Document dYyDXwZ03j2Kgd9rRExwdmwLb
Document Control Office Office of Pollution Prevention and Toxics
Page 3 8 January 2004
AR226-1883
ATTACHMENT
Analytical Report West Virginia Department o f Environmental Protection
Analysis o f Perfluorooctanoic Acid in Fish Samples Exygen Report No. L35217 (50 pages)
Proven Resulte.
Analytical Report
West Virginia Department of Environmental Protection Analysis of Perfluorooctanoic Acid in Fish Samples Exygen Report No, L35217
Testing Laboratory Exygen Research
3058 Research Drive State College, PA 16801
Requester Janice Smithson WVDEP/ DWWM 414 Summers Street Charleston, W V 25301
PAGE 1OF5
3058 Research Drive State College, PA 16801, USA
T: 800.281.3219 F: 814.272.1019 exygen.com
1 (Introduction
Results are reported for the analysis of perfluorooctanoic acid (C8 acid / PFOA) in fish samples received at Exygen from Robert Row at WVDEP/DWWM. The Exygen project number assigned to the samples is L35217. Table I lists the analyte quantitated for these samples.
Table!. Target Analytes
Parameter
Acronym
Formula
Perfluorooctanoic acid
C8 acid or PFOA
C7F15COOH
A total of four samples were received at Exygen frozen on dry ice in a cooler. Samples were
collected on 09/25/03 and were received on 09/30/03. Each sample was placed in a Hobart food
processor and homogenized with dry ice. The samples were placed in plastic bags and left open
in frozen storage overnight to allow for C 02 sublimation. The samples were sealed and placed
in frozen storage below -10C until analysis. Chain-of-custody information is presented in
Attachment A.
...
3 Me' '
lytical and Preparatory
3.1 Sam ple P reparation
Five grams of homogenized sample were weighed into 50 mL disposable polypropylene centrifuge tubes. Samples were extracted with 30 mL of acetonitrile, capped and allowed to shake on a wrist action shaker for 15 minutes. The tubes were then frozen for ~1 hour at - 1 0C. After freezing, the tubes were centrifuged at -2000 rpm for -10 minutes. The extracts were decanted onto conditioned SPE columns. The columns were packed using 2 g of florisil, 2 g of silica gel, 2 g of carbon and 1 g LC-NH2 and conditioned with 20 mL of methanol followed by 20 mL of acetonitrile. The eluate was collected in a 125 mL siianized pear-shaped flasks. Another 10 milliliters of acetonitrile were added to the samples in the centrifuge tubes. The frozen fat phases were then homogenized using a Tissumizer for -3 0 seconds. The Tissumizer was rinsed with -10 mL of acetonitrile into the tubes. The samples were again allowed to shake for 10 minutes, were then frozen for -1 hour and again centrifuged for 10 minutes. The extracts were decanted onto the same SPE columns. The eluate was collected into the same pear shaped flasks and combined with the eluate from the initial extractions. Twenty milliliters of acetonitrile were then passed through the SPE columns and combined with the eluate in the same pear shaped flasks. 3-4 drops of 1-octanol were added to the extracts in the flasks and the extracts were evaporated to dryness at reduced pressure using a rotary evaporator. Final volume was made by adding 2 mL of 2% ascorbic acid in methanol to the pear shaped flasks.
PAGE2 OF5
The samples were swirled and vortexed for ~30 seconds. The extracts were then transferred to
HPLG vials for analysis.
.
3.2 Sample Analysis by LC/MS and 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 mobile 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.
A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. A gradient elution through a Jones Chromatography-Genesis C -8,50 x 2.1 mm x 4pm column was used for separation.
The following gradient was performed:
Mobile Phase (A): Mobile Phase (B):
2mM Ammonium Acetate in Type I Water Methanol
T im e 0.0 0.4 1.0 7.0 7.5 9.0 9.5 15.0
%A %B 60 40 60 40 10 90 10 90 0 100 0 . 100 60 40 60 40
The following parameters were used for operation of the mass spectrometer:
Parameter Ionization Mode Polarity Transition Monitored Gas Temperature Drying Gas (N2)
Setting
Electrospray Negative 413->369 (C8 acid/PFOA) 300C 7.0 L/min
4 Analysis
4.1 Calibration
A 7-point calibration curve was analyzed throughout the analytical sequence for PFOA. The calibration points were prepared at 0.5, 1.0, 2.5, 5.0, 10, 25, and 50 ng/mL for PFOA. The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and coefficient of determination (r) were determined. A calibration curve is acceptable if r2 > 0.985.
PAGE3 OF5
For the results reported here, calibration criteria were met. The calibration curves are included in the raw data in Attachment C.
4.2 Surrogates
. Surrogate spikes are not a component of the LC/MS/MS analytical method.
4.3 Laboratory Control Spikes
Laboratory control spikes in the analytical set were prepared by adding a known concentration of the analyte to control fish purchased at a local grocery store and processed identical to study samples. Laboratory control spikes are used to assess method accuracy. The laboratory control spikes must show recoveries between 70-130% or the data is rejected. For the results reported here, the spikes were within the acceptable range.
4.4 Matrix Spikes
-
A matrix spike for each sample was prepared by adding a known concentration of the target
analyte to the sample. 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 Sample Related Comments
Every sample in the analytical set was extracted and analyzed in duplicate. Duplicate sample results are reported along with the sample results in Attachment B.
Data Summary
: .: :
Please see Attachment B for a detailed listing of the analytical results. Results are reported in ng/g (parts per billion) for the analyte on an as-received basis.
Samples are disposed of one month after the report is issued unless otherwise specified. 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. WVDEP will be notified 30 days prior to the disposal of hardcopy data.
7 Attachments
!Ur,.*: V r - ; i--Xt
7.1 Attachment A: Chain of Custody' 7.2 Attachment B: Analytical Results 7.3 Attachment C: Raw Analytical Data
PAGE 4OF5
PAGE 5OF5
Composite
Species
(Common name)
Channel Catfish 1 Channel Catfish
Channel Catfish
Size Class (3.0 cm classes)
17 17 17
Sauger 2 Sauger
Sauger
12 9 12
Common Carp Common Carp 3 Common Carp Common Carp Common Carp
18 19 19 19 20
Hybrid Striped Bass Hybrid Striped Bass 4 Hybrid Striped Bass Hybrid Striped Bass Hybrid Striped Bass
15 13 14 15 14
Weiqht (grams)
830 1020 960
l_ $ - 2 - n ~ i
280
128 L } ? * - n - T 276
2021 2324 2692 2564 3090
768 525 740 <- J P f z / 7 - H 785 630
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DIVISION OF ENVIRONMENTAL PROTECTION - WATERSHED ASSESSMENT SECTION
-- ,
Analysis Request Form, Rev. 7/03
_____ - 1 '
^ T-Mtr"W A F-
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Laboratory Name: 3, V j g f i-,_____
Circle one
Stream Name: : JL
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Watershed Name:
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Station Number:
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Acid Lot #, Nitric: ___________ ^_____ Acid Lot #, Sulfuric:.
Random #
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'Lv-hPe'
Specified Method 40 CFR 136
Field Meter #
Flow meter #
GRAB: Date-Time / ' /
S'.OO " l i ' OO
p,
Am
Lat: '
Long:
Positioning Method (Circle one): Map GPS GPS (corrected) WCMS
FIELD VALUES1' Temp._
pH (meter)_
D.O. (probe)_
Cond.
Flow:
_ yo
H ot H
CQ
Pres. ANALYSIS 3 Acidi) y (Hot) 3 Alkali iity
5 Hardn SS .
3 Sulfat
3 Turba Ity i
. 2 Chloride 3
4 coij 4 TO(jI
7 Fee'll coli., MF i
24 Ijiour Holding Fecal Coli, MF 7 6 HSour Holding 7 E. Coli, numeric 7 Fedal Strep.
3 pHj(iab) 3 Cond. (Lab)
TOO a i 1
Pres. ANAL YS1S 3 Tot. So ids 3 Dis. So ids 3 Tot. Susjp. Solids 4 Tot. P h|s. ! 8 Ortho Pjhos. 4 TKN | 4 Ammojua-N 4 Unionized NHj 4
3 NO.,-lj
i 3 N O ;-|
4 N 0 2.- 4 0 3-N 5 Magr esium 5 Potassium
Pres. ANALYSIS
Tot*
5 Sodium --------- j i
5 Aluminum
H
5 Cadmi ujn
L
5 Chromii m
HL
5 Copper 5 iron
L H
5 Lead
L
5 Manganese
H
5 Mercury j
5 Nickel
L
5 Zinc
5 Calcium 5 Seleniurr
L
H L
Dis`+
PRESERVATION CODE:
1. None - determined on site
H 2. None
L @ IcedDry
H L 4. H2SO4to pH <2, iced (phenols in glass container)
L 5. HNOj to pH<2
H 6. (Cyanide) NaOH to pH > 12, iced (0.6 g
L ascorbic, acid used on samples with residual chlorine)
7. Sterile + .008% N a,S20.->, iced
8. Filtered immediately, iced 1.
9. Other (specify):
L REMARKS Irr
u
/ D ry JU t j
I (SSu. Anct|\/A(L3 -faz-'
C L 8 m ( L i ) C o '- n p o s i k s
^\* r vy>tAJUV^' W tln ij CG'
* Indicate (circle) desired detection level: H = High (e.g. 5 pph) L = Low (e.g. 0.05 ppb)
+ Filtered in the field, nitric acid added.
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^Rsliqcjuisheti hy:
Bale J - Z 9 - O S Received b\:
Relinquished hy:
Date
LL / ( O L - : Time
Lab: Time
MAIL RESULTS TO: ATTN: Janice Smithson
, (Lab Instructions for Billing ; On Invoice bill to Organizational Unit 9480)
Division o f Water and Waste Managment, Watershed Branch. 414 Summers Street. Charleston. WV 25301 Phone (304) 558-2837
WHITE - Sample collector CANARY - Laboratory
Received by: Lab:
yt
RESEARCH
3058 Research Drive State College, P A 16801
Phone: 800-281 -321S Fax: 814-272-101S
Laboratory Sample Log-in Sheet (Environmental)
Complete upon sample receipt:
Client and/or Project Name
Method of Delivery
Walk-in Trackina#:
Pick-up
GUPS 57/" ?
77
D t-s f
FedEx
P s c -J rc
Air Borne Other (exolain!
......
Chain of Custody
Custody Seals:
present, & intact / broken (explain)
^absent
Temperature Preservation
_i
Thermometer ID: . noL^f Cooler ID: S '/ / > - f Cooler ID: Cooler ID: Cooler ID:
Cooler temo: Cooler temo: Cooler temo: Cooler temo:
C C C C
Chain of Custody Record: /^ETpresent
absent
Samples Received: on ice in ice melt _ with ice paclc none
tr*
-
Explanation Completed by
' Sionature:
/
............ ....... , ............................................................ Date (Time): c < j e / e } / c l #
Complete during sample log-in:
L1MS Log-in #
PhysicalCondition
Samplesjntact?
Chain of Custody
Samples received agree with COC record?
Analysis Request
Analysis request clear?
Preservation
Sample containers appropriate?
Chemical preservation appropriate?
Samples received within holding time?
Sample volume/mass adequate?
/ s Y e s 5 * ^ (explain)
/f^Y es No (explain)
^ 0 Y e s No (explain)
Yes No (explain) Yes No (explain) Yes No (explain) Yes No (explain)
Explanation Completed by Sionature:
/
/
Date:
/ f i r * - `'O J t f ^
.......................... .
Complete foilowing resolution of anv nonconformances:
Client Contacted
Yes Client: No
'
Resolution
.
....... Date (Time): .................. .
Completed by Slanature: Lab Sx Log-in Sheet -Ex
. Date: . ...
11-5-01/0
LOGIN CHAIN OF CUSTODY REPORT (InOl) Oct 21 2003, 09:03 am
Login Number: L35217 Account: 3056 WEST VIRGINIA DEPT OF ENV PROTECTION
Laboratory
Cirant
Collect Receive
Due
L 3 E ;2 E V -y
CHANNEL ::;aATRTSK;
|B H :^ S P lG 3 1 E 0 H S P : U ;3 i
SAMPLES TO BE ANALYSIZED FOR PFOA--STORED IN FREEZER 10.
Page 1 Signature : Date :
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5 Packaging f~l FedEx Envelope*
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* DnrrlBicrl vntrrn limit $9K)
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6 Special Handling n SWBDfDevery
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Not available for
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Docs this s ltljm ip itl con iato dnnyerotis goods? j., ;' * f`n * 't i R f 'i i f i Imrl
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m Yes'. '* n Yes
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Questions? Visit our Web site at fectex.com
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Proven Resulte.
Summary of PFOA in Fish Samples
Analyte Found (ng/g)
C8 Acid PFOA
Sample ID
_____ Perfluorooctanoic Acid
Catfish Catfish* Sauger Sauger* Common Carp Common Carp*
ND ND ND ND ND ND
Hybrid Striped Bass Hybrid Striped Bass*
ND ND
ND Response less than LOQ (0.50 ng/g) la b o ra to ry Duplicate
t3058 Research Drive State College, PA 16801, USA J : 814.272.1039 F: 814.231.1580 exygen.com
Proven Results.
Recovery Summary fo r PFOA in Fish
Sample Description Channel Fish Spike C
5 ppb Spike
Amount Spiked (ng/g)
C8 Acid PFOA
Amt Found Amount
in Sample Recovered Recovery
(ng/g)
(ng/g)
(%)
5
ND
5.97
119
Sauger Spike D
5 ppb Spike
5 ND 5.65 113
Common Carp Spike E
. 5 ppb Spike
5 ND 5.75 115
Hybrid Striped Bass Spike F
*. 5 ppb S p ik e
5
ND
4.60
92
.. \
.
1
ND = Response less than LOQ (0.50 ng/g)
3058 Research Drive M State College, PA 16801, USA
T: 800.281.3219 m F: 814.272.1019
exygen.com
RAW DATA REPORT
Sponsor Study No: Exygeii Study No: Analyte:
ions Monitored:
NA L35217 PPOA 413-> 369
Centre ID
C 101703-7 C101703-6 CW1703-5 C10I703-4 C101703-3 C101703-2 C101703-1 Methanol Wash Reagent Blank 0302405 Control 0302405 Spk A 0302405 Spk B Cl 01703-7 C 101703-6 L35217-1 SpkC L35217-2 Spk D L35217-3 SpkE L35217-4 SpkF C101703-5 L35217-1 L35217-1 Dup L35217-2 L35217-2 Dup C101703-4 C101703-3 L35217-3 L35217-3 Dup L352I7-4 L35217-4 Dup C101703-2 C101703-1
Sponsor ID
-
-
-
-
-
-
-
-
na na na na
-
-
. Channel Catfish Sanger
Common Carp Hybrid Striped Bass
-
Channel Catfish Channel Catfish
Sauget Sauger
-
Common Carp Common Carp Hybrid Striped Bass Hybrid Striped Bass
-
-
Sample
Run
Code
No.
CS 11703A-3001
CS 101703A-3002
CS 101703A-3003
CS 101703A-3004
CS 101703A-300S
CS 101703A-3006
CS 101703A-3007
C 101703A-3008
C 101703A-3009
c 101703A-3010
. LCS 101703A-3011
LCS 101703A-3012
CS 101703A-3013
CS 101703A-3014
LF 101703A-3015
LF 101703A-3016
LF 101703A-3017
LF 101703A-3018
CS 101703A-3019
S 101703A-3020
S 101703A-3021
S 101703A-3022
S 10V703A-3023
CS 101703A-3024
CS 101703A-3025
S 101703A-3026
s 101703A-3027 s 101703A-3028 s 10I703A-3029
CS 101703A-3030
CS 101703A-3031
Analyte Pound (ng/mL) = (peak area - intercept) / slope
Set No: Limit of Quantitation: Injection Volume: Matrix:
101703A 0.5 ng/g 15 pL Fish
Std. Cone. Sample Wt . Final Voi. (ng/mL) ____ isl___ (mL) 0.5 - 1.0 - 2.5 - 5.0 - 10 - 25 50 - -
-- 5.0 2.0
- 5.0 2.0 " 5.0 2.0
5.0 2.0 0.5 - 1 --
- 5.0 2.0 5.0 2.0
- 5.0 2.0
- 5.0 2.0 2.5 - ,, 1 " 5.0 2.0
- 5.0 2.0
- 5.0 2.0 - 5.0 2.0 5.0 - 10 - - 5.0 2.0
- 5.0 2.0
- 5.0 2.0
5.0 2.0 25 - 50 " *
Dilution Peak Factor Area
- 26313 - 55201 - 126624 - 266356 - 531599 - 1328415 - 2643608 -0 1 2181 1 18604 1 94390 1 627917 - 29622 - 59620 1 810840 1 767131 1 781039 1 624701 - 147839 1 36224 1 24567 1 32576 1 44751 - 258881
- 530191 1 43465 1 36415 1 14727 1 26367 - 1380092
- 2832280
Analyte Found (ng/mL)
-
-'
-
-
-
-
0.027 0.329 1.725 11.553
-
-
14.922 14.117 ' 14.373 11.493
-
0.654 0.439 0.587 0.811
-
-
0.787 0.657 0.258 0.472
-
-
Analyte Found (ng/g) = [(analyte found (ng/mL) - average analyte found in blanks (ng/mL)) x final voi (mL) x dii. factor] / (sample wt (g)) Recovery (%) = ________ analyte found (ng/g) x 100%________
(amount added (ng/g))
Analyst: Instrument Type: Extraction Date: Analyzed on:
Karen Rislin LC/MS/MS K 10/17/03 10/18/03
Analyte Found Amount Added
(ng/g)
(ng/g)
Recovery (%)
..
-
_
-
_
_
ND 0.13* (ND)
0.69 4.62
-
_
5.97 5.65 5.75 4.60
-
ND ND ND ND
. .
0.5 5.0
5.0 5.0 5.0 5.0
112 90
119 113 15 92
_
ND .
ND ND ND
-
-- -
Standard Curve : Linear (l/x weighted) Intercept = 733.016 Slope = 542S9.3
Coef. Of Det. = 0.998247
CS = Calibratiun standard C = Control sample
LF = Lab fortified sample KF = Field fortified sample
ND = Response less than LOQ (0.5 ng/g)
S = Sample
LCS - Laboratory Control Spike
Spreadsheet prepared by:
'"Value used to correct for Spk A and B.
RESEARCH
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
SAMPLE TRANSFER'SHEET
Protocol Number: ___
NA
Exygen Study Number:
L35217
Exygen Sample # Y L3527-1 - Y L35217-2 J l L3 5217-3 Y L35217-4 ( j ) 0302405
-
-
-
Sponsor Sample # Channel Catfish Sauger ' Common Carp
Hybrid Striped Bass Library Fish
-
Exygen Sample #
_
-
Sponsor Sample # .. .
-
-
--
Karen Risha 10/16/03 1025
Requested By (Printed Name/Date/Time)
-
Samples removed frorqj^
/Q
OAJ Box# -trS ' - 6 } (
Samples removed from: - jf F (k z .H f ________Box# f ) Aj p /n r J
0,, Shelf# - ) -
Shelf#
/o/^/e
JkSamples transferred to the custody of _
LML.
j, jc
a /y / o
/a y s ~.
Sample Custodian Initials/Date/Time
Samples received from custodian; Samples moved to fv&lZgir ^ * 4
iditloa I0SO
Laboratory Persoxmel Initials/Date/Time
Samples removed from
3V
Samples returned to - 'Qr-c; Q r f~ JO
Sample Custodian Initials/Date/Time
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
Internai Chain of Custody/Fortifxcation Sheet
Exygen Study Number:
L35217
Matrix: Fish
Sponsor Study/Protocol No: NA
The samples listed below were removed from freezer No. 3 4
Time P A S O
Date_ i Q l n l o a
Initials.
CLIENT SAMPLE ID na na na na
Channel Catfish Sauger
Common Carp Hybrid Striped Bass
Channel Catfish Channel Catfish
S auger Sauger Common Carp Common Carp Hybrid Striped Bass Hybrid Striped Bass
EXYGEN ID NUMBER
Reagent Blank
0302405 Control
0302405 Spk A
0302405 Spk B
L35217-1 Spk C
L35217-2 SpkD
L35217-3 Spk E
.
L35217-4 SpkF.
L35217-1
. L35217-1 Dup
L35217-2
.
L35217-2 Dup
L35217-3
L35217-3 Dup
L35217-4
L35217-4 Dup
-
WEIGHT (g) _
FORTIFICATION (ng) -
5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 . * 5.0 5.0 5.0 5.0 5.0 ` -
-
2.5 25.0 25.0 25-0 25.0 25.0
_
-
-
-
-
- - --
0302405 Spk A " 0302405 Spk B
L35217-1 Spk C L35217-2 SpkD L35217-3 SpkE L35217-4 Spk F
Spiking Solution Used F092203-5 (10 ng/mL) F092203-4 (100 ng/mL) F092203-4 (100 ng/mL) F092203-4 (100 ng/mL) F092203-4 (100 ng/mL) F092203-4 (100 ng/mL)
_-
All samples were weighed on balance No.
Time 0 3 4 0
Date I0j'~ f)03 '
Volume Used for Spiking 250 pL (100 pL micropipet) 250 pL (100 pL micropipet) 250 pL (100 pL micropipet) 250 pL (100 pL micropipet) 250 pL (100 pL micropipet) 250 pL (100 pL micropipet)
-
Initial/Date
^ 1 In o3 ^ /Jfllnio3 t !L /l liik 3 L /lojnl 3 m minio S M , /ljnk 3 U- -
Initials.
After weighing samples were returned to freezer No. _ M -
Time DflOO
Date | D j n ) n ^
Initials. % r -
C o m m e n t s : 200 jiL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date:.
.ip ln lo s
Analysis Summary': .
Data Set: Data Set: Data Set:
Tnitials/Date: -- Tnitials/Date: ~
/ tp \n jfr3 / W' /
Set extraction/analysis data verified b y :. <:iM f*
Date: f /$ '/ 5 July 26, 2001/1
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
SAMPLE: EXTRACTION AND ANALYSIS TRACKING SHEET
EXYGEN STUDY NUMBER: L35217 MATRIX: Fish
METHOD: "
PROTOCOL. NUMBER: NA
--------------------------------------- - . lo in r a it O T o a L ,. ,fw ,, _________
h iitia ls/D a te
f Z 2: SPEcolumn
' ` h "
STEP 3: Concentrate to almost dryness
STEP 4: Adjust final volume to 2 mL
STEP 5: LC/MS/MS analysis
STEP 6: LC/MS/MS reanalysis.
^ "" "
f' " " ~ ' h " ' #3. -j
Final extracts stored in refrigerator D / -- Initials-
Hm trals and date under each step indicates the personnel that perform ed tills step.
W p t n An ? f S f r * e Determinaticm of Fluorochemicals in Green Beans, Apples, Pork Muscle, Cow Milk, Chicken Muscle, Chicken Eggs, Bread, Hotdogs, and Catfish by LC/MS/MS.
je jn |i
-Dale: 7/o3
COMMENTS:
LC/MS/MS SYSTEM AND OPERATING CONDITIONS
Sponsor Protocol No: NA
Exygen Study No: L35217
Instrument:
Micromass Quattro Ultima (LC/MS/MS Unit #6)
Computer:
COMPAQ Professional Workstation AP200
Software:
Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004
HPLC Equipment:
Hewlett Packard (HP) Series 1100
HP Bin Pump
HP Vacuum Degasser
HP Autosampler
HP Column Oven
HPLC Column:
Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E)
Mobile Phase (A) : Mobile Phase (B) :
2 mM Ammonium Acetate in Type I Water
Methanol
.
Analyst: .
Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580
NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set.
All Handwritten Peak ID's by: y f o ) 0 3
Scanning Method Report
Method:
C:\MASSLYNX\OO8 -AFFO.RRO\ACQUDB\OO8 PFOA
hast Modified: Tue Mar 05 09:37:05 2002
Printed:
Fri Oct 17 14:40:59 2003
o3
Solvent Delay ( mins ) :
0.00
Function : 1
MKM of 1 Mass Pair ( ESP- )
Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeat's :
Channel Parent Daughter
0.03 0.00 0.00 8.00 1 Dwell
. (Secs)
Coll Energy
(eV)
Cone
1
413.00 369.00
0.20
10
10
Rage 1
Method Report Method File : Last Modified: Printed:
HP1100 LC Pump Initial Conditions
c :MaSsLilBCX 008-APFO.PRO\ ACQTJDB \water Friday, October 17, 2003 14:41:04
Friday, October 17, 2003 14:41:07 .j
M ite
Page 1
Solvents A% B% C% D%
Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C)
60.0 40.0
0.0
-0
0.300 15.0
0 400
35.0 ' 35.0
HP1100 LC Pump Gradient Timetable
The gradient Timetable contains 10 entries which are
Time
A%
B%
C%
D% Flow Pressure
0.00
60.0
40.0
0.0
0.0 0.300
400
0.40
60.0
40.0
0.0
0.0 0.300
400
' 1.00
10.0
90.0
0.0
0.0 0.300
400
7.00
10.0
90.0
0.0
0.0 0.300
400
7.50
0.0 100.0
0.0
0.0 0.300
400
9.00 0.0 100.0 0.0 0.0 .4 00 400
9.50
60.0
40.0
0.0
0.0 0.400
400
13.50
60.0,
40.0
0.0
0.0 0.400
400
14.00
60.0
40.0
0.0
0.0 0.300
400
15.00
60.0
40.0
0.0
0.0
0.300
, 400
HP1100 LC Pump External Event Timetable
The Timetable contains 7 entries which are :
Time Initial
0.00 0.05 3.00 3.05 8.00 8.05 *
Column Switch Off Off Off Off Off Off Off
Contactl Off On Off Off Off Off Off
Contact2 Off On Off Off .Off Off Off
Contact3 Off Off Off Off Off On Off
Contact4 Off Off Off Off Off Off
Off
HP1100 Autosampler Initial Conditions
Draw Speed Eject Speed (il/min) Draw Position (mm) Stop Time (mins) Injection Volume (/il) Vial Number
200.0 200
.0.10 15.00 15.0.
7
Tuning Method Report
Method:
C :\ M A S S L Y N X \ 0 0 8 - A P F O .PRO'SA C Q U D B \ P F O A TUNE
Printed:
Fri Oct 17 14:41:18 2003
Page 1
Dan 413.00
SOURCE ( ESP- )
Capillary
Cone
.
Hexapole 1
Aperture 1
Hexapole 2
Source Block Temp.
Desolvation Temp.
Set Rdbk
3.00 10 0.0 0.0 0.0 100 300
-2.93 -31
100 299 .
Pressures
Analyser Vacuum Gas Cell
Rdbk
OFF 3 . 4e-3
Analyser
LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 lEnergy 2 Multiplier
Gas Flows
Cone Gas Desolvation
Set Rd
14.0 14.0 1.0 -2 10 '2 14.0 14.0 2.0 700
37 39 41
-6
Rdbk
133.6 764.5
Quantify Calibration Report Study N o L 3 5214, Set No.:101703A, Ext .Pate:10/17/03, Analyst :K.Risha
Calibration: P: \Data\I.CMSMS6\Masslynx\Fluorochexttiaals .PRO\CurveDB\101703A WV
Past modified: Mon Oct 20 07:57:19 2003
Printed:
Mon Oct 20 03:01:29 2003
\o\x>\D3
Page 1
Exygen Research, 3058 Research Drive, State College, PA 15801
Quantify Sample Report
Study No. :L3 52 li, Set M o .:101703A, JExt.Date:10/17/03, Analyst:X.Risha
7
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SarapleDB\101703A WV
Last modified Mon Oot 20 07:49:09 2003
Method:
P: \Data\LCMSMS6\Masslynx\:Fluoroch.emicals ,PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
'
Job Code:
Initials
Page 1
Printed:
Mon Oot 20 08:01:30 2003
5 e u fe s K rS q o iToj i " I Q5ft=-3Bg 1
Name: 101703A-3001 Text:
1: C8 A c i d
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
.
Study No.:L3521, Set N o .:101703A, Ext .'Date:10/17/03, Analyst :K.Risha
.,
7
Sample Lxst: P: \Data\LCMSMS6\Masslynx\Fluorochemi.aals.PRO\S^mpleDB\1017D3A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Page 2
Name: 101703A-3002 Text: 1: C8 Acid
C101703-6,1.0 ng/mL standard
101703A-3002 Sm (Mn, 2x2)
100-1
%-
5-14 55201^
A
18-Oct-2003 02:30:35 LC/MS/MS #6
MRM of 1 Channel ES413 >369 2.75e5 A re a
0 -->--
1.00
~T.1it t 1"117..
2.00 3.00
1 I 1 ` 1 '"'I"1" 1' n r t r r t r r r i ' T i - ) - ' 'i ' | n - r - f r n - T f r r i 7 ( T i m e
4 .0 0
5 .0 0
6 .0 0
7 .0 0
8.00
Exygen Research, 3058 Research Drive, State College, PA 15801
Quantify Sample Report
Study No.: L3 521^, Set N o .:101703A, Ext .Date: 10/17/03, Analyst-.K.Risha
7 ..
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SanipleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P: \Data\LCMSMS6\Masslynx\Fluorochemicals-PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Page
Name: 101703A-3003 Text:
1; C8 A c i d
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No.:L352li, Set N o .:101703A, Ext.Date.-10/17/03, Analyst:K.Risha
7
Sample List: P:\Data\LCMSMS6\Massiynx\Fluorochemicals.PR0\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P :\Data\LCTSMS6\Masslynx\Fluorochemicals- PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Page 4
Name: 101703A-3004 Text.: 1: C8 Acid
C101703-4, 5,0 ng/mL standard
101703A-3004 Sm {Mn, 2x2)
100-
%-
5.15 266356
18-Oct-2003 03:04:00 LC/MS/MS #6
MRM of 1 Channel ES413 > 369 1.26e6 Area
0 -W
1.00
2.00
11 r1 `
3.00
I 1 1 n - r-r'T
4.00
5.00
t ` * I * i
6.00
7.00
Time 8.00
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No. :L35214, Set No.:101703A, :Ext.Date:10/17/03, Analyst:K.Risha
,. 7 .
'
Sample List: P: \Data\LCMSMS6\Masslynx\Fluorochemicals .PRO\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code: '
'
Printed:
Mon Oct 20 08:01:30 2003
Page 5
Name: 101703A-3005 Text:
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No. :Xi352l4/ Set No.:101703A, Ext.Date:10/17/03, Analyst:K.Risha
,7
Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P :\Bata\LCMSMS6 \Masslynx\Fluorochemicals .PRO\MethDB\PFOA 101703
Last modified: Mon Oct .20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Page 6
Name: 101703A-3006 Text : 1: C8 Acid
C101703-2, 25 ng/mL standard
101703A-3006 Sm (Mn, 2x2)
10^
%: '
18-Oct-2003 03:37:31 _ LC/WIS/WIS #6
MRM 5 1 Channel ES5.15 413 > 369
6.01 e6 A re a
0- T *1--1--I--;--l--TT
T-r-r-r
>'11,1 1I 1'' i Tim e
1.00
2.00
3.00
4 .0 0
5 .0 0
6.00
7.00
8.00
Exygen Research, 3058 Research Drive, State College, PA 15801
Quantify Sample Report
Study No.:L352.1f, Set N o .:101703A, Ext.Date:10/17/03,- .Analyst :K.'Risha 1
Sample List: P: \Data\LCMSMS6\Masslynx\Fluorochemicals .PRO\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Page 7
Name: 101703A-3007 Text:
1: C8 Acid
Exygen Research, 3053 Research Drive, State College, PA 16801
Quantify Sample Report
Stuy N o .:L3 521-4, Set Wo. :101703A, Ext.Date: 10/17/03, analyst :K.Risba
7
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P: \.Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MsthDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Page 8
Name: 101703A-3008 Text:
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample -Report
Study No. :L35214, Set No.:1017Q3A, Ext-Date: 10/17/03, Analyst:K.Risila
,7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\101703A WV
Last modified: Mon Oot 20 07:49:09 2003
Method:
P :\Dat a\LCMSMS 6\Mas slynx\Fluorochemi cals.PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
,
Page 9
Name: 101703A-3009 Text:
1 : C8 Acid
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No. :1.35214, Set No.:101703A, .Ext ..Date:.10/17/03, Analyst :K.-Risha
7-
Sample List: P:\Data\LOMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\1017 03A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P :\Data\LCMSMS 6\Mas Slynx\Fluorochemical s .PRO \MethDB \PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Page 10
Name: 101703A-3010 T e x t ::
1: C8 Acid
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No.: L35214 , Set .No .:101703A, Ext .Date:ID/17/03 , Analyst :K.Risha
7
Sample List: R:\Data\LCMSMS6\Masslynx\Fluoroclaemicals.PRO\SaitipleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FRO\MethDB\PFOA 1017 03
Last modified: Mon Oct 20 07:50:10 2003
.
Job Code:
Page 11
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3011 Text: 1: C8 Acid
0302405 Spk A, 0.5 ppb
101703A-3011 Sm (Mn, 2x2) 10CH
%:
18-Oct-2003 05:00:57
LC/MS/MS #6
5.25
MRM of 1 Channel ES413 >3 69
5.22e5 Area
0 " h - T - r i- '| , , 1 - q 'T T i i j . V I i j
1.00 2.00
3.00
4.00
''"r i' | m - T
5.00
, j i- / t "]r r r - j i i
6.00
7.00
i Time 8.00
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report ~
Study No.:L35214, Set No.:101703A, Ext.Date:10/17/03, Analyst:K.Risha
Sample List:
7
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P: \Data\LCMSMS6\Masslyixx\Fluorochemieals .PROYMethDBYPFOA 101703
Last modified: Mon Oct 20 07:30:10 2003
Job Code:
Page 12
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3012 Text:
1 : C8 Acid
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No.:L352l4, Set N o .:101703A, Ext .Date:10/17 /03 , Analyst :K.Risha
7
Sample List: P: \Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003"
Method:
P:\Data\LCMSMS6\Masslynx\Pluoroohemicals.PRO\MethDB\PPOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
v
Page 13
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3013 Text s
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L3523.4/ Set No.:101703A, Ext.Date:1 0 / 1 7 / 0 3 , .AnalystrK.Risha
1 Sample List: R :\Data\LCMSMS6 XMasslynxXFluorochemrcals .RRO\SampleDB\1017 03A W
Last modified: Mon Oct 20 07:49:09 2003
Method:
R : \Data\LCMSMS6\Masslynx\Fluorochemicals.RRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Rage 14
Name: 101703A-3014 Text:
Exygen Research, 3058 Research Drive, State College, DA 16801
Quantify Sample Report
Study No.:L35214, Set No.:101703A, East .Date -.10/17/03, Analyst :K.Risha
7
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\lQ1703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P: \Data\LCMSMS6\Masslymx\Fluorochemicals-PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Page 15
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3015 Text:
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No. :L352.l4, Set No .:101703A, .Ext.Date:10/7/03, Analyst sE.Risha
1
Sample List: P :\Data\LCMSMS6\Masslynx\Fluarochemicals.PRO\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Page 16
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3016 Text:
1: C8 Acid
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study N o .:L35214, Set N o .:101703A, Exfc.Date:10/17/03, Analyst:K.Risha
' , '7
Sample List: P: \Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\101703A WV Last modified: Mon Oct 20 07:49:09 2003 Method: . P:\DataYLCMSMS6\Masslynx\E,luarochemiaals.PRO\MethDB\PFOA 101703 Last modified: Mon Oct 20 07:50:10 2003 Job Code:
Page 18
Printed:
Mon Oct .20 08:01:30 2003
Name: 101703A-3018 Text: 1 : C8 Acid
L35217-4 Spk F, 5.0 ppb
1017Q3A-3018 Sm (Mn, 2x2) 100-
%\
' 5.23
18-Oct-2003 06:57:55 LC/MS/MS #6
M RM f 1 Channel ES413 > 369 3.44e6 Area
0 - L ' i - r ,1 "1 i - i v r - l ...I r - r - i - f - T " , T - r - H T r f T r T T p -
1.00
2.00
3.00
4.00
5.00
6.00
T r-i -r - f i i T r r r r r i" | T i f i l e
7.00
8.00
Exygen Research, 3058 Research Drive, State College, PA 15801
Quantify Sample Report
Study -No .:L352l4/_.-Set No.:101703A, Ext.Date:10/17/03, Analyst :K.Risha
70 Sample List: P: \Data\LCMSMS6\Masslynx\Fluorochemieals.PR0\SampleDB\1017 03A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Page 21
Printed:
Mon Oct 20 08:01:30 2003
.
Name: 101703A-3021 Text:
1 : C8 A c i d
Exygen Research/ 3058 Research Drive/ State College, PA 15801
Quantify Sample Report
'
Study N o . :L35214, Set No.:101703A, Ext.Date:10/7/03, Analyst:K.Risha
70
Sample .List: P:\Data\LCMSMS6\Masslynx\Fluorochemiaals.PR0\SampleDB\101703A VJV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\DataYLCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 101703
Last modified: Mon Oct 20 07:50:10 .2003
Job Code:
'
Page 22
Printed:
Mon Oct 20 08:01:30 2003
.
Name: 101703A-3022 Text:
1: C8 Acid
iDUDto
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No. :L3521/4, Set No.:101703A, Ext.Date:10/17/03, Analyst:K.Risha
Sample Li.st: 1P:\Data\LCMSMS6\Masslyirx\Fluorochemxcals.PR0\SampleDB\i01703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\Data\LCMSMS6\Masslynx\Fruprochemicals.PRO\MethDB\PFOA 101703.
Last modified: Mon Oct 20 07:30:10 2003
Job Code:
Page 23
Printed:
Mon Oct 20 08:01:30 2003
Name:: 101703A-3023 T e x t ::
1 : C8 Acid
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No. :L3521-4, Set No. :101703A, Ext.Date:10/17/03, Analyst.-K.Risha
1 Sample List: P:\Data\LCMSMS6\Masslyxtx\Fluorochemicals.PR0\SampleDB\101703A WV Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Page 24
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3024 Text: 1 : C8 Acid
C101703-4, 5.0 ng/mL standard
101703A-3024 Sm (Mn, 2x2) 10CH
%-
5 .1 4
2
18-Oct-2003 08:38:37 LC/MS/MS #6
MRM of 1 Channel ES413 > 369 1.24e6 Area
1.00
2.00
T
3.00
11I1'J 1I`11'I1
4.00
5.00
T r - j -- '-Tj -"-i`-rI -ri "~i nI T1 im e
6.00
7.00
8.00
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L3S214, Set N o .:101703A, Ext.Date:10/17/03, Analyst:K.Risha
.. Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemzcals.PR0\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code :
Page 25
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3025 Text : 1: C8 A c i d
C101703-3,10 ng/mL standard
101703A-3Q25 Sm (Mn, 2x2) 100-1
%:
5.15 53019^^
18-Oct-2003 08:55:24 _LC/MS/MS #6
MRM of 1 Channel ES413 >369 2.46e6 Area
0 I"<--r-v I ITT'-I I1 . I . p - n T '["I r r i p .r-rr-p -r
1.00
2.00
3.00
4.00
f 1 1 ' 1 I 1 J 1 kI *-- fT -rT T r;' i r .-n-T-TTTi-r.-rri Time
5.00
6.00
7.00
8.00
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L3521^, -Set No. :101703A, E x t .Date: 10/17/03, -Analyst :iC.Risha
Page 26
Sample List: P: \Data\LCMSMS6\Massly3ix\Fluorocfaemicals.PRO\SamrpleDB\101703A WV
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Method:
P:\Data VLCMSMS 6\Mas slynx\Fluorochemicals.PRO\MethDB\PFOA 101703
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Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3026 Text:
1: C8 A c i d
m ) U O ) o3>
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report
Study No.:L3521&, Set N o .:101703A, Ext .Date: 10/17/03, Analyst :K.Risha
, 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\101703A W
Last modified: Mon Oct 20 07:49:09 2003
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals-PRO\MetbDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003 Job Code:
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Mon Oct 20 08:01:30 2003
Page 27
Name: 101703A-3027 Text :
1 : C8 Acid
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample :Report Study N o .:L3521^l, Set N o .:101703A, Ext.Date:10/17/03, Analyst:K.Risha
1 fi) Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SanrpleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P :\Data\LCMSMSS\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
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Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3028 Text:
1 : C8 Acid
D3
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L3521^, Set No. :101703A, Ext ..Date :1 0 /17/03, Analyst 'S:Ri sha
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Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocliemicals.PR0\SainpleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
P :\Data\LCMSMS6\Masslynx\Fluorochemicals .PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3029 Text:
1: C8 Acid
(!)()
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L35214j^, Set No. :1017 03a , Ext.Date:10/17/03, AnalystrK.'Risha
Page 30
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\101703A WV
Last modified: Mon Oct 20 07:49:09 2003
Method:
p :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
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Mon Oct 20 08:01:30 2003
Name: 101703A-3030 Text: 1: C8 Acid
C101703-2, 25 ng/mL standard
101703A-3030 Sm (Mn, 2x2) 100-
%:
5.15 1380092"!
18-Oct-2003 10:19:13 LC/MS/MS #6
MRM of 1 Channel ES413 > 369 6.41 e6 Area
o- 1' ' 1 l~~'M1T"11' 11 1` `1"II' 1' 11 .' '1 I' 1` '1 11 11 II 11T' " i1- r1 i i'- i`...i1t1- I ' 1 1 I 1 1 ' 1 1 1 1T ' I ` I ' r T"' 1 ' '"I ' 1 ` II' J I I I I I, ,I ,. ,I...Jr -ipm e. v'V'i |
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Exyge.n Research, 3058 Research Drive, State College, PA 15801
Quantify Sample Report Study No.:L352l4, Set No.:1017Q3A, TExt.Date: 10/17/03 , Analyst:K.Risha
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Sample List: P: \Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\SampleDB\101703A WV
Last modified: Mon' Oct 20 07:49:09 2003
' '; ' v '
Method:
P :\Data\LCMSMSS\Masslynx\Fluorochemicals .PRO\MethpB\PFOA 101703
Last modified: Mon Oct 20 07:50:10 2003
Job Code:
'
Printed:
Mon Oct 20 08:01:30 2003
Name: 101703A-3031 Text:
1: C8 Acid
Exygen Research, 3058 Research Drive, State College, PA 16801
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