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Proven Results.
M 3.8.6 - I 7/3
Analytical Report
Fiuorochemical Characterization of W ater Sam ples
Daikin America, Inc. Exygen Research Laboratory Report No. L0001714
Testing Laboratory Exygen Research
. 3058 Research Drive State College, PA 16801
Requester Neal Waddell Daikin America, Inc. PO Box 2252 Decatur, AL 35609
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800.281.3219 F: 814.272.1019
exygen.com O M I
1 Introduction
Results are reported for the analysis of water samples received by Exygen Research (Exygen) from Daikin America. The Exygen study number assigned to the project is L0001714.
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 samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals:
Table 1: Target Analysis
Compound Name Perfluorooctanoic Acid
Acronym C8 Acid (PFOA)
The analytical methods used were originally developed for groundwater samples and were validated by Exygen. The validation protocol and results are on file with Exygen.
2 Sample Receipt
The samples were submitted in plastic containers. All samples were cooled to 4C from time of collection to receipt at Exygen Research. Samples were stored at 4C from receipt at Exygen Research until analysis. Samples were collected on 1/24/04. Chain-of-custody information is presented in Attachment C.
j \ ' Holding Times
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.
Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 30 days of receipt.
4 Methods - Analytical and Preparatory
4.1 LC/M S/M S 4.1.1 Sample Preparation for LC/MS/MS Analysis
Samples were initially treated with 200 uL of 250 mg/L 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 used for analysis. The samples were transferred to a C18 SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatment resulted in an eight-fold concentration of the diluted samples prior to analysis.
PAGE2 OF5
000481 c \
r 4.1.2 Sample Analysis by LC/MS/MS
t In 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, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of
I i known fluorochemicals are observed and quantitated against standards.
A Hewlett-Packard HP1100 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 on 2/3/04 and analyzed on 2/9/04. Raw analytical data is provided in Attachment D.
b 5 Analysis
I ! 5.1 C alibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence
r for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/MS/MS analysis. 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 >0.985 (r2> 0.970).
Calibration standards are prepared using the same SPE procedure used for samples.
v)\T***' Calibration check standards were analyzed periodically (every three to five sample injections)
IL J throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value.
All calibration criteria were met for this analysis.
5.2 Blanks 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 concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant.
If
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 low-level calibration standard. For the 4:. samples presented here the instrument blanks are compliant.
t
5.3 Surrogates ft Surrogate spikes are not a component of the LC/MS/MS analytical methods.
5.4 Matrix Spikes m A matrix spike was prepared for sample DSN002. Matrix spike recoveries are given in 4. Uk Attachment B.
ft'
PAGE3 OF5
000482
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5.5 Duplicates Sample DSN002 was analyzed in duplicate. The duplicate results are included with the
i sample results in Attachment A.
5.6 Laboratory Control Sam ples
For LC/MS/MS analyses, Milliq water was spiked with all compounds with each extraction set.
All recoveries for all compounds were between 70-130% in each LCS. Results are given along with the raw data in Attachment D. V1
* * 6 Data Summary
^
Please see Attachment A for a detailed listing of the analytical results. Results are reported in
pmmt units of parts per billion (ppb) (ug/L).
{"
y - Data/Sample Retention
H1
\ / 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 i < folders maintained by Exygen.
r 8 Attachments
l) i 8.1 Attachment A: Results
<H?lh:', 8.2 Attachment B: Matrix Spike Recoveries
8.3 Attachment C: Chain of Custody !;
8.4 Attachment D: Raw Analytical Data
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PAGE4 OF5
000483
Other Lab Members Contributing to Data Karen Risha
PAGE50F5
000484
Report 1
Sum m ary of PFOA in W ater Sam ples
Analyte Found (|jg/L)
Sample ID______________________ PFOA
n DSN002
56.2
u DSN002*
55.6
DSN003
244
i(
DSN004
67.2
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Laboratory Duplicate
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exygen.com
STANDARD TERMS AND CONDITIONS
Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract.
CONFIDENTIALITY-- Ixygtn Research ("Exygen," "us," or " we")
maintains the strictest confidentiality in a!! of our client interactions, if a
signed confidentiality agreement is required, we will provide one. If a
regulatory or legal body subpoenas information, the client will be notified
promptly. The client agrees not to use Exygen's name and/or data in any
manner that might cause harm to Exygen's reputation or business.
Approval must be obtained, in writing, before Exygen's name can be
published in any way.
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CONTRACTS--All contracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer.
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INDEMNIFICATION, LIABILITY, AND INSURANCE-- xEygen agrees to indemnify, defend, and save the client, its officers, directors, employees, agents, and representatives harmless from all losses, expenses, demands, and claims made against the client, its officers, directors, employees, agents and representatives because of any personal injuries, death, or propertydamage to the extent caused by the negligence or willful misconduct of Exygen. its employees, agents, or representatives in connection with the performance of services under this agreement, except to the extent such losses, expenses, demands, or claims. o c o f as a result of the negligent or willful acts or omissions of the client, its officers, directors, employees, agents, and representatives; however, such indemnification and damages shall, in the aggregate, be limited to the amount equal to the lesser of (a) damages suffered by the client as the direct result thereof, or (b) the total amount paid to Exygen for the work herein covered. Exygen will, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate Insurance coverage.
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ACCEPTANCE OF PURCHASE ORDER-- This Purchase Order becomes a
binding agreement, subject to the specific terms and conditions stated
herein, upon Exygen's commencement of work.
^
000486
Proven Results.
Recovery Sum m ary for PFOA in W ater
PFOA
HH1;
Sam ple
Amount Amt Found Am ount Spiked in Sam ple R ecovered R ecovery
D e scription
(Mg/L)
(ug/L)
(Mg/L)
(%)
n DSN002
*i
500 ng/L Spike
500 56.2 501 89
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mw 3058 Research Drive State College, PA 16801, USA T: 800.281.3219
i m F: 814.272.1019 exygen.com
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
; Company Name: Daikin America
Submitted By: Neal Waddell and Randy Roussel
rn Login Type:
Immediate Receipt o f Samples
Started:
T
Date Start:
01/28/2004
Due Date:
02/11/2004
p Received Date: 01/27/2004
? Received By:
AMMERMAN, MARK
Spread Sample:
*, Label:
I Project Title/Type: Analysis of PFOA in W ater / ROUTINE
Exygen SD/PI: RISHA, KAREN
Login Notes:
f"! Conform Notes:
Conform COC: Conform Sample: Conform Request:
Packages / Containers
r e package Ifcf- i ' . 'K0002305
m r Container # ' C0018564
C0018617
` C0018620
Carton
Mail Date / Condition
1/27/2004 3:30:06PM Package & Contents Uncompromised
Gross Weight pH
Container Type
604.6 g 616.3 g 615.6 g
500 mi Clear Plastic Narrow
500 ml Clear Plastic Narrow
500 ml Clear Plastic Narrow
Shipper /_ID FEDEX
8402386192820215
Preservative NONE
NONE
NONE
Temp. Control/Temp. W et Ice 0.4
Mfg. Lot 3232010
3232010
3232010
Direction / Handled By RECEIVED
AMMERMAN, MARK
Mfg. ID 471374
471606
471609
, Sample ID L0001714-0001 ; L0001714-0002 L0001714-0003
Matrix LIQUID
LIQUID LIQUID
Fraction Water
Water
Water
Sample DSN002 DSN003 DSN004
S am p les
Date Sampled Date Received 01/24/2004 01/27/2004 01/24/2004 01/27/2004 01/24/2004 01/27/2004
Date Due 02/11/2004 02/11/2004 02/11/2004
j p 1/28/2004 ?! Login.rpt
Report Version: Jan 28 2004 10:19AM Page 1 of 2
000488
Instance:
R0082454
R0082454
H)001714-0001 Container
C0018620 / 500 ml Clear Plastic Narrow / NONE
L0001714-0002 n Container
| ]C0018617 / 500 ml Clear Plastic Narrow / NONE
|*p001714-0003 ri t ! Container
1 CO018564 / 500 ml Clear Plastic Narrow / NONE
r~
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Bottles Method Method Method
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Report Version: Jan 28 2004 10:19AM Page 2 of 2
000489
R0082454
0Q0490
PROJECT INFORMATION Client (name & address):
CHAIN OF CUSTODY/ANALYSIS REQUEST FORM
Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com
Page / o f 7
ANALYSES REQUESTED
Project Manager (Name & E-mail Address):
______ A z a / c ttJ - a e jt__________________________
Phone: Fax:
Sampler: A */ijk / T a^/^r
Project Name:
_________ Sds___________________________
P 7#:
7
Quotation # :
Please fill out this form com pletely to ensure correct analysis and proper handling of your samples.
SAMPLE ANALYSIS
ExyLtMS# Client Sample Identification SA/QOZ
Collection Collection
D ate
Tim e
2 VMS'
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Comments
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LAB USE ONLY
CHAIN OF CUSTODY
Relinquished by _ -,
Date
z z i- o /
Time O<?oi)
Cooler ID #
Receiy/d/V
r u t - -------------
OTHER INFORMATION
LAB USE ONLY
L . - L- I -** L... CL.*. C-a. L.,.*.-- L*-. t. - L
f~ Cooler Temp. (C) ),y
Date
o fI / l l k l1
Time
Ifh
PROJECT REQUIREMENTS Results Deadline:
Laboratory Report Options: I | Sample results only 0 Add case narrative Add quality control summary 1 I Add calibration summary
D Add raw data
E ] O ther_________________
L --. CL.j ( ,, * . L,... L -. L*...
3-<L
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RESEARCH
Precise Research. Proven Results.
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Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site:
NA L1714 PFOA 413 -> 369 NA
RAW DATA REPORT
Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume:
50 ng/L 15 pL Water 40.0 mL 5.0 mL
Set No: Analyst: Instrument Type: Extraction Date: Analyzed on:
020304D Karen Risha LC/MS/MS Unit # 7 02/03/04 02/09/04
Exygen ID
XC012804-0 XC012804-1 XC012804-2 X C 0 12804-3 X C 0 12804-4 XC012804-5 XC012804-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spk B L1714-1 SpkC X C 0 12804-1 X C 0 12804-2 XC012804-3
L 1714-1 L1714-1 Rep
L1714-2 L1714-3 XC012804-4 XC012804-5 X C 0 12804-6
Sponsor ID -
-
-
-
-
-
NA NA NA DSN002
DSN002 DSN002 DSN003 DSN004 -
-
Sample Code
c CS CS CS CS CS CS c c LCS LCS LF CS CS CS
s s s s
CS CS CS
Run No. 020304D-1001 020304D-1002 020304D-1003 020304D-1004 020304D-1005 020304D-1006 020304D-1007 020304D-1008 020304D-1009 020304D-1010 020304D-1011 020304D-1012 020304D-1013 020304D-1014 020304D-1015 020304D-1016 020304D-1017 020304D-1018 020304D-1019 020304D-1020 020304D-1021 020304D-1022
PFOA Found (ng/L) = (peak area - intercept) / slope x DF
Recovery (% ) =
[PFOA found (ng/L)-PFOA found in control (ng/L)]
amount PFOA added (ng/L)
Std. Cone. (ug/L)
0 25 50 100 250 500 1000
-
25 50 100 250 500 1000
x 100
Dilution Factor
-
-
-
-
-
1 1 1 2000 200 200 2000 200 -
-
Peak Area
0 972 1269 1984 4657 9137 18604 0 0 1010 8894 4577 749 1212 1927 5081 5034 2437 6000 4031 8028 16371
PFOA Found (ng/L)
-
-
-
ND 36.6 510 501000
56200 55600 244000 67200 -
Amount PFOA Added (ng/L)
-
-
-
-
-
50 500 500000 -
Recovery (Vo) -
-
-
-
-
73 102 89 -
-- -
Standard Curve : Linear (1/x weighted) Intercept = 401.121 Slope = 16.6567
Coef.OfDet. = 0.990702
CS = Calibration standard C = Control sample S = Sample
LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike
CK = Check Standard ND = Not detected = Response between 0 and LOD NQ = Not quantifiable = Response between LOD and LOQ
Spreadsheet prepared by:.
f t.,,
000493
j4
RESEARCH
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
Internal Chain of Custody/Fortification Sheet
Exygen Study Number:
L1714
Matrix: Water
Sponsor Study/Protocol No: NA
The samples listed below were removed from refrigerator N o .___3_X___
Time 0 7 *40
Date Q 2-(o3{0^
&Initials
CLIENT SAMPLE ID
EXYGEN ID NUMBER
VOLUME (mL) FORTIFICATION (ng)
na
Reagent Control
40.0
_
na
Reagent Spk A
40.0
2.0
na Reagent Spk B 40.0 20.0
DSN002
L1714-1 SpkC
40.0 20000.0
DSN002
L1714-1
40.0
DSN002
L1714-1 Rep
40.0
_
DSN003
L17I4-2
40.0
_
n
DSN004
L1714-3
40.0
-
--
-
__
- - __
il -
-
-_ - __
-
r" ! -
- -- __
--
_
- - __
- __
- - __
- - -_
- - --
Spiking Solution Used
Volume Used for Spiking Initial/Date
Reagent Spk A
F120903-5 (10 ng/mL)
200 pL (200 pL micropipet) v L /m Jt l& i
Reagent Spk B
F120903-4 (100 ng/mL)
200 pL (200 pL micropipet)
n L1714-1 SpkC -
F120903-1 (100000 ng/mL)
_
200 pL (200 pL micropipet)
_
/62-(yy0-
- _ __
- - __
P- 1 - - -
All samples were measured:
,
Time_
______
D ate 02-^031 D-j1
Initials 4 = -
After measuring samples were returned to refrigerator N o.. 32-
Time
Date O
4 1Initials
Comments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date:
-
Analysis Summary:
DataSet: bT C M rb
D ata Set:____ ~ ________ 4 ' i Data Set: *~_______
Set extraction/analysis data verified by: jQ C
Initials/Date: Initials/Date: Initials/Date:
Date:
4 k J jL
July 26, 2001/6
000494
'"'"n i n im1
in m
r rs*Hp'*n
> : 133 m
II
RC H
3058 Research D rive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
io o
000495
SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET
EXYGEN STUDY NUMBER: L1714
METHOD: $$
PROTOCOL NUMBER: NA
MATRIX: Water
ANALYTES: PFOA
Client ID
na na na DSN002 DSN002 DSN002 DSN003 DSN004 -
-
-
-
-
ExygenID
Reagent Control Reagent Spk A Reagent Spk B L1714-1 Spk C
L1714-1 L1714-1 Rep
L1714-2 L1714-3
-
-
-
-
STEP 1
____ 1f -
-
-
-
T,,
STEP 2
\L
-
-
-
*Initials/Date
- o^S)o<4
STEP 1: SPE column clean-up STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reanalysis.
Dilutions (mL/mL)
-
--
STEP 3
o
-*V io
NI1
--------
-------
)-
$62 P f
Dilutions (mL/mL)
-
-- --
_
-
-
-
-
-
-
-
-
-
--
STEP 4 --
-
-
_
-
-
-
-
-
--
Reagents/ Materials Methanol C18 SPE
Water .
Lot#
l^ 2 l0 b i H?>2S\0
_
.
-
-
Initials/Date
-
-
_
-
).
T7 -
_
-
_
_. --
HPLC
Methanol
AmmoniumAcetate Water
M !o\S\ 4 .^ 0
- ):
Initials/Date
edSiW
1
Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water
COMMENTS:
Final extracts stored in refrigerator. 3 2 - Initials:
Date:
July 19,2001/4
PREPARATION OF EXTRACTED CALIBRATION STANDARDS
Protocol-No.: None Method No.: 01M-008-046*
Exygen Study No.: NA
Analytes:
PFOA
Matrix:
Iy peIW atex y g e n STUDY N O . L \ U ' f
Sample Vol: 40 mL
Sponsor Sample
ID
NA
Exygen Sample
ID
0106020
Sample Description
Type I WaterA
Fort. Solution
ID
-
. Fort. Soin. Cone.
(ng/mL)
-
Fort. Volume
(uL)
-
Micropipet used (ML)
Fort. Level (ppt)
Final Solution ID #**
XC012804-0
Reagents/ Materials
Methanol
,, Lot#
NA
0106020
TypeIW aterA F120903-5
10
100 200
25 XC012804-1
C18 SPE
NA
0106020
Type I WaterA F120903-5
10
200 200
50 XC012804-2 Type I Water
NA
NA
0106020
Type I WaterA F120903-5
10
400 200 100 XC012804-3
NA
0106020
Type I WaterA F120903-4
100
100
200
250 XC012804-4
NA
0106020
Type I WaterA F120903-4
100
200
200
500 XC012804-5
-
_
-
_ _
NA
0106020
Type I WaterA F120903-4
100
400
200 1000 XC012804-6
-
-
NA 0106020 Type I WaterA F012804-2 100
100 200
250 XC012804-7
-- - Vertical arrows in a yolumn indicate identical values.
- ---
- Initials/Date:
**This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3, etc.
Samples removed fr9 ^7efrigerato^ / freezer # 3 2 - Time: CROP 40 mL of each sample measured using a 0 mL graduated cylinder. After measuring, samples returned to ^frigerator7)freezer # 3 2 - Time: ^ 5 0
Initials/Date:_ Initials/Date:_ Initials/Date:_
/6 l| Z j^l
T H IS IS AN EXACT COPY OF THE ORIGINAL DOCUMENT.*
Samples fortified: SPE clean-up: Final volume adjusted to 5 mL: Extracts placed in refrigerator #
3~2-
Initials/Date:. Initials/Date:. Initials/Date:. Initials/Date: _
/ lte j t i
/_O jj2B j"'
/o\\z&
c -V O ll 2-8
J D A T E jd c W ;
STANDARD EXPIRATION DATE: 2/11/04
Comments:
AThis type I water has been filtered through a hypercarb filter
* Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water.
000496
July 10, 2001/0
i r > m
i
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r
Masslynx - Sample List
Sample List: C:\MASSLYNX\Fluorocherr ls.PRO\SampleDB\020304D Daikln.spl
Printed: Mon Feb 09 09:16:25 2004 tJ d e c o r i
Vial File Name
LIMS ID Client ID Sample Description
1 1 020304D-1001 -- 2 2 020304D-1002 -- 3 3 020304D-1003 -- 4 4 020304D-1004 -- 5 5 020304D-1005 -- 6 6 020304D-1006 -- 7 7 020304D-1007 -- 8 92 020304D-1008 -- 9 11 020304D-1009 -- 10 12 020304D-1010 -- 11 13 020304D-1011 -- 12 14 020304D-1012 -- 13 2 020304D-1013 -- 14 3 020304D-1014 -- 15 4 020304D-1015 -- 16 15 020304D-1016 -- 17 16 020304D-1017 --
18 17 020304D-1018 -- 19 18 020304D-1019 -- 20 5 020304D-1020 -- 21 6 020304D-1021 -- 22 7 020304D-1022 --
-- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- --
XC012804-0, 0 ng/L standard XC012804-1, 25 ng/L standard XC 012804-2, 50 ng/L standard XC012804-3, 100 ng/L standard XC012804-4, 250 ng/L standard XC012804-5, 500 ng/L standard X C 012804-6,1000 ng/L standard Methanol Wash 0106020 Control 0106020 Spk A, 25 ng/L 0106020 Spk B, 500 ng/L L1714-1 Spk C, 500000 ng/L, DF=2000
XC012804-1, 25 ng/L standard XC012804-2, 50 ng/L standard XC012804-3,100 ng/L standard L1714-1, DF=200 L1714-1 Rep, DF=200
L1714-2, DF=2000 L1714-3, DF=200 XC012804-4, 250 ng/L standard XC012804-5, 500 ng/L standard X C 012804-6,1000 ng/L standard
000497
7 crz
Exygen study n o .
> :.:i
:j
Page 1 Page Position: ( 1 , 1 )
Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF
-- Blank -- Standard -- Standard -- Standard -- Standard -- Standard ------- Standard -- Blank -- Blank -- QC -- QC -- QC
-- Standard -- Standard -- Standard -- Analyte -- Analyte
-- Analyte -- Analyte -- Standard -- Standard -- Standard
0 25 50 100 250 500 1000
--
--
50 500 500000 25 50 100
--
--
--
--
250 500 1000
-- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- --
0____ --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0
--0 --0 --0 --0 --0
1 1 1 1 1 1 1 1 1 1 1 2000 1 1 1 200 200
2000 200 1 1 1
'3 ' '" > 3
'* " 3
:3
'3
':
Masslynx - Sample List
Sample List: C:\MASSLYNX\Fluorochems P R C A S a m p eDB\020304D Daikin.spl
Printed: Mon Feb 09 09:16:25 2004
61 &H
MS Method HPLC Method MS Tune File Inj Volume (pL)
1 APFO 12 MIN 2 APFO 12 MIN
3 APFO 12 MIN
4 APFO 12 MIN 5 APFO 12 MIN 6 APFO 12 MIN 7 APFO 12 MIN 8 APFO 12 MIN 9 APFO 12 MIN 10 APFO 12 MIN 11 APFO 12 MIN 12 APFO 12 MIN 13 APFO 12 MIN 14 APFO 12 MIN
15 APFO 12 MIN 16 APFO 12 MIN 17 APFO 12 MIN 18 APFO 12 MIN 19 APFO 12 MIN
20 APFO 12 MIN 21 APFO 12 MIN 22 APFO 12 MIN
pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water
pfbs water pfbs water pfbs water
Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems
Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems
15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15
15 15 15
000498
Vo
) :::3
Exygen study n o .
1
Page 2 Page Position: (2 ,1 )
8 I
LC/MS/MS SYSTEM AND OPERATING CONDITIONS
Sponsor Protocol No: N A
Exygen Study No: L I714
Instrument:
Micromass Quattro Ultima (LC/MS/MS Unit #7)
Computer:
COMPAQ Professional Workstation AP200
f*V
Software:
Microsoft Windows NT: Version 4 Build 1381: Service Pack 5
I Micromass Limited: MassLynx 3.4 Build 004
HPLC Equipment:
Hewlett Packard (HP) Series 1100
HP Quat Pump
HP Vacuum Degasser
HP Autosampler
HP Column Oven
n
HPLC Column:
Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID:MA12842)
(JONESCHROMATOGRAPHY: Part No. FK5962EJ)
>--
Mobile Phase (A)
2 mM Ammonium Acetate in Type I Water
ui
Mobile Phase (B)
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.
A ll Handwritten Peak ID 's by:.
t' .fn
f'
f!
000499
A 1,--," -->",)
f~*
Scanning Method Report
Method:
C:\MASSLYNX\FLUOROCHEMS.PRO\ACQUDB\APFO 12 MIN
Last Modified: Mon Jan 26 14:19:30 2004
I\
Printed:
Mon Feb 09 09:16:34 2004
Solvent Delay ( mins ) :
0.00
Function : 1
MRM of 1 Mass Pair ( ESP- )
I* *' Inter Channel Delay ( Secs ) : 0.03
Span ( Daltons ) :
0.00
Start Time ( Mins ) : End Time ( Mins ) :
0.00 12.00
Repeats :
1
Channel Parent Daughter Dwell (Secs) Coll Energy (eV) Cone ( V )
J? -
1:
J
1 413.00 369.00 0.20
10
50
A k
Page 1
r* k:
iS
&t -i tj
000500
Method Report
Method File: Last Modified:
Printed:
C:\MASSLYNX\FLUOROCHEMS.PRO\ACQUDB\pfbs water Monday, Fbruary 09, 2004 08:19:05
Monday, February 09, 2004 09:16:39
Page X
HP1100 LC Pump Initial Conditions
Solvents A% B% C% D%
Flow (ml/min)
I I' Stop Time (mins)
* ' Min Pressure (bar) Max Pressure (bar)
p*, Oven Temperature Left(C) t . Oven Temperature Right(C)
HP1100 LC Pump Gradient Timetable
90.0 10.0
0 .0 0 .0
0.300 20.0
0
400 35.0 35.0
The gradient Timetable contains 8 entries which are :
Time
0.00
2.00 f ' 5.00
9.00 9.50 r* 14.00 f 14.50 20.00
A% 90.0 90.0 10.0 10.0
0.0 0.0 90.0 90.0
B% 10.0 10.0 90.0 90.0 100.0 100.0 10.0 10.0
C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
MJrr HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are :
Time j Initial
0.00
0.10
12.00
t
Column Switch Off Off Off Off
Contactl Off On Off Off
Contact2 Off Off On Off
Contact3 Off Off Off Off
HP1100 Autosampler Initial Conditions
Draw Speed Eject Speed (1/min) Draw Position (mm) Stop Time (mins) Injection Volume {xl) ' Vial Number
200.0 200
0.00 20.00 15.0
7
Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300
Contact4 Off Off Off Off
Pressure 400 400 400 400 400 400 400 400
H
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Tuning Method Report
Method:
n? *
Printed:
C :\MAS SLYNX\FLUOROCHEMS .PRO\ACQUDB\FLUOROCHEMS Mon Feb 09 09:33:24 2004
Page 1
M
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4-
SOURCE ( ESP- )
i'
't Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp.
i&k i' !.
Pressures
Analyser Vacuum Gas Cell
n
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Set Rdbk
3.00 30 0.0 0.0 0.0 100 300
-2.93 -50
100 300
Rdbk
OFF 3.0e- 3
Analyser
LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 .. HM Res 2 IEnergy 2 Multiplier
Gas Flows
Cone Gas Desolvation
Set Rd] 14.0 14.0 1.0 -2 8 30 9 2 11 ` 14.0 14.0 2.0 700 -6 Rdbk 86.7 692.7
000502
1" J
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; Quantify Calibration Report Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Calibration: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\CurveDB\020304D Daikin
Last modified: Tue Feb 10 08:06:54 2004
Printed:
Tue Feb 10 08:08:40 2004
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000503
Quantify Sample Report Study N o .:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Sample List: Last modified: Method: Last modified: Job Code:
Printed:
P :\Data\LCMSMS7\Masslynx\Fluorochems .PRO\SampleDB\020304D Daikin
Tue Feb 10 08:04:16 2004
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Tue Feb 10 08:06:53 2004
,
Tue Feb 10 08:08:41 2004
Initials. Date.
R u n # S a ^ s k ^ r ) 6 o \ To
Page 1
lo ' ? -
Name: 020304D-1001 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000504
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f? Quantify Sample Report i Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
^ Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
f Last modified: Tue Feb 10 08:04:16 2004
| / Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
|-a Job C o d e ;
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Printed:
Tue Feb 10 08:08:41 2004
Page 2
fl Name: 020304D-1002 * ; Text:
1: PFOA
f
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Exygen Research, 3058 Research Drive, State College, PA 16801
f> '
000505
Quantify Sample Report Study No.:Ll714, Set No.:020304D, Ext.Pate:02/03/04, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Page 3
Name: 020304D-1003 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
0050G
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f"*j Quantify Sample Report : Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
^ Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304D Daikin
' Last modified: Tue Feb 10 08:04:16 2004
t i Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
"** Job Code;
Printed:
Tue Feb 10 08:08:41 2004
Page 4
1 ; Name: 020304D-1004 * ` Text :
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t
000507
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r - Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304DDaikin
i Last modified: Tue Feb 10 08:04:16 2004
` Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 8min RT
Last modified: Tue Feb 10 08:06:53 2004
(Fl Job Code:
' Printed:
Tue Feb 10 08:08:41 2004
Page 5
f ; Name: 020304D-1005 Text:
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000508
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^ Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
: ; Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
f --. Job Code:
>.
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Printed:
'" "
Tue Feb 10 08:08:41 2004
Page 6
f Name: 020304D-1006 1 Text :
r~i
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Exygen Research, 3058 Research Drive, State College, PA 16801
000509
Quantify Sample Report Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Rage 7
Name: 020304D-1007 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000510
n
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| , Quantify Sample Report Study No.:L1714, Set N o . :020304D, Ext.Date:02/03/04, Analyst:K.Risha
^ Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
: Last modified: Tue Feb 10 08:04:16 2004
* Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
;-- ; Job Code: t;
Printed:
Tue Feb 10 08:08:41 2004
Page 8
Name: 020304D-1008
t
Text :
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f
Exygen Research, 3058 Research Drive, State College, PA 16801
r
000511
Quantify Sample Report Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Page 9
Name: 020304D-1009 Text:
1 : PF0A
Exygen Research, 3058 Research Drive, State College, PA 16801
000512
S "I
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11
f~ Quantify Sample Report ' Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Page 10
^ Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304D Daikin
| ; Last modified: Tue Feb 10 08:04:16 2004
* ' Nethod:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\NethDB\PFOA. 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
p > Job Code:
Printed:
Tue Feb 10 08:08:41 2004
I i Name: 020304D-1010 h Text :
L
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. t' -
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00051.3
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Quantify Sample Report 1 Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Page 11
Sample List: E:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304D Daikin
I , Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
r~>
I I Name: 020304D-1011 Text :
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Exygen Research, 3058 Research Drive, State College, PA 16801
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000514
Quantify Sample Report Study Mo.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Page 12
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Marne: 020304D-1012 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000515
Quantify Sample Report Study No.:L1714, Set No.:020304D, Ext .Date:02/03/04, Analyst:K.Risha
Page 13
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Name: 020304D-1013 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000516
Quantify Sample Report Study No.:L1714, Set No.:020304D, Ext.Bate:02/03/04, Analyst:K.Risha
Page 14
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Name: 020304D-1014 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000517
Quantify Sample Report Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Page 15
,, Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304D Daikin
. Last modified: Tue Feb 10 08:04:16 2004
' Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
, Job Code:
Printed:
Tue Feb 10 08:08:41 2004
f Name: 020304D-1015 Text :
r - 1 : PFOA
|k. 4
J--!
fI
Exygen Research, 3058 Research Drive, State College, PA 16801
000518
t-... '1
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| 1 Quantify Sample Report
Study No.:L1714, Set N o . :020304D, Ext.Date:02/03/04, Analyst:K.Risha
Page 16
,r--: Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304D Daikin
; Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 8 min RT
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Last modified: Tue Feb 10 08:06:53 2004 Job Code:
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Tue Feb 10 08:08:41 2004
Name: 020304D-1016 Text:
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Page 17
f* ! Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin
f4i Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
n Job Code:
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Name: 020304D-1017 Text:
1 : PFOA
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Page 18
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Name: 020304D-1018 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000521
Quantify Sample Report Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K .Risha
Rage 19
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\Sa2iqpleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Name: 020304D-1019 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000522
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Quantify Sandle Report Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Page 20
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Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304D Daikin Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
rn Job Code:
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f Name: 020304D-1020 Text :
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Page 21
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\020304D Daikin
Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Name: 020304D-1021 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000524
Quantify Sample Report Study No.:L1714, Set No.:020304D, Ext.Date:02/03/04, Analyst:K.Risha
Page 22
Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\020304D Daikin Last modified: Tue Feb 10 08:04:16 2004
Method:
P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 8 min RT
Last modified: Tue Feb 10 08:06:53 2004
Job Code:
Printed:
Tue Feb 10 08:08:41 2004
Name: 020304D-1022 Text:
1 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
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