 7-polnt calibration curve was analyzed initially and throughout the analytical sequence for PFOA, PFOS and ,3C PFOA. The calibration points were prepared at 0,25.50,100,250,500, and 1000 ng/L (ppt) for LC/MS/MS analysis. Calbration standards are prepared using the same SPE procedure used for samples. The Instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, /-intercept
PAGE 3 OF5
and coefficient of determination (r2) were determined. A calibration curve is acceptable if r2 > 0.985. For the results reported here, calibration criteria were m et The calibration curves are Included in the raw data in Attachment C.
4.2 Surrogates 13C PFOA (CqF15[,3C)F2[1!C]OOH) is used as a surrogate for the water samples. 1SC PFOA was added to the empty sample containers before the bottles were sent to the field for sampling. In the field, all sample and quality control battles were filled to & volumetric fll line with the sample. 13C PFOA recoveries can be found in Attachment B,
4.3 Laboratory C ontrol Spikes Laboratory control spikes in the analytical set were prepared by addng a known concentration of PFOA, 13C PFOA, and PFOS to laboratory reagents. Laboratory control spikes are used to assess method accuracy. The laboratory control spfces must show recoveries between 70* 130% or the data is rejected. For the results reported here, the laboratory control spikes were within the acceptable range.
4 .4 Field M atrix Spikes A low and a high matrix spike were prepared with toe sample and sample duplicate in toe field. Compounds were added to the empty sample containers before the bottles were sent to the field for sampling. Matrix spikes are used to assess method accuracy in the matrix. The matrix spikes should show recoveries between 70*130%. For the results reported here, the matrix spikes were within the acceptable range.
4 .5 S a m p le R e la te d C o m m en ts The water samples were collected in duplicate, Duplicate sample results are reported in Attachment B.
5 Data Summary
Please see Attachment B for a detailed listing of toe analytical results. The results are reported in parts per bilion (ng/ml) for PFOA and PFOS .
PAGE4 OF 5
6 Statement of Accuracy
Based on results of laboratory control spikes, field matrix spikes, and surrogate spices, the analytical accuracy for PFOS and PFOA results is 30%. Laboratory control spices, surrogate spikes, and field matrix spikes showed recoveries within this range. Specific sample recoveries are given in Attachment B.
7 Data/Sample Retention
Samples w ii be returned to 3M 60 days after final reporting. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. Hardcopy data is stored for a minimum of five years. The client will be notified 30 days prior to the disposal of hardcopy data.
8 Attachments
7.1 Attachment A: Analytical Results 72 Attachment B: Spike Recovery Data 72 Attachment C; Chain of Custody Forms 7.4 Attachment D: Raw Analytical Data
PAGE 5 OF 5
51
SECTION A
1 __AnaMU al ^
Rejxirt 1
Sum m ary o f PFO A and PFOS in W ater Sam ples E 05-0186
L4709-1 L47Q9-2
H -W 6-207M 3 H-W6-207643 Pup
Analyte Found (ng/mL)
CS Acid PFOA
C8 Sulfonate PFOS
Perfluorooctanoat*
PerfkioroocUnMiilfonat
ND NO ND ND
ND = Not detected at or above 0.025 ng/mL NQ * Not quantifiable * Measured concentration between 0.025 ng/mL end the Umit of
Quantitation (LOQ) which is 0.050 ng/mL.
0006
53
^ ^ 3 0 5 8 Researrcdh Drive J v s ta te CoKege * 16801, USA
^ L Jt:: 8114422772X1089
S F F;; 814.231.1580
exigen,tum
SECTION B
Ewgen RESEARCH
Precise Research. Proven Results.
Figld M atrix Spike Recovery Sum m ary fo r PFOA and PFOS In W ater E05-0186
S am ple,
Description
H-W(1461-4260*73B,04.13pLpobSwptSk*p)ike
H-W(6U-2uCe746,4i 3ppHbigsphoSrt)pike
Amount Spiked (ng/m L)
CB Add PFOA_____________ C6 Sutfonate PFOS
Amt Found Amount
Amt Found Amount
In Semple Recovered Recovery fn Sample Recovered Recovery
(ng/mL) In a im i)
(% )
(ng/m L) (ng/m L)
f%)
0.1
ND
0.128
128
ND
0.117
117
1 ND
1.04 104
ND
1.03 103
ND = Not detected at or above 0.029 ng/mL NO " Not quantifiable Measured concentration between 0.025 ng/mL and fte Limit of
Quantitation (LOQ) which to 0.050 ng/mL \
55
J ^ 3 0 S d Research Drive J f ^SStatie Collegei, PA 16801, USA
^ T T:: 8000..2288113219 m FFrr 814.27,2.1019 exygen.com
n
RESEARCH Precise Research.
Proven Results.
Surrogate Spike Recovery Summary for u C-PFOA in W ater E05-0186
Exygon ID
Sample D e scrip tio n
L4709-1 L4709-2 L4709-3L4709-4 ,
H-W6-207643 H-W6-207643 Dup H-W6-207643 Low Spk H-W6-207643 High Spk
Amount Spiked (ng/m L)
1C-PFOA
Amount Recovered
(n g/m L)
Recovery (*)
0.5 0.491 0.5 0.522 0.5 0.546 0.5 0.540
98 104 109 108
0007
56
J ^ 3 0 5 S Researchh Drive State College, PA 16801, USA
^ T T:: 800..228811.3219
I fF: 814.272.1019 exygen.com
SECTION C
Fw pn
3068 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
I Loqin
L o g in G ro u p : L 0 0 0 4 7 0 9
Login#; Project:
Company Name: Submitted By: Login Type;
4819 P0001275
3M KENT LINDSTROM Immediate Receipt of Samples
Conform COC Sample; Conform COC: Conform Sample: Conform Request:
Started;
True
Date Start;
03/01/2005
Due Date:
03/11/2005
Received Date: 03/01/2005
Received By:
Ammerman, Mark
Spread Sample:
Label:
Exygen SD/P1: Ristia* Karen
Project Title/Type: Cottage Grove Residential Water Sampling / ROUTINE
Login Notes:
Conform Notes:
True
Tnje True True
|
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$
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Packed PK0005WO
Carton
P acka g e ? / C o n ta in e rs
Dato / Condition
Login Date: 3/1/2005 11;31;4AM Packeis* & Contents Unoompromised
UPS 126795560142913994
Tsfim. Cootrol/TumD.
None 22.3
Direction f Handled Bv
RECEIVED Ammerman, Mark
Container#
C0063087 C0063088
PKOOOSsei
container.#
C0063089 C0063090
Gross Wekitit dH Container T v
253.90 g
500 ml Clear Plastic Narrow
258.00 g
500 ml Clear Plastic Narrow
Login Date: 3/1/2005 11:34:30AM Package & Contents Uncompromised
Grots Weight dd Oontalntt.Tvpe
292.90 g
500 ml Clear Plastic
Narrow
244.40 g
500 ml Clear Plastic Narrow
P re se rva tive NONE
NONE
UPS 1Z57955E0140675806
Preservative
NONE
NONE
Mffl, ,,Lot
Nona 22.3
Mfa, -Lot
Mfa. ID
ill:
RECEIVED Ammerman, Mark
Mfa. ID
Samal* ID L004709-0001
L0004709-0002
L0004709-0003
LQ004709-004
Container C0063067 CO063089 C0063068 C0063090
Matrix LIQUID
LIQUID
LIQUID
LIQUID
Fraction Water
Samples
Sample HW6-2D7643
Water
HW8-207643 Dup
Water
HW6-20743 Low Spice
Water
HW6-207643 Hlgti Spike
0008
3/1/2005 Report Version; Feb 22 2005 0:53AM
Login,rpt
Page 1 o f2
52
Puts.SampledPale.kwgetiIn
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02/28/2005 02/28/2005 02/28/2005
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2/28/2005 Project: E05-0186
CONTRA3CMT ELNAVBOIRROANTMOERNYTWAOLRLAKBOORRDAETROBRYYSAMPLE Contract Lab(s): EXYGEN
Page I of I
Requester: Hohenstein, Gary A (0042-Q2E-27) DDPPrraeootpejjeeaRccrtttemDNceeeuinsmvcterb5diep3:rt0:2i7o/021n051:2/H2260a70st45i4n4g9s Municipal Well PC's 11
Completion Date: PPEhrmooajneilecAtNLduedmardebs:esrK:: ek6nr5lti1nL-d7ins7td8rso-t5mr3o@5m2mmm.com
Comments: Pace field sampling.
Note: Reference trip blank on E05-0184. BGJ 2/28/05
05-0186 samples traveled withE05-0184 samples. AC, PLf, 2/28/2005.
3M Sample Number Sampled Date Sample Description
E05-0186-79868 Ana^ia Code PFA PFOS
2/28/2005 H-W6-207643
i CffmBapcaft
PFOA PFOA
PFOSbyESMS
PFOS
E05-0186-79869 Analysis Code PFOA PFOS
2/28/2005 Analytical
Method1H-W6-2076C4f3tmDouoonciits
PFOA PFOA
PFOSbyESMS
PFOS
3A/m15lY/2g6i0i 5P it Pute 3/15/2005 Anilvijj put Date 3/15/2005 3/15/2005
oon
C/
