Document 6wQnz5MOme60zrK92wyXMqr5R
Prep Run#: 105742
Team:
Petroleum HC/SMCDONALD
Number of Copies to make: 1
# Lab Code
Client ID
1 K1001011-001
Hagler W ell" Raw"
2 K1001011-020
Royce Street "Treated"
3 K1001011-019
Royce Street "Raw"
4 K1001011-018
Villa "Treated"
5 K1001011-017
Villa "Raw"
6 K1001011-016
Muldoon "Treated"
7 K1001011-015
Muldoon "Raw"
8 K1001011-014
Tennant `Treated"
9 K1001011-013
Tennant "Raw"
10 K1001011-012
Broad "Treated"
11 K1001011-011
Broad "Raw"
12 K1001011-010
Humphrey "Treated"
13 K1001011-009
Humphrey "Raw"
c 4 K1001011-008 K1001011-007
McAllister "Treated" McAllister "Raw"
16 K1001011-006
Airport North "Treated"
17 K1001011-005
Airport North "Raw"
18 K1001011-004
Spanish Trail "Treated"
19 K1001011-003
Spanish Trail "Raw"
20 K1001011-002
Hagler W ell" Treated"
21 KQ1000664-03 ` K1001011-007 MS
22 KQ1000664-04 ' K1001011-007 DMS
23 KQ1000664-01 J K1001011-008 MS
24 KQ 1000664-02 J- K1001011-008 DMS
25 KQ1000664-05 ^ LCS
26 KQ1000664-06 .J MB
t*reparation information encnsneet
Prep WorkFlow: OrgExtAq(14) Prep Method: Method
Status: Prepped Prep Date/Time: 2/9/10 07:34 AM
B# Method /Test
.01 PFOATFOA .02 PFOA/PFOA .01 PFOA/PFOA .02 PFOA/PFOA .01 PFOA/PFOA .01 PFOATFOA .02 PFOAPFOA .01 PFOA'PFOA .01 PFOAPFOA .01 PFOA'PFOA .01 PFOATFOA .01 PFOATFOA .02 PFOATFOA .01 PFOATFOA .02 PFOATFOA .01 PFOATFOA .02 PFOAPFOA .02 PFOAPFOA .01 PFOATFOA .01 PFOATFOA .02 PFOAPFOA .02 PFOATFOA .01 PFOATFOA .01 PFOAPFOA
PFOAPFOA PFOAPFOA
PH Matrix
W'ater Water Water Water Water Water Water Water Water Water Water Water W'ater Water Water Water Water Water Water Water Liquid Liquid Liquid Liquid Liquid Liquid
Amt. Ext.
200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL 200mL
Final Voi Sample Description
l.OOmL 1 OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL. l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL 1 OOmL 1 OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL l.OOmL
\
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Printed 2 9 10 14:29
Preparation Information Benehsheet
Page
Prep Run#: 105742
Team:
Petroleum HC/SMCDONALD
Spiking Solutions
Name: Perfluorinated Surfactant Isotopes 1ppm
K1001011-001 K1001011-007 K.1001011-013 K 1001011 -019 K Q 1000664-05
K 1 0 0 1 0 1 1-002 K 1 0 0 1 0 1 1-008 K 1 0 0 1 0 1 1-014 K 1 0 0 1 0 1 1-020 KQ 1000664-06
Preparation information tsencnsneet
Prep WorkFlow: OrgExtAq(14) Prep Method: Method
Status: Prepped Prep Date/Time: 2/9/10 07:34 AM
Inventory ID 5362
K 1 0 0 1 0 1 1-003 K1001011-009 K 1 0 0 1 0 1 1-015 KQ 1000664-01
lO.OOpL 10.00 p L 10.00 p L lo .o o p L
Logbook Ref: LCMS2-26C
K 1 0 0 1 0 1 1-004 K 1 0 0 1 0 1 1-010 K 1 0 0 1 0 1 1-016 KQ 1000664-02
o
K 1 0 0 1 0 1 1-005 K 1001011 -011 K1001011-017 KQ 1000664-03
o o
Expires On. 09/09/2009
K 1 0 0 1 0 1 1-006 K 1001011 -012 K 1 0 0 1 0 1 1-018 KQ 1000664-04
OOO OO o o o o o oooo o o o o
1
Name: Perfluorinated Surfactants Targets 2ppm
Inventory ID 13189
KQ1000664-01 lO.OOpL
KQ 1000664-02 lo .o o p L
KQ 1000664-03 lo .o o p L
Preparation Steps
Step: Started: Finished: By:
Extraction 2/9/10 07:34 2/9/1014:28 SMCDON'ALD
Logbook Ref: LCMS2-76P KQ 1000664-04 lo .o o p L
KQ1000664-05 lo.oo p L
Expires On: 10/29/2010
348
Comments:
Reviewed By: Chain of Custody
Relinquished By: Received By:
___ _______________
Printed 2 9 10 14:29
Date:
Date:
Date:
'
lo
( Yes/
Preparation Information Benchsheet
No
p to
Pagt
Preparation information isenchsneet
rep Run#: 105742
Prep WorkFlow: OrgExtAq(14)
Status: Draft
earn: Petroleum HC/SMCDONALD
Prep Method: Method
Prep Date/Time: 2/9/10 07:34 AM
Number of Copies to make: 1
___________________________________________ _________________________________________________________________________________________
# Lab Code
C lie n t ED
B# V M eth o d /T e st
M atrix
A m t. Ext. P Int. Voi F inal Voi S u rr A m t Spike An
1 K 1001011-001 2 K 1001011-002 5 K 1001011-003 i": K 1001011-004 5 K 1001011-005 1 : K1001011-006 7 K1001011-007 :;:; K l O lfil 1-008 ? K1001011-009 10 K 1 0 0 1 0 1 1-010 11 K 1 0 0 1 0 1 1-011
m K101O11-012 13 K 1 001011-013 1 K1001011-014 d i K1001011-015 K1001011-016 17 K1001011-017 18 K1Q01011-018 19 K1001011-019 20 K1001011-020 21 KQ1000664-01 22: KQ1000664-02 23 KQ1000664-03 24 KQ1000664-04 25 KQ1000664-05 to KQ1000664-06
Hagler W ell" Raw" Hagler Well " Treated" Spanish Trail "Raw'" Spanish Trail `Treated*; Airport North "Raw"
McAllister "Raw" McAllister 'Treated" Humphrey "Raw" Humphrey 'Treated" Broad "Raw" Broad ''Treated' Tennant "Raw" Tennant 'Treated" Muldoon "Raw" Muldoon'Treated" Villa "Raw" Villa "Treated" Royce Street "Raw" Royce Street "Treated" K1001011-008 MS kt0010H-U()8 DMS K1001011-007 MS K 1001M 1-007 DMS LCS MB c/y./.v. .
::
P I PFOA/PFOA ( f M PFOA/PppA | > PFOA/PFOA
\ .s f. PFOA / PFOA
7 PFOA / PFOA O'
S PFOA/ m m :.
,(- f PFOA/PFOA PFOA/PFOA
A 7 PFOA / PFOA
" M :: PFOA t PFOA H
7 PFOA PFOA ri
y PFOA ' PFOA ii .0^ y PFOA/PFOA
m PFOA i PFOA
;(!t 7 PFOA / PFOA
L g : PFOA ' PFOA
M 7 PFOA/PFOA
.0 l f i
i P/ .p \ p:
a
# i^ i.
PFOA/PFOA PFOA `PFOA PFOA/PFOA PFOA/PFOA PFOA/PFOA PFOA/PFOA , /y. PFOA PFOA
.
'
PFOA - PFOA &
Water Water Water yiWptsty/: Water /:Wstii;; Water
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Water Water Water ;y;;/;. Water Water Water Liquid d ilu id ;://:;////. Liquid liquid /y Liquid Liquid :
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________________________________________________________
Surrogate ID: i P M S f o b l
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Witnessed By:
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Printed 2 9 10 7:37
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Page 1 c
EMERALD COAST
U TILITIES AUTHORITY
Emerald Coast U tilities A u th o rity
Preliminary Investigations of Potential PFOA and PFOS in Specific ECUA Production Wells Escambia County, Florida
January 2007
CDM
325 John Knox Road, Building M, Suite 100 Tallahassee, Florida 32303
tel: 850 386-5277 fax: 850 386-6691
P-5
January 3,2007
Mr, Stephen Sorrell, P.E. Executive Director Emerald Coast Utilities Authority 9300 Sturdevant Street Pensacola, Florida 32514-0311
Subject:
.. Sam pling a n d Analysis of PFOA and PFOS CDM Project N o. 36484-55122
Dear Mr. Sorrell:
Emerald Coast Utilities Authority (ECUA) staff w as recently contacted by outside parties inform ing them of possible contamination in certain water production w ells (specifically, Airport North, McAllister, Hagler, and Bronson Field) ow ned and operated by ECUA.
Perfluorooctanoic acid (PFOA or C8) and perfluorooctane sulfonate (PFOS), w h ich are m an m ade and do n ot occur naturally in the environment, are tw o specific constituents of concern that w ere allegedly occurring at these particular ECUA w ells. A t this time, neither the U.S. Environmental Protection A gency (EPA) nor the Florida Departm ent of Environmental Protection has established m axim um contaminant levels (MCLs) for these tw o constituents.
Because of the concern regarding the safety of the drinking water supply, ECUA desired to be proactive in addressing the issue due to the potential impact that PFOA and PFOS could have on the supply wells. ECUA contracted w ith CDM to determine if the information identified by the outside parties w as valid. This issue w as of the highest importance to ECUA and w e were directed to m ove forward on an expedited schedule to address the potential concerns.
CDM w as authorized to proceed w ith a scope of services that included:
D evelopm ent of a sam pling plan that identified m ethodology for collection, location, number of sam ples per site, storage/transport techniques, chain of custody records, and laboratories certified to perform the analysis for PFOA and PFOS.
Coordination w ith laboratories for the analysis. Performance of field sampling. M eeting w ith ECUA staff to provide status reports. * Preparation of a letter report identifying the findings. To ensure that an accurate analysis w as performed on the samples, CDM determined that two independent laboratories w ou ld be needed to separately run chemical analysis on the
itr lo S Sorrell re Results of PFOA and PFOS Analysis 1-3-07.doc
consulting engineering -construction - operations
CDM
P-6
Mr. Stephen Sorrell, P.E. January 3, 2007 Page 2
sam ples for com parison of the results. Because PFOA and PFOS are not com m only observed chemicals in drinking water, identification of tw o laboratories capable of performing the analysis proved to be more difficult than anticipated. H ow ever, after m uch research, tw o su ch laboratories in the U n ited States w ere identified: Severn Trent Laboratories (STL) located in Arvada, Colorado; and Columbia Analytical Services (CAS) located in Kelso, W ashington.
O n Novem ber 15,2006, CDM along w ith ECUA staff collected and tagged for identification tw o separate sets of sam ples for the four concerned wells. In addition, a sample w as collected from the Sum m it Boulevard "Blending Point" station. The sam ples w ere sent by overnight carrier to the tw o identified laboratories for analysis.
CDM collected and subm itted know n research articles regarding PFOA and PFOS to ECUA staff for review. Follow ing the submittal of the research articles, CDM held a conference call w ith senior ECUA staff as a briefing on the issues regarding the tw o chemicals in question.
A lthough there is no established MCL for these constituents, EPA has published support information (dated Novem ber 17,2006) prepared by a governmental toxicologist for im plem entation in a consent order that established a site-specific action level for PFOA of 0.50 parts per billion, also expressed as micrograms per liter (ug/1). H ow ever, CDM could n ot find any information that indicates that even a preliminary level has been established or considered by EPA for PFOS.
O n December 14,2006, laboratory analysis w as received from both CAS and STL and is sh ow n o n the attached sum m ary spread sheet (Table 1). The analytical results from CAS and STL are included in Attachm ent 1 and 2, respectively. The analysis from the tw o laboratories compares favorably especially w h en comparing numbers in the parts per billion (ug/1) range. The highest reported value for either PFOA or PFOS w as at the McAllister Well (raw sample) w ith PFOS detected at a concentration of 0.12 ug/1. This is 76% b elow the level established by EPA in the consent order for drinking water near the DuPont W ashington Works Facility, W est Virginia. A ll other values for both PFOA and PFOS are expressed in hundredths of ug/1. The PFOA results are significantly below the 0.50 u g/1 level established in the previouslyreferenced consent order. From the confirming data provided by the laboratory analysis, it can be concluded that the PFOA and PFOS values found in the water sam ples should not be a cause of concern given to EPA's apparent direction thus far.
Ur to S Sorrell re Results of PFOA. and PFOS Analysis t-3-Q7.doc
CDM
p.7
Mr. Stephen Sorrell, P.E. January 3,2007 Page 3
A n initial response to the ability to treat and remove both PFOA and PFOS can be m ade from review ing the laboratory analysis. As part of its water treatment process the McAllister W ell has granular activated carbon (GAC) pressure vessels in use on-site. Raw water from the w ell is routed through these vessels to reduce contaminants found in the groundwater. Both raw and treated water sam ples w ere collected and analyzed from the McAllister Water Treatment Plant. The raw water level for PFOS as reported by the tw o labs w as 0.110 u g /1 and 0.120 u g /1 and for.PFOA the results w ere 0.028 ug/1 and 0.036 ug/1. After passing through the GAC units, both PFOA and PFOS were below laboratory detection limits. In the future, if PFOA and PFOS become regulated constituents, they could be readily treated w ith GAC based on the N ovem ber 15,2006 data collected from the McAllister Well.
CDM review ed the m ost recent standards issued by EPA concerning unregulated contaminants published in December 2006. Before a constituent of concern is regulated by EPA, it w ill first appear on the unregulated contaminant list. Neither PFOA nor PFOS has appeared on the m ost recently published unregulated contaminant list. It takes several years for the testing, scientific review, publishing of a proposed standard, and public com m ent before a contaminant becom es regulated in drinking water after it is placed on the unregulated contaminant list. From the chemical analysis performed, EPA's current position, and the apparent ability to rem ove PFOA and PFOS with GAC treatment, there does not appear to be a reason for ECUA to be concerned at this time. W e w ill continue to follow the status of PFOA and PFOS as potential contaminants of concern and advise ECUA of future changes if they occur.
If you have any questions concerning the information presented, please contact us at your earliest convenience. A s always, it is a pleasure to work w ith ECUA on challenging projects.
Sincerely,
Charles E. Cook, P.E., BCEE Vice President Camp Dresser & McKee Inc.
Attachments
c: Pat Byrne - ECUA D anny Majors - ECUA Steve Medlar - C D M / EDI David Anderson - CDM /TAL
Hr to S Sorrell re Results of PFOA and PFOS Analysis 1-3-07.doc
Table 1 Perfluorooctane Sulfonate and Perfluorooctanoic Acid Groundwater Analytical Results
November 15, 2006 Specific ECUA Production Wells Pensacola, Escambia County, Florida
i ECUA Production Well Sample Location
;
Sample Collection
Time
(CST)
Sample Result Units
ug/L
PFOS Results -.
CAS
STL
PFOA Results
CAS
STL
Location-SampleType
McAllister - Raw McAllister-Treated
9:00 ug/L 9:04 ug/L
0.110 0.010 u
0.12 0.010 U
0.028 0.010 U
0.036 0.010 U
Airport North - Raw
9:20 ug/L
0.062
0.051.
0.016
0.020
Airport North - Treated Summit Blvd. - Blending Point Hagler - Raw
9:25 9:40 9:55
ug/L ug/L ug/L
' 0.058 fcT030)
0.067
(0.049 ( ' 0.028 >
0.048
0.015 0.012 0.012
0.020 . 0.015 0.018
oCoO d
Hagler-Treated Bronson Field - Raw
10:00 13:05
ug/L ug/L
0.099
L 0.051 0.067
fo o ij 0.022
0.029
NOTES:
CST Central Standard Time.
ug/L Micrograms per liter.
PFOS Perfluorooctane Sulfonate.
f
PFOA Perfluorooctanoic Add.
U Indicates the compound was analyzed but less than the reporting limit PFOS and PFOA split analyses were performed by Columbia Analytical Services (CAS) of Kelso, Washington and STL Denver (STL) of Arvada, Colorado.
CDM
Table 1 to Letter Report Dated 1-2-07jds
Emerald Coast Utilities Authority Preliminary Investigations of Potential PFOA and PFOS in Specific ECUA Production Wells Escambia County, Florida
Columbia Analytical Services Kelso, Washington Groundwater Analytical Results
Attachment 1
1317 South 13lh Avenue P.O.Box 479
Kelso, Washington 98626
(360)577-7222
(360) 636-1068 fax
p. 10
3(B
Columbia k Analytical M I Services
An Employee - Owned Compa
December 14,2006
Service Request No: K 0610096
David Anderson Camp Dresser & M cKee, Incorporated 325 John Knox Road Building M, Suite 100 Tallahassee, FL. 32303
RE: ECUA-PFOA/PFOS AnaIysis/36484- RT.FLD
Dear David:
Enclosed are the results o f the sam ple(s) submitted to our laboratory on Novem ber 16,2006. For your reference, these analyses have been assigned our service request number K 0610096.
A ll analyses were performed according to our laboratory's quality assurance program. The test results meet requirements o f the N E L A C standards. Exceptions are noted in the case narrative report where applicable. A ll results are intended to be considered in their entirety, and Columbia Analytical Services, Inc. (C A S) is not responsible for use o f less than the complete report. Results apply only to the item s submitted to the laboratory for analysis and individual items (samples) analyzed, as listed in the report.
Please call if you have any questions. M y extension is 3281. Y ou may also contact m e via Email at LV o@ kelso.caslab.com .
Respectfully submitted,
C :s, Inc.
Loan V o, Ph.D. Project Chemist
LV/lmb
\ELAP Accredited
4CIL Seal of Excellence Award
tOtt.tevtied
ASTM A2LA CARB CAS Number CFC CFU DEC DEQ DHS DOE DOH EPA ELAP GC GC/MS LUFT M MCL
MDL MPN MRL NA NC NCASI ND NIOSH PQL RCRA SIM TPH tr
p. 11
Acronyms American Society for Testing and Materials American Association for Laboratory Accreditation California Air Resources Board Chemical Abstract Service registry Number Chlorofluorocarbon Colony-Forming Unit Department o f Environmental Conservation Department o f Environmental Quality Department o f Health Services Department o f Ecology Department o f Health U. S. Environmental Protection A gency Environmental Laboratory Accreditation Program Gas Chromatography Gas Chromatography/Mass Spectrometry Leaking Underground Fuel Tank Modified Maximum Contaminant Level is the highest permissible concentration o f a substance allowed in drinking water as established by the USEPA. Method Detection Limit M ost Probable Number Method Reporting Limit Not Applicable N ot Calculated National Council o f the Paper Industry for Air and Stream Improvement Not Detected National Institute for Occupational Safety and Health Practical Quantitation Limit Resource Conservation and Recovery Act Selected Ion Monitoring Total Petroleum Hydrocarbons Trace level is the concentration o f an analyte that is less than the PQL but greater than or equal to the M D L
08002
p. 12
Inorganic Data Qualifiers
* The result is an outlier. See case narrative. # The control limit criteria is not applicable. See case narrative. B The analyte was found in the associated method blank at a level that is significant relative to the sample result. E The result is an estimate amount because the value exceeded the instrument calibration range. J The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL. U The compound was analyzed for, but was not detected ("Non-detect") at or above the MRL/MDL. i The MRL/MDLhas been elevated due to a matrix interference. X See case narrative.
Metals Data Qualifiers
# The control limit criteria is nof applicable. See case narrative. B Theresult is an estimated concentration that is less than the MRL but greater than or equal to the MDL.
E The percent difference for the serial dilution was greater than 10%, indicating a possible matrix interference in the sample.
M The duplicate injection precision was not met.
N The Matrix Spike sample recovery is not within control limits. See case narrative.
S The reported value was determined by the Method of Standard Additions (MSA). U The compound was analyzed for, but was not detected ("Non-detect") at or above the MRL/MDL. y j The post-digestion spike for lumace AA analysis is out of control limits, while sample absorbance is less than 50% of spike
absorbance. i The MRL/MDL has been elevated due to a matrix interference. X See ease narrative. * The duplicate analysis not within control limits. See case narrative. + The correlation coefficient for the MSA is less than 0.995.
Organic Data Qualifiers
* The result is an outlier. See case narrative. # The control limit criteria is not applicable. See case narrative. A A tentatively identified compound, a suspected aldol-condensation product. B The analyte was found in the associated method blank at a level that is significant relative to the sample result. C The analyte was qualitatively confirmed using GC/MS techniques, pattern recognition, or by comparing to historical data. D Thereported result is froma dilution. E The result is an estimate amount because the value exceeded the instrument calibration range. J The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL. N The result is presumptive. The analyte was tentatively identified, but a confirmation analysis was not performed. _ The GC orHPLC confirmation criteria was exceeded. The relative percent difference is greater than40% between the two
analytical results (25% for CLP Pesticides). U The compound was analyzed for, but was not detected ("Non-detect") at or above the MRL/MDL. i The MRL/MDL has been elevated due to a chromatographic interference. X See case narrative.
Additional Petroleum Hydrocarbon Specific Qualifiers
F The chromatographic fingerprint of the sample matches the elution pattern of the calibration standard. The chromatographic fingerprint of the sample resembles a petroleum product, but the elution pattern indicates the presence of a greater amount of lighter molecular weight constituents than the calibration standard.
,, The chromatographic fingerprint of the sample resembles a petroleum product, but the elution pattern indicates the presence of a greater amount of heavier molecular weight constituents than the calibration standard.
O The chromatographic fingerprint of the sample resembles an oil, but does not match the calibration standard. Y The chromatographic fingerprint of the sample resembles a petroleum product eluting in approximately the correct carbon
range, but the elution pattern does not match the calibration standard. Z The chromatographic fingerprint does not resemble a petroleum product.
09003
Columbia Analytical Services, Inc. Kelso, WA
State Certifications, Accreditations, and Licenses
Program
Alaska DEC UST Arizona DHS Arkansas - DEQ California DHS Colorado DPHE Florida DOH Hawaii DOH Idaho DH W Indiana DOH Louisiana DEQ Louisiana DHH Maine DH S M ichigan DEQ Minnesota DOH Montana DPHHS Nevada DEP N ew Jersey DEP N ew M exico ED North Carolina DW Q Oklahoma DEQ Oregon - DHS South Carolina DHEC Utah DOH W ashington DOE W isconsin DNR W yoming (EPA Region 8)
Number
UST-040 AZ0339 88-0637 2286
-
E87412
-
-
C -W A -01 3016 LA050010 W A0035 9949 053-999-368 CERT0047 W A35 W A005
-
605 9801 W A200001 61002 COLU C l 203 998386840
-
lim AOL
fSEUEBi CM) :D 4
COLUMBIA ANALYTICAL SERVICES, INC.
Client: Project: Sample Matrix:
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis Water
Service Request No.: Date Received:
K0610096 11/16/2006
CASE NARRATIVE
All analyses were performed consistent with the quality assurance program of Columbia Analytical Services, Inc. (CAS). This report contains analytical results for samples designated for Tier 111 validation deliverables including summary forms and all of the associated raw data for each of the analyses. When appropriate to the method, method blank results have been reported with each analytical test.
Sample Receipt
Eight water samples were received for analysis at Columbia Analytical Services on 1l/16/2006The samples were received in good condition and consistent with the accompanying chain of custody form. The samples were stored in a refrigerator at 4C upon receipt at the laboratory.
PFOA/PFOS bv HPLC/MS/MS
Surrogate Exceptions: The recovery of surrogate (PFDA-C13) in sample Airport North-Raw were outside the control limits listed in the results summary. The limits are default values temporarily in use until sufficient data points are generated to calculate statistical control limits. Based on the method and historic data, the recoveries observed are in the range expected for this procedure. No further corrective action was taken.
No other anomalies associated with the analysis of these samples were observed.
Approved by
i^ju Date i-Z- 14.C7Z
p. 15
Chain of Custody Documentation
0 ' 0 $ O'?
p. 16
UHurrtDia Analytical Services
An Em ployee - Ow n od Com pany
CHAIN OF CUSTODY
1317 South 13th Ave. Kelso, WA 98626 {360)577-7222 {800)695-7222x07 FAX (360) 636-1068
- PFOA / PF O S AMtyriS-
PROJECTNUMBER 3 W _
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REMARKS
y * X X
X8
REPORT REQUIREMENTS
_ I. Routine Report: Method Blank, Surrogate, as required
_ II. Report Dup., MS, MSD as required
)( II. Data Validation Report
(includes all raw data)
___ IV. CLP Deliverable Report
___ V. EDD
INVOICE INFORMATION
P.O. # ________________
Bill To: ___________________
Total Metals: Al As Sb Ba Be B Ca Cd Co Cr Cu Fe Pb Mg Mn Mo Ni K Ag Na Se Sr Tl Sn V Zn Hg DissolvedMetals: Al As Sb Ba Be B Ca Cd Co Cr Cu Fe Pb Mg Mn Mo Ni K Ag Na Se Sr Tl Sn V Zn Hg
' INDICATE STATE HYDROCARBON PROCEDURE: AK CA Wl NORTHWEST OTHER:,
TURNAROUND REQUIREMENTS SPECIAL INSTRUCTIONS/COMMENTS:
_____24 hr.
_____ 48 hr.
.5 Day
X.Standard (10-15 working days)
fejpcrl^vbz
0 - 0 / u g i L.
Provide FAX Results
.(CIRCLE ONE)
RELINQUISHED BY:
Signature Printed Name
Date/Time Firm
K N RECEIVED BY: ^ ' * 4 C%fev
Signature . , Dpvuftii-AvJW -ibA Printed Name
// /3-ofo / /5 --W 5 Date/TIme
cp rv\ . Firm
A \ n ^RELINQUISHED BY:
a RECEIVED BY:
VSignature .
Printed Name
/ / - /S ', o G / / * > i
aaa Y ja id ^ k l t e / t b f W O
Date/Time
Signature<
, Date/Time
Firm
Printed Name'
m ' Firm
RCD-GJl 06/0,3
Project/Client_
p. 17
C olum bia A nalytical Services Inc. Cooler R eceipt and Preservation Form
PC lJ J ^
thrill*_________________________ Service Request K06_
i\ iwCooler received on
tV
and opened on \ [ iU tlO if
by 7 % i - U L
1. Were custody seals on outside of coolers?
If yes, how many and where?_____________ __
2 . Were custody seals intact?
3. Were signature and date present on the custody seals?
4. Is the shipper's airbill available and filed? If no, record airbill number:_
5. coc# Tem perature of cooler(s) upon receipt: (C)
_____
f
_________ __________
____ _____
Tem perature Blank: (C)
__________ _____
Were samples hand delivered on the same day as collection?
6. Were custody papers properly filled out (ink, signed, etc.)?
7. Type of packing material present _____________________ l U '
8. Did all bottles arrive in good condition (unbroken)?
9. Were all bottle labels complete (i.e analysis, preservation, etc.)?
10. Did all bottle labels and tags agree with custody papers?
11. Were the correct types of bottles used for the tests indicated?
12. Were all o f the preserved bottles received at the lab with the appropriate pH?
13. Were VOA vials checked for absence of air bubbles, and if present, noted below?
14. Were the 1631 Mercury bottles checked for absence of air bubbles, and if present, noted below?
15. Did the bottles originate from CAS/K or a branch laboratory?
16. Are CWA Microbiology samples received with >1/2 the 24hr. hold time remaining from collection?
17. Was C12/Res negative?
Explain any discrepancies:
_____________________________________________________________
H
0N N
Y
Y <)
(S) N
<8 0 OD JY -__
N N N N N.
TN vJr _\
N V -- XT
y
RESOLUTION: Samples that required preservation or received out o f temperature:
Sample ID
Reagent Volume
Lot Number
Rec'd out of Bottle Type Temperature initials
Client: Project: Sample Matrix:
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
p. 18
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006
Sample Name: Lab Code: Test Notes:
Analyte
PFOA PFOS
Airport North- Raw K0610096-001
Perfluorinated Compounds
Units: ng/L Basis: NA
.. . Prep Method
EPA 3535 EPA 3535
Analysis Method
MRL
HPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date
Date
Factor Extracted Analyzed Result
1 11/22/2006 12/14/2006 16 1 11/22/2006 12/14/2006 62
Result Notes
Approved By:
1S2M0?P
K06!00?6phc met 'PFOA-PFOS) I i l 14-2006
Date:
Cl-'
Client: Project: Sample Matrix:
Sample Name: Lab Code: Test Notes:
Analyte PFOA PFOS
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
ServiceRequest: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006
Perfluorinated Compounds
Airport North- Treated K0610096-002
Units: ng/L Basis; NA
Prep Method
EPA 3535 EPA 3535
Analysis Method MRL
HPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date Date Factor Extracted Analyzed Result
1 11/22/2006 12/14/2006 15 1 11/22/2006 12/14/2006 58
Result Notes
Approved By:
IS22AH0597p
K06l0096phc me I (PFOA-?FOS>- 2 12;14/2006
Date:
Page No.
0011
Client: Project: Sample Matrix:
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006
Sample Name: Lab Code: Test Notes:
Analyte PFOA PFOS
McAllister-Raw K0610096-003
Perfluorinated Compounds
Units: ng/L Basis: NA
Prep Method
EPA 3535 EPA 3535
Analysis Method MRL
HPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date
Date
Factor Extracted Analyzed Result
1 11/22/2006 12/13/2006 28 1 11/22/2006 12/13/2006 110
Result Notes
Approved By:
IS22/01059-'p
Ui
K0610W6phc.mel (PFOA-PFOS) * 12/ 1-1/2006
Date:
Client: Project: Sample Matrix:
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006
Sample Name: Lab Code: Test Notes:
Analyte PFOA PFOS
McAllister-Treated K0610096-004
Perfluorinated Compounds
Units: ng/L Basis: NA
.. . Prep Method
EPA 3535 EPA 3535
Analysis Method
MRL
HPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date
Date
Factor Extracted Analyzed Result
1 11/22/2006 12/13/2006 ND 1 11/22/2006 12/13/2006 ND
Result Notes
Approved By:
!S22TO20597p
K06 0095phc.met (PFOA-PFOS) - 4 12/ ( 4/3006
Date:
Pag No..
Client: Project: Sample Matrix:
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006
Sample Name: Lab Code: Test Notes:
Analyte
PFOA PFOS
Hagler-Raw K0610096-005
Perfluorinated Compounds
Units: ng/L Basis: NA
.. . Prep Method
EPA 3535 EPA 3535
Analysis Method MRL
BPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date
Date
Factor Extracted Analyzed Result
1 11/22/2006 12/13/2006 12 1 11/22/2006 12/13/2006 67
Result Notes
UylApproved By:_________ ____________________________________ _______Date:
]S22/020597p
K0610096phc.nlI (PFOA-PFOS) % 12/14/2006
12-j j <-lj d o
Page X o .
Client: Project: Sample Matrix:
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water-
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006
Sample Name: Lab Code: Test Notes:
Analyte PFOA PFOS
Hagler-Treated K0610096-006
Perfluorinated Compounds
Units: ng/L Basis: NA
.. . Prep Method
EPA 3535 EPA 3535
Analysis Method MRL
HPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date
Date
Factor Extracted Analyzed Result
1 11/22/2006 12/13/2006 13 1 11/22/2006 12/13/2006 80
Result Notes
111Approved By:___ _______ _________________________________________ Date:
IS22/020597p
K0fil0096phejnel (PFOA-PFOS) - 6 H /142006
( 2 ,/ U-f/ofc
Page No
Client: Project: Sample Matrix:
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006
Sample Name: Lab Code: Test Notes:
Analyte PFOA PFOS
Bronson Field-Raw K0610096-007
Perfluorinated Compounds
Units: ng/L Basis: NA
Prep Method
EPA 3535 EPA 3535
Analysis Method MRL
HPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date
Date
Factor Extracted Analyzed Result
1 11/22/2006 12/13/2006 22 1 11/22/2006 12/13/2006 99
Result Notes
Approved By:
tS22/020597p
K0ilC096phc rasi (PFOA-PFOS) 7 I/14/2006
Date:
Page Mo.
-noi $
Client: Project: Sample Matrix:
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006
Sample Name: Lab Code: Test Notes:
Analyte
PFOA PFOS
Perfluorinated Compounds
Summit Blvd.- Blending Point K0610096-008
Units: ng/L Basis: NA
.. . Prep Method
EPA 3535 EPA 3535
Analysis Method MRL
HPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date
Date
Factor Extracted Analyzed Result
1 11/22/2006 12/13/2006 12 1 11/22/2006 12/13/2006 30
Result Notes
Approved By:
IS22/0J059'p
j.l [
K0!009iphc.[tiel (PFOA-PFOS) 8 Il'lJ/IOOi
Date:
nk.
Pig Vo
n0 0 lT
Client: Project: Sample Matrix:
COLUMBIA ANALYTICAL SERVICES, INC.
Analytical Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
Service Request: K0610096 Date Collected: NA Date Received: NA
Sample Name: Lab Code: Test Notes:
Analyte PFOA PFOS
Method Blank KWG0620369-3
Perfluorinated Compounds
Units: ng/L Basis: NA
.. . Prep Method
EPA 3535 EPA 3535
Analysis Method MRL
HPLC/MS/MS 10 HPLC/MS/MS 10
Dilution Date
Date
Factor Extracted Analyzed Result
1 11/22/2006 12/14/2006 ND 1 11/22/2006 12/14/2006 ND
Result Notes
Approved By:_________ U .1.
lS2M2059"p
KM!009iphc_nl5l (PFOA-PFOS). mb I2-*l4^006
_________________________________ Date:
Page No
p. 27
COLUMBIA ANALYTICAL SERVICES, INC.
QA/QC Report
Client:
Camp Dresser & McKee, Incorporated
Project:
ECUA-PFOA/PFOS Analysis/36484- RT.FLD
Sample Matrix: Water
Perfluorinated Compounds
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006 Date Extracted: 11/22/2006 Date Analyzed: 12/13-14/2006
Prep Method:
EPA 3535
Analysis Method: HPLC/MS/MS
Sample Name
Airport North-Raw Airport North- Treated McAllister-Raw McAllister-Treated Hagler-Raw Hagler-Treated Bronson Field-Raw Summit Blvd- Blending Point Airport North- TreatedMS Airport North- TreatedDMS Lab Control Sample Duplicate Lab Control Sample Method Blank
Lab Code
K0610096-001 K0610096-002 K0610096-003 K060096-004 K0610096-005 K0610096-006 K0610096-007 K0610096-008 K0610096-002MS K0610096-002DMS KWG0620369-1 KWG0620369-2 KWG0620369-3
Test Notes
Units: PERCENT Basis: NA
Percent Recovery PFDA-C13
47 * 74 62 59 59 70 51 57 76 90 77 99 110
CAS Acceptance Limits:
50-150
Approved By:___________ {1 _________________________________________ Date:
SUft.I/U0697p K<Wt009dphcniel (PFOA*PFOS)*SUR. 12/1 V2006
Page No..
*0019
Client: Project: Sample Matrix:
Sample Name: Lab Code: Test Notes:
Analyte PFOA PFOS
COLUMBIA ANALYTICAL SERVICES, INC.
QA/QC Report
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
Matrix Spike/Duplicate Matrix Spike Summary
Perfluorinated Compounds
Airport North- TreatedMS
K0610096-002MS
K0610096-002DMS
Service Request: K0610096 Date Collected: 11/15/2006 Date Received: 11/16/2006 Date Extracted: 11/22/2006 Date Analyzed: 12/14/2006
Units: ng/L Basis: NA
Prep Method
Analysis Method
Spike Level Sample MRL MS DMS Result
Percent Recovery
CAS
Relative
Spike Result
Acceptance Percent
MS DMS MS DMS Limits Difference
Result Notes
EPA 3535 HPLC/MS/MS 10 50 50
15
84 82 138 134 50-150
EPA 3535 HPLC/MS/MS 10 50 50 58 106 125 96 134 50-150
2 16
Approved By.
iU
DMS'' 38MC0i00S5phCmsl (PFO.VPFOS) - OMS 12/140QM
Date:
1f
Page N'o.t
COLUMBIA ANALYTICAL SERVICES, INC.
QA/QC Report
Client: Project: LCS Matrix:
Camp Dresser & McKee, Incorporated ECUA-PFOA/PFOS Analysis/36484- RT.FLD Water
Service Request: K06I0096 Date Collected: NA Date Received: NA Date Extracted: 11/22/2006 Date Analyzed: 12/14/2006
Laboratory Control Sample/Duplicate Laboratory Control Sample Summary Perfluorinated Compounds
Sample Name: Lab Code: Test Notes:
Analyte
Lab Control Sample KWG0620369-1, KWG0620369-2
Units: ng/L Basis: NA
Prep Method
Analysis Method
Percent Recovery
CAS Relative
True Value Result
Acceptance Percent
LCS DLCS LCS DLCS LCS DLCS Limits Difference
Result Notes
PFOA PFOS
EPA 3535 HPLC/MS/MS 50 50 68 EPA 3535 HPLC/MS/MS 50 50 56
62 136 124 63 112 126
50-150 50-150
9 12
Approved By:_________ [ ( J
OLCS/0?289Si> KWlOWSphcjnel (PFOA-PfOS)-DLCS 12/1*^/2006
_______ _________ _______ _________ _ Date: ( 2-irWjfsk?
Pag No
Group ID: Department:
KWG0620369 Petroleum HC
Preparation Information
Prep Method:
METHOD
Prep Date:
p. 30 11/22/06 00:00
L ab Code
C U entID
K0610096-001 K 0610096-002 K 0 6 10096-003 K 0 6 10096-004 K 0 6 10096-005 K 0 6 10096-006 K0610096-007 K 0 6 10096-008 KWG0620369-1 KWG0620369-2 KWG0620369-3
Airport North- Raw Airport North- Treated McAllister-Raw McAllister-Treated Hagler-Raw Hagler-Treated Bronson Field-Raw Summit Blvd.- Blending Po Lab Control Sample Duplicate Lab Control Sampl Method Blank
P ro d u c t
PFOAPFOA PFOAPFOA PFOAPFOA PFOAPFOA PFOAPFOA PFOAPFOA PFOA PFOA PFOAPFOA PFOAPFOA PFOAPFOA PFOA PFOA
M atrix
WATER WATER WATER WATER WATER WATER WATER WATER WATER WATER WATER
A m t. Ext.
200ml 200ml 200ml 200ml 200ml 200ml 200ml 200ml 200ml 200ml 200ml
F in al Voi.
1ml 1ml 1ml 1ml 1ml 1ml 1ml 1ml 1ml 1ml 1ml
L ab Code
K0610096-001 K0610096-002 K0610096-003 K 0 6 10096-004 K 0 6 10096-005 K0610096-006 K0610096-007 K 0 6 10096-008 KWG0620369-1 KWG0620369-2 KWG0620369-3
P re p E vent ID
554828 554829 554830 554831 554832 554833 554834 554835 554846 554847 554848
Surrogate Solution ID
LCMS1-63L 200PP LCMSI-63L 200PP LCMS1-63L 200PP LCMS1-63L 200PP LCMS1-63L 200PP LCMS1-63L 200PP LCMS 1-63L 200PP LCMS1-63L 200PP LCMS1-63L 200PP LCMS1-63L 200PP LCMS 1-63L 200PP
Amount Added Spike Solution ID
50uL 50uL 50uL 50uL 50uL 50uL 50uL 50uL 50uL 50uL 50uL
LCMS1-63E 200 LCMS1-63E 200
Am ount Added
50uL 50uL
Witness
KCravey KCravey KCravey KCravey KCravey KCravey KCravey KCravey KCravey KCravey KCravey
?
Comments:
Started By: Com pleted By:
ESinclai ESinclai
Reviewed By: j , 1
Chain o f C ustody Relinquished By: R eceived By:
^
Printed: 12/13/2006
16:23:59
u -Stealth'Crystal tpt'prepl rpl
Assisted By: A ssisted By:
*
D ate:
* M v 1 !-!'* /
Preparation Information
S to ra g e:
'
D ate: D ate:
)}J^rz./< ?4
///Z 2 /^
Trainine Yes No
Yes `
No
Extracts Exam ined Yes No
l of 1
Sample ID: Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
Quan Peak Results
B:33 Sample Type:
ACQPHC09
12/14/0602:24:03 AM
43.60000
569.39899
15488
20.00
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(gl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-001 SPB B:30 0.00 10.00 0.00 0.000 1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFC\PFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA .. CI3-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
R T :f c 2N 1& 2? S J f c t t O
C13-PFOA RT:10.77
Nl:
2.23E5
Area
1625973 2178029
137009 1645770 480245
Calc. Amt.
4.65 N/A N/A 3.26 12.45
Voi. Corr. Amt
23.25 0 0
16.3 62.25
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: 10.10-13.10 SM: 11Q
C13-PFOS
NUUH4
RT
12.64 10.77 Al 11.60 10.76 ^ 11.62 M
[There is no signature data to report.
C:\Xcalibur\121306
121306-024
After Initials___
DEC142U
Wror-!i ^ask/Poakr>otround OSr, r.uO'rsct
Page 1 of 2
00023
AT: 9.26.12.26 SU: UG
PFOA AT:I0.76
Quan Peak Results
Nt:
1.52E5
Bast P a a k ft.p SAUn*2 412.9S@12.0O{ 368.37-369.37) US 121304-024
AT: 9.62.14.62 SU: HQ
PFOS RT:t 1.82
NL:
2.67E4
Base PeakF:-p SAU/r2 49B.90@41.0OI 79.44-90.44) MS 1213064)24
AT: 10.14.15.14 SM: 110
Time (rrin)
C13-PFDA RT:1264
KL:1.46E5
8se PiXF:*p SftU mi2 514.65@12-00( 469.35470.3$) US JC1S $21308024
There is no signature data to report. C:\Xcalibur\l 21306
121306-024
Page 2 of 2
0024
Sample ID: Operator:
Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 33
Quan Peak Results
B:33 Sample Type:
ACQPHC09
12/14/0602:24:03 AM
43.60000
569.39899
15488
20.00
Calibration Level:
Unknown
Sample Name:
0096-001 SPE
Vial: B:30
Sample Volume(fil): 0.00
Inj Volume (pi): 10.00
Sample Weight: 0.00
ISTD Amount:
0.000
Dilution Factor: 1.00
Revision:
1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFOTFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
Cl 3-PFOA N/A N/A
Cl 3-PFOA Cl 3-PFOA
AT; 9.60 *2.60 SU: HG
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
1625973 56625 137009
1632059 540983
Calc. Amt
158.64 N/A N/A
34.85 40.05
Vol. Corr. Amt
793.2 0 0
174.25 200.25
M.:2J23
B u P e ik F :*p SRUm$3 418.75 t.00[
371.22472L22) MS SCfS J213M424
RT: t0.*0* 13.10 SU: t1G
CRttai-tPl.FfiOaS
Units
ng/mL ng/rnL
ng/L ng/mL ng/mL
NBLa:iUP3ti4kfr-p
SRUm2 502.M40.00[ 79.49-80.4] MS tC IS IJt 306-024
RT
12.64 11.10 11.60 10.76 11.62
[There is no signature data to report.
C:\Xcalibur\121306
121306-024
/S t"J>
DEC 1h 2006
Page l of 2
it
RT;9.2- 12.28 SM: 110
PFOA RT:10.76
Quan Peak Results
NUU2S BmPukF:.p
SRMms2 412.S5S1ZOO | 268.37.369.37)
MS fCIS 1230W24
RT: 8.62-14.62 SUMIO
PROS RT:11.82
NL: 2.67E4
Bat# PeiJcF:-p SRM me2 459,90@41.00 ( 79,44-50.44) IAS 1CIS 121306-024
RT: 10.14 -15.14 SW:HG
Tim#(nil)
C13-PF0A RT;t2.64
NI: 1.46ES
Bit# Ptakp:. p SfUI ms2
514.M1Z00[ 469.3S-470.3S] MS (CIS 1213064)24
[There is no signature data to report.
C:\Xcalibur\121306
121306-024
Page 2 of 2
iw s
Sample ED: Operator: Acquisition Date:
Low Mass(m/z):
High iviass(m/z): Scans: Rim Time(min): Comments:
p. 35
Quan Peak Results
B:34 Sample Type:
ACQPHC09
12/14/06 02:44:48 AM
43.60000
569.39899
15488
20.01
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-002 SPE B:31
0.00 10.00 0.00 0.000 1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\XcaIibur\Ewan PFCVPFCEFS.meth
N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA .. 13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT1S.27-12.27 S it 11G
C1J-PFOA RTM0.77
Nl:
2.4365
Area
2933778 2380997
146076 1695705 495047
Calc. Amt.
7.41 N/A N/A 2.99 11.67
Vol. Coir. Amt
37.05 0 0
14.95 58.35
Units
ng/inL ng/mL
ng/L ng/mL ng/mL
RT: 19.10.13.10 S ltU G
C1J.RPOS
NL: 1.5524
RT
12.64 10.77 ^ 11.60 10.77 n 11.60 ><*7
iThere is no signature data to report,
C:\XcaIibur\l 21306
121306-025
A fter In iite is
Zrt
D E C 1 4 2006
Dritcr} r
:
cot ~ct;nd K.ccr.'oct
Paee j of 2
''~ ~ ft ft ft 9 7
RT: 9.27 12.27 SMM1G
PFOA RTil.77
Quan Peak Results
NI: 1.44ES
SBfttsMerPt2akF:-p
412.M@12.OOf 389.37-369.37] MS 121306*025
RT:8.60.14.60 SM:11G
PFOS RT:11.60
NI: 2.83E4
Basi PsakF:-p SRUms2 49B.90@41.C0( 78.44*00.44] MS 121006*02$
RT: 10.14-15.14 SRfc HQ
C13.PFOA RT:12.64
Nl:2J7eff
Base PeakF.'.p SRMmi2 514.65812.001 460.35-470.35] MS tels 121306*02$
[There is no signature data to report.
C:\Xcalibur\l21306
121306-025
Page 2 of 2
WW2
Sample ID: Operator:
Acquisition Date: Low Mass(m/z):
High Mass(m/z): Scans: Run Time(min): Comments:
Quan Peak Results
B:34 Sample Type:
ACQPHC09
12/14/06 02:44:48 AM
43.60000
569.39899
15488
20.01
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-002 SPE B:31 0.00
10.00
0.00 0.000
1.00 1.2
Instrument Method:
Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFC\PFCEFS.meth
N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT: 0.00-JO.02 S it 11G
Area
2933778 N/A
146076 1804444 547323
Calc. Amt.
0.00 N/A N/A 0.00 0.00
Vol. Corr. Amt
0 0 0 0 0
rt: 10.10- 0.10 su. n a
Units ng/mL ng/mL
ng/L ng/mL ng/mL
Nl:1.33E4
RT
12.64 N/A 11.60 10.77 11.60
Tfm*(irifl)
(There is no signature data to report.
C:\Xcalibur\121306
121306-025
D E C 1 4 206
FJ>
Page 1 of 2
iAXU . 70 <
RT: 9.27- 12.27 Sfcfc 110
PFOA RT:t0.77
Quan Peak Results
*1:1.4455
Bm PeiJcF:-p SfiM m*2
412.95012.00 1 35.373*9.371 MS ICIS 121305425
RT:8.W- 14.50 SW; I (Q
PFOS RT:11.50
Nt:2.83E4
B u e P e ik F :-p SRMms2 498.9041.001 79.44-80.44) US ICIS 121305-025
RT: 10.14- 1S.14 Slfc 110
C1J-PFOA RT.I1B4
Nl:2J7ES
B in PcikFi'P SRM rrs2 5105012.00 ( 4*9.35-470.35] MS (C(S 121305-025
iThere is no signature data to report.
C:\Xcalibur\121306
121306-025
Page 2 of 2
Sample ID: Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(nun): Comments:
Quan Peak Results
B:38 Sample Type:
ACQPHC09
12/13/0608:21:43 AM
43.60000
569.39899
15472
20.01
Calibration Level:
Unknown
Sample Name:
Vial: Sample Volume(jjl): Inj Volume (fil): Sample Weight: ISTD Amount: Dilution Factor: Revision:
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFC\PFCEFS.meth
N/A N/A
0096-003 SPE B:34 0.00 10.00
0.00 0.000 1.00 1.2
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RI": 9.28.12.28 SU: 110
CI-PFOA RT:!0.78
NI: 2.85
Area
2795968 2251985
197224 2670824
932158
Calc. Amt.
6.17 N/A N/A 5.54 21.97
Voi. Coir. Amt
30.85 0 0
27.7 109.85
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
R T M 0.1l-tl.il SU: IIS
CRUT-.1PUFO1S
HU t.WEi B*s# PiaknV
RT
12.65 10.78 r-1 11.61 /H 10.78 /"i 11.61
Im(trin)
There is no signature data to report.
C:\Xcalibur\121206
121206-057
After initials
D E C 3 2006
Oy/rc-tifl Fe3k/?9t*notPound '.'K-JA-inserisci
. ,v -j
Page 1 of 2
ftftft V I
RT: 9.28 12.28 51b 118
PFOA irnio.79
Quan Peak Results
Hi: 2.39S5
Bast Pt akF;.p SRMm2 4I2.95@12.001 35S.37-M9.37J
MS1212GM57
RT: 8.81-14.81 SM; 110
PFOS RT:ll.61
p . 40
Nl: 5.0SE4 Sast PtakF :-p
S4SRBM.9c8m@241.Oai
79.44-60.44) MS 121205-057
RT: 18.15 15.15 SM: 11G
CtO-PFDA RT:12.6S
W.:
2.J0E5
Bast Peak F:p SRMra2 5t4.S5@12.00{ 469.35-470J51 MS 121208-057
There is no signature data to report,
C:\Xcalibur\121206
121206-057
Paae 2 of 2
55532
Sample ID: Operator:
Acquisition Date: Low Mass(m/z):
High Mass(m/z): Scans: Run Time(min): Comments:
p. 41
Quan Peak Results
B:38 Sample Type:
ACQPHC09
12/13/06 08:21:43 AM
43.60000
569.39899
15472
20.01
Calibration Level:
Unknown
Sample Name:
Vial: Sample Volume(frl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-003 SPE B:34 0.00 10.00 0.00 0.000 1.00
1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCVPFCEFS.meth N/A N/A
Component Name C13-PFDA C13-PFOA C13-PFOS PFOA PFOS
*T:3.63-1J.61 SIS: 110
1DO
SO-
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
N/A 29132.73
N/A 76745.52
N/A
NU 3,1565
S ili P tik F:-p SRU m l 41O.7$01t.QO( 371.22-37123) US (CIS 1212C9-0S7
RT: 050 - 20.02 SM: 110
70-
0-
60-
40-
30-
20-
10-
0- 8.81 10.07
10.0
RT: 11.13 Afe 29133
C3-PFOA RT:11.13
; *__\ _i__t___p_i__'f__T__1__I__\ 1I1-T77t ;12r.12r i 1i2.4i 7r 105 11.0 11.9 125 12.9
Tim* (min)
Calc. Amt.
N/A N/A N/A 13.7446 N/A
Units
ng/mL ng/mL
ng/L ng/mL rig/mL
RT
N/A 11.13 N/A 11.13 N/A
[There is no signature data to report.
C:\Xcalibur\121206
121206-057
PS
DEC ! 3 2006
Paee 1 of 2
\
WW3
RT; 9.63 *12.63 Slfc HG
Quan Peak Results
Nl: 2J8SS Base PeakF:*p
4$1R2M.9m5*^21a.oo(
368.37-369.37) US lets 1212C6-0S7
p. 42
RT:0.00-20.02 B ifc liG
Ibne{ffin)
iThere is no signature data to report. C:\Xcalibur\12l206
121206-057
Page 2 of 2
W TO
r c t
Sample ID:
Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Rim Time(min): Comments:
p. 43
Quan Peak Results
B:39 Sample Type:
ACQPHC09
12/13/06 08:42:27 AW
43.60000
569.39899
15488
20.01
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl):
Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-004 SPE B:35 0.00
10.00
0.00 0.000
1.00
1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCXPFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name Component Type
C13-PFOA Target compound N/A Internal Standard N/A Internal Standard
C13-PFOA Target compound .. 13-PFOS Target compound
RT:9.27-12.27 SlfcltG
C tlF F O A RT:tO,77
2.4IE5
Area
2675471 2248774
172893 483177
13853
Calc. Amt.
5.88 N/A N/A -0.20 -2.93
Voi. Corn Amt
29.4 0 0 -1
-14.65
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: 10.12-13.12 S I tll O
CI3-PF05 RTill.62
NI: 1.9SE4 Base PeaJcriVr*
RT
12.64 n 10.77 n 11.62 7-1 10.81 11.64 .n
Tim* (rrin)
IThere is no signature data to report.
C:\Xcalibur\12l206
121206-058
After initials
r J * ____ _
D E C 1 3 2U06
Wrong PesWPoai: not round
BrsslinsV/icidd#fcrrfsct
Page 1 of 2
RT: 9.31 - 12.lt SM:11Q
PFQA RT:10J1
Quan Peak Results
Nl: S.11E4
Base PeakF:-p $AMrrs2
456152.3.975-3g5!293.0?0}{
MS 121206058
RT: 8.64 - 14,64 SM:11Q
pros
RT.t1.54
NL:
1.91S3
$4BSRe8Ms.tSiOPreeg2a4k1.FO;Oip
79.44-40.44] MS 121206-063
RT: 10.14-15.14 SM; 11Q
C13-PF0A RT:12.64
Nl: 2.5465
B n* PiakF:-p 5RMms2 l4.iSg12.OOt 469.3M70J5J 145121208-058
|There is no signature data to report.
C:\Xcalibur\121206
121206-058
Page 2 of 2
W OP
Sample ED: Operator:
Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: .Run Time(min): Comments:
p. 45
Quan Peak Results
B:39 Sample Type:
ACQPHC09
12/13/06 08:42:27 AM
43.60000
569.39899
15488
20.01
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(gl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-004 SPE B:35 0.00 10.00
0.00 0.000 1.00
1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCVPFCEFS.meth N/A N/A
Component Name C13-PFDA C13-PFOA C13-PFOS PFOA PFOS
si;.zi.12.71 s i t u a
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
N/A 24113.84
N/A 504675.34
N/A
rt: o.o -so.o s u ttts
Calc. Amt
N/A N/A N/A 0.0000 N/A
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT
N/A 11.21 N/A 10.81 N/A
There is no signature data to report. C:\Xcalibur\121206
121206-058
D E C 1 3 2006
P3
Page 1 of 2
RT: 9.31 -12.31 SM: HO
PFOA RT:tO'ftt
Quan Peak Results
NL: 5.11E4
0 j$ e P ia k F :.p
S41R2M.0m5@i2f2.00r
508.07059.37) MS JC1S 121205-050
RT: 0.00 20.02 SM: HO
AT: 0.00 - 20.02 SfcUlO
Tta\*
(There is no signature data to report.
C:\Xcalibur\l21206
121206-05&
Page 2 of 2
Sample BD: Operator: Acquisition Date: Low Mass(m/z):
High Mass(m/z): Scans: Run Time(min): Comments:
Quan Peak Results
p. 47
B:40 Sample Type:
ACQPHC09
12/13/06 09:03:12 AM
43.60000
569.39899
15472
19.99
Calibration Level:
Unknown
Sample Name:
Vial: Sample Volume(pl):
Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-005 SPE B:36
0.00 10.00
0.00 0.000 1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCYPFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT; 3.57 -12.27 Slfc 11Q
C tJ-P fC * RT:10.77
NU 2.22E5
Area
2474620 2081767
119806 1349822 384546
Calc. Amt.
5.88 N/A N/A 2.34 13.40
Voi. Con. Amt
29.4 0 0
11.7 67
Units
ng/niL ng/mL
ng/L ng/mL ng/mL
RT: 10.10-11.10 SU: MO 01l.PfOS
M : 1.21E4
RT
12.64 /n 10.77 t~t 11.60 "t 10.77 ^ 11.60 A1
52 355
iThere is no signature data to report.
C:\Xcalibur\121206
121206-059
After initiais
D E C 1 3 2006
V /re rg peaL'Pesknol Found
? ;:$.Sonisi^correct
Page 1 of 2
RT $.27*12.27 SVt ttG
PFOA. RT10.77
Quan Peak Results
NU
1.33ES
Bate P e *k f:-p SR!Am$2
412.95@t2.00C 369.37.369.37) MS 1212064359
RT: 8.60* 14.60 SUM1G
PFOS RTiH.60
p. 48
HI:
2.01E4 Bit P n k f:*p 496.90041.00) 79.44-90.44) MS 121209469
RT: 10.14-15.14 SUMIO
C13-PFOA RT.12.tt
NI: 3.35E&
B u t Peak F: -j> SRM m 2
514.65@12.00r 469.3547025) MS 121206-059
[There is no signature data to report.
C:\Xcalibur\121206
121206-059
Page 2 of 2
Sample ID:
Operator:
Acquisition Date: Low Mass(xn/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 49
Quan Peak Results
B:40 Sample Type:
ACQPHC09
12/13/06 09:03:12 AM
43.60000
569.39899
15472
19.99
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(gl): Ihj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-005 SPE B:36
0.00 10.00
0.00 0.000
11..200
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCVPFCEFS.meth
N/A N/A
Component Name C13-PFDA C13-PFOA C13-PFOS PFOA PFOS
R T : .M -U .M SM: 1IO
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
N/A 15127.99
N/A 57848.33
N/A
Rr.fl.M-20.00 5t* tIO
Calc. Amt.
N/A N/A N/A 21.1278 N/A
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT
N/A 11.14 N/A 11.12 N/A
[There is no signature data to report. C:\Xcalibur\121206
121206-059
DEC 13 2006
Page l of 2
tiv\.
RT:9.62-12.62 SM.11G
Quan Peak Results
NUU3E6
$BRaMstrPnae2ik F .-p 431626..397S.@36192.3.070]{
MS IC1S 121206459
RT: 0.00. 20.00
Nt:
2.01E4
& * PeakF:p SRM/r2 490.9O@41.OO{ 79.44-80.44] MS 121205459
AT: O.CO.20.00 SM: 11G
Nt:
2.25E5
Base Peak F:*p SRMms2 5t4.65@l2.00( 4S9.3W70J5] MS 121206459
iThere is no signature data to report.
C:\Xcalibur\121206
121206-059
Page 2 of 2
-ft# # *
Sample ID:
Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z):
Scans: Run Time(min): Comments:
p. 51
Quart Peak Results
B:40 Sample Type:
ACQPHC09
12/13/06 09:23:57 AM
43.60000
569.39899
15472
19.99
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl):
Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-006 SPE B:37 0.00 10.00
0.00 0.000 1.00
1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCVPFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA .. 13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT: 9.27 -12.27 S li 110
CU-PFOA RTrl0.77
W.-. USES
Area
3048410 2189371
125915 1529717 463216
Calc. Amt.
6.99 N/A N/A 2.64 16.00
Vol. Coit. Amt
34.95 0 0
13.2 80
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: 10.08-13.08 SM: 110
M3-PFOS RTl 1.58
NI: 1.41E3 6$ Peak rr/z
RT
12.63 #*1 10.77 A? 11.58 ,*i 10.77 /*1 11.60
(There is no signature data to report.
C:\Xcalibur\121206
121206-060
After initials F F 3
DEC 1 3 Mb'
V>roRS
net Found
Page 1 of 2
RT: $.27* 12.27 SM:11G
PfOA RT:10.77
Quan Peak Results
Nt; USES
8 m Piak F: -p
4S1*M2.m93s92l2.d0|
368.37-369.371 MS 121209-060
RT: 8.60 14.60 SU: 11G
PFOS RTtl.60
NV.
2.4SE4
BanPeifcF:p 4S9R8M.9m0$9241.001
79.44-80.441 MS 121206-000
RT: 10.13-15.13 SPA ftO
C13-PF0A RT:12.03
Nt:
2.93ES
Bm P*i1cF;.p SRUm*2 St4.0S912.00t 469.35-470.3S! MS 1212004360
There is no signature data to report.
C:\Xcalibur\121206
121206-060
Page 2 of 2
Sample ID: Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
Quan Peak Results
B:40 Sample Type:
ACQPHC09
12/13/06 09:23:57 AM
43.60000
569.39899
15472
19.99
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl): In] Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCNPFCEFS.meth N/A N/A
p. 53
0096-006 SPE B:37 0.00 10.00 0.00 0.000 1.00 1.2
Component Name C13-PFDA C13-PFOA C13-PFOS PFOA PFOS
RT: 0.00 20.00 5VC 11G
ISTD Name
C13-PFOA N/A N/A
Cl 3-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
39162.58 N/A N/A
60056.35 N/A
NL:
2.36E5
0 m PiaJcF:*p SRMmrt 416.7511J)0( 37UM72J2] 145 1212004
RT:0.00*50.00 S M itlQ
Calc. Amt.
0.0000 N/A N/A
0.0000 N/A
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT
13.24 N/A N/A 11.14 N/A
Nl:
1.4i U
0$3R0m7M.6rP0ree924ik0F.0:01p
70.40*00.49} 140 121205-000
[There is no signature data to report. C:\Xcalibur\121206
121206-060
DEC
Page 1 of 2
W W S
RTt9.e4.t2.64 SMM1G
Quan Peak Results
N l:U 85
BaiePaakFt-p SRM ms2 4I2.95SI2.00 ( 399.37-359.27) US (CIS 121206-060
RT: 0.00. 20.00 SUM TG
p. 54
Nt:
2-45E4 a m PUcF:.p SRM ms2 49B.90S4f.Q01 79.44-80.44] MS 121208-060
Tim (frffl)
RTM0.74-15.74 SM; flG
100- 12.53
90-
80-
708
| 80-
| 50
&| 4030-
20-
10-
1211.19 11.77"T"~r
CIJ-PfOA RP13J4
13
Tixa (frin)
NV.243ES Bass P*akF:-p SRM<n*2 S14.6SS12.00 [ 489.3S-470.35) MS (CIS 12(2054)50
-r1"4f-^"4r-1r5.18 15
[There is no signature data to report.
C:\Xcalibur\121206
121206-060
Page 2 of 2
Sample ID:
Operator: Acquisition Date:
Low Mass(m/z): High Mass(m/z): Scans:
Run Time(min): Comments:
Quan Peak Results
B:40 Sample Type:
ACQPHC09
12/13/06 09:44:43 AM
43.60000
569.39899
15472
19.99
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(jrl): Inj Volume (pi):
Sample Weight: ISTD Amount: Dilution Factor: Revision:
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFC\PFCEFS.meth N/A N/A
p. 55
0096-007 SPE B:38 0.00
10.00
0.00 0.000
1.00
1.2
Component Name______ ISTD Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
AT: 9.27 12.27 SJ 11Q
C11-PFOA
AW077
Component Type_________Area
Target compound Internal Standard Internal Standard
Target compound Target compound
2803891 2683010
135296 2672225
587646
Calc. Amt.
5.10 N/A N/A 4.40 19.76
Vol. Corn Amt___ Units_______ RT
25.5 ng/mL 0 ng/mL 0 ng/L 22 ng/mL
98.8 ng/mL
12.64 10.77 11.60 10.77
11.60
Nt:
2.9IE5
AT: 10.10 13.10 SU: !1Q
HLz 1.24
Bat* ftakm fe*
S75A0MM20*m46024.50.00F0:\.
79.4040*0) US (CIS 121206-061
c
iThere is no signature data to report.
C:\Xcalibur\I2I206
121206-061
After Initials
D E C 1 3 2006
C '/.'reps Psa/P; cot Ccund Ct o /.ir *; Kci-icrinecrrsct C v r----- ------ ---- --
Page 1 of 2
I. tfrtH r?
RT: 9.27 12.27 SM: HQ
PFOA RTilC.77
Quan Peak Results
Nl:
2.42E5
Bas PeakF:-p SAM ere2 412.9S@12.00l W9.37069.371 US 1212064361
RT: 8.60 14.60 SUL UG
PfOS RT.11.60
Nl:
2.85E4
8se PaifcF:-p SflM ns2 498.90@4l.l0( 79.44*60.44] US 1212064361
RT: 10.14-15.14 SU: l i a
Tim(min)
C13-PF0A RT12.64
Nl: 2.8BE5
Bai Peak f'.-p 5RMma2 514.6S912.00I 460.36470J3J U5 1212064361
fThere is no signature data to report.
C:\Xcalibur\121206
121206-061
Page 2 of 2
Sample ID: Operator:
Acquisition Date: LowMass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
Quan Peak Results
B:40 Sample Type:
ACQPHC09
12/13/06 09:44:43 AM
43.60000
569.39899
15472
19.99
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl):
Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-007 SPE B:38 0.00 10.00 0.00 0.000
1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCVPFCEFS.meth N/A N/A
Component Name C13-PFDA C13-PFOA C13-PFOS PFOA PFOS
RT:.77-117? SS* 11Q
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
N/A 11171.80
N/A 85777.70
N/A
RTi 0.00.20.00 51*110
Calc. Amt.
N/A N/A N/A 47.0272 N/A
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT
N/A 11.27 N/A 11.16 N/A
(There is no signature data to report,
C:\Xcalibur\12l206
121206-061
Pane 1 of 2
BFJ
'U tH A
RT:9.6S. 12.CS SM: HQ
Quan Peak Results
NU2.42E5
SasePei^F:-p SRMa n t
412.95@12.00( 3fl8.37-W9.37I MS (CIS 121208481
ftT: O.CO. 20.00 S l t i t G
RT: 9.00- 20.00 SM: H O
T{iM(nin)
{There is no signature data to report,
C:\Xcalibur\121206
121206-061
Page 2 of 2
Sample ED: Operator:
Acquisition Date:
Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 59
Quan Peak Results
B:40 Sample Type:
ACQPHC09
12/13/06 10:05:28 AM
43.60000
569.39899
15472
20.00
Calibration Level:
Unknown
Sample Name: Vial: Sample Vohrme(pl): Inj Volume (pi):
Sample Weight: ISTD Amount: Dilution Factor: Revision:
Instrument Method:
Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCNPFCEFS.meth N/A N/A
0096-008 SPE B:39
0.00 10.00
0.00 0.000 1.00
1.2
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT: 9.27 12.77 SMM1Q
Ctl-PFOA RT.10.77
Nt: 2.12E5
Area
2450391 2109858
174124 1405717 315766
Calc. Amt.
5.73 N/A N/A 2.45 5.91
Voi. Corr. Amt
28.65 0 0
12.25 29.55
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: 10.0S-13.08 51* 110
C13-PFOS RTH.53
Nt:1.7IE4 aatsPtakmte*
RT
12.64 10.77 11.58 10.77 11.60
iThere is no signature data to report.
C:\Xcalibur\121206
121206-062
After initials & F 5
.
DEC niM
VirongPe-iMPs#.wt Pound Ir i;:.'aiderhccrrect
Page 1 of 2
u.
RT: 9.27-12.27 SM: 11G
PFOA RT:10.77
Quan Peak Results
Kt:
1.27E5
Sue Peik F: - p SRMim2 412.95@12.00 369.37-359.37} MS 121206-062
RT; 8.60* 14.(6 SH: 110
PFOS RP.1U0
Nt:
1.69E4
B$RaMst rPme2ikF:-p
499.90^41,00 ( 79.44-90.441 US 121206-062
RT: 10.14-15.14 SM: 11(3
C13-PF0A RT:I2.64
Nt:
2.2965
Sue PikF:-p
S5tR4M.6m5sa2i2JlO[
4(9.35470.35} US 121206-062
iThere is no signature data to report. C:\Xcalibur\12l206
121206-062
Page 2 of 2
"W W 1
Sample ID:
Operator: Acquisition Date:
Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
Quan Peak Results
B:40 Sample Type:
ACQPHC09
12/13/06 10:05:28 AM
43.60000
569.39899
15472
20.00
Calibration Level:
Unknown
Sample Name: Vial:
Sample Volume(pl): Inj Volume (pi):
Sample Weight: ISTD Amount: Dilution Factor: Revision:
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFC\PFCEFS.meth
N/A N/A
0096-008 SPE B:39
0.00 10.00
0.00 0.000 1.00 1.2
Component Name C13-PFDA C13-PFOA C13-PFOS PFOA PFOS
RT: fi.62- 12.82 SU: HQ
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOS
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
10406.91 42056.48
N/A 125635.15
N/A
HL-2JJE5
4StReU.7mse2n.oof
371.22072.22) MS (CIS 121205082
RT: 0.00-20.01 SM: \\Q
Calc. Amt
0.0000 N/A N/A
15.9093 N/A
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT
13.12 11.12 N/A 11.08 N/A
{There is no signature data to report. C:\Xcalibur\121206
121206-062
DEC 13200b
Page 1 of 2
LWV.
At; 9.58* 12.53 Sht MG
Quan Peak Results
AT: 0.00 20-01 SM:11G
39PakF:-p SRUmi2 4119$12.00[
3UfSi8.J9C7|-$U9.37i
121205-062
AT: 10.S2-15.52 SiC ItG
Time (rrfn)
Nt:2J9E5
&as*PeiKF:p SAUms2 514.85012.00 f 46fl.J5-470.G51
US ICtS 121205-062
Tkr#(tn'ft)
Ifhere is no signature data to report. C:\Xcalibur\121206
121206-062
Page 2 of 2
$559$
Sample ID: Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 63
Quan Peak Results
B:30 Sample Type:
ACQPHC09
12/14/06 01:21:49 AM
43.60000
569.39899
15488
20.00
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl):
Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
MB B:27 0.00 10.00 0.00 0.000 1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCVPFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
AT; 9:27'12.27 SM rttO
C tl-P fO A RT:10.77
NL: 2.0765
Area
3714984 1995933
146790 532518 25028
Calc. Amt.
10.99 N/A N/A 0.25 0.11
Voi. Corn Amt
54.95 0 0
1.25 0.55
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
AT; 10.12-13.12 SU. 11(3
C1&>WOS
Nt: 1.59E4
RT
12.66 10.77 /I 11.62 10.83 7 11.64
Um(tri*)
[There is no signature data to report,
C:\Xcalibur\121306
121306-021
After initiais
__
D Wrong Peak/Feskr.ot rotinn
^nseline/choutdernewest
Q ase*
--
Page 1 of 2
RT: 9.33.12.33 SM: 113
PRFTOAOAJte
Quan Peak Results
NI: 4.59E4 fiate Paak F:-p
4S1R2M.9m50i212.001
3SB.37-389.71 MS 12IM-021
SM: I1G
PFOS RT:11.M
NL 2.97J
Base P tkF:-p
S<3R3M.9m0@s241.001
79.44-80.44) MS (OS 121300-021
RT: 10.1-15.1 SM; 113
CRnr,-1P2F.6O8A
M:3,42E5 fin Peak F ;-p
5R5@12.00( 468^5-470.35) US (CIS 121308-021
filiere is no signature data to report
C:\Xcalibur\l 21306
121306-021
Paee 2 of 2
13 y)
Sample ID:
Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 65
Quan Peak Results
B:30 Sample Type:
ACQPHC09
12/14/06 01:21:49 AM
43.60000
569.39899
15488
20.00
Calibration Level:
Unknown
Sample Name: Vial:
Sample Volume(pl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
MB B:27
0.00 10.00 0.00 0.000
1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFC\PFCEFS.meth N/A N/A
Component Name
CI3-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
CI3-PFOA N/A N/A
C13-PFOA .. C13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
3714984 33688 146790
624329 25028
Calc. Amt.
608.05 N/A N/A 0.25 1.45
Vol. Corr. Amt
3040.25 0 0
1.25 7.25
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: 8 .W . 12.6J SUMIO
NU2j07S
B ii*P tkF :-p SRUm2
4ie.7$Q11.CO( 3?1.72*572.22) MS KHS I2U06421
AT! 10.12-13.12 SU; 113
C13-PFOS
NL1.S9E4
RT
12.66 11.16 11.62 10.83 11.64
[There is no signature data to report,
C:\Xcalibur\l2t306
121306-021
ft F i
DEC 1 2006
Pao^ 1 r\f "i
i ,
HT: 9.33- .3 3 SVfc 110
PFOA RT:t0.83
Quan Peak Results
Nl:iSSU
Bait PtakF:? SRUrrsl
412.95912.00 ( 3S0.37-1S9.37}
MS {CIS
(21303-021
FT:8.04*14. SM: 11(3
PFOS RT;t1.04
NU 2.9763 Base PeakF:*p
498.90941.00) 79.44-80.44) MS ICIS 121308-021
RT: 10.16-15.1 SV tH O
C13-PFDA RT:12.M
NU 3.4265
Base Peak F:-p SAUmi2 514.6591200 { 469.35-470.35) MS (CIS 121306-021
iThere is no signature data to report.
C:\Xcalibur\l 21306
121306-021
Page 2 of 2
Sample ED: Operator: Acquisition Date:
LowMass(m/z): High 3vfass(m/z): Scans: Run Time(min): Comments:
p. 67
Quan Peak Results
B:35 Sample Type:
ACQPHC09
12/14/06 03:05:35 AM
43.60000
569,39899
15488
20.01
Calibration Level:
Unknown
Sample Name:
Vial: Sample Volume(pl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-002MS SPE B:32 0.00
10.00 0.00 0.000 1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFOPFCEFS.meth
N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT: 3.2. 12.2 SU: I t a
CfJ-PFC* RT:10.7
HI: 2.5265
Area
2849523 2251424
142203 6517729
800856
Calc. Amt.
7.60 N/A N/A 16.86 21.21
Voi. Corn Amt
38 0 0 84.3 106.05
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: 15.10.13.10 S U rttS
Ct J-PFOS
SI: I.ME4
RT
12.63 10.76 h 11.60 10.76 f 1 11.59 n
[There is no signature data to report. C:\Xcalibur\121306
121306-026
After initiais
D E C 1 h 2006
V m ' -j ?:jfcPsafc not Found
O >/;!:'' 'c-.'.'cs-
Page 1 of 2
RT: 9.20* 12.26 SM: 11G
PFOA RT:10.76
Quan Peak Results
Nl:
6.76ES
Bass PakF:-p 5RMms2 412.9512.00( 36B.37-349.37J MS t2130S<026
RT:B-59. 14.59 SM:I1G
pros RT:11.59
Nt:
5.19E4
Bast PsiJcF:-p 5RMms2 49a.90Q41.00I 79.44-60.44J MS 121306-026
RT: t0.13* 15.t3 SM: 11G
C13-PFOA RT:12.63
M :2J4 E 5
Bass Paa!cF:-p SRUmi2 514.5I2.00 ( 469.35-470.35] MS 1CIS 121306-026
(There is no signature data to report.
C:\Xcalibur\121306
121306-026
Page 2 of 2
Sample ID: Operator: Acquisition Date:
Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 69
Quan Peak Results
B:35 Sample Type:
ACQPHC09
12/14/06 03:05:35 AM
43.60000
569.39899
15488
20.01
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl):
Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCNPFCEFS.meth
N/A N/A
0096-002MS SPE B:32
0.00 10.00 0.00 0.000 1.00 1.2
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT: 3.59. 13.59 S ii: ( t o
Area
2849523 44700 142203
6618812 864712
Calc. Amt
351.68 N/A N/A
41.07 45.07
Vol. Corr. Amt
1758.4 0 0
205.35 225.35
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: 10.10-n . i a si* n o
C13-PFOS
NU 1.S4E4
RT
12.63 11.09 11.60 10.76 11.59
[There is no signature data to report.
C:\XcaliburU21306
121306-026
DEC 1 h 2006
Page 1 of 2
RT: 9.26-12.26 SMMtG
PFOA RT:10.76
Quan Peak Results
NL: 6.7S5
Bise PikF:> p
SRUmt2 412.95912.00{ 36B.37.369.37J MS ICiS 121300-026
RT: 9.59-14.59 SM: 11G
PFOS RT:11.$9
p . 70
NL* 5.1SE4
BSRisMb mPse2akFi.p
498.90@41.001 79.44-80.44} MS ICIS 1213054)26
RT; 10,13-15.13 SM: 11G
C13-PF0A RT:12.63
K l: 2.64ES
8i PckF;.p
SRM<ns2 S14.8S@12.OOi 469.35-470.3S} MS ICIS 121306-026
iThere is no signature data to report.
C:\Xcalibur\121306
121306-026
Page 2 of 2
Sample ED: Operator:
Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 71
Quan Peak Results
B:36 Sample Type:
ACQPHC09
12/14/06 03:26:22 AM
43.60000
569.39899
15488
20,00
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl):
Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-002MSD SPE B:33
0.00 10.00 0.00
0.000 1.00 1.2
Instrument Method: Original Processing Method:
Current Processing Method:
C:\Xcalibur\Bwan PFC\PFCEFS.meth N/A
N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA . C13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
a n 9j . . s s u n s
CtJ-PFCA
Nl:
Area
2701654 1784111 154091 5026836 730996
Calc. Amt.
9.01 N/A N/A 16.35 24.90
Voi. Corr. Amt
45.05 0 0
81.75 124.5
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT
12.63 10.76 A 11.59 10.76 /*'. 11.59 .*1
KT: 10.09.. 10.09 SM: 11S
C12.PFOS
NL- M0E<
S u tP ia k F:-p SRMm$2 502.M40.00{ 79.4i-60.49] US ICtS 121303-027
(There is no signature data to report. C:\Xcaiibur\121306
121306-027
After
Initials
DEC k 006
D-Arr'c1 riwrsA.'Xi ilGUl G?i
P a a t* I r*f 9
W S1
RT: 9.26-12.26 SU: HG
PFOA RT:10.76
Quan Peak Results
W.:
S.39E5
Bast Psak f : p SRM<ts2 412.95t2.00{ 389.37489.371 MS 1213084)27
R T:e.59-t4i9 SM: HG
PFOS R1:11.59
Nl: 4.I5E4
Biss Psik F :-p SRMmt2 498.SO4!.OOf 79.44-80.44] MS 121306-027
RT: 10.13-15. 5K: 11G
C13-PFDA RT:12.53
M.:249E5
Bast PeakF:-p snumsz 5t4.85912.00f 46945-470.35] US ICI5 1213094)27
There is no signature data to report,
C:\Xcalibur\121306
121306-027
Page 2 of 2
Sample ID: Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 73
Quan Peak Results
B:36 Sample Type:
ACQPHC09
12/14/06 03:26:22 AM
43.60000
569.39899
15488
20.00
Calibration Level:
Unknown
Sample Name:
Vial: Sample Volume(pl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
0096-002MSD SPE B:33
0.00 10.00 0.00 0.000 1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCYPFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA 13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT: 9.59-12.59 SU: UQ
NU USES
Area
2701654 17746 154091
5421717 775783
Calc. Amt.
839.26 N/A N/A
47.38 54.70
Voi. Corr. Amt
4196.3 0 0
236.9 273.5
RT; 10.09-11.09 SU; 11Q
CR1TJt-PtMFOtS
AA.'IM M t
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
NU 1.E0E4 t i n P<aVf:*p SRUmsl 502.64040.00 ( 79.49-80.49] MS JClSt2i3094>27
RT
12.63 11.09 11.59 10.76 11.59
iThere is no signature data to report.
C:VXcalibur\l 21306
121306-027
DEC 1h 2006
Page 1 of 2
'tHfei
RT: 9.26- 12,25 SM: 110
FFOA
Quan Peak Results
nUSJSES
RT: 8.59- 14.59 SM: 11G
RT: 10.11-15.13 SW: i t o
Tir-# (rrin) C13-PFD
ML:2.49ES
7T/T*(rr)
iThere is no signature data to report.
C:\XcaliburM21306
121306-027
Page 2 of 2
Sample ID:
Operator: Acquisition Date: Low Mass(m/z):
High Mass(m/z): Scans: Run Time(min): Comments:
Quan Peak Results
B:31
Sample Type:
ACQPHC09
12/14/0601:42:34 AM
43.60000
569.39899
15472
19.99
Calibration Level:
Unknown
Sample Name:
Vial: Sample Volume/pi):
Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFC\PFCEFS,meth N/A N/A
LCS B:28 0.00 10.00 0.00 0.000 LOO 1.2
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT 7 -12.27 SM: 1tQ
C13-PFO* RT:10.77
K it 2.49=5
Area
3060817 2374707
107565 5685498
477385
Calc, Amt.
7.73 N/A N/A 13.61 11.25
Voi. Corn Amt
38.65 0 0
68.05 56.25
Units
ng/mL ng/rriL
ng/L ng/mL ng/mL
RT: 10,10-1.10 SU: 110
RT
12.64 h 10.77 n 11.60 10.77 A) 11.60
Time (frin)
[There is no signature data to report.
C:\XcaUbur\121306
121306-022
After
__ _
initiais__ E-ZZ2TM_TM.
D E C 1 k 2006'
Wrong PeaWPsafcnot Found
Bcjftne/siiciirterincorrect Objs
Page 1 of 2
l\ * h.
TJ
RT: 9.27- 12.27 SW: 11G
PFOA RT:tO,77
Quan Peak Results
Nl:
6.1465
Base Peak F;-p SRMms2 412.9512.00 ( 368.37-369.37} MS121306-022
RT: 8.-14.60 SM: 119
PfOS RT:11.60
p . 76
HU 3.44E4 Base P e akf:-p SRMms2 498.90fi41.00l 79.44-80.44} MS 1C1S 121306-022
RT: 10.14-15.14 SM: HG
C13-PPDA RT:12.4
Nl: 2.796S
8ase PaakF:-p SftUms2 S14.6Sfi12.00i 468.3S-470.35J US JCIS 121306-022
iThere is no signature data to report.
C:\Xcalibur\121306
121306-022
Paee 2 of 2
# >>6 1
Sample ED:
Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
p. 77
Quan Peak Results
B:3l Sample Type:
ACQPHC09
12/14/06 01:42:34 AM
43.60000
569.39899
15472
19.99
Calibration Level:
Unknown
Sample Name: Vial: Sample Volume(pl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
LCS B:28 0.00
10.00 0.00 0.000 1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Bwan PFCXPFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA .. CI3-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT: 0.00-50.00 SU; MS
Area
3060817 N/A
107565 5863339
477385
Calc. Amt.
0.00 N/A N/A 0.00 0.00
Vol. Corr. Amt
0 0 0 0 0
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: 10.10-13.10 SSfcllQ
C13-PFOS
NLM.0SE4
RT
12.64 N/A 11.60 10.77 11.60
llhere is no signature data to report.
C:\XcaliburU21306
121306-022
BEC 1 4 201)6
PflP 1 ff 1
'JJ-
RT: 9.27-12.27 SM: 110
PFOA RT:t0.77
Quail Peak Results
NL4.14E5
Base Peak?:- p SRMrasZ
46182.4.r75-@34l29..307Oj{
MS (CIS 121309-022
RT: 8.40-14.60 SMrttO
PFOS RTilt.SO
N l: 3.44E4
Base P takF :-p SAM ms2 499.90Q41.00 ( 79.44-80.44) MS ICS 121306-022
8T.10.t4-15.14 S it 11Q
C13-PFDA f t * ! 2.64
Nl:2J9ES
Base P tkF:-p SRMmrt S14.6512.C0| 46t.35-470.3SJ MS ICtS
121308-022
[There is no signature data to report.
C:\Xcalibur\121306
121306-022
Pace 2 o f 2
Sample ID: Operator:
Acquisition Date: Low Mass(m/z):
High Mass(m/z): Scans: Run Time(inin): Comments:
Quan Peak Results
B:32 Sample Type:
ACQPHC09
12/14/06 02:03:19 AM
43.60000
569.39899
15472
20.00
Calibration Level:
Unknown
.
Sample Name:
Vial: Sample Volume(pl): Inj Volume (pi):
Sample Weight: ISTD Amount: Dilution Factor: Revision:
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFC\PFCEFS.meth N/A N/A
DLCS B:29 0.00 10.00
0.00 0.000 1.00 1.2
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOA
RT: 9-12.2 SVt I IQ
CIWFOA RTOQ.79
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
Area
3846062 2309497
150146 5092472
513944
Calc. Amt.
9.87 N/A N/A 12.39 12.58
Voi. Corr. Amt
49.35 0 0
61.95 62.9
Kl:
2.45
Sl uRUi rPa2ikF:-p
371.22-372.22J MS 121306-021
RT: 10.10-1110 SM; 110
C tlP fO S
Units ng/mL ng/mL
ng/L ng/mL ng/rnL
N 1.72E4
RT
12.64 10.79 r 1 11.60 10.77 n 11.62
There is no signature data to report.
C:\Xcalibur\l21306
121306-023
After
.t
Initials --
-------- --
DEC ' <>2006
Wrong PeaWPaak not Pound Bas&iineii'l-oui-isr incorrd
Page 1 of 2
V'-'aS"
i 3
RT; 9.27- 12.27 SM:1tG
PfOA
RP.10.77
Quan Peak Results
Nl:
S.37E5
8 1 1 c PeakF:*p SAMms2 412.SS@t2.OOi 368.17-J09.3?) US 121806*023
AT:8.02 14.02 SKt 11G
pros RT:1 M l
NL' J.7Q64
$0RaMs*mPse2akF:-p
4S3.90@41.OOf 79.44-80.aj MS KtS 121306-023
RT; 10.14 -15.14 SVt 110
CU-PFOA RT.t2.04
NLJJSES
Baa* Pe ikF:*p SRMmtl
5t4.0512.OOf 4S9.35a70.3S)
ms rets
121300-023
There is no signature data to report.
C:VXcaIibur\l 21306
121306-023
Page 2 of 2
-WfrT
Sample ID:
Operator: Acquisition Date: Low Mass(m/z): High Mass(m/z): Scans: Run Time(min): Comments:
Quan Peak Results
B:32 Sample Type:
ACQPHC09
12/14/06 02:03:19 AM
43.60000
569.39899
15472
20.00
Calibration Level:
Unknown
Sample Name: Vial:
Sample Volume{pl): Inj Volume (pi): Sample Weight: ISTD Amount: Dilution Factor: Revision:
DLCS B:29 0.00 10.00 0.00 0.000 1.00 1.2
Instrument Method: Original Processing Method: Current Processing Method:
C:\Xcalibur\Ewan PFCVPFCEFS.meth N/A N/A
Component Name
C13-PFDA C13-PFOA C13-PFOS
PFOA PFOS
ISTD Name
C13-PFOA N/A N/A
C13-PFOA C13-PFOA
Component Type
Target compound Internal Standard Internal Standard Target compound Target compound
RT: *.62 12.42 SU: 110
Nl:2.49E5
Area
3846062 28644 150146
5206949 513944
Calc. Amt
740.27 N/A N/A
42.55 44.41
Vol. Corr. Amt
3701.35 0 0
212.75 222.05
Units
ng/mL ng/mL
ng/L ng/mL ng/mL
RT: lO.JU.13.tO SM: 11G
NL 1.7264
RT
12.64 11.12 11.60 10.77 11.62
{There is no signature data to report.
C:VXcalibur\l 21306
121306-023
&
DEC14 20(16
Page 1 of 2
RT; 9.27 -12.27 SMM1G
PFOA RT:10.?7
Quan Peak Results
NL: 547E5
Bast Peak f : - g SRM mt2
4t7.95dl2.00C 380.37*359.371 MS (CIS (21306-023
RT: 8.52 -14.62 5M:1tG
PFQS RT:1 (.62
p. 82
N l: 3.70E4 8ase P*kF:*p SRM ms2 4&8.9041.0Q( 79.44-80.441 MS fCIS 121306-023
RT: 10.14 -15.14 SM; 11G
CI3-PF0A RT:I2.
Nl:3.5S65
B m P eakFi-p SRMms2 514.65912.00 ( 469.35-470.35] MS (CIS 121306-023
[There is no signature data to report.
C:\Xcalibur\121306
121306-023
Page 2 of 2
Emerald Coast Utilities Authority Preliminary Investigations of Potential PFOA and PFOS in Specific ECUA Production Wells Escambia County, Florida
Severn Trent Laboratories Arvada, Colorado Groundwater Analytical Results
Attachment 2
ANALYTICAL REPORT
STL Denver 4955 Yarrow Street Arvada, CO 80002
Tel: 303 736 0100 Fax: 303 431 7171 www.stl-inc.com
PFOA/PFOS Analysis Lot#: D6K160299
David Anderson
Camp Dresser & McKee, Inc. 325 John Knox Road Suite 100
Tallahassee, FL 32303
Severn Trent Laboratories, Inc./STL Denver
Gail DeRuzzo Project Manager
December 4, 2006
Severn Trent laboratories. Inc.
Table Of Contents
Standard Deliverables with Supporting Documentation
Report Contents
Number of Pages
S ta n d a rd D e liv e ra b le s (The Cover Letter and the Report Cover page are considered integral parts o f this Standard Deliverable package. This report is incomplete unless allpages indicated in this Table o f Contents are included.)
Table of Contents Case Narrative Executive Sum m ary - Detection Highlights M ethods Sum m ary M ethod/A nalyst Sum m ary Lot Sam ple Sum m ary Analytical Results QC Data Association Summary Chain-of-Custody
S u p p o rtin g D o c u m e n ta tio n (Note: A one-page "Description o f Supporting Documentation" is provided at the beginning o f this section.).
Volatile GC/M S
Check below when supporting
documentation is present.
Semivolatile GC/MS Volatile GC
Semivolatile GC
LC/MS or HPLC Metals General Chemistry Subcontracted Data
Case Narrative
D6K160299
The results included in this report have been reviewed for compliance with the Laboratory Quality Manual. All results have been found to meet all requirements of NELAC and any exceptions are noted below.
This report shall not be reproduced except in full, without the written approval o f the laboratory or sponsor. Dilution factors and footnotes have been provided on each datasheet to assist in the interpretation o f the results.
Sample Arrival and Receipt
The eight water samples presented in this report were received at the STL Denver laboratory at a temperature o f 2I4C on November 16, 2006. The sample containers were received in an acceptable condition.
Standards
Analytical standards were prepared using the acid form o f the compound perfluorooctanoic acid (PFOA). PFOS is a commercial prepared and certified solution.
A di-carbon-13 labeled perfluorooctanoic acid, [l,2-di-13C] was introduced at the extraction step and was used as an internal standard for quantitation o f PFOA and PFOS.
Sample Extraction and Analysis
The samples presented in this report were analyzed for the target analytes by STL Denver's SOP DENLC-0012.
For water samples a 250 mL aliquot o f each sample is acidified with 1 mL o f 6N HC1 solution and it is extracted using solid phase extraction technique with methanol conditioned C l 8 cartridges. Each sample is spiked with the internal standard, prior to extraction. After the sample is passed through the cartridge, the analytes are eluted with 4 mL o f methanol. The final volume is brought to 5 mL using methanol and the extract is analyzed by LC/MS/MS.
Method OC Samples
The Method Blank is processed reagent water spiked with surrogate and prepared with each batch o f 20 samples o f the same matrix. The method blank was non-detect at the reporting limit for the target analytes.
Each batch is prepared with Laboratory Control Samples (LCS). The recoveries o f two concentration levels o f Laboratory Control Samples were within control limits.
Analytical Comments
Sample AIRPORT NORTH-RAW was chosen for matrix QC. A sample duplicate and matrix spike was performed on this sample with all QC criteria within control limits.
All QC criteria were met. No anomalies were noted.
EXECUTIVE SUMMARY - Detection Highlights
D6K160299
PARAMETER
RESULT
AIRPORT NORTH-RAW 1 1 / 1 5 / 0 6 0 9 : 2 0 0 0 1
PFOS PFOA
0.051 0.020
AIRPORT NORTH-TREATED 1 1 / 1 5 / 0 6 0 9 : 2 5 0 0 2
PFOS PFOA
0.049 0.020
MCALLISTER-RAW 1 1 / 1 5 / 0 6 0 9 : 0 0 0 0 3
PFOS PFOA
0.12 0.036
HAGLER-RAW 1 1 / 1 5 / 0 6 0 9 : 5 5 0 0 5
PFOS PFOA
0.048 0.018
HAGLER-TREATED 1 1 / 1 5 / 0 6 1 0 : 0 0 0 0 6
PFOS PFOA
0.051 0.016
BRONSON FIELD-RAW 1 1 / 1 5 / 0 6 1 3 : 0 5 0 0 7
PFOS PFOA
0.067 0.029
SUMIT BLVD.-BLENDING POINT 1 1 / 1 5 / 0 6 0 9 : 4 0 0 0 8
PFOS PFOA
0.028 0.015
REPORTING
LIM IT
UNITS
0.010 0.010
u g/L u g/L
0.010 0.010
u g/L u g/L
0.010 0.010
u g/L u g/L
0.010 0.010
u g/L u g/L
0.010 0.010
u g/L u g/L
0.010 0.010
u g/L u g/L
0.010 0.010
u g/L u g/L
ANALYTICAL METHOD
DEN - L C - 0 0 1 2 DEN - L C - 0 0 1 2
DEN - L C - 0 0 1 2 DEN - L C - 0 0 1 2
DEN - L C - 0 0 1 2 DEN - L C - 0 0 1 2
DEN - L C - 0 0 1 2 DEN - L C - 0 0 1 2
DEN - L C - 0 0 1 2 DEN - L C - 0 0 1 2
DEN -L C -0 0 1 2 DEN - L C - 0 0 1 2
DEN -L C -0 0 1 2 DEN -L C -0 0 1 2
METHODS SUMMARY
D6K160299
ANALYTICAL PARAMETER_________________________________________________________ METHOD________
LC /M S/M S, PFOA
DEN -L C -0 0 1 2
R eferen ces:
DEN Severn Trent Laboratores, Denver, Facility Standard Operating Procedure.
PREPARATION METHOD
METHOD / ANALYST SUMMARY
D6K160299
ANALYTICAL METHOD_________________________________ ANALYST________________________________
DEN -L C -0 0 1 2
S te v e C ow lin g
R eferen ces:
DEN Severn Trent Laboratores, Denver, Facility Standard Operating Procedure.
ANALYST ID _______
008738
p. 90
SAMPLE SUMMARY
D 6K 160299
w o # SAM PLE# C L IE N T SA M PLE ID
JJV 63 JJV 67 JJV 69 JJV 7C JJV 7E JJV 7F JJV 7G JJV 7H
001 002 003 004 005 006 007 008
A IR P O R T N O R TH -R A W A IR P O R T N O R T H -T R E A T E D M C A L L IST E R -R A W M C A L L IST E R -T R E A T E D H A G L E R -R A W H A G L E R -T R E A T E D BRONSON F IE L D -R A W S U M IT B L V D .-B L E N D IN G P O IN T
N O T E ( S ) ;__________________ ^ _______________________________________________________________________________________________ The analytical results of the samples listed above are presented on the following pages. A ll calculations are performed before rounding to avoid round-off errors in calculated results. Results noted as 'N O * were not delected at or above the stated limit. - This report must not be reproduced, except in full, without the written approval of the laboratory. - Results for the following parameters are never reported on a dry weight basis: color, corrosivity, density, flashpoint, ignitability, layers, odor,
paint filter test, pH, porosity pressure, reactivity, redox potential, specific gravity, spot tests, solids, solubility, temperature, viscosity, and weight.
SAM PLED DATE
SAM P T IM E
1 1 /1 5 /0 6 1 1 /1 5 /0 6 1 1 /1 5 /0 6 1 1 /1 5 /0 6 1 1 /1 5 /0 6 1 1 /1 5 /0 6 1 1 /1 5 /0 6 1 1 /1 5 /0 6
0 9 :2 0 0 9 :2 5 0 9 :0 0 0 9 :0 4 0 9 :5 5 1 0 :0 0 1 3 :0 5 09 :4 0
Camp Dresser & McKee Inc.
Client Sample ID: AIRPORT NORTH-RAW
HPIiC
Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #... Dilution Factor
D6K160299-001 Work Order
11/15/06 09:20 Date Received..
11/21/06
Analysis Date..
6325618
Analysis Time..
1
M e t h o d ........
JJV631AA 11/16/06 11/29/06 21:53
DEN -LC-0012
Matrix
PARAMETER PFOS PFOA
RESULT 0.051 0.020
REPORTING LIMIT 0.010 0.010
UNITS ug/L ug/L
SURROGATE 13C2
PERCENT RECOVERY 114
RECOVERY LIMITS (50 - 200)
: WATER
Camp Dresser & McKee Inc.
Client Sample ID: AIRPORT NORTH-RAW DUP
HPLC
Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #... Dilution Factor
D6K160299-001 Work Order #...: JJV631AD
11/15/06 09:20 Date Received..: 11/16/06
11/21/06
Analysis Date..: 11/29/06
6325618 1
Analysis Time..: 22:19
Method..... ... : DEN -LC-012
Matrix
PARAMETER PFOS PFOA
RESULT 0.055 0.019
REPORTING LIMIT 0.010 0.010
UNITS ug/L ug/L
SURROGATE 13C2
PERCENT RECOVERY
112
RECOVERY LIMITS (50 - 200)
: WATER
Camp Dresser & McKee Inc.
Client Sample ID: AIRPORT NORTH-TREATED
HPLC
Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #... Dilution Factor
D6K160299-002 Work Order
: JJV671AA
11/15/06 09:25 Date Received..: 11/16/06
11/21/06
Analysis Date..: 11/29/06
6325618
Analysis Time..: 22:32
1
Method..... ...: DEN -LC-0012
Matrix
PARAMETER PFOS PFOA
RESULT 0.049 0.020
REPORTING LIMIT 0.010 0.010
UNITS ug/L ug/L
SURROGATE 13C2
PERCENT RECOVERY 117
RECOVERY LIMITS (50 - 200)
: WATER
Camp Dresser & McKee Inc.
Client Sample ID: MCALLISTER-RAW
HPLC
Lot-Sample #.. . Date Sampled... Prep Date..... Prep Batch #... Dilution Factor
D6K160299-003 Work Order #... JJV691AA
11/15/06 09:00 Date Received.. 11/16/06
11/21/06
Analysis Date.. 11/29/06
6325618
Analysis Time.. 22:45
1
Method........ : DEN -LC-0012
Matrix
PARAMETER PFOS PFOA
RESULT_________ 0.12 0.036
REPORTING LIMIT
0.010 0.010
UNITS ug/L ug/L
SURROGATE 13C2
PERCENT
RECOVERY
RECOVERY_______ LIMITS
115 (50 - 200)
: WATER
Camp Dresser & McKee Inc.
Client Sample ID: MCALLISTER-TREATED
HPLC
Lot-Sample #... : D6K160299-004 Work Order #. .. : JJV7C1AA
Date Sampled...: 11/15/06 09:04 Date Received..: 11/16/06
Prep Date..... : 11/21/06
Analysis Date..: 11/29/06
Prep Batch
: 6325618
Analysis Time..: 22:58
Dilution Factor: 1
Method........ : DEN -LC-0C
Matrix.
PARAMETER PFOS PFOA
RESULT ND ND
REPORTING LIMIT 0.010 0.010
UNITS ug/L ug/L
SURROGATE I3C2
PERCENT RECOVERY 115
RECOVERY LIMITS (50 - 200)
: ViATER
Camp Dresser & McKee Inc.
Client Sample ID: HAGLER-RAW
HPLC
Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #.. . Dilution Factor
D 6K 160299-005 1 1 /1 5 /0 6 09:55 1 1 /2 1 /0 6 6325618
1
Work Order #... Date Received.. Analysis Date.. Analysis Time..
Method
:
JJV7E1AA 11/16/06 11/29/06 23:24
DEN - L C - 0 0 1 2
Matrix
PARAMETER PFOS PFOA
RESULT____________
0.048 0.018
REPORTING LIM IT
0.010 0.010
UNITS
ug/L ug/L
SURROGATE 13C2
PERCENT
RECOVERY
RECOVERY_______ LIMITS
117 (50 - 200)
: WATER
p. 97
Camp Dresser & McKee Inc.
Client Sample ID: HAGLER-TREATED
HPLC
Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #.. . Dilution Factor
D6K160299-006 Work Order #...: JJV7F1AA
11/15/06 10:0( Date Received..: 11/16/06
11/21/06
Analysis Date..: 11/29/06
6325618
Analysis Time..: 23:36
1
Method.. ...............: DEN -LC-0012
Matrix....
PARAM ETER
PFOS PFOA
RESULT 0.051 0.016
REPORTING LIMIT 0.010 0.010
UNITS ug/L ug/L
SURROGATE 13C2
PERCENT RECOVERY 119
RECOVERY LIMITS (50 - 200)
WATER
Camp Dresser & McKee Inc.
Client Sample ID: BRONSON FIELD-RAW
HPLC
Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #. .. Dilution Factor
D6K160299-007 Work Order #...
11/15/06 13:05 Date Received..
11/21/06
Analysis Date..
6325618
Analysis Time..
1
M e t h o d ........
JJV 7G 1A A
11/16/06 11/29/06 23:49
DEN -L C -0 0 1 2
Matrix
PARAM ETER
PFOS PF0
R E S U L T ________________
0.067 0.029
R E P O R T IN G
L IM IT
0.010 0.010
U N IT S
ug/L ug/L
SURROGATE
13C2
PER C EN T RECOVERY
119
RECOVERY L IM IT S
(50 - 200)
: WATER
Camp Dresser & McKee Inc.
Client Sample ID: SUMIT BLVD.-BLENDING POINT
HPLC
Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #... Dilution Factor
D6K160299-008 Work Order #...
11/15/06 09:40 Date Received..
11/21/06
Analysis Date..
6325618
Analysis Time..
1
M e t h o d ........
JJV7H1AA 11/16/06 11/30/06 00:02
DEN -LC-0012
Matrix
PARAMETER______________________ RESULT_________
PFOS
0.028
PFOA
0.015
REPORTING LIMIT 0.010 0.010
UNITS ug/L ug/L
SURROGATE 13C2
PERCENT
RECOVERY
RECOVERY_______ LIMITS
119 (50 - 200)
: WATER
p. 100
QC DATA ASSOCIATION SUMMARY
D6K160299
Sample Preparation and Analysis Control Numbers
SAMPLE# 001 002 003 004 005 006 007 008
MATRIX WATER WATER WATER WATER WATER WATER WATER WATER.
ANALYTICAL METHOD DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 DEN -LC-0012
LEACH BATCH #
PREP BATCH # 6325618 6325618 6325618 6325618 6325618 6325618 6325618 6325618
MS RUN# 6325438 6325438 6325438 6325438 6325438 6325438 6325438 6325438
p. 101
METHOD BLANK REPORT
HPLC
Client Lot
D6K160299
MB Lot-Sample #: R6K210000-618
Analysis Date..: 11/29/06 Dilution Factor:.1
Work Order #. ..: JJ7QR1AA
Prep Date.... ..: 11/21/06 Prep Batch #. ..: 6325618
Matrix........ : WATER Analysis Time..: 21:14
PARAMETER PFOA PFOS
RESULT ND ND
REPORTING
LIMIT
UNITS
0.010
ug/L
0.010
ug/L
METHOD DEN -LC-0012 DEN -LC-0012
SURROGATE________________ 13C2
PERCENT RECOVERY 102
RECOVERY LIMITS (50 - 200}
NOTE(S) ;______________________________________
Calculations are performed before rounding to avoid round-off errors In calcutaied results.
p. 102
LABORATORY CONTROL SAMPLE EVALUATION REPORT
HPLC
Client Lot #...: D6K160299
Work Order #...: JJ7QR1AC
LCS Lot-Sample#: RSK210000-618
Prep Date..... : 11/21/06
Analysis Date..: 11/29/06
Prep Batch #...: 6325618
Analysis Time..: 21:27
Dilution Factor: 1
Matrix
PARAM ETER
PFOA PFOS
SURROGATE
13C2
-
PER C EN T
RECOVERY
121 86
RECOVERY L IM IT S
(70 - 130) (39 - 120)
PERCENT RECOVERY
102
M ETHOD
DEN -LC-0012 DEN -LC-0012
RECOVERY L IM IT S
(50 - 200)
NOTE(S):
Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters
: WATER
p. 103
LABORATORY CONTROL SAMPLE DATA REPORT
HPLC
Client Lot #...: LCS Lot-Sample#: Prep Date..... : Prep Batch #...: Dilution Factor:
D6K160299
Work Order #...: JJ7QR1AC
R6K210000-618
11/21/06
Analysis Date..: 11/29/06
6325618
Analysis Time..: 21:27
1
Matrix....... .: WATER
PARAMETER PFOA PFOS
SPIKE AMOUNT 0.200 0.200
MEASURED AMOUNT 0.241 0.172
UNITS ug/L ug/L
PERCENT RECOVERY 121 86
METHOD DEN -LC-0012 DEN -LC-0012
SURROGATE 13C2
PERCENT RECOVERY 102
RECOVERY LIMITS (50 - 200)
NOTE(S ) ;______________________________________
Calculations are performed before rounding to avoid round-off errors In calculated results. Bold print denotes control parameters
I I
p. 104
LABORATORY CONTROL SAMPLE EVALUATION REPORT
HPLC
Client Lot
D6K160299
Work Order #...: JJ7QR1AD
LCS Lot-Sample#: R6K210000-618
Prep Date..... : 11/21/06
Analysis Date..: 11/29/06
Prep Batch #...: 6325618
Analysis Time..: 21:40
Dilution Factor: 1
Matrix
PARAMETER PFOA PFOS
PERCENT RECOVERY 92 66
RECOVERY LIMITS (70 - 130) (39 - 120)
METHOD DEN -LC-0012 DEN -LC-0012
SURROGATE 13C2
PERCENT RECOVERY 103
RECOVERY LIMITS (50 - 200)
NOTE(S) :______________________________________
Calculations arc performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters
: WATER
1
LABORATORY CONTROL SAMPLE DATA REPORT
HPLC
Client Lot #...: D6K160299
Work Order #...: JJ7QR1AD
LCS Lot-Sample#: R6K210000-618
Prep Date..... : 11/21/06
Analysis Date..: 11/29/06
Prep Batch #...: 6325618
Analysis Time..: 21:40
Dilution Factor: 1
Matrix.... ___ : WATER
PARAMETER PFOA PFOS
SPIKE AMOUNT 0.0200 0.0200
MEASURED AMOUNT 0.0185 0.0132
UNITS ug/L ug/L
PERCENT RECOVERY 92 66
METHOD DEN -LC-0012 DEN -LG-0012
SURROGATE 13C2
PERCENT RECOVERY 103
RECOVERY LIMITS (50 - 200)
NOTE(S):
Calculations arc performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters
p. 106
MATRIX SPIKE SAMPLE EVALUATION REPORT
H PLC
Lot-Sample MS Lot-Sample #: Date Sampled...: Prep Date. Prep Batch #...: Dilution Factor:
D 6K 160299 D 6 K 1 6 0 2 9 9 -0 0 1 1 1 /1 5 /0 6 0 9 :2 0 1 1 /2 1 /0 6 6325618
1
Work Order #...
Date Received.. Analysis Date..
JJV 631A C
1 1 /1 6 /0 6 1 1 /2 9 /0 6
Matrix
PARAMETER PFOA PFOS
PERCENT RECOVERY 112 71
RECOVERY LIMITS {70 - 130) (39 - 120)
SURROGATE 13C2
PERCENT RECOVERY 114
NOTE(S):
Calculations are performed before rounding to avoid round-off errors in calculated results. Bold print denotes control parameters
METHOD DEN -LC-0012 DEN -LC-0012
RECOVERY LIMITS (50 - 200)
: WATER
MATRIX SPIKE SAMPLE DATA REPORT
H PLC
Lot-Sample #... MS Lot-Sanple # Date Sampled... Prep Date..... Prep Batch # -- Dilution Factor
D6K160299
Work Order
JJV631AC
D6K160299-001
11/15/06 09:20 Date Received..: 11/16/06
11/21/06
Analysis Date..: 11/29/06
6325618
1
Matrix........ : WATER
PARAMETER PFOA PFOS
SAMPLE SPIKE MEASRD AMOUNT AMT AMOUNT 0.020 0.199 0.243 0.051 0.199 0.192
UNITS ug/L ug/L
SURROGATE 13C2
PERCENT ' RECOVERY
114
NOTE(S):
Calculations are performed before rounding to avoid round-off errors in calculated results. Bold prim denotes control parameters
PERCENT RECOVERY 112 71
METHOD DEN -LC-0012 DEN -LC-0012
RECOVERY LIMITS (50 - 200)
p. 108
SAMPLE DUPLICATE EVALUATION REPORT
HPLC
Client Lot #. .. SD Lot-Sample # Date Sampled... Prep Date..... Prep Batch #... Dilution Factor
D6K160299 D6K16Q299-001 11/15/06 09:20 11/21/06 6325618 1
Work Order #...: JJV631AA JJV631AD
Date Received..: 11/16/06 Analysis Date..: 11/29/06 Analysis Time..: 22:19
-SMP Matrix...... : WATER -DUP
MS Run # ...... :
PARAMETER PFOS PFOA
SAMPLE RESULT 0.051 0.020
DUPLICATE RESULT 0.055 0.019
UNITS ug/L ug/L
RPD RPD LIMIT 6.6 (0-20) 7.1 (0-20)
METHOD DEN -LC-0012 DEN -LC-0012
SURROGATE RECOVERY" 13C2
SAMPLE % RECOVERY 114
DUPLICATE % RECOVERY 112
RECOVERY LIMITS (50 - 200)
I
p. 109
C h a in o f C u s to d y R e c o rd
El STL
Severn Trent Laboratories, Inc.
STl-4 M i (CW01] Client
Oviv\f r x /w
5
~Xac..
325"
O u * & ), BIJf-M-lOO
Project Name and Location (State)
C .0A
State Zip Code
FL 3 2 3 * 3
~
f<aarA-ccfA,
Contract/Purchase Order/Ouote No.
_________________ ^ 3 0 2 /
Sam ple I.D. No. and Description (Containers tor each sample may be combined on one line)
D a te
iYPorf //br+K - R ftV j
~ w ~ /l./r.o t,
Project Managet--
At
I/A ^ ia Z.- /X nJaj-tfO A
Telephone Number (Area Code)/Fax Number
CSS) 3&L-Sxfr / 3$(o~ (eifil
Site C on tact.
Dftwfd L- farjbsts&s*
Camer/Waybiit Number
Lab Contact
*
Time
Matrix
Containers & Preservatives
b SN i
3
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OS 2,0
^llJS.Ole
Lab Number
Analysis (Attach list if more space is needed)
ll-lS.ofo 0 1X5
/V^oA IL'j'4-v.v --- ^ . f m j
ll-lf.ot. *76b
ctr R * u j -- ~7h *A O
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ll-IS.oi U s
Ll-lS-ob O *?Y 0
STL Denver 4 9 5 5 Yarrow Street Arvada, CO 8 0 0 0 2
Chain of Custody Number
343801
Page
^
of ^
Special Instructions/ Conditions o f Receipt
L C /l* /frS . /'.rf' P-Of
Possible Hazard Identification
Sample Disposal
Turn Around Time Required
24 Hours D 48 Hours
I. Relinquished By
7 Days
V
TO& A-
3. Relinquished By
1$ U Days
: d2IOays
...........
O Other
Date
Date / M >6 Date
Time
Time /$T ; 0 0
Time
OC Requirements (Specify!
T. OecBtved By t K f t - f
fe/ -
L v -m - R -
, /]
2. Received By
y
/m
3. Received By* *
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Comments
DISTRIBUTION: WHITE Returned to Client with Report: CANARY - Stays with the Sample: PINK Field Copy
n :loDate U - i l oi,
Time
Date/ !
. Time
iiiHnko i o m
Dite ' '
Time
p. 110
LC/MS
Supporting Documentation
Sample Sequence, Chromatograms/Mass Spectra
SEVERN
TRENT
Lot ID:
0 6 ( 7 2 9 3 _________
Client: ( J ^ v y h + < .
Method:
- n p f a a <8-^p?<
Associated Samples:__________j -- _____________
Batch#(s):__ |
% _________
I certify that, to the b est o f m y knowledge, the attached p a c k a g e represents a complete and accurate copy o f the original data.
Signature/Date:_
p. 111
LC/MS SEMIVOLATILE ORGANIC EXTRACTION
LOG SHEETS
RQC058
Severn Trent Laboratories, Xnc. EXTRACTION BENCH WORKSHEET
Run Date: 11/21/06
Time:
1:59
i t ' k ' k ' k i t 'k i t i e i t i K i e i c k 'i f k i i i t 'k i r i f l t + 'k *
* *
* QC BATCH: 6325618 * ****************************
PREP DATE: 11/21/06 18:30 COMP DATE: 11/21/06 23:30
EXTR EXPR
ANL LOT#,MSRUN#/ TEST DUE WORK ORDER FLGS
D6K160299-006
11/22/06 12/04/06 JJV7F-1-AA
D
COMMENTS:
EXT MTH MATRIX B7 H5 WATER
INIT/FIN
PH`'S
SOLVENTS
WT/VOL INIT ATOT ADJ2 EXTRACTION'~VOL--EXCHANGE
258roL
NA NA NA MEOH
5.0 OmL
4.0
SPIKE STANDARD/ VOL SURROGATE ID
.0 1.0ML 878.73.2 6/19/06
D6K160299-007
11/22/06 12/04/06 JJV7G-1-AA
D B7 HS WATER 252ml.
NA NA NA MEOH
COMMENTS:
5. OOmL
4.0
.0 1.0ML 878.73.2 6/19/06
D6K16O299-O08
11/22/06 12/04/06 JJV7H-1-AA
D B7 H5 WATER 251tnL
NA NA NA MEOH
COMMENTS:
S .OOmL
4.0
.0 1. OML 878.73.2 6/19/06
D6K160304-001
11/22/06 12/04/06 JJV7X-1-AA
D B7 H5 WATER 254xnl*
NA NA NA MEOH
COMMENTS:
5.00ml*
4.0
.0 1. OML 878.73.2 6/19/06
D6K160304-002
11/22/06 12/04/06 JJV75-1-AA
D B7 H5 WATER 254raL
NA NA NA MEOH
COMMENTS:
5.0 OmL
4.0
.0 1. OML 878.73.2 6/19/06
D6K160304-003
11/22/06 12/04/06 JJV79-1-AA
D B7 H5 WATER 25OmL
NA NA NA MEOH
COMMENTS;
S.OOmL
4.0
.0 1. OML 878.73.2 6/19/06
D6K160304-004
11/22/06 12/04/06 JJV8E-1-AA
D
COMMENTS:
B7 H5 WATER
256mL
NA NA
5.OOmL
NA MEOH
4.0
.0 1. OML 878.73.2 6/19/06
R6K210000-618 11/22/06 0/00/00 JJ7QR-1-AAB COMMENTS
B7 H5 WATER 250mL
NA NA NA MEOH
S.OOmL
4.0
.0 1. OML 878.73.2 6/19/06
R6K210000-618 11/22/06 0/00/00 JJ7QR-1 -ACC COMMENTS : MID LCS
B7 H5 WATER 25OmL
NA NA NA MEOH
5.OOmL
4.0
.0 1 .OML LCMS0040 6/28/06 1 -OML 878.73.2 6/19/06
R6K210000-618 11/22/06 0/00/00 JJ7QR-1-ADC COMMENTS : LOW LCS
B7 H5 WATER 250trtL
NA NA NA MEOH
5.OOmL
4.0
.0 0.1ML LCMS0040 6/28/06 1.0ML 878.73.2 6/19/06
p. 112
DEN-LC-0012 H20:ELGA,C31E23 ME0H:C15E75 CART:S201-38,24012-4 6M HCL:919.63.3
5/bTHT,lP'AA501.2 W:JB
""....
...
RQC0S8
Severn Trent Laboratories, Inc. EXTRACTION BENCH WORKSHEET
LEV LEV
LEV LEV
1~ ~ 7 ~ I Y Blank
~T ~
Y
~ ` ~ ~
Y
nes
Y Y Check Y Y Spike & Surrogate Worksheet
Y Y MS/MSD Y Y Vial contains correct volume
Y Y Labels, greenbars, worksheets
computer batch: correct & all match
Anomalies to Extraction Method
Extractionist: 007183 Michael T. Dedio
Concentrt ionis'd TTO'7183 Michael T. Dedio
** ** OC BATCH: 325618 **
Run Date: 11/21/06
Time:
1:59
Expanded Deliverable
COC Completed Bench Sheet Copied Package Submitted to AnalvticalGroup Bench Sheet Copied per COC
PREP DATE: 11/21/06 18:30 COMP DATE: 11/21/06 23:30
Reviewer/Date: DEDIOMA / 11/21/06
EXTR EXPR
AN-L LOT#,MSRUN# / TEST DUB WORK ORDER FLGS
D6K160299-001
11/22/06 12/04/06 JJV63-1-AA
D
COMMENTS :
EXT MTH MATRIX B7 H5 WATER
LC/M S/M S, PFOA SOLID PHASE EXTRACTION (NOMINAL)
INIT/FIN
PH"S
WT/VQL INIT SDJI ADJ2
SOLVENTS
251mL
NA NA NA MEOH
S.OOmL
4 .0
SPIKE STANDARD/ VOL SURROGATE ID
.0 1.0ML 878.73.2 6/19/06
D6K160299-001
11/22/06 12/04/06 JJV63-1-ACS COMMENTS :
B7 H5 WATER 250mL
NA NA NA MEOH
5.00mL
4 .0
.0 1.0ML LCMS0040 6/28/06 1.0ML 878.73.2 6/19/06
D6K160299-001 11/22/06 12/04/06 JOV63-I-ADX
COMMENTS :
B7 HS WATER 250mL
NA NA NA MEOH
5.OOmL
4.0
1.0ML 878.73.2 6/19/06
D6K160299-002
11/22/06 12/04/06 JJV67-1-AA COMMENTS :
B7 H5 WATER 25SmL
NA NA NA MEOH
5.OOmL
4.0
.0 1.0ML 878.73.2 6/19/06
D6K160299-003 11/22/06 12/04/06 JJV69-1-AA COMMENTS :
B7 HS WATER 2S3mL
NA -NA NA MEOH
S.OOmL
4.0
.0 1.0ML 878.73.2 6/19/06
D6K160299-004
11/22/06 12/04/06 JJV7C-1-AA COMMENTS :
B7 H5 WATER 252mL
NA NA NA MEOH
5.OOmL
4.0
.0 1.0ML 878.73.2 6/19/06
D6K160299-005 11/22/06 12/04/06 JJV7E-1-AA COMMENTS :
B7 HS WATER 258mL
NA NA NA MEOH
5.OOmL
4.0
.0 1.0ML 878.73.2 6/19/06
p. 113
ft *_ P tT C W
gQ Q T jp
E - EPA 600 D - EXP.DEL)
M - CLIENT REQ MS/MSD
I
NUMBER OF WORK ORDERS IN BATCH:
17
p. 114
p. 115
LC/MS SEMIVOLATILE INSTRUMENT RUN LOG
p. 116
Sample List Report
MassLynx 4.1
Sample List: C:\MassLynx\PFOA.PRO\SampleDB\pf36k29(2).SPL Last Modified: Thursday, November 30,2006 07:06:14 Mountain Standard Time
Printed:
Thursday, November 30,2006 07:07:31 Mountain Standard Time
Page 1 of 2 Page Position (1,1)
Fite Name Sample ID File Text
Sample Type Cone A Cone B Bottle Extract mL
1 pf36k2954 930.86.1 Blank
Blank
2 pf36k2955 930.86.2 0.2pg/L
Standard
3 pf36k2956 930.86.3 0.5/yg/L
Standard
4 pf36k2957 930.86.4 1 aq/l
Standard
5 pf36k2958 930.86.5 2/yg/L
Standard
6 pf36k2959 930.86.6 5pg/L
Standard
7 pf36k2960 930.86.7 10pg/L
Standard
8 pf36k2961 930.86.8 20 pg/L
Standard
9 pf36k2962 930.86.1 Blank
Blank
10 pf36k2963 930.86.9 2 pg/L 1CV
QC
11 pf36k2964 930.86.3 0.5 fjg IL RLV
QC
12 pf36k2965 JJ7QR1A R6K210000-618 MB Blank
13 pf36k2966 JJ7QR1AC R6K210000-618 LCS QC
14 pf36k2967 JJ7QR1AD R6K210000-618 LCS QC
15 pf36k2968 JJV631AA D6K160299-1
Analyte
16 pf36k2969 JJV631AC D6K160299-1 MS QC
17 pf36k2970 JJV631AD D6K160299-1 DUP Analyte
18 pf36k2971 JJV671AA D6K160299-2
Analyte
19 pf36k2972 JJV691AA D6K160299-3
Analyte
20 pf36k2973 JJV7C1AA D6K160299-4
Analyte
21 pf36k2974 930.86.6 5 pg/L CCV
QC
22 pf38k2975 JJV7E1AA D6K160299-5
Analyte
23 pf36k2976 JJV7F1AA D6K160299-6
Analyte
24 pf36k2977 JJV7G1AA D6K160299-7
Analyte
25 pf36k2978 JJV7H1AA D6K160299-8
Analyte
26 pf36k2979 JJV7X1AA D6K160304-1
Analyte
27 pf36k2980 JJV751AA D6K160304-2
Analyte
28 pf36k2981 JJV791AA D6K160304-3
Analyte
29 pf36k2982 JJV8E1AA D6K160304-4
Analyte
30 pf36k2983 930.86.1 Blank
Blank
31 pf36k2984 930.86.2 0.2 pg/L
QC
32 pf36k2985 930.86.3 0.5 pg/L
QC
33 pf36k2986 930.86.4 1 pg/L
QC
34 pf36k2987 930.86.5 2 pg/L
QC
35 pf36k2988 930.86.6 5 pg/L
QC
36 pf36k2989 930.86.7 10 pg/L
QC
37 pf36k2990 930.86.8 20 pg/L
QC
0 0.2 0.5 1 2 5 10 20 0 2 0.5 0 10 1.0 0 10 0
0 0 0 5 0 0 0 0 0 0 0 0 0 0.2 0.5 1 2 5 10 20
0 0.208 0.520 1.041 2.082 5.205 10.411 20.821
0 2.082 0.520
0 10.411 1.0411
0 10.411
0 0 0 0 5.205
0
0 0 0 0 0
0 0 0 0.208 0.520 1.041 2.082 5.205
10.411 20.821
1:1,A 1.000000
1:1,B 1.000000
1:1,C 1.000000 1:1,D 1.000000
1:1,E 1.000000 1:1,F 1.000000 1:2,A 1.000000 1:2,8 1.000000
1:1,A 1.000000 1:2,C 1.000000
1:1,C 1.000000 2:1,A 5.000000 2:1,B 5.000000
2:1,C 5.000000 2:1,0 5.000000 2:1,E 5.000000 2:1,F 5.000000
2:2,A 5.000000
2:2,B 5.000000 2:2,C 5.000000
1:1,F 1.000000 2:2,D 5.000000
2:2,E 5.000000 2:2,F 5.000000 2:3,A 5.000000 2:3,B 5.000000 2:3,C 5.000000
2:3,D 5.000000
2:3,E 5.000000 1:1,A 1.000000 1:1,B 1.000000
1:1,C 1.000000
1:1,0 1.000000 1:1,E 1.000000 1:1,F 1.000000 1:2,A 1.000000 1:2,B 1.000000
Sample List Report
MassLynx 4.1
Sample List: C:\MassLynx\PFOA.PRO\SampleDB\pf36k29(2).SPL Last Modified: Thursday. November 30,2006 07:06:14 Mountain Standard Time
Printed:
Thursday, November 30, 2006 07:07:31 Mountain Standard Time
Sample m l or g Dilution Inject Volume MS Tune File Inlet File MS File
1.000000 1.000000 1.000000 1.000000 1.000000
1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 250.000000 250.000000 250.000000 251.000000 250.000000 250.000000 255.000000 253.000000 252.000000 1.000000 258.000000 258.000000 252.000000 251.000000 254.000000 254.000000 250.000000 256.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000
1.000000 1.000000 1.000000 1.000000 1.000000
1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000
1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000
20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000
PFOA PFOA PFOA PFOA
PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA
PFOA PFOA PFOA PFOA PFOA
PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA
PFOAZTesi PFOA2Test PFOA2Test PFOA2Test
PFOA2Test PFOA2Test
PFOA2Test PFOA2Test
PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Te$t PFOA2Test PFOA2Test PFOA2Test
PFOA2Test PFOA2Test PFOA2Test PFOA2Test
PFOA2Test PFOA2Test PFOA2Test PFOA2Test
PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test PFOA2Test
PFOSLong PFOSLong PFOSLong PFOSLong
PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong PFOSLong
i
p. 117
Page 2 of 2 Page Position (2,1)
I (
p. 118
LC/MS SEMIVOLATILE STANDARD DATA
I I I
Quattro Prem ierTune Parameters
M as sL y nx 4 .1
File:
C:\MassLynx\PFOA.PRO\ACQUDB\PFOAms1.ipr
Printed:
Tuesday, November 2 8 ,2 0 0 6 12:06:27 Mountain Standard Time
p. 119 Page 1 of 1
Type MS Scan
Source (ES-) Capillary (kV) Cone (V) Extractor (V) RF Lens (V) Source Temperature (C) Desolvation Temperature (C) Cone Gas Flow (L/Hr) Desolvation Gas Flow (L/Hr)
Analyser LM 1 Resolution HM 1 Resolution Ion Energy 1 Entrance Collision Exit LM 2 Resolution HM 2 Resolution ion Energy2 Multiplier (V) Syringe Pump Flow (uL/mln)
Pressure Gauges Gas Cell Pirani Pressure(mbar)
MUX Configuration Probe
Source T-WAVE Parameters Automated
Collision Cell T-W AVE Parameters Automated
Start Mass 412
Settings 1.50 20.00 5.00 0.2 120 300 19 699
Settings 12.5 12.5 0.8 50 2 50 12.5 12.5 2.5 650 20.0
< 1e-4
Standard
End Mass 414
Readbacks 1.46 -26.25 -5.98
119 296
Set Mass
Readbacks
50 2 49
-649
Quattro Premier Tune Param eters
M assLynx 4.1
File:
C:\MassLynx\PFOA. PRO\ACQUDB\PFOA.ipr
Printed:
Tuesday, November 2 8 ,2 0 0 6 12:08:12 Mountain Standard Time
p. 120
Page 1 of 1
Type Daughter Scan
Source (ES-) Capillary (kV) Cone(V) Extractor (V) RF Lens (V) Source Temperature (C) Desolvatlon Temperature (C) Cone Gas Flow(L/Hr) Desolvation Gas Flow (L/Hr)
Analyser LM 1 Resolution HM 1 Resolution Ion Energy 1 Entrance Collision Exit LM 2 Resolution HM 2 Resolution Ion Energy 2 Multiplier (V) Syringe Pump Flow (uL/min)
Pressure Gauges Gas Cell Pirani Pressure(mbar)
MUX Configuration Probe
Source T-WAVE Parameters Automated
Collision Cell T-W AVE Parameters Automated
Start Mass 368
Settings 1.50 20.00 5.00 0.2 120 300 19 699
Settings 12.5 12.5 0.8 0 10 1 12.5 12.5 0.8 650 20.0
5.35e-3
Standard
End Mass 370
Readbacks 1.47 -26.01 -6.23
119 296
Set Mass 413
Readbacks
10 10 10
-649
Quattro Prem ier Tune Parameters
M assLynx 4,1
File:
C:\MassLynx\PFOA.PRO\ACQUDB\PFOA.ipr
Printed:
Tuesday, November 28, 2006 12:08:37 Mountain Standard Time
p. 121 Page 1 of 1
Type Daughter Scan
Source (ES-) Capillary (kV) Cone (V) Extractor (V) RF Lens (V) Source Temperature (C) Desolvation Temperature (gC) Cone Gas Flow (UHr) Desolvation Gas Flow (L/Hr)
Analyser LM 1 Resolution HM 1 Resolution Ion Energy 1 Entrance Collision Exit LM 2 Resolution HM 2 Resolution Ion Energy 2 Multiplier (V) Syringe Pump Flow (uL/min)
Pressure Gauges Gas Cell Pirani Pressure(mbar)
MUX Configuration Probe
Source T-WAVE Parameters Automated
Collision Cell T-W AVE Parameters Automated
Start Mass 218
Settings 1.50 20.00 5.00 0.2 120 300 19 699
Settings 12.5 12.5 0.8 0 16 1 12.5 12.5 0.8 650 20.0
5.30e-3
Standard
End Mass 220
Readbacks 1.47 -26.01 -5.49
119 295
Set Mass 413
Readbacks
15 15 17
-649
p. 122
p. 123
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p. 124
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