Document X7Qnz47bjY9a5v456xMm44GEy
M I S lG - I 7 0 ^
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Analytical Report
: f~ FKiorochemical Characterization of Water Samples
Daikin America, Inc.
n
Exygen Research Laboratory Report No. L0001563
Testing Laboratory
Exygen Research ! , 3058 Research Drive
State College, PA 16801
..H
H Requester
M
" " Randy Roussel
p Daikin America, Inc.
!J PO Box 2252
4 Decatur, AL 35609
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r ; 3058 Research Drive State College, PA 16801, USA
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1 introduction
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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 L0001563.
n Specific fluorochemica! 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 Prfluorooctanoic Acid Perfluorooctane Sulfonate
Acronvm C8 Acid (PFOAj C8 Sulfonate (PFOS)
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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 1/5/04. Chain-of-custody information is presented in Attachment C.
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3 Holding Times
<-- 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
p-- 4.1 LC/MS/MS
4.1.1 Sample Preparation for LC/MS/MS Analysis L;
Samples were initially treated with 200 uL of 250 mg/L sodium thiosulfate solution to remove n 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 C i8 SPE cartridge. The cartridge was eluted with 5 mL of 100%
f methanol. This treatment resulted in an eight-fold concentration of the diluted samples prior to t . analysis.
PAGE2 OF 5
000050
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;
4.1.2 Sample Analysis by LC/MS/MS n
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
H 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 1/8/04 and analyzed on 1/14/04. Raw analytical data is provided in Attachment D.
n
t :! 5 Analysis
ff 5.1 Calibration
I A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence 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.
Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value.
i' ! All calibration criteria were met for this analysis.
j j
f**! 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.
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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 samples presented here the instrument blanks are compliant.
5.3 Surrogates
Surrogate spikes are not a component of the LC/MS/MS analytical methods.
5.4 Matrix Spikes
A matrix spike was prepared for sample DAI-010504-DD-MW4. Matrix spike recoveries are given in Attachment B. :>
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PAGE 3 OF 5
000051
5.5 Duplicates
Sample DAI-010504-DD-MW4 was analyzed in duplicate. The duplicate results are included with the sample results in Attachment A.
5.6 Laboratory Control Samples
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.
6 Data Summary
Please see Attachment A for a detailed listing of the analytical results. Results are reported in units of parts per billion (ppb) (ng/mL).
7 Data/Sample Retention
:\ /
V, ' ' ' -'
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 Custody 8.4 Attachment D: Raw Analytical Data
PAGE4QF5
9 Signatures
Other Lab Members Contributing to Data Karen Risha
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PAGE5 OF5
$ 0 0 S ft
Analytical ^
L Report 1
i Summary of PFOA and PFOS in Water Samples
p\
*
Analyte Found (ng/mL)
Analyte Found (ng/mL)
Sample IP
PFOA
PFOS
DAI-0105Q4-DD-MW4
969-
495
DAI-01 0504tDD-MW4`
968
496
D AI-010504-D D -M W 2
167
319
D AI-010504-D D -M W 7
981
514
Laboratory Duplicate
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000053
r. f , ^ ^ 3 3005568 Research Drive
* ^ L sStatatte College, PA 16801, USA J: 814.272.1039
Vf ; F: 814.231.1580
I . exygen.com
STANDARD TERM S A N D C O N D IT IO N S
Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract.
CONFIDENTIALITY-- Exygen Research ("Exygen," "us," or "w e") maintains the strictest confidentiality in all 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 dient 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.
CONTRACTS--All contracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer.
PAYMENT TERMS--Unless otherwise set forth in this Purchase Order, terms o f payment are "Net 30 Days." The time allowable for payment shall begin after both: (a) client's receipt of Exygen's invoice: and (b) the satisfactory performance o f the services contemplated hereunder. A 1.5% monthly service charge shall be added to all past due balances. Notwithstanding any payment terms to the contrary set forth in this Purchase Order, Exygen, in its sole discretion, reserves the right to request payment in advance from client. In the event of default in payment for services rendered, Exygen shall be entitled to reasonable costs o f collection, including, but not limited to, attorneys' fees.
BILLING--All fees and charges are billed directly to the client requesting services. Exygen will not bill a third party without prior notification in writing, via a signed statement acknowledging and accepting responsibility for paym ent Exygen will assume that the paperwork submitted with a sample describes the desired testing protocol. Any changes to the protocol must be submitted in writing. Please fax changes to Exygen marked, "URGENT" to your assigned representative. If changes are made after the originally requested testing has been initiated or completed, the client accepts responsibility for payment, Exygen will not be responsible for hold times that are missed due to such changes.
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M IN IM U M AGE--The minimum fee for commercial services is one hundred dollars ($100).
SAMPLE COLLECTION/SUBMISSION--Client shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law and good commercial practice. Title and risk of loss with respect to submitted samples shall at all times remain with client prior to acceptance by an Exygen sample custodian. Exygen will initiate a chain-of-custody upon sample receipt unless the client includes one with the sample(s). By request, Exygen will provide chain-of-custody forms for client's use.
All samples submitted must be accompanied by: purchase order, or signed quotation; sample description, including sample type, source, time and date o f collection; specific analyses requested; estimated concentration levels; requested report date; current billing address; and other relevant information.
Upon request, Exygen will provide and ship appropriate sample containers to clients. These containers w ill include the appropriate preservative if particular analyses require one. It is the responsibility of the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers.
SAMPLE DISPOSAL-- Exygen retains samples for one month after reporting results, then disposes of or returns the sample. Unless the client
requests that the sample(s) be returned, or prior arrangements have been , made for long-term storage, Exygen shall dispose of the samplefs). Exygen shall charge a monthly fee for long-term storage. Samples found or suspected to contain hazardous waste, according to definitions in state and /o r federal guidelines, will be returned to the client upon completion o f the analysis. The cost of returning the sample(s) will be invoiced to the client. Exygen reserves the right to charge a disposal fee for the disposal o f any and all samples unless returned by Exygen to client. Exygen shall, unless the nature and character of the sample dictates otherwise, store all samples under Socked, temperature-controlled conditions. An internal chain-ofcustody is maintained for each lot o f samples received.
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ETHICS POLICY-- Exygen Research strives to provide its clients with the highest quality data in the fastest realistic turnaround tim e. We balance the high standards of this goal by insisting that each employee also perform within the guidelines of the highest possible professional ethics. Each Exygen employee is required to sign a statement o f personal and professional integrity.
SPECIAL REPORTS--M <M ona\ charges may be necessary for custom report formats.
LITIGATION--All costs associated with compliance to any subpoena for documents, for testimony in a court of law, or for any other purpose relating to work performed by Exygen Research shall be invoiced by Exygen and paid by client. These costs shall include, but are not limited to, hourly charges for the persons Involved, travel, mileage, and accommoda tions, and for any and all other expenses associated with said litigation.
INDEMNIFICATION, LIABILITY, A N D INSURANCE--Exygen 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 property damage 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, occur 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.
WARRANTY AND LIM ITS OF LIABILITY-- in accepting analytical work, Exygen guarantees the accuracy o f the test results for the sample as submitted within the tolerances set forth in the SOPs. We disclaim any other warranties, expressed or implied by law. Exygen does not accept any legal responsibility for the purposes for which client uses the test results. Exygen will not accept any purchase order or any other order for .work that includes conditions that vary from these Standard Conditions.
ACCEPTANCE OF PURCHASE ORDER-- This Purchase Order becomes a
binding agreement, subject to the specific term s and conditions stated
herein, upon Exygen's commencement of work.
,
0OO >S 3A
Recovery Summary for PFOA and PFOS in Water
PFOA
PFOS
r
Amount Amt Found Amount
Amt Found Amount
<
Sample
Spiked in Sample Recovered Recovery in Sample Recovered Recovery
Description
(ng/mL) (ng/mL) (ng/mL)
(%)
(ng/mL) (ng/mL)
(%)
f--m,
t ' DAI-010504-DD-MW4
500 ng/mL Spike
500 969
1550
116
495
1060
113
t
000054
3058 Research Drive State College, PA 16801, USA
VT. 800.281.3219 F: 814.272.1019 exygen.com
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
1673
Project:
P0000449
^ P ro je c t Storage:
j Company Name: Daikin America
Submitted By: Neal Waddell and Randy Roussel
-L o g in Type:
Immediate Receipt o f Samples
Started:
T
Date Start:
01/07/2004
Due Date:
01/21/2004
r * Received Date: 01/07/2004
} Received By:
ROBB, SHAWN
Spread Sample:
Label:
^ P ro je c t Title/Type: Analysis of PFOA in W ater / ROUTINE
; Exygen SD/Pl: RISHA, KAREN
Login Notes:
-- Conform Notes:
orm Conform COC: Conform Sample: Conform Request:
--Package K0002162
Carton
Packages / Containers
Mail Date / Condition
Shipper /_ID
1/7/2004 10:18:56AM Package & Contents Uncompromised
FEDEX 8402386190870215
Temp. Control/Temp.
Wet Ice 1.1
Container #
i C0018611 C0018614
"C0018618
Gross Weight pH
Container Type
608.9 g
500 ml Clear Plastic
603.0 g
500 ml Clear Plastic
598.8 g
500 ml Clear Plastic
Preservative NONE NONE NONE
Mfg. Lot 3232010 3232010 3232010
Miscellaneous r Item Key
None
Description
ICOC
True True True
Direction / Handled By RECEIVED
ROBB, SHAWN
Mfg, ID
471600 471603 471607
Sample ID ,--1.0001563-0001
L0001563-0002 ! L0001563-0003
Matrix LIQUID LIQUID LIQUID
Fraction Water Water
Water
Samples
Sample DA1-010504-DD-MW4 DA1-010504-DD-MW2 DA1-010504-DD-MW7
Date Sampled Date Received 01/05/2004 01/07/2004 01/05/2004 01/07/2004 01/05/2004 01/07/2004
Date Due 01/21/2004 01/21/2004 01/21/2004
1/16/2004 i .ogin.rpt
Report Version: Dec 22 2003 10:44AM Page 1 of 2
0000S5
Instance:
R0080499
R0080499
r >001563-0001
C o n ta in e r ^00018611 / 500 ml Clear Plastic / NONE
L001563-0002
C o n ta in e r i C0018618 / 500 ml Clear Plastic / NONE
p 0 0 1 563-0003
C o n ta in e r C0018614 / 500 ml Clear Plastic / NONE
Bottles
Method Method Method
mm
r-1 /1 6/2004 Login.rpt
Report Version: Dec 22 2003 10:44AM Page 2 of 2
000056
Instance:
R0080499
R0080499
Composite Number of Containers
000057
CHAIN OF CUSTODY/ANALYSIS REQUEST FO RM
RESEARCH
Exygen Research Sample Receiving * 3 1 1 7 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com
,/ Page / o f __ (_
PROJECT INFO RM ATIO N
ANALYSES REQUESTED
Client (name & address):
Affl&PJc-A
Phone: Fax: Sampler:
3o&'*fooo
'
Project M anager (Name & E-mail Address):
/ioKssei //*-*( (dadoed!
Project Name:
d/vJ- sn<<d>' RO. # : / A > 3 o Zz3~30
Quotation # :
Please fill out this form completelyto ensure correct analysis and proper handling of your samples.
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SAMPLE ANALYSIS
_Q
Collection Collection
ExyLIAAS# Client Sample Identification
Date
Time O
A(-/S'od- AA - siu d i-s-o-y ZfT3S' V MZ-o/orod- - siiZ 9\ /fS -7
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CHAIN OF CUSTODY
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Date
Time
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(TV Cooler Temp. (C) 7, /
Received by
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OTHER INFORMATION
LAB USE ONLY
I .. 1 ... * i I I I I-- - l L l I i i l
PROJECT REQUIREMENTS Results Deadline:
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ED Add quality control summary
I I Add calibration summary
EH Add raw data
Other________________
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Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site:
NA L1563 PFOA 413-> 369 NA
RAW DATA. REPORT
Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume:
50ng/L 15 pL Water 40.0 mL 5.0 mL
Set No: Analyst: Instrument Type: Extraction Date: Analyzed on:
010804B Karen Risha LC/MS/MS Unit # 6 01/08/04 01/14/04
Exygen ID
XC010804-0 XC010804-1 XC010804-2 XC010804-3 XCO10804-4 XC010804-5 XC010804-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spk B XC010804-1 XCO10804-2 L1563-1 SpkC
L1563-1 L1563-1Rep
L1563-2 L1563-3 XC010804-3 L 1563-1 Spk C L1S63-1 L1563-1Rep L1563-2 L1563-3 XC010804-4 XC010804-5 XC010804-6
Sponsor ID
-
-
-
-
-
NA NA NA
DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW2 DAI-010504-DD-MW7 DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW2 DAI-010504-DD-MW7 '-
-
Sample Code
c CS
CS CS
CS CS
CS
c c
LCS LCS CS CS LF
S
s s s
CS LF
s s s s CS
CS CS
Run No. 010804B-801 010804B-802 010804B-803 010804B-804 010804B-805 010804B-806 010804B-807 010804B-808 010804B-809 010804B-810 010804B-811 010804B-812 010804B-813 010804B-814 010804B-815 010804B-816 010804B-817 010804B-818 010804B-819 010804B-820 010804B-821 010804B-822 010804B-823 010804B-824 010804B-825 010804B-826 010804B-827
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. (ng/L)
0 25 50 100 250 500 1000 25 50 100 250 500 1000
Dilution Factor
-
1 1 1 10000 1000 1000 1000 1000 1000 100 100 100 100 -
-
-
Peak Area 1252 9216 16778 29280 70662 134827 256647 1089 2309 14971 134534 8148 15880 42814 251863 251606 .45817 254844 29934 423514 2385296 2372619 422232 2343410 65517 129677 257279
x 100
PFOA Found (ng/L)
-
-
-
Amount PFOA Added (ng/L)
-
Recovery (%) -
-
-
-
ND 47.0 512
1550000 969000 968000 167000 981000 * * * * *
-
-
-
so 500 500000 500000 -
-
94 102 116
-
'
---
Standard Curve : Linear il/x weifhtedl Intercept = 2884.19 Slope = 256.944
Coef. Of D et = 0.999438
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
^Sample was analyzed at several dilution levels in the same run. Appropriate results are reported.
Spreadsheet prepared by:
/ l|
Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site:
NA L1445 PFOS 499 -> 99 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:
010804B Karen Risha LC/MS/MS Unit # 6 01/08/04 01/14/04
Exygen ID
XC010804-0 XC010804-1 XC010804-2 XCO10804-3 XC010804-4 XCOI0804-5 XC010804-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 SpkB XCO10804-1 XC010804-2 L1563-1 Spk C
L1563-1 L1563-1 Rep
L1563-2 L1563-3 XC010804-3 L1563-1 SpkC L1563-1 L1563-1 Rep L1563-2 L1563-3 XC010804-4 XC010804-5 XC010804-6
Sponsor ID -
NA NA NA
DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW4 D A I-0 10504-DD-MW2 D A I-0 10504-DD-MW7 D A I -0 10504-DD-MW4 DAI-010S04-DD-MW4 D A I-0 10504-DD-M W4 DAI-010504-DD-MW2 DAI-010504-DD-MW7 -
-
Sample Code
C CS CS CS CS CS CS c c LCS LCS CS CS LF S S
s s
CS LF S
s s s
CS CS CS
Run No. 010804B-801 010804B-802 010804B-803 010804B-804 010804B-805 010804B-806 010804B-807 010804B-808 010804B-809 010804B-8IO 010804B-811 010804B-812 010804B-813 010804B-814 010804B-815 010804B-816 010804B-817 OI0804B-818 010804B-819 010804B-820 010804B-821 010804B-822 010804B-823 010804B-824 010804B-825 010804B-826 010804B-827
Std. Cone. (ng/L)
0 25 50 100 250 500 1000 25 50 100 250 500 1000
PFOA Found (ng/L) = (peak area - intercept) ! slope x DF
Recovery (%) =
______[PFOA found (ng/L)-PFOA found in control (ng/L)]_____ x 100
amount PFOA added (ng/L)
Dilution Factor
1 1 1 10000 1000 1000 1000 1000 1000 100 100 100 100 -
-
Peak Area
0 587 1088 1807 4818 9066 17644
0 0 1048 9872 581 1023 2155 9686 9706 6263 10040 2141 21638 92651 98339 62657 96675 5227 10572 21117
PFOA Found (ng/L)
-
-
ND 49.3 505 1060000 495000 496000 319000 514000 * * * * *
-
-
Amount PFOA Added (ng/L)
50 500 500000 -
-
500000
-
-
Recovery (%) _ _ _ _
-
-* 99 101 113 -
-
-
-
,
Standard Curve : Linear (1/x weighted) Intercept = 92.7055 Slope = 19.3657
Coef. Of D e t = 0.986278
CS = Calibration standard C = Control sample S = Sample
LF as Lab fortified sample FF ss Field fortified sample LCS = Laboratoiy Control Spike
Sample was analyzed at several dilution levels in the same run. Appropriate results are reported.
CK = Check Standard ND = Not detected = Response between 0 and LOD NQ = Not quantifiable = Response between LOD and LOQ
Spreadsheet prepared by:
000080
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
Internal Chain of Custody/Fortification Sheet
Exygen Study Number:
L1563
Matrix: Water
Sponsor Study/Protocol No: NA
The samples listed below were removed from refrigerator No.
Time
Date Oi M jo L
Initials P-
CLIENT SAMPLE ID na na na
DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW2 DAI-010504-DD-MW7
EXYGEN ID NUMBER 0106020 Control 0106020 Spk A 0106020 SpkB L1563-1 Spk C L1563-1 L1563-1 Rep L1563-2 L1563-3
VOLUME (mL) 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0
FORTIFICATION (ng)
_
2.0 20.0 20000.0
-
-
.-
_
- - -_
- - -_
- - -_
- - -_
- - _-
- - -_
--
.- -
---
- - __
- - _-
- - --
- - --
Spiking Solution Used
Volume Used for Spiking Loitial/Date
0106020 Spk A
F121603-2 (10 ng/mL)
200 pL (200 pL micropipet) W e - lb\ fift *]
l& *
0106020 SpkB
F121603-1 (100ng/mL)
200 pL (200 pL micropipet) f f r /Oilfifcb-
L1563-1 SpkC
FI 20803-1 (100000 ng/mL)
200 pL (200 pL micropipet)
------ /:--o i'l1 0
-- _
- __
- _ __
- - --
All samples were measured:
T im e _ ./Q 3 Q ______
Date OijoP>jo^f
Initials Q t E
After measuring samples were returned to refrigerator No. , 3 2
Time i/i O _______
Date iOij h A j <y-l
Initials flE fc
Com m ents: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: c e s j Q i j c A j o t f
Analysis Summary:
Data Set: 0 l 0 f l 4 & Data S e t:____ ~ _______ Data S e t:____ ZZ.______
Set extraction/analysis data verified by:
Initiiaallss//DDaattee::. frciC / 01
Initials/Date:
/___ ~
Initials/Date:________ /
D ate:__ / July 26, 2001/6
000061
11
1 RESEARCH
y i I '-'i
3058 Research Drive State College, PA 16801
I 11
I
Phone: 814-272-1039 Fax: 814-231-1580
11
SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET
EXYGEN STUDY NUMBER: L1563 MATRIX: Water
METHOD: f ANALYTES: PFOAandPFOS
PROTOCOL NUMBER: NA
Client ID
na na na DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW4 DAI-010504-DD-MW2 DAI-010504-DD-MW7
-
-
. _ _ _ -
-
*Initials/Date
Exygen ID
0106020 Control 0106020 Spk A 0106020 SpkB L I563-1 SpkC
L1563-1 L1563-1 Rep
L1563-2 L1563-3
-
-
STEP 1
/
-
CE. oiitM
o
STEP 2
Dilutions (mL/mL)
-
-
STEP 3
G >u ^ -`/.o*V 0 & '/ > O , ^ .D
QD 0 ^ o X ,0 V ( S ^ A / ) LoNJ/
--
- --
- --
- --
- --
- --
- --
- --
- --
- --
- --
- --
- --
- --
-
A
Dilutions (mL/mL)
STEP 4
---- ---- --- -- -- -
----------------
--
--
Reagents/ Materials Methanol C18SPE
Type I Water
Lot# NA
--
--
--
--
--
-
Initials/Date
-
-
CJcZ- oiloloH j1 -
- ..
--
--
--
--
-
HPLC
Methanol Ammonium Acetate
-
Type I water
NA
-
Initials/Date
STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes
o STEP 3: LC/MS/MS analysis
o STEP 4: LC/MS/MS reanalysis.
- D lH U iilO O D
K
*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
N
COMMENTS:
Final extracts stored in refrigerator 3 2 - _ Initials: C tE Date: O ^ Q ^ j o ^
July 19, 2001/4
3058 Research Drive State College, PA 16801
RC
Phone: 814-272-1039 Fax: 814-231-1580
PREPARATION OF EXTRACTED CALIBRATION STANDARDS
_ w l_ ,
E x y g e n s t u d y n o . j =.
Protocol No.: None Method No.: S i
Sponsor Sample
ID
NA
Exygen Sample
ID
0106020
Sample ' Description
Type I WaterA
Exygen Study No.: NA
Analytes:
PFHS. PFOS. PFOA
and FOSA
Fort. Solution
ID
Fort. Soin. Cone.
(ng/mL)
Fort. Volume
(uL)
Micropipet used (uL)
- - - -
Matrix:
Tvne I WaterA
Sample Vol: 40 mL
Fort. Level (ppt) .
Final Solution ID#**
- XC010804-0
Reagents/ Materials
Methanol
Lot# 'H330&5HS
NA 0106020 T ypeIW aterA . F121603-2 10
100 200
25 XC010804-1
C18 SPE W 3ife13 1
NA
0106020
Type I WaterA F121603-2
10
200 200
50 XC010804-2 Type I Water
NA
NA
0106020
Type I WaterA F121603-2
10
400 200 100 XC010804-3
-
-
NA 0106020 Type I WaterA F121603-1 100
100 200 250 XC010804-4
-
-
NA
0106020
TypeIW aterA F121603-1
100
200 ..
200
500 XC010804-5
-
-
NA
0106020
Type I WaterA F121603-1
100 400
200 1000 XC010804-6
-
-
- - - - - --- fif ,
- - - - - - - - - Initials/Date:
Vertical arrows in a column indicate identical values.
**This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3. etc.
Samples removed from<jefrigeralSr^ freezer # ,5 2 - Time: CPiOO
Initials/Date: f'E S lOijaHl&I
40 mL of each sample measured using a S O mL graduated cylind After measuring, samples returned tgTefngemTgp/ freezer # S i
Initials/Date: Initials/Date:
! 0sh'Ajr)4 lijojrti
T H IS IS AN EXACT COPY OF THE ORIGINAL. DOCUMENT.*
Samples fortified: SPE clean-up (omitting 40% Wash):
Initials/Date: Initials/Date:.
DATE
Final volume adjusted to 5 mL:
Initials/Date: Q E S I6ijo& jo{
Extracts placed in refrigerator #
Initials/Date: C S E /Oljii&l/'ytf
STANDARD EXPIRATION DATE: 1/22/03
rvimments:
AThis type I water has been filtered through a hypercarb filter
$$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water
July 10,2001/0
0000
'* 1 1 ! 1 I \ T }
Masslynx - Sample List
Sample List: C:\MASSLYNX\Fluorochemicals.PRO\SampleDB\010804B Daikin Water.SPL
Printed: Wed Je. 14 09:49:11 2004
____________________________
Vial File Name LIMS ID Client ID Sample Description
1 1 010804B-801 _ 2 2 010804B-802 -- 3 3 010804B-803 -- 4 4 010804B-804 --
5 5 010804B-805 --
6 6 010804B-806 -- 7 7 010804B-807 -- 8 92 010804B-808 -- 9 31 010804B-809 -- 10 32 010804B-810 -- 11 33 010804B-811 -- 12 2 010804B-812 -- 13 3 010804B-813 -- 14 34 010804B-814 -- 15 35 010804B-815 -- 16 36 010804B-816 -- 17 37 010804B-817 -- 18 38 010804B-818 -- 19 4 010804B-819 -- 20 39 010804B-820 -- 21 40 010804B-821 --
22 41 010804B-822 -- 23 42 010804B-823 -- 24 43 010804B-824 -- 25 5 010804B-825 --
26 6 010804B-826 --
27 7 010804B-827 TM
--
--
--
--
--
--
--
--
--
-- -- -- -- -- -- -- -- -- --
--
--
--
--
--
--
--
...
XC010804-0, 0 ng/L standard XC010804-1,25 ng/L standard XC010804-2, 50 ng/L standard XC010804-3,100 ng/L standard
XC010804-4,250 ng/L standard XC010804-5, 500 ng/L standard XC010804-6,1000 ng/L standard Methanol Wash 0106020 Control
0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/L XC010804-1,25 ng/L standard XC010804-2, 50 ng/L standard L1563-1 Spk C, 500000 ng/L, DF=10000 L1563-1, DF=1000 L1563-1 Rep, DF=1000 L1563-2, DF=1000 L1563-3, DF=1000 XC010804-3,100 ng/L standard L1563-1 Spk C, 500000 ng/L, DF=1000 L1563-1, DF=100 L1563-1 Rep, DF=100 L1563-2, DF=100 L1563-3, DF=100 XC010804-4,250 ng/L standard XC010804-5, 500 ng/L standard XC010804-6,1000 ng/L standard
000064
} 1
L\%3>txygen stu d y n o .
Page 1 Page Position: (1,1)
Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF
___ Blank
0
0 1___ ___
--
Standard
25
-- -- 01
--
Standard
50
-- -- 01
--
Standard
100
-- -- 01
--
Standard
250
-- -- 01
--
Standard
500
--- --
01
--
Standard
1000
-- -- 01
-- Blank
--
--
01
-- Blank
--
-- -- 01
-- QC
50 -- -- 0 1
-- QC
500 -- -- 0 1
--
Standard
25
-- -- 01
--
Standard
50
-- -- 01
-- QC
500000
--
--
0 10000
-- Analyte
...
-- -- 0 1000
-- Analyte -- Analyte
-- --
-- -- 0 1000 -- -- 0 1000
-- Analyte
--
-- -- 0 1000
--
Standard
100
-- -- 01
-- QC
500000
--
--
0 1000
-- Analyte
--
-- -- 0 100
Analyte
--
-- -- 0 100
Analyte - - - Analyte
-- --
-- -- 0 100 -- -- 0 100
--
Standard
250
-- -- 01
--
Standard
500
-- -- 01
Standard
1000
-- -- 01
\ 1) 1 l1 I i i T
Masslynx - Sample List
Sample List: C:\MASSLYNX\FluorochemicaJts.PRO\SampleDB\010804B Daikin Water.SPL Printed: Wed Jan 14 09:49:11 2004
MS Method HPLC Method MS Tune File Inj.Volume
1 PFOS AND PFOA Fluorochems Fluorochems 15 2 PFOS AND PFOA Fluorochems Fluorochems 15 3 PFOS AND PFOA Fluorochems Fluorochems 15 4 PFOS AND PFOA Fluorochems Fluorochems 15 5 PFOS AND PFOA Fluorochems Fluorochems 15 6 PFOS AND PFOA Fluorochems Fluorochems 15 7 PFOS AND PFOA Fluorochems Fluorochems 15 8 PFOS AND PFOA Fluorochems Fluorochems 15 9 PFOS AND PFOA Fluorochems Fluorochems 15 10 PFOS AND PFOA Fluorochems Fluorochems 15 11 PFOS AND PFOA Fluorochems Fluorochems 15 12 PFOS AND PFOA Fluorochems Fluorochems 15 13 PFOS AND PFOA Fluorochems Fluorochems 15 14 PFOS AND PFOA Fluorochems Fluorochems 15 15 PFOS AND PFOA Fluorochems Fluorochems 15 16 PFOS AND PFOA Fluorochems Fluorochems 15 17 PFOS AND PFOA Fluorochems Fluorochems 15 18 PFOS AND PFOA Fluorochems Fluorochems 15 19 PFOS AND PFOA Fluorochems Fluorochems 15 20 PFOS AND PFOA Fluorochems Fluorochems 15 21 PFOS AND PFOA Fluorochems Fluorochems 15 22 PFOS AND PFOA Fluorochems Fluorochems 15 23 PFOS AND PFOA Fluorochems Fluorochems 15 24 PFOS AND PFOA Fluorochems Fluorochems 15 25 PFOS AND PFOA Fluorochems Fluorochems 15 26 PFOS AND PFOA Fluorochems Fluorochems 15 27 PFOS AND PFOA Fluorochems Fluorochems 15
000065
1III
}3
}]
Exygen STUDY N O . U S b S
Page 2
Page Position: ( 2 ,1)
LC/MS/MS SYSTEM AND OPERATING CONDITIONS
Sponsor Protocol No: N A
Exygen Study No: LI 563
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) :
Analyst:
2 mM Ammonium Acetate in Type I Water Methanol
Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580
ov
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
000066
Scanning Method Report
C* Method:
C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\PFOS AND PFOA
Last Modified: Fri Jan 17 14:09:44 2003
Printed:
Wed Jan 14 09:50:04 2004
Solvent Delay ( mins ) :
0.00
Analog Channel 4 : Unused
Function : 1
M R M of 2 Mass Pairs ( ESP- )
Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins } : Repeats :
Channel Parent Daughter
0.03 0.00
0.00 8.00 1
Dwell
(Secs) Coll Energy
(eV)
1 413.00 369.00 0.20
2
499.00 99.00
0.20
10 40
Cone ( V )
10 30
Page 1
I
000067
Method Report
Method File: Last Modified:
C j\MASSLYNX\FLUOROCHEMICALS. PRO\ACQUDB\Fluorochems Wednesday, January 14, 2004 09:48:05
Page 1
Printed: HP1100 LC Pump Initial Conditions
Wednesday, January 14, 2004 09:50:15 i.X/)..! , ./
Solvents A% B% C% D%
60.0 40.0
0.0 0.0
Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C)
0.300 14.0
0 400
35.0 35.0
HP1100 LC Pump Gradient Timetable
The gradient Timetable contains 9 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 0.400 400
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
HP1100 LC Pump External Event Timetable
The Timetable contains 6 entries which are
Time Initial
0.00 0.05 0.10 7.95 8.00
Column Switch Contactl Off . Off Off On Off Off Off Off Off Off Off Off
Contact2 Off Off Off On Off Off
Contact3 Off Off Off Off On Off
Contact4 Off Off 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
0.50 14.00 15.0 43
Tuning Method Report
Method:
C :\MASSLYNX\FLUOROCHEMICALS. PRO\ACQUDB\FLUOROCHEMS
Printed:
Wed Jan 14 09:50:30 2004
Page 1
SOURCE ( ESP- )
Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp.
Set Rdbk
3.00 20 0.0 0.0 0.0 100 300
-2.92 -21
99 305
Pressures
Analyser Vacuum Gas Cell
Rdbk
OFF 3.5e-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 Rdbj
14.0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650
12 14 16
-64
Rdbk
131.8 758.6
000069
Quantify Calibration Report Study No.:L1563, Set N o . :010804B, Ext.Date:01/08/04, AnalysttK.Risha
Page 1
Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\010804B Daikin Water
Exygen Research, 3058 Research Drive, State College, PA 16801
000070
Quantify Calibration Report Study No.:L1563, Set No.:010804B, EKt.Date:01/08/04, Analyst:K.Risba
Page 2
Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\CurveDB\010804B Daikin Water
Last modified: Thu Jan 15 08:19:27 2004
Printed:
Thu Jan 15 10:46:37 2004
Exygen Research, 3058 Research Drive, State College, PA 16801
000071
Quantify Sample Report Study No.:L1563# Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 1
Sample List: Last modified: Method: Last modified: Job Code:
Printed:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FR0\SampleDB\010804B Daikin Wate:
Thu Jan 15 08:09:45 2004
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO \MethiDDBB\\P>FOS and PFOA 010804 Thu Jan 15 08:12:08 2004
Thu Jan 15 10:46:39 2004
Initials
Data m l ' - r x - y . __________ ___________
Run*
Tn 0\tfcCHE>~ BIT
Name: 010804B-801 Text:
1: PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College PA 16801
000072
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 2
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Wate: Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-802 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000073
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Rage 3
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Watei
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-803 Text:
1 : PFOS
2 : PFOA
XC010804-2,50 ng/L standard
010804B-803 Sm (M n, 2x3)
10&1
14-Jan-2004 11:02:47 LC/MS/MS #6
MRM o f 2 Channels ES5.22 413 >369
1.05e5 A re a
1.00
2.00
3 .0 0
T T --T
4.00
' 1 1 l 1 1 r . p ".-!--r-p r-
5.00
6.00
p rrp i p 7.00
Tim e
Exygen Research, 3058 Research Drive, State College, PA 16801
74
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 4
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFQA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-804 Text:
1: PFOS
XC01 0804-3,100 ng/L standard
0108<34B-804 Sm (Mn, 2x3) 10CH
%:
o-^ I 1 1 I f 1T"' .1' '_T 'T-- T p r , r i J I T T l
11 1 1 11
r1
1.00 2.00 3.00
2 : PFOA
XC0110804-3,100 ng/L standard
0108(D4B-804 Sm (Mn, 2x3) lo o
ker
5.44 180^
14-Jan-2004 11:18:26
LC/MS/MS #6
MRM of 2 Channels ES499 > 99 1.20e4 Area
4.00
| r- i Timer - T ' , - r I n - n - r - | - r-1--r- r-j- i - r - 1 - r - ( -r i t i p i v i r
ii
5.00 6.00 7.00
5.22
14-Jan-2004 11:18:26 LC/MS/MS #6
MRM o f 2 Channels ES413 >369 1.79e5 A re a
0~ 1 1 1 1 1 1 < 1 1 1 ` 1 1 1 1 111 1 1 1 1 11 11T1 r 1 r-i~1
1.00
2 .0 0
3.00
4.00
I n rriT T T T ! ,.,i ! , , r 1 , t 1r , r-| i-i 1 Tim e
5 .0 0
6.00
7 .0 0
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 5
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-805 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
00007S
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 6
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate: Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-806 Text:
1 : PFOS
Exygen Research, 3058 Research Drive State College PA 16801
000077
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 7
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-807 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000078
Quantify Sample Report Study No.:L1563, Set N o . :010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 8
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFQA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-808 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, AnalystsK.Risha
Rage 9
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-809 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000080
Quantify Sample Report Study No.:L1563, Set No.:010804B, E x t .Date:01/08/04, Analyst:K.Risha
Page 10
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-810 Text:
1 : PFOS
0106020 Spk A, 50 ng/L
0108<D4B-810 Sm (Mn, 2x3) 100n
%:
14-Jan-2004 12:52:36
LC/MS/MS #6
5.22
MRM of 2 Channels ES4 1 3 > 369 9.74e4 Area
0 , , , , I . 1I TI i-i 11I 1I 11I I 1 r 1 111111111 11111.i'_,"`r"r 111111l ''"1.H 1 1 1 1 I 1 1 I 1 I 1 I 1 1 I 1 1 1 1 I 1 1 1 1 Tim e
1.00
2.00
3.00
4.00
5.00
6.00
7.00
Exygen Research 3058 Research Drive State College PA 16801
000081
Quantify Sample Report Study No. :I>1563, Set No.:010804B E x t .Date:01/08/04, Analyst :K .Risha
Rage 11
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Watei
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-811 Text:
1 : PFOS
0106020 Spk B, 500 ng/L
010804B-811 Sm (Mn, 2x3)
100n
5.23
%:
0 ' TT I I I I I I I ITTI | I I I I | I I I I | 1.00 2.00
!---I---j---I---I---I---I---j---I---I---I---1---|---I---I---I---I---| I l I ! |
3.00
4.00
5.00
14-Jan-2004 13:08:19 LC/MS/MS #6
MRM of 2 Channels ES413 >369 8.21 e5 Area
1) - 1"i 11 ' ' I i" i"I"'i'"*.' ' Time
6.00
7.00
Exygen Research 3058 Research Drive State College, PA 16801
Quantify Sample Report Study N o .:L1563, Set No.:010804B Ext.Date:01/08/04, AnalystrK.Risha
Page 12
Saiqple List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-812 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College PA 16801
Quantify Sample Report Study No.:L1563, Set N o . :010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 13
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-813 Text:
1 : PFOS
2 : PFOA
XC0110804-2, 50 ng/L standard
0108<D4B-813 Sm (Mn, 2x3) 10Ch
%:
0 ' 1.00 ' 2.00 ' 3.00
14-Jan-2004 13:39:38 LC/MS/MS #6
MRM of 2 Channels ES5.22 413 > 3 6 9
1.03e5 Area
1
11' ' I * 1I "* 1` 1 ' 1 i 1 1 ` `
4.00
5.00
1 i-'i 1 1 i 111-1 * '1 '1 [ i'TT-r 1' r i l t* Time
6.00
7.00
Exygen Research 3058 Research Drive State College, PA 16801
000084
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 14
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Wate: Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-814 Text:
1 : PFOS
2 : PFOA
L1563-1 Spk C, 500000 ng/L, DF=10000
010804B-814 Sm (Mn, 2x3) 10Ch
%:
0-W -i i fT T i 1- f 111I 1111I 11'"I" I', r i I T T n I I ' I I
1.00
2.00
3.00
4.00
5.22 4281^^
14-Jan-2004 13:55:25
LC/MS/MS #6
MRM of 2 Channels ES413 >369 1.91e5 Area
111111111111-r r 1 1 I 1 I 1 1 1 1 r i"i 1 1 1 1 1 1 1- Time
5.00
6.00
7.00
Exygen Research, 3058 Research Drive, State College, PA 16801
000085
Quantify Sample Report Study No.:L1563# Set No.:010804B, Ext.Date:01/08/04, AnalystsK.Risha
Page 15
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Watej Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S anri p f q a 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-815 Text: 1 : PFOS
L1563-1, DF=1000
0108<D4B-815 Sm (Mn, 2x3) 100:
%:
5.43.
96^^
14-Jan-2004 14:11:02 LC/MS/MS #6
MRM of 2 Channels ES-
499 > 99
4.65e4 Area
0- *i *1* * i 1rTr i r 1r'r i
1.00
2.00
2 : PFOA
111i 111 ........ ' 1
3.00
4.00
5.00
L 'i 111i 111 f ' ~ ! m . . i TTime
6.00
7.00
Exygen Research, 3058 Research Drive State College PA 16801
000086
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risila
Page 16
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-816 Text:
1 : PFOS
Exygen Research, 3058 Research Drive State College, PA 16801
000087
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 17
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Watei
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFQA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-817 Text: 1 : PFOS L156 3-2, D F=1000
0108<34B-817 Sm (Mn, 2x3) 100:
%:
5.43
6263~k
14-Jan-2004 14:42:35
LC /M S /M S #6
MRM of 2 Channels ES499 > 99 2.99e4 Area
11i i ' i i ' 1 ' 111i 1 1 11 1111i 1111 1111i 1111i i rr i | i i i i | i i n | i
1.00
2.00
3.00
4.00
5.00
6.00
7.00
nj i t | ime
2 : PFOA
L1563-2, DF=1000
0108134B-817 Sm (Mn, 2x3) 100n
%~
5.22 4 5 8 ^^
14-Jan-2004 14:42:35 LC/MS/MS #6
MRM of 2 Channels ES413 >369 1.93e5 Area
u - 1W r - r - p T T T i ! T T T r 1 i - r i I 1 T"T=r=f=j i l l l j I i i i
1.00
2.00
3.00
4.00
| , T l-T |' T 1 '1 1
5.00
'' T I ' I "1...r n r |...t'-'t r -r j i i r T ^ i - r r r '
6.00
7.00
lim e
Exygen Research 3058 Research Drive State College, PA 16801
000088
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Rage 18
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate: Last modified: Thu Jan 15 08:09:45 2004
Method:
B:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Mama: 010804B-818 Text: 1: PFOS
L1563-3, DF=1000
010804B-818 Sm (Mn, 2x3) 100]
/c r
14-Jan-2004 14:58:25 LC/MS/MS #6
MRM of 2 Channels ES5.44 499 > 99
4.59e4 Area
0-* = '" I I I I i I I I I -f I - I ! r I I | ' I -T " f i I TT-) , I , I I , I" ! !"] I
1.00
2.00
3.00
4.00
2 : PFOA
1 1 I 1 1 1 1 I-1 r r 1 I - r
5.00
6.00
7.00
Time
Exygen Research 3058 Research Drive State College, PA 16801
000089
Quantify Sample Report Study No.:L1563, Set No.:010804b , Ext.Date:01/08/04, Analyst:K.Risha
Rage 19
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Wate]
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-819 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 20
Sample List: P:\Data\DCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Watei Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\IiCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Bast modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-820 Text:
1 : PFOS
2 : PFOA
L1563-1 Spk C, 500000 ng/L, DF=1000
010804B-820 Sm (Mn, 2x3) 10Ch
5.22
%:
1O ' '>" I-- i-- I-- F t 5*!-- I I I I-- I-- I-- I-- I I I I I-- !-- r-T -- I-- p n -- I-- l~ [ ~ i-- !-- r 1.00 2.00 3.00
4.00
5.00
14-Jan-2004 15:30:03 LC/MS/MS #6
MRM of 2 Channels ES413 >369 1.73e6 Area
[-r-i T--r-,[ r i i i j i i I I Time
6.00
7.00
Exygen Research, 3058 Research Drive, State College, PA 16801
000091
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 21
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Watea Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-821 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive State College, PA 16801
000092
Quantify Sample Report Study No.:Ll563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 22
Sample List: Last modified: Method: Last modified: Job Code:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Watej Thu Jan 15 08:09:45 2004 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804 Thu Jan 15 08:12:08 2004
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-822 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:L1563, Set No.:010804B, Ext.Bate:01/08/04, Analyst:K.Risha
Rage 23
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-823 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
000094
Quantify Sample Report Study H o . :1.1563, Set No.:010804B Ext.Date:01/08/04, Analyst:K.Risha
Page 24
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Watei Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Harne: 010804B-824 Text:
1 : PFOS
L1563-3, DF=100
010804B-824 Sm (Mn, 2x3) 100i
5.43 96675
14-Jan-2004 16:32:54 LC/MS/MS #6
MRM of 2 Channels ES499 > 99 4.25e5 Area
1.00
2 : PFOA
L1563-3, DF=100
2.00
010804B-824 Sm (Mn, 2x3) 100-1
%:
0-' r r r v |T T T r| i i t . | i i ! i | i
1.00 2.00
3.00 3.00
I I IIIrI
4.00
5.00
5.22
4.00
5.00
6.00
7.00
T im e
14-Jan-2004 16:32:54 LC/MS/MS #6
MRM of 2 Channels ES413 >369 9.38e6 Area
6.00
n -' ' * I 1* 1I 1111 Time 7.00
Exygen Research 3058 Research Drive, State College, PA 16801
000095
Quantify Sample Report Study No.:1.1563, Set No.:010804B, E x t .Date:01/08/04, Analyst:K.Risha
Page 25
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Watei Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PPOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-825 Text:
1 : PFOS
2 : PFOA
Exygen Research, 3058 Research Drive, State College, PA 16801
Quantify Sample Report Study No.:il563. Set No.:010804B, Ext.Date:01/08/04, Analyst:K. Ri sha
Page 26
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\010804B Daikin Wate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Name: 010804B-826 Text:
1: PFOS
XC010804-5, 500 ng/L standard
010804B-826 Sm (Mn, 2x3) 100n
%\
5.22 1296771
1
i
14-Jan-2004 17:04:17 LC/MS/MS #6
MRM of 2 Channels ES413 >369 8.10e5 Area
0 J i - .I` T T 'i n T " i ' I t1 II I iI'1 )I Ii-'i[--rI I 1r iI I! '1I I 1 TT""Ii Ii rI" iI iI iI iI iI iI iI 1I tr -i 1 1I r rp" ii'1 iI i~~ tt-- |i..ri rrr "i i1i,r ^ ^ ^ >p 'i '`i i - r"-|'r Ti 'in \ r r|` "ii i i""<i ' | i 11
it titi
1.00 2.00 3.00 4.00_______5TX)______ a 0 0 ______ 7XX)
T im e
Exygen Research, 3058 Research Drive State College, PA 16801
Quantify Sample Report Study Ho.:L1563, Set No.:010804B, Ext.Date:01/08/04, Analyst:K.Risha
Page 27
Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\010804B Daikin Hate:
Last modified: Thu Jan 15 08:09:45 2004
Method:
P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOA 010804
Last modified: Thu Jan 15 08:12:08 2004
Job Code:
Printed:
Thu Jan 15 10:46:39 2004
Harne: 010804B-827 Text:
1 : PFOS
XC010804-6,1000 ng/L standard
010804B-827 Sm (Mn, 2x3) 10Ch
14-Jan-2004 17:19:58 LC/MS/MS #6
MRM of 2 Channels ES499 > 99 1.36e5 Area
ri il IIIr-T 11f 1.00
2 : PFOA
- r c i i - i - r | t --i--r i r
2.00
3.00
1 1'i 1 1 p I 1
I 1-
4.00
5.00
6.0Q
7.00
t t - Time
Exygen Research, 3058 Research Drive, State College, PA 16801
