Document DDGm6JVwV5LGg82XR6491LxVN
Proven Results.
4 R &<86 - I 7 0 3
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n Analytical Report
1*P* j*! Fluorochem ical Characterization of Water Sam p les Daikin America Well Installation
Exygeh R esearch Laboratory Report No. L0001309
2fe- a Testing Laboratory Exygen Research
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Requester John Simmons E. Roberts Alley and Associates 210 N. Atlanta Boulevard Sheffield, AL 35660
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Results are reported for the analysis of water samples received by Exygen Research (Exygen) from E . Roberts Alley and Associates. The Exygen study number assigned to the project is L0001309.
Specific fluorochemical characterization by liquid chromatography / tandem m ass spectrometry (LC/MS/MS) was requested for all sam ples. A total of 4 sam ples were received for analysis.
The sam ples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals:
T able 1: T arget Analysis
Compound Name Perfluorooctanoic Acid
Acronym C8 Acid fPFO A)
The analytical methods used were originally developed for groundwater sam ples and were validated by Exygen. The validation protocol and results are on file with Exygen.
2 Sample Receipt
The sam ples were submitted in plastic containers. All sam ples 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. Sam ples were collected on 11/12/03. Chain-of-custody information is presented in Attachment C.
3 Holding Times
Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Sam ples were analyzed within 30 days of receipt.
4 Methods - Analytical and Preparatory
4.1 LC/MS/MS
4.1.1 Sample Preparation for LC/MS/MS Analysis
Sam ples were initially treated with 200 uL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (S P E ) was used to prepare the sam ples for LC/MS/MS analysis. A forty-milliliter portion of sample was used for analysis. The samples were transferred to a C18 S P E 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
000004:
4.1.2 Sample Analysis by LC/MS/MS
In H PLC, 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 H PLC separation, ES/M S provides a rapid and accurate m eans 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 known fluorochemicals are observed and quantitated against standards.
A Hewlett-Packard H P1100 H PLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM ). Sam ples were extracted on 11/19/03 and analyzed on 11/26/03. Raw analytical data is provided in Attachment D.
5 Analysis
5.1 Calibration
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 sam e S P E procedure used for sam ples.
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.
All calibration criteria were met for this analysis.
5.2 Blanks
Extraction blanks were prepared and analyzed with every extraction batch of sam ples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these sam ples, 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 sam ples. 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 Sp ikes
A matrix spike was prepared for sample MW-2. Matrix spike recoveries are given in Attachment B .
PAGE30F5 0 0 0 0 0 5
5.5 Duplicates
Sample MW-2 was analyzed in duplicate. The duplicate results are included with the sample results in Attachment A.
5.6 Laboratory Control Sam ples
For LC/MS/MS analyses, Milliq water w as spiked with all compounds with each extraction set. All recoveries for all compounds were between 70-130% in each LC S . 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 million (ppm) (ug/mL).
7 Data/Sample Retention
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
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-- Analytical. ^
Report 1
Proven Results.
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n Sum m ary of PFO A in Water Sam ples
t. i Analyte Found (pg/mL)
n Sample ID
PFOA
(t5 ''J'
, MW-2 \ MW-2*
0.0664 0.0668
\ MW-4
0.952
\ Duplicate
0.0772
1:
, Trip Blank
ND
r\ j[ j ` Laboratory. Duplicate
ND = Not Detected. Response between 0 and 0.00005 pg/mL.
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exygen.com
STANDARD TERMS A N D CONDITIONS
Services provided by Exygen Research are limited to th e terms and conditions stated herein, unless otherwise agreed to in a formal contract.
CONFIDENTIALITY-- Exygen Research ("Exygen," "us," or "we") maintains the strictest confidentiality in all of our client interactions. If a signed confidentiality agreement Is required, vve 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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BILLING--AH 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 payment 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 original!y 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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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 p'ovide chain-of-custody forms for client's use.
All samples submirted must be accompanied by: purchase order, or signed quotation: sample description, including sample type, source, time and date of collection; specific analyses requested; estimated concentration levels; requested report date; current billing address; and other relevant information.
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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 sample(s). Exygen shall charge a monthly fee for long-term storage. Samples found or suspected to contain hazardous waste, according to definitions in state and /or federal guidelines, will be returned to the client upon completion of 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 of 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 locked, temperature-controlled conditions. An internal chain-ofcustody is maintained for each lot of samples received.
HAZA R D CO M M U N IC A TIO N --Ih e client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law.
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ACCEPTANCE O F PURCHASE ORDER--1ms Purchase Order becomes a binding agreement, subject to the specific terms and conditions, stated herein, upon Exygen's commencement of work.
QOOOO[
Recovery Sum m ary for PFO A in Water
PFOA
: 4 Amount Amt Found Amount
Sample
Spiked in Sample Recovered Recovery
Description
(ng/mL) (ng/mL) (ng/mL)
(%)
MW-2 500 ng/mL Spike
500 66.4
630 113
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3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
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Login Group: L0001309
Login #:
L0001309> 1,419
Project:
P0000440
Project Storage: Refrigerated
Submitted By: John Sim mons
Status:
U n rece ived
r . Login Type: Started:
Immediate Receipt of Sam ples T
Date Start:
11/14/2003 11:20:09AM
Due Date:
11/28/2003
Received Date: 11/14/2003
Received By:
AMMERMAN, M ARK
Spread Sam ple:
r~ Label:
Project Title/Type: PFO A in Soil and W ater / RO U TIN E
Conform C O C Sam ple: Conform C O C : Conform Sam ple: Conform Request:
Login Notes: r~ Conform Notes:
True True True True
Package /`
. K0001883
<n Container # C0019853 C0019854 C0019855 C0019856
Packages / Containers
Mail Date / Condition
Shipper/ IP
Temp. Control / Temperat
11/14/2003 10:30:58AM Package &Contents Uncompromised
FEDEX 842521251084
REFRIG
0.00
Gross Weight
1135.4 g 1145.2 g 1136.2 g
531.9 g
pH Container Type
1000 ml Amber Plastic 1000 ml Amber Plastic 1000 ml Amber Plastic
500 ml Clear Plastic
Preservative
NONE NONE NONE NONE
Mfg. Lot
Direction / Handled By RECEIVED
AMMERMAN, MARK
Mfg. ID
Miscellaneous Item Key
None
Description
ICOC
H Sample ID * L0001309-0001
L0001309-0002 L0001309-0003 f L0001309-0004
Matrix LIQUID LIQUID LIQUID LIQUID
Fraction Water Water
Water Water
Sample MW-2 MW-4
Duplicate Trip Blank
Sam p les
Date Sampled Date Received 11/14/2003 11/14/2003 11/14/2003 11/14/2003
Date Due 11/28/2003 11/28/2003 11/28/2003 11/28/2003
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Report Version: Nov 13 2003 4:51PM Page 1 of 2
Instance:
R0072814
R0072814
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C o n ta in e r ---C0019853 /1000 ml Amber Plastic/ NONE
H
L0001309-0002
Container | ;C0019854 /1000 ml Amber Plastic / NONE
H>001309-0003
` Container CO019855 /1000 ml Amber Plastic / NONE
pm*'
1001309-0004
C o n ta in e r C0019856 / 500 ml Clear Plastic / NONE
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Report Version: Nov 13 2003 4:51PM Page 2 of 2
000012
Instance:
R0072814
R0072814
C T0000
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
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PROJECT INFORMATION
ANALYSES REQUESTED
Client (name
_________
P I P A ),
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Phone: ,.
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Fax: U Z lA U . 3 $ \ \ ? ______
Sam p ler:
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Project Manager (Name & E-mail Address):
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_________
Project Naaime:
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RO. #: M 7 / ^ ) ^ - D 68Z -A -OP!
Quotation # : _________________________
Please fill out this form completely to ensure correct analysis and proper handling of your samples.
SAMPLE ANALYSI
"SWw A tS ip if
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Client Sample Identification
/ V S-Z . M S I - 1/ lSr.O 1*CA^,.. a 'A J M -
Collection Collection
Date
Time
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LAB USE ONLY
Relinquished^
OTHER INFORMATION
Date
Time
Il/l-z/3 H :aO
Cooler ID #
Cooler Temp. (C)
_____ ;_______________________________ J--1--Sjj S S t lS
LAB USE ONLY
L.
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PROJECT REQUIREMENTS Results Deadline:
Laboratory Report Options: Q Sample results only Add case narrative O Add quality control summary Add calibration summary Add raw data Other______________________
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R E C IP IE N T : P E E L H ER E
000014
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SRFRev. Date4/02*Part#TS76tOS*<E1994--2002FedExPRINTEOINUSA
Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site:
NA L1309 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:
111903C Karen Risha LC/MS/MS Unit # 7 11/19/03 11/26/03
Exygen ID
XCl 12403-0 XC112403-1 XCl 12403-2 XCl 12403-3 XCl 12403-4 XCl 12403-5 XCl 12403-6 Methanol Wash 0106020 Control
L1309-4 0106020 Spk A 0106020 Spk B
XCl 12403-1 XCl 12403-2 XCl 12403-3 L1309-1 SpkC
L1309-1 L1309-1 Rep
L1309-2 L1309-3 XCl 12403-4 XCl 12403-5 XCl 12403-6
Sponsor ID -
-
-
-
NA Trip Blank NA NA MW-2 MW-2 MW-2 MW-4 Duplicate -
-
-
Sample Code
c CS CS CS CS CS CS C c c LCS LCS CS CS CS LF
s s s
s
CS CS CS
Run No. 111903C-2001 11193C-2002 111903C-2003 111903C-2004 111903C-2005 111903C-2006 111903C-2007 111903C-2008 111903C-209 111903C-2010 111903C-2011 U1903C-2012 111903C-2013 111903C-2014 111903C-2015 111903C-2016 111903C-2017 111903C-2018 111903C-2019 111903C-2020 11903C-2021 111903C-2022 111903C-2023
PFOA Found (ng/L) = (peak area - intercept) / slope x DF
Recovery (%) =
fPFOA 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 1 1000 100 100 1000 100 -
x 100
Peak Area 733 4963 9860 18693 46259 95288 181530 793 429 794 9603 94364 4851 9677 19243 115087 121191 121939 173514 140949 45747 93963 176391
PFOA Found (ng/L)
Amount PFOA Added (ng/L)
Recovery (%)
- --
- ---- -*
-
-
ND ND 49.8 516 630000 66400 66800 952000 77200 -
-
50 500 500000 -
-
-
-
100 103 -
-
113
-
-
-
- --
Standard Curve : Linear (I/x weighted) Intercept = 558.878 Slope = 181.756
Coef. Of Det. = 0.998740
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:
ff"5'
3058 Research Drive
Phone: 814-272-1039
H
RESEARCH
State College, PA 16801
Fax: 814-231-1580
Internal Chain of Custody/Fortification Sheet
Exygen Study Number:
L1309
Matrix: Water
Sponsor Study/Protocol No: NA
The samples listed below were removed from refrigerator No.
Time tr7QO
aDate 1' D3_
Initials
4
CLIENT SAMPLE ID
EX Y G EN ED NU M BER
VOLUM E (mL) FORTIFICATION (ng)
na
0106020 Control
40.0
_
na
0106020 Spk A
40.0
2.0
?:
na
0106020 Spk B
40.0
20.0
MW-2 MW-2 MW-2 MW-4
L1309-1 SpkC L1309-1
L1309-1 Rep L1309-2
40.0
20000.0
40.0 _
40.0 _
40.0 _
t Duplicate Trip Blank
-
-
f-
-
-
H -
-
-
r-
-
-
LI309-3 LI309-4
-
40.0 40.0
-
_
_
_ _ -
-
__ _, -_ _-_ __ __
t,
- --
Spiking Solution Used
Volume Used for Spiking Initial/Date
0106020 Spk A
F092203-5 (10 ng/mL)
200 pL (200 pL micropipet)
W r ' n fttaa
0106020 Spk B
F092203-4 (100 ng/mL)
200 pL (200 pL micropipet)
W k /u w o-
LI309-1 SpkC
F092203-1 (100000 ng/mL)
200 pL (200 pL micropipet)
/njw )oa
i1 - - _
- -_
- _ __
- - - '-
A ll samples were measured:
Time m O ______
Date l\|\^ l |o 3
n
Initials.
After measuring samples were returned to refrigerator N o. 3 2
Time Vo2 47______
Date
Initials
C om m ents: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date:
Analysis Summary:
Data Set: W fS&C'
Data Set: --_____
Data Set:
Set extraction/analysis data verified by:. D -t.
Initials/Date:. &
Initials/Date: --^ Initials/Date:
/ w\&\03
Date: M / t S July 26, 2001/6
000016
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RESEARCH
3058 Research Drive State College, PA 16801
Phone: 814-272-1039 Fax: 814-231-1580
SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET
EXYGEN STUDY NUMBER: L1309 MATRIX: Water
METHOD: * ANALYTES: PFOA
PROTOCOL NUMBER: NA
Client ID
na na na MW-2 MW-2 MW-2 MW-4 Duplicate Trip Blank . -
-
_
-
Exygen ID
0106020 Control 0106020 Spk A 0106020 SpkB L1309-1 Spk C
L1309-1 L1309-1 Rep
L1309-2 L1309-3 L1309-4
-
STEP 1
____\ ( -
1-
STEP 2
. -
-
. j
Dilutions (mL/mL)
-- -- w -y M o v ,o 7 io ^'/lO O -X r
-- -
STEP 3
/ / \ -
*Initials/Date
- n ife
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.
l -b
f; I0DD
Dilutions (mL/mL)
-
-
-
--
STEP 4 -
-- -
--
Reagents/ Materials
Lot#
Methanol
H 3IZ3ZO
C18 SPE Type IWater
-
>2. NA -
_-
-.--
--
Initials/Date -
uP -U to 0 T3
--
-_-
--
--
--
--
HPLC
Methanol
Ammonium Acetate
Type I water
-
NA
Initials/Date
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.
Initials:
Date:
July 19, 2001/4
0 0 0 0 1 ,7
3058 Research Drive State College, PA 16801
Phone: 8i4-272-1039 Fax: 814-231-1580
PREPARATION OF EXTRACTED CALIBRATION STANDARDS
Exygen STUDY N O ,
Protocol No.: None Method No.: 01M-008-046*
Exygen Study No.: NA
Analytes:
PFOA
Matrix:
Type I WaterA
Sample Vol: 40 mL
Sponsor Sample
ID
NA
Exygen Sample
ID
0106020
Sample Description
Type I WaterA
Fort. Solution
ID
. Fort. Soin. Cone.
-
Fort. Volume
(uL)
-
Micropipet used
(ML)
Fort. Level (ppt)
-
Final Solution ID #**
XC112403-0
!
Reagents/ Materials
Methanol
Lot# H30I361
NA
0106020
Type I WaterA F092203-5
10
100 200
25 XC112403-1
C18 SPE vi3ibTh7~
NA
0106020
Type I WaterA F092203-5
10
200 200
50 XC112403-2 Type I Water
NA
NA
0106020
Type I Water'' F092203-5
10
400 200 100 XC112403-3
-
-
NA
0106020
Type I WaterA F092203-4
100
100
200
250 XC112403-4
-
-
NA
0106020
Type I WaterA F092203-4
100
200
200
500 XC112403-5
-
-
NA
0106020
Type I WaterA F092203-4
100
400
200 1000 XC112403-6
-
-
NA
0106020
Type I WaterA F102703-2
100
100
200 250 XC112403-7
I
- - - - - - - - - Initials/Date: Il ZHf
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^feffigerator)/ freezer # 37-___ Time: C/dQO
Initials/Date: (JFK / II
TH IS IS AN EXACT COPY OF
40 mL of each sample measured using a S b mL graduated cylinder.
Initials/Date: PEE / llh jo 3
THE ORIGINALDOCUMENT.'
After measuring, samples returned to ^rigerator/ freezer # ,-? 2 .. Time: I>30 Initials/Date: CEE /Mj2fp3
.date M
Samples fortified:
Initials/Date:.
SPE clean-up:
Initials/Date: t OE / lljlHjZ
Final volume adjusted to 5 mL:
Initials/Date: C fE / tjzdjcz
Extracts placed in refrigerator # c h i'
Initials/Date: 7B /
STANDARD EXPIRATION DATE: 12/8/03
r 'nmmpnts:
AThis type I water has been filtered through a hypercarb filter
* Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water.
July 10, 2001/0
Masslynx - Sample List
Sample List: C:\MASSLYNX\008 APF0.PR0\SampleDB\111903C.spl Printed: Wed Nov 26 08:20:07 2003 \ @ \ \ Q ^ _______________
Vial File Name
M S ID Client ID Sample Description
1 1 111903C-2001 2 2 111903C-2002 -- 3 3 111903C-2003 -- 4 4 111903C-2004 -- 5 5 111903C-2005 -- 6 6 111903C-2006 -- 7 7 111903C-2007 -- 8 92 111903C-2008 -- 9 51 111903C-2009 -- 10 52 111903C-2010 -- 11 53 111903C-2011 -- 12 54 111903C-2012 -- 13 2 111903C-2013 -- 14 3 111903C-2014 -- 15 4 111903C-2015 -- 16 55 111903C-2016 -- 17 56 111903C-2017 -- 18 57 111903C-2018 -- 19 58 111903C-2019 -- 20 59 111903C-2020 -- 21 5 111903C-2021 -- 22 6 111903C-2022 -- 23 7 111903C-2023 --
-- -- -- -- --
-- --
---
--
-- -- -- -- -- '-- -- -- -- -- --
--
XC112403-0, 0 ng/L standard XC112403-1, 25 ng/L standard XC112403-2, 50 ng/L standard XC112403-3,100 ng/L standard XC112403-4, 250 ng/L standard
XC112403-5, 500 ng/L standard XC112403-6,1000 ng/L standard Methanol Wash 0106020 Contrai L1309-4 0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/L XC112403-1, 25 ng/L standard XC112403-2, 50 ng/L standard X C 112403-3, 100 ng/L standard L1309-1 Spk C, 500000 ng/L, DF= L1309-1, DF=100 L1309-1 Rep, DF=100 L1309-2, DF=1000 L1309-3, DF=100 XC112403-4, 250 ng/L standard XC112403-5, 500 ng/L standard XC112403-6,1000 ng/L standard
Ooo
Exygen STUDY NO. L ^ \
Page 1 Page Position: (1,1)
Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF MS Method
____ -- -- -- -- -- -- -- -- -- -- -- -- -- --
=1000 --
-- -- -- -- -- -- --
Blank
Standard Standard Standard Standard
Standard Standard Blank Blank Analyte
QC QC Standard Standard
Standard QC Analyte Analyte
Analyte Analyte Standard Standard Standard
0 25 50 100 250 500 1000
--
--
--
50 500 25 50 100 500000
--
--
--
--
250 500 1000
-- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- --
. . . 0 1 008 PFOA
-- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA
-- 0 1 008 PFOA
-- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA
-- 0 1 008 PFOA
-- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA
-- 0 1 008 PFOA
-- 0 1 008 PFOA -- 0 1000 008 PFOA -- 0 100 008 PFOA -- 0 100 008 PFOA
-- 0 1000 008 PFOA -- 0 100 008 PFOA -- 0 1 008 PFOA
-- 0 1 008 PFOA -- 0 1 008 PFOA
> n 1 i l i nra r; r
Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO.RRO\SampleDB\111903C.spl Printed: Wed Nov 26 08:20:07 2003 ' *
HPLC Method MS Tune File Inj Volume (pL)
1
water
PFOATune 15
2
water
PFOATune 15
3
water
PFOATune 15
4
water
PFOATune 15
5
water
PFOA Tune 15
6
water
PFOA Tune 15
7
water
PFOATune 15
8
water
PFOATune 15
9
water
PFOATune 15
10
water
PFOATune 15
11
water
PFOATune 15
12
water
PFOATune 15
13
water
PFOATune 15
14
water
PFOATune 15
15
water
PFOATune 15
16
water
PFOATune 15
17
water
PFOATune 15
18
water
PFOATune 15
19
water
PFOATune 15
20
water
PFOA Tune 15
21
water
PFOATune 15
22
water
PFOATune 15
23
water
PFOATune 15
:r $
Exygen STUDY N O . 1136*1
" :i )
i
Page 2 Page Position: (2,1)
LC/MS/MS SYSTEM AND OPERATING CONDITIONS
Sponsor Protocol No: N A
Exvgen Study No: LI309
,
t*
Instrument:
Micromass Quattro Ultima (LC/MS/MS Unit #7)
rim
Computer:
COMPAQ Professional Workstation AP200
Software:
Microsoft Windows NT: Version 4 Build 1381: Service Pack 5
k 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
HPLC Column:
Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID:MA10464) (JONESCHROMATOGRAPHY: Part No. FK5962EJ)
i*S Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water 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:.
(P
i
000021
t. < Scanning Method Report
Method:
C:\MASSLYNX\008 APFO.PRO\ACQUDB\008 PFOA
Last Modified: Wed Mar 20 15:07:50 2002
I- *
Printed:
Wed Nov 26 08:20:13 2003
1 M
,
X
i ...... Solvent Delay ( mins ) :
0.00
X2>
U'
jp1 Function : 1
MRM of 1 Mass Pair ( ESP- )
Inter Channel Delay ( Secs ) : 0.03
Span ( Daltons ) : Start Time ( Mins ) :
0.00 0.00
End Time ( Mins ) :
8.00
Repeats :
1
Channel Parent Daughter Dwell (Secs) Coll Energy (eV) Cone ( V )
n 413.00 369.00
0.20
10
10
r*'
Page 1
,!**' .
IS*
!" :
] t
1**
000022
Method Report
Method File: Last Modified:
Printed:
C :\MAS SLYNX\008 APFO.PRO\ACQUDB\water Wednesday, November 26, 2003 07:39:50
Wednesday, November `26, 2003 08:20:21
iikf'"!1 HP1100 LC Pump Initial Conditions
Solvents
if3"
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 15.0
0 400
35.0 35.0
HP1100 LC Pump Gradient Timetable
f ; The gradient Timetable contains 10 entries which are.
Time
0.00 0.40
1.00
7.00
7.50
t > 9.00 9.50
13.50
14.00 n0,**1 15.00 'ttt i-.
A% 60.0 60.0 10.0 10.0
0.0 0.0 60.0 60.0 60.0 60.0
B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0
C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
HP1100 LC Pump External Event Timetable
n The Timetable contains 4 entries which are :
It i
Time Initial
0.00 0.10 8.00
Column Switch Contactl Off Off Off On Off Off Off Off
Contact2 Off Off On Off
D% 0.0 0.0 0.0 0.0 ' 0.0 0.0 0.0 0.0 0.0 0.0
Contact3 Off Off Off Off
Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300
Contact4 Off Off Off Off
HP1100 Autosampler Initial Conditions
Draw Speed
f0"": Eject Speed (/zl/min)
1h.
:
,
Draw Position (mm)
Stop Time (mins)
Injection Volume (^1)
Vial Number
Thermostat On
Thermostat Temperature(C)
200.0 200
0.10 15.00 15.0
1
12.0
i
I
Page 1
o3
Pressure 400 400 400 400 400 400 400 400 400 400
1
000023 1:
Tuning Method Report
Method:
C:\MASSLYNX\008 APFO. PRO\ACQUDB\PFOA TUNE
Printed:
W e d Nov 26 08:20:26 2003
Page 1
Dau 413.00
SOURCE ( ESP- )
Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp.
Pressures
Analyser Vacuum Gas Cell
Set Rdbk
3.00 10 0.0 0.0 0.0 100 300
-2.93' -10
101 300
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 Rdbk
14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700
8 9 11
-695
Rdbk
78.3 704.4
000024
n
P'' Quantify Calibration Report Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
Page 1
Exygen Research, 3058 Research Drive, State College, PA 16801 if6** .
I Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:11/19/03, Analyst:K.Risha
Rage 1
Sample List: P:\Data\LCMSMS7\Masslynx\008 ARFO.PRO\SampleDB\111903C
` Last modified: Tue Dec 02 08:11:40 2003
i ! Method:
P:\Data\LCMSMS7\Masslynx\008 APF. PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code :
In itials
I
Date T u o T F S ____________________________
Printed:
Tue Dec 02 08:14:58 2003
Run# Am 036-2001 To
{ , Name: 111903C-2001 ` Text :
'
r
xf ;
Ii \Exygen Research, 3058 Research Drive, State College, PA 16801
000026
Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
Printed:
Tue Dec 02 08:14:58 2003
Name: 111903C-2002 Text:
1 : PFOA
Page 2
Exygen Research, 3058 Research Drive, State College, PA 16801
000027
Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
Printed:
Tue Dec 02 08:14:58 2003
Name: 111903C-2003 Text:
1 : PFOA
Page 3
Exygen Research, 3058 Research Drive, State College, PA 16801
000028
n
", Quantify Sample Report Study No.:Ll309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
r*6 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
; : Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
f-- Job Code:
Printed:
Tue Dec 02 08:14:58 2003
Page 4
Name: 111903C-2004 Text:
XC112403-3,100 ng/L standard
t J. 1 1 1903C-2004 Sm (M n, 2x2)
\? K
100-
(t--S, Li
%:
5.49 18693
26-Nov-2003 16:37:55 LC/MS/MS #7
MRM of 1 Channel ES413 >369 3.91 e5 A re a
n I H h "T r I 1 i r- 1 I i i 1 i I 'r-1 I '1 "I r 1 -1 1 I i I i i I i i i-"t"IT- r I r j 1 I I i | I i i i | I I I i I.__i____i____I__1 I I I 1 1 I 1 I I I I I I____1____I____I_ 1 1 1 1 j Ti !mm~
1 .0 0
2 .0 0
3 .00
4 .0 0
5 .0 0
6 .0 0
7 .0 0
8 .0 0
i:
t: :
) ! >
P-
i
r
p:
M .
Exygen Research, 3058 Research Drive, State College, PA 16801
000029
r-i t Quantify Sample Report
-
' Study No.:L1309, Set No.:1 1 1 9 0 3 c , Ext.Date:ll/19/03, Analyst:K.Risha
^ 5 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
I Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
f--' Job Code:
l - - - - - '
-
Printed:
Tue Dec 02 08:14:58 2003
/**->
Name: 111903C-2005 Text:
1
Page 5
\\ ?f t:
ti
r1
f*.
r* t!
Exygen Research, 3058 Research Drive, State College, PA 16801
000030
Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
Printed:
Tue Dec 02 08:14:58 2003
Name: 111903C-206 Text:
1 : PFOA
Page 6
Exygen Research, 3058 Research Drive, State College, PA 16801
000031
j- : Quantify Sample Report f Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
j. Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dec 02 08:11:40 2003
i * Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
s Printed:
Tue Dec 02 08:14:58 2003
Rage 7
i j Name: 111903C-2007 \ Text : m 1 : PFOA
fr *
I*1 -3 X C 1 12403-6,1000 ng/L standard
tr 111903C -2007 Sm (M n, 2x2) ( 10Ch
%:
5.49 181530
26-NOV-2003 17:28:13 LC/MS/MS #7
MRM of 1 Channel ES 413 >369 3 .7 5 e 6 A re a
1.00
2.00
3 .0 0
4 .0 0
............. ...
5 .00
' M '
6 .0 0
7 .00
-H Tim e 8.00
t
n
i
nr 5
r* r-i
Exygen Research, 3058 Research Drive, State College, PA 16801
000032
| } Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:11/19/03, Analyst:K.Risha
I**, Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
, . Last modified: Tue Dec 02 08:11:40 2003
' Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
H Job Code: t.J .
Printed:
Tue Dec 02 08:14:58 2003
!i .
p ' Name: 111903C-2008 Text:
Rage 8
r<
Exygen Research, 3058 Research Drive, State College, PA 16801
r~>
000033
n
Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
Printed:
Tue Dec 02 08:14:58 2003
<r" i
f: ; * Name: 111903C-2009
Text :
Page 9
n
*>
(I i
Exygen Research, 3058 Research Drive, State College, PA 16801
000034
Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dee 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
Printed:
Tue Dec 02 08:14:58 2003
Name: 111903C-2010 Text:
1 : PFOA
Page 10
Exygen Research, 3058 Research Drive, State College, PA 16801
000035
Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:11/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
Printed:
Tue Dec 02 08:14:58 2003
Name: 111903C-2011 Text:
1 : PFOA
Rage 11
Exygen Research, 3058 Research Drive, State College, PA 16801
000030
Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, AnalystsK.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
Printed:
Tue Dec 02 08:14:58 2003
Page 12
Name: 111903C-2012 Text:
1 : PFOA
0106020 Spk B, 500 ng/L
111903C-2012 Sm (Mn, 2x2) 100-
m
%-
5.49 94364
26-NOV-2003 18:52:28 LC/MS/MS #7
MRM of 1 Channel ES413 >369 2.02e6 Area
n 11I * 1' ' I 11' 1I 1' ' ' I '"r 111 1T ,'-,-"r'1.1 111111*11 1111' 11I 11 r 11 111 1111 1' 111 ' 111 1 ' ' 11i Tim e
1.00
2.00
3.00
4.00
5.00
6.00
7.00
8.00
n n
t
#~i
Exygen Research, 3058 Research Drive, State College, PA 16801
oooor^^#
Quantify Sanale Report Study No. :L1309, Set No.:111903C, Ext.Date:ll/19/03, AnalystsK-Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dec 02 08:11:40 2003
Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
Job Code:
Printed:
Tue Dec 02 08:14:58 2003
Name: 111903C-2013 Text:
1: PFOA
Page 13
Exygen Research, 3058 Research Drive, State College, PA 16801
000038
^ Quantify Sample Report f ' Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
^ Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
f I Last modified: Tue Dec 02 08:11:40 2003
* Method:
P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA
Last modified: Fri Nov 14 10:37:34 2003
r--! Job Code:
Printed:
Tue Dec 02 08:14:58 2003
n 1 Name: 111903C-2014
Text:
Page 14
j*
P
f
o
i I1 '
Bxygen Research, 3058 Research Drive, State College, PA 16801
000033
Quantify Sample Report Study No.:Ll309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
Last modified: Tue Dec 02 08:11:40 2003
Method:
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Name: 111903C-2015 Text: 1 : PFOA
XC112403-3,100 ng/L standard
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Exygen Research, 3058 Research Drive, State College, PA 16801
000040
Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:11/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
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Exygen Research, 3058 Research Drive, State College, PA 16801
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Exygen Research, 3058 Research Drive, State College, PA 16801
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Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:ll/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
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Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:11/19/03, AnalystsK.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
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Exygen Research, 3058 Research Drive, State College, PA 16801
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Quantify Sample Report Study No.:L1309, Set No.:111903C, Ext.Date:11/19/03, Analyst:K.Risha
Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111903C
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Exygen Research, 3058 Research Drive, State College, PA 16801
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