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 \ \\ \ \ \ \ \ \ \ \ \ \\ \ \ \ \\ \\ \\ \ \ \ V 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 Water sf f m M i ______ ^ ------^ m s' i;:;;:;/: / |(y _ v x \........ /.ii/i i f i - i f t i y i / Water Waer Water Water Water Water ;y;;/;. Water Water Water Liquid d ilu id ;://:;////. Liquid liquid /y Liquid Liquid : ^ a ^ i 1 p1 i if M ;/l c X'- y s M t - : :i j i f - i i k s' s ', s' Y T :. \ i L i./. \s i LAIQ i M !d u i f M J b io . h c ^ e , Lj S f t t . Wi ' Vf ) H icT tfc i f f t PAHuei bfaF, C K 1 66 1 l 1 2 5 hA. ____________1.5, U * A S 2 -- g 4 V ________________________________________________________ Surrogate ID: i P M S f o b l Io m I spikeiD ____ ( o a , i Witnessed By: Analvst: -WA. Printed 2 9 10 7:37 Assisted Bv: Preparation Information Benehsheet w 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 _ _ PROJECTMANAGER f%. , t A 1 U- A v ie ta r-r**'' COMPANY/ADDRESS/-* n 'AS --r t^A m p v u s s w ) M c m * 3c)l\./\ Krtyc /2<S. , /Vi - /fro crvrsw^P -7 ^ (U k ftX ^ / P z 3 ^ . 3 0 3 E-MAILADDRESS v * .* A A iiW ftq l 1_ Cca,f*v- Cci/v> PH0NE' FAX,g s k - r e f e - 9 / .......... / c / 4r / ,T i t ! o/ /& / j& "" & J i u ^ - SAMPLE I.D. DATE TIME /# / LAB I.D. MATRIX / ? / AiVPOrri' uj l l .l f .6 i , 0 7 2 0 gU) A i r Pc'-FA ^ "^ -~ T n a A tS I1-/S-.6L liJCbfc 0 7 0 0 GW (ytt /tl\ AUtf-lojr - *77>gA.g3 U. Ifo fo 6 ? o 7 GW I k f/gr- il-lie 0 7 5 5 u rti /C 6 0 Gw u> BroAipft ? w - Raw tt.lS.b\o / 3 o 5 U> ibfnn.4 S/v- -- g/cmJ.-rtV PoAVr J/.l/.ofer f 0 7 7 0 GW M ilC A b 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 s 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 II IS.oic e r o i 3 ^ " ll-i.olp 7SS* w u.ir.olo ! o o O Bronx* F f ^ - Rj 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* * ( j? f i/'/ / (V /M y > 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 i ii a p. 124 1J i p. 125 Project No. romiPageNo. i y L , -zsMJ!1* ML4L s l -- k: H 11 0 -C tz. * ;1r { 1i 1 L cCL O . iV -ft. *6.L -- L r: ( ( c0 2d k~\ ( c -- y i)*'TC ;f/ >- kif Ai^'- i j r j .. --j 0 -- U so L tlQ t <7xt %* F? \s tj (--( < 1 (. 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