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Exwen - RESEARCH
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Analytical Report
Fluorochemical Characterization of Aqueous Samples
Fayetteville C8 Sampling 11/0 5 Exygen Research Laboratory Report No . L0006767 (Amended Final Repo rt)
Testing Laboratory Exygen Research
3058 Research Drive State College, PA 16801
Requester Michael D . Aucoin URS Corporation Barley Mill Plaz a Bldg 19 Room 2118 Lancaster Pike and Rt 141 Wilmington, DE 19805
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058 Research Drive State College, PA 16801, USA
T: 800 .281 .321 9 F : 814 .272 .1019 exygen .com
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I Introductio n
Results are reported for the analysis of water samples received by Centre Analytical Laboratories, Inc . (dba Exygen Research) (Exygen) from DuPont Corporation . This report presents results assigned to Exygen Research study number L0006767 . This report is an amended report of Exygen Research study number L0006767 . This amended report utilizes a different technique for determining signal to noise ratios for the determination of limit of detection and limit of quantification than in the original report . Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples . A total of 3 samples were received for analysis . The sample was prepared and analyzed by LC/MS/MS for the following list of fluorochemicals :
Table 1 : Target Analysi s Compound Name Acronv Ammonium Perfluorooctanoate APFO Perfluorooctanoic Acid PFOA
2 Sample Receip t The samples were submitted in plastic containers, cooled with wet ice . The samples were collected on 11/16/05 and were received on 11/17/05 . Chain-of-custody information is presented in Attachment C .
3 Holding Times
The analytical method used was validated against a maximum holding time of 14 days in water samples. All samples were analyzed within the required holding time .
4 Methods - Analytical and Preparatory 4.1 LC/MS/M S
4.1 .1 Sample Preparation for LC/MS/MS Analysi s Water samples were initially treated with 200 uL of 250 mg/mL sodium thiosulfate solution to remove residual chlorine . Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis . A forty-milliliter portion of sample was transferred to a C18 SPE cartridge . The cartridge was eluted with 40% methanol : water . The eluate was discarded . The cartridge was then eluted with 100% methanol . A 5 mL portion of methanol was collected for analysis by LC/MS/MS . This treatment resulted in an eight-fold concentration of the samples prior to analysis .
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4.1 .2 Sample Analysis by LC/MS/M S A Hewlett-Packard HP1 100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts . Analysis was performed using selected reaction monitoring (SRM) . Samples were extracted and analyzed on 11/18/05 . Raw analytical data can be found in Attachment D .
5 Analysis 5.1 Calibration
An 8-point calibration curve was analyzed at the beginning of the analytical sequence and throughout the run for the compounds of interest . The calibration points were prepared at 5, 10, 25, 50, 100, 250, 500, and 1000 ng/L (ppt), as perfluorooctanoic acid (PFOA) . The instrument response versus the concentration was plotted for each point . Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined . A calibration curve is acceptable if r > 0 .992 (rz > 0 .985) . Calibration standards for MS/MS analysis were prepared using the same SPE procedure used for samples . For the results reported here, calibration criteria were met.
5.2 Blank s Extraction blanks were prepared and analyzed with every extraction batch of samples . The extraction blanks should not have any target analytes present at or above the limit of detection . For these samples, the extraction blanks were compliant. Instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples . Again, the blanks should not have any target analytes present at or above the limit of detection . For the samples presented here the instrument blanks are compliant.
5.3 Surrogate s Surrogate spikes are not a component of the LC/MS/MS analytical method .
5.4 Matrix Spikes A matrix spike was prepared for each field sample at 5000 ng/L . The matrix spike recovery was within the acceptable range of 70 - 130% . Matrix spike recoveries are given in Attachment B .
5.5 Duplicates
Each field sample was analyzed in duplicate . Results are given along with the sample results in Attachment A.
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5.6 Laboratory Control Samples Milliq water was spiked with PFOA at 50 and 500 ng/L . with each extraction set. All laboratory control samples showed recoveries between 70 and 130% .
5 .7 Sample Related Comments
A single analytical run was performed to complete the sample analysis . The following is a brief quality control narrative for the run. Analytical Samples Analyzed Comments Run Numbe r 111805 A FAY-D-4328MLR, FAY-D-6999PED, All quality control results were
FAY-K-FBLK-1 acceptable and all data are useable .
6 Data Summayr Please see Attachment A for a detailed listing of the analytical results . All results are reported in (ng/L) parts per trillion as APFO and PFOA .
7 Data/Sample Retentio n
E_ . 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 .
8 Attachments
8.1 Attachment A: Results 8 .2 Attachment B : Matrix Spike Recoveries 8 .3 Attachment C : Chain of Custod y 8 .4 Attachment D : LC/MS/MS Raw Analytical Data 8 .5 Attachment E : Standards Data
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V enIt Precise Research. Proven Results .
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IVMAL
Analytical Results Fayetteville C8 Sampling 11/0 5
DuPont Sample Identification APFO ( ng/L) PFOA (ng/L) FAY-D-4328MLR NQ NQ FAY-D-4328MLR (laboratory duplicate) NQ NQ FAY-D-6999PED ND ND FAY-D-6999PED (laboratory duplicate) ND ND FAY-K-FBLK-1 ND ND
Limit of Detection (LOD) for the procedure is approximately 4 .5 ng/L Limit of Quantitation (LOQ) for the procedure is 22 ng/L ND - Compound not detecte d
NQ - Compound detected at a level betweerl the LOD and LOQ . Result is not quantifiable . ND < LOD < NQ < LOQ
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Analytical Results Fayetteville C8 Sampling 11/0 5
DuPont Sample Identification
APFO (ng/L) PFOA (ng/L)
FAY-D-4328MLR NQ NQ FAY-D-6999PED ND ND FAY-K-FBLK-1 ND ND
Limit of Detection (LOD) for the procedure is approximately 4 .5 ng/L Limit of Quantitation (LOQ) for the procedure is 22 ng/L ND - Compound not detecte d
NQ - Compound detected at a level between the LOD and LOQ . Result is not quantifiable . ND < LOD < NQ < LOQ
Results are calculated according to the following criteri a If the sample and laboratory duplicate are greater than 5X LOQ, and the relative percent difference (RPD) is less than 20, the average value is reportecL . If the RPD is greater than 20, the higher value is reported .
If the sample and laboratory duplicate are less than 5X LOQ, and the absolute difference is less than LOQ, the average value is reported . If the absolute difference is greater than LOQ, the higher value is reported .
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Attachment B : LC/MS/MS Laborato ry Spike Recove ry
Sample ID : FAY-D-4328MLR Spiked Amount (ng/L) : 5000
PFOA
Sample Matrix Spike Matrix Spik e
Concentration
Result
Recovery Criteria
(ng/L) (ng/L) (%) (Pass / Fail)
9 .95 5870 117 .2 PASS
Lower Recovery Limit : 70 Upper Recovery Limit : 13 0 Concentrations represent amount present as the PFOA anion
Note : Sample results less than 13 ng/L are reported as NQ in the results sec ti on as they are below the limit of quan titation . Results are given in this table for recovery calcula tions only.
0008
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Attachment B : LC/MS/MS Laboratory Spike Recovery
Sample ID :
FAY-D-6999PED
Spiked Amount (ng/L) : 5000
JPFOA
Sample Matrix Spike Matrix Spik e Concentration Result Recovery Criteria
(ng/L) (ng/L) (%) (Pass / Fail)
0 5250 105 .0 PASS
Lower Recovery Limit: 7 0 Upper Recovery Limit : 13 0 Concentrations represent amount present as the PFOA anio n
0009
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3058 Research Drive Phone : 814-272-1039 State College, PA 16801 Fax : 814-231-1580
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Login Group : L0006767
Login #: 6878 Conform COC Sample : True Project : P0000418 Conform COC : True Company Name : DuPont Conform Sample : True Submitted By : Michael D . Aucoin Conform Request : True Login Type : Immediate Receipt of Samples Started : True Date Start : 11/17/2005 Due Date : 11/27/2005 Received Date : 11/17/2005 Received By : Ammerman, Mark Spread Sample : Label : Exygen SD/PI : Risha, Kare n Project Title/Type : Analysis of Fluorochemicals in Water / ROUTINE Login Notes :
Package Ca rton Date! Condition
Packages / Containers
Shipper/ ID
Temp. Control/Temp.
Direction I Handled By
K0007848 Received Date : 11/17/05 11 :10 FEDEX Wet Ice RECEIVED
Package & Contents Uncompromised
72742 6564 6567
0 .8 Ammerman, Mark
Container # Gross Weight pH Container Type Preservative Mfg .
C0119853
562.80 g 8 .40 500 ml Clear Plastic NON E
Narrow
C0119854 551 .20 g 8 .20 500 ml Clear Plastic NONE
f
Narrow
I_ C0119855 540 .90 g 4 .70
500 ml Clear Plastic NON E Narrow
C0119856 549 .00 g 4 .40
500 ml Clear Plastic NONE Narrow
C0119857 574 .40 g 9.70 500 ml Clear Plastic NONE Narrow
C0119858 585.80 g 9 .80 500 ml Clear Plastic NON E Narrow
Lot
Mfg . ID
Samples
Sample ID Container Matrix Fraction Sample
L0006767-0001 LIQUID Water FAY-D-4328MLR C0119853 C0119854
Date Sampled
Date Due
11/16/2005 11/27/2005
L0006767-0002 LIQUID Water FAY-D-6999PED 11/16/2005 11/27/2005 C011985 5 C0119856
L0006767-0003 LIQUID Water FAY-K-FBLK-1 11/16/2005 11/27/2005 C0119857
C0119858
0010
11/17/2005 Report Version : Aug 24 2005 3 :47PM Instance : R0209072 Login
.rpt Page 1 of 2 IIIIIII~IIIIIIuIIIIII~~II~III~IIIII~
Login Reviewed By : Date/Time :
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11/17/2005 Repo rt Version : Aug 24 2005 3 :47PM Instance : R0209072 Login .rpt Page 2 of 2 ~~~~~~~~~~~~~ 11111, 11
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ORIGIN ID : FAYA (91o1 67-6ZLTfi46 Ship DaE : 16NOV05' KEN',[ERDBETTER ' Aotuo Wgt : 381 .0 LB MAN ~ E I DtJPONTISIFt SUPPORT -Systemi : 3857901CAFE2264 22828 NC HIGHWAY 87 W , .Account : S 02830017 4
Dimmed : 13x14x24 IN
FAYETTEVILLE : NC 2830 6 UNITED STATES US. . : .', '
roATTN : SAM,E RECEIVING_ (81 O 231-8032
EXYGEGWRESEARCH
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RAW DATA REPORT
Sponsor Study No
Limit of Quantitation (LOQ) : 22.4 ng/I-
Exygen Study No : NA Limit of Detection (LOD) : 4 .47 ng/L Set No: 111805A
Analyte
: L6767 Injection Volume: 15 L Analyst:
Karen Risha
: APFO Ions Monitored: 413 ->
Matrix : Water Instrument Type: LC/MS/MS Unit # 7
369 Sample Volume : 40 .0 mL Extraction Date: 11/18/05
Site: Fayetteville Final Volume :
5 .0 ML Analyzed on: I1/1S/O5
Amount
Std. PFOA APFO PFOA
Oxygen ID
XC110705-0
SpI onsDor Sample Run Conc . - Code 111805A-1001 (n0 )
Dilution Peak Found
Factor
oea (n
Found Added Recovery n ) (n (%)
XC110705- 1
- CS 111805A-1002 5 - 494
XC110705-2 - CS
1 11805A-1003 10 - 826
XC110705-3 - CS 111805A-1004 25 - 2065
XC110705-4 - CS 111805A-1005 50 - 3584
XCI10705-5 - CS
111805A-1006 100 - 7752
XC110705-6 - CS I118 05A-1007 250 - 16331
XC110705-7 - CS 1118 05A-1008 500 - 35308
XC110705-8 - CS 111805A-1009 1000 - 69493
XC110705-9 CK 111805A-1010 250 - 1669 4
Methanol Wash C 111805A-1011 - -
0
Reagent Control NA C 111805A-1012 - 1 73 ND ND
L6 767-3 FAY-K-FBLK-1 S I1180SA-1013 - I 0 ND N
Reagent Spk
D
A Reagent Spk
NA
LCS
111805A-1014
-
1
4065
55 .5 57.8 50
B NA LCS 111805A-1015 - 1 39560 555 578 500
111 Ill
L6767-1 Spk C FAY-D 3328MLR LF 111805A-1016 - 10 41817 5870 6110 5000 117
L6767-2 Spk D FAY-D-6999PED LF 1I1805A-1017 - 10 37432
Methanol Wash - C 111805A-1018 - -
0
5250
5470 5000 105
XC110705-1 CS 11180SA-1019 5 410
XC110705-2 CS 11180SA-1020 10 807
XC110705-3 - CS II1808A-1021 25 - 1937
XC110705-4 - CS 111805A-1022 50 - 381 4
L6767-1 FAY-D-4328MLR S 111805A-1023 - 1 832 9 .95 N Q
L6767- 1 Rep FAY-D-4328MLR S 111805A-1024 - 1 917 11
L6767-2 FAY-13-6999PED S 111805A-1025
. 1 0
.1 NQ - -
ND ND
L6767-2 Rep FAY-D-6999PED S 1118o5A-f026 - 1 0 ND ND -
XC110705-5 - CS 11 1 805A-1027 100 - 7939
XCI10705-6 CS 111805A-1028 250
-
17931
:
XC110705-7 CS 111805A-1029 500 35873
XC1I0705-8 - CS 111805A-1030 1000
-
7290 3
PFOA Found (ng/L) _(peak area - intercept) / slope x DF
Recovery (%) _
[PFOA found (npJL)-PFOA found in control (np,/L))
amount PFOA
APFO Found (ng/L) = PFOA found (ng/L) x (MW APFO
x 100 added (431) / MW
Standard Curve : Linear (1/x weighted) Intercept = 125.839 (ng/L) Slope - 70 .9929 PFOA (414)) Coef . Of Det = 0.998929
CS = Calibration standard LF = Lab fortified sample CK = Check Standard
C= S
Control
sample
FF
=
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sample
ND
=
Not
detected
=
Response
between
0
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LO D
Sample LCS = Laboratory Control Spike NQ = Not quantifiable = Response between LOD and LOQ
Avg Resp. of the 250 ppt Standards (area): 1713 1 Response of the Check Standard (area): 16694 Percent Difference (%) : 3 Spreadsheet % difference acceptable if within 15%
prepared by.
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E~ygeil 3058 Research Drive Phone: 814-272-1039 R E EN F; t, ;-+ State College, PA 16801 Fax : 814-231-1580
Exygen Study Number: Sponsor Study/Protocol No :
Internal Chain of Custody/Fortification Shee t
L6767 NA
Matrix : Water
The samples listed below were removed from refrigerator No .
Time Date Initials Ep,p
CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME mL FORTIFICATION (ng)
na
Regent Control 40 .0 -
na
Reagent Spk A 40 .0 2.0
na
Reagent Spk B 40 .0 20 .0
FAY-D-4328MLR L6767-1 Spk C FAY-D-6999PED L6767-2 Spk D
40.0 40 .0
200 .0 200 .0
FAY-D-4328MLR L6767-1 40 .0 -
FAY-D-4328MLR L6767-1 Rep
40 .0 -
FAY-D-6999PED L6767-2 40.0 _
FAY-D-6999PED L6767-2 Rep
40 .0 _
FAY-K-FBLK-1 L6767-3 40 .0
_
-
-
-
-
-
-
_ _
'
-
-
Spiking Solution Used
Volume Used for Splicing Initial/Dat e
Reagent Spk A F091305-5 (10 ng/mL) 200 L (200 L micro i et) i
Reagent Spk B F091305-4 (100 ng/mL)
200 L (200 L micro pipet)
/
L6767-1 Spk C F091305-3 (1000 ng/mL) 200 L (200 L micro i t) /
L6767-2 Spk D F091305-3 (1000 ng/mL) 200 L (200 L micro i et) /l l
-
-
-
-
All samples were measured: Time /0 : 6,5-,41n
Date / l$ aiaS
Initials
After measuring samples were returned to refrigerator No .
Time ~: a 0 ]~/rl
Date // 14
Initial s
Comments : 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: ) d f~~
Analysis Summary:
Data Set : Data Set : Data Set :
Initials/Date: / Initials/Date : / Initials/Date : - /
Set extraction/analysis data verified by:
0015
Date: ~ July 26, 2001/6 c.v~ ub~/e <
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p . 25
Scanning Method Report Page
Method :
C :\MASSLYNX\00B APFO .PRO\ACQUDB\008 PFOA
Last Modified : Wed Mar 20 15 :07 :50 2002
Printed : Fri Nov 18 13 :17 :55 2005
l0
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Function : 1 MRM of 1 Mass Pair ( ESP-
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0 .00
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1
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1 413 .00 369 .00 0 .20
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10
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0021
p. 26
Method
Report
Page
1
Method File :
c :\masslynx\008 apfo .pro\acqudb\wate r
Last Modified : Friday, November 18, 2005 13 :18 :43
Printed : Friday, November 18, 2005
- - - ---------HP1100 LC Pump Initial Condition s
-
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13 :18 :4 8 ----
-
Solvents As
B% C% D%
60 .0
40 .0 0 .0 0. 0
Flow (ml/min) 0 .300 Stop Time (mins) 15 .0 Min Pressure (bar) 0
Max Pressure (bar) 400
Oven Temperature Left(C) 35 .0 Oven Temperature Right(C) 35 .0
~
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HP1100 LC Pump Gradient Timetabl e
The gradient Timetable contains 10 entries which ar e
Time A% 0 .00 60 .0
0 .40 60 .0
1 .00 7 .00
10 .0 10 .0
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9 .00 0 .0
9 .50 60 .0
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HP1100 LC Pump External Event Timetabl e The Timetable contains 4 entries which ar e
Time Column Switch Contactl Contact2 Contact3
Initial Off Off Off Off
0 .00 0 .10
Off Off
On Off Off On
Off Off
8 .00 Off Off Off Off
Contact4 Off
Off Off Off
HP1100 Autosampler Initial Condition s
Draw Speed
200 .0
Eject Speed (l/min) 200
Draw Position (mm) 0 .10 Stop Time (mins) 15 .00 Injection Volume(Al) 15 .0 Vial Number 9
0022
p . 27
Tuning Method Report
Method :
C :\MASSLYNX\008 APFO .PRO\ACQUDB\PFOA TUN E
Printed : Fri Nov 18 13 :20 :17 2005
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0023
p . 28
enRESEARCH
Precise Research. Proven Results .
In oider to verify mass resolution, a calibration check is performed on the mass spectrometer using a NaIURb/Cs tuning solution . The tuning solution is infused onto the mass spec using an infusion pump set to a flow rate of 10 L/min. An MS scan from 80 to 1380 amu is performed on both MS 1 and MS2 . The calibration is considered acceptable if the following 11 peaks are found within f 0.2 amu of.their known masses on both MS 1 and MS2 : 84.9, 132 .9, 172 .8, 322.7, 472.6,'6.22.5, 772.4, 922 .3, 1072 .2, 1222 .1 and 1372 .0. If any of the masses are outside the 0.2 amu, then the instrument will be recalibrated and another calibration check performed . The printouts from the calibration check c an be found on the following 2 pages .
\\~`07
00 2`~
\30518 Rese arch Drive te College, PA 16801, USA :800.281 .3219 F: 814 .272 .101 9 exygen .com
p . 29
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p . 31
Exygen Study No. : L6767 Set No : 111805A
Extraction Date : 11/18/05 Analyzed on : 11/18/05
Initial Calibration Curv e
The first curve of the data set is used to determine performance. A linear regression (with no weighting) is performed using the first eight standards of the analytical run . The coe ffi cient of determination (R Square) must be 0.985 or greater . If the set fails to meet this requirement, the run must be rejected and the samples reanalyzed .
Standard
Concentration
Exygen ID
(ng/L) Peak Area
XC110705-1 5 494
XC110705-2 10 826
XC110705-3 25 2065
XC110705-4 50 3584
XCI 10705-5 100 7752 Coefficient of Determination : 0 .999502113 XC110705-6 250 1633 1 XC110705-7 500 35308
XC 110705-8 1000 69493
SUMMARY OUTPU T
Regression Statistics
Multiple R 0.999751025 R Square 0 .999502113
Adjusted R Square 0 .999419132
Standard Error 584 .264172
Observations
8
\~\
ANOVA
Regression Residual Total 7
df
SS
MS F
1 4111709682 4111709682
6 2048187 .736 341364.6227
4113757970
Significance F 12044 .92032 3 .85766E-11
Coe~lcients Standard Error I Stat P-value Lower 95% Upper 95% Lower 95 D% Upper 95 0% Intercept 167 .9081974 257.1792017 0 .652884045 0 .538027981 -461 .3870993 797 .2034941 -461 .3870993 797 .2034941 X Variable 1 69.33491465 0.631756937 109.7493523 3 .85766E-11 67.78905998 70 .88076932 67.78905998 70 .88076932
0027
p . 32
LOD and LOQ Determinatio n
Exygen Study No. : L6767 Set No : 111805A
Extraction Date: 11/18/05 Analyzed on : 11/18/05
The height of the first 5 ng/L standard of the analytical run is measured in centimeters and recorded . The height of the noise in a one minute range before the PFOA retention time in the reagent control is measured in centimeters and recorded. The noise height is then divided by the standard height . The result is converted to to ng/L by multiplying by the concentration of the standard measured (5 ng/L) . The LOD is calculated by taking 3 times the signal to noise ratio in ng/L . The LOQ is calculated by taking 5 times the LOD .
Concentration Height Exygen ID (ng/L) (cm) xC 110705-1 5 15 . 1 Reagent Control 0 4 . 5
Signal to Noise Ratio = [height of the noise in the reagent control (cm) / height of the 5 ng/L standard(cm)] x 5 ng/mL
Signal to Noise Ratio (ng/L) = 1 .490 ng/L LOD = 4.47 ng/L LOQ = 22 .4 ng/L
0028A
p . 33
XC110705-1, 5 ng/L standard 18-Nov-2005 13 :50 :5 8
LC/MS/MS #7 111805A-1002 Sm (Mn, 2x3) MRM of 1 Channel ES-
10
5 .33 413 > 36 9 1 .06e4
5 .19
4 4 .82
4 .3 7 0.95 1 .01 .27 0 1 .2 74.343 20 3 .44 4.13 0.37 2.61
5 .82 6.17 6 .40
6.59 7.23
7 .0 7 .74
Time 1 .00 2.00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .0 0
00288
p. 34
Reagent Control
18-Nov-2005 16:37:4
LC/MS/MS #7 111805A-1012 Sm (Mn, 2x3) MRM of 1 Channel ES-
10
413
>
36 9 1 .06e4
%
5.71 5 .93 6.20
5.44 6 .83
5 .34 (6.s8 7.107.49
5 .07 7 .76
4 .8
7 .85
~{',~j
4 .70
0.64 0.91
. 8
.15 1
.36 3.62 4.22 4
0.37 1
.82 2'98 3
fUlYl
7 .91
1 .00
2 .00
3 .00
4 .00
5 .00
6 .00
7 .00
1Time 8 .00
0028C
p . 35
Quantify Calibration Report Page 1 Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Rish a
Calibration : P :\Data\LCMSMS7\Masslynx\008 APFO .PRO\CurveDB\111805A Last modified : Mon Nov 21 06 :36 :43 200 5 Printed : Mon Nov 21 06 :44 :55 2005
Compound 1 name : PFO A
Coefficient of Determination : 0 .998929 Calibration curve : 70 .9929 * x + 125 .839 Response type : External Std, Are a Curve type : Linear, O ri gin : Exclude, Weighting : 1/x, Axis trans : None
7 .29e4
x
X
Respons
x
0 .0
200 .0
400 .0
600 .0
ng/L 800 .0 1000 .0
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0029
p . 36
Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :ll/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 APFO .PRO\SampleDB\111805A Last modified : Mon Nov 21 06 :36 :20 200 5
Method : P :\Data\LCMSMS7\Masslynx\008 APFO .PRO\MethDB\112204 PFOA Last modified : Wed Dec 01 06 :25 :13 200 4
Job Code :
Initials
Date Printed : Mon Nov 21 06 :44 :55 2005 Run# To 1
1
Name : 111805A-100 1 Text :
1 : PFOA
XC110705-0, 0 ng/L standard 18-Nov-2005 13 :34:17
LC/MS/MS #7 111805A-1001 Sm (Mn, 2x2) MRM of I Channel ES-
10
5 5 .16 . 4575 6 .117 .14 8 1 7.63 5 5>.1336e39
q/
0.570 .68
1 .96 2 .91 3 .9 4 .39 4 .68
1 .00
2 .00
3 .00
4 .00
5 .00
6 .00
7 .00
Time 8 .0 0
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0030
p . 37
Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Sxt .Date :11/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMS14S7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
2
Name : 111805A-100 2 Text :
1 : PFO A
XC110705-1, 5 ng/L standard 18-Nov-2005 13 :50 :5 LC/MS/MS #7
111805A-1002 Sm (M n, 2x2) MRM of 1 Channel ES-
10
5 .33 413 >369
494
1 .12e4
Area
1 .00
2 .00
3 .00
4 .00
5 .00
6 .00
7 .00
.00 Time 8
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0 031
p . 38
Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :l1/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
3
Name : 111805A-100 3 Text :
1 : PFOA
XC110705-2, 10 ng/L standard 18-Nov-2005 14 :07:3 LC/MS/MS #7
111805A-1003 Sm (M n, 2x2) MRM of 1 Channel ES-
10
5.35 413 $26
>36 9 1 .31e4
Area
Tim e 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0032
p . 39
Quantify Sample
Report
Page
Study No . :L6767, Set No . :111805A, Ext . Date : l1/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
4
Name : 111805A-100 4 Text :
1 : PFOA
XC110705-3, 25 ng/L standard 18-Nov-2005 14:24:1 LC/MS/MS #7
11 11805A-1 0 004 Sm (Mn, E 2x2) MRM S of 1 Channe- l ES5 .35 413> 369 2065 3 .26e4 Are a
1 .00
2 .00
3 .00
4 .00
5 .00
6 .00
7 .00
Time 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0033
p . 40
Quantify Sample
Report
Page
Study No . :L6767, Set No . :111805A, Ext .Date :l1/18/05, Analyst :K .Risha
Sample List :
P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5
Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4
Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
5
Name : 111805A-100 5 Text :
1 : PFOA
XC110705-4, 50 ng/L standard 18-Nov-2005 14:40:5
LC/MS/MS # 11 1805A-1005 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
5 .34 413 >36 9 3584 5.54e4 Area
%
1 .00
2 .00
3 .00
4 .00
5 .00
6 .00
7 .00
Time 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0034
p . 41
Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Risha
Sample List :
P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5
Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4
Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
6
Name : 111805A-100 6 Text :
1 : PFOA
XC110705-5, 100 ng/L
111805A-1006 Sm 10
standard 18-Nov-2005 14:57:29
LCIMS/MS # (Mn, 2x2) MRM of 1 Channel ES-
5 .33 413 >36 9 7752 1 .20e5
Area
Tim e 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0035
p . 42
Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
7
Name : 111805A-100 7 Text :
1 : PFOA
XC110705-6, 250 ng/L standard 18-Nov-2005 15 :14 :0
LC/MS/MS #7
111805A-1007 Sm (Mn, 2x2) MRM of 1 Channel ES-
100-
5.34 413 >369
16331 2 .48e5
Area
%
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .0 0
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0 036
p . 43
Quantify Sample Study No . :L6767, Set No . :111805A,
Report
Page
Ext .Date :11/18/05, Analyst :K .Rish a
Sample List :
P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5
Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
8
Name : 111805A-100 8 Text :
1 : PFOA
XC110705-7, 500 ng/L standard 18-Nov-2005 15 :30 :5 LC/MS/MS #7
111805A-1008 Sm (Mn, 2x2) MRM of 1 Channel ES-
10 %
5 .34 413 >36 9 35308 5 .30e5
Area
1 .00
2 .00
3 .00
4 .00
5 .00
6 .00
7 .00
Tim e 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0037
p . 44
Quantify Sample Report Study No . :L6767, Set No . :111805A, Ext .Date :ll/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
Page 9
Name : 111805A-100 9 Text :
1 : PFO A
XC110705-8, 1000
111805A-1009 Sm (M n, 2x2) 10
ng/L standard 18-Nov-2005 15:47:40
LC/MS/MS #7 MRM of 1 Channel ES-
5 .33 413 >36 9 69493 1 .06e6 Area
%
nII I'll . . . 1-11111111
Time
1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
o 03 8
p . 45
-
--
-
Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date : 1 1/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
10
Name : 111805A-101 0 Text :
1 : PFOA
XC110705-9, 250 ng/L check standard 18-Nov-2005 16 :04:21
LC/MS/MS #7 111805A-1010 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
535 413 >36 9
16694 2 .48e5
Area
%
1 .00 2 .00 3 .00 4 .00 5 .00 6 .00
Time 7.00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
~039
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Quantify Sample Report Page Study No . :L6767, Set No . : 111805A, Ext . Date : ll/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
11
Printed : Mon Nov 21 06 :44 :55 2005
Name : 111805A-101 1 Text :
1 : PFO A
Methanol Wash 18-Nov-2005 16 :21 :0
LC/MS/MS #7 111805A-1011 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
5.10 5.645 .75 6 .306 .39 6 .97 413 >369 7.67 4.76e3
a 0 .440-/ 64 0o .89 1 .32 1 .62 7 2 .7.91 6 3 .74 2 .27 4 .80 7.93
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0040
p . 47
Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :l1/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
12
Name : 111805A-101 2 Text :
1 : PFO A
Reagent Control
18-Nov-2005 16 :37 :
111805A-1012 10
%
Sm (Mn, ~
2x2) ~~~t~~~3 ~O MRM 1'21'05 413
cl~w F ((12J
LC/MS/MS #7 of 1 Channel ES>36 9
4 .90e3
Area
I
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .0 0
plb~ltl~s w~re.fi~r ~~ed -~a~-~.1~45~1v,w~ ~-twute . %I\ 1z+ Ia5
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0041
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
13
Name : 111805A-101 3 Text :
1 : PFOA
L6767-3 18-Nov-2005 16 :54:17
LC/MS/MS #7
111805A-1013 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
5.68 6.046.24 6 .66 413 >36 9
525 7 44 5.05e3
4 .89 7 .95
%1. 0 .820.91 1 .03 1 .98 2 .29 2 .70 2.96 4 .26 4.42
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, state college, PA 1680 1
0042
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Report
Page
Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
14
Name : 111805A-1014 Text :
1 : PFO A
Reagent Spk A, 50 ng/L 18-Nov-2005 17 :10:57
LC/MS/MS #7
111805A-1014 Sm (Mn, 2x2) MRM of 1 Channel ES-
100~
5 .36 413 >36 9 4065 6 .28e4
Area
Tim e 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0043
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Quantify Sample Study No . :L6767, Set No . :111805A,
Report
Page
Ext .Date : 1 l/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified ; Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
15
Name : 111805A-101 5 Text :
1 : PFOA
Reagent Spk B, 500 ng/L 18-Nov-2005 17:27:3
LC/MS/MS #7
11 1805A-1015 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
5 .35 413>36 9 39560 5.62e5
Area
%
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .0 0
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0044
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :l1/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
16
Name : 111805A-101 6 Text :
1 : PFO A
L6767-1 Spk C, 5000 ng/L, DF=10 18-Nov-2005 17 :44 :19
LC/MS/MS #7
111805A-1016 Sm (Mn, 2x2) MRM of 1 Channel ES-
5 .36
413> 369
10
41817
6 .28e5
Area
nI .
Time
1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0045
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :R .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
17
Name : 111805A-101 7 Text :
1 : PFO A
L6767-2 Spk D, 5000 ng/L, DF=10 18-Nov-2005 18 :01 :11
111805A-1017 Sm 10
LC/MS/MS #7
(Mn, 2x2) MRM of 1 Channel ES5 .35 413 >369 37432 5 .51 e5 Area
Tim e 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0046
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
18
Name : 111805A-101 8 Text :
1 : PFO A
Methanol Wash 111805A-1018 Sm (Mn, 10
0 .67
18-Nov-2005 18 :17 :5
LCIMS/MS #7 2x2) MRM of 1 Channel ES-
.74 5.88 5 .98 6.42 6.98 413 >36 9 5.35 '42 7.42 5.03e3 4.88 7.95
Time 1 .00 2 .00 3 .00 4.00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0047
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
19
Name : 111805A-101 9 Text :
1 : PFO A
XC110705-1, 5 ng/L standard 18-Nov-2005 18 :34 :42
LC/MS/MS #
111805A-1019 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
5.35 413 >36 9
410 9 .94e3
Area
Tim e 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0048
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Report
Page
Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Risha
Sample List :
P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5
Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4
Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
20
Name : 111805A-102 0 Text :
1 : PFO A
XC110705-2, 10 ng/L standard 18-Nov-2005 18 :51 :21
LC/MS/MS #7
111805A-1020 Sm (M n, 2x2) MRM of 1 Channel ES-
10
5.34 413>36 9 807 1 .43e4
Area
Tim e 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0049
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
21
Name : 111805A-102 1 Text :
1 : PFOA
XC110705-3, 25 ng/L standard 18-Nov-2005 19 :08 :04
LC/MSIMS #7
111805A-1021 Sm (Mn, 2x2) MRM of 1 Channel ES-
100- 413 >369
10
1937
3 .42e4
Area
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8.0 0
Exygen Research, 3058 Research Drive, State College, PA 1680 1
005 0
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Report
Page
Study No' . :L6767, Set No . :111805A, Ext .Date :ll/18/05, Analyst :R .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
22
Name : 111805A-102 2 Text :
{ 1 : PFOA
XC110705-4, 50 ng/L standard 18-Nov-2005 19 :24:47
111805A-1022 Sm 10
LCIMS/MS #7
(Mn, 2x2) MRM of 1 Channel ES5 .33 413 >36 9 3814 5 .91e4 Area
Tim e 1 .00 2 .00 3 .00 4.00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Res e arch Drive, State College, PA 1680 1
0 01 5 1
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :ll/18/05, Analyst :R .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
23
Name : 111805A-102 3 Text :
1 : PFOA
L6767-1 18-Nov-2005 19:41 :24
LC/MSIMS #7
111805A-1023 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
5 .36 413 >369 832 1 .69e4
Area
%
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8.0 0
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0052
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :l1/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
24
Name : 111805A-102 4 Text :
1 : .PFO A
L6767-1 Rep 18-Nov-2005 19 :58 :07
LCIMS/MS #7
11 1805A-1024 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
5 .38 413 >36 9
917 1 .69e4
Area
%
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, Stas~te College, PA 1680 1
0 05J
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Quantify Sample
Report
Page
Study No . :L6767, Set No . :111805A, Ext .Date :ll/18/05, Analyst :K .Risha
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
25
Name : 111805A-102 5 Text :
1 : PFO A
L6767-2 18-Nov-2005 20 :14:49
LC/MS/MS #
111805A-1025 Sm (Mn, 2x2) MRM of 1 Channel ES-
10
5 .5 5,77 6 .196 28 6.88 413 >36 9
5.11 7.15 5 .49e3
% % 0 .1 100 .. 7 88 944 .0244 4.52
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 1680 1
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Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :11/18/05, Analyst :R .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
26
Name : 111805A-102 6 Text :
1 : PFOA
L6767-2 Rep 18-Nov-2005 20 :31 :27
LC/MS/MS #7
111805A-1026 Sm (M n, 2x2) MRM of 1 Channel ES-
10
5.62 5.88 6 .16 6 89 413> 36 9
.99 6.99 7 .41 7
0.11 0 .81 1 .19 1 .66 3 .23 4.28 4 .88 4
.98e3
% I'll
1-111
Time
1 .00 2 .00 3 .00 4.00 5 .00 6 .00 7 .00 8 .00
I ~-
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0055
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Page
Study No . :L6767, Set No . :111805A, Ext .Date :ll/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
27
Name : 111805A-102 7 Text :
1 : PFOA
XC110705-5, 100 ng/L
111805A-1027 Sm 10
standard 18-Nov-2005 20 :48 :1 LC/MS/MS #7
(Mn, 2x2) MRM of 1 Channel ES.35 413 >369
57939 1 .23e5 Area
Tim e 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
~
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0056
p . 63
Quantify Sample Report Study No . :L6767, Set No . :111805A, Sxt .Date :11/18/05,
Analyst :X .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008 Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
Page 28
Name : 111805A-102 8 Text :
1 : PFO A
XC110705-6, 250 ng/L standard 18-Nov-2005 21 :04:52
LC/MS/MS # 111805A-1028 Sm (M n, 2x2) MRM of 1 Channel ES-
10
5.34 413 >36 9 17931 2.61 e5
Area
%
Time 1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .0 0
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0057
p . 64
Quantify Sample Report Page Study No . :L6767, Set No . :111805A, Ext .Date :ll/18/05, Analyst :K .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008
Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
29
Name : 111805A-102 9 Text :
1 : PFOA
XC110705-7, 500 ng/L standard 18-Nov-2005 21 :21 :39
LC/MS/MS #7 111805A-1029 Sm (M n, 2x2) MRM of 1 Channel ES-
10
5 .34 413 >36 9 35873 5 .32e5
Area
%
0
Time
1 .00 2 .00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
r
Exygen Research, 3058 Research Drive, State College, PA 1680 1
0058
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Report
Page
Study No . :L6767, Set No . :111805A, Ext .Date :l 1 /18/05, Analyst :R .Rish a
Sample List : P :\Data\LCMSMS7\Masslynx\008 Last modified : Mon Nov 21 06 :36 :20 200 5 Method : P :\Data\LCMSMS7\Masslynx\008
Last modified : Wed Dec 01 06 :25 :13 200 4 Job Code :
APFO .PRO\SampleDB\111805A APFO .PRO\MethDB\112204 PFOA
Printed : Mon Nov 21 06 :44 :55 2005
30
Name : 111805A-103 0 Text :
1 : PFO A
XC110705-8, 1000 ng/L standard 18-Nov-2005 21 :38 :22 LC/MS/MS #7
111805A-1030 Sm (Mn, 2x2) MRM of 1 Channel ES5 ..3 535 413 > 369 72903 1 .07e6 Area
%
UI)
Time
1 .00 2.00 3 .00 4 .00 5 .00 6 .00 7 .00 8 .00
Exygen Research, 3058 Research Drive, State College, PA 16801
p . 66 f
p . 67
en~RESEARCH
Precise Research . Proven Results .
The following pages are exact copies of information for the standards used in this study .
Pentadecafluorooctanoic acid (Inventory # : SP3800), obtained from Aldrich (lot # 23116HB) was used to make a stock solution (ID # S061605-1), which in turn, was used to make intermediate solutions (ID#'s F091305-1, F091305-2, F091305-3, F091305-4 and F091305-5) . These intermediate solutions are used to prepare extracted calibration standards, laboratory control samples, and matrix spike samples .
Pentadecafluorooctanoic Acid (Inventory # : SP5444), obtained from Oakwood Products Inc., Fluorochem USA (lot # 203) was used to make a stock solution (ID # S040505-1), which in turn, was used to make intermediate solutions (ID#'s F091305-6 and F091305-7) . These intermediate solutions are used to prepare the check standard, which is designed as an independent source verification of the calibration standards .
The information on the following pages provides the exact sources, lot numbers, shipping information, expiration dates and storage conditions of the neat standards . Also included are the preparation of stock standard and fortification solution forms . These pages show the exact details of the preparation of each of the stock and fortification solutions, as well ~ as their expiration dates and storage conditions .
0060
3058 Research Drive State College, PA 16801, USA
T: 800.281 .321 9 F: 814 .272 .1019 exygen .com
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1 ALLENTOWN, PA 18106
00 3 610-391-9'I 07 - y =
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EXYGEN RESEARCH
KAREN
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3048 RESEARCH D R
STATE COLLEGE PA
REFN e14938862
16801
ORIGIN SHIPMENT NO .
SHIP DATE
ABE 46275411462 12/05/200 3
pi IIIIaII~IIIINI~IIIIIIi~~II~IIIIIIIIIIi~l l l l l l l IIII I ~ ADDITIONAL INFORMATION
81493086 4 0 31 K R 1
Track 0 :48275417462
PHONE :
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11-5165
Dooument r81493e8e2
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SIGMA-ALDRICH
Cer t ifleat eofAn alysi s
Product Name Product Number CAS Number Molecular Formula Molecular Weight
Pentadecafluorooctanoic aci d
17,146-8 335-67-1
C8HF1S02 414 . 1
TEST SPECIFICATION LOT 2311 RE6 SUH LTS B
APPEARANCE
WHITE TO OFF-WHITE POWDER WHITE CRYSTALLIN E POWDER
INFRARED SPECTRUM
CONFORMS TO STRUCTURE AND STANDARD AS ILLUSTRATED CONFORMS TO ON PAGE 507B OF EDITION I, VOLUME 1 OF THE ALDRICH STRUCTURE AN D LIBRARY OF FT-IR SPECTRA' . STANDARD
TITRATION 95 .5% :- 104 .5% (WITH NAOH) 101 .1% (WITH NAOH)
GAS LIQUID CHROMATOGRAPH Y
95 .5% (MINIMUM) 97 .7%
TITRATION
QUALITY CONTRO L ACCEPTANCE DATE
2%
H20
(MAXIMUM)
H2 FIS0 C ER''K REAA G ENR T) L JUNE, 2003
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Ronnie J Marti; Supervisor Quality Control
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SP 3800
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RESEARC H
3058 Research Drive State College, PA 16801
Phone : 814-272-1039 Fax : 814-231-1580
Protocol No . :
-"
Exygen Study No :
STUDY TELEPHONE/COMMUIVICATIONS<LO G
Page I of ~
Person :
Ken
Company : Aldrich
-
Originator. Exygen
x
Sponsor
Date : 12/08/03
Time: 1022
Notes :
I called Aldrich tech service at 1-800-231-8327 to ask the shelf life of the PFOA standard I received today . Ken, an Aldrich rep in technical service, told me that the shelf life i s 2 years from the date of receipt stored at room temperature .
Signature :
--- - w Date :
0066 August 7, 2001/1
p . 74
n 3058 Research D rive Phone : 814-272-1039 State College, PA 16801 Fax : 814-231-1580 RESEARC H
PREPARATION OF STOCK STANDARD SOLUTION
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Exygen Study / Project Number. Customer Project Number.
Prima t . :Standard Compound Name: Exygen Invento ry ID :
Purity:
a i o SPoo0 3 00 Primary Standard Expira tion Date :
%
1 os os
Stock S'ol'ution' P~re. aratlo:nr =: ~ :> .
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Net Wt of Compound :
t ~ 2~2 Net Wt. Adjusted for Purity:
OC DD
Final Volume: Stock Solution Concentration :
JC)D mL
100 mL
Solvent Exygen Inventory ID : Solvent Name:
REnniq 3
Stock Soluti on ID : Stock Solu tion Expirati on Date:
(SMMDDYY-1,2,3, eta) 5 i DS -`
Storage Cond~tiorx and C'o'catio~ ::;:::.
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12.1 DI) [7 5
Freezer ID:
^
Refri gerator ID: 33
Room Temperature : --
Walkin Freezer ID : -
Welkin Cooler ID:
-
Storage Cabinet -
(Enter the Instrument or Room ID under the appropriate condition)
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Date :
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LIBRARY ID : V0000986-5 LABORATORY FOR M
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Oakwood Products, Inc
741 Old Dun bar Road
W e s't;.Golumbia, SC 299 72 Phane(303 )739-8840 Fax(.003)739-69 57
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CERTIFICATE OF ANALYSI S
.
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Date :
, 3-31-U5
.
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Material.
Pentadttafluoraactsaoic acitt
Cat. Na : 1319
Cas No . : (335-67-11
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Assay : 9 9+%'o by N a O H TBtrativn
Appeatsnce : Colorless, low-malting so lid
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%Ve have out prrformed a staAdardrixcd bil,ili4y test on 64 to mpoood. We k ave scored this compound at room temperature In a tightly scaled container for m2ny
p mn and not aooticed any i n effects.
Ytmti Yang QC Manage r
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F U cNE OAKWOOD PRODUCTS, INC . L CRO M USA 1741 OLD DUNBAR ROA D
WEST COLUMBIA . Sc 29172 Phone : 803-739-8800 FAX : 803-739-6957
p . 77
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3 =17 Research Drive Sta-no cd__eqc, PA 16301 st ;~::e College, PA 16301 l31.4 ', 231-8+732 8^_4 ; 231-903 2 page 1
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3058 Research Drive Phone : 814-272-1039
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State College, PA 16801 Fax : 814-231-1580
RESEARC H
PREPARATION OF STOCK STANDARD SOLUTION
P:ro'e'ct
Exygen Study T Project Number. NA
Customer Project Number.
Primary Standard .'
:
Compound Name :
Exygen Inventory ID :
?txtto~uo+-oocd-oano 1C.Nd FFoA~
SPCO0I-9444
Purity: Primary Standard Expiration Date:
`19 %
0313110 1
Stock Sofution .Pre; aration:
Net Wt. of Compound: Net Wt. Adjusted for Purity :
0OlOl 1
O .OtOol
Final Volume: Stock Solution Concentration:
100
mL
1 DD /mL
Solvent Exygen Inventory ~ 1
Solvent Name:
I
2015
f4d-Ioom
Stock Solution ID : Stock Solu tion Expiration Dat :
(SMMDDYY- 1 ,2,3, etc.) S040605 - I ~ 05 D~
Storage Condition and : Locatio n
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...
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Freezer ID: Walkin Freezer ID :
Remarks .
Refrigerator ID : 33
Room Temperature :
-
Walkin Cooler ID : -
Storage Cabinet:
-
(Enter the Instrument or Room ID under the appropriate condition)
source,
s C)akyqcoa -pad ucf5 - CEE oil 57106
Signature :
~~,~~- ,~ F vn~~n ,
LIBRARY ID : V0000986-5
0072
Date : p- ~ LABORATORY FOR M
p . 80
3058 Research Drive Phone : 814-272-103 9
E''geri State Cotlege, PA 16801 Fax : 814-231-1580
RESEARCH ~ PREPARATION OF FORTIFICATION STANDARD SOLUTIONS
Pro'ec t Exygen Study / Project Number. Customer Project Number.
fortifica.tion Solution Preparativn .
IaOS 1oS2 o5 ; !f 2`or:rinore inifia/solutfo~~ns are.zoiribcieif"fndbate .th~combined :solutions<vith a.bracket "
Date Prepared : Fortification Solution Expiration Date:
Solvent Exygen Inventory ID : Solvent Name :
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. ID Compound CIniotianl cSoln . F InAiltiian l Sa olnl. Soln . Final Soln.
Initial Soln
Description
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mL ( mL) (pglmL)
Final Soln . ID (FMMDDYY .1,2,3,
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Freezer ID :
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Refrigerator ID : ' 33
Room Temperature : --
Walkin Freezer ID : -
Walkin Cooler ID : --
Storage Cabinet -
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Reriiarks:
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:, .
G)SWRCZ aF Pfok V5 6AtFLMNb, Mb.k-TS . 0111 2>w
Signature: Cl.~ Date :
L
LIBRARY ID : V0000987-4
0073
LABORATORY FORM