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Precise Research. Proven Results. Enclosure 5 Analytical Report Fluorochemical Characterization of Water and Sediment Samples Decatur Bakers Creek #2 -July 2003 (E03-0561) Exygen Research Laboratory Report No. L34910 Revision 1 Testing Labora tory Exygen Research 3058 Research Drive State College, PA 16801 Requester Jess Eldridge 3M Environmental Technology and Safety Services 935 Bush Avenue Building 0002-03-E-09 PO Box 33331 ST. Paul, MN 55133-3331 000010 State College, PA 16801, USA 7 introduction Results are reported for the analysis of surface Exygen Research (Exygen) from Pace Analytical. project is L34910. water and sediment samples received by The Exygen study number assigned to the Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/M!YMS) was requested for all samples. A total of 26 samples were received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicak: l Table 1: Target Analysis Comwund Name Perfluorohexanesulfonate Perfluorooctanesulfonate . Perfluorooctanoic Acid _ Perfluorocctanesulfonvlamide Acronvrn C6 Sulfonate fPFHS) C8 Sulfonate (PFOS) C8 Acid (PFOA) FOSA The analytical methods used were originally developed for groundwater samples and were validated by Exygen. The validation protocol and results are on file with Exygen. Only the C8 Sulfonate, FOSA, and C8 Acid were included in the original method validation. It should be noted that the quality control elements included in this analysis demonstrate the applicability of the method to the additional analytes. 2 Sample Receipt The samples were submitted in plastic containers. All samples were cooled to 4'C from time of collection to receipt at Exygen Research. Samples were stored at 4% from receipt at Exygen Research until analysis. Samples were collected on 7/21/03 and 7/23/03. Chain-ofcustody information is presented in Attachment C. 3 Holding Times Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 30 days of receipt. PAGEZoF5 uw011 4 Methods -Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Water samples were initially treated with 200 UL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliter portion of sample was used for analysis. The samples were transferred to a Cl8 SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatment resulted in an eight-fold concentration of the diluted samples prior to analysis. Sediment samples were first extracted into methanol (5 grams of sediment to 5 mL of methanol). The methanol extract was diluted to forty-milliliters and treated in the same manner as the water samples, using SPE. 4.1.2 Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. fans characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard HP1 100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples extractions and analyses were performed between 7/31/03 and 8/13/03. Exact dates for extraction and analysis of each sample batch are given in the raw data. Raw analytical data is provided in Attachments D and E. 5 Analysis 5.1 Calibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ngR (ppt) for LC/MS/MS analysis. The instrument response versus the concentration was plotted for each point. Using linear regression with l/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (?) were determined. A calibration curve is acceptable if r 20.985 (rc?~0.970). Calibration standards are prepared using the same SPE procedure used for samples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. All calibration criteria were met for this analysis. PAGE3UF5 000012 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant. instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LCNNMS analytical methods. 5.4 Matrix Spikes Field matrix spikes were prepared at low and high levels for each sample for all compounds of interest. Single laboratory matrix spikes were also performed for each sample. Laboratory control spikes (see section 5.6) consisting of laboratory water spiked at the time of extraction were performed with each analytical set. Matrix spike recoveries are given in Attachment B. For sediment samples, recovery is calculated from the amount present in the sample extract. Please see Section 5.7 for additional discussion of matrix spike recoveries. 5.5 Duplicates Field and laboratory duplicates were performed for each sample. The duplicate results are included with the sample results in Attachment A. 5.6 Laboratory Control Samples For LCIMSNS analyses, Milliq water was spiked with all compounds with each extraction set. All recoveries for all compounds were between 70-130% in each LCS. Results are given along with the raw data in Attachment D. 5.7 Statement of Accuracy Based on results of field spikes, laboratory spikes, field blank spikes, and laboratory control spikes, the analytical accuracy for all compounds is + 30%. Exceptions for the water samples are as follows: BC2 SW-04 high spike (PFOA - 57%, PFOS - 62%, FOSA - 58%). BC2 SW05 high spike (PFOA - 66%, FOSA - 40%), BC2 SW-66 high spike (FOSA - 60%) Outfall to River SW-25 (FOSA - 58%). Also, several low spike samples showed unacceptable recoveries in cases where the spiking concentration was comparable or below the inherent sample concentration. However, all laboratory control spikes, laboratory matrix spikes, and all other field spikes showed recoveries between 70% and 130% for all compounds. The accuracy for the sediment samples is based upon laboratory spike recoveries, all of which were between 70% and 130% for all compounds. 6 Data Summary Please see Attachment A for a detailed listing of the analytical results. Results are reported in parts per billion (ppb) (@ml) for the water samples. Sediment samples are also reported in units of parts per billion (ppb) (rig/g). Sediment results are reported on both an as-received and dry-weight basis. PAGE4ffS 000013 7 Da t&ample Retention Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. 8 Attachments 8.1 Attachment A: Results 0.2 Attachment B: Matrix Spike Recoveries a.3 Attachment C: Chain of Custody 8.4 Attachment D: Raw Analytical Data (Surface Water Samples) 8.5 Attachment E: Raw Analytical Data (Sediment Samples) 9 Signatuies Paul Connolly, Team Leader - L&MS Date Date Other Lab Members Contributing to Data Karen Rlsha PAGE5oF5 oc)oo14 SECTION A 000015 pQfgM!iH Precise Research. Proven Results. Summary of PFOA, PFHS, PFOS and FOSA in Water Samples Sample ID Em SW-04 BC2 SW-04' i3C2, SW-04 Dup BC2 SW-05 BC2 SW-05' BC2 SW-05 Dup BC2-SW-06 BC2-SW-06' BC2-SW-06 Dup Outfall to River SW-25 Outfall to River SW-25' Outfall to River SW-25 Dup Equipment Blank-Pump Equipment Blank-Dredge ... Field Controlflravel Blank Analyte C8 Acid PFOA Perfluorooctanolc Acid 4.21 4.21 2.54 0.591 0.616 1.56 12.1 12.3 11.6 15.8 16.0 14.4 ND ND ND Found (ng/mL) C6 Sulfonate PFHS Perfluorohexanesulfonate 0.896 0.882 0.571 0.155 0.152 0.377 6.06 6.30 5.87 7.66 7.10 6.77 ND ND ND Sample ID BC2 SW-04 BC2 SW-04' BC2 SW-04 Dup BC2 SW-05 BC2 SW-05* BC2 SW-05 Dup BC2-SW-06 BC2-SW-06" BC2-SW-06 Dup Outfall to River SW-25 Outfall to River SW-25' Outfall to River SW-25 Dup Equipment Blank-Pump Equipment Blank-Dredge Field Control/Travel Blank Analyte ,$8 Sulfonate PFOS Perfluorooctanasulfonate 11.5 : 11.5 8.25 -1.67 1.54 4.33 26.1. 26.7 25.1 31.2 31.5 30.8 ND ND ND Found (ng/mL) FOSA Perfluorooctsnesulfonylamide 1.39 1.37 0.790 0.146 0.150 0.389 2.43 2.30 2.57 3.26 3.18 3.28 ND ND ND ND=Not Detected=Response NQ=Not Quantifiable=Response *Laboratory Duplicate between 0 and 0.025 nglmL between 0.025 ng/mL and LOQ (0.05 ng/mL) 000016 State college, PA 16801, USA F: 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. RUSH SERWG-Exygen routinely offers expedited turnaround times on c&Cal ,malyrcs. Rush analysis services are contingcnf upon ,~~ailabill:y and prearrangement with an authorized Exyi;en representative A sulcharge i\ u:ur~iIy added lo lhe lrst bee i/ rush ~nclly~s is reqursteci M/N/MUM F&--The dollars (610c1) mlntmum fee for colnmelci.tl servicts is one hundred SAMPLE COLLEfflO~~`SUBMI-C~~e~~t shll be rrsponsrblr tar proper collectton preservation. packrng and packag~np, and sh:p!"cnt of the `;amplc$s) in accordance with apDllcablrZ IW any good commercial practice Title and risk of lobi with tecpect to subnlitted sanlplcs shd~l ai ,111 tmes reman with client prior to dcccptancr by dn Exygen sample c;uslodian Exygen will inlttale a chain-of-custody upon szmplc recetpt unless the client Includes one wtt,h the s~mplc(s). Up request. Exyg~ wtll provrde ehain.of-custody forms for client's use All iamprcs submitted must be acrompamecl hv purchase urcler. or stgned quotal~on; s4mple description, including sJr*ple type. source. time ancl date of collection. specthc cmalyse\ requested, esti~n.ttecl concerilralirrn levels. requested report date, current i:iltrng address. and other relev,~nt ftltorrn,~tion upon reqtrest Exygen WIII provide .?nd slrlp ;~ppropt I;{ttl ~c~rn~~le colalalncrb to clients. Thesr cnntalners w11l include the apptopri;te preservative it partrcular an,dyses require one. It IS the respor:sibMy of the clienl to handle these preserved containers sntely, and using ~11appropriate safety precautions Clients requesting ovetnighl delivery of s;,mple tontainers will be involccd ior freight Exygen r-cserves the right to charge `I fee for samplt~ colllalrlerj 5AMPLE reporting DISPOSAL.-Exygen retzns samples for one month after resells. then disposer of or return, the salnple. Unless the cltent Oooolr gyg@L Precise Research. ,, Proven Results. Summary sul1m`*$ of PFOA, PFHS, PFOS and FOSA In sb/ll Samples Sample ID BC2 SED-04 BC2 SED-04 BCti-SED-05 BC2kED05* BC2-SED-06 BC2-SED-06' Outfall to River SED-25 Outfall lo River S@-25' Outfall to River SED-25 Dup Analyte Found (rig/g, as received) Ead44 5 C8 Acid PFOA C6 Sulfonate PFHS Perfluorooctanolc Acfd Perfluorohexanesulfonate 3.02 0.566 2.14 0.413 5.14 1.45 4.41 1.75 14.2 2.46 13.6 2.61 10.7 3.19 7.59 2.26 17.7 4.98 Sample ID BC2 SED-04 BC2 SED-04' BC2 SED-05 BC2 SED-05' BC2-SED-06 BC2-SED-06' Outfall to River SED-25 Outfall to River SED-25' Outfall to River SED-25 Dup Analyte Found C8 Sulfonate PFOS Petfluorooctanesulfonate 14.6 11.9 `.. 22.8 25.0 880 . . 992 `,. 107 72.1 140 (rig/g, as received) FOSA Perfluorooctanesulfonylamlde 7.15 7.84 7.86 12.1 71.4 83.2 28.0 23.5 35.7 N&Not Detected=Response NQ=Not Quantifiabledesponse 'Laboratory Duplicate between 0 and 0.2 rig/g between 0.2 rig/g and LOO (0.4 y/g) 00003B State College, PA 16801, USA F: 814.231 .1580 exygen.com STANDARD TERMS Services provided by Exygen and conditions stated herein, formal contract. AND CONDITIONS Research are limited to the terms unless otherwise agreed to in a MINIMUM F&S-The doilars (S!Oa). minimum fee fct commercial servtces is one hundred SAMPLE COLLECTlON/SUBMfSS/ON-Cilen! shall be re<ponstble fat pr-ol,er collection, preservntron packm, 17 and paclthgir~g, and sh!pnlrnt of the sample(s) in accordance with applicable law dnd goocl comnit'rcial practtce Title and ri,k of loss wtth r~`.`spuct to submitted samples shall al J/I t~rvs remain with cltent prior tL) acceptance by dn Exv~:*I salnple cusx~di,ln Exygen WI/I inttiate 11chatn-of-custody upon sample tecetpt unlev the client Includes one wt!h the sample(<) IQ rrq~~e~t, Exygen will provtcje chain.of.custody forms for cltet:t's use AI! samples sttbmttted must be accompanied by, purchclse utder, or st;ned quots~ion; sample descriptton. iticludin g sample type, source, time and d;tte of collection. specific analyses requesked; estit:lated concentration levels. tequested report Me current btll~tt~ address: and other rrltw,<nt Itlformatton Upon request. Exygen WI/I provide xrd ship apptopri.tte satnple wtttriwt~ to clients. l'hese containers wtll Include the appropriate preservative tf particular analyses requtre one. It IS the tesponsibtltty ot the citent to hnnd:c these preserved contatners safely. ancl using Lull approprialt safety precauttons Clients requesting overnight delivery ot sample containers will be InvoIced for freight. Euygen reserves the rtght to charge `1 fee for sample contattlers SAMPLE rcporttttg DISPOSAL-Exygen retatns s<~mples for one month dftcr results. then disposes of or returns lhc sclmple. Unle,r the client -. "---_ -- --.. 000019 Proven Results. Summary of PFOA, PFHS, PFOS and FOSA in@ Samples Sample ID BC2 SED-04 BC2 SED-04' BC2-SED-05 BC2 SED-05' BCP-SED-06 BC2-SEDGG' Outfall to River SED-25 Outfall to River &D-25' Outfall to River SED-25 Dup Analyte Found C8 Acid PFOA Perfluorooctanolc Acid 4.31 3.06 7.39 6.34 23.6 22.5 16.9 12.0 26.2 (nglg, dry weight) C6 Sulfonate PFHS Petfluorohexanesulfonate 0.809 0.591 2.09 2.51 4.08 4.33 5.05 3.57 7.39 Sample ID BC2 SED-04 BC2 SED-OC BC2 SED-05 BC2 SED-05' BCP-SED-06 BC2-SED-06 Outfall to River SED-25 Outfall to River SED-25' Outfall to River SED-25 Dup Anaiyte Found C8 Sulfonate PFOS Perfluorooctanasulfonate 20.9 17.0 32.8 36.0 1460 1640 169 .,114 208 (rig/g, dry weight) FOSA Perfluorooctanesulfonylamlde 10.2 11.2 11.3 17.4 118 138 44.3 37.2 52.9 ND=Not Detected=Response N&Not Quantifiable=Response `Laboratory Duplicate between 0 and 0.2 rig/g behveen 0.2 rig/g and LOQ (0.4 q/g) 000020 State College, PA 16801, USA F: 814.231.1580 eqgen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. _-_._. -I__ _ . . ._-. ..L - SECTION B 000022 !!qgtxL Precise Research. Proven Reds. Recovery Summary lor PFOA, PFHS, PFOS and FOSA In Water Slmpl* DalErlplian Amount Spiked CBAcldPFOA AmtFound AlllCUllI InSempla Recovsnd Rocowr BCZ SW-04 Lab sprrs 5 4.21 9.14 79 5 0.696 BC2 SW-04 LOW spike Bc2 SW-04 HlQh Splk. Pa02 SW-05 Lab Sp4lia 002 SW-05 Low spIti* 0.1 4.21 10 4.21 5 0.591 0.1 0.591 2.76 -1450' 0.1 0.896 9.92 57 10 o.as6 4.96 87 5 0.165 2.17 1579' 0.1 0.155 EC2SW-05H1~Spikn 10 0.591 7.21 66 10 0.155 SCZSWQGLabSpika. 5 12.1 17.6 114 5 6.06 BC2SW-CSLwS~ke 0.1 12.1 13.9 1600 0.1 6.06 BC2SW.OSHiph Spike 10 121 24.2 121 10 6.06 OuUslltoRlverSW-25LebSpl~ OulfPlltoRivWSW-25LaS@k~ 5 15.8 22.1 126 6 7.66 0.1 15.8 15.0 .a00 0.1 7.66 Duusl(loRwr SW-25"i9kS@ks 10 15.8 26.2 lo4 10 7.66 fleldCalbdlTravelBlankLwSpks 0.1 NO 0.114 114 0.1 NO Field Cmlrob'l'ravsl Blank Hi,,h Spike 10 ND 11.9 11s 10 ND 6.52 92 0.647 -249 9.73 aa 5.00 97 0.607 452 9.58 94 11.6 115 7.11 1050 17.4 113 12.2 91 6.64 -1020' la.1 104 0.119 119 10.8 108 ca SUIfMe1C PFOS haunt AmI Found Amount 5plbd InSampt@ Rscowmd Recovr~ Ut~Punl Spiked AmtFaund lnt%mpto FOSA Atnoun Resowred Recover Bc2sw41LabspJlP 5 11.5 q C2SW-OILowS~ke 0.1 11.5 BC2Sw.o4HIghSol!u 10 11.5 BC2SW05LabSplk~ 5 1.67 EC2SW05LowSpke BC2SW.O5Hi@tSpik~ 0.1 1.67 10 1.67 BC2SW06LabSplke 25 26.1 6C2SW-C6LwSp~ka 0.1 26.1 6C2Sw-C6MphSpika 10 26.1 oUfta"loFfiww SW.25 LnbSplks 50 31.2 ouaant0RivwSW.25LowSpikE 0.1 31.2 OuUdl IO Rlvar SW-25 Hiph Splks 10 31.2 FMd Canlr~rav~ Blank La* SPtks 0.1 ND Nkl ConfrWTrw.1 B(mk High Spike 10 NO 17.1 112 5 1.39 6.69 -4610 0.1 1.39 17.7 62 10 1.39 5.94 ' 65 5 0.146 5.37 3703' 0.1 0.146 12.8 111 10 0.146 49.8 95 6 2.43 32.1 6mO' 0.1 2.43 43.9 178 10 2.43 80.9 9?3 5 3.26 29.4 .iaoo- 0.1 3.26 41.2 100 10 3.26 0.109 109 0.1 ND 11.4 114 10 ND 5.58 a4 0.672 -718. 7.18 sa 4.66 94 0.496 35.2 4.14 40 7.18 95 2.55 120' a.44 60 7.97 94 2.66 -600' 9.02 58 0.0895 SC 11.9 119 3058 Research Drive Cokge, PA 16801, USA F: 814272.1019 exygen.com pQq$x!"CH ,Precise Research. `, Proven Results. Recovery Summary for PFOA, PFHS, PFOS and FOSA in Soil CB Acid PFOA CB Sulfonate PFHS BC2 SED-04 Lab Spike 40 3.02 41.5 96 40 0.566 42.2 104 EC2 SED-05 Lab Spike 40 5.13 43.7 96 40 1.46 44.2 107 EC2 SED-06 Lab Spike 40 14.2 49.4 88 40 2.46 44.5 105 Outfall to River SED25 Lab Spike 40 10.7 47.1 91 40 3.19 44.5 103 CB Sulfonate PFOS FOSA I EC2 SED-04 Lab Spike BC2 SED-05 Lab Spike 40 14.6 40 2T.8 BC2 SW-06 Lab Spike 800 880 Outfall to River SW-25 Lab Spike 40 107 51.8 93 I 40 7.15 61.0 95 40 7.86 1720 105 800 71.4 153 114 40 28.0 Results reported on an as-received basis 46.5 98 48.1 101 650 72 59.0 77 000024 State College, PA 16801, USA T: 800.2813219 F: 814.272.1019 exygen.com SJ-CTION C 000025 Required ""mz;"' Clint Infonllatim: fcks s. Section E I ddq, CHAIN-OF-CUSTODY / Analytical Request The Chain-of-Custody IS 6 LEGAL DOCUMENT: All relevant fields must k completed Document eccurirtely. B Page: / of 52, Ctiint lnlormation (Check t3ecWrlad Due oate: quotelcontract): `TAT: 715679 To Be Completed by PaoeAnatytttd and Uient Section C aala Refefencs: Pmjmzl Manager: Iiiil r-----.IA-~Z-I-. Q-9-.' I -I I ,Ir;l;C.;N; V ,u I I Sample IDS MUST BE UNIQUE AIT e I I I WLE CONDITION SAMPLE NOTES _ - l- - l- - r - e </, - bi-t-'.., `. :+:. - T 5 aI.,7. L 7 7L L - - .-;:f I' ; G..- - - - - - - - - - - - - - - -.%--.,.`-. 1 `> -. - yJi "- 7 ,' & Y .-,I ,.s I: : L `.L L -. " : ,`,..' `5: q 712112003 lof3 3M ENVIROl'lMENT~ LAJ3QRATORY `J Pretimhry/Unautl~o~ Report Project: E03-0561 Requester: Schnobrich. Dana M (223-lN-08) Department: 5307 11 Project Number: 0022674449 Date Received: 6/26/2003 Project Description: Decatur Bakers Creek Comments: #2 Surface Water and Sediment proiect Results/Activity Pace Field Samphng Event Completion Date: project Lead: Jess S. Eldridge Phone Number 65 l-778-5233 Email Address: jseldridge@mmm.com Yna Kc IJbe -- dJ tit> @I\ w ~u-1~ ~7 fag pr,+ p&y* e-- -f--Q psoisf - .- mdistjw> 3M Sample Numiw * SampledDate E03-0561-49786 l/22/2003 EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49787 hpalvtical Method PFOS by ESMS PFHS FOSA PFOA 7/22'2003 EXY `ZEN %f EXYGEN EXYGEN PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49788 7/u/2003 i$dl EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49789 PFOS by ESMS PFHS FOSA PFOA 7l22/2003 EXY GEN EXYGEN EXYGEN EXYGEN E03-0561~49790 ~oalvtlcd Method PFOS by ESMS PFHS FOSA PFOA 7i2z2003 LAB EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49791 ~nrlvtical Method PFOS by ESMS PFHS FOSA PFOA 7l22L2003 L&i w EXYGEN j4nrlvtlclll w PFOS by ESMS EXY GEN PFHS EXYGEN FOSA sample De3criptlon BC2 SW-04 ComDoaents PFOS PFHS FOSA PFOA BC2 SW-04 DUP PFOS PFHS FOSA PFOA BC2 SE&O4 Qmoonenb PFOS PFHS FOSA PFOA BC2 SW-05 PFOS PFHS FOSA PFOA BC2 SW-OS DUP ComDonenta PFOS PFHS FOSA PFOA BC2 SED-05 ComDonenta PFOS PFHS FOSA B!d 9uelifie~ RL Oullilicr BL Oullincc u00028 3M IDMRONMENTAL LABORATORY Preliminary/LJnauthoriwdReport Project: E03-0561 (ant.) 3M SampleNumber 303-056349791 (cont.) sampled Date 71'22/2003 Sample Description BCZ SED-05 AkAB EXY GEN &&yticr1 w PFOA E03-0561-49792 PPOA BC2 SW-06 La& EXY GEN EXY GEN EXYGEN EXYGEN E03-0561-49793 Aaalvtical Method PFOS by ESMS PFHS FOSA PFOA 7izz2003 Comlloaeats PFOS PFHS FOSA PFOA BC2 SW-06 DUP EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49794 ,hrlvticrl Method PFOS by ESMS PFHS FOSA PPOA 7im2003 PFOS PFHS FOSA PFOA BC2 SED-06 EXY GEN ~nalvtical Method PFOS by ESMS EXYGEN EXYGEN - EXYGEN PFHS FOSA PFOA E03-0561-49795 7Lzzr.m3 PFOS PFHS FOSA PFOA Outfall to River SW-25 EXYGEN EXY GEN EXYGEN EXYGEN E03-0561-49796 l4AE EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49797 hpdlvtical lk@&fj PFOS by ESMS PFHS FOSA PFOA 7moo3 &@tical Me&&d PFOS by ESMS BFHS FOSA PFOA 7i2mw3 ComPonents PFOS PFHS FOSA PFOA Outfall to River SW-25 DUP PFOS PFHS FOSA PFOA Outfall To River SED-25 EXYGEN EXY GEN EXYGEN EXY GEN E03-0561-49813 PFOS by ESMS PFHS FOSA PFOA 7LnROQ3 $hmoom .- PFOS PFHS FOSA PFOA Outfall to River SED-25 DUP EXYGEN EXYGEN w EXYGEN EXYGEN &slvtlcal MetboQ PFOS by ESMS PFHS FOSA PFOA Crm PFOS PFHS FOSA PFOA BuvLt 2 of3 4i!d Qualifier: I&! OIllliricr EL Qualifier Iad Qualifier 4% ad Oualllicr k!i Qunllfler 000029 3M ENWROlVMENTAL PrenmblaryNnautbor LABORATORY Report Projea: EO3-0561 (cont.) 3M Sample Number E03-0561-59479 Sampled Date sample Descriptioo Field ControYrravel Blank EXYGEN EXYGEN EXY GEN EXY GEN E03-0561-59480 PFOS by ESMS PFHS FOSA PFOA C,msoocnrr PFOS PFHS FOSA PFOA Equipment Blank - Pump EXY GEN EXYGEN EXY GEN EXYGEN E03-0561-59481 PFOS by ESMS PFHS FOSA PFOA Q&&J&g& PFOS PFHS FOSA PFOA Equipment Blank - Dredge LAB EXY GEN EXYGEN EXYGEN EXYGEN cal M&t@ PFOS by ESMS PFHS FOSA PFOA -oonenQ PFOS PFHS FOSA PFOA 000030 W' Laboratory Sample Log-in Sheet (Environmental) Comcrlete upon ample receipt: Client andror Project Name Method ot Delivery 0 Walk-in Tracking r: a Pick-up YY/nv~ JM Gm*nk 0 UPS zrfi L/' j' d FedEx. `. r:, Cl AlrBome . 0 Other (explain) Chain of CUStOdy Temperature Preservation Custody Seals: intact / 0 broken [explain) ~~~~~ter'>72%F Cooler ID: Coder ID: 5 Cool& ID: Coolertemp: 1. 7 *C Cooler temp: -*c Cooler temp: -"C Cooler temp: - OC Chain of Custody &resent cl absent Record: I sBmpw~i~~e,t 0 with ice pack U none Completed hy Complete durfn LIMS Log-in # Physical Condition Chain of cusbdy Analysis Request Preservation / / l Signature: Samples intacf? Samples received agree with COC record7 AAlysis request clear7 Sample containers appropriate? Chemical preservation appropriate? Samples received within holding time? Sample volume/mass adequate? Explanation Completed by Signature: Complete tollou 9 resolution of any nonconformances: Slient Zoritacted Cl Yes client: lesolution Date flme): I / L/ 2f c 7 /c d 0 No (explaii) -06 .O No (explain) 0 No (explain) a Yes 0 Yes Cl Yes 0 Yes Cl No (explain) 0 No (explain) Cl No (explain) 0 No (explain) / / I Date (Time): Completed by Signature: Date: Lab Sx Log-in Sheet -Ex : . " " .:. `. : .: .. 1,: `. .: : _" :. :. . . .:_`. . : ,,' .' 1: `. .I: : `. : . . " : ., `. : -: ,' : `., ... . : : .: : . `. LOGIN Account: CHAIN OF CUSTODY REPORT (ln01) Jul 28 2003, 07:54 am Login Number: L34910 2046 3M ENVIRONMENTAL LABORATORY L34910-1' ,.. BC2 Sy-.04 SAMPLES KEPT IN D0000539. :.: ', .; .-21*JUL:O3 25-J-U&-03 L34910.-2 .: BC2 L~i4:910-3 " BC2 L34910-4 L3-49.10 -5 SOIL BC2 EC2 SEE+04, s PERC SOLID :.: `: :~.:.:23-~~:~3: 25+JIjL-.~3~ H;.ld~:$l-AUG-03 do000539 ,: :; L.349lo-6 BC2 SyT- 05 : ,: : ,.,.`..`.' $&tJyL-:Oi3 1 25+&ijy.o3:;,; .' :., Lg4910 -7 BC2 SW:-.05 LOW S?K:.~::(,~:,,:~.,PP.B);!2l;:JUL:O:3. ,25,-JUL-O3 L34910-8 BC2 SW-05 HIGH SPK (10 'P?:~.~:.:,;21-J~~.-0~3: 25+IUL-O3. .. ., L34910-9 '4 BCZ SW-85.DUP .. : 21-~~L:-.0.3 ,25.;+.:JqLf8~:.,:: ;. ., '. L34910-10 BC2 SEDtOS .2l-JUL:f-j3 25-~U~+.83,; " SOIL S PERC SOLID Hold:til-AUG-03 do000539 L3.4910-11 SOIL BC2 SED.-06. S PERC SOLID '. 23-JUL,.-03.: ~s-JuL-.o~:.. Holdhl-AUG-03 do000539 L3.4910.-12 BC2 SIT",0 6 ., '1 ,:: :, .&y;,+J~.~Q:3:: `25.4JTJ&.fQ3 .:.:..\: ; "5 .; :,, &3-4910-n BC2 SW.-.06 LOW SPK;:fO ;.'i:.;.I?,Pa:f.,~2'3::;iSUL.~03:.2~-1;7U~.-03 L34910-14 BC2 SW::O,6 HIGH: SP'K'. (10 ::PPB:):.j23 -JUL:-Q:3-. .25-:J'UL-.o3; L34910-15 B.C2 SW-..06 DUP ,'-. :23---JU&yO3 ,25'JuL-03, L34910-16 OUTFALL,,T.Q:..RIVER :SW~2.5...2,3~,~L-03 .2,5-.JUI,.+3, .,:: L34910-l-7 /' OUTFALL :TO RIVER. SW-.25 23:.;:JUL-03 2.5~JULto'3 COMPLETE ID READS OUTFALL TO RIVER SW-25 LOW SPK (0.1 PPB). L34910-18 OUTFALL'TO. RIVER SW-25 23.2.:JUL-03 .'. COMPLETE ID READS OUTFALL Td RIVER SW-25 HIGH SPK (10 L34910-19 OUTFALL TQ RIVER-:.SWk25 D~.P;23tJULyQ.3 25.+UL-O3 : : Page 1 LOGIN Account: CHAIN OF CUSTODY REPORT (h01) Jul 28 2003, 07:54 am Login Number: L34910 2046 3M ENVIRONMENTAL LABORATORY L34910-20 SOIL OUTFALL TO RIVER S.ED'2'5' 23-JUL.+03 25.2JUL-03 : S PERC SOLID Hold:Ol-AUG-03 d0000539 :L34910-21 SOIL OUTFALLTO S PERC SOLID RIVER SED-25 :D:uF 23,-JUL-03 Hold:Ol-AUG-03 do000539 2.5.-WL-03 L349fO-22 F'IELD CONTROL/TRAVEL BLANK, 23-JUL-03: 25i",JUL;-O3 '.. ,:.::' L34910-23 FIELD ,CCNTROL/TRAVEL.. BLANK LOW- 23 -JUL.-'03 .2.5.-;3UL-03 COMPLETE ID'READS FIELD CONTROL/TRAVEL BLANK LOW SPIKE (Oil PPB). L34910-24 FIELD CONTROL/TRAVEL.BL,ANR 23-:JUL-03 25.-JUL,-03 ,. COMPLETE ID READS FIELD CONTROL/TRAVEL BLANK HIGH SPIKE (10 PPB). L34910-25 EQUIPMENT BLANK-PUMP :Zl-JUL-03. .2S-JUL:-03:.,: L34910-26 EQUIPMENT BLANK-.DREDGE 23';'JUL-;03 25.-J&-03. Page 2 Signature: Date: _I fr, ;. ,.J& :1).:.. : '. ,,: ', 000034 SECTION D 000035 IhI3058 Research Drive n State College, PA 16801 RESEARCH Phone: 814-272-1039 Fax: 814-231-1580 Date: 08/26/03 Exygen Study # L34910 NOTE TO FILE NOTE: Throughout the raw data generated for study L34910 the 498 > 78 monitored transition (perfluorooctanesulfonylamide) was assigned the acronym PFOSA instead of FOSA. Any reference to PFOSA in the raw data is equivalent to FOSA. Initials: $ Od2blfl3 000036 SpmwxSnuly No: Exygcn Siuiy No: .balyl.e: Ions Manitolul: Site: NA I34910 PFOA 413 -> 369 Daanu B&r', Creek RAW DATA REPORT Limit of Quaotiutim: lnjatiw Volume: M&X: Sampls Vdumc: Pinal Volume: JO PPC 1Jrr. W-1 40.0 mL 5.0 mL Set No: AdYSli Luinrmcnc Extlaction AdYzcd Type: oak cm 073103A IbmRiti LGUSMS 07fxm O&m-02/03 Unit Y 6 xco72503-0 xCO72503-1 XCO72JO3-2 xco72Jo3-3 xCu72sa3-4 xco72Jo3-5 XcO72503-6 McduMl Wash 0106020 Cwual 01 Cd020 Spk A 010602OSpkB W4910.1 Spk C L34910-6 Spk D U4910-12 L34910-16Spk xco72Jo3-I Spk E F u49 IO. 1 w4910.1 Rsp I349104 U4910-2 L34910-3 xCTl72503-2 U4910-6 L34910-6 Rep w49m9 w4910.7 L34910-8 xCo72Jo3-3 L3491Mt L34910.12 Rep U491O.H U49m.13 U4910-14 xCO72so3-4 U4910-16 W4910-16Rcp L34910-I9 U4910-17 U4910.18 xcomo3-s U4910.25 L34910.26 U491422 w49 IO-23 U4910-24 XCO71003.6 . .-., -_I BC2 SW04 BCZ SW-05 BC2 SW-06 outfall tcl River SW-25 Bc2 SW-04 BC2 SWM BCZ SW-04 Dup BC2 SW-04 Low Spk BC2 SW+i Hi,& Spk BCZ SW-OS BQ SW-OS BC2 SW-Q5 Dup BC2 SW-OS Low Spk BQ SW-05 Hip,! Spk BCZ SW-06 BQ SW-M Bc.2 SW-06 Dup BC2SW~LowSpk BQ SW-06 High Spk chaau lo uher SW-2s outfall la River SW-25 outfall u) Rivet SW-U Dup Outfdl LO River SW-U Low Spk Outiall 10 RivaSW-2J High Spk equipmult Blmk-pump Equipmm Bhnk-Dmlgc Pi&i GxmoUthvcl Blank Field Control/hvcl Bhk Low Spk Picld CwrmKl'mel Blank High Spk c-s on 103A-1001 cs 073103A-lm cs 073103A-1003 cs 073103A.I@34 c-5 073103A-LWS cs 073103A.1006 cs 073lO3A.1007 low C 073103A.1008 C 073103A-lW9 LCS 073103A.1010 LCS 073103A-101 I LP 073103A.1012 LP 073IO3A-1013 LF Otiti3A.1014 LP 073103A-1015 cs 073103A-1016 2s s 073103A-1017 S 073103A.1018 S 073103A-1019 PF 073103A-1020 FF 073103A-1021 cs 073103A-1022 SO S 073103A.IO23 5 073103A.lU24 S 073103A.1025 IT 073103A.lM6 IT 073103A-1027 cs 073103A-1028 100 S 073103A.1029 S 073103A-1030 S 073103A.1031 ff 073103A. 1032 PP 073103A-1033 cs 073103A.1034 2.50 s Of3103A.103s S 073103A.1036 S 073103A-1037 m 073lO3A.1038 ff 073103A.1039 cs 073103A-I040 Jw S 073103A-1041 S 073103A.1042 s 073103A.1043 PF 073103A.1044 PF 073103A.1045 cs 073103A-1046 1ooa Analytc RaovcIy Found (Ppo (%) - i (peak arca - intempt) [mlyte found I slop x Dp (p&It).arwlyls alxwunt hmd added in cwaol (ppt) (ppt)] 1 ml CS I C&bmdw rmdud c = conml rampls s - Slmplc CX.CbcckSmdd ND = Nor detecti NQ -Not qwmifmble P Rerpantc I Rupocua lJ' D Lb fmilicd FF I Fild fatiticd LCS m Wontory "mph rampk Cmi~ol Spike bcrwecn 0 and 2S pp, betwcta 25 pp' and LOQ (JO ppl) `Sample l Sampk wu cwrsetcd usinS the data foucd in w(O73103AR. quirw furbcr dilution. See data w073103AR J50 8614 16102 29438 66169 142891 264459 267 659 14411 132909 239247 145872 418651 515606 693 1 849301 826648 575640 605630 29529 13780 173871 181075 3JJlY'J 521363 21J% 317J8 2411389 2425189 2J27002 2849870 71294 75537 3012978 3276529 275829) 3102823 77205 156964 652 940 808 34004 35258 322068 NO 47.6 JO 95 452 500 w 8140 SW0 79L 4ha JWO a7 * m . Jow I . . * 100 99247 1ww J7" SYl 616 l * 100 7210 lcml 66 . * . . 100 24200 loow 121" l * . I IO0 26200 weal 104A ND ND ND I14 loo 114 11900 mooa 119 slnndprd Imrcopt Slope cocf. Of DeL : Lbmr (Ilx - 44J.OJ7 i 293.343 3 0.986042 weighmd) SprewJshcec prepared by: 000037 SjmvxStudy No: Bxyrcn Study Na: kldytc: IOIU Monitored: Site: NA I34910 PFHS 399 -> x0 Dccaiur B.&&s Creek R4 W DATA REPORT Llmll of Qupntitatlon lnjcction Value: Mti sampk Volum: Fl Vdum: JopP( 15 rr. Ww 40.0 mL 5.0 ml. &NIX AdYlC hlkumml Bxinctiw Adyrcd Type: fhk w: 0731rnA lcanmfurhn LUMS/MSUail#d 07x3 1x13 OaAlIrn ID CC& NO. (PPI) Facta Area x0372503-0 Gs 0731rnA.UYJI 0 a xc072503-I cs 073 103A. 1002 25 1401 XCO72503-2 cs 073103A-Iw3 SO 2842 xco72503-3 cs 073103.4-1004 100 5604 xCO72503-4 cs 073103A.lws 250 13137 XCO72503-5 xCm2so3-6 cs 0731mA-1006 500 26976 cs 073103A-1w7 lca 51345 Methanol wash C 073103A-1w8 0 Olca7.a conlral OlOW2OSpk A C u73lrnA-1009 LCS 07310x-1010 1 0 I 2759 OlWO20 Spk B LCS 073103&101 I 1 26598 W4910-I SpkC BCZ SW.O4 LF 073103A.1012 10 30859 I349104 Spk D BCZ SW-05 LP 0731mA-1013 10 27946 U4910-12SpkE BC2 SW06 LP U73103A.1014 LO 55454 l.3491~16 Spk F cutfall 10 River SW-23 LF 073103A-1015 10 60284 xwwo3-I cs 0731rnA-1016 25 1444 U491Q1 Bc2 SW.04 s 0731rnA-1017 1 50162 w4910.1 Rep BC2 SW.04 S 073103A-1018 1 49342 L349104 EC2 SW-M Dup S 073103A-1019 I 31968 L349102 BC2 SW-04 Low Spk FF 073103A-IOU) I 36223 u4910-3 BC2 SW-04 Hi@Spk w 073103A-1021 100 5426 xcx72.503-2 cs 0731mA-lU22 So 2420 W4910-6 Be2 swos S 073lMA-ICC3 I a666 U4910.6 Rep BC2 SW-05 S 073103A-1024 I 150s w4910-9 BCZ SW-05 Dup S 073103A- 1025 I 21096 L349m7 BCZ SW-OS Law Spk FP 073103A-1026 1 33965 L34910-8 BCZ SW.05 Hiph Spk FF 073103A.1027 LCQ 5342 xCo72503-3 cs 073103A.1028 100 5959 L3491&12 BC2 SW&i S 0731rnA.1019 I 2.59042 U4910.12 Rep BCl SW-W s 073103kIWO 1 237649 w4910.15 Bcmwwoup S 073lrnA-1031 I 245687 l.34910.13 BC2 SW-06 Low Spk FF 073103A.1032 I 275858 L34910-14 BCZ SW-06 Hi@t Spk FF 073103A-1033 100 YIN xCO72503-4 CS 0731rnA-1034 250 14198 W4910.16 f.34910.16 Rep w4910.19 w4910-17 talddl IO ltivcr SW-25 S oulfall to River SW-25 s o.ldalIlORiverSW-2I5hp S outfzll11R0ivarSW.2L3owSpk IT 073 103A- LO35 073tm.4-Im6 0731rnA.1037 073imA4-1038 1 283517 1 302530 I 276429 I 7J8698 l.34910.18 &fail lo River SW.25 High Spk FF 073103A.1039 100 10133 xco72503-5 w4910.25 Eqtipmcat Blank.i'ump CS 0731mA-IWO s 0731mA.1041 SW 29038 1 0 U4910.26 Wiwm~ Blank-hdgc S 073IMA-1042 1 0 W491Q22 Field Caatrdfhvcl Blank S 073lrnA.1043 1 0 U4910.23 Field C~nvOlfTnvcl Blank Law Spk FF 073103A.3044 I 664a L34910.24 Field C~nUol/hve.l Blank Hi@ Spk FF OnlrnA-lo45 loo 6002 XCO71003.6 cs 073103A.1046 Iwo 60941 Amlyre Found (ppt) RccaYay (%I = - (peak area - intercept) (amlytc found I rlapc x OF (Ppt)-allalyw. found 10 EODWI UmlJnl .adcd (pp) (tJFt)I 1. 100 CS = Calibnwm xacniwd c = CMtrOl sample s - SYnple CK-CiwkSund&d LF ILabhtlficdurrpk FF - Weld fmifkd sampk La = Iiabamtciy CMud spike fpPl) - No 49.7 99 475 95 5520 54m 92 sm 5cKJo 97 . sow . scol 896 a82 571 647 100 -249+ 9730 Iwoo 88 155 IS2 377 607 100 452 9580 tm 94 . . . l 100 17400 low0 113* l . . l 100 18100 lotm 104~ f-40 ND No 119 loo 119 10800 loo00 108 B : Linw (I/r tnlaccqi - -23.56k4l Slope 3 55.9970 Cd. of De!. - 0.98w93 weighted) Vhqlc l Sampk Maqk was corralal using dm data found in set 073103AR. mquim futhcr dilution. See dua St 073 103A.R. residue signiricnntly cxceedr the spiking kvel; tbxcfcix. an YEUIILS rccovcry cannot bc czdculud, 000038 Spmvw Stiy No: Baypen SMy No: Andytc: lnnr MrJnilmd: Site: NA w4910 PFOS 499->vv Dccanu Bakm'r Crick RAW DATA REPORT Limil of Qantilatiw: Injection Mti: Volwnc Sample volume: Fmal Volunr: soppc IJ NWater 40.0 mL 5.0 mL SOI No: AlUIYSC lluullmull Bauactiw my?.cd Type: Dam an: 073103A KMnRisha ms/Ms O7AIrn3 o8mLo2m3 Unil Y 6 @YW m XCa77503-O XC0725OE I xco72.nl3.2 xcO72.ul3-3 xco7?.m3-4 xco72so3-J XCUf2503-6 MedIano wash 01~20Conual 0106020 spk A 0106O20 W491O-1 Spk B Spk C W4910-6 Spk D l34910-12 Spk E L34910-16 Spk F xco72303-I L3491aI w4910-1 Rep w491w 134910.2 L3491O.3 XCO72503-2 L34910.6 u4910-6 Rep u491O.9 L3491O.7 L34910.8 xCO72.m3-3 u4910-12 w4910.12 Rep L349m1s u4910-13 w491O-14 xCO72503-4 L3#10-16 uA9LO16 Rep L3491019 w491O-17 l349lO-18 XCO725is5 U4910.23 L3491&26 w4910-22 W49lOa 134910.24 XCO71Do3-6 spaoaor m - BC2 SW-O4 BC2 SWJJ5 BC2 SW06 ouddl to River swa _ l BC2 SW.04 BC2 SW-O4 EC2 SW44 lxp BC2 SWU4 Law Spk BCZ SW-O4 Hi& Spk EC2 SW45 BC2 SW-05 BC2 SWOS tip BC2 SWOS Low Spk BC2 SW-O5 H~@I Spk BC2 SW-O6 Bc2 SW55 BC2 SW06 Dup BC2 SW-06 Low Spk BC2 SW06 Hi#t Spk oulfdl In RIvlwsw.2s cuddl Lo RIVW SW-25 Gutfau to Rivcrsw-25 OAfall IO River SW-2S IhIp IAW Spk Chffdl to RIverSW-ZS Hi@ Spk Equipnm Blank-Pump Eqtipmnl Bhuk-lhdy Fidd ControUhvel Blank Field CoUraUhvel Blank Low Spk Field Conudthvd Blauk High Spk sam$de CCdC CS cs cs cs cs cs cs C C l.cs L&s iF ,tF LP LF CS S S S m FF cs S S S FF FlJ cs S S S IT IT cs S s s FF FF cs S S S IT FF cs Rue No. O73103A-1001 073103.4-1002 O73103A.LOO3 O731MA-IMY 073lmA.n3.5 073103A-1006 073103A-I@37 O73lMA-IOOS 073103A-1009 O73103A-1010 073103A-101 I 073103A.1012 O73lMA.1013 073103A.1014 O73103A-lOIS O73103A.1016 O73103A-1017 O73103A-1018 073103A.1019 O73103A.1020 073103A.1021 O73103A-1022 073103A-1023 013103A-1024 0731O3A-1025 073103A.1026 O73103A.1027 O73103A-IO28 073103A-1029 073lrnA-1030 O73103A.1031 073103A.1032 O73103A-IO33 O731O3A.1034 073103A.103s 073103A.1036 073103A. 1037 073103A.1038 073103A.1039 073103A-1040 073103A-1041 073103A-1012 073103A-lO43 O73103A.IO44 073103A-IO44 073 103A-1046 Std. COIIC. (Ppl) 0 23 Jo 100 2.50 SW l(Mo Dludon Factor 1 1' 1 10 IO 10 10 as 1 1 I 1 100 so 1 I I I IW loo 1 I 1 I loo 250 I I I 1 100 SW 1 t 1 I loo IWO Peak AM 0 971 I%3 M40 7.518 17228 32298 :o: -0 1673 ISIS?? SO011 202% 96754 120697 954 280183 274170 21172S 191631 6016 1656 44922 46036 112926 149088 4333 3500 558236 571211 56OllS 667186 14981 8S2I 691166 707270 6S6533 68w9 14072 19341 316 0 0 3691 38S3 3se.l Andyte. Fnund (PPO Amwnt Added @PO - : -3.. -. .-. - . I - ;.. ND so.4 445 1 SV40 * * . . l . 17700 . . . . 12800 . . I . 43900 . . * . 41200 ND ND ND 109 11400 Rcwvcly (%) -...- . . 101 09 115" 62" IllA 17e.u IW +mpIc **SampIe l Sunpla VP) mmcred ws curccted acquirer flUhI usinK rhc data found in set 073 103AR. U&IS lhe dam found in YI 08O6O3k dilution. See data sat 073 103AR. 000039 Sponsor Study No: Exygcn Study No: `4tidyCC: Ions Monitored: Site: NA L34910 FOSA 498 -> 78 Decatur Bakct's Creek RAW DATA REPORT Limit of Quntiution: Injection Vohtmc: Matrix: SatlQle Valunlc: Final Volume: 50 PPt ISllL W?.tcr 40.0 mL 5.0 mL Set No: Analyst: Insuument Type: Extraction Da&: Analyzed on: 073 103A Karen Riiha LUMSiMS Unit # 6 07/3 1103 08/01-02/03 EXYl3.= ID xco72503-0 xco72sa3-1 XCO72503-2 xco72503-3 XC0725034 XCO72503-5 XCO72SO3-6 Metbrnol Wash 0 106020 Control 0106020 SpkA 0106020SpkB L34910-I SpkC L34910-6 SpkD L34910-12 Spk E L34910-16 Spk F XCO72503.1 L349 10-I L34910-1 Rep L349 IO-4 L349 1o-2 L349 I o-3 XCO72503-2 w4910-6 L349 IO-6 Rep L349 1o-9 L.34910.7 W4910-8 X0372503-3 L349 IO- 12 L34910.12 Rep L34910-15 L34910.I3 L34910-I4 xcor2503-4 L34910-16 L34910-16 Rep L34910-19 L34910-17 L34910-18 XCO72503-5 u4910-25 L34910.26 L34910-22 L349 lo-23 L34910-24 xc071003-5 Sponsor ID BC2 SW-04 EC2 SW-05 BCZ SW-06 Outfall to River SW-25 BCZ SW-04 BC2 SW-04 BQ SW-04 Dup BQ SW-04 Low Spk BQ SW-04 High Spk BC2 SW-05 BC2 SW-OS BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk Bc2 SW-06 EC2 SW-06 BC2 SW-C-5Dup BC2 SW.06 Low Spk BC2 SW-06 High Spk Dutfall to River SW-25 Outfall to River SW-25 Cutfkll to Rive?SW-25 Dup Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk Equipment Blank-Pump Equipment Blmk-Dmdge Field CantrolTnvcl Blmk Field Conuo~ravel Blank Low Spk Field ControI~Trrvcl Blank High Spk smpk Code cs cs cs cs cs cs cs C C LCS LCS LF LF LF LF cs S S S FF FP cs S S S PF FF CS S S S FF FF cs S S S FF FF cs S S S FF FF cs Run NO 073103A.1001 073103A-1002 073103A-1003 073103A.1004 073103A-ICG5 073103A-1006 073103A-1007 073103A-1008 073103A-1009 073103A-1010 073103A-1011 073103A-I012 073103A-1013 073103A-1014 073103A-lOIS 073103A-1016 073103A-1017 073103A-1018 073103A-1019 073103A-1020 073103A-1021 073103A-1022 073 lO3A-1023 073103A.1024 073 l03A.I025 073103A.1026 073103A-1027 073103A-1028 073103A-1029 073103A.1030 073103A-1031 073103A-1032 073103A-1033 073103A.1034 073103A-1035 073103A-1016 073103A-1037 073103A.1038 073103A-1039 073103A.1040 073103A.1041 073103A.1042 073103A.lC43 073103A.1044 073103A.IO45 073103A.1046 An&`@ Found (ppt) - (peak uca - intercept) I slope x DF Recovery (%) - ~vralyte found (ppt).aoalyte found in cm~uol @pt)] x 100 rmouat added @pt) Std. COW. (ppt) 0 25 50 100 250 500 ICC0 DihtiOll Factor 1 1 1 10 IO 10 10 25 I 1 I I 100 50 I I 1 1 IO0 IO0 I 1 1 1 100 250 1 1 1 1 100 500 1 I I I lo0 loo0 Peak Arca 0 3440 6725 13321 3 1340 65687 127765 0 0 6872 62898 74954 65330 96.556 107094 3545 148109 143575 106161 90364 9716 6634 19717 20175 52363 6703 I 5639 13989 269067 2634 11 276134 284082 11410 33866 358032 358tt72 369645 311246 12191 72430 0 814 0 I2140 16047 139302 Anriylc Found (ppt) Attwunt Added (ppt) RCCOVCIY w ND 50.6 468 5580 4860 7180 7970 * l 790 672 7180 146 I50 389 498 4140 . l L * 8440 l I . . 9020 ND ND ND 89.8 II900 50 IO1 St30 94 5OwJ 84A 5ooo 94 5ooa 95" sow 94^ loo IOOCQ -71x"+ 58^ IO0 3.51 IOOCQ 40 100 10000 60" 100 loo00 5aA loo 90 Iwo0 119 &!a&&&& : Linear (I/x weighted) 1nurccpt = 78.1882 Slope = 134.313 Coet Of Dct = 0.995963 CS = Calibration stand& LF = Lab fortified sample C = Conrrol ramplc FF - Field fortified sample S = Sample LCS = I.&omtory cowJo spike CK = Cheek Stllrdard ND - Not detected - Rcsponx between 0 and 25 ppt NQ - Not quDntiflablc - Rcspawc bchveen 25 ppt sod LOQ (50 ppt) Spreadsheet prcpucd by: ^Sampk was conected using tbc data found in ICI 073103AR *Sample requires tuther dilution. Seedata set 073103AR. +Sampk residue rigniticurtly cxccc& the spiking level; therefore, ao KCW~~Crecowy cannot be calculned. 000040 Protocol Number: n nEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLETRANSFERSHEET NA Exygen Study Number: L34910 Exygen Sample # 1 Sponsor Sample # I BC2 SED-06 BC2 SW-06 BC2 SW-06 Low Spk Karen Risha 7/3 l/O3 0800 Requested By (Printed Nan&Date/Time) Samples removed from: Samples removed from: &#$-%7 - Box# --W Box+! - Shelf# - Shelf# - Samples transferred to the custody of Samples received from custodian; Samples moved to f%F 3% L4 7-Y&3 a9ca7 Sample Custodian Initials/Date/Time Laboratory It,3 ocloo Personnel InitiaWDattlTime Comments: r/d73 Sample Custodian 0% 3g Inkials/Date/Time December 19,2002/6 000041 E. n BI EAI<CH 3058 Research Drive State College, PA 16801 Internal Chain of Custody/Fortification Bxygen Study Number: L34910 Sponsor Study/protocol No: NA The samples listed below were removed from refrigerator No Tie fltl I I Sheet Matrix: EXYGEN ID NUMBER VOLUME (mL) na 0106020 Control 40.0 na 0106020 Splc A 40.0 na 0106020 Spk B 40.0 BC2 SW-04 L34910-1 Spk C 40.0 BC2 SW-OS L34910-6 Spk D 40.0 BC2 SW-06 L34910-12 Spk E 40.0 OutfaIl to River SW-25 L34910-16 Spk F 40.0 BC2 SW-04 L34910-1 40.0 BC2 SW-C4 L34910-1 Rep 40.0 BC2 SW-04 Dup L349 1o-4 40.0 SC2 SW-04 Low Spk L34910-2 40.0 BC2 SW-04 High Spk L34910-3 40.0 BC2 SW-OS L34910-6 40.0 BC2 SW-05 L34910-6 Rep 40.0 BC2 SW-05 Dup L34910-9 40.0 BC2 SW-05 Low Spk L34910-7 40.0 BC2 SW-05 High Spk L349 10-g 40.0 BC2 SW-06 L34910-12 40.0 BC2 SW-06 L34910-12 Rep 40.0 BC2 SW-06 Dup L34910-15 40.0 BC2 SW-06 Low Spk L34910-13 40.0 BC2 SW-06 High Spk L34910-14 40.0 Phone: 8 14-272-1039 Fax: 814-231-1580 m Initials &Z FORTIFICATION (ng) 2.0 20.0 200.0 200.0 200.0 200.0 L34910-12 Spk E L349 lo-16 Spk F F&50203-2 (loo0 ng/rnL) FO60203-2 (1ooQ ng/mL) All samples were mtaaured: Time lOW Date ?&/0?i After measuring samples were returned to refrigerat r No. 32 Time l/m Date J-?/3/ 0.3 c0nUIIeIIt.S: Analysis 200 pL of 250 mg/mL sodium thiosulfale was ad&d to all wnpla Summary: Data Set: Data Set: Data Set: b731 ah Set extraction/analysis data verified by: `Initials /!.!. Initials m before spiking. InitialslDatc: u - July 26,2001/6 000042 nR( 3058 Research Drive EARCH State College, PA 16801 Phone: 814-272-1039 l3x: 814-231-1580 EXYGEN STUDY SAMPLE NUMBER: m MATIUX: &gg EXTRACTION AND ANALYSIS TRACKING SHEET METHOD: " ANALYTES: PFHS, PFOS. @OA and PFOSq PROTOCOL NUMBER: u Client ID I Exygen ID STEP 1 STEP 2 Dilutions (muml.) STEP Dilutions STEP 3 (mualL) 4 I F Reagents/ Materials Mclhaml Cl8 SPE Lot % 43lKpJyB W5PGi3?J L3491@16 Spk L34910-I BC2 SW-05 Dup L34910-9 BC2 SW-OS Low Spk L34910-7 BC2 SW-05 High Spk L34910-8 BC2 SW-06 L34910-12 I BC2 SW-06 L34910-12 Rep BC2SW-06Dup L34910-15 I BC2 SW-06 Low Spk L34910-13 BC2 SW-06 High Spk L34910-14 *lnitialr/Dorr I STEP 1: SPE columo clean-up (omitting 40% wash) I 1 I STEP 2: Final vohme IO 5 mL collected in I5 mL polypropolene tubes STEP 3: LC/?&lMS analysis STEP 4: LC/MS/MS reanatysis. I 0 . I/ I I I I I 1 I ,l; I w O*`/I, 0 O-`/r.0 O151.0 1 I I \1/ 1 1 ;w_ AmmoniumAccl.ate e, I c;4 NA i!lsw=m lq3ua.q tswd &bin& ra*F?w twJm.LWcL~eAhF=Ico. tp&b3 *Initials and dale under each stp indicates the personnel that performed this step. $I Mebd of Analysis for the Dmmination of P~~~wo~ctaoc sulfonatc (PFOS). Perfluorooctanc sulfonylamide (PFOSA), and Pcfluorooctanoate (PoAA) in Water coh4hENTs: u Final extracts stored in refrigerator& Initials: E Date: o?l??,/& July 19,2001/4 n m EARCH 3058 Research Drive State College. PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 - Internal Chain of Custody/Fortification Sheet Exygcn Study Number: L34910 Matrix: m Sponsor Study/Protocol No: k.iA The samples listed below were removed from refrigerator No. Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk Field ControVTraveI Blank Field ControbTravel Blank Low Spk Field ControVI'ravel Blank High Spk Equipment Blank-Pump Equipment Blank-Dredge I I L34910-17 L34910-18 L349 1o-22 I349IO-23 L34910-24 L34910-25 L34910-26 40.0 40.0 40.0 40.0 40.0 I 40.0 I 40.0 I ! ! I Spiking Solution Used 1 Volume Used for Spiking I InitiaYDate I I I I All samples were measured: Time 1020 Date After measuring samples were returned to refrigerator No. ~32 Time /Ia Date Q@t,$!)3 Initials f= Initials f'lEE C0mnWIt.S: 200 pL of 250 mghL sodium ti~iorutfatcwasadded to all rvnpta bcfar~spiking. InilirldDate: Analysis Summary: DataSet: 6731%4 ' Data Set: b73lb3S Set extraction/analysis data verified by: _- _.,-. l-"._l.l---- .-.__. .".-_.- ,-_- - -- .._~. - c E nM EARCH 3058 Research Drive State College. PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 EXYGEN STUDY SAMPLE NUMBER: m MATRIX: &&I EXTRACTION AND ANALYSIS TRACKING SHEET METHOD: ff ANALYTES: J'FHS. PFOS. PFOA and PFOS4 PROTOCOL NUMBER: Nl Equipment Blank-Dredge *Initials and date under each step indicates the personnel that performed t&s step. $$ Method of Analysis for the Determination of Pwfhwwctane sulfonate (PFOS), Perfluorooctane sulfonylarnidc (PFOSA), and Peffluorowtaooate (POAA) in Water Final extracts stored io refiigcrator~ Initials: E Date: July 19. 200114 -. Masslynx - .- Sample List Sample List: C:WIASSLYNX\Fluoroch Printed: Fri Aug 01 O&36:23 2003 ___ - -_-. -I- -~-__---.----___ 103A Decatur BCSPL -@o%?m fiUDY NO. Page 1 Page Position: (I. 1) Vial File Name 41 073103A.1001 42 073103A-1002 43 073103A-1003 44 073103A-1004 45 073103A-1095 46 073103&1006 47 073103A-1007 92 073203A-1008 51 073103A-1009 52 073103A-iOl0 53 073103A-1011 54 073103A-1012 55 073103A-1013 56 073103A-1014 57 073103A-1015 42 073103A-1016 58 073103A-1017 59 073103A-1018 60 073103A-1019 61 073103h1020 62 073103A-1021 43 073103A-1022 63 073103A-1023 64 073103A-i024 65 073103A-1025 66 073103A-1026 67 073103A-1027 44 073103A-1026 68 073103A-1029 69 `073103A-1030 70 073103A-1031 71 073103A-1032 073103A-1033 073103A-1034 73 073103A-1035 74 073103A-1036 75 0731 03A-1037 76 073103A-1038 77 073103A-1039 46 073103A-1040 78 073103A-1041 io" 073103A-1042 073103A-1043 81 073103A-1044 LIMS ID Client ID Sample Description --- --- -- - -- - --- - -- --- -- -- -- --- -- --- - -- -- --- -- - -- --- -- _- -- __- -- --- -- --- -- -_- -- --_ - -- -- -7 - -- - -__ - -- -- --_ - -- - -_- -- I- - -- -- --- -- --- - -__ - - - --- - --- -- --- -- -- - -__ - -__ -- --_ - --- - -- -- --- - -- --- -_ XCO72503-0,O nglL Standard XCO72503-`i I ngR Standard XCO72503-2,50 ngR Standard XCO72503-3. 100 r@L Standard XCO72503-4,250 rig/L Standard XCO72503-5, 509 rig/L Standard XCO72503-6.1000 nglL Standard Methanol Wash 0106020 Control 0106020 Spk A, 50 rig/L 0106020 Spk B, 500 rig/L L34910-1 Spk C. 5000 rig/L, DF=lO L34910-6 Spk D, 5000 mJL, DF=lO L34910-12 Spk E, 5000 rig/L, DF=lO L34910-16 Spk F, 5000 rig/L, DF=lO XCO72503-1, 25 nglL Standard L34910-1 L34910-1 Rep L34910-4 L3491 O-2 L34910-3. DF-100 XCO725O?b2. 50 nglL Standard L34910-6 L34910-6 Rep L34910-9 L34910-7 L34910-8, DF=lOO XCO72503-3. 100 ng& Standard L34910-12 L34910-12 Rep L34910-15 L34910-13 L34910-14, DF=lOO XCO72503-4,250 rig/L Standard L34910-16 L34910-16 Rep L34910-19 L34910-17 L34910-18, DF=lOO XCO72503-5,500 rig/L Standard L34910-25 L349 lo-26 L34910-22 L349 lo-23 Matrix -----_ ---_-- ------- --- -- _- --- --- -- -_- -- ___ -- -- ___ - -- --_ - -- -- -_- -- ___ -__ -__- r__-- Samplefype Standard Standard Standard Standard Standard Standard Standard Blank Blank :: EE QC QC Standard Analyte Analyte Analyte :: Standard Analyte Analyte Analyte :cc Standard Analyte Analyte Analyte :: Standard Analyte Analyte Anatyte :: Standard Analyte Analyte Analyte QC Cone (rig/L) 85 50 100 250 500 1000 ---- 100 ZEO 5000 5000 5000 25 ---_ -- 100 10000 50 _----- 100 10000 100 ___ -_--100 10000 250 ----- 100 loo00 500 ---100 Cone B Cone C Test ID DF -- ___ 0 ___ --- 0 -- --_ _- -__ x -_- --- 0 e- ___ - ___ 8 -- -- -- -__ x --- --_ 00 : - --- -- --e 0 IO - -- 0 10 --- 0 IO -- 10 -- --_ 8 1 - -- 0 1 _- --- 0 - --- 0 1 _- -- 0 1 - -- 0 100 -_ - 0 1 - -- 0 1 --- - 1 -- - : 1 _- - 0 1 - -_ 0 100 -- -_ 1 --- -- i - -- 1 -_- --_ : 1 - _- 0 -- -- 0 100 -- 0 1 - -- 0 1 - --_ 1 --_ 0" 1 -- -- 0 -_ 0 100 - ___ 0 1 1 --- 0 - ___ 0 - --_ 0 - --- 0 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroc Printed: Fri Aug 01 O&36:23 2003 MS Method 1 C6 CB SULF 2 C6 CB SULF 3 C.6 CB SULF 4 C6 CB SULF 5 C6 CB SULF 6 C6 Cf3 SULF 7 C6 CB SULF 8 C6 CB SULF 9 C6 CB SULF 10 C6 CB SULF C6 CB SULF :: C6 CB SULF 13 C6 CB SULF 14 C6 CB SULF C6 CB SULF :t C6 CB SULF C6 CB SULF :i C6 C8 SULF 19 C6 CB SULF C8 CEi SULF t: C6 CB SULF 2'5 C6 CB SULF C6 C8 SULF 24 C6 CB SULF 25 C6 CB SULF C6 C8 SULF :; C6 C8 SULF 28 C6 C8 SULF C6 CB SULF C6 C8 SULF 31 C6 CB SULF 32 C6 CB SULF C6 CB SULF C6 Ci3 SULF C6 CB SULF C6 C8 SULF C6 C8 SULF C6 C8 SULF C6 CB SULF C6 CB SULF C6 C8 SULF C6 CB SULF C6 C8 SULF C6 CB SULF C8 ACID C8 ACID CB ACID C8 ACID CB ACID C8 ACID C8 ACID CB ACID C8 ACID CB ACID C8 ACID C8 ACID CB ACID CB ACID CB ACID CB ACID C8 ACID CB ACID CB ACiD CB AClD CB ACID CB ACID CB ACID C8 ACID CB ACID CB ACID CB ACID CB ACID CE ACID C8 ACID C8 ACID CB ACID C8 ACID CB ACID C8 ACID C8 ACID CB ACID CB ACID CB ACID CB ACID CB AC10 CB ACID C8 ACID CB ACID PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA PFOSA HPLC Method pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water ppfbms swwaatteerr pfbs water pfbs water pms water pfbs water pms water pmswater ppmmsswwaatteerr ppfbms swwaatteerr ppfbms swwaatteerr ppfbms swwaatteerr ppfbms swwaatteerr ppfbms swwaatteerr pmswater pmswater pfbs water pmswater pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pf4s water pfbs water ppfbms swwaatteerr MS Tune File Fluorochems Fluarochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems f luorochems Fluorochems Fluomchems Fluorochems Fluorochams Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Inj.Volume 15 15 :z 15 15 15 15 15 2 15 15 15 15 15 15 E iii :: :55 :z 15 15 15 15 2 :z 15 15 15 15 15 E 15 15 -&Y@Ql STUDY NO. @-.-fib - - Page 2 Page Position: (2, 1) Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroc hinted: Fri Aug 01 O&36:23 2003 mlcals.PRO\SampleD8\073~03A Decatur EJCSPL .-en STUDY NO. .&b!%!?. Page 3 Page Position: (1, 2) Vial File Name 45 82 073103A-1045 46 47 073103A-1046 LIMS ID Client ID Sample Description -- -- -- - 134910-24,OF=loa XCO72503-6. 1000 ngli Standard Matrix --- Sample Type QC Standard Cone (ngll) 10000 1000 Cone I3 Cone C Test ID DF -- -- 0 100 - -- 0 1 000049 LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Qygen Studv No: L349 10 Instrument: Micromass Quattro Ultima (LCMSIMS Unit #6) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven ._ HPLC c01urnn: Genesis C-8,5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by.* lcif%plb3 000050 `brrl Scanning Method Report Method: Last Modified: C:/MAS~LYNX\FLUOROCK~?X~CALS.PRO\ACQUDB\C~ Thu Jul 31 16:23:50 2003 Page 1 CS SULF C8 ACID PFOSA Printed: Fri Aug 01 08:36:30 2003 u Solvent Delay ( mins ) : 0.00 Analog Function Channel : 1 4 : Unused MlW of 4 Mass Pairs ( ES?- ) Inter Channel Delay ( Sets ) : 0.03 Span ( Daltons ) : 0.00 Start Time ( Mins ) : 0.00 End Time ( Mins ) : 12.00 Repeats : 1 Channel Parent Daughter Dwell (Sets) 1 399.00 80.00 0.20 2 413.00 369.00 0.20 3 498.00 78.00 0.20 4 499.00 99.00 0.20 Co11 Energy 35 10 30 40 (eV 1 Cone 50 10 50 30 (v 1 Ix--_ __II._^__^___- 00005~ __."-. .__..__-,-,__"--.,-_..-...--.-..-. - Method Report Method File: Last Modified: 14 Printed: c:\masalynx\fluorochemicale.pro\acqudb\pfbe Friday, August 01, 2003 08:27:00 Friday, August 01, 2003 08:36:39 HP1100 LC Pump Initial Conditions Solvents A% 90.0 B% 10.0 C% 0.0 D% 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(aC) 0.300 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time A% B% C% D% 0.00 90.0 10.0 0.0 0.0 2.00 90.0 10.0 0.0 0.0 5.00 10.0 90.0 0.0 0.0 9.00 10.0 90.0 0.0 0.0 9.50 0.0 100.0 0.0 0.0 14.00 0.0 100.0 0.0 0.0 14.50 90.0 10.0 0.0 0.0 20.00 90.0 10.0 0.0 0.0 $4 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contact1 Off On Off Off Off Off Contact2 Off Off Off On Off Off 'Contact3 Off Off Off Off On 'Off Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300 Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(pl) Vial Number 200.0 200 0.50 20.00 * 15.0 69 water Page 1 Pressure 400 400 400 400 400 400 400 400 000052 ~4 Tuning Method Report Method: C:\MASSL~\!?LUOROC~MICALS.PRO\ACQUDB\FLUOROCHEMS Printed: Fri Aug 01 08:37:00 2003 u ' Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set R&k 3.00 -2.93 20 -21 0.0 0.0 0.0 100 100 300 299 Rdbk OFF 3.4e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set 14.0 14.0 1.0 -2 15 2 14 .o 14.0 2.0 650 Rdbk 131.4 754.2 Rdbk 12 14 16 -648 000053 --- -- ------em -- Quantify Calibration %& Study No. :L34910, Report Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Calibration: Last modified: Printed: -- --- P:\Data\L~~S6\MaPqlynx\Fluoroch~cals.PRO\~~eDB\O73103A Sun Aug 03 07:12:46 2003 Sun Aug 03 07:19:26 2003 ---- -- :ompound 1 name: C8 Acid (PFOA) Coefficient of Determination: 0.986042 >alibration curve: 293.343 l x + 445.057 Response type: External Std, Area :urve type: Linear, Origin: Exclude, Weighting: 3.22e5 l/x, Axis trans: None --Page 1 Decatur BC X X Response 0.0 Rxygen Research, 200.0 I r I ,, I 1 I ,, . 400.0 600.0 I ,I I 1 )I r I $, I I IT ,ng/l 800.0 1000.0 3058 Research Drive, State College, PA 16801 000054 ----- ---------- _---------- ------mm- Quantify Calibration Report \J Study No.:L34910, Set No.: 073103A, Eact.Date:07/31/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\L~SBIS6\~sslynx\Fluoroch~cals.PRO\~~eDB\O73lO3A Sun Aug 03 07:12:46 2003 Sun Aug 03 07:19:26 2003 Compound 2 name: C6 Sulfonate (PFHS) Coefficient of Determination: 0.989093 lalibration curve: 55.9970 * x + -23.5660 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 6.09e4 1 l/x, Axis trans: None -- Page 2 Decatur BC . X E%y!Jen Research, 3058 Research Drive, State College, PA 16601 Quantify Calibration Report td Study No.:L34910, Set No .:073103A, Ext.Date:O7/31/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMflrlS6\Masslynx\Fluorochemicals.PRO\~~eDR\O73103A Sun Aug 03 07:12:46 2003 Sun Aug 03 07:19:26 2003 ;ompound 3 name: C8 Sulfonate (PFOS) ioefficient of Determination: 0.992844 ialibration curve: 34.2805 ' x + 56.2500 tesponse type: External Std, Area :urve type: Linear, Origin: Exclude, Weighting: 3.57e4 l/x, Axis Vans: None Page 3 Decatur BC Response 0.0 Oxygen Research, 200.0 400.0 600.0 3058 Research Drive, State College, EA 16801 800.0 1000.0 000056 Quantify Calibration Report w Study No .:L34910, Set No.: 0731031, Ext.Date:O7/31/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\~~eDB\O73103A Sun Aug 03 07:12:46 2003 Sun Aug 03 07:19:26 2003 Compound 4 name: PFOSA Coefficient of Determination: 0.995963 :alibration cuwe: 134.313 l x + 78.1882 Response type: External Std, Area :urve type: Linear, Origin: Exclude, Weighting: 1.39e5 l/x, Axis trans: None Page 4 Decatur BC X Response Exygen Research, 3058 Research Drive, State College, PA 16801 ---- ----- ___l----- -----__---_ Quantify Sample Report Lif Study No. :L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LC3HSMS6\Masslynx\Pluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ------- Sun Aug 03 07:19:29 ___----------- 2003 ________-------l_-l____________I____ Name : 073103A-1001 Text: 1: C8 Acid (PFOA) XCO72503-0,O rig/L Standard 073103A-1001 Sm (Mn, 2x3) 01 -Aug-2003 09:24:14 LC/MS/MS #6 MRM of 4 Channels ES- 413> 369 1.22e4 9.14 Area 550 $4& 2: c6 Sulfonate (PFHS) XCO72503-0,O rig/L Standard 073103A-100l'Sm (Mn, 2x3) , 3: C8 Sulfonate (PFO.5) XCO72503-0,O rig/L Standard 073103A-1001 lOO- Sm (Mn, 2x3) Ol-Aug-2003 09:24:1 I, w MRM of 4 Channels ES- 01 -Aug-2003 09:24:11 LC/MS/MS #it il MRM of 4 Channels ES- (J .,.,,,,.,,,,,,,,,,,,,~,,,,.~,,,,,,,,,,,,,,~,,.~,,,,,,~,~.,,~Tjme W- 2.00 4.00 6.00 8.00 10.00 Wgen Research, 3056 Research Drive, State College, PA 16601 12.00 000058 Quantify Sample Report \d Study No.:L34910, set NO .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 2 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LWSMS6\Wllsslynx\Fluorochemicals.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCWSMS6\Wasslynx\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ---------------A----_------- -----p B---e-- Name : 073103A-3001 Text: 4: PFOSA XCO72503-0, 0 rig/L Standard 073103A-1001 Sm (Mn, 2x3) 09:24:14 LC/MS/MS #6 RM of 4 Channels ES- 2.00 4.00 6.00 8.00 10.00 12.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 000059 Quantify Sample Report Y& Study No.:L34910, Set No.: 073103A, Ext,Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LO1I~S6\Wlsslynx\Bluoroch~cals.~RO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochsmicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 3 Decatur BC BC 080103 Name: 073103A-3002 Text : L: C8 Acid (PFOA) KC072503-I,25 rig/L Standard 073103A-1002 10 Sm (Mn, 2x3) % j 9.16 8614 I . . 01 -Aug-2003 09:45:57 LC/MS/MS #6 MRM of 4 Channels ES413> 369 5.36e4 Area I, Time 2.00 2: C6 Sulfonate KC072503-1,25 (PFHS) rig/L Standard 073103A-1002 Sm (Mn, 2x3) 10 8.99 1401 %- om.-. `I ' " a, ", , r " `I x s ' , 7 8 ' I " " ,"`I 2.00 4.00 6.00 8.00 Ol-Aug-2003 09:45:5 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 8.90e3 Area Y^-------------I 10.00 I Time 12.00 3: C8 Sulfonate XCO72503-1,25 (PFOS) rig/L Standard 073103A-1002 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 09:45:57 LC/MS/MS #6 MRM of 4 Channels ES- 9.26- 499 > 99 971 6.30e3 Area 0 ,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,r,,,~,~~~~,~~~~,~~~~,~~~~1Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000060 Quantify Sample Report WI& Study No.:L34910, Set No.: 073103A, Ext,Date:O7/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluoroch~ca~s.PRO\SamgleDB\073l03A Sun Aug 03 07:08:13 2003 P:\Data\L~sMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 4 Decatur BC BC 080103 Printed: -------------_------ Sun Aug 03 07:19:29 2003 _I_-____----------- --------------_ Name: Text: 073103A-1002 4: PFOSA XCO72503-1,25 rig/L Standard 073103A-1002 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 0934535; LC/MS/MS #E MRM of 4 Channels ES- 9.88- 498 > 7E 3440 1.94e4 Area 0 "",,`","","","","","","","","' , , , , , , ,-,Time 2.00 4.00 6.00 8.00 10.00 12.00 when Research, 3058 Research Drive, State College, PA 16801 000061 Quantify Sample Report qJI Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:X.Risha SarPple List: Last modified: Method: Last modified: Job code: P:\Data\LCMSMS6\~eslynx\Fluoroch~cal~.PRO\S~~eDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\FluorochemicalaB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 5 Decatur BC BC 080103 Name: 073103A-1003 Text : 1: C8 Acid (PFOA) XCO72503-2, 50 rig/L Standard 073103A-1003 loo- Sm (Mn, 2x3) %- 01 -Aug-2003 10:07:44 LC/MSNS #6 MRM of 4 Channels ES- 9.15 413> 369 9.76e4 Area : C6 Sulfonate :CO72503-2,50 (PFHS) rig/L Standard ,73103A-1003 Sm (Mn, 2x3) 8.9s ) 284: z 01 -Aug-2003 10:07:44 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.82e4 Area 2.00 4.00 I S 8.00 - 10.00 Time 1 12.00 I: C8 Sulfonate (PFOS) cCO72503-2,50 q/L Standard 01 -Aug-2003 10:07:44 LC/MS/MS #6 373103A-1003 10 %!3 Sm (Mn, 2x3) MRM of 4 Channels ES9.2E 196: Area lir_;;., 4919T.1im7>ee499 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000062 ----I_------______--------- ---- -- Quantify SalrQle Report 'IW Study No .:L34910, Set No.:O731031, Ea&.Date:07/31/03, Analyst:K..Risha Page 6 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Bluoroch~ca~s.P~\S~~eDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\FluorochamicalsB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 -----_ -we-___ ------we---__ --_^_--- Name: 073103A-1003 Text : 4: PFOSA XCO72503-2, 50 rig/L Standard 073103A-1003 100- Sm (Mn, 2x3) %- 01 -Aug-2003 10:07:44 LC/MS/MS #t MRM of 4 Channels ES- 9.89- 498 > 7~ $725 3.6aef AreE Oxygen Research, 3058 Research Drive, State College, PA 16801 000063 Qlmeify Sample Report 'W Study No.: L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 7 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~SMS6\Masslynx\Fluorochemica~s.~RO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMmS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: --- Sun Aug 03 07:19:29 ~------ 2003 -~---_ -I___- ----- Name: 0731031-3004 Text : : C8 Acid (PFOA) *.' :': b:-.-. . (CO72503-3,100 rig/L Staijd'ard - )73103A-1004 10 Sm (Mrt, 2x3) 9.15 29438 01 -Aug-2003 10:29:31) LC/MS/MS #6 MRM of 4 Channels ES413>369 1.81e5 Area 2: C6 Sulfonate XCO72503-3,100 (PFHS) rig/L Standard 073103A-1004 10 Sm (Mn, 2x3) Time 12.00 _ 01 -Aug-2003 10:29:31 LC/MS/MS #6 MRM of 4 Channels ES- 9.01 399 > 80 5604 3.44e4 Area - 3: C8 Sulfonate XCO72503-3,100 (PFOS) rig/L Standard 073103A-1004 lOO- Sm (Mn, 2x3) %- 9.26 3040T 0%Aug-2003 10:29:31 LC/MS/MS #6 MAM of 4 Channels ES499 > 99 1.92e4 Area 0 I , , 1 , TT-& , I I 1 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000064 Quantify Sample Report V Study No.:L34910, Set No. :073103A, Rxt.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~~6\Masslynx\Fluoroch~cal~.PRO\S~~eDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCIMSMS6\Masslynx\Fluorocheacicals.PRO\Met~R\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 8 Decatur BC RC 080103 NallW: 073103A-1004 Text : 4: PFOSA XCO72503-3,100 rig/L Standard, 073103A-1004 100- Sm (Mn, 2x3) %- 01 -Aug-2003 10:29:3' LC/MS/MS #t MRM of 4 Channels ES- 9.89 498 > 71 7.20er Are: 0 ~"`["","","","","`,~,,,`,,,`,,,`,,,,,,, Time 2.00 4.00 6.00 8.00 10.00 12.00 J RxYgen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report I,& Study No.:L34910, Set No.: 073103A, E&.Date:O7/31/03, Analyst:K.Risha Page 9 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluoroch~cal~.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:X3 2003 P:\Data\L~fl3S6\nsslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ---- ----___-___-----------------__-_l__l_______ Name : 0'?3303A-3005 Text : 1: C8 Acid (PFOA) YCO72503-4,250 rig/L Standard )73103A-1005 Sm (Mn, 2x3) . + 9.15 66169 01 -Aug-2003 lo:51 :16 LCYMSIMS #6 MRM of 4 Channels ES413>369 4.06e5 Area 2.00 4.00 6.00 8.00 10.00 12.00 1: C6 Sulfonate XCO72503-4,250 (PFHS) rig/L Standard 073103A-1005 10 Sm (Mn, 2x3) 8.99 13137 Ol-Aug-2003 10:51:1i/ LC/MS/MS #6 MRM of 4 Channels ES399 > 80 8.1 Oe4 Area pm Time / 2.00 4.00 6.00 8.00 10.00 12.00 1 3: c8 Sulfonate XCO72503-4,250 (PFOS) rig/L Standard 073103A-1005 Sm (Mn, 2x3) Ol-Aug-2003 10:51:16 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.43e4 -;roioo. Tim/e 6.00 8.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16301 Quantify Saw18 Report &,& Study No.:L34910, Set No.: 0731031, Rxt.Dats:07/31/03, A.nalyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQ1ISMS6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LQISMS6\Maoslyax\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 10 Decatur BC SC 080103 Name: 073103A-1005 Text : 4: PFOSA XCO72503-4,250 rig/L Standard 073103A-1005 lob Sm (Mn, 2x3) %- Ol-Aug-2003 10:51:16 LC/MS/MS #6 MRM 9.90 313403 .. .- of 4 Channels ES498 > 78 1.69e5 Area 0 "","",l"`,"","","","l',"","","' , , , I, ,Time 2.00 4.00 6.00 a.00 10.00 12.00 ExyOen Research, 3058 Research Drive, State Collage, PA 16801 000067 ----m-------v _------- Quantify SaqG3 Report 94 Study No.:L34910, Set No .:073103A, Ekt.Date:O7/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~~S6\~sslynx\Fluorochamfcale.PRO\SampleDB\O731O3A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\Masslynx\FluorochemicaR\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 -----_ Page 11 Decatur BC EC 080103 Name : 07310331~1006 Text : 1: CB Acid (PFOA) XCO72503-5,500 rig/L Standard 073103A-1006 100- Sm (Mn, 2x3) %- 0%Aug-2003 11:12:56 LCYMWMS #6 MRM of 4 Channels ES413>369 8.51e5 Area 0 ",,I;;","","","","","",",`,"" I , , I 1 ( I / , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 Fr3' 2: C6 Sulfonate XCO72503-5,500 (PFHS) rig/L Standard 073103A-1006 100-J Sm (Mn, 2x3) %- 01 -Aug-2003 11 :12:58 LC/MS/MS #6 8.99 269767 MRM of 4 Channels ES399 > 80 1.64e5 Area - 0 "","","",",.,,,.`,"","","","",`,","",",., Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate XCO72503-5,500 (PFO.5) &L Standard 073103A-1006 10 Sm (Mn, 2x3) % Ol-Aug-2003 11:12:561 LCYMWMS #6 MRM of 4 Channels ES499 > 99 1.03e5 Area 1 ExYCJea Research, 3058 Research Drive, State College, PA 16801 000068 Quantify Sample Report w Study No.rL34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\FluorochbmicalS.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCM~S6\bsslynx\FluorocbemiB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 12 Decatur BC BC 080103 Name: 073103A-1006 Text : : PFOSA KO72503-5,500 rig/L Standard 01 -Aug-2003 11:12:56 LWMWMS #6 173103A-1006 Sm (Mn, 2x3) MRM of 4 Channels ES- IO 7 i 9.90 65685 r %3O'~~","`~,~~~~,~~~~,`~~~,~~~~,~~~',,~~~,~~~~,~~~ i-- 2.00 4.00 6.00 8.00 10.00 498 > ,78 3.53e5 Area Time 12.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 060069 Quantify Sanqple Report stuay No.: L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modifiec: Method: Last modified: Job Code: P:\Data\L~S6\Msslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\~SMS6\Masslynx\Fluorochamicals.PRO\~et~B\D~catur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 13 Decatur BC BC 080103 Name: Text: 0731031-1007 1: C8 Acid (PFOA) )I:CO72503-6, 1000 rig/L Standard C)73103A-1007 10 Sm (Mn, 2x3) 9.13 264455 I 01 -Aug-2003 11:34:&j LC/MS/MS #6 MRM of 4 Channels ES413> 369 1.57e6 Area 2: C6 Sulfonate XCO72503-6,lOOO (PFHS) rig/L Standard 073103A-1007 Sm (Mn, 2x3) A-- Time 12.00 8.97 51345' 01 -Aug-2003 11:34:44 LCNSIMS #6 MRM of 4 Channels ES399 > 80 3.1485 Area 2.00 4.00 6.00 8.00 10100 12100 1 3: C8 Sulfonate XCO72503-6,1000 (PFOS) rig/L Standard 073103A-1007 lOO- Sm (Mn, 2x3) %- 9.25 _ 32298 01 -Aug-2003 11:34:42 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.87e5 Area 0 "","","","","","","","","", , , , , , , , , , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000070 s---m- ---w-- ------ ----w---Y- Quantify S-10 Report v Study No.:L34910, Set No.: 073103& Ext.Date:07/31/03, Analyst:K.Riaha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\bsslynx\Fluoroch~cals.P~O\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\Masslyax\Fluorochemicals.PRO\MathDB\Decatur Sun Aug 03 07:13:59 2003 Printed: Sun Aug 03 07:19:29 2003 ---- Pags 14 Decatur EC BC 080103 Name: Text: 073103A-1007 4: PFOSA XCO72503-6,lOOO rig/L Standard 073103A-1007 loo- Sm (Mn, 2x3) %- Ol-Aug-2003 11:34:4: LC/MS/MS #E MRM of 4 Channels ES- 9.91 12776Cj7 498 > 7e 6.79e5 Area Oxygen Research, 3058 Research Drive, State College, PA 16801 000071 --- ---- Quantify Sample Report I& Study No.:L34910, Set No .:073103A, --------Ext.Date:07/31/03, -------___ Analyst:K.Rfsha Page 15 Santgle List: Last modified: Method: Last modif isd: Job Code: P:\Data\MIMSraS6\Masal~\Fluoroch~Ca~S.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LQrl~S6\Massl~\Fluorochemica\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 --------------____----__---------- ----------------_- Name: 073103A-1008 Text : 1: C8 Acid (PFOA) Methanol Wash 073103A-1008 IOO- Sm (Mn, 2x3) %- ,. . 01 -Aug-2003 11:56:3C . LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 >. 369 3.92e3 Area 1 0 ,~,~,.,,~,.~,~,~.,,,,,,,,,,~~,~~~~,~~~~,~~~~,~.~~,~,~~,~~~~,Time 2.00 4.00 6.00 8.00 10.00 \ 12.00 I& 2: C6 Sulfonate (PFHS) Methanol Wash 073103A-1008 lOO0.21 Sm (Mn, 2x3) %- 01 -Aug-2003 11:56:3C LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 1.03e3 * 0 "","","","","","","","","'*,",~I~~',I..~~l 2.00 4.00 6.00 Time 8.00 10.00 12.00 3: C8 Sulfonate [Methanol Wash (PFOS) 073103A-1008 Sm (.Mn, 2x3) , . 01 -Aug-2003 11:56:3( LC/MS/MS #E MRM of 4 Channels ES499 > 9s 932 J 0 ,,,,,,,,,,,~,,,,,,,,,,,,,,,,.,,,,,,,~~~,~,,~,,,~,,~~~,,~,,~~Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000072 Quantify Sample Report \d Study No.:L34910, Set No.: 073103A, Eact.Date:07/31/03, Analyst:K.Risha Page 16 Sample List: Last amdified: Method: Last modified: Job Code: P:\Data\L~~S6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~~S6\Massl~\Fluoroch~cals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 -------em -----__ ---- -- --- Name: 073103A-1008 Text : 4: PFOSA Methanol Wash 073103A-1008 Sm (Mn, 2x3) -Aug-2003 11:56:3( LC/MS/MS #E MRM of 4 Channels ES498 > 7E 90: r t Time 12.00 EKygsn Research, 3058 Ressarch Drive, State College, PA 16801 000073 Quantify Sample Report Study No.: L34910, Set No.:073103A, Eact.Date:07/31/03, Analyat:K.Risha Sample Li6t: Last modified: Method: Last modified: Job Code: P:\Data\LCW~S6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\~SMS6\Mnsslyrur\FluorochsmicaB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page i7 Decatur BC BC 080103 Nemo: 073103A-1009 Text : 1: C8 Acid (PFOA) 10106020 Control /073103A-1009 Sm (Mn, 2x3) %- . .* _. -. . . -.- 01 -Aug-2003 12:18:Ofj LCNSIMS #6. MRM of 4 Channels ES413 > 369 1.72e4 Area 9.15 859 0 "",""""`,"","",""I"","",`,,`,,,",,,,,,,,,', Time 2.00 4.00 6.00 8.00 10.00 12.00 2: c6 Sulfonate 0106020 Control (PFHS) 073103A-1009 Sm (Mn, 2x3) 01 -Aug-2003 12:18:08 LC/MS/MS #6 MRM of 4 Channels ESloo42 l l .55 3% > 80 765 0 "","","","","","","","`.I"","","","", Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate 0106020 Control (PFOS) 01 -Aug-2003 12:18:08 I LClMS/MS #6 MRM of 4 Channels ES- 499 > 99 Exygen Research, 3058 Research Drive, State College, PA 16801 000074 --w---m-- Quantify Ssmpls Report &,# Study No.:L34910, Set No .:073103A, Ext.Date:O7/31/03, Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\~sslynx\Bluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\~~S6\Masslynx\FluorochemiB\Decatur Sun Aug 03 07:11:59 2003 Printed: ----- Sun Aug 03 07:19:29 2003 --- ------------ Name: 073103A-1009 Text : -4: PFOSA 0106020 Control 073103A-1009Sm(Mn,2x3) loo- : %- --P--------w tialyst:K.Risha -- Page 18 Decatur SC BC 080103 m---- Ol-Aug-2003 12:18:0t LC/MS/MS #E RMof4ChannelsES498> 7E I I Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Saxqle Report Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\M1WSMS6\~ssl~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Rug 03 07:08:13 2003 P:\Data\M41SMS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07x11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 19 Decatur BC BC 080103 Name: 073103A-1010 Text : I1.: CB Acid (PFOA) 0106020 Spk A, 50 rig/L 073103A-1010 Sm (Mn, 2x3) 01 -Aug-2003 12:39:57 LC/MS/MS #6 MRM of 4 Channels ES413>369 8.95e4 Area 2.00 'u 2: C6 Sulfonate (PFHS) 0106020 Spk A, 50 rig/L 073103A-1010 100- Sm (Mn, 2x3) %- Time 6.00 8.00 10.00 12.00 01 -Aug-2003 12:39:57 LC/MS/MS #6 MRM of 4 Channels ES- 8.99 399 > 80 1.73e4 Area 0 ..,.,.~,,,,,,,,,,,,,,,,.,,.,.,,,,,,,...,, , , , , , I , , , , , , ,Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) 0106020 Spk A, 50 rig/L 073103A-1010 lOO- Sm (Mn, 2x3) %- 01 -A~~-2003 12:39:57 LC/MS/MS #6 MRM of 4 Channels ES- 9.27 499 > 99 1673 1.08e4 Area Or--, 1 rTITime 2.00 4.00 6.00 8.00 10.00 12.00 EKygen Research, 3058 Research Drive, State College, PA 16801 000076 Quantify Sample Report '114 Study No.:L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\bLasslynx\Pluoroch~cals.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\L(SMSWS6\Masslynx\Fruorochamicalr Sun Aug 03 07:11:59 2003 Printed: ---- Sun Aug 03 07:19:29 2003 ------Pm..-------es ---e-s-_ Name: 073103A-1010 Text : 4: PFOSA 0106020 Spk A, 50 rig/L 073103A-1010 Sm (Mn, 2x3) Page 20 Decatur BC BC 080103 -- 01 -Aug-2003 12:39:57 LCIMSIMS #6 MRM of 4 Channels ES498 > 78 3.70e4 Area Time 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000077 ---- ----__-____- -----B--P m--e-- Quantify Sample Report rd Study No .:L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: La;tCFdiified: : P:\Data\LCWSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\Massl~\Fluorochemica\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 21 Decatur BC BC 080103 Printed: ---_---- Sun Aug 03 07:19:29 2003 -----------------a-- _-------__ --- --- Name: 073103A-1013 Text : 1: C8 Acid (PFOA) 0106020 Spk B, 500 rig/L 073103A-1011 lOO- Sm (Mn, 2x3) %- : 9.15 13290g7 01 -Aug-2003 13:01:43 LC/MS/MS #6 MRM of 4 Channels ES413>369 7.82e5 Area O-o*, , , I I I , t , , 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 !: C6 Sulfonate (PFHS) D106020 Spk B, 500 rig/L 073103A-1011 10 Sm (Mn, 2x3) 8.99 26598 Ol-Aug-2003 13:01:43j LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.54e5 Area `-"I"`-`T"" Time 1 2.00 4.00 6.00 8.00 10.00 12.00 : C8 Sulfonate (PFOS) 1106020 Spk B, 500 rig/L )73103A-1011 10 "i % Sm (Mn, 2x3) ^ ^- Y.Z/ 151919 Ol-Aug-2003 13:01:4: LCYMWMS #E MRM of 4 Channels ES499 > 99 8.83e4 Area i L-- Time 2.00 4.00 6.00 8.00 10.00 12.00 men Research, 3058 Research Drive, State College, PA 16801 0000%3 Quantify Sam&a ReDort &f Study No.:L34910, Set No .:073103A, Ext.Dater07/31/03, Analyst:X.Risha Page 22 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~~S6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ----------- ---------- Name: 073103A-1011 Text : 4: PFOSA 0106020 Spk B, 500 rig/L 073103A-1011 100- Sm (Mn, 2x3) %- , 01 -Aug-2003 13:01:43 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 3.29e5 Area ExyOen Research, 3058 Research Drive, State College, PA 16801 Quantify Sanlpls Report Study No.: L34910, Set No.: 073103A, Ext.Datar07/31/03, A.ualyrrt:K.Risha Sampls List: Last modified: Method: Last anodifisd: Job Code: P:\Data\LQIS1IIS6\~ssl~\F~uoroch~cal6.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LOHSMS6\Masslynx\Fluorochsmicr\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 23 Decatur BC BC 080103 Name: 073103A-1012 Text : L: CB Acid (PFOA) L34910-1 Spk C, 5000 rig/L, DF=lO 073103A-1012 lOO- Sm (Mn, 2x3) %- 9.14 2392473 01 -Aug-2003 13:23:31 LC/MS/MS #6 MRM of 4 Channels ES- 413>369 1.38e6 - Area 0 ~,,,~-,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,~,,,~,.,,,..,,,,,,Time 1 2.00 4.00 6.00 w 2: C6 Sulfonate (PFHS) L34910-1 Spk C, 5000 rig/L, DF=lO 073103A-1012 100- Sm (Mn, 2x3) %- 8.00 8.98 _ 30859 10.00 12.00 , 0%Aug-2003 13:23:31 LCfMS/MS #6 MRM of 4 Channels ES399 > 80 1.8485 Area () ,,,,,,,,.,,,,~,,,,,,,,,,,,~~,,.~,,,~.~~,~~~~~~~,~~~~,~.~~,Time 2.00 4.00 6.00 : Ck3 Sulfonate (PFOS) -3491 O-l Spk C, 5000 rig/L, DF=lO 173103A-1012 Sm (Mn, 2x3) 8.00 9.27 5001, 10.00 12.00 01 -Aug-2003 13:23:31 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.91 e5 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 :\i, Exygsn Research, 3058 Research Drive, State College, PA 16801 000080 Quantify Sample Report \rcrf Study NO.:L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Sanlple List: Last modified: Method: Last snodified: Job Code: P:\Data\LCbl~S6\Massl~\Fluoxoch~cals.PXO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masalynx\Fluorochsmicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 24 Decatur EC BC 080103 Name: Text: 073103A-1012 : PFOSA -3491 O-l Spk C, 5000 rig/L, DF=lO )73103A-1012 10 Sm (.Mn, 2x3), % 01 -Aug-2003 13:23:31] ' LC/MS/MS #6 MRM of 4 Channels ES- 9.92 7495r I 498 > 78 4.01e5 Area 4 O',`,,,,,,,,`~,.,,,,,,,.,,,,,,`,.,.,,,,,,,,,.,,,,, L.. Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000081 ---- -----_ ---- Quantify Sampls Report lJ, study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Laat modified: Job Code: P:\Data\M41S)blS6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~sMS6\Masslynx\Fluorochemicacatur Sun Aug 03 07:11:59 2003 Page 25 Decatur BC BC 080103 Printed: -------- Sun Aug 03 07:19:29 Name: 073103A-1013 Text : 2003 ---- I----- -- L: C8 Acid (PFOA) L34910-6 Spk D, 5000 rig/L, DF=lO 073103A-1013 10 Sm (Mn, 2x3) % 1 0%Aug-2003 13:45:17' LCNSIMS #6 MRM of 4 Channels ES413>369 8.79e5 Area Time L 2.00 4.00 6.00 8.00 lo:oo 12:oo ] 14 2: Cfi Sulfonate (PFHS) L34910-6 Spk D, 5000 rig/L, DF=lO 073103A-1013 I tnf-L Sm (Mn, 2x3) 01 -Aug-2003 13:45: 1i LCnbwMS #f MRM of 4 Channels ES- 8.98 399 > 8C 1.64eE Aree 3#: C8 Sulfonate rI-34910-6 Spk (PFOS) D, 5000 rig/L, (>73103A-1013 10 Sm (Mn, 2x3) DF=lO , , I , , . , , , 10.00 , ,--, Time 12.00 9.25 2029t 3-l Ol-Aug-2003 13:45:1? LCltWMS #6 MRM of 4 Channels ES499 > 99 1.21 e5 Area Time w 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000082 ---- P--_------ v-w --- Quantify Sample Report q,,& Study No.:L34910, Set No.: 073103A, Ext.Date:07/31/03, AnalYst:K.Risha Page 26 Sample List: Last modified: Method: Last nmdified: Job Code: P:\Data\L(41SPIS6\Msslynx\Fluoroch~ca~s.PRO\S~leDB\O73lO3A sun Aug 03 07:08:13 2003 P:\Data\LQll~S6\~eolynx\Pluorochsmica\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ------____--- --------p-s I----- Name: 073103A-1033 Text : 4: PFOSA L34910-6 Spk D, 5000 rig/L, DF=lO 073103A-1013 100- Sm (Mn, 2x3) %- 01 -Aug-2003 13:45: Ii LC/MS/MS #E MRM of 4 Channels ES- 9.88 498 > 7E 3.48eE Area 0 "","`~,""I"","","","","","","' , , , , , , , , , , Time L 2.00 4.00 6.00 8.00 10.00 12.00 QJ Oxygen Research, 3058 Research Drive, State College, PA 16801 000083 Quantify Sample Report 1G Study No.rL34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\lvhssl~\Fluorochsmicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~SMSb\Masslynx\FluorochemicalB\Decatur Sun Aug 03 07:11:59 2003 Page 27 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ----- ---- -.-----------I---- ----v-- Name: 0731031-3014 Text : * L34C981 OAc-lid2 S(pPkFOEA,)5000 rig/L, DF=l 0 373103A-1014 Sm (Mn, 2x3) 9.14 i-2 416651 0%Aug-2003 14:07:06 LCNWMS #6 MRM of 4 Channels ES413 2.>493e669 Area L w 2: C6 Sulfonate (PFHS) L34910-12 Spk E, 5000 rig/L, DF=lO 073103A-1014 lO@ Sm (Mn, 2x3) %- 0 "~`,""1"","~`,"~`,~~~),~,,`,~~~,,~~' 2.00 4.00 6.00 I: C8 Sulfonate (PFOS) -34910-12 Spk E, 5000 rig/L, DF=lO 373103A-1014 10 Sm (Mn, 2x3) % 4 10.00 Time 12.00 01 -Aug-2003 14:07:06 LC/MS/MS #6 MRM of 4 Channels ES- 399 > 80 3.30e5 Area - 8.00 9.24 9675r Time 12.00 01 -Aug-2003 14:07:06 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 5.61e5 Area Time Oxygen Research, 3058 Research Drive, State College, PA 16801 000084 Quantify Sqlo Report *J Study No.:L34910, Set No.: 073103A, Ext.Date:O7/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Cods: P:\Data\LCMSMSb\MaaslyPx\Fluorochemicals.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\L(3WSMS6\Masslynx\FluorochamiCals.PRO\Met~B\~catur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 28 Decatur BC BC 080103 Name: 073103A-1014 Text: : PFOSA -3491 O-12 Spk E, 5000 rig/L, DF=l 0 173103A-1014 Sm (Mn, 2x3) %1O'~~",~~~~,`~~.,`.~~,`.`~,...~,~"',"~~,~~~'I~~~' 2.00 4.00 6.00 01 -Aug-2003 14:07:06 LC/MS/MS #6 MAM of 4 Channels ES- 9.89 96556 7 78 1 4985.0A2ree5a Time 8.00 10.00 12.00 , Wren Re8earch, 3058 Research Drive, State College, PA 16801 000085 --------------- ___-_-_--- --------------me- Quantify Sample Report N& Study No .:L34910, Set No .:073103A, m&.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~SaaS6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\Masslynx\FluorochamicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 29 Decatur BC BC 080103 Neme: 073103A-1015 Text: .: CEI Acid (PFOA) L3491 O-1 6 Spk F, 5000 rig/L, DF=lO 373103A-1015 Sm (Mn, 2x3) ,. lOO- %- 01 -Aug-2003 14:28:57j LC/MS/MS #6 MRM of 4 Channels ES413>369 2.96e6 Area L34910-16 Spk F, 5000 rig/L, DF=lO 073103A-1015 100- Sm (Mn, 2x3) %- L34910-16 Spk F, 5000 rig/L, DFdO 073103A-1015 lOO- Sm (Mn, 2x3) %- 0 "")""I""I""1~"`I""I~"`l""1""1 2.00 4.00 6.00 0%Aug-2003 14:28:57 LWMSNS #6 MRM of 4 Channels ES- 8.98 399 > 80 3.61 e5 Area ,,,, , , , , , III ,lTime 10.00 12.00 01 -Aug-2003 14:28:5? LCIMSIMS #6 MRM of 4 Channels ES499 > 99 6.80e5 Area , 1 I I , j I . I I I Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000086 Quantify Sarqple Report lulr/ Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massl~\Fluoroch~cals.PRO\S~leDB\O73~03A Sun Aug 03 07:08:13 2003 P:\Data\LCMSNS6\Masslynx\Fluorochemicars\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Name: 0733.031-I.015 Text : Page 30 Decatur BC BC 080103 L3491 O-1 6 Spk F, 5000 rig/L, DF=lO 073103A-1015 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 14:28:57 LCNSIMS #6 MRM of 4 Channels ES- 9.90 1070943 498 > 78 5.50e5 Area 0 ~,,,~,,,.,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,~,,,,,~,,,~,,,~,lTime 2.00 4.00 6.00 8.00 10.00 12.00 ExyOen Research, 3050 Research Drive, State College, PA 16801 000087 Quantify Sample Report p4 Study No.: L34910, Set No .:073103A, Xxt.Date:O7/31/03, Analyst:X.Risha Page 31 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQMSMS6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\~sslynx\Fluarochemicalr Sun Aug 03 07:11:59 2003 Decatur BC EC 080103 Printed: ----_- Sun Aug 03 07:19:29 --- ------ 2003 --------- I---------- Name: 073103A-1016 Text : 1: CB Acid (PFOA) XCO72503-1,25 rig/L Standard 073103A-1016 Sm (Mn, 2x3) 01 -Aug-2003 14:50:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.13- 413 > 369 6931 4.38e4 Area 0 "","","","`~,"","",""~""," , , , 7mTime 2.00 4.00 6.00 8.00 10.00 12.00 !: c6 Sulfonate (PFHS) KC072503-1,25 rig/L Standard 073103A-1016 `OO7 Sm (Mn, 2x3) 8.98 1444 1 01 -Aug-2003 14:50:44 LC/MS/MS #6 MRM of 4 Channels ES- 399 > 80 8.96e3 Area %$ 4 lr-;;:., Time - 2.00 4.00 6.00 8.00 1o:oo 12100 3: C8 Sulfonate XCO72503-1,25 (PFOS) rig/L Standard 073103A-1016 Sm (Mn, 2x3) 01 -Aug-2003 14:50:44/ LC/MS/MS #6 MRM of 4 Channels ES- 9.26 499 > 99 954 5.75e3 Area m Time 2.00 4.00 6.00 8.00 10.00 12.00 Xxygen Research, 3058 Research Drive, State College, PA 16801 000088 Quantify Sample Report $,# Study No.:L34910, Set No .:073103A, Ext,Date:07/33./03. Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~~S6\~rrasslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:00:13 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\~catur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 32 Decatur BC BC 080103 Name: 073103A-1016 Text : 4: PFOSA XCO72503-1,25 rig/L Standard 073103k1016 100- Sm (Mn, 2x3) %- . 01 -Aug-2003 14:50:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1.95e4 Area or,,,,,,,,.,,~,,,,,,,,,,, 2.00 4.00 . , , , I , 1Time 10.00 12.00 Exygsn Research, 3058 Research Drive, State College, PA 16801 000089 -- -- --e-w I_-------- Quantify Sample Report Study No.: L34910, Set No.:O731031, Ext.Date:07/31/03, Analyst:K.Risha Ssmple List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Massl~\Fluoroch~cals.P~\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\~SMS6\~sslynx\PluorochemlcalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 ----_-------___-------------_______I____________- Name: Text: 073103A-I.017 1: C8 Acid L3491 o-1 (PFOA) 073103A-1017Sm(Mn,2x3) lOO- %- Page 33 Decatur EC BC 080103 -- 01 -Aug-2003 15:12:28 LC/MS/MS #6 MRM of 4 Channels ES413,369 5.12e6 Area 0 ~lll,llll,llll,llll,II.~,IIII,I,II/,,rl,llll , , , , , , , , s7Tjme 2.00 4.00 6.00 8.00 10.00 12.00 2: C6 Sulfonate L3491 O-l (PFHS) 073103A-1017Sm(Mn,2x3) 100- %- 01 -Aug-2003 15: 12:28 LC/MS/MS #6 a.99 5Ol627 MRM of 4 Channels ES399 > 80 3.04e5 Area * 0 ~~~.,~~,~,,~~~,~,,,,.,,,,,,,,,,,,.,,,,,,,,,,~,~,,,,,,,,,,,,Time 2.00 4.00 6.00 3: C8 Sulfonate L3491 O-l (PFOS) 073103A-1017 10 Sm (Mn, 2x3) %- 8.00 9.25 2eo1a3- 10.00 12.00 01 -Aug--2003 15:12:2d LCIMSIMS #6 MRM of 4 Channels ES499 > 99 1.61e6 Area 0 ,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,.,,,,~,,.,cc,.,,,,,,,.,,,Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Reeearch, 3058 Research Drive, State CoJ.lege, PA 16801 000090 Quantify Sanwle Report '4 Study No.: L34910, Set No .:073103A, Ext.Data:O7/31/03, Analyst:K.Risha Smle List: Last modified: Method: Last modified: Job Code: P:\Data\L~SblS6\~Haaslynx\Fluoroch~cals.PRO\S~l~DB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LWSMS6\Masslynx\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 34 Decatur EC BC 080103 Name: 073103A-1017 Text : 4: PFOSA IL3491 O-I 073103A-1017 Sm (Mn, 2x3) 100- %- 01 -Aug-2003 15:12:28j LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 7.51e5 Area WSJen Research, 3058 Research Drive, State College, pa 16801 _---_- --.- . 000091 Quantify Sample Report -4 Study No .:L34910, Set No.: 073103A, Ext.Data:O7/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCbl~S6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSblS6\bsasslynx\Fluorochemicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 35 Decatur BC BC 080103 Name: 073103A-1018 Text: t: C8 Acid (PFOA) L3491 O-l Rep 073103A-1018 10 Sm (Mn, 2x3) % 9.13 626646 01 -Aug-2003 15:34:16 LC/MS/MS #6 MRM of 4 Channels ES413> 369 4.94e6 Area i Time 2.00 4.00 6.00 8.00 lo:oo 12.00 ] \IJ 2: C6 Sulfonate L3491 O-1 Rep (PFHS) ~-.n-.--,.7RlfY?Lblnl6.-. 4-n IUU- Sm(Mn,zxa) %- 9.00 49342 01 -Aug-2003 15:34:18 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.99e5 Area : C8 Sulfonate -3491 O-1 Rep (PFOS) 373103A-1018 10 "$ J Sm (Mn, 2x3) 9.26 27417C I Ol-Aug-2003 15:34:1 E LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.56eE Area L Time 12.00 Oxygen Research, 3058 Research Drive, State College, pA 16801 000092 Quantify Sample Report w Study No.:L34910, Set No.. .073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LBISMS6\Masslynx\Fluoroch~ca~s.PRO\S~~eDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LC1M~S6\MsslyPx\FluorochamicB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 36 Decatur BC BC 080103 Name : 073103A-1018 Text : 4: PFOSA L3491 O-l Rep 073103A-1018 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 15:34: 1E LciMslMs #f MRM of 4 Channels ES- 9.90 498> 7E 7.30eE Area , , , , , , , , 1Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000093 Quantify Sample Report w Study No.rL34910, Set No.. *073103A, Ext.Date:O7/31/03, Analyst:K.Risha Smnple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Maselynx\Fluorochamicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LWSMS6\Kaaslyrur\Pluorochemicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 37 Decatur BC BC 080103 Name: Text: 073103A-1019 1: CB Acid 1-3491 o-4 (PFOA) (173103A-1019 10 Sm (Mn, 2x3) 9.14 575640 01 -Aug-2003 15:56:0$ LC/MS/MS #i MRM of 4 Channels ES413>369 3.34e6 Area O',,,,,,,,,,,,,,,,,,,,~,,,,,,,,,,~~~,,~,~,~~~~~~~~,~~~,,~~~~rTime 2.00 4.00 6.00 'ccl, 2: C6 Sulfonate L3491 o-4 (PFHS) 073103A-1019 Sm (Mn, 2x3) 8.00 8.98 3196i 10.00 12.00 01 -Aug-2003 15:56:Od LC/MS/MS #ii MRM of 4 Channels ES399 > 80 &-- 1T.9iAm7r8e5a - 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate L3491 o-4 (PFOS) 073103A-1019 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 15:56:09 LC/MS/MS #6 MRM of 4 Channels ES- 9.26 499 > 99 1.19e6 Area 0 `~`,,"","","","","",""I"","", , r . I v , , I , , Time 2.00 4.00 6.00 8.00 10.00 12.00 u Oxygen Research, 3058 Research Drive, State College, PA 16801 000094 Quantify Sample Report \*f Study No.:L34910, Set No.: 0731031, Ext.Date:07/31/03, Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LC3YI~S6\~ssl~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LWSMS6\~sslynx\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Analyst:K.Risha Page 38 Decatur BC BC 080103 Name: 073103A-1019 Text : 4: PFOSA . L349l o-4 ' _. .. 073103A-1019 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 l&56:09 LC/MS/MS #6 MRM of 4 Channels ES- 9.91 498>78 5.46e5 Area 0 I#,# 1 II,llll,,jl,,l,l,,,,,,l,l 2.00 4.00 I , , I I > ,,I,,, 6.00 8.00 I 10.00 , , , ,Time 12.00 Eaqygen Research, 3058 R&march Drive, State College, PA 16801 00009s Quantify Sample Report w Study No.:L34910, Set No.: 073103A, lZxt.Date:07/31/03, Analyst:K.Ri.sha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\M3MSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\~catur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 39 Decatur BC BC 080103 Name: 073103A-1020 Text : . : C8 Acid 1-3491 o-2 (PFOA) (173103A-1020 10 Sm (Mn, 2x3) 9.13 605630 01 -Aug-2003 16:17:55 LC/MS/MS #6 MRM of 4 Channels ES413>369 3.49e6 Area `- q,& 2: C6 Sulfonate IL3491 o-2 (PFHS) 073103A-1020 lO& Sm (Mn, 2x3) %- 0 "","","","","","",`~","", 2.00 4.00 6.00 3: C8 Sulfonate L3491 o-2 (PFOS) 073103A-1020 100- Sm (.Mn, 2x3). %- 0 ,~,~,,~,,,,,,,,~,~,,,,,,,.,,,,,,,,,,,,,,~~~,,~,,,,,,,,.,,,,Time 2.00 4.00 6.00 V` L Time 12.00 0%Aug.2003 16:17:5Ei] LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 2.18e5 Area , , I,, , , , , I, a1Tjme 8.00 10.00 12.00 9.27 1916313 0%Aug-2003 16:17:55 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.08e6 Area 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000096 Quantify Sample Report Study No.:L34910, Set No .:073103A, Ext.Dats:07/31/03, Analyst:K.Risha Page 40 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\M3HSMS6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCM~S6\Masslynx\Fluoroch~cals~PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 --1- -- --------- --P--------P____ ---- Neme: Text: 0731031-3020 4: PFOSA 1L3491 o-2 073103A-1020 loo- Sm (Mn, 2x3) %- 01 -Aug-2003 16:17:55j LC/MS/MS #6 MRM of 4 Channels ES- 9.92 490 w 78 4.67e5 Area Exygen Research, 3058 Research Drive, State College, PA 16801 000097 Quantify Sample Report w Study No.:L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 41 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCbl~S6\~sslynx\Fluoroch~ca~s.PRO\S~leDB\O73103A Sun AUg 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: m-m- Sun Aug 03 07:19:29 2003 ----------___ --------a--- Name: 073103A-1021 Text : -----__ ---- * C8 Acid (PFOA) -3491 O-3, DF=lOO 373103A-1021 10 Sm (Mn, 2x3) 01 -Aug-2003 163393423 LClMS/MS #6 MRM of 4 Channels ES- 413>369 3 1.73e5 Area ` 1: C6 Sulfonate (PFHS) L3491 O-3, DF=l 00 073103A-1021 10 Sm (Mn, 2x3) Ol-Aug-2003 16:39:4 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 5426 3.25e4 Area 1 - 3: C8 Sulfonate (PFOS) L3491 O-3, DF=l 00 073103A-1021 Sm (Mn. 2x3) 01 -Aug-2003 16:39:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 6016 3.45e4 Area L______, 10.00 Time 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 _^ ._-.-.. ~-- l___lll_. - _-..-....- 000098 -------___ Quantify Sample Report \*uf Study No.:L34910, Set No.. *073103A, --_I_ Ext,Date:07/31/03, -Analyst:X.Risha --Page 42 Sarqple List: Last modified: Method: Last modified: Job Code: P:\Data\~S6\Masslynx\Fluorochsmicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\~et~B\~catur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: -----w--w--- Sun Aug 03 07:19:29 2003 -v----e--- ---- ------------___ Name: 073103A-1021 Text: 4: PFOSA -3491 O-3, DF=lOO 01 -Aug-2003 16:39:42 LC/MS/MS #6 )73103A-1021 Sm (Mn, 2x3) MRM of 4 Channels ES- %110O-4 9.92 498 > 78 5.15e4 Area , o~,~i~,l~~~,~~~`,`~~~,`~~~,~,~~,~~~~,~~~~,,~~~,~~~ 2.00 4.00 6.00 a.00 Exygsn Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report q& Study No.:L34910, Set No.. *073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 43 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\asslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\~ssl~\Fluorochemi\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ---e-m- Sun Aug 03 07:19:29 2003 ------_------------- --e------ Name: 013103A-1022 Text : : c8 Acid (PF~A) (CO72503-2,50 rig/L Standard )73103A-1022 10 Sm (Mn, 2x3) 01 -Aug-2003 17:01:2d LC/MS/MS #6 MRM of 4 Channels ES413>369 8.40e4 Area !: C6 Sulfonate KC072503-2,50 (PFHS) rig/L Standard 373103A-1022 Sm (Mn, 2x3) 6.00 8.99 2420 3: C8 Sulfonate XCO72503-2,50 (PFOS) rig/L Standard 073103A-1022 `Oo1 Sm (Mn, 2x3) I ' ' ' I '7 Time 10.00 12.00 01 -Aug-2003 17:01:26 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.73e3 Area z Time 12.00 Exygen Research, 3058 Research Drive, Stats College, PA 16801 oooioo --_I_-- -- --- Quantify Sample Report && Study No.:L34910, Set No.: 0731031, Ext,Date:07/31/03, Analyst:X.Risha Page 44 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQMSMS6\Masslynx\Fluorochamicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:3.9:29 2003 --- --- --------- ---- -----I------ Nsme: 073103A-1022 Text : 4: PFOSA XCO72503-2,50 rig/L Standard 073103A-1022 Sm (Mn, 2x3) 01 -Aug-2003 17:01:21 LC/MS/MS #t MRM of 4 Channels ES 498 > 7t 3.55er Are: Time 12.00 -en Research, 3058 Research Drive, State College, PA 16801 00~0?L01 Quantify Smle Report fullrf Study No.:L349l.O, Set No.: 073103A, Ext.Dats:07/31/03, Analyst:K.Risha Samgle Liat: Last xmdified: Method: Last modified: Job Code: P:\Data\LCHSMS6\~ssl~\Fluorochemicals.PRO\S~leDB\O73lO3A !&XII Aug 03 07:08:13 2003 P:\Data\L(41SMS6\Esslynx\Fluorochamict~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 45 Decatur BC BC 080103 Name: 073103A-I.023 Text : 1: C8 Acid IL3491 o-6 (PFOA) 073103A-1023 IOO- Sm (Mn, 2x3) %- 9.14 _ 173871 0%Aug-2003 17:23:1j LC/MS/MS #6 MRM of 4 Channels ES- 413>369 1 .Ol e6 Area 0 "","","~`,"","",`~"~"","",`~~' , I I , , , , 1 , , L , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 , q& 2: C6 Sulfonate L3491 O-6 (PFHS) 073103A-1023 Sm (Mn, 2x3) 0%Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 5.16e4 Area r13 : C8 .3491 Sulfonate o-6 (PFOS) C)73103A-1023 Sm (Mn, 2x3) 100-l Time 12.00 Ol-Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.66e5 Area I 2.00 4.00 6.00 8.00 10.00 12.00 1 Emen Research, 3058 Research Drive, State College, PA 16801 000102 Quantify Sample Report I,, Study No.:L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 46 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Msslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Wlselynx\Pluorochemicals.PRO\~~t~B\D~=atur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed : Sun Aug 03 07:19:29 2003 -m-------------w----------- Name: 073103A-1023 Text : --------- 4: PFOSA L3491 O-6 073103A-1023 loo- Sm (Mn, 2x3) %- 01 -Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 Channels ES- 9.88 498 > 78 l.Ole5 Area W Exygen Research, 3058 Research Drive, State College, PA 16801 000103 Quantify Sample Report 'IJ Study No.:L34910, Set No .:073103X, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last mmiifiedr Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluorochamicals.PRO\S~l~DB\O73~O3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 47 Decatur BC BC 080103 Name: 073103A-I.024 Text : : C8 Acid (PFOA) -3491 O-6 Rep )73103A-1024 10 Sm (Mn, 2x3) 9.13 181075 i 01 -Aug-2003 17:45:01 LC/MS/MS #6 MRM of 4 Channels ES413>369 1.07e6 Area 2: C6 Sulfonate IL3491 O-6 Rep (PFHS) 073103A-1024 Sm (Mn, 2x3) 01 -Aug-2003 17:45:Oj LC/MS/MS #6 MRM of 4 Channels ES399 > 80 5.23e4 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 L3491 O-6 Rep 073103A-1024 100- Sm (Mn, 2x3) %- 01 -Aug-2003 17:45:071 LCIMSNS #6 MRM of 4 Channels ES499 > 99 2.62e5 Area 0 (~~~,"`~,~~~1,`)~`,~`~`1""1""l""l""l , , , , I I 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 WSIen Research, 3050 Research Drive, State College, PA 16801 000104 ----------_ ------ w--w Quantify Sample Report ljj& Study No.:L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~~eDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 -----Page 48 Decatur BC BC 080103 Name: Text: 073103A-1024 4: PFOSA l.3491 O-6 Rep 073103A-1024 lOO- Sm (Mn, 2x3) 01 -Aug--2003 17:45:Oi LCIMSNS #E MRM of 4 Channels ES* 498 > 7E! 1 .OleZ Bxygen Research, 3058 Research Drive, State College, PA 16801 000105 ---- ----- ----- M---e-_ Quantify S-10 Report ~II,& Study No.:L34910, Set No .:073103A, Ea&.Date:07/31/03, Rnalyat:K.Riaha Sample List: Last modified: Method: Last nmdifisd: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals~PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\U3M~SS\~sslyPx\Fluorochamic\Decatur Sun Aug 03 07:11%59 2003 Printed: -em- Sun Aug 03 07:19:29 2003 -------------_-- Name: 073103A-1025 Text : ---me- L: C8 Acid L34910-9 (PFOA) 073103A-1025 `*OJ Sm (Mn, 2x3) 9.13 I 35519c ) ----- Page 49 Decatur BC BC 080103 01 -Aug-2003 l&06:53) LC/MS/MS #6 MRM of 4 Channels ES413 >A3re6a9 2.13e6 L 'culrf 2: C6 Sulfonate IL3491 o-9 (PFHS) 073103A-1025 IOO- Sm (Mn, 2x3) %- 8.00 8.99 _ 21096 10.00 Time 12.00 ~ Ol-Aug-2003 18:06:53/ LC/MS/MS #6 MRM of 4 Channels ES399 r 80 1.26e5 Area 0 "","",",`,"","","",""I"","' , , I , , , 1 , I I , Time 2.00 4.00 6.00 8.00 10.00 12.00 3 : C8 Sulfonate r I -3491 o-9 (PFOS) ()73103A-1025 Sm (Mn, 2x3) 9.24 112921 01 -Aug-2003 18:06:54 LCIMSMIIS #6 MRM of 4 Channels ES499 > 99 6.60e5 Area Time wW+n Research, 3058 Research Drive, State College, PA 16801 000106 --- --- Quantify Sample Report $rf Study No.:L34910, Set No.: 0731031, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCbl~S6\bZasslynx\Fluoroch~ca~s.PRO\S~leDB\O73103A Sun AUg 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochenieals.PRO\Met~B\Decatur Sun hug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 50 Decatur BC BC 080103 Name: 073103A-1025 Text : -. c 4: PFOSA-" L3491 O-9' .: - 073103A-1025 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 18:06:53 LC/MS/MS #6 MRM of 4 Channels ES- 9.88 498 > 78 2.66e5 Area 0 "","","","","","",""l"","", , I r r ( Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygea Research, 3058 Research Drive, State College, PA 16801 000107 v-e------- ----- __-_- ------------ -------_ Quantify Sample Report *d Study No.: L34910, Set No.: 0731031, Ext.Date:07/31/03, Analyst:K.Rfsha Sampl.e List: Last modified: Method: Last modified: Job code: P:\Data\L~SblS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73~03A Sun Aug 03 07:08:13 2003 P:\Data\LClblSMS6\Maselynx\Fluoroch~cals.PRO\~et~B\Decatur Sun Aug 03 07:11x59 2003 Page 51 Decatur BC BC 080103 Printed: Sun hug 03 07:19:29 2003 ----------------____----------- -Be---- --------- Name: 073103A-1026 Text : 1: C8 Acid 13491 o-7 (PFOA) 073103A-1026 IOO- Sm (Mn, 2x3) %- 01 -Aug-2003 18:28:44 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 2.97e6 Area b& 2: C6 Sulfonate 13491 o-7 2.00 (PFHS) 073103A-1026 loo- Sm (Mn, 2x3) %- I I ( I I I, ( I I I ,, Time 6.00 8.00 10.00 12.00 8.98 _ 33965 01 -Aug-2003 18:28:44 LWMSNS #6 MRM of 4 Channels ES399 > 80 2.04e5 Area 0 "","","",`,","","","","","","","",',,,, Time 2.00 4.00 6.00 8.00 10.00 12.00 #: C8 Sulfonate -3491 o-7 (PFOS) 373103A-1026 Sm (MI-I, 2x3) 9.26 149081 01 -Aug-2003 18:28:44) LC/MS/MS #6 MRM of 4 Channels ES499 > 99 8.38e5 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000108 ---- ------- --- Quantify Sample Report $,& Study No.:L34910, Set No.: 0731031, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Pluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 52 Decatur BC BC 080103 Name: 073103A-1026 Text : 4: PFOSA IL3491 o-7 073103A-1026 IOO- Sm (Mn, 2x3) %- 01 -Au.g-2003 18:28:44/ K/MS/MS #6 MRM of 4 Channels ES- 9.92 67031 498 > 78 3.44e5 Area 0 "",""/"","~`,`~","(`,"","`J,"(`,") I I I I I 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 1680; 000109 --- --- v------p Quantify Sample Report $I& study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:lC.Risha Salnple List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lo3A Sun Aug 03 07:08:13 2003 P:\Data\L~~S6\blasslynx\FluorochamicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: -- Sun Aug 03 07:19:29 2003 ------------------------------~~~---~~~~ Name: 0731033-1027 Text : 1: C8 Acid (PFOA) IL3491 O-8, DF=lOO 073103A-1027 Sm (Mn, 2x3) 9.13 Page 53 Decatur BC BC 080103 --- Ol-Aug-2- 003 18:50:3d LC/MS/MS #6 MRM of 4 Channels ES413>369 1.32e5 Area `md 2I- C6 Sulfonate (PFHS) d4910-8, DF=lOO 173103A-1027 10 Sm (Mn, 2x3) Time 12.00 01 -Aug-2003 18:so:ad LC/MS/MS #6 MRM of 4 Channels ES- 8.9: 399 > 80 534 3.1 Oe4 Area m Time i 2.00 4.00 6.00 8.00 1o:oo 12100 3: C8 Sulfonate (PFOS) L3491 O-8, DF=lOO 073103A-1027 Sm (Mn, 2x3) 01 -Aug-2003 18:50:30 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.67e4 Area Time 12.00 Rxygen Research, 3058 Research Drive, State College, PA 16601 000110 p-m-- --------------- ----ye Quantify Sample Report l,& Study No.:L34910, Set No .:073103A, Ekt.Dats:07/31/03, Analyet:K.Risha Page 54 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L(3MSMS6\Masslynx\Fluorochamicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L(1MSMS6\Masslynx\Fluor4chsmical\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ------------I_--- Sun Aug.03 07:19:29 2003 ------- -p-s--- Name: 073103A-1027 Text : : PFOSA -3491 O-8, DF=lOO )73103A-1027 10 Sm (Mn, 2x3) % Ol-Aug-2003 18:50:8 LC/MS/MS #I t&M 9.9c 1 563: 3 of 4 Channels ES. 498 > 71 3.03e( Are; / OL;~~~,~~`~,"~~,~~`~,~~`~,~~~`,~~'.,~~~~,~"~,~~~ L Time 2.00 4.00 6.00 8.00 10.00 12.00 ExyOen Research, 3058 Research Drive, State College, PA 16801 000111 --- ---- ----m-w------- --------- Quantify Sample Report 'hd Study No.:L34910, Set No .:073103A, Ext,Dats:07/31/03, Analyst:lC.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\blassl~\Fluoroch~ca~s.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 3003 P:\Data\LCMSMS6\Ezasslynx\Fluorochemicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19$29 2003 s----v- Page 55 Decatur BC BC 080103 Name: Text: 073103A-1028 1: C8 Acid (PFOA) XCO72503-3,100 rig/L Standard 073103A-1028 Sm (Mn, 2x3) 01 -Aug-2003 19:12:2C LC/MS/MS #6 MRM of 4 Channels ES413>369 1.85e5 Area Yd 2: C6 Sulfonate XCO72503-3,100 (PFHS) rig/L Standard 073103A-1028 Sm (Mn, 2x3) Time 12.00 ~ Ol-Aug-2003 19:12:2C LC/MS/MS #6 MRM of 4 Channels ES399 > 80 3.59e4 Area rI3': C8 Sulfonate l(CO72503-3,100 (PFOS) rig/L Standard 173103A-1028 Sm (Mn, 2x3) 10 Time 12.00 01 -Aug-2003 19:12:2d LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.09e4 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State Collega, PA 16801 000112 -- --- ----- Quantify Sample Report V& Study No.rL34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:IC.Risha Page 56 sample List: Last modified: Method: Last modified: Job Code: P:\Data\~MS6\~8slynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LQMSMS6\Masslynx\FluorochemicalsB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ------- ---m---e --I---P------_1 Name: 073103A-1028 Text : 4: PFOSA sXC072503-3, 100 rig/L Standard 073103A-1028 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 19:lmd LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 7.45e4 Area Exrgen Research, 3058 Research Drive, State College, PA 16801 000113 Quantify Sample Report Study No.: L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample Lfstr Last modified: Method: Last modified: Job Code: P:\Data\LClrLSMS6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\MJM~S6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07~19~29 2003 Page 57 Decatur BC BC 080103 Name: 073103A-1029 Text : r1: C8 Acid L34910-12 (PFOA) 073103A-1029 lOO- Sm (Mn, 2x3) 01 -Aug-2003 19334303 LC/MS/MS #6 MRM of 4 Channels ES413>369 1.47e7 Area %- J 0 "","",""(""(`,,`,"","","","" , , , , , , , , , , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 2: C6 Sulfonate 13491 o-1 2 (PFHS) 073103k1029 lOO- Sm (Mn, 2x3) %- 8.99 259042 01 -Aug-2003 19:34:03 K/MS/MS #6 MRM of 4 Channels ES399 > 80 1.50e6 Area 0 "")"",`"`i'"`,"`~,`.","",""l"' ~ , . , , , I . , ~ , , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 . 3: C8 Sulfonate L3491 o-1 2 (PFOS) 073103A-1029 iOO-- Sm (Mn, 2x3) %- 9.27 _ 558236 01 -Aug-2003 19:34:03 LCYMSIMS #6 MRM of 4 Channels ES499 > 99 3.19e6 Area 0 ,,.,,,,,~,,,,,,.,,,,,,,,,,~,,,~~~~,~~~~,~,~~,~~~,~~~~,~~.~lTime 2.00 4.00 6.00 8.00 10.00 12.00 Exygea Research, 3058 Research Drive, State College, PA 16801 000114 Quantify Sample Report \IIJ Study No.:L34910, Set No .:073103A, Ea&.Date:07/31/03, Analyst:R.Risha Pags 58 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Mssslynx\Fluorochamicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: --- Sun Aug ------------------______________I_____c_-------- 03 07:19:29 2003 Name: 0731031-1029 Text : 4: PFOSA L3491 o-1 2 073103A-1029 lOO- Sm (Mn, 2x3) %- Ol-Aug-2003 19:34:03 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1.36e6 Area 0 ~~~~,~~`~,(~(`,J,`~,~~J/,/"~,~(~I,'~(',~'~~,/(~ 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State Collage, PA 16801 000115 Quantify Sample Report p3 Study No.:L34910, Set No .:073103A, Ea&.Date:O7/31/03. Analyst:X.Risha Page 59 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCW~S6\Hassl~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 --~-----------------~---------- Name: 073103A-1030 Text : ----- --w-m-- 1: C8 Acid (PF~A) L3491 O-12 Rep 073103A-1030 loo- Sm (Mn, 2x3) %- 9.11 24251891 01 -Aug-2003 19:55:5C LC/MS/MS #6 MRM of 4 Channels ES413 > 369 1.43e7 Area () ,,,,,,,.,,,,,,,~,,,,,,,,,,,,,,,,~~,~~~~,~~~~~~~~,~~~~,,,,,lTime 2.00 4.00 6.00 w 2: C6 Sulfonate (PFHS) L3491 o-1 2 Rep 073103A-1030 100, Sm (Mn, 2x3) %- 8.00 6.98 _ 237649 10.00 12.00 Ol-Aug-2003 19:55:5C LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.45e6 Area i: Cf3 Sulfonate L34910-12 Rep (PFOS) 073103A-1030 10 Sm (Mn, 2x3) % 1 4 9.24 571211 0%Aug-2003 19:55:5C LCIMWMS #6 MRM of 4 Channels ES499 > 99 3.17e6 Area I Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000116 Quantify Sample Report bit Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 60 Sam;ple List: Last modified: Method: Last modified: Job Code: P:\Data\LQvI~S6\Wassl~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCLvISMS6\Masalynx\FluorochemicalS.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ----------------- ------ -_-_ --------_-- ----- Name: Text: 073103A-I.030 4: PFOSA L3491 O-l 2 Rep 073103A-1030 I `7lfXI-7 %- Sm (Mn, 2x3) Oi-Aug-2003 19:55:5d LCIMSNS #6 MRM of 4 Channels ES- 9.90 498 > 78 1.32e6 Area 0 "","","","","","","",`l"~"","' , , , , , , , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 W Oxygen Research, 3058 Research Drive, State College, PA I.6801 -.- "_,---- - -. ".. . ,Ill-.--.------ 000117 -------l____l_------____----------- Quantify Sample Report %a.# Study No .:L34910, Set No.:O73103A, Ext.Date:07/31/03, knalyat:X.Risha Swle List: Last modified: Method: Last modified: Job Code: P:\Data\W3blSMS6\Wsssl~\F~uorochemicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMSC\Mssslynx\Pluorochemicals~\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 -- Page 61 Decatur BC BC 080103 Name : 073103A-1031 Text : : C8 Acid .34910-15' (PFOA) . )73103A-1031 10 % 1 Sm (Mn, 2x3) 9.13 252700: 01 -Aug-2003 20: 17:38 LC/MS/MS #6 MRM of 4 Channels ES413>369 1.47e7 Area L 2.00 4.00 6.00 8.00 10.00 12.00 %& 2: C6 Sulfonate (PFHS) L3491 o-1 5 I073103A-1031 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 20:17:38( LC/MS/MS #6 MRM of 4 Channels ES- 399 >- 80 1.43e6 Area 0 "","","","","","","`l,"" 2.00 4.00 I: C8 Sulfonate 134910-15 (PFOS) 373103A-1031 10 Sm (Mn, 2x3) , , , ,, , ( , I,, , Time 6.00 8.00 10.00 12.00 9.25 560111 8 Ol-AUQ-2003 20:17:3d LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.15e6 Area L- Time %d 2.00 4.00 6.00 8.00 10.00 12.00 J Oxygen Research, 3058 Research Drive, State College, PA 16801 000118 Quantify Sample Report UJ Study MO.:L34910, Set No.:073103A, Ext.Date:O7/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\~ssl~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L(SM~6\Mas~l~\Fluorochemicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 - Page 62 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 -----e-------------P -___-------- ----m-m- ------- Name : 073103A-1031 Text : 4: PFOSA L3491 o-1 5 073103A-1031 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 2O:i 7:3d LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1.39e6 Area 0 "~~,~~~~/~~~~/~I.I,llll,llll[llll,l,lI,llll,,,, I r ' I Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000119 Quantify S-10 Report `4 Study No. : L34910, Set No.:O73103A, Ea&.Data:07/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCJM~6\~sslynx\Fluoroch~cals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\L(3KSMS6\Masslynx\Fluorochemicalr Sun Aug 03 07:11:59 2003 Printed: ----~-----_----_I-_------- Sun Aug 03 07:19:29 2003 ------ -------____.wl_l Name: 073103A-3032 Text : Papa 63 Decatur BC BC 080103 L3491 o-1 3 073103A-1032 10 Sm (Mn, 2x3) % 9.11 2649670 01 -Aug-2003 20:39:2 LCYMWMS #6 MRM of 4 Channels ES413~369 1.69e7 Arear -i L d Time i 2.00 4.00 6.00 8.00 10.00 12100 qd 2: C6 Sulfonate L3491 o-1 3 (PFHS) Ol-Aug-2003 20:39:2 073103A-1032 loo- Sm (Mn, 2x3) %- MRM of 4 Channels ES- 6.98 _ 275858 399 > 80 1.67e6 Area - 0 ",`,"","","","",,"`,"","","' , , , , , , , t , , , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 I: C8 Sulfonate -34910-13 (PFOS) 373103A-1032 Sm (Mn, 2x3) 9.24 66718t 3 Ol-Aug-2003 20:39:25 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.69e6 Area L-- Time 2.00 4.00 6.00 8.00 10.00 12.00 XJWOen Research, 3058 Research Drive, State Collegta, PA 16801 000120 ---- --a------------- --- Quantify Sample Report '1~ Study No .:L34910, Set No.:O73103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~~S6\~8slynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCblSMSb\Masslynx\FluorochemicalR\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 -- Page 64 Decatur BC SC 080103 Name: 073103A-1032 Text : 4: PFOSA L3491 o-1 3 073103A-1032 loo- Sm (Mn, 2x3) %- 01 -Aug-2003 20:39:25 LCNWMS #6 MRM of 4 Channels ES- 9.90 498>7a 1.4286 Area , , , , , , , ,, Time 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report VI& Study No.rL34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\Masslynx\Fluoroch~ca~s.PRO\S~l~DB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicale~\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 65 Decatur BC BC 080103 Name: 0731031-1033 Text : .: C8 Acid (PFOA) -3491 O-1 4, DF=lOO 373103A-1033 10 Sm (Mn, 2x3) 9.12 71294 01 -Aug-2003 21:00:54 LC/MS/MS #6 MRM of 4 Channels ES413>369 4.14e5 Area W 2: c6 Sulfonate (WI-IS) /IL3491 O-14, DF=lOO 073103A-1033 Sm (Mn, 2x3) 3: C8 Sulfonate (PFOS) L3491 O-l 4, DF=lOO 073103A-1033 100, Sm (Mn, 2x3) %- ~":.,,,,,,,,,,~,,,~,,,~,,~,,,~~,,,,,,~~~~,~~~~,~l~,~~~~,~~l'~Time 2.00 4.00 6.00 i.-10.00 Time 12.00 Ol-Aug-2003 21:00:58 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 9718 5.83e4 Area I 10.00 Time 12.00 01 -Aug-2003 21:00:58 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 _ 14981 499 > 99 8.40e4 . Area 8.00 10.00 12.00 mea Research, 3058 Research Drive, State College, PA 16801 000122 ------- Quantify Sample Report V Study No.:L34910, Set No .:073103A, ----Ext.Date:07/31/03, -Analyst:K.Risha ------_ Page 66 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\MZd~S6\Masslynx\Fluorochamicals.PRQ\S~leDS\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\bhsslynx\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: --we- Sun Aug ---------- 03 07:19:29 2003 -----es-----s-e------ ---------__-___- Name: 073303A-1033 Text : : PFOSA -3491 O-l 4, DF=lOO 173103A-1033 10 %4"i Sm (Mn, 2x3) 01 -Aug-2003 21 :OO:SE LC/MS/MS #E MRM of 4 Channels ES- 9.90 1141( 3 498 > 7e 5.88e4 Area oL;-`~~,"~~,~~~`,`~`~,~`~~,~~~~I'~~'l~~~~I~~'~I~~r L Time 2.00 4.00 6.00 8.00 -en Research, 3058 Research Drive, State College, PA 16801 000123 Quantify Simple Report V Study No.:L34910, Sat No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 67 Sqle List: Last modified: Method: Last modified: Job Code: P:\Data\LQMSMS6\Masslynx\Fluoroch~cals.PRO\S~laDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~S6\Massl~\Fluoroch~cals.PRO\Met~B\D~catur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ----- --a-__-- ------ ---------_-------------_-- ------ Name: 073303A-1034 Text : 1: C8 Acid (PFOA) . XC072503-4,250 rig/L Standard 073103A-1034 10 Sm (Mn, 2x3) 9.13 75537 01 -Aug-2003 21:22:34 LCNSIMS #6 MRM of 4 Channels ES- 413>369 4.32e-5 Area TT.rl Time 2.00 4.00 6.00 8.00 10.00 12.00 !: C6 Sulfonate XC072503-4,250 (PFHS) rig/L Standard 073103A-1034 loo- Sm (Mn, 2x3) %- 01 -Aug-2003 21:22:31 LC/MS/MS #1 MRM of 4 Channels ES399 > 8( 8.49er Are: i: C8 Sulfonate l(CO72503-4,250 (PFOS) rig/L Standard 9.25 8521 Time Exygan Research, 3058 Research Drive, State Collage, PA 16801 000124 Quantify Sample Report W Study No. :L34910, Set No.: 073103A, Ext.Date:07/31/03, Analyst:K.Risha Samgle List: Last modified: Method: Last nrodified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~ca~s.PRO\SanrpleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LWSMS6\Masslynx\Fluorochemicals.PRO\~et~B\Decatur Sun Aug 03 07:11x59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 68 Decatur BC BC 060103 Name: 0731031-1034 Text : 4: PFOSA KO72503-4,250 rig/L Standard 173103A-1034 lOC- Sm (Mn, 2x3) %- 01 -Aug-2003 21:22:34 LC/MS/MS #6 MRM of 4 Channels ES- 9.92 336667 498 > 78 1.7Se5 Area %Ygen Research, 3058 Research Drive, State College, PA 16601 000125 ------_l__l ---- ---- -----me Quantify Sample Report Study No .:L34910, Set No.r073103A, Ext.Date:07/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\F~uotochsmicals.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatu~ Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 69 Decatur BC BC 080103 Name: 073103A-I.035 Text : 1: C8 Acid L34910-16 (PFOA) 073103A-1035 lO(F Sm (MI-I, 2x3) %- : 9.11 307297tq . 01 -Aug-2003 21:44:25 LC/MS/MS #6 MRM of 4 Channels ES413> 369 1.8587 Area 0 ,,,~,~~~~,~~~,,~,~~,~~,,,,~~~,~~,~,~~,~,~~~~~~~~,~,,~,,~~~~Time 2.00 4.00 6.00 2: C6 Sulfonate L3491 O-16 (PFHS) 073103A-1035 100- Sm (Mn, 2x3) %- 0 IIII,IIII,II.~,lll.(.lll,llll,lll,,IIII 2.00 4.00 6.00 3: C8 Sulfonate IL3491 O-16 (PFOS) 073103A-1035 100- Sm (Mn, 2x3) %- 8.00 8.98 10.00 12.00 I 01 -Aug-200321:44:23 LCNS/MS #6 MRM of 4 Channels ES399 > 80 1.74e6 Area ,,,, / ,,,, I, v,Time 8.00 10.00 12.00 9.24 691 16S7 Ol-Aug-2003 21:44:24 LC/MS/MS #6 MRM of 4 Channels ES- 499 > 99 3.86e6 Area 0 ,,,~,,,,;,~,,,,,,,.,,.,,,~,,,,,,~,,,,,,,,,,,~,,,..,,,,,,.,Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000126 Quantify Sample Report l& Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 70 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluoroch~ca~s.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\Massl~\FluorochsmicaB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 -------m-e----- -------------------- ------_ Name: Text: 073103A-1035 4: PFOSA L3491 O-l 6 073103A-1035 lOO- Sm (Mn, 2x3) %- Ol-Aug-2003 21:44:2! LC/MS/MS #E MRM of 4 Channels ES- 9.90 498 > 7E 1.82eE Aree Exygen Research, 3058 Research Drive, State College, PA 16801 000127 Quantify Sample Report w Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Anal.yst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SblS6\MasslyPx\Fluorochamica~s.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~Ca~s.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 I_-------------I---------____l_l- --------------__I_ Name: 0731038-1036 Text : Page 71 Decatur BC BC 080103 -------- L3491 O-1 6 Rep 073103A-1036 lOO- Sm (Mn, 2x3) %- 0%Aug-2003 22:06:04 LC/MS/MS #6 MRM of 4 Channels ES413>369 1.89e7 Area L3491 O-l 6 Rep 073103A-1036 10 Sm (Mn, 2x3) % /j 3: CB Sulfonate L3491 O-1 6 Rep (PFOS) 073103A-1036 10 9 Sm (Mn, 2x3) %- a.98 302530 0%Aug-2003 22:06:04 LCiMSNS #6 MRM of 4 Channels ES399 > 80 1.79e6 Area 9.25 707270`1 01 -Aug-2003 22:06:04 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.94e6 Area Exyoen Research, 3058 Research Drive, State College, PA 16801 000128 Quantify S-10 Report Lf Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemica~s.P~O\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSblS6\Masslynx\Pluoroch~cais.PRO\Met~B\Decat~r Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 72 Decatur BC BC 080103 Name: 073103A-1036 Text: 4: PFOa$A L3491 O-l 6 Rep 073103A-1036 1OCb Sm (Mn, 2x3) %- 01 -Aug-2003 22:06:04 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1.83e6 Area 0 "","","","","","","","",`I" 2.00 4.00 6.00 8.00 , 1 I I I Time 12.00 Eawgen Research, 3058 Research Drive, State College, PA 16601 000129 Quantify Sample Report b# Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:X.Risha Page 73 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LBISMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Kasslynx\FluorochamicaleB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ---- ---I_-------_-_____-_----------------------- F-m---- Name: Text: 073303A-3037 1: C8 Acid L34910-19 (PFOA) m ' .-.. " 073103A-1037 Sm (Mn, 2x3) 100, .- `.. %- 9.11 _ 2758295 01 -Aug-2003 22:27:50 LCIMSIMS #6 MRM of 4 Channels ES413>369 1.68e7 Area 00, I I , 1 1 , I I I 1Time 2.00 4.00 6.00 8.00 10.00 12.00 `4 2: C6 Sulfonate L3491 o-1 9 (PFHS) 073103A-1037 lOO-4 Sm (Mn, 2x3) 8.98 276429 01 -Aug-2003 22:27:X LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.67e6 Area A--- Time 2.00 4.00 6.00 8.00 lo:oo 12100 J 3: C8 Sulfonate L3491 o-1 9 (PFOS) 073103k1037 loo- Sm (Mn, 2x3) %- 01 -Aug-2003 22:27:X LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.82e6 Area , , , , I , , , , . / , Time 10.00 12.00 RW%en Research, 3058 Research Drive, State College, PA 16801 000130 Quantify Sample Report w Study No.:L34910, Set No .:073103A, Bxt.Date:07/31/03, Analyst:X.Risha Page 74 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\~sslynx\Fluoroch~ca~S.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LQ3SMS6\Masslynx\FluorochamicalaB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 -------------------_~ e-_---s--- --------e_ ------m- Name: 073103A-1037 Text : 4: PFOSA L3491 o-1 9 073103A-1037 lOO- Sm (Mn, 2x3) %- 01 -Aug-2003 22:27:5C LC/MS/MS #6 MRM of 4 Channels ES- 9.67 498 > 78 1.89e6 Area 0 "",~~`~,~~1~,~~~~,~~~~,~~`~/~~~~,~~~',~"~,~' 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 ."_~ ___." - -- --- ----------------------- ------_I_ Quantify Sarqple Report 'd Study No.:L34910, Set No .:073103A, m&.Dats:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSbIS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 75 Decatur BC BC 080103 Printed: ---- Sun Aug 03 07:19:29 2003 ----~------__---------____I_____----- Name: 0731031-1038 Text : --e-m -- I: C8 Acid (PFOA) L3491 o-1 7 I(173103A-1038 10 Sm (Mn, 2x3) 9.12 I1_ 310282: 01 *Aug-2003 223493403 LC/MS/MS #6 MRM of 4 Channels ES413>1 Be3769 Area v 2: C6 Sulfonate L3491 o-1 7 (PFHS) 073103A-1038 loo- Sm (Mn, 2x3) %- 3: C8 Sulfonate L3491 o-1 7 2.00 (PFOS) 073103A-1038 1 100-l I .-- i %- Sm (Mn, 2x3) 10.00 Time 12.00 01 -Aug-2003 mm401 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 1.69e6 Ares I Ir,.,,,,,.,, 10.00 / Time 12.00 Ol-Aug-2003 22:49:4d LCIMSIMS #6 MRM of 4 Channels ES499 > 99 3.82e6 Area ExygOa Research, 3058 Research Drive, State College, PA 16801 000/32 ---w-s- ---------- -----------------_----P-e- - QLmltify Sample Report hd Study No.: L34910, Set No .:#73103A, Ea&.Date:Q7/31/03, Analyet:R.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCIMSbiS6\Maaslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LQMSMS6\Masslynx\Fluorochemicals\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 76 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ----e-P -------------I------c---- ------p Name: 0731031-1038 Text : v----s-- -- 4: PFOSA L3491 o-1 7 073103A-1038 100- Sm (Mn, 2x3) %- 01 -Aug-2003 22:49:4( LCIMSNS #f MRM of 4 Channels ES- 9.90 498 > 7E 1.60eE Ares Exygen Research, 3058 Research Drive, State College, PA 16801 000133 ----- ------ -----__---______ ---v---P-- Quantify Sample Report &# Study No.:L34910, Set No .:073103X%, Ext.Dtite:O7/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMS~S6\Masslynx\BluotocbemicaleDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCHSMS6\Masslynx\Pluoroch~ca~s.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 -----------_ Page 77 Decatur BC BC 080103 Name: 073103A-1039 Text: : C8 Acid (PFOA) .3491 O-l 8, DF=i 00 )73103A-1039 10 Sm (Mn, 2x3) 9.12 77205 Ol-Aug-2003 23:11:32 LCNSIMS #6 MRM of 4 Channels ES413>369 4.47e5 Area U 2: c6 Sulfonate (PFHS) L3491 O-1 8, DF=lOO 073103A-1039 `OOJ Sm (Mn, 2x3) I_ Time 12.00 8.96 10133 01 -Aug-2003 23:11:32 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 6.07e4 Area 2.00 4.00 6.00 8.00 #: C8 Sulfonate (PFOS) 3491 O-l 8, DF=lOO )73103A-1039 Sm (Mn, 2x3) 01 -Aug-2003 23:11:32 LC/MS/MS #6 9.26 1407: MRM of 4 Channels ES499 > 99 8.21 e4 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 Enqgen Research, 3058 Research Drive, State College, PA. 16801 000134 ----- __------------- --- Quantify Sample Report bd Study No.: L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\2sal~\Fluorochemic\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 ---Page 78 Decatur BC BC 080103 Name: 073103A-1039 Text : 4: PFOSA L34910-18,DF=lOO 073103A-1039 lo9 Sm (Mn, 2x3) %- 0%Aug-2003 23:11:3: LC/MS/MS#~ MRM of 4 Channels ES- 192.199011 4986.5>1 7eEL O-;,,,,,,,,,,,,,,,,,,,,~~,,,,,,,,,,,,,,,~,,,~,,,,, I I I , I I 1 1Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000135 ---- ------_ ______________------------- !Juantify Sample Report 'kd Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\L~SMS6\Masslynx\FluarachemicaB\Decatur Sun Aug 03 07:11:59 2003 Printed: ------- Sun Aug 03 07:19:29 2003 ------------------------~~-------------_____ Name: 073103A-1040 Text : .: C8 Acid (PFOA) l(CO72503-5,500 rig/L Standard 373103A-1040 10 % 1 Sm (Mn, 2x3) 2.00 4.00 llw( 2: C6 Sulfonate (PFHS) XCO72503-5,500 rig/L Standard 9.12 156964 L I 8.00 073103A-1040 lOO- Sm (Mn, 2x3) 8.98 29038`-` %- --- --- Page 79 Decatur BC BC 080103 Ol-Aug-2003 23:33:24 LC/MS/MS #6 MRM of 4 Channels ES413s 369 9.33e5 Area 10.00 Time 12.00 01 -Aug-2003 23:33:24 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.78e5 Area 0 ~`~`,`~`~,"~~,`~",~`~~,~`~~,"`~,'~~~,~~~~~'..,,,.`~,.~`~l 2.00 4.00 6.00 : C8 Sulfonate (CO72503-5,500 (PFOS) rig/L Standard 373103A-1040 10 Sm (Mn, 2x3) 8.00 9.24 1934' I 10.00 Time 12.00 01 -Aug-2003 23:33:24 LCIMWMS #6 MRM of 4 Channels ES499 > 99 1.13e5 Area w I 2.00 4.00 6.00 8.00 Time 12.00 Oxygen Research, 3058 Research Drive, state College, PA 16801 000136 Quantify Sax@ple Report 14 Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 80 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~~S6\Masslynx\Fluoroch~cals.PRO\S~laDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: sun Aug 03 07:19:29 2003 ----------w--D---_- -w-m--- --------__ ----__---______ Name: Text: 073103A-3040 4: PFOSA XCO72503-5,500 rig/L Standard 073103A-1040 IOO- Sm (Mn, 2x3) . %- :. ,. ., f 01 -Aug-2003 23:33:24 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 3.86e5 Area Oxygen Reiearch, 3058 Research Drive, State Collage, PA 16801 000137 Quantify Sample Report 'ru/ Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~~S6\Massl~\Fluoroch~cals.PRO\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\L(3MSMS6\Masslynx\FluorochsmicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1041 Text : Page 81 Decatur BC BC 080103 L3491 o-25 . 073103A-1041 Sm (Mn, 2x3) 01 -Aug-2003 23:55:0 LC/MS/MS #6 MRM of 4 Channels ES-4 413> 369 1.72e4 Area 9.13 . 652 $4 2: C6 Sulfonate L3491 o-25 2.00 (PFHS) 073103A-1041 Sm (Mn, 2x3) I 1 0 ~~~.,~,.~,~..,,...~,~,.~,,,~~,~~~,,~.~~,,,,,,,.,,,,,~,,,,.,,Time 2.00 4.00 6.00 3: C8 Sulfonate L3491 O-25 (PFOS) 073103A-1041 I lob I -1 Sm (Mn, 2x3) %- O'.,.,,,,,,,,.,,,,,..,,~.,,,,,,,,,,,,,,,,,..,~,,,,,,,,.,,,,,,,Time 2.00 4.00 6.00 10.00 12.00 01 -Aug-2003 23:55:08 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 738 I 8.00 10.00 12.00 0%Aug-2003 23:55:08 LC/MS/MS #6 MRM of 4 Channels ES- 9.22 499 > 99 3161 2.21e3 Area 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000138 Quantify Sauqle Report '4 Study No.: L34910, Set No.: 073303A, Ext.Date:O7/31/03, Analyst:K.Risha Sample Ilist: Last modified: Method: Last modified: Job Code: P:\Data\LCHSMS6\Masslynx\Fluorochemicbls.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 P&ted: Sun Aug 03 07:19:29 2003 Page 82 Decatur BC BC 080103 Name: 0731031-1041 Text : 4: PFOSA L3491 o-25 073103A-1041 Sm (Mn, 2x3) I 1-Aug-2003 23:55:08 LC/MS/MS #6 MRM of 4 Channels ES498 > 78 1.12e3 ExyOen Research, 3058 Research Drive, State College, PA 16801 000139 Quantify Saxnple Report & Study No.:L34910, Set No .:073l.O3A. Ea&.Date:07/31/03, Analyst:K.Risha Page 03 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\U3H~S6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslyax\Pluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 ---------_------_----------------~-----------___--- N-2 073103x&-I.042 Text : 1: C8 Acid (PFOA) L3491 O-26 073103A-1042 10 Sm (Mn, 2x3) . . 02-Aug-2003 00:16:59 LC/MS/MS #6 MRM of 4 Channels ES- 413>369 1.93e4 Area 2.00 4.00 6.00 8.00 10.00 12.00 %& 2: C6 Sulfonate L3491 O-26 (PFHS) 02-Aug-2003 00:16:59 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate L3491 O-26 (PFOS) 073103A-1042 lOO- Sm (Mn, 2x3) 02-Aug-2003 00:16:5$ LC/MS/MS #E MRM of 4 Channels ES- 9.27 499 > 9s 1.55e? 0 ,,,,,,,,,,,,,,,,,~,,,,,,,,,~,,~~,,,,,,,,,,~,,,,,~,,,,,,,,,,,Tjme `1113' 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000140 Quantify Sample Report `ha& Study No .:L34910, Set No.:O731031, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCNSMS6\Masslyax\Fluoroch~calS.PRO\S~leDB\O73lO3A Sun Aug 03 07x08:13 2003 P:\Data\LC3rISMS6\Essl~\Fluorochemic\Met~B\Decatur Sun hug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 84 Decatur BC BC 080103 Name: Text: 0731031-1042 4: PFOSA L3491 O-26 073103A-1042 100- Sm (Mn, 2x3) %- 02-Aug-2003 00:16:5! LC/MS/MS #( MRM of 4 Channels ES- 9.90 498 > 7t 4.77e: Are: Exygen Research, 3058 Research Drive, State College, PA 16601 000141 Quantify Swle Rsport Study No.: L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Ssrnpls List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\bs8l~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\~sslynx\FluorochemicB\Decatur Sun hug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 ------~------------------I_______- Name: 073103A-1043 Text : ---__-- 1: CB Acid L3491 o-22 (PFOA) 073103A-1043 Sm (Mn, 2x3) o1LJ-; ,,,, ~,,,,,,, s>,,7,-,,, ;,,c,,,-,M, 9.15 608 Page 85 Decatur BC BC 080103 ---------- 02-Aug-2003 00:38:46 LCRvlSJMS #6 MRM of 4 Channels ES413s 369 2.10e4 Area 2.00 2: C6 Sulfonate (PFHS) IIL3491 o-22 A-l 043 Sm (Mn, 2x3) A0.89 0.13 1 AA1 7An-m 4.00 6.00 -- E r4.c Time 8.00 10.00 12.00 \ 020Aug-2003 00:38:44 G9.53 0.31 0.84 LC/MS/MS #6 MRM of 4 Channels ES- 0 "","","",~"`,"","","","`~,"","","","", Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate L3491 o-22 (PFOS) 073103A-1043 Sm (Mn, 2x3) 02-Aug-2003 00:38:46 LC/MS/MS #6 MRM of 4 Channels ES- Exygan Research, 3058 Research Drive, State College, PA 16801 000142 Quantify Sample Report q& Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~~S6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCM~S6\Massl~\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: ----------------_ Sun Aug 03 07:19:29 2003 --_-------------------- Name: 073103A-1043 Text: 4: PFOSA L3491 o-22 073103A-1043 Sm (Mn, 2x3) Page 86 Decatur BC BC 080103 I Aug-2003 00:38:41 LCIMSIMS #l MRM of 4 Channels ES- 2.00 4.00 6.00 8.00 10.00 12.00 -Glen Research, 3058 Research Drive, State Colleps, PA 3.6801 000143 Quantify Sample Report &# Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sappls List: Last modified: Method: Last modified: Job Code: P:\Data\L~SWS6\~sslynx\8luoroch~cals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\~sslynx\FluorochamicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun hug 03 07:19:29 2003 Page 87 Decatur BC BC 080103 Name: 073103A-1044 Text : 1: C8 Acid (PFOA) L3491 O-23 I073103A-1044 IO Sm (Mn, 2x3) 02-Aug-2- 003 01:00:38/ LC/MS/MS #6 MRM of 4 Channels ES413>369 2.09e5 Area L W 2: C6 Sulfonate 13491 O-23 (PFHS) 073103A-1044 Sm (Mn, 2x3) Time 12.00 02-Aug-2003 01:00:38 LCBMMS #6 MRM of 4 Channels ES399 > 80 4.02e4 Area I: C8 Sulfonate -3491 O-23 2.00 (PFOS) `OOJ 373103A-1044 Sm (Mn, 2x3) 10.00 Time 12.00 396.2941 L--, 02-Aug-2003 01:00:3d LC/MS/MS #6 MRM of 4 Channels ES- 499 > 99 2.2A1reea4 0 ~`~`,~`,,`.,`,,,,,,,,,`,,".,`,,,,,"',,,,'f Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Rosearch Drive, State college, PA 16801 000144 ---_-___--__--------- ---w-e--- --- Quantify Sauple Report 14 Study No .:L34910, Set No.:073103A, Eact.Date:07/31/03, Analyst:K.Risha Page 88 Sanple List: Last modified: Method: Last modified: Job Code: P:\Data\L(SMSMS6\~sslynx\Fluoroch~cals.P~\S~leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 08OiO3 Printed: Sun Aug 03 07:19:29 2003 --------------------------- Name: 073103A-I.044 Text : ----------------------- : PFOSA -3491 O-23 173103A-1044 Sm (Mn, 2x3) 104 . %4o'~~~~,`~~`,~`~`r'~~~,~~~`,~~~~,"~'I~"',"~'r" 2.00 4.00 6.00 02-Aug-2003 01:00:31 LC/MS/MS #E MRM of 4 Channels ES- 9.8s 3 1214 498 > 7E 6.45e4 Aree Time 8.00 W Exygen Research, 3058 Research Drive,.Stats College, PA 16801 000145 ------- - ---_---- ------------_ Quantify Sample Report b# Study No. : L34910, Set No .:073103A, Ext.Dats:O7/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\MasalyPx\Fluoroch~cala.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\M3MSMS6\Masslynx\Fluorocbamicals\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 -Page a9 Decatur BC BC 080103 Name: Text: 073103A-1045 1.: C8 Acid (PFOA) -3491 O-24, DF=lOO 173103A-1045 10 1 %$ Sm (Mn, 2x3) 02-Aug-2003 01:22:1 C LC/MS/MS #6 MRM of 4 Channels ES413>369 2.06e5 Area !: C6 Sulfonate (PFHS) L3491 O-24, DF=lOO 073103A-1045 10 Sm (Mn, 2x3) Time 12.00 02-Aug-2003 01:22:1 tj LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 6002 3.39e4 Area ! w Time / 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) L3491 O-24, DF=lOO 02-Aug-2003 01:22: 1C LC/MS/MS #6 073103A-1045 I "`1lf-ln, I 1 Sm (.Mn, 2x31, MRM of 4 Channels ES- 9.25 499 > 99 3853 2.26e4 Area L Time 2.00 4.00 6.00 8.00 10.00 12.00 Exyoen Research, 3058 Research Drive, State college, PA 16801 000146 Quantify Sample Report I& Study No.:L34910, Set No .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 90 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~SPIS6\Mssl~\Fluoroch~cals.P~O\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCblSMS6\Masslynx\Fluorochemical\Decatur Sun Aug 03 07:11:59 2003 Decatur BC EC 080103 Printed: -----__-_ Sun Aug 03 07:19:29 3003 -------- ------- __-----____ -w--m-- ---- Name: 0731031-1045 Text : 4: PFOSA IL3491 O-24, DF=lOO 073103A-1045 1nl-L Sm (Mn, 2x3) 02-Aug-2003 01:22:1 C/ LCAWMS #6 MRM of 4 Channels ES- 9.89 498 > 78 8.50e4 Area r , , , r , , 1Time 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000147 Quantify Sample Report \IJ Study No.:L34910, Set No.: 0'73103A, Ext.Date:07/31/03, Analyst:K.Risha Szizuple List: Last modified: Method: Last modified: Job Code: P:\Data\L~~6\Masslynx\Fluorochemicals.PRO\S~leDB\O73lO3A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed; Sun Aug 03 07:19:29 2003 Page 91 Decatur BC BC 080103 Name: 0731031-1046 Text : 1: C8 Acid (PFOA) XCO72503-6,lOOO rig/L Standard 073103A-1046 10 Sm (Mn, 2x3) 3 9.13 322068 02-Aug-2003 01:43:42] LC/MS/MS #6 MRM of 4 Channels ES413>369 1.93e6 Area 2.00 4.00 6.00 8.00 10.00 12.00 !: C6 Sulfonate XC072503-6,1000 (PFHS) rig/L Standard 073103A-1046 loo- Sm (Mn, 2x3) %- 02-Aug-2003 01:43:4: LCWYMS #f MRM of 4 Channels ES- 8.98 399 > 8C 3.71 e5 Area 0 `,","","","","","","","", , ~ , , , , , , , , , ,Time 2.00 4.00 6.00 8.00 10.00 12.00 I: C8 Sulfonate YCO72503-6,1000 (PFOS) rig/L Standard 373103A-1046 10 9 Sm (Mn, 2x3) % i 02-Aug-2003 01:43:42/ LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 3566! 2.09e5 Area `~1 Time 2.00 4.00 6.00 8.00 10.00 12.00 J RXXJen Research, 3058 Research Drive, State College, pA 16801 000148 Quantify Sample Report &if Study No .:L34910, Set No.:073103A, Bxt.Dats:07/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.~RO\S~leD~\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\M~t~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 92 Decatur BC BC 080103 Name: 0731034-1046 Text : 4: PFOSA XCO72503-6,lOOO rig/L Standard 073103A-1046 Sm (Mn, 2x3) . 100- %- 02-Aug-2003 01:43:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498>78 7.38e5 Area Exygen Research, 3058 Research Drive, State College, PA 16801 oool.+!s Spowx Study No: Fkygecn Study No: Adytr: looa Monitored: site: NA I34910 PFOA 413 -> 369 Decaau Baker's Geek RAW DATA REPORT Limit or Quaacicarion: Iojection Volum: Mati Sample Volum: Fd Volume: 50 ppc 15 IJwaler 40.0 mL 5.0 mL 5s No: AdYSU Insmuncnt Pabaclion Aonlyzad Typ: Dale: on: 073103AR Karen Risba LClMSlhIS unit d 6 07/31x)3 08/03-04!03 kYP= ID xCO72503-0 xco72503- I xco72503-2 xc072503-3 XCO72503-4 xCo72503-5 XCO725+33-6 l34910.1 Spk C L34910-12Spk E W4910-16 Spk F xco72503-1 u49mI U4910-I Rep u49 IO-4 u4910-2 XcO72503-2 w4910-6 W910-6 Rep w4910-9 l349la-7 xco72503-3 w4910.12 L34910-I2 Rep w4910.15 w910.13 xc0m03-4 U4910-16 W49lC-16 Rep w4910-19 w4910-17 xco72503-5 W4910-16 W4910-16 Rep w4910.19 w910-17 xCa71003-6 Spoasor m BC2 SW-@4 BCZ SW06 outfali lo River SW-U BC2 SW.04 BC2 SW-04 BQ SW-04 Dup EC2 SW-04 Low Spk BC2 SW-05 BCZ SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk Bcz SW-06 BC2 SW.06 BC2 SW-06 Dup BC2 SW-06 Low Spk ChItfall to River SW-zi outfall to River SW-25 oudall to River SW-U Dup Chtfdl to River SW-2S Low Spk Chidail to River SW-25 Chtfall to River SW-25 oudall to River SW-25 Dop Outfall to River SW-25 Low Spk sccl SUItpiS RUP cont. Code No. (PPO wI^ 073103AR-101 0 cs 073103AR-102 25 cs 073103AR-103 50 cs 073103AR.104 loo cs 073103AR.105 250 cs 073103AR-106 500 cs 073103AR-107 low LF 073103AR-108 LF 073103.&R-109 LF 073103AR.110 cs 073103AR-111 25 S 073103AR-112 S 073103AR-113 S 073103.&R-1 14 FF 073103AR-115 cs 0731MAR-116 50 S 073103AR-117 S 073103AR-1 I8 S 073103AR-119 FF 073103AR-120 cs 073103AR-121 loo S 073103AR-122 S 073103AR-123 -. S 073103AR-124 FF 073103AR.I25 cs 073103AR-126 250 S 073103AR-I27 S 073103AR.128 S 073103AR-129 FF 073103AR.130 cs 073103AR-131 SW S 073103AR-132 S 073103AR-133 * s 073103AR-134 ff 073103AR.135 cs 073103AR-136 loo0 Aaalytc Found (ppt) = (peak arep - intercept) I slope x DF Recovery (%) = [adyte found (ppthnalyte found in control (ppc)) x 100 MWt added cm) cilution Factor lcul Km loo 10 10 10 10 10 10 10 10 20 20 20 20 100 100 ml loo 20 20 2n 20 Peti Area 794 147.21 27994 54680 128556 264862 516215 SO564 92540 114710 14631 216041 216268 131415 142555 29284 40498 39782 81652 112700 55667 30891 I 315651 29773s 354730 127797 82515 83658 75424 78536 271906 380900 391789 364595 362898 477931 Aodyte Foond (Ppt, Amounr Ad&d (pwt) R.XOVU-j (a) .* 17800 22100 4210 4210 2540 27W .* I* 1560 2170 12100 12300 11fxlO 13900 I5800 wxa I4um lSw0 l * . . l . .* 5ooa mm mm 100 100 loo loo loo 114 126 -1450+ 1579A+ 1800+ -Boo+ i5&U&W8 : Lioepr (11x weigbtod) Iomccp~ = 220217 Slap = 508.394 Cod. Of Lkt. = 0.99621 I CS = Calibrationstandard LF I lab fwtitied saqde c = control sample FF = Field foftified sample s = Sample LCS = Labaatay Cootml spikm CK = Check Standard ND = Not dctixted = Respoue bxwcen 0 and 25 ppc NQ = NWquantifiable = Responsebetween 25 ppt and LOQ (50 ppt) Sprwishcet prepared by: l *Sampk WBIanalyzed with reveal dilution factorsin order to rcommcdatc all compounds. Th appropriate resulu M reported. %unplc was cormrsd using the data found in sot 073103A. +Sample residue si8rtif~aotIy exceeda du apiking level; thmfw. an accurate recovery cannot ix calculated. 000150 Spoo~v Study No: ibygan Study No: Adyte: Iom Monitored: Site: NA U4910 PFHS 399.>so Decaha Baker's Creek RAW DATA REPORT Limit of Q!lantitation: hjecdon Vohm: Maaix Svnple Volum: Final Volume: 50 PPt l5rr War 40.0 OIL 5.0 mL Sot No: AMlys1: InsmmcalTypc: Enaacfion Dam: Analyzed on: 073103AR Karen Rkha LcIMslMs unit w 6 o7i3iiv3 oam3-o4m3 xc0725030 xco72503-I xco72503-2 XCD72503-3 xco72503-4 xco72503-s xco72503-6 W4910-1 Spk C 04910-12 Spk E U4910-16Spk F xc072.503- I U4910.1 U4910-1 Rep I349 lo-4 u4910-2 XCO72503-2 u4910-6 U4910-6 Rep L34910-9 w4910-7 xc07.2503-3 w49w12 U4910.12 Rep u4910-I5 w4910-13 xco72503-4 U4910-16 U4910-16Rcp L34910-19 w910-17 xco72503-s U4910-16 U4910.16 Rep U4910-19 u4910-17 xc071003-6 spolww UJ BU SW-04 BU SW-06 outfall to River SW-25 BQ SW-04 BQ SW-04 BU SW-04 Dup EC2 SW-04 Low Spk BU SW-05 BC.? SW-05 BC2 SW-05 Dup BCZ SW.05 Low Spk BCZ SW-06 BC2 SW-06 BQ SW-06 Dup BG! SW-06 Low Spk chdnll to River SW-Z OutMl to River SW-25 axfaIl 10 River SW-23 Dup Outfall to River SW-U Low Spk Gutfnll to River SW-25 cwfau at River SW-23 outfall to River SW-25 tip Cutfail to River SW-25 Low Spk SOlpie Code cs cs cs cs cs cs CS LF LF LF cs s S S FF cs S s S ff c-s S s S FF cs S S S FF cs S S S FF cs RUll NO. 073103AR-101 073 103AR-102 073103AR-103 073 103AR.1w 073103AR-105 0?3103AR-106 073103AR-107 073103AR.I08 073103AR.109 073lO3AR-1 IO 073103AR.I I I 073103AR-112 073103AR.113 073103AR-I14 073103AR-115 073103AR-116 073103AR-117 073103AR-11s 073 103AR-I 19 073103AR-120 073103AR-121 073 103AR-122 073103AR-123 073103AR-12.4 073103AK125 073103AR-126 073103AR.127 073103AR-128 073103AR-129 073imAR.130 073103AR-131 073103AR.132 073103AR-133 0731mAR-134 073103Ah135 073103AR.136 A~Iylc Found (ppt) = (peak MP - ialercept) / slope x DF Recovuy (%) = [anaiytc found (ppthnllycc found in conaol (ppt)] x 100 ammat added (ppt) std. COOC. @PO 0 25 50 loo 250 Dilulian Facrm 100 100 100 10 IO 10 10 10 10 10 10 20 20 20 20 100 IO0 100 100 20 20 20 7.0 peak Area 0 2074 4718 9231 21488 43819 87115 S566 10314 10701 2324 9381 10152 6122 7036 4266 1526 1565 3729 602.3 9486 26169 27209 25364 30673 21551 6872 6261 6156 6030 45496 33004 30633 29219 2ab60 80818 AOalytC Found (pet) Amount Ad&d (PPO Recovery (`k) I. 11800 127lIO I. . . .* I. l * *. *. I. bob0 6300 5a70 7110 ** l * l . . . 7bb0 7100 6770 6640 SIandard : Liocar (Ih rcighrcd) Intenpt = 218.845 Slope = 8S.6521 Cccf. Of Dcr - 0.99b560 CS - Calibcrtionswuiard LF I Lnb fortified sample c - commnl sampk FF = Field fm-tifiid sample s = Sample LCS = I;lbaatory Cona Spika CK = Clwck Staodud ND = Not detected i: Rwponr between 0 and 25 ppt NQ = Not quantifiable I Rwponse between 25 ppt and WQ (50 ppt) Spread&cat prepared by: 000151 Sp~nscrr Study No: ~y&o Study No: Analyte: ions Monitmcd: Site: NA I24910 PFOS 499 -a 99 Dscafur Raker's Creek RAW DATA REPORT Limit of Qusntitation: Injection VoIume: MOUiX Smplo Volume: Fi v01umc: 50 ppc 15 6 w*lcr do.0 mL 10 mL Sat No: AdySt Instmmcnt Bxtr~don Amfyazd Type: Date: 08: 073103AR Karen Risk LUMSIMS 07txn3 0&03-04803 Unit Y 6 XC072503-0 xc072503- I xc072503.2 xco72503.3 xca7m3-4 xco72503-5 XCO72503d W4910-1 Spk C L34910-12 Spk E L34910-16 Spk F xco72503-1 w4910-1 u4910-I I&p w4910-4 w4910-2 XC072503-2 W4910-6 W4910-6 Rep L34910-9 u4910-7 XC072503-3 W49lD-12 w4910.12 Rep w4910-15 w4910-13 xco72503-4 w4910-16 l34910-16 Rep w4910-19 u4910-17 XCO725M-5 W491&16 W910-16 Rep L34910-19 Ud910-17 XCO71003d SpSCU w EC2 SW-04 BU SW-06 oudal lo River SW-25 BQ SW-&i BU SW-04 BC2 SW-04 Dup EC2 SW-04 Low Spk BQ SW-OS Bc2 SW-OS BC2 SW-05 Dup EC'2 SW-05 Low Spk BC2 SW.06 BCZ SW-Q6 BU SW-06 Dttp BC2 SW-06 Law Spk fhdtdl 10 River SW-25 oudnl to Ftivm SW-z.5 oldl to Rivu SW-U Dup OIldell Ia River SW-25 law spt Oudall to River SW-25 cwfall to River SW-25 Dudal to River SW-25 IxIp Chdal to River SW-25 Low Spt Sample Code cs cs cs cs cs cs cs LF LF LF cs S S S PF cs S S S FP cs S S S FP cs S S S FF cs s S S .FP cs SKL Run chx. NO. (ppt) 073103AR-101 0 073103AR-102 25 073103AR.103 SO 073103AR.104 loo 073103AR-105 250 073103AR-106 500 073103AR.107 Iow 073103AR-108 073103AR-109 073103.&R-I 10 073103AR.Ill 25 073103AR.112 073103AR-113 073103AR-114 073103AR-II5 073103AR-II6 SO 073103AR-117 073 103AR-118 073103AR-119 073103AR-120 073103AR-121 1W 073103AR-122 073103AR.123 073103AR-I24 -. 073103AR-125 073103AR-126 250 073103AR-127 073103AR-128 073103AR-129 073103AR-I30 073103AR-131 500 073103AR-132 073103AR-133 073103AR-134 oniomrb135 073103AR-136 loo0 Adyte Recovery Fouod @pt) = (@ (57) = area - intctcept) (malyk found I slap x DF (ppt)-mrdy(c found in conool pmarnt added (ppt) (ppt)] 1 100 Dilution F- 1W loo 100 10 10 10 IO 10 10 10 IO `20 20 20 20 loo ml 1Gu loo 20 20 20 20 PC& Area 0 1481 2986 Sloe 13285 28978 53617 9428 171% 22403 1473 61501 59888 44921 37560 2882 9224 8484 23649 29284 bw4 64499 64047 646s6 77839 13289 17094 17264 16861 16123 28469 81862 84263 822Ql 79698 53157 CS = Calibratioartmdud c I Conud sample s = sample LF a Lah fortified m&c IT = Fmld fwtified wmple LCS - hbwamy Cmtml spike CK = (hck Stmdiud ND = Ncr detected = Rupopre bctwcen 0 and 25 ppt NQ 9 Not qwtifiablc I Response between 25 ppt and L0Q (50 ppc) **Sample ~%Samph `Sample YSample +!hmplc was analyzed with several dilution fvtorr in order to lffomtt~bt(I WPI comeed uiag the data found in set 080603A rquim lbkr dilutioa See data act OUl603A requires a higkr spiking level. Sea data set 080603A. nriduc rignificamly exceeda the spiking level; thercforc. aa acarak all cotttpOUad%. lb sppopriacC ~CCOVC~J CU~MI be calculated. rmdta (LIa nponcd. MY= Found (PP0 Amount Added (PPU Recovery W) 171M) 5wQ 112* AA mco 5ooo * . 82.50 68% 100 -4610% 1670 IJU) 4330 5370 100 37co+ . l l I loo 31200 3 1soo 308txl 29400 100 -1800+ 1. . . . . *. lD0 S(andard lnterxpt Slope Cat Of C-a : tinerr (Ih = 152.345 P 34.2582 ii 0.998217 weighted) 000152 Sponsor Study No: Exygcn Study No: Adytc: Ions MoniWred: Site: NA L34910 FOSA 490 -=- 78 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitxion: Injection Volume: Math: Sample Volume: Final Volume: so ppl 1s )IL Wstcr 40.0 mL 5.0 mL Set No: Analyst: lnstzumcnl Extractian Analyzed Type: Date: on: 073103AR Karen Rirha LG?&&!S Unit # 6 0713 II03 oa/o3-04103 Exygen ID xc0725034 XCO72503-I XCO72503.2 xco72503-3 XCO72503-4 XCO72503-5 xc012s034 L34910-1 SpkC 134910-12 SpkE L34910-16 SpkF XCO72503-I w4910-I L34910-1 Rep L34910-4 L34910-2 xco72503-2 L34910-6 L34910-6 Rep L34910.9 L34910-7 XCO72503-3 L349IO.12 134910-12 Rep L34910-15 L34910.13 XCO72503-4 L34910.16 L349lO-16Rep L34910-19 "4910.I7 XCO72503-5 L34910-16 L34910-16 Rep L34910-19 L349lO-17 xc071003-6 Sponsor ID BCZ SW-04 BC2 SW-06 outfall to River SW-25 EC2 SW-04 K-2 SW-04 BC2 SW-04 Dup EC2 SW-04 Low Spk BC2 SW-05 BC2 SW-05 BC2 SW-05 Dup EC2 SW-OS Low Spk BC2 SW-06 BCZ SW-06 8'22 SW-06 Dup BCZ SW-06 Low Spk Outfall w River SW-2s Outfall W River SW-25 Outfall w River SW-25 Dup OddI w River SW-25 Low Spk outfall to River SW-25 Outfsll w River SW-25 Outfall w River SW-25 Dup Outfall w River SW-25 Low Spk Sample Code cs cs cs cs cs cs cs LF LF LF cs S S S FF cs S S S FF cs S S S 5-F cs S S S FF cs S S S FF cs Atnlyte Rccavcry Found (ppt) = (peak (%) - arcs _ inwtcept) / slope x DF fsnalytc found (ppt)-snalyte smotmt found in control added (ppt) Run NO. 073103AlG101 073103,4&102 073103AR-103 073103AR.104 073103AR-105 073 103AR-IO.5 073103AR-107 073103AR-108 073 103AR-109 073103AR.II0 073103AR-Ill 073103AR-I I2 073103AR-113 073103AR-I 14 073103AR-t1s 073103AR-116 073103AR-II7 073103AR-I I8 073103.x+-I 19 073103AR.120 073103AR-121 073103AR-122 073103AR-I23 073103AR.124 073103AR.12$ 073 103AR-126 073103AR-127 073 103AR-128 073103AR-129 073103AR-t30 073103AR.I31 0731'33AR.132 073103AR-133 073103AR-134 073103AR-135 073103AR-136 @tJ x IO0 Std. COUC. @pt) 0 25 SO IW 250 So0 1000 25 50 100 250 SW 1000 CS = Cslibrstion c = Controlssmpk s = s4mpk standard CK = Check Sundsrd ND - Nat detected NQ - Not qustttitisble LF = Lab fortiftcd FF - Field fortiticd LCS = Lsborzwry sample sample Control Spike - Rcsponsc between 0 and 25 ppt = Response between 25 ppt snd LOQ (50 ppt) l *Sampk +bmpk ~1s analyzed with several dilution facwrs in order w rccommodate residue significantly excccdr the spiking Icvcl; therefore, u1 sccuntc all compottttds. The spproptia(e recovery cannot be calculated. Dilution Facwr 100 100 I00 IO 10 IO IO 10 10 IO 10 20 20 20 20 loo loo loo 100 20 20 20 20 Peak ~rca 0 5175 10303 207 IV 48632 104085 196920 13039 16006 18398 5382 27920 27505 20497 16630 10890 3460 3402 8876 11595 21221 2449s 23261 25908 25736 49195 6718 6206 6506 5831 to2292 32659 31916 32869 26761 190680 Analytc Found (ppt) Amount Added (PPt) Recovery (%) .* 5000 . . 5000 4. 5000 1390 1370 . . l * loo l . ** l . . . I00 2430 2300 2570 2550 1w 120 l . l * l * 6. loo 3260 3180 3280 2660 loo -6CO+ Staadsrd m lotcmpt Slope Gxf. Of Der : Linear (I/x - 61 1.080 = 196.925 - 0.998392 weighted) Sprcrdshcct prcprnd by: results are reported 000153 Masslynx -Sample List Sample List: C:\MASSLYNX\Fluoroch Printed: Sun Aug 03 08:19:25 2003 Is.PRO\SampleD8\073103AR i Decatur BC.SPL Exygen STUDY NO- w Page 1 Page Position: (1 I 1) Vial File Name LIMS ID Client JD Sample Description Matrix SampleType Conc(ng/L) Cone 6 Cone C Test ID DF 41 073103AR-101 -- --- : 42 073103AR-102 - - 3 43 073103AR-103 - - 4 44 073103AR-104 -- 45 073103AR-105 - -- 073103AR-106 - -- XCO72503-0.0 rig/L Standard ;5 XCO72503- I,25 rig/L Standard 50 XCO72503-2,50 rig/L Standard 100 XCO72503-3. 100 rig/L Standard -_ Standard --- Standard --- Standard --- Standard - _- 0 1 - -- 0 - _- 0 : - -- 0 XCO72503-4. 250 nglL Standard XCO72503-5, 500 nglL Standard --- Standard -- Standard Ei _- -- 0 : - -- 1 7 1; 073103AR-107 - -- XCO725W6,1000 rig/L Standard -- Standard 1000 - -- x 1 8 51 073103AR-108 - -- L34910-1 Spk C, 5000 q/L. OF=100 --- 5000 - _-- 100 365 j 9 52 073103AR-109 - - L34910-12 Spk E. 5000 q/L, DF=lOO -- :: 5000 - -- 00 100 / 10 53 073103AR-110 - -- L34910-16 Spk F. 5000 I-@., DF=lOO --- QC 5000 - -- 0 100 42 073103AR-111 - -- XCO72503-1.25 naiL Standard -- Standard 25 - -- 0 1 54 073103AR-112 - -- L34910-1, Di=lO" -- Analyie - I_ -- 55 073103AR-113 -- -_ L34910-i Rep, OF=10 -- Analyie ___ - _- 8 :: 56 073103AR-114 -- -- L34910-4. DF=lO -- Analyte - _I 0 IO 073103AR-115 --- - L34910-2: DF=lO - QC Go - - 10 073103AR-116 -- - XCO72503-2, 50 nglL Standard - Standard 50 - _- 8 1 17 073103AR-117 -- - L34910-6, DF=lO - Analyie -- - --- 0 10 073103AR-118 --- L34910-6 Rep, OF=10 - Analyte -- - --- 0 10 :: 073103AR-119 - - L34910-9, DF=lO - Analyie - - 0 10 20 073103AR-120 -- - L34910-7, DF=lO - QC Gd -__ 0 10 21 073103AR-121 - - XCO72!%3-3,100 nglL Standard - Standard 100 -- - 0 1 22 073103AR-122 - me L34910-12. DF=20 - Analyte -__ --- -- 0 20 073103AR-123 -- - L34910-12.Rep, OF=20 - Analyte - -- -- 0 20 t: 073103AR-124 - -- L34910-15, DF=20 - Analyte -_ -- -_- 25 073103AR-125 -- - L34910-13,DF=20 - QC - -- 0" si 45 073103AR-126 - - XCO72503-4,250 rig/L Standard - Standard El - --- 1 66 073103AR-127 - - L34910-16, DF=lOO - Analyte --- - --- x 100 28 67 073103AR-128 - L34910-16 Ret). DF=lOO - Analyte --- _- --- 100 29 68 073103AR-129 - L34910-19, Di=lOO - Analyte --_ - -- 0" 100 30 69 073103AR-130 - - L34910-17. DF=lDO - QC 100 - -- 0 loo 31 46 073103AR-131 - XCO72503%, 5001-&L Standard - Standard 500 - --- 0 1 70 073103AR-132 - -- L34910-16, DF=PO - Analyte --. - -- 335 71 073103AR-133 - -- L3491O-16 Rep, OF=20 - Analyte --- - _-- : ;: 34 72 OMl03AR-134 -- -- L34910-19,OF=20 - Analyte ..-- - --- 0 20 73 073103AR-135 -- -- L34910-17, DF=PO - QC 100 - -_ 20 47 073103AR-136 -- --- XCO72503-6, 1000 nglL Standard -- Standard 1000 - -- 8 1 Masslynx - Sample List MS Method HPLC Method 1 C6 03 SULF 03 ACID PFOSA 2 C6 C8 SULF C8 ACID PFOSA 3 C6 C8 SULF C8 ACID PFOSA 4 C6 C8 SULF C8 AC10 PFOSA C6 C8 SULF C8 ACID PFOSA 65 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 AC10 PFOSA x C6 C8 SULF C8 ACIO PFOSA 9 C6 C8 SULF C8 ACIO PFOSA C6 C8 SULF C8 ACID PFOSA :: C6 C8 SULF C8 ACID PFOSA 12 C6 C8 SULF C8 ACID PFOSA 13 C6 C8 SULF C8 ACID PFOSA 14 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA :i C6 C8 SULF C8 ACID PFOSA 17 C6 C8 SULF C8 ACID PFOSA la C6 C8 SULF C8 ACID PFOSA 19 C6 C8 SULF C8 ACID PFOSA 20 C6 C8 SULF C8 ACID PFOSA CS C8 SULF 03 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 CB SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA 27 C6 Cfl SULF Cl3 ACID PFOSA 28 C6 C8 SULF C8 ACID PFOSA 29 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA 3: C6 C8 SULF C8 ACID PFOSA 32 C6 C8 SULF C8 ACID PFOSA C6 Cl3 SULF 03 AC10 PFOSA if C6 C8 SULF C8 ACID PFOSA 35 C6 C8 SULF C8 ACID PFOSA 36 C6 C8 SULF CB ACID PFOSA pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs wa?er pfbs waler pfbs water ptbs water pfbs water pfbs water pfbs water pfbs water pfbs water $2 z:z pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water MS Tune File Fluomchems Fluorocherns Fluomchems Fluomchems Fluomchems Fluorochems Fluorochems Fluorochems Fluomchems Fluorochems Fluarochems Fluomchems Fluomchems Fluorochems Fiuorochems Fluorochems Fluorochems Fluomchems Fluorochems Fluomchems Fluorochems Ftuorochems Fluorochems Fluorpchems Fluorochems Fluomchems Fluorochems Fluorochems Fluorochems Fluorochems Fluomchems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Inj.Votume ::zz :2 15 :: 15 15 15 15 15 15 15 15 :z 15 15 15 15 :: 15 ii 15 15 15 15 15 15 ;: _-(&%I) Exygen STUDY NO* ----- Page 2 Page Position: (2, 1) LC/MS/M.S SYSTEM AND OPERATING CONDITIONS Snonsor Protocol No: NA Exvgen Studv No: L34910 Instrument: Micromass Quattro Ultima (LUMS/MS Unit #6) Computer: COMPAQ Professional Workstation Al?200 Software: Microsoft Windows NT: Version 4 Build 138 1: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8,5 cm x 2.1 mm i.d. x 4 l.r (Exygen ID: 74A) (JONESCHROMATOGR.APHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by :j!p!o@3 V _, .I_^___ . ^-."."--.*""- 000156 ____ __-..- .--- w Scanning Method Report Method: Last Modified: C:\MASSLYNX\FXUOROCHEMICALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 Page 1 C8 SULF C8 ACID PFOSA Printed: Sun Aug 03 08:20:40 2003 Solvent Delay ( mins ) : 0.00 &%3103 u Analog Function Channel : 1 4 : Unused MEW of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Sets ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 1 399.00 80.00 2 413.00 369.00 3 498.00 10.00 4 499.00 99.00 0.03 0.00 0.00 12.00 1 Dwell 0.20 0.20 0.20 0.20 (Sees) Co11 Energy 35 10 30 40 (eV 1 Cone ( v ) 50 LO 50 30 000157 Method Report Method File: Last Modified: 'Ird Printed: C~\&fASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs Sunday, August 03, 2003 08:06:07 Sunday, August 03, 2003 08:20:45 HP1100 LC Pump Initial Conditions Solvents A% 90.0 B% 10.0 C% 0.0 D% 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Oven Temperature Right(OC) 0.300 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time A% B% C% D% 0.00 90.0 10.0 0.0 0.0 2.00 90.0 10.0 0.0 0.0 5.00 10.0 90.0 0.0 0.0 9.00 10.0 90.0 0.0 0.0 9.50 0.0 100.0 0.0 0.0 14.00 0.0 100.0 0.0 0.0 14.50 90.0 10.0 0.0 0.0 20.00 90.0 10.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300 HP1100 LC Pump External Event Timetable The TimetabLe contains 6 entries which Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off. Off Contact1 Off On Off Off Off Off are : Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On 'Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(fll) Vial Number Conditions 200.0 200 0.50 20.00 15.0 27 water Page 1 Pressure 400 400 400 400 400 400 400 400 000158 Id Tuning Method Report Method: ~:\~SSLYN~\FLUOROCHEMICA.LS.PRO\ACQUDB\FLUOROCHEMS Printed: Sun Aug 03 08:20:54 2003 v '. Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set Rdbk 3.00 -2.93 20 -15 0.0 0.0 0.0 100 100 300 299 Rdbk OFF 4.2e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation set Rdbk 14.0 14.0 1.0 -2 8 15 9 2 11 14.0 14.0 2.0 650 -647 Rdbk 135.1 767.4 000159 --- ------~ Quantify Calibration Report %& Study No.:L34910, Set No.: 073103AR, --Ext.Date:O7/31/03, -------Analyst:K.Risha Calibration: Last modified: Printed: - P:\Data\LQH~S6\WaselyPx\Fluorochemica Tue Aug 05 07:03:45 2003 Wed Aug 06 11:03:59 2003 --_--_- >ompound 1 name: C8 Acid (PFOA) :oefficient of Determination: 0.996211 :alibration curve: 508.394 ' x + 2202.17 qesponse type: External Std, Area >urve type: Linear, Origin: Exclude, Weighting: 5.16e5 l/x, Axis trans: None -------_- Page 1 Decatur BC X Response- V 0.0 ExypCm Research, 200.0 400.0 600.0 3058 Research Drive, State College, PA 16601 800.0 WL 1000.0 000160 Quantify Calibration Report w Study No.:L34910, Set No.: 073103AR, Ext.Date:O7/31/03, Analyst:K.Risha Calibration: P:\Data\LCM~S6\~sslynx\Bluoroch~cals.~RO\~~eDB\O73lO3~ Last modified: Tue Aug 05 07:03:45 2003 Printed: wed Aug 06 11:03:59 2003 ------------------l_-_____L_I_____________----- ;ompound 2 name: C6 Sulfonate (PFHS) ;oeffkient of Determination: 0.996560 ;alibration curve: 85.6521 ' x + 218.845 Response type: External Std, Area ;urve type: Linear, Origin: Exclude, Weighting: 8.71e4- l/x, Axis trans: None Page 2 Decatur BC ------ X Response 0.0 Exygan Research, 200.0 400.0 600.0 3058 Research Drive, State College, PA 16801 800.0 1000.0 000161 ------- ---------- --_---------____--w-- Quantify Calibration Report l,& Study No. :L34910, Set No. .-073103AR, Ext.Date:07/31/03, Analyat:K.Risha Calibration: Last modified: Printed: ---- --------- P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\~~eDB\O73103~ Tue Aug 05 07:03:45 2003 Wed Aug 06 11:03:59 2003 _------ ------------I_-------- :ompound 3 name: C8 Sulfonate (PFOS) ::oefficient of Determination: 0.998217 Cialibration ewe: 54.2582 * x + 152.345 Rasponse type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 15.44e4- l/x, Axis trans: None ------- Page 3 Decatur BC Response- Exygen Research, 3058 Research Drive, State Collega, PA 16801 000162 Quantify Calibration Report '%& Study No .:L34910, Set No .:073103AR, Ext.Date:07/31/03, &alyst:X.Rioha Calibration: P:\Data\LCM~S6\Masslynx\Fluorochemicals.PRO\~~eDB\O73lO3~ Last nmdified: Tue Aug 05 07 :03:45 2003 Printed: Wed Aug 06 11:03:59 2003 ---------1-----~--~-~--~-~~--~ >ompound 4 name: PFOSA :oeff icient of Determination: 0.998392 2alibration curve: 196.925 ' x + 611.080 qesponse type: External Std, Area htve type: Linear, Origin: Exclude, Weighting: 1.98eE l/x, Axis trans: None Page 4 Decatur BC -w--m------ Response 200.0 400.0 600.0 800.0 looo.b Oxygen Research, 3058 Research Drive, State College, Ph 16801 000163 Quantify SaxQ?le Report S, Study No.:L34910, Set No.: 073103Ak Ext.Date:07/31/03, Analyst:K.Riaha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Wasslynx\Fluorochemicals.PRO\S~leDB\O73lO3~ !I!ue Aug 05 06:59:53 2003 P:\Data\LCM~S6\bss~~\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 1 Decatur SC BC 080103 Name: 073103AR-101 Text : 1: C8 Acid (PFOA) XCO72503-0,O rig/L Standard 073103AFb101 Sm (Mn, 2x3) , , , , , , , , , , , , , , 1 I II 2.00 4.00 w r2: C6 Sulfonate (PFHS) XCO72503-0,O rig/L Standard 1 I ,nlTime 6.00 03-Aug-2003 19:10:54 * LC/MS/MS #6 MRM of 4 Channels ES- 413>369 3.99e4 Area 9.13 794 8.00 10.00 12.00 03-Aug-2003 19:10:54 LChWMS #6 MRM of 4 Channels ES399 > 80 797 2.00 4.00 3: C8 Sulfonate (PFOS) XCO72503-0,O rig/L Standard 1073103AA-101 Sm (Mn, 2x3) 1.27 1 6.00 8.00 10.00 12.00 03-Aug-2003 19:10:51 LC/MS/MS #t MRM of 4 Channels ES499 > 95 1.69eI 6.73 n cl" 11.16 01,,,.,,,,~,,,,,,,~,,,,,~,,,~.~,,~~~,~~~~,~~~~,~~~~,~~~~,~~,~tTime 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16601 000164 Quantify Sample Report ~14 Study No.:L34910, Set No .:073103AR, Ext,Date:07/31/03, Analyst:K.Risha Page 2 Ssqple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyax\Fluoroch~calr.PRO\SampleDB\073103~ Tue Aug 05 06:59:53 2003 P:\Data\L~S#IS6\Masslynx\Fluorochermic\Decatur Sun Aug 03 07:11:59 2003 Decatur Bc BC 080103 Printed: Wed Aug 06 11:04:02 2003 ---_------------___ --1--------------- ------m-w- ------ Name: 073103A.R-101 Teat : 4: PFOSA XCO72503-0,O rig/L Standard 073103AR-101 Sm (Mn, 2x3) 03 -Aug-2003 19: 1054 IX/MS/MS #6 MRM of 4 Channels ES- 10.02 498 3 78 O',,,`,,,,,,,.`,,l,,`,,,.,,.,,,,,l,,,,',,,,,..,,,,,,,,,,,,,,., Time 2.00 4.00 6.00 8.00 10.00 12.00 _ Eacygen Research, 3058 Research Drive, State College, PA 16801 000165 Quantify Sxmple Report 'd Study No.: L34910, Set No.:O73103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method : Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Bluorochsmicals.P~O\S~l~DB\O73lO3~ Tue Auu 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 3 Decatur BC BC 060103 Printed: - Wed Aug 06 11:04:02 2003 -L_-------I---------------- --------P-m----_ NamS: 073103AR-102 Text : : C8 Acid (PFOAI KO72503-1,25 rig/L Standard )73103AR-102 10 Sm (Mn, 2x3) 03-Aug-2003 19:32:33 LCRWMS #6 MRM of 4 Channels ES- 9.13 413>369 1422 &We4 Area 2.00 4.00 6.00 8.00 10.00 12.00 'I& 2: C6 Sulfonate (PFHS) XCO72503-1,25 rig/L Standard 073103AR-102 lOO- Sm (Mn, 2x3) %- 03-Aug-2003 19:32:33 LC/MS/TvlS #6 MRM of 4 Channels ES399 > 80 1.28e4 Area O~,,,,,,~-,,,,,,~,,,,.,~,,~,,,,,:~~~,~~~ , , , , , ; , , Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate XCO72503-1,25 (PFOS) rig/L Standard 073103AFb102 lOO- Sm (Mn, 2x3) %- 03-Aug-2003 19:32:33 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 8.99e3 Area RJC'YO*n Research, 3058 Research Drive, State College, PA 1.6601 _. .I I----~ 000166 Quantify Sample Report ba# study No.:L34910, Set NO.: 073103AR, Ext.Dats:07/31/03, Analyst:X.Risha Page 4 Sample List: Last modifiad: Method: Last modified: Job Code: P:\Data\LCMSMS6\~lasalynx\Pluoroch~cals.PRO\S~laDB\O73lO3~ Tus Aug OS 06:59:53 2003 P:\Data\L~SS\~sslynx\FluorochsmiB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 -- ------- --_-__--_---- -w--e---- - -- Name: 073103AR-102 Text : 4: PFOSA XCO72503-1,25 rig/L Standard 073103AR-102 Sm (Mn, 2x3) 03-Aug-2003 19:32:3I LCIMWMS #E MRM of 4 Channels ES498 > 723 2.76e4 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 aul, Exysren Research, 3058 Research Drive, State College, PA 16801 --. 000167 ------ Quantify Sample Report %w' Study No .:L34910, Set No .:073103AR, Ext.Date:07/31/03, --A.nalyst:K.Risha Page 5 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSbiS6\blasslynx\Fluoroch~c~ls.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.P~O\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 --__--------------------_II_-----------------------~_ --s-s-- Name: 073103AR-103 Text : 1: C8 Acid (PFOA) XCO72503-2,50 rig/L Standard 073103AFb103 1001 Sm (Mn, 2x3) %- 03-Aug-2003 19:54:17 LCNSIMS #6 MRM of 4 Channels ES- 9.13 413>369 1.66e5 Area 2.00 4.00 6.00 8.00 10.00 12.00 _ : C6 Sulfonate (CO72503-2,50 (PFHS) rig/L Standard )73103AR-103 10 Sm (Mn, 2x3) % 4 03.Aug-2003 19:54:14 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 47lE 2.93e4 Area 3: C8 Sulfonate I XCO72503-2,50 (PFOS) rig/L Standard 073103AR-103 Sm (Mn, 2x3) Time 12.00 03-Aug-2003 19:54:1 LC/MS/MS #6 MRM of 4 Channels ES- 1.79e4 Area Time 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 000168 Quantify Sample Report w Study No .:L34910, Set No .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha S-18 List: Last modified: X&hod: Last modified: Job Code: P:\Data\LCblSMS6\Masslyax\Fluoroch~cala.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorocb~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 6 Decatur BC BC 080103 Name: Text: 073103AR-I.03 4: PFOSA XCO72503-2,50 rig/L Standard 073103AFb103 lOO- Sm (Mn, 2x3) %- 03-Aug-2003 19:54:11 LC/MS/MS #c MRM of 4 Channels ES- 9.89 _ 498 > 7E 10303 5.55e4 Area 0 ,~~~,~~~,I,,,,,,,,,,,,,,,,,~,,~~,,,,~,,,~,~~,,,~~,~,,,,,,,,Time 2.00 4.00 6.00 8.00 10.00 12.00 J RxYgea Research, 3058 Research Drive, State College, PA 16801 0003.69 Quantify Sample Report && Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, A,nalyet:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochsmicals\Uet~B\Dacatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 7 Decatur BC BC 080103 Name: 073103AR-104 Text : 1: CE? Acid (PFOA) XCO72503-3,100 rig/L Standard 073103AR-104 1Af-L Sm (Mn, 2x3) 03-Aug-2003 20:16:01 LC/MS/MS #6 MRM of 4 Channels ES- 9.15 4'13> 369 3.21 e5 Area : C6 Sulfonate KiO72503-3,100 (PFHS) rig/L Standard 173103AFb104 10 Sm (Mn, 2x3) Time 12.00 03-Aug-2003 20: 16:Olj LCIMSNS #6 MRM of 4 Channels ES- 6.98 399 > 80 9231 5.35e4 Area Time 12.00 3: C8 Sulfonate XCO72503-3,100 (PFOS) rig/L Standard 073103AFb104 loo7 % 4 Sm (Mn, 2x3) 03-Aug-2003 20:16:0' LC/MS/MS #f MRM of 4 Channels ES- 9.25 499 > 9: 5100 2.99er Are: Time `IN 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000170 Quantify Sarqple Report \r, Study No.:L34910, Set No.: 073103AR, Ext.Date:O7/31/03, Analyat:R.Ri.sha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluorach~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCWSblS6\Masslynx\BluorochamfcalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2OQ3 Page 8 Decatur BC BC 080103 Name: 073103AR-104 Text : r4: PFOSA XCO72503-3,100 q/L Standard 073103AB104 lOO- Sm (Mn, 2x3) %- 03-Aug-2003 20:16:01 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 1.07e5 Area 0 "~`,"","",""i"","","","",~"`,"' , r I I 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000171 -- w-e--- -------------- Quantify Saxaple Report &,+ Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:lC.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQnSMS6\Masslyax\Fluorochemicals.PRO\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\~asslynx\PluorochamicB\Decatur Sun hug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 ---- Page 9 Decatur BC BC 080103 Name : 073103AR-105 Text : 1: C8 Acid (PFOA) XCO72503-4,250 rig/L Standard 073103AR-105 la?- Sm (Mn, 2x3) %- 9.13 _ 128556 03-Aug-2003 20:37:5C LC/MS/MS #6 MRM of 4 Channels ES413>369 7.38e5 Area 0 `~~~,~,,,.,,,,"",.,;,,,,.`,,,,l,,",,.',,~~,,I',`~I~~~~l 2.00 4.00 6.00 k# 2: C6 Sulfonate XCO72503-4,250 (PFHS) rig/L Standard 073103AR-105 loo- Sm (Mn, 2x3) %- 0 "","","","","","","",i"`( 2.00 4.00 6.00 : C8 Sulfonate (CO72503-4,250 (PFOS) rig/L Standard 173103AFb105 IO 9 Sm (Mn, 2x3) 8.00 a.98 10.00 Time 12.00 03-Aug-2003 20:37:5C LC/MS/MS #6 MRM of 4 Channels ES- 399 > 80 1.2985 Area , , , , , , , , , , , , , Time 8.00 10.00 12.00 03-Aug-2003 20:37:5C LC/MS/MS #6 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000172 ----- ---------- Quantify Sample Report L, Study No.:L34910, Set No.:O73103AR, -- Ext.Date:07/31/03, Analyst:K.Risha ------Page lo Sampla List: Last modified: Method: Last modified: Job Code: P:\Data\~~S6\Masslynx\Fluoroch~cals.P~O\S~leDB\O73lO3~ Tue Aug OS 06:59:53 2003 P:\Data\L~S6\Massl~\Fluoroch~cals.PXO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 --_----- _I-- ---Pm-- ---- ----- Name: 073103AR-105 Text : : PFOSA X072503-4,250 rig/L Standard 173103AR-105 10 %1"I Sm (MI-I, 2x3) 03-Aug-2003 20:37:X( K/MS/MS #6 MRM of 4 Channels ES- 9.90 4863: ! 498 > 78 2.52e5 Area I 10.00 Time 12.00 V Oxygen Research, 3058 Research Drive, State College, PA 16801 000173 Quantify Sample Report chd Study No.: L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:R.Risha Sample List: Laet modified: Method: Last modified: Job Code: P:\Data\LQbSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LC=MSMS6\Nassl~\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 11 Decatur BC BC 080103 NWM: 073103AR-106 Text : : C8 Acid (PFOA) (CO72503-5,500 rig/L Standard )73103AR-106 10 7 %-I Sm (Mn, 2x3) 9.13 264862 03-Aug-2003 20:59:3$ LC/MS/MS #6 MRM of 4 Channels ES413> 369 lSie6 Area o',,,,,~,,,".,,"`.,`..`,"",."`,""," I , , , , , , , , , , ,Time i 2.00 4.00 6.00 8.00 10.00 12.00 _ qd 2: C6 Sulfonate XCO72503-5,500 (PFHS) rig/L Standard 073103AFb106 10 Sm (Mn, 2x3) % 8.98 43819-J 03-Aug-2003 20:59:3$ LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.5465 Area I--- 3: C8 Sulfonate XCO72503-5,500 b"`L""i 2.00 `I ub,ml 4.00 (PFOS) rig/L Standard 073103AR-106 IOO- Sm (Mn, 2x3) `II' trllllll,Txr 6.00 4' 8.00 9.27 %- rflls' 10.00 m\rma `1 Time 12.00 _ 03-Aug-2003 20:59:3< LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.65e5 Area Oxygen Research, 3058 Research Drive, State College, PA 16801 000174 ---__l------- ---- _-___------ -----mm- Quantify Sample Report &,J study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: - Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.P~\S~leDB\O73lO3~ Tue hug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 ----- Page 12 Decatur EC BC 080103 Name: 073103hR-106 Text : 4: PFOSA XCO72503-5,500 073103AR-106 Sm .rig/L IMn. ,Standard 2x3) %- 03-Aug-2003 20:59:39 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 104085 498 > 78 5.47e5 I Area 0 ~~`~,"","l~,`~"/"",~)","","","~`l"' 2.00 4.00 6.00 8.00 ti Time / 12100 Oxygen Research, 3058 Research Drive, State College, PA 16801 000175 -- ---- --- ------- Quantify Sampls Report &,& Study No.:L34910, Set No.. *073103AR, Eixt.Date:07/31/03, Analyst:K.Risha Samgle List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\~sslynx\Fluorochemicals.PRO\S~leDB\O73lO3~ Tus Aug 05 06:59:53 2003 P:\Data\L~S6\Maeslynx\Fluorcchermic\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 ---- Page 13 Decatur BC BC 080103 Name: Text: 073103AR-107 1: C8 Acid (PFOA) XCO72503-6,1000 t-q/L Standard 073103AR-107 loo- Sm (Mn, 2x3) %- 9.15 516215 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of 4 Channels ES413>369 2.96e6 Area 0 ~`~~,`~`~/`~~~/~~`~,`r"l""l""l'("1"" I I I I I , I I . I 1Time 2.00 4.00 6.00 8.00 10.00 12.00 1: C6 Sulfonate KCO72503-6,1000 (PFHS) rig/L Standard 073103AR-107 10 Sm (Mn, 2x3) %$ 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 871t5 399 > 80 5.03e5 Area 3: C8 Sulfonate XCO72503-6,1000 (PFOS) rig/L Standard 1-0.73-1.0--3.AFb10.7. .- I 910 1 %- Sm(Mn,2x3) I Time 12.00 . 03-Aug-2003 21:21:27 LCJMWMS #6 MRM of 4 Channels ES499 > 99 3.12e5 Area Exygen Research, 3058 Rwearch Drive, State College, PA 16801 000176 -----___ --p----m-------- Quantify Sample Report w Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Wasslynx\Fluorochemica~s.PRO\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\Lc3MflrlS6\Masslynx\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-107 Text : Page 14 Decatur BC BC 080103 XCO72503-6,1000 rig/L Standard 073103AR-107 100- Sm (Mn, 2x3) %- 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1 .Ol e6 Area 0 `lll,/`l'(l'll,llll,lll',"ll,"l',"",IJ'I,II , I I . 1 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 EXYgen Research, 3058 Research Drive, State College, PA 16601 000177 Quantify Sample Report w Study No.: L34910, Set No.:O73103AR, Ea&.Date:07/31/03, Analyst:K.Risha Sample List: Last modifies: Method: Last modified: Job Code: P:\Data\LQI~S6\Pssl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue hug 05 06:59:53 2003 P:\Data\LCMSMS6\~sslynx\FluorochemicalB\Decatur Sun hug 03 07:11:59 2003 Printed: Wed hug 06 31:04:02 2003 Page 15 Decatur BC BC 080103 Name: 073103AR-108 Text : 1: C8 Acid (PFOA) L34910-1 Spk C, 5000 rig/L, DF=lOO 073103AB108 Sm (Mn, 2x3) 03-Aug-2003 21:43:18 LC/MS/MS #6 MRM of 4 Channels ES- 413>369 2.96e5 Area k# 2: C6 Sulfonate (PFHS) L3491 O-l Spk C, 5000 rig/L, DF=lOO 073103AFb108 Sm (Mn, 2x3) Time 12.00 03-Aug-2003 21:43:18 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 3.37e4 Area : C8 Sulfonate (PFOS) -34910-l Spk C, 5000 q/L, DF=lOO )73103AR-108 10 Sm (Mn, 2x3) % : Time 12.00 I 03-Aug-2003 21:43:1d LCNWMS #6 MRM of 4 Channels ES499 > 99 5.51e4 Area I 10.00 Time 12.00 ExVgen Research, 3058 Research Drive, State College, PA 16801 000178 Quantify Sample Report 'ln14 Study No.: L34910, Set No.: 073103AR, Ra&.Date:O7/31/03, Analyst:R.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~SMS6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 16 Decatur BC BC 080103 Printed: --- Wed Aug 06 11:04:02 2003 --------- ___----- _-------- Name: 073103AR-108 Text : 4: PFOSA L3491 O-l Spk C, 5000 rig/L, DF=lOO " 073103AFb108 10 Sm (Mn, 2x3) 03-Aug-2003 21:43:18 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 13039 498 > 78 6.85e4 Area -en Research, 3058 Research Drive, State College, PA 16801 000179 ---- --- ------ ------ Quantify Sample Report 4d Study No.:L34910, Set No.: 073103AR, F.xt.Date:07/31/03, Analyst:R.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LeMSMS6\Masslynx\Fluorochamicals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Pluorocb~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 - Page 17 Decatur BC BC 080103 Name: Text: 073103AR-109 : C8 Acid (PFOA) -3491 O-l 2 Spk E, 5000 rig/L, DF=lOO 173103AFb109 Sm (Mn, 2x3) %110 "$-1 2.00 4.00 6.00 1: C6 Sulfonate (PFHS) L3491 O-1 2 Spk E, 5000 rig/L, DF=l 00 073103AFb109 10 Sm (Mn, 2x3) 9.13 92540 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 5.53e5 Area i-- 8.00 10.00 Time 12.00 03-Aug-2-003 22:04:56/ LC/MS/MS #6 MRM of 4 Channels ES- 8.98 10314 399 > 80 6.00e4 Area 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) L3491 O-1 2 Spk E, 5000 rig/L, DF=lOO 073103AR-109 100- Sm (Mn, 2x3) %- ". 8.00 10.00 Time 1 12.00 03-Aug-2003 22:04:5( LC/MS/MS #6 MRM of 4 Channels ES499 > 9s 1.03e5 Area muen Research, 3058 Research Drive, State College, PA 16801 000180 ---- _-__-- _--_-B------B -__-____ --- Quantify Sample Report &,# Study No.:L34910, Set No.: 073103AR, Rxt.Date:07/31/03, Analyst:K.Risha Page ia Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\bssl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCHSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 060103 Printed: Wed Aug 06 11:04:02 2003 .-______-__-__________________--___I_____-------------~-- Name: Text: 073103AR-109 4: PFOSA L3491 O-l 2 Spk E, 5000 rig/L, DF=lOO 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 49a> 78 8.15e4 Area WrJen Research, 3058 Research Drive, State College, PA 16801 -_-- 000181 -.-_-_-,_.. l__---_l____------__ ------- ------ Quantify Sample Report -4 Study No.:L34910, Set No.: 073103AR, Ext,Date:07/31/03, -----_1_-- Analyst:X.Risha - Page 19 Sample List: Last modified: Method: Last modified: Job code: P:\Data\L~~S6\~ssl~\Fluarochemicals.PRO\S~leDB\O73lO3~ Tus Aug 05 06:59:53 2003 P:\Data\L~SMS6\Masslynx\Fluorochemical$.PRO\~t~B\Decatur Sun Aug 03 07:11:59 2003 Printed: __-----___ Wed Aug 06 11:04:02 2003 -------- ----_____-___-___-- Name: 073103AR-110 Text: ---__--- Decatur BC BC 080103 --_--- 1 1.3491 O-l 6 Spk F, 5000 rig/L, DF=lOO C)73103AR-110 10 Sm (Mn, 2x3) % 9.13 11471r 03-Aug-2003 22:26:4 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 6.50e5 Area i I 2.00 4.00 6.00 8.00 2 : C6 Sulfonate (PFHS) 1-3491 O-l 6 Spk F, 5000 rig/L, DF=lOO ( 173103AR-110 10 Sm (Mn, 2x3) % 8.96 10701 03-Aug-2003 22:26:4d LC/MS/MS #6 MRM of 4 Channels ES399 > 80 6.13e4 Area /: 2.00 4.00 8.00 ,, , I II, 10.00 I, ,lTime 12.00 3 : C8 Sulfonate (PFOS) 1-3491 O-l 6 Spk F, 5000 rig/L, DF=lOO ( 173103AR-110 10 Sm (Mn, 2x3) 9.25 22405 03-Aug-2003 22:26:4C LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.26e5 Area w Exysen Research, 3058 Research Drive, State College, PA 16801 000182 Quantify san@e Report 114 Study No.:L34910, Set No.. *073103AR, Ext.Date:07/31/03, A.nalyst:K.Rieha Sample List: Last modified: Method: Last modified: ifob Code: P:\Data\LCMSMS6\Masslynx\Fluorochsmicals.PRO\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\Masslynx\Fluorochemicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Auq 06 11:04:02 2003 Page 20 Decatur BC EC 080103 Nsme: 073103AR-110 Text: 4: PFOSA L3491 O-l 6 Spk F, 5000 rig/L, DF=lOO 1073103AR-110 I--,-f--ih -.- I"T Sm(Mn,2x3) %- 03-Aug-2003 22:26:4C LC/MS/MS #6 MRM of 4 Channels ES- 9.90 18398- 498 > 78 9.42e4 Area Exygen Research, 3058 Research Drive, State College, PA 16801 000183 Quantify Sample Report Q& Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\L(1MSMS6\Masslynx\FluorocbamicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 21 Decatur BC BC 080103 Name: 073103AR-111 Text : 1: 03 Acid (PFOA) XCO72503-I,25 rig/L Standard 073103AR-111 10 Sm (Mn, 2x3) 9.13 14631 03-Aug-2003 22:48:24 LC/MS/MS #6 MRM of 4 Channels ES413> 369 8.76e4 Area 2: C6 Sulfonate XCO72503-1,25 (PFHS) rig/L Standard 073103AFb111 100- Sm (Mn, 2x3) %- 03-Aug-2003 22:48:23 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 2324 1.44e4 Area o-,,~-r;,,,`,,,,,,:.,,,`,.,,,,.,,-,;-?,,,.,,,. , , , , , , , , ,-, , I, Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate XCO72503-I,25 (PFOS) rig/L Standard ,073103AR-111 lOO- Sm (Mn, 2x3) %- 03-Aug-2003 22:48:23 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.17e3 Area Oxygen Research, 3050 Research Drive5 State College, pA 16601 000184 Quantify San@0 Report q& Study No.:L34910, Set No.: 0?3103AR, Ext.Date:07/31/03, AnalystxX.Risha Page 22 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L(3MSMS6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue hug 05 06:59:53 2003 P:\Data\LCMSMS6\blass~~\FluorochemicalB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 ---------------------------------------- ------ -------0----- Name: 073103AR-111 Text : 4: PFOSA XCO72503-1,25 rig/L Standard 073103AFb111 Sm (Mn, 2x3) 03-Aug-2003 22:48:2: LC/MS/MS #E MRM of 4 Channels ES498 > 78 2.92e4 Area Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 800185 - -----a-- ---- Quantify Sample Report Id Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQ3SMS6\~6slynx\Bluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSnS6\MasslyPx\FluorochamicalsB\Decatur Sun Aug 03 07:11:59 2003 Page 23 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 -------- -----------------___I___--__ -- Name : 073103AR-112 Text : 1: C8 Acid (PFOA) IL3491 O-l, DF=lO 073103AFb112 10 Sm (Mn, 2x3) % 1 9.13 216041 03-Aug.2003 23:lO:Od LCIMSNS #6 MRM df 4 Channels ES413 > 369 1.26e6 Area II& 2: C6 Sulfonate (PFHS) L3491 O-1, DF=l 0 073103AR-112 loo- Sm (Mn, 2x3) I_ Time 12.00 03-Aug-2003 23:10:02 LCYMWMS #6 MRM of 4 Channels ES- 6.98 9381 %- `m Time 2.00 4.00 6.00 8.00 10.00 : C8 Sulfonate (PFOS) 83491O-l, DF=l 0 73103AFb112 `OOl Sm (Mn, 2x3) 03-Aug--2003 23:10:02j LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 61501 3.57e5 Area m Time 2.00 4.00 6.00 8.00 10.00 12.00 Eawgen Research, 3058 Research Drive, State College, PA 16801 000186 Quantify Sample Report 14 Study No.:L34910, Set No.: 073103AR, Ext.Dats:O7/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\MasslyPx\Fluoroch~cal~.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2903 P:\Data\L~SMS6\Ma6slynx\Fluorochamicals.?RO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 24 Decatur BC BC 080103 Name: 073103AR-112 Text : 4: PFOSA L3491 O-l, DF=l 0 073103AFb112 lOO- Sm (Mn, 2x3) %- . . .. 03-Ayg-2FII3 23:10:02 LC/MS/M'S #6 MRM of 4 Channels ES- 9.89 _ 27920 498 > 78 1.43e5 Area Oxygen Research, 3056 Research Drive, State Collage, PA 16801 OQOl87 Quantify Sample Report Study No.: L34910, Set No .:073103AR, Ext.Date:07/31/03, Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQIISMS6\Masslyax\Fluoroch~cals.PRO\S~leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMSC\Masslynx\Fluoroch~cals.PRO\lsthDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003' ------------------------------_________I_ Name: Text: 073103AR-113 1: CB Acid (PFOA) L34910-1 Rep, DF=10 073103AFL113 lOO- Sm (Mn, 2x3) %- 4 0 ,,,,~,,,,,,,~,,,~,,,,,,I,,,,,~,,,,,,,,, 2.00 4.00 6.00 2: C6 Sulfonate (PFHS) L3491 O-1 Rep, DF=lO 073103AR-113 lOO- Sm (Mn, 2x3) %- 0 "I 87 " ' , s 8 `T I"",' 2.00 3: C8 Sulfonate (PFOS) L3491 O-l Rep, DF=lO r 8 8 ,I 8 r - / 4 I, f 4.00 6.00 073103AR-113 lOO- Sm (Mn, 2x3) %- AnalystrK.Risha Page 25 Decatur BC BC 080103 ----P--P- 03-Aug-2003 23:31:52 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 1.26e6 Area `. 8.00 8.98 I t , 10.00 I , I I 1Time 12.00 03-Aug-2003 23:31:52 LCNWMS #6 MRM of 4 Channels ES399 > 80 5.8Oe4 Area Time 8.00 10.00 12.00 9.25 59888 03-Aug-2003 23:31:52 LClMStMS #6 MRM of 4 Channels ES499 > 99 3.52e5 Area wgea Research, 3058 Research Drive, State College, PA 16801 000188 Quantify Sample Report '4 Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:R,Risha Sample List: Last modified: Method: Last modified: ifoh Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\O73103~ Tue Auq 05 06:59:53 2003 P:\Data\L(SMSMS6\Masslynx\Fluorochamicals.PRO\MethllB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 26 Decatur BC BC 080103 NW: 073103AR-113 Text : 4: PFOSA -34910-l Rep, DF=lO 173103AFb113 10 "i %- Sm (Mn, 2x3) 03-Aug.2003 23:31:5: LC/MS/MS #r MRM of 4 Channels ES- ExygeP Research, 3058 Research Drive, State College, PA 16801 000189 Quantify San&Jle Report TJ Study No.:L34910, Set No .:073103AR, Ext.Date:07/31/03, Analyst:R.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\FluotochemicalsB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 27 Decatur BC BC 080103 Name: 073103AR-114 Text : 1: C8 Acid (PFOA) L3491 O-4, DF=lO 073103AFb114 100- Sm (Mn, 2x3) %- 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413>369 7.7405 Area o'v ,,,~,,,,,,,,,,.,,,,,,,,,,,,,., 2.00 4.00 2: C6 Sulfonate (PFHS) L3491 O-4, DF=lO 073103AR-114 loo- Sm (Mn, 2x3) %- # I,III,,IJII 6.00 8.00 a , , , , , , , , , , , Time 10.00 12.00 ) 8.98 _ 6122 03-Aug-2003 23:53:41 LCIMSNS #6 MRM of 4 Channels ES399 > 80 3.73e4 Area 0 ,,, . , , ,, , ,qTime 2.00 4.00 6.00 8.00 10.00 12.00 , * C8 Sulfonate (PFOS) -3491 O-4, DF=lO )73103AR-114 %110 Sm (Mn, 2x3) 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.59e5 Area Time ExyOen Research, 3058 Research Drive, State College, PA 16801 00019d Quantify Sample Report v Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\bssl~\Fluoroch~ca~s.PRO\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\~SWS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 28 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 ---------_-_-__-___ -m-v---- ---------------e __.-_ Name: 073103AR-114 Text : 4: PFOSA L3491 O-4; DF=l 0 073103AFb114 lOO- Sm (Mn, 2x3) `7. ' %- 03-Aug-2003 23:53:41 LCIMSIMS #6 MRM of 4 Channels ES- 9.90 498 > 78 1.05e5 Area 0 "","","","","","",""I',",""," I I x I I Time 2.00 4.00 6.00 8.00 10.00 12.00 Ewgen Research, 3058 Reseaxch Drive, State College, PA 16801 000191 Quantify S-10 Report w Study No.: L34910, Set No.:O73103AR, Ext.Dats:07/31/03, Analyst:K.Risha Page 29 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQrlSMS6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LWSMS6\Masslynx\Fluotochamicals.~O\~et~E\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: s-m---- Wed Aug 06 11:04:02 2003 ----- ------- --- ------__ Name: Text: 073103AR-115 1: C8 Acid (PFOA) L3491 O-2, DF=lO I(173103AR-I 10 7 15 Sm (Mn, 2x3) % 9.15 142555 i 04-Aug-2003 00:15:3Cj LCYMWMS #6 MRM of 4 Channels ES413 > 369 8.29es Area i 2.00 !: C6 Sulfonate (PFHS) L3491 O-2, DF=l 0 I a.00 10.00 Time 12.00 04-Aug-2003 oo:l6:3d 073103AFb115 Sm (Mn, 2x3) 8.98 7036 L 6.00 3: C8 Sulfonate (PFOS) L3491 O-2, DF=lO 073103AR-115 ff-ln, I i _. Sm (.Mn, 2x3) . 0 ~~`,~`~~,"~~,~`~~,~~~~,~"`,~`~~,~"~I~~~~, 2.00 4.00 6.00 a.00 9.27 37566 04-Aug-2003 oo:l sad LC/MS/MS #6 MRM of 4 Channels ES- 499 > 99 2.19e5 Area bm a.00 10.00 Time / 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ._..,_X_*-,II _._- ._,--- 000192 ___-.. ..- ------_--- --s-----w- ------ ---s----w - Quantify San@e Report td Study No.:L34910, Set No .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 30 Sanpls List: Last modified: Method: Last modified: Job Code: P:\Data\LCblSMS6\Masslynx\Fluorochsmicals.PRO\S~leDB\O73lO3~ Tue hug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.P~O\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC EC 080103 Printed: --____--_--------- Wed hug 06 11:04:02 2003 -----_--A- Name : 073103AR-115 Text : ----v--------- 4: PFOSA L3491 O-2, DF=lO 073103AFb115 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 00:15:30 LCfMS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 8.43e4 Area 0 "","",1"`,"`1,"`1,"`1,"`1,"","",'11 , , ( , , , , ,Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ..l^^.~---_l_--- .~"_^._"._ _"l-ll---ll ..- .- 000193 ---I__ _____I___--___________________I---------------- Quantify Sample Report IJ Study No.:L34910, Set No.. -073103AR, Ext.Dats:07/31/03, Analyst:K.Risha Page 31 Sample List: Last modifieh: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluorochemical~.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\Masslynx\Fluorochemica\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 _--------______I__--~ -------------c------------- ------- Name : 073103AR-116 Text: : C8 Acid (PFOA) (CO72503-2,50 rig/L Standard )73103AR-116 10 Sm (Mn, 2x3) 04-Aug-2003 00:37:14 LC/MS/MS #6 9.13 292% MRM of 4 Channels ES413>369 1.78e5 Area 4 2.00 4.00 6.00 a.00 KC072503-2,50rig/L Standard 073103AK116 Sm (Mn, 2x3) 04-Aug-2003 00:37:1 q LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 4266 2.73e4 Area I: C8 Sulfonate KC072503-2,50 (PFOS) rig/L Standard 073103AFb116 10 Sm (Mn, 2x3) 4 04-Aug-2003 00:37: 19 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 2882 1.77e4 Area L-; Time 12.00 Oxygen Research, 3058 Research Driira, State College, PA 16801 000194 Quantify Sample Report W Study No.:L34910, Set No.. -073103AR, Ext.Date:O7/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQt~S6\Lrlassl~\Fluoroch~cal~.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Page 32 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 -_____-I_--------------- __----------- ----- Name : 073103AR-I.16 Text : 4: PFOSA XCO72503-2,50 rig/L Standard 073103AR-116 loo- Sm (Mn, 2x3) %- 04-Aug-2003 00:37:19 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 5.94e4 Area 0 "`~,"`~,~~`~/)~~`,`~(~,~~~~,~`~J,~"',~(~l, 2.00 4.00 6.00 8.00 , I I I 1 1 Time 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 800195 ----__-----_ -__------I_----I_____ --w-p Quantify Szmqls Report sf Study No.:L34910, Sat No .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Pluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\~ss~~\FluorochemicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 -VW---_ Page 33 Decatur BIJ BC 080103 Name: Text: 073103AR-117 1: C8 Acid (PFOA) L3491 O-6, DF=lO ~073103AR-117 loo- Sm (Mn, 2x3) %- 04-Aug-2003 00:59:01 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 419 >369 2.33e5 Area 2: C6 Sulfonate (PFHS) L3491 O-6, DF=lO 073103AFb117 loo- Sm (Mn, 2x3) %- 04-Aug-2003 00:59:01 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 9.39e3 Area - : C8 Sulfonate (PFOSI -3491 O-6, DF=l 0 173103AR117 Sm (Mn, 2x3) 04-Aug-2003 00:59:011 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 9224 5.40e4 Area Time 12.00 Rawgem Research, 3058 Research Drive, Stats Collage, PA 16801 000196 Quantify Sample Report 1~ Study No.:L34910, Set No.: 073103AR, Ext.Date:O7/31/03, ?malyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~.SbiS6\Uasslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSbiS6\Maaslynx\FluorochemicB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed hug 06 11:04:02 2003 Page 34 ' Decatur BC EC 080103 Name: 073103AR-117 Text: 4: PFOSA L3491 O-6, DF=lO 073103AFb117 100-l Sm (Mn, 2x3) %- 04-Aug-2003 00:59:01 LCPMSNS #6 MRM of 4 Channels ES- 9.09 498 > 78 1.84e4 Area r I I I , r I e I I Time 10.00 12.00 mgen Rasektch, 3058 Research Drive, State College, PA 16801 000197 Quantify Sample Report $& Study No.rL34910, Set No .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~ssl~\Fluorochemicals.PRO\S~l~DB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\~sslynx\Pluorochemicalr Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-118 Text : Page 35 Decatur BC BC 080103 .34910-6 Rep, DF=lO )73103AR-118 10 Sm (Mn, 2x3) 04-Aug-2003 01:20:44 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 2.33e5 Area w 2: C6 Sulfonate (PFHS) L34910-6 Rep, DF=iO 073103AR-118 lOO- Sm (Mn, 2x3) %- , , , , I , , , , , , ,-l Time 10.00 12.00 04-Aug-2003 01:20:44 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 9.36e3 Area - O~,,,r,.~,i,,,,,,,~,~,,,r,,,,,~,~~I~,~ , t .m, Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-6 Rep, DF=lO 073103AFb118 10 "i %- Sm (Mn, 2x3) 04-Aug-2003 01:20:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.27 499 > 99 5.02e4 Area 0 ~~~~~~~~,~~~~,`~~~,`~"I"~ Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, pA 16801 000198 ------ -_------ -1--_1 ---------~--I_-- Quantify Sarqple Report '4 Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Ri.sha Page 36 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCbI~S6\Masslynx\Fluoroch~calS.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 B:\Data\LCNSMS6\Masslynx\Fluoroch~ca~S.PRO\Met~B\Decatur Sun Aug 03 07:X1:59 2003 Decatur BC BC 080103 Printed: ----- Wed Aug 06 11:04:02 2003 --a--- ---_-----_---------------------_-__ Name: 073103zm118 Text : : PFOSA -34910-6 Rep, DF=lO )73103AR-118 10 Sm (Mn, 2x3) 04-Aug-2003 01:20:4r LC/MS/MS #t MRM of 4 Channels ES- 9.89 498 > 72 3402 1.76eL AreE O',,`~,,`,,,,,,,,,r.,,`,,,,,,,`,,,.,,,,,,,,.,,,,,,' I.. Time 2.00 4.00 6.00 8.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 .,_-^-- -~ 000199 _.---.- - Quantify Sample Report u Study No.:L34910, Set No .:073103AR, Ext.Dats:07/31/03, Analyst:K.Risha Page 37 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQrlSMS6\~ssl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ !I'ue hug 05 06:59:53 2003 P:\Data\L~SMS6\Maselynx\Fluorochemica\~et~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC EC 060103 Printed: -----__ Wed Aug 06 11:04:02 2003 ------_-------I_-----------------------------_- ---_-_- Name: 073103AR-119 Text : 1: CB Acid (PFOA) IL3491 O-9, DF=l 0 073103AR-119 100- Sm (Mn, 2x3) %- 04-Aug-2003 01:42:3tj LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 4.77e5 Area 0 I,1 ,(-?Y I ,,1111,/111/1/~1(1~11,1111,1111,111 2.00 4.00 6.00 `4 !: C6 Sulfonate (PFHS) -3491 O-9, DF=l 0 173103AFb119 Sm (Mn, 2x3) > 8.00 8.98 3725 , , I , , , , Time 10.00 12.00 04-Aug-2003 01:42:36] LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.31 e4 Area 3: ca Sulfonate (PFos) L3491 O-9, DF=l 0 073103AR-119 Sm (Mn, 2x3) , I.,,j .,,I , 10.00 I 1 Time 12.00 9.25 23649 04-Aug-2003 01:42:36 LCNSIMS #6 MRM of 4 Channels ES499 > 99 1.3505 Area wgen Research, 3056 Research Drive, State College, PA 16801 QOO200 Quantify Sample Report bd Study No.: L34910, Set No.:O73103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~~S6\Maselynx\Bluoroch~cals.PRO\S~~eDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 ------_-_------___--- m--------v- --------m_ Name: 073103AR-119 Text : Page 38 Decatur BC EC 080103 L3491 O-9, DF=lO 073103AR-119 Sm (Mn, 2x3) 04-Aug-2003 01:42:36 LCIMSNS #6 MRM of 4 Channels ES490 > 78 4.44e4 Area Time 12.00 E%ygen Research, 3058 Research Drive, State College, PA 16801 000201 ----- ---------------- ----a------ p-v-- Quantify Sampl.e Report `Id Study No. : L34910, Set No .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last nmdified: Job Code: P:\Data\L~SMS6\~sslynx\Fluorochamicals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCM~S6\blasslynx\Pluoroch~cals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Page 39 Decatur BC BC 060103 Printed: Wed Aug 06 11:04:02 2003 -I----------__-------------__________II________---- --m--P-_ Name: 073103AR-120 Text : 1 : C8 Acid (PFOA) 1-34910-7, DF=lO r t )73103AR-120 Sm (Mn, 2x3) 9.13 1127010 04-Aug-2003 02:04:23 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 6.62e5 Area 2.00 : C6 Sulfonate (PFHS) -3491 O-7, DF=lO 173103AR-120 10 Sm (Mn, 2x3) A-- Time 12.00 6.97 6025 04-Aug-2003 02:04:23 LC/MS/MS #6 MRM of 4 Channels ES- 399>80 3.66e4 Area 3: C8 Sulfonate (PFOS) L3491 O-7, DF=lO 073103AFb120 lOO- Sm (Mn, 2x3) %- 0 ,,,,-;-,,,,,,,,,,~,,,,~2,,.,0,,0,~,,,,,,,~,,,,,,~,~~~4,.~0~0,~,~~,~,Time 6.00 > 9.25 _ 29284 04-Aug-2003 02:04:22 LC/MS/MS #E MRM of 4 Channels ES499 > 9E 1.69eE Aree 8.00 10.00 12.00 wgen Research, 3058 Research Drive, State College, PA I.6601 . .--- .-.- ll^ll_l_---- --... - -. ---- - --__----------- Quantify Sample Study No .:L34910, Report Sat No .:073103AR, Ext.Data:07/31/03, Samgle List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Wasslynx\Fluotochrmicals.PRO\S~i~DR\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCM93S6\Masslynx\Fluorochsmicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: e--v-- Wed Aug 06 11:04:02 2003 --- m---w------- Name: 073103A?i-120 Text : --e------- 4: PFOSA L34910-7,DF=lO 073103AFb120 Sm (Mn, 2x3) -__-- Analyat:K.Risha ---- Page 40 Decatur BC BC 080103 I--------___ 04-Aug-2003 02:04:23/ LC/MS/MS#6 MRM of 4 Channels ES- 9.89 11595 490 > 78 5.91 e4 I Area w Time 6.00 10.00 12.00 Exygen R-earth, 3058 Research Drive, State college, PA 16801 000203 Quantify Sample Report qrf Study No.:L34910, Set No.: 073103AR, E&.Dater07/31/03, Analyst:K.Risha Salnple List: Last modified: Method: Last modif ied: Job Code: P:\Data\L~SMS6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMSb\Masslynx\Fluorochemical~.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 I___------____-_---m--w------w------------- Name : 073103AR-121 Text : .: C8 Acid (PFOA) <CO72503-3,100 rig/L Standard 373103AR-121 10 O-4 Sm(Mn,2x3) 9.15 5566: Page 41 Decatur BC BC 080103 -A---- 04-Aug-2003 02:26:03( LC/MS/MS #6 MRM of 4 Channels ES413>369 3.27e5 Area ---~--r-rrpq Time I 2.00 4.00 6.00 8.00 10.00 12.00 I: c6 Sulfonate KO72503-3,100 (PFHS) rig/L Standard 173103AR-121 Sm(Mn,2x3) 04-Aug-2003 02:26:03 LCIMSIMS #6 MRM of 4 Channels ES- 8.9E 399 > 80 948t 5.49e4 Area , e I I I , I - I I 1 Time 10.00 12.00 3: C8 Sulfonate (PFOSI XCO72503-3,100 rig/L Standard 04-Aug-2003 02:26:03 LC/MS/MS #6 073103AR-121 10 % $ Sm (Mn, 2x3) MRM of 4 Channels ES- 9.27 499 > 99 6004 3.49e4 Area I Time 2.00 4.00 6.00 8.00 10.00 12.00 I Exyoen Research, 3058 Research Drive, State College, PA 16801 __ .--..1- 000204 - ----. ------------s--m- ------m-w Quantify SamQle Report %& Study No.:L34910, Set No.: 073103hR. Eact.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job code: P:\Data\LCMSMS6\Maaslynx\Fluorochemicals.PRO\S~leDB\O73lO3~ Tue hug 05 06:59:53 2003 P:\Data\L~SMS6\Masslynx\Fluoroch~cals.PRO\Met~R\~catur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 --m-p- Page 42 Decatur BC BC 080103 Nanm: 073103AR-121 Text : 4: PFOSA (CO72503-3,100 rig/L Standard 373103AR-121 Sm (Mn, 2x3) 04-Aug-2003 02:26:03 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 21221 490 > 78 1.12e5 Area O',",,"`,,.`..,,,,,,,,,,,`..`,.,.,,,,',,,,'.,.,, i-- Time 2.00 4.00 6.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000205 Quantify Sample Report q.# Study No.:L34910, Set No.. *073103AR, Ext.Date:07/31/03, Analyst:K.Risha sanQ1s List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluorochemicals.P~\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\Met~B\~catur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11x04:02 2003 Name: 073103AR-122 Text : I: C8 Acid (PFOA) L3491 O-l 2, DF=20 073103AB122 10 Sm (Mn, 2x3) 9.13 308911 %- Page 43 Decatur BC BC 080103 04-Aug-2003 02:47:47 LCIMWMS #6 MRM of 4 Channels ES413 > 369 1.81e6 Area Q ,,,~~,,,,,,,,,,,,,,,,,~,,,~,,,,~ 2.00 4.00 !: C6 Sulfonate (PFHSI L3491 O-l 2, DF=20 073103AFb122 Sm (Mn, 2x3) IIIII\/III I 1 I I I I I v 1 I I I I ,lTime 6.00 8.00 10.00 12.00 1 04-Aug-2003 02:47:47 LC/MS/MS #6 8.98 26169 I7 MRM of 4 Channels ES399 > 80 1.54e5 Area s L3491 O-l 2, DF=20 073103AR-122 10 Sm (Mn, 2x3) 9.25 64499 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.81 e5 Area o',,~,,,,,,,`,`,,`,,`,`,,,r,"`,`,,',,",,"',l' - -- I 2.00 4.00 6.00 8.00 Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0002OE Quantify Simple Report s& Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SXS6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 44 Decatur BC BC 080103 Name: 073103AR-122 Text : 4: PFOSA L3491 O-l 2, DF=20 073103AR-122 100- Sm (Mn, 2x3) %- 04-Aug-2003 0234734; LC/MS/MS #c MRM of 4 Channels ES- 9.88 490 > 7E 1.25ef Area 0 "","","","","","","","","", I , , , , , , , 1Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 kd 3 iL3.n ---------_--_-P ------------------m--w--- --- -------_ Quantify Swle Report &d Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\~ssl~\Fluorochamicals.PRO\S~leDB\O73lO3~ Tue Aug OS 06:59:53 2003 P:\Data\LCMSMS6\~sslynx\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 45 Decatur BC BC 080103 Name: 073103AR-123 Text : 1: C8 Acid (PFOA) 13491 O-l 2 Rep, DF=20 073103AFb123 IOO- Sm (Mn, 2x3) %- 04-Aug-2003 03:09:25 LCNWMS #6 MRM of 4 Channels ES413>369 I .84e6 Area 0 ~~~~~~~~,~~~`I~~~~I~~~~,"",`~","", , , v I , I , I , Time 2.00 4.00 6.00 8.00 10.00 12.00 _ : C6 Sulfonate (PFHS) .3491 O-l 2 Rep, DF=20 173103AFb123 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 03:09:25 LC/MS/MS #6 k;1RM of 4 Channels ES- 8.98 399 > 80 1.56e5 Area 3: C8 Sulfonate (PFOS) 13491 O-l 2 Rep, DF=20 073103AR-123 10 Sm (Mn, 2x3) 1 I , . , , I r 1 Time 6.00 8.00 10.00 12.00 9.25 64047 04-Aug-2003 03:09:24 LCYMWMS #6 MRM of 4 Channels ES499 > 99 3.75eS Area I/ 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 I -0a Research, 3058 Research Drive, State College, pA 36801. 000288 Quantify Sample Report w StuUy No.:L34910, Set No.. *073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LWSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemieals.PXO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-123 Text : Page 46 Decatur BC BC 080103 L3491 O-l 2 Rep, DF=20 073103AFk123 10 Sm (Mn, 2x3) %- 04-Aug-2003 03:09:25 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 23261 498>78 1.19e5 Area i Time Wgen Research, 3058 Research Drive, State College, PA 16801 000209 --- ----- ----- ---- ----- Quantify SanTQle Report \crl Study No.rL34910, Set No.. -073103A.R, Ext.Date:O7/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 ---Page 47 Decatur BC BC 080103 Name: 073103AR-124 Text : : C8 Acid (PFOA) -3491 O-l 5, DF=20 )73103AR-124 10 Sm (Mn, 2x3) 04-Aug-2003 03:31:09 LC/MS/MS #6 MRM of 4 Channels ES413>369 1.70e6 Area O',,,~_r,,,,,,,,,,,,,,,,,,,,~~,,,~,,,,,,,,,,~,, I I , I I Q I , I I I I 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 !: C6 Sulfonate (PFHS) L3491 O-l 5, DF=20 073103AR-124 10 Sm (Mn, 2x3) % i 8.98 25364 04-Aug-2003 03:31 :Od LCYMSIMS #6 MRM of 4 Channels ES- 399 > 80 1.46e5 Area 2.00 4.00 6.00 8.00 ' 10.00 12.00 I 3: C8 Sulfonate (PFOS) L34910-15, DF=20 073103AFb124 100- Sm (Mn, 2x3) %- 04-Aug-2003 03:31:05 LC/MS/MS #e MRM of 4 Channels ES499 > 96 3.74e5 Area ExyOen Research, 3058 Research Drive, State Collage, PA 16801 000210 ----w------e-- --------_I ----e-e---- -----v Quantify Sample Report w study No.:L34910, Set No.. -073103AR, Ext.Date:07/31/03, Analyst:K.Riarha Page 48 Sample List: Last modified: Method: Last modified: ?ob Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 __----- ----------------e---B-- ----- --- ------ Name: 073103AR-124 Text : 4: PFOSA L3491 O-l 5, DF=20 04-Aug-2003 03:31:0 073103AFb124 Sm (Mn, 2x3) 9.90 25908 498 > 78 1.30e5 Area 2.00 4.00 6.00 8.00 10.00 12.00 W Oxygen Research, 3058 Research Drive, State College, PA 16801 000211 Quantify Swle Report \IJ Study No.:L34910, Set No .:073103AR, Ext.Date:07/31/03, Analyst:K.Rieha Page 49 Santple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochamieals.PRO\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Bluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: --------h----P Wed Aug 06 11:04:02 2003 -----_ ------------------- Name: 073103AR-125 Text : L: C8 Acid (PFOA) L3491 O-l 3, DF=20 073103AFk125 lo9 % 4 Sm (Mn, 2x3) 9.13 3547x ) 04-Aug-2003 03:52:55 LC/MS/MS #6 MRM of 4 Channels ES413>369 2.09e6 Area !: C6 Sulfonate (PFHS) L3491 O-l 3, DF=20 IL-- Time 12.00 04-Aug-2003 03:52:55/ 073103AFb125 10 Sm (Mn, 2x3) 8.98 30673 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) IL3491 O-l 3, DF=20 (373103AFb125 10 Sm (Mn, 2x3) 04-Aug-2003 03:52:55 LCIMSIMS #6 9.25 7783: MRM of 4 Channels ES499 > 99 4.48e5 Area r I , I , I , I . r I , Time 10.00 12.00 Exygea Research, 3058 Research Drive, State College, PA 16801 000212 -------__ ---- mm-- ~-----__ -- Quantify Sample Report Study No .:L34910, Set No.: 073103AK Ext.Date:07/31/03, Analyst:K.Risha Page 50 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCblSMS6\~ssl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: wed Aug 06 11:04:02 2003 ----------------__-----------------------------------_ ----- Name: 073103A.R-125 Text : 4: PFOSA i-3491 O-l 3, DF=20 073103AR-125 I 1001 I --- i %- Sm (Mn, 2x3) 04-Aug-2003 03:52:55;' LCIMWMS #6 MRM of 4 Channels ES- 9.90 25736 498 ~78 1.29e5 Area 0 Jr~`,~,~`/,`~`,~I~~,`11',1~~//"II,~'~',~'I,,~~I 2.00 4.00 6.00 a.00 RJWgen Research, 3058 Research Drive, Stats College, PA 16801 000213 ---------------------------------------~--- ----- Quantify Sample Report ,4 Study No.:L34910, Set No.. *073103AR, Ext.Dats:07/31/03, Analyst:K.Risha Page 51 Sample List: Last modified: Method: LJz;tCzFfiad: : P:\Data\LCMSMS6\Hasslynx\Fluorochamicals.P~O\S~lsDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\FluorochemicalaB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: -____----------------- Wed Aug 06 11:04:02 2003 -______-___-----_------------------- Name: 073103AR-126 Text : 1: C8 Acid (PFOAI XCO72503-4,250 rig/L Standard 073103AFb126 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 04:14:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 7.35e5 Area Q ,,,,,~,.,.,,,,,,,,,,,,,,,.,,,,,,,,,,,,,,,,, , , . , , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 : C6 Sulfonate KO72503-4,250 (PFHS) rig/L Standard 04-Aug-2003 04:14:44 173103AFb126 10 Sm (Mn, 2x3) 8.96 21551 3: C8 Sulfonate XCO72503-4,250 (PFOS) rig/L Standard 073103AR-126 loo7 i % i Sm (Mn, 2x3) 2.00 4.00 9.27 1328s Time 12.00 _ 04-Aug-2003 04:14:42 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 7.65e4 Area Time 8.00 10.00 12.00 , -en Research, 3058 Research Drive, State College, PA 16601 00021.4 Quantify Sample Report w Study No.rL34910, Set No.: 073103AR, Ext.Dats:07/31/03, Analyst:K.Risha Page 52 Sqle List: Last nmdifiad: Method: Last modified: Job Code: P:\Data\~SMS6\~sslynx\Fluoroch~ca~S.PRO\SampleDB\073103A Tue Aug OS 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicalsc&tur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ----__----- wed Aug 06 11:04:02 v-s---- Name: 073103AR-126 Text : 2003 ---__--__-----------___l____________l___- : PFOSA (CO72503-4,250 rig/L Standard )73103AR-126 10 7 %14 Sm (MI-I, 2x3) 04-Aug-2003 04:-l 4:4ii LCJMSIMS #6 MRM of 4 Channels ES- 9.92 498>7a 4919f 2.56e5 Area Time Exygen Resaarch, 3058 Research Drive, State College, PA 16801 000215 --A----------s-------s---- Quantify Sample Report w Study No.:L34910, Set No. :073103AR, Ext.Date:07/31/03, ---- Analyst:K.Risha --- Page 53 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LQ3~S6\Masslynx\Fluorochsmicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: -----B----P Wed Aug 06 11:04:02 ---m----_-p 2003 ------------_- vm-------- Naxm: 073103AR-127 Text : 1 . C8 Acid (PFOA) a491 O-1 6, DF=lOO 173103AFb127 100- Sm (Mn, 2x3) % 9.13 82515 04-Aug-2003 04:36:3C LC/MS/MS #6 MRM of 4 Channels ES- 413>369 4.73e5 Area O-,,,~,,,,,,,.,,,.,,.,.,,,,,,,,,,..,,.,,,,~.,,~,,..,,,.:..,Time 2.00 4.00 6.00 8.00 10.00 12.00 c !: C6 Sulfonate (PFHS) 073103AFb127 Sm (Mn, 2x3) MRM of 4 Channels ES- - 3: C8 Sulfonate (PFOS) L3491 O-l 6, DF=l 00 073103AFb127 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 04:36:30 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.90e4 Area Bxygen Research. 3050 Research Drive, State College, PA 16601 000216 QuaId.fy Sample Report W Stucly No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 54 SaroQle List: Last modified: Method: Last modified: Job Code: P:\Data\L~:SMS6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\Masslynx\Bluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ------------- Wed Aug 06 11:04:02 2003 ------------------e-e-- ---------------- Name: 073103AR-127 Text : 4: PFOSA IL3491 O-1 6, DF=lOO 073103AR-127 Sm (Mn, 2x3) 04-Aug-2-003 04:36:3( LWvlS/MS #t MRM of 4 Channels ES498 5 7E 3.52& Ares Time 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000217 Quantify Sample Report t,& Study No.:L34910, Set No.: 073103AR, Ext.Dats:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug OS 06:59:53 2003 P:\Data\LCMSMS6\~ssl~\FluorochemicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 55 Decatur BC BC 080103 Name: 073103AR-120 Text : : C8 Acid (PFOA) -3491 O-l 6 Rep, DF=lOO )73103AR-128 10 Sm (Mn, 2x3) "j 04-Aug-2003 04:58:16 LC/MS/MS #6 9.13 836% MRM of 4 Channels ES413>369 4.68e5 Area Time 2.00 4.00 6.00 8.00 10.00 12100 b# 2: C6 Sulfonate (PFHS) L3491 O-16 Rep, DF=l 00 073103AR-128 100- Sm (Mn, 2x3) %- 04-Aug-2003 04:58:1 d LC/MS/MS #6 MRM of 4 Channels ES- 8.96- 6261 399 > 80 3.59e4 Area 0 ,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,~,~_,~,,,,,~~,ITime 2.00 4.00 6.00 3: Ca Sulfonate (PFOS) L3491 O-16 Rep, DF=lOO 073103AR-128 10 4 Sm (Mn, 2x3) 8.00 / 9.27 17264 10.00 12.00 . 04-Aug--2003 04:58:1 d LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.56e4 Area W L wgen Research, 3058 Research Drive, State College, PA 16801 -,- .-III"_"x.-, I- ll.".l,",", -- _. .--.-" -.-. ^-- - 000228 Quantify Sample Report cy Study No.:L34910, Set No.: 073103AR, &.Date:07/31/03, Analyst:K.Risha Page 56 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\Masslynx\Fluoroch~c~ls.PRO\S~l~DB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\Massl~\Fluorochemical\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ----------- Wed Aug 06 11:04:02 2003 -w-m-- ----- --- ----- ---w---w--___ Name: 073103AR-128 Text : 4: PFOSA L3491 O-l 6 Rep, DF=lOO 073103AFb128 Sm (Mn, 2x3) 04-Aug-2003 04:58:1 t LC/MS/MS #c MRM of 4 Channels ES498 > 7.5 3.19e4 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 %d Exygen Research, 3058 Research Drive, State College, PA 16801 - -" ..-..- -.- -._ 000219 Quantify Sample Report td Study No.:L34910, Set No.: 073103AX, Xxt.Date:07/31/03, Aualyst:K.Risha Page 57 San&e List: Last modified: Method: Last xmdified: Job Code: P:\Data\LQISblS6\Maaslynx\Fluorochemicals.PXO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCM[SMS6\Masslynx\Fluorochemical\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: --es- Wed Aug 06 11:04:02 2003 -------------_-----------------------~----------- ----s---e- Name: 073103AX-129 Text: : C8 Acid (PFOA) -3491 O-l 9; DF=l 00 173103AFb129 Sm (Mn, 2x3) 10 % 1 Ol"..,".`,`.`.,`~`~,~ 2.00 9.13 75424 ~`J,~`~`,`(( 4.00 6.00 1,s I'#,# 1,s 8.00 04-Aug-2003 05:20:01 LChlS/MS #6 MRM of 4 Channels ES413>369 4.39e5 Area , I ,, 10.00 , I Time 12.00 W 2: C6 Sulfonate (PFHS) IL3491 O-l 9, DF=lOO I073103AR-129 10 Sm (Mn, 2x3) 04-Aug-2003 05:20:01 LCIMSIMS #6 MRM of 4 Channels ES- 8.96 399 > 80 6156 3.49e4 Area 3: C8 Sulfonate (PFOS) L3491 O-l 9, DF=lOO 073103AR-129 lOtI- Sm (Mn, 2x3) %- Time 12.00 04-Aug-2003 05:20:01 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.96e4 Area 0 ,,,/,,,,,/~1,,,,,/,,/III,1111(~111,111I,~I I . , 1 I I , Q I I 1 1 Time W- 2.00 4.00 6.00 8.00 10.00 12.00 NWgen Research, 3058 Research Drive, State College, PA 16801 000220 Quantify Sample Report Study No.: L34910, Set No.: 073103AR, Ext.Date:07/31/03, +4 Analyst:K.Rieha S7mple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluorochsmicals.P~\S~leDB\O73lO3~ Twe Aug 05 06:59:53 2003 P:\Data\LCMSMSb\Masslynx\Fluorocheuaicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Page 58 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 ----- --------------v------- --m----d-- ------ ----- Name: 073103x+129 Text: 4: PFOSA L3491 O-l 9, DF=l 00 073103AR-129 Sm (Mn, 2x3) 04-Aug-2003 05:20:0' LC/MS/MS #E MRM of 4 Channels ES498 > 7E 3.33eL Are: Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000221 Quantify Sazqple Report '4 Study No. : L34910, Set No.:073103AR, Ext.Dats:07/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\bfasslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\Masslynx\Bluorochamical\Met~B\D~catur .Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 59 Decatur BC BC 080103 Name: 073103AR-130 Text : 1: C8 Acid (PFOA) 1-3491 O-l 7, DF=lOO 173103AFb130 100 Sm (Mn, 2x3) 9.13 78536 i 04-Aug-2003 OS:41 :44 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 4.61 e5 Area ). C6 Sulfonate (PFHS) i3491 O-l 7, DF=l 00 373103AB130 `O@l Sm (Mn, 2x3) I 8.98 6030` Time 12.00 04-Aug-2003 05:41:4 LCNWMS # MRM of 4 Channels ES399 > 80 3.55e4 Area : 3: C8 Sulfonate (PFOS) L3491 O-l 7, DF=lOO 073103AR-130 Sm (Mn, 2x3) 9.25 16123 04-Aug-2003 05:41:49 IX/MS/MS #6 MRM of 4 Channels ES499 > 99 9.43e4 Area b Time Exygen Research, 3058 Research Drive, State College, PA 16801 000222 Quantify Sample Report `d' Study No.: L34910, Sat No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Sample List: Last modified: Method: Laat modified: Job Code: P:\Data\LWSMS6\biaaslynx\Fluoroch~ca~s.PRO\S~leDB\O73lO3~ Tue hug 05 06:59:53 2003 P:\Data\LC1MSMS6\~sslynx\FluorochemicalB\Decatur Sun hug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 60 Decatur BC EC 080103 Name: 073103AR-130 Text : 4: PFOSA L3491 O-17, DF=lOO 073103AR-130 Sm (Mn, 2x3) 04-Aug-2003 05:41:49 LC/MS/MS #6 MRM of 4 Channels ES490 B 78 3.01 e4 Area Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0002'23 -----_-e-------------m -------- m------ Quantify s-10 Report 'J Study No .:L34910, Set No .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha SamQle List: Last modified: blethod: Last modified: Job Code: P:\Data\LCM~S6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73~03~ Tue Aug 05 06:59:53 2003 P:\Data\LQ3SMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 61 Decatur EC BC 080103 Printed: --------------------- Wed Aug Name: 073103AR-131 Text : 06 11:04:02 2003 -----__~--__----~------~-~~~ P---Y- 1: C8 Acid (PFOA) XCO72503-5,500 rig/L Standard 073103AFb131 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES- 9.15 413>369 1.53e6 Area *J 2: C6 Sulfonate (PFHS) XCO72503-5,500 rig/L Standard 073103AFb131 10 Sm (Mn, 2x3) % 8.96 45496- 04-Aug-2003 06:03:36 LCh/lSh/lS #6 MRM of 4 Channels ES399 > 80 2.61 e5 Area I-- ~~I~~~' 1~>~~1 I? raI, rx!I' *X,1 `rma I>ss k~~`.~~..l!~~~l Time - 2.00 4.00 6.00 8.00 10.00 12.00 _ 3: C8 Sulfonate XCO72503-5,500 (PFOS) ng./L Standard 073103AFb131 10 Sm (Mn, 2x3) 9.27 28469 04-Aug-2003 06:03:36 LCYMSIMS #6 MRM of 4 Channels ES499 > 99 1.62e5 Area j , I I I , 1 I I q 1Time 10.00 12.00 _ Exygen Research, 3058 Research Drive, State College, PA 16801 000224 -v-----_- B-e- -- Quantify Sample Report Study No.:L34910, Set No.: 073103hR, Ext,Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Maaalynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\MSMSMS6\Masslynx\FluorochsmfcalPB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 62 Decatur BC BC 080103 Name: 073103A.R-131 Text : 4: PFOSA XCO72503-5,500 rig/L Standard 073103AR-131 IOO- Sm (Mn, 2x3) %- 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1 0229z7 5.22e5 Area o-,,,,,,,,.,,.,,,,,,.,~,,,,.,.,,,,,.,,,,,,,,,~,.,. I , , I , , , 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 W!Jen Research, 3058 Research Drive, State College, PA 16801 000225 Quatify Sample Report w Study No.:L34910, set NO.. .073103AR, Ext.Date:07/31/03, Analyat:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCblSMS6\Wassl~\Fluorochgmicals.PRO\S~leDB\O73lO3~ !tUe Aug 05 06:59:53 2003 P:\Data\LCMSMS6\~asslynx\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 63 Decatur 8C BC 080103 Name: 073103AR-132 Text: 1: C8 Acid (PFOA) L3491 O-l 6, DF =20 073103AW132 lOO- Sm (Mn, 2x3) %- 9.13 _ 380900 04-Aug-2003 06:25:24 LCNWMS #6 MRM of 4 Channels ES413 > 369 2.20e6 Area 0 ,,,~~~~~,,,,,,,~,,,,,,,,r,~,,,,,,,,,.,,,, III 2.00 4.00 6.00 8.00 10.00 12.00 : C6 Sulfonate (PFHS) 8.96 33004 I 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.86e5 Area L 2.00 3: C8 Sulfonate (PFOS) L3491 O-1 6, DF=20 073103AR-132 lOO- Sm (Mn, 2x3) %- I 8.00 10.00 Time - 12.00 _ 9.26 _ 81862 04-Aug-2003 06:25:24 LCNSIMS #6 MRM of 4 Channels ES499 a 99 4.68eS Area 0 ~~J~,~",,`~)`,`~~~1'~"I""I""I""l""I , I , I I , I l Time w 2.00 4.00 6.00 8.00 10.00 12.00 , qgen Research, 3058 Research Drive, State College, PA 16801 000226 ----- ------- -- -------_ Quantify Saraple Report u Study No.:L34910, Set No.: 073103&R, Ext.Date:07/31/03, Analyst:X.Risha Page 64 S~19 List: Last modified: Method: Last modified: Job Code: P:\Data\LCPISbiS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ me hug 05 06:59:53 2003 P:\Data\L~SMS6\blasslynx\Pluorocheunicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: wed Aug 06 11:04:02 2003 ----------- --I_--------------- ----------e-----F-_ -- Name: 073103AFl-132 Text : 4: PFOSA IL3491 O-l 6, DF=20 073103AFb132 100- Sm (Mn, 2x3) %- 04-Aug-2003 06:25:24 LC/MS/MS #f MRM of 4 Channels ES- 9.89 498 > 7t 1.64e! Are2 Oxygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report u Study No.:L34910, Set No.: 073103AR, Ext.Dats:07/31/03, knalyat:K.Risha Sample Liat: Last modified: Method: Last modified: Job Code: P:\Data\L~flulS6\Massl~\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:03 2003 Page 65 Decatur BC BC 080103 Name: 0?3103AR-133 Text: : C8 Acid (PFOA) -3491 O-16 Rep, DF=20 )73103AR-133 Sm (MIT. 2x31 9.12 391789 04-Aug-2003 06:47:22/ LC/MS/MS #6 MRM of 4 Channels ES413>369 2.26e6 Area \a& 2: C6 Sulfonate (PFHS) L3491 O-l 6 Rep, DF=20 073103AW133 Sm (Mn, 2x3) %- 2.00 3: C8 Sulfonate (PFOS) L3491 O-l 6 Rep, DF=20 0?3103AR-133 Sm (Mn. 2x3) , , , , , I , , , I , , Time 6.00 8.00 10.00 12.00 04-Aug-2003 06:47:22 LC/MS/MS #6 MRM of 4 Channels ES- 8.97 399 > 80 1.81e5 Area I I , I I I , I 1 I I 1 Time 10.00 12.00 9.25 84263 I 04-Aug-2003 06:47:22 LWMSNS #6 MRM of 4 Channels ES499 > 99 4.80e5 Area 2.00 4.00 6.00 8.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 a- ---------p- ----- --- Quantify Sample Report 14 Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 66 Saqple List: Last modified: Method: Last modified: Job Code: P:\Data\~SMS6\Masslynx\Fluoroch~cals.PRO\S~~eDa\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur EC BC 060103 Printed: -----------------c-- wed Aug 06 11:04:02 2003 -------------_------ --------m----e_- Name: 073103AR-133 Text : I4: PFOSA L3491 O-16 Rep, DF=20 073103AFb133 100- Sm (Mn, 2x3) %- 04-Aug-2003 06:47:22 LC/MS/MS #6 MRM of 4 Channels ES- 9.91 _ 31916 496 > 78 t .61e5 Area 0 /Il~,llll/llrl,llll/~ll,,,~/~,lll,,lll,,llll/lll , , , , , , , 1 Time 2.00 4.00 6.00 a.00 10.00 12.00 W Oxygen Research, 3056 Research Drive, State College, PA 16801 000229 ------c-----_I----II____ -- ---- ----- Quantify Sample Report w Study No.:L34910, Set No.: 073103JUI, Ext.Date:07/31/03, AnalystrK.Rieha Page 67 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PR0\SampleDB\073103A Tue Aug 05 06:59:53 2003 P:\Data\M3MSMS6\Hasslynx\Fluorochamicals\Decetur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 -------_--------------__l________________l Name: 073103xm-134 Text : -------w-e- I: CfI Acid (PFOA) L3491 O-1 9, DF=20 073103AR-134 loo- Sm (Mn, 2x3) %- 04-Aug-2003 07:09:05 LCIMSIMS #6 MRM of 4 Channels ES413 > 369 2.02e6 Area 0 ,,,,~,,~,,~,,,,,,,,,,,,,,,,,I,~,,,,,,~, , , , , , , , , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 : C6 Sulfonate (PFHS) -3491 O-1 9, DF=20 )73103AR-134 10 Sm (Mn, 2x3) 8.96 2921 E3 04-Aug-2003 07:09:05 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.65e5 Area 2.00 3: C8 Sulfonate (PFOS) L3491 O-l 9, DF=20 073103AFb134 loo- Sm (Mn, 2x3) %- I 8.00 10.00 Time - 12.00 04-Aug-2003 07:09:05 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.64e5 Area 0 ,`,,"`,,`,",""i',","","`l,"","", I I , I r I , r I I I 1 Time w _ 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ..--- --. --- .- - 000230 Quantify Sample Report cw Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\Hasslynx\Fluorochamical\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 68 Decatur BC BC 080103 Name: 073103AR-134 Text : 4: PFOSA L3491 O-1 9, DF=ZO 073103AR-134 100- Sm (Mn, 2x3) %- 04-Aug-2003 07:09:0 LChrWMS #$ MRM of 4 Channels ES- 9.90 _ 32869 498 > 78 1.88e5 Area 0 ""I"","","","","","","",,"`,"' I I I 8 I I Time 2.00 4.00 8.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ^.I -t.i,.l.".-lll ----. 000231 Quantify Samgle Report Study No.: L34910, Set No .:073103A.R, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L(1MSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\FluorochemicalsB\Decatur Sun Aug 03 07:11:59 2003 Printed: wed Aug 06 11:04:02 2003 Page 69 Decatur BC BC 080103 Name: 073103AR-135 Text: .: C8 Acid (PFOA) -3491 O-1 7, DF=20 173103AR-135 Sm (Mn, 2x3) I. 9.11 I3_ 362892 04-Aug-2003 07:30:42 LC/MS/MS #6 MRM of 4 Channels ES413 2.>083e669 Area 1 2.00 Vd .?: C6 Sulfonate (PFHS) L3491 O-l 7, DF=20 073103AR135 lOO- Sm (Mn, 2x3) 8.00 8.96 10.00 Time 12.00 _ 04-Augi2003 07:30:4 %- 0 /lll,lll~,/I~/,III.,llll,llll,l,ll,II,l,lll , , , , , , , , , , , , ,Time 2.00 4.00 6.00 8.00 10.00 12.00 - 3: C8 Sulfonate (PFOS) L3491 O-17, DF=20 073103AFG135 loo- Sm (Mn, 2x3) %- 04-Aug-2003 07:30:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 4.44e5 Area 0 "",",`,"","`1,"","",1"`,~"`," , , , , , , , , , ,,Time 2.00 4.00 6.00 8.00 10.00 12.00 VW Exygen Research, 3058 Research Drive, State College, PA 16801 000232 Quantify Sample Report tws~ Study No.:L34910, Set No.: 073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LM~S6\Maaalynx\Fluorochemiea~s.PRO\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\LCHSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\~catur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Pag's 70 Decatur BC BC 060103 Name : 073103AR-135 Text : 4: PFOSA L3491 O-1 7, DF=20 073103AR-135 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 07330342 LCYMSIMS #6 MRM of 4 Channels ES- 9.91 498 > 78 1.33e5 Area 0 "","","",""i"","","","",""," , I I 1 ITime 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000233 --- ------e-v----- --e--m ------ -mm---- Quantify Sample Report I& Study No.:L34910, Set No.. -073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 71 Sany7le List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\O73103~ Tue Aug 05 06:59:53 2003 P:\Data\L~SMS6\Massl~\FluorochamicaB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: --------------__m__ Wed Aug 06 11:04:02 2003 ---------_--------I_-__-_ ---- --w-e-- Name : 073103AR-136 Text : : C8 Acid (PFOA) (CO72503-6,lOOO rig/L Standard 173103AFb136 10 Sm (Mn, 2x3) % 9.12 477931 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 2.78e6 Area i !: C6 Sulfonate (PFHS) KC072503-6,lOOO rig/L Standard 073103AR-136 10 Sm (Mn, 2x3) L a.96 80818 Time 12.00 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 4.81e5 Area I 0 "",,`,`,,.,..",`,.,,,,`.,.,,.,,,,,..,,'.i 2.00 ' 4.00 6.00 hm 8.00 10.00 Time 1 12.00 ] 3: C8 Sulfonate (PFOS) XCO72503-6,lOOO rig/L Standard 04-Aug-2003 07:52:21 LC/MS/MS #6 073103AR-136 Sm (Mn, 2x3) MRM of 4 Channels ES- 100-J 499 > 99 3.02e5 Area %- 0 ~"`,`~`~,~"`,~~"/`~~`i~~~`l~`~~I~~~~I~~"I , , , , I , , , I mlTime 2.00 4.00 6.00 8.00 10.00 12.00 W' Oxygen Research, 3058 Research Drive, State College, PA 16801 000234 Quantify Sample Report q,d Study No.:L34910, Set No.: 073103bR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluoroch~cals.PRO\S~leDB\O73lO3~ Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicalscatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 72 Decatur BC BC 080103 Name : 073103AR-136 Text : 4: PFOSA XCO72503-6,lOOO rig/L Standard 073103AR-136 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 _ 190680 498 > 78 9.76e5 Area 0 ~~~~,~~~/,"~~,I,~~,~~I~,,~~),`~~1,,/(~,'~~I,~~~ Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 00023s SQOnlor Study No: Exygcn Sludy No: AnalytC lous Monitotd: Sk NA l34910 PFOS 499~>99 Decaw Baker's Cnek RAW DATA REPORT Limit of Quai-ltiladoo: bjecdoa Volum: MUSiX Sample Volume: Fd Vohm: JO PP' 15rr. Water 40.0 mL 5.0 mL Set No: Analyst: lnst~ment Exfracdoa Analyrad Typ: Dar&: w: 080603A Karen Risba LCJMS/?.iS Unit U 6 07r31/03 & 08/06K'3 08fwO3 fiYt?CO m xc0725030 xco72503-I XCO72SO3-2 xco77503-3 xco72503-4 XCO72503-s XCO72503-6 0106020 control OlC6020 Spk A 01064213 Spk B W4910-12 Spk E W910-16 Spk F L34910-16 SQk F xco72Jo3-1 XCO72503-2 xco72103-3 u4910-I W4910.1 Rep w4910-12 W4910-12Rcp l34910-15 w4910.13 xCO72503-4 XCO72JO3-J XCO71003-6 SQonsor m BC2 SW-06 cutfall to River SW-U CkItNl lo River SW-l.5 BQ SW-04 BQ SW-04 BCZ SW-06 BCZ SW-W BC2 SW-06 Dup BQ SW-06 Low Spk Sample cc& cs c-9 cs cs cs cs cs C La LC.S LF LF LF cs cs cs S S S S S FF cs cs cs Analytc Rmvery Found (ppb (%I = = (peak ama - intercept) / alopc x DF InnalYU found (pp0-iloalyu found in cootml anmum added (pit) RUlI NO. 080603A-1001 080603A-3002 080603A-1003 080603A-1004 080603A-1005 080603A-1006 080603A-lW7 080603A-lW8 080603A-IM)9 080603A-1010 080W3A.1011 080603A.1012 080603A.1013 080603A.1014 080603A-1015 080603A-1016 080603A-1017 080603A-1018 OEO&l3A-1019 080603A.1020 080603A.1021 080603A-1022 080603A.1023 080603A-1024 OE4l603A-1025 (QQt)] x ml Std. cont. Dilution (QQl) Factm 0 25 50 100 250 loo ILXSI I 1 1 100 2w 1W 2s SO loo 100 100 IW 1W IW loo 2SO 500 IMJO Peak AKn 0 1238 2170 6155 105Jl 22336 43039 0 2436 21693 22031 18543 35655 1229 2338 4928 5143 523s 11612 11877 11205 14257 10803 23323 4427 I Analytc Fouad (QPt) AilXHlnt Added (PQt) Recovery (5) ND 51.3 SO 103 490 SW 98 49800 mw 9s l 5oow 80900 mwo 99 lI5W IlSca 26100 26700 25100 32100 100 Sllndard h&`CCQ~ SOQC Cal. Of Dct. : Linear (I/x = 184.312 = 43.8624 = 0.998804 weighted) CS = Calibration frpndard C = Cma0i umplc s = Sample CK = Clvck Standard ND = No( dctexcd NQ = Nor quamifinble I Rcsponv betw~n 0 md 2S ppr = Reapawe between 25 ppr nod LOQ (SO ppt) l !hmple +Samplc WY analyzed with sevwal dilution factors. The lppopriatc ruiduc signifcmtly cxcccda the spiking level; tbcrefore, result is reported. an accurate recovery cancat be calculated SprePdtbctt pnpmd by: 000236 n I" EAKCH 3058 Research Drive State College, PA 16801 Internal Chain of Custody/Fortification Exygen Study Number: Sponsor StudyProtocol No: The samples listed below were removed from refrigerator No, Tie 1030 Sheet Matrixr Phone: 814-272-1039 Fax: 814-231-1580 Water t All samples were measured: Time !Z`kJ Date bB)cd!b3 After measuring samples were returned to refrigerator No. .a Time \XS Date ~%!&!a3 Initials COKImenkX 200 pL of 250 mghL sodium thiosulfak was added to all aamplo bcfcm spiking. lni~i~ls/Da~: Analysis Summary: Data Set: m Data Set: - Data Set: - Set extraction/analysis data verified by: n-E.4 R C H 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 EXYGEN STUDY SAMPLE EXTIUCTION NUh%BER: L3491 Q MATRIX: J&&g AND ANALYSIS TRACKING SHEET METHOD: I' ANALYTES: PFHS. PFOS. PFOA and PFOSA PROTOCOL NUMBER: NA STEP Dilutions STEP 3 WJW 4 \ / e i ReagentsI Materials hfnbaaol Ct8 SPE Type I Wnta Lot # IIizmE uJ31 I2l31 NA I I - I InitiaMDatr I I 1 -I-I-I I - I I I I I I t, I- kziiim- HPt Mcdlanol Ammonium Acetate v3(asc1 TypeIwater NA InitialsDate STEP 1: SPE column cltzm-up (omitting 40% wash) STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes OhF: Km 2&a. ca)403 % STEP 3: LCYAWMS analysis STEP 4: Lcxwhfs reaualysia. 00 *Initials and date under each step indicates the personnel that perfotmed this step. $$ Method of Anafysis for the ~~~ina~on of Perfluorooctane sulfanate (PFOS), Pctfluomoctane sulfonylamide (PFOSA). and Perfluorocctanoate (POAA) in Water COhMENTS: Final extracts stored in refrigerator 32 Initials: j&Date: @!-j&v! 03 July 19.2001/4 Masslynx - Sample List Sample List: Printed: Wed Aug 06 13:15:20 2003 Exygen STUDY NO. C3ct"llO __-- -.- Vial File Name LlMS ID Client ID Sample Description Matrix Sample Type Cone (ng&@%!f?!?nc 1 41 080603A-1001 -- -- XCO72503-0,O nglL Standard Standard 0 -. 2 42 080603A-1002 --- -. XCO72503- 1,25 rig/L Standard -. Standard 25 -. 3 43 080603A-1003 --- -. XCO?2503-2.50 nglL Standard . . . Standard 50 -. 4 44 080603A-1004 -- -.. XCO72503-3. 100 rig/L Standard --- Standard 100 - 5 45 080603A-1005 --- -. XCO72503-4. 250 rig/L Standard --- Standard 250 - 6 46 080603A-1006 --- -- XCO72503-5.500 t-q/L Standard -- Standard 500 -- 7 47 080603A-1007 --- XCO72503-6. 1000 rig/L Standard -- Standard 1000 -. 8 51 080603A-3008 -- 01 06020 Control -. Blank -- -. 9 52 080603A-1009 -- 0106020 Spk A, 50 rig/L .. . QC 100 -. 10 53 080603A-1010 --- -. 0106020 Spk B, 500 iq/L -. 500 -. 11 54 080603A-1011 -- - L34910-12 Spk E. 25000 rig/L. DF=IOO -- :: 25000 -. 55 080603A-1012 - -. L34910-16 Spk F, 50000 rig/L. DF=200 -- 50000 -. :i 56 080603A-1013 -- L34910-16 Spk F, 50000 rig/L. DF=lOO --- :: 50000 -. 42 080603A-1014 -- - XCO72503-1.25 rig/L Standard . . . Standard 25 --. :`: 43 080603A-1015 - - XCO72503-2.50 rig/L Standard -. Standard 50 - 16 44 080603A-1016 -- - XCO72503-3. 100 rig/L Standard -- Standard 100 -. $7 57 080603A-1017 -- -- L34910-1. DF=lOO -. Analyte -. -. 58 080603A-1018 -- -. L34910-1 Rep, DF=lOO - Analyte -. --. :t 59 080603A-1019 -- - L34910-12, DF=lOO -. Analyte - --. 20 60 080603A-1020 -- L34910-12 Rep, DF=lOO -. Analyte -. -. 21 61 080603A-1021 -- - L34910-15, DF=lOO . .. Analyte -. -. 22 62 080603A-1022 -- -. L3491@13, DF=lOO - QC 100 -. 23 45 080603A-1023 -- -. XCO72503-4,250 rig/L Standard - Standard 250 -. 24 46 080603A-1024 -- XCO72503:5.500 rig/L Standard -- Standard 500 -. 25 47 080603A-1025 -- .- XCO72503-6, 1000 rig/L Standard -- Standard 1000 . . . Page 1 Page Position: (1, 1) C Test ID DF - 0 - - x - 0 .- 0 . . . - t: . . . 0 - 0 . . . 0 .- 0 .- - x . .. 0 - .I : -. 0 - 0 .- 0 .- 0 .- 0 .- 0 .- 0 .- 0 .- 0 1 1 1 : 1 1 1 1 :oo 200 100 1 : 100 100 100 100 100 100 1 1 1 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroche Printed: Wed Aug 06 13:15:20 2003 .PRO\SampleOB\080603A Decatur BC.SPL MS Method HPLC Method MS Tune File Inj.Volume 1 C6 C8 SULF C8 ACID PFOSA 2 C6 C8 SULF C8 ACID PFOSA 3 C6 C8 SULF C8 ACID PFOSA 4 C6 C8 SULF C8 ACID PFOSA 5 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA ; C6 CB SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA ii C6 C8 SULF C8 ACID PFOSA 10 C6 C8 SULF C8 ACID PFOSA 11 C6 C8 SULF C8 ACID PFOSA 12 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA :: C6 C8 SULF C8 ACID PFOSA 15 C6 C8 SULF C8 ACID PFOSA 16 C6 C8 SULF CB ACID PFOSA 17 C6 C8 SULF C8 ACID PFOSA ia C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C-8 ACID PFOSA ;i C6 C8 SULF C8 ACID PFOSA 21 C6 C8 SULF CB ACID PFOSA 22 C6 C8 SULF C8 ACID PFOSA 23 C6 C8 SULF C8 ACID PFOSA 24 C6 C8 SULF C8 ACID PFOSA 25 C6 C8 SULF C8 ACID PFOSA pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water Fluorochems 15 Fluorochems Fluorochems :z Fluorochems 15 Fluorochems 15 Fluorochems Fluomchems iz Fluorochems Fluorochems :2 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems Fluorochems 1; Fluorochems 15 Fluorochems 15 Fluorochems 15 F lwrochems 15 Fluorochems Fluorochems :z Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 ~xYtiX)n STUDY NO. m'+? 10 Page 2 Page Position: (2. I) , . LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exxen Studs No: L34910 Instrument: Micromass Quattro Ultima (LUMSIMS Unit #6) Computer: COMPAQ Professional Workstation Al'200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HPBinPump HP Vacuum Degasser HP Autosampler HP Column Oven . HPLC Column: Genesis C-8.5 cm x 2.1 mm id. x 4 p (Exygen ID: 74A) (JONESCHROMATOGRAFWY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by: I(&3 v '* 000241 .,& Scanning Method Report Method: Last Modified: C:\MASSLYNX\FLvOROCHEMICALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 Printed: Wed Aug 06 13:15:53 2003 Page 1 C8 SULF C8 ACID PFOSA Solvent Delay ( mins ) : 0.00 Analog Channel Function : 1 4 : Unused MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Sets ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Sets) Co11 Energy 1 399.00 80.00 0.20 35 2 413.00 369.00 0.20 10 3 498.00 78.00 0.20 30 4 499.00 99.00 0.20 40 (eV) Cone ( V ) 50 10 .50 . 30 000242 Method Report Method File: Last Modified: qur) Printed: C:\MASSLYNX\FLUOROCHEXICALS.PRO\ACQUDB\pfbs Wednesday, August 06, 2003 13:15:26 Wednesday, August 06, 2003 13:16:00 HP1100 LC Pump Initial Conditions Solvents A% 90.0 B% 10.0 C% 0.0 D% 0.0 Flow (ml/min) Stop Time (mins) Min pressure (bar) Max Pressure (bar) Oven Temperature Left lC) Oven Temperature Right(OC) 0.300 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time A% 0.00 90.0 2.00 90.0 5.00 10.0 9.00 10.0 9.50 0.0 14.00 0.0 14.50 90.0 20.00 90.0 8% 10.0 10.0 90.0 90.0 100.0 100.0 10.0 10.0 C% D% Flow 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 water Page 1 b@i,lIG Pressure 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contact1 Off On Off Off Off Off are : Contact2 Off Off Off On Off Off 'Contact3 Off Off Off Off On 'Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(pl) Vial Number Conditions 200.0 200 0.50 20.00 15.0 82 000243 hd Tuning Method Report Method: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS Printed: Wed Aug 06 13:19:13 2003 Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set Rdbk 3.00 -2.93 20 -43 0.0 0.0 0.0 100 99 300 299 Rdbk OFF 4 .Oe-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 24 15 29 2 27 14.0 14.0 2.0 650 -646 R&k 132.1 770.3 000244 Quantify Calibration Report \rrf Study No. :L34910, Set No.: 080603A, Ext.Date:07/31 br 06/06/03, Analyst:K.Risha Page 1 Calibration: Last modified: Printed: --------- P:\Data\LCMSMS6\MassLynx\Fluorochamicals.PRO\~~eDB\O60603A Thu Aug 07 12:27:57 2003 Thu Aug 07 12:49:55 2003 Y-w---- --_-----___ Decatur BC --------_ Compound 1 name: C8 Sulfonate (PFOS) 2oefficient of Determination: 0.998804 >alibration curve: 43.8624 l x + 184.312 qesponse type: External Std, Area kwve type: Linear, Origin: Exclude, Weighting: 4.43e4 l/x, Axis trans: None Response 0.0 ExMen Research, 200.0 400.0 600.0 3058 Research Drive, State College, PA 16601 800.0 1000.0 000245 Quantify Sample Report w Study No.:L34910, Set No .:080603A, Ext.Date:07/31 bc 08/06/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SllrS6\1sslynx\Fluoroch~cals.PRO\S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masolynx\Fluorochemica~s.PliO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: -__------------- Thu Aug 07 12:49:56 ----- 2003 -----------------1---- e--w--------- Name : 0806031-1001 Text: 1: C8 Sulfonate (PFOS) XCO72503-0,O rig/L Standard 06-Aug-2003 14:57:47 K/MS/MS #6 MRM of 4 Channels ES499 > 99 1.71e3 0 "","","",""l"","",""l"","","","","" Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000246 Quantify Sample Report bJ Study No.:L34910, Set No.: 080603A, Ext.Date:07/31 k 08/06/03, Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\bIasslyruc\Fluoroch~cals.PRO\S~leDB\~aO6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MetbDB\PFOS Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 Analyst:K.Risha Page 2 Decatur Bc o111y 080603 Name: 080603A-1002 Text : 1: (?8 Sulfonate XCO72503-1,25 (PFOS) rig/L Standard 080603A-1002 lOO- Sm (Mn, 2x3) %- 9.35 ._ 06-Aug-2003 15:19:26 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 5.57e3 Area P;K;ygen Research, 3058 Research Drive. State College, PA 16801 000247 --- ---L-_--__---__--____I ----- ------P--P_- Quantify Sample Report uk) Study No.:L34910, Set No.: 080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 3 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQiSMS6\Masslynx\Bluoroch~cals.PRO\S~leDB\O80603A Thu Aug 07 08:12:#8 2003 P:\Data\LCMSMS6\Masslynx\F~uorochamicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 X2:49:56 2003 -------- --------------------_______I_____I______------ I_----- Name : 080603A-1003 Text : .: CB Sulfonate tCO72503-2,50 (PFOS) rig/L Standard 06-Aug-2003 15:4l :O-/ LC/MS/MS #6 9.32 , 257( I MRM of 4 Channels ES499 > 99 1.18e4 Area I; Time c Oxygen Research, 3058 Research Drive, State College, PA 16801 000248 Quantify Sax&e Report w Study No.: L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 4 Sample List: Last modified: Method: Last modified: Job Cods: P:\Data\~CMSMS6\MasslyPx\FluOroch~cals.PRO\S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\~ssl~\Fluorach~cals.PRO\~et~B\P~OS Thu hug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 ---------------------------------------------------~ --------_ Name : 080603A-1004 Text : L: C8 Sulfonate KC072503-3,100 (PFOS) q/L Standard 080603A-1004 loo- Sm (Mn, 2x3) %- 06-Aug-2003 16:02:51 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.99e4 Area 0 ,,,,~,,,.,.,,,,,.,..,,,,,.,,....,.,.,,.,. , , r , I , , , , Time 2.00 4.00 6.00 8.00 10.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 0002a9 ------se- ------------------ ----------- Quantify Szuqple Report w Study No.:L34910, Set No.: 080603A. Ext.Date:07/31 & 08/06/03, -- m-------_ Analyst:K.Rieha Page 5 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQ3SlrlS6\Masslynx\Pluaroch~cals.PRO\S~leDB\O80603A Thu Aug 07 08:12:08 2003 P:\Data\LCbISMS6\Masslyw\Fluorochemicals.PRO\~et~B\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 ------------------------__I_________________--_-_____- Name: 080603A-1005 Text : L: C8 Sulfonate KC072503-4,250 (PFOS) rig/L Standard 080603A-1005 10 %$-I Sm (Mn, 2x3) 06-Aug-2003 16:24:39 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.71 e4 Area Time Oxygen Research, 3058 Research Drive, State College, PA 16801 "l_ll--_l--(l.-c-- ---_^ ._" ._^_I - 000250 ---I_------- ------- ---I_- ------- Quantify Sample Report \& stuay k.:L34910, set No.: 000603A, Ext.Date:07/31 6 08/06/03, Analyst:X.Risha Page 6 Saraple List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\bla8sl~\Fluoroch~cals.PRO\S~leDB\O6O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur EC only 080603 Printed: ------mm- Thu Aug 07 12:49:56 2003 ----------------____ Name: 0806031-1006 Text : -------- --we------_-------___ L: C8 Sulfonate KC072503-5,500 (PFOS) rig/l Standard 080603A-1006 `Oq %-4 Sm (Mn, 2x3) 9.31 22336 06-Aug-2003 16:46:17 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.64e4 Area L Time Exygen Research, 3058 Research Drive, State College, PA 16801 ..-. .~---.----_.-.~~ -w-(_l_ll-. -_..- ._._~..__ ----- 000251 Quantify Sample Report ll(rc, Study No.:L34910, Set No.: 080603A, Ext.Date:07/31 L 08/06/03, Analyst:K.Risha Page 7 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~S6\Masslynx\Fluoroch~cals.PRO\S~leDB\O80603A Thu Aug 07 08:12:08 2003 P:\Data\L~SMS6\Masal~\Fluoroch~calB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: ---------------------- Thu Aug 07 12:49:56 2003 ------------~-----_-___-____ Name: Text: 080603A-I.007 1: C8 Sulfonate (PFOS) XCO72503-6,1000 rig/L Standard 080603A-1007 100- Sm (Mn. 2x31 . I %- 06-Aug-2003 17:08:OC LC/MS/MS #6 MRM of 4 Channels ES- 9.33 499 > 99 1.8385 Area I 1 r I , I I I Time 10.00 W Bxygen Research, 3058 Research Drive, State College, PA 16801 000252 Quazfitify Sample Report \r/ Study No.:L34910, set NO.: 0806031, Ext.Date:07/31 br 08/06/03, Analyst:K.Risha Page 8 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCblSMS6\Masslynx\Fluorochsmicals.PRO\S~l~DB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur.BC only 080603 Printed: Thu Aug 07 12:49:56 2003 ----_--_____ -------_---_____ ~-------------l____ -----_ Name: 080603A-1008 Text : 1: C8 Sulfonate 0106020 Control (PFOS) 080603A-1008 Sm (Mn, 2x3) 06-Aug-2003 17:29:43 LWMSIMS #6 MRM of 4 Channels ES499 > 99 2.05e3 Time ExyOen Research, 3058 Research Drive, State collsga, PA 16801 000253 --- -------__----------------------_ Quantify Sample Report `,M Study No.:L34910, Set No.: 080603A, Ext.Date:O7/31 P 08/06/03, Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Maselynx\Fluorochemicals.PRO~S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masel~\Fluoroch~cals.FRO\Met~B\PFOS Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 Name: 0806031-1009 Text : 1: C8 Sulfonate (PFOS) 0106020 Spk A, 50 rig/L 080603A-1009 loo- Sm (Mn, 2x3) %- 0 . . ..~......,,.,,,,...,....,.~.~,,~~~,.. 2.00 4.00 6.00 8.00 Analyst:K.Risha only e-P--_ Page 9 Decatur BC 080603 06-Aug-2003 17:51:2t LC/MS/MS #E MRM of 4 Channels ES499 > 9s 1.06e4 Area 10.00 , y, , 7 Time WSJen Research, 3058 Research Drive, State College, PA 16801 000254 m---e-- _c--_-__------I__ -------_ Quantify Sample Report qd Study No.:L34910, Set No.: 0806031, Ext.Date:O7/31 & 08/06/03, Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQISMS6\~sslynx\Fluorochrsmical~.PRO\S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LC!MSUS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 Analyst:K.Risha only Page 10 Decatur BC 080603 Name: 080603A-1010 Text : 1: C8 Sulfonate (PFOS) i;0106020 Spk B, 500 rig/l. 080603A-1010 10 Sm (Mn, 2x3) 9.31 21693 06-Aug-2003 18: 13:04 IX/MS/MS #6 MRM of 4 Channels ES499 > 99 9.58e4 Area L Time t -en Research, 3058 Research Drive, State College, PA 16801 000255 ---- e-------------------------- Quantify Sample Report yw' Study No.:L34910, Set No.. *080603A, Eact.Date:07/31 & 08/06/03, Samgls List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMS&S6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 ~---------------_---__---l____I________ Name: 080603A-I.011 Text : .: C8 Sulfonate (PFOS) -34910-12 Spk E, 25000 rig/L, DF=lOO 380603A-101 100 3 I Sm (Mn, 2x3) % Analyst:K.Risha only -- Page 11 Decatur BC 080603 ----_-- w---m-- 06-Aug-2003 18:34:45 LC/MS/MS #6 MRM of 4 Channels ES- 499 a 99 9.36e4 Area men Research, 3058 Research Drive, State College, PA 16801 0002564 ----- __--------- ----- w--v--- -------- Quantify Sample Report 'CJ Study No.: L34910, Set No .:080603A, Ext.Data:07/31 & 08/06/03, Analyst:X.Risha Page 12 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\lHasslynx\Pluoroehsmicals.PRO\S~leDB\O8O6O3A Thu Aug 07 08:32:08 2003 P:\Data\LCMSMS6\Masslynx\PluorochamicalsB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: --------------------------- Thu Aug 07 12:49:56 2003 ------___------------ ---_---_-_ Name: 080603A-1012 Text : ,: C8 Sulfonate (PFOS) -3491 O-15 Spk F, 50000 rig/L, DF=200 180603A-1012 10 %1-I Sm (Mn, 2x3) 2.00 4.00 9.32 1054: 3 06-Aug-2003 18:56:25 IX/MS/MS #6 MRM of 4 Channels ES499 > 99 7.99e4 Area L Time 8.00 10.00 EWgen Research, 3058 Research Drive, State College, PA 16801 000257 Quantify Sample Report 'd' study No.:L34910, Set No.: 080603A, Ea&.Date:07/31 br 08/06/03, Analyst:K.Rlsha Page 13 Saauple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LC%SMS6\XasslyPx\Fluorochemicals.PFtO\MethDB\PEOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: _L__------ Thu Aug 07 12:49:56 2003 --------------------------- Name: 080603A-1013 Text : ----------mm ,: C8 Sulfonate (PFOS) -34910-16 Spk F, 50000 rig/L, DF=lOO 180603A-1013 100- Sm (Mn, 2x3) %- 9.29 3565! A3 - 06-Aug-2003 19:18:10 K/MS/MS #6 MRM of 4 Channels ES499 > 99 1.54e5 Area 0 ,I,,,,',,,,,,,,,,,',.,,,,,,,',"","",""~ 2.00 4.00 6.00 8.00 10.00 Time J Exyg0n Research, 3058 Research Drive, State College, PA 16801 000258 Quantify Sarnpls Report ld Study No.: L34910, Set No.:O80603A, Ext.Date:07/31 tr 08/06/03, Analyst:X.Risha Page 14 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\MasslyPx\Fluoroch~cals.PRO\S~leDB\O~O603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSNS6\BZasslymc\Fluorochedcals.PRO\UethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1014 Text : 1: CB Sulfonate XCO72503-1,25 (PFOS) rig/L Standard 080603A-1014 Sm (Mn, 2x3) 1Ol-h 192.32691 06-Aug-2003 19:39:5 LCNSIMS #6 MRM of 4 Channels ES- 4995.58>e9396 Area 2.00 4.00 6.00 8.00 Eacygan Research, 3058 Research Drive, State College, PA 16801 .-. _I_-._1..-.,-- -* ",,"__.l,_l,_ .l-- .._.--..---.. 000259 Quantify Sample Report Study No.: L34910, Set No .:080603A, Ext.Date:07/31 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\~ssl~\Fluoroch~cals.PRO\S~~eDB\O80603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Pluorochemica\PFOS Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 I 08/06/03, Analyst:K.Risha only Page 15 Decatur RC 080603 Name: 080603A-3015 Text : 1: CB Sulfonate XCO72$03-2,50 (PFOS) rig/L Standard 080603A-1015 100- Sm (Mn, 2x3) %- 06-Aug-2003 20:01:4C LC/MS/MS #6 MRM of 4 Channels ES- 9.36 499 > 99 1.08e4 Area 6.00 8.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 000260 Quantify Sample Report Study No.: L34910, Set No .:080603A, Ext.Date:07/31 & 08/06/03, Sm4ple List: Last modified: Method : Last modified: Job Code: P:\Data\LCM~S6\Masslynx\Fluoroch~cal~.PRO\S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\FluorochemicaleB\PFOS Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 Analyst:K.Risha only Page 16 Decatur BC 080603 Name: 080603A-1016 Text : .: C8 Sulfonate <CO72503-3,100 (PFOS) rig/L Standard 380603A-1016 Sm (Mn, 2x3) 06-Aug-2003 20:23:22 LCIMSIMS #6 MRM of 4 Channels ES- 9.35 499 > 99 4928 2.20e4 Area I Time wgen Research, 3058 Research Drive, State College, pA 16801 --- 000261 Quantify Sample Report w Study No.:L34910, Set No.. *080603A, Ext.Date:07/31 & 08/06/03r Analyst:K.Risha Page 17 Sam~la List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\Kasslynx\Fluorochamica~s.~RO\S~~eDB\O~O603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\~etbDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: __--I_-------____ Thu Aug 07 12:49:56 2003 -------------a--------------- Name: 0806031-1017 Text : 1: C8 Sulfonate (PFOS) L3491 O-l, DF=l 00 080603A-1017 loo- Sm (Mn, 2x3) %- 06-Aug-2003 20:45:0; LCIMSIMS #6 MRM of 4 Channels ES499 > 99 2.21 e4 Area ;I Time 10.00 Exygsn Research, 3058 Research Drive, State College, PA 16801 000262 ---- Quantify Sample Report w Study No.:L34910, Set No.. *080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 18 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\M3MSMS6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\O80603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemical.s.PRO\M&ADB\PFOS Tbu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1018 Text : .: C8 Sulfonate (PFOS) L3491 O-l Rep, DF=l 00 380603A-1018 10 Sm (Mn, 2x3) 9.35, L 5235 06-Aug-2003 21:06:44 LCNS/MS #6 MRM of 4 Channels ES4992.41> e949 Area- Time 2.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000263 Quantify Sample Report I,& Study No.zL3493.0, Set No.: 080603A, Ekt.Date:07/31 bs 08/06/03, Analyst:X.X.isha Page 19 Sarqple List: Last modified: Method: Last modified: Job Code: P:\Data\L(23SMS6\Masslynx\Fluoroch~cal8.PRO\S~leDB\OSO6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCb%MS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: ------------- Thu Aug 07 12:49:56 --------___I Name: 0806031-1019 Text: 2003 -----~ v--m--- ------ ---_ 1: C8 Sulfonate (PFOS) L3491 O-12, DF=lOO .. D80603A-1019 10 Sm (Mn, 2x3) 9.31 11612 06-Aug-2003 21:28:28 LCIMSIMS #6 MRM of 4 Channels ES499 > 99 5.04e4 Area Time Oxygen Research, 3058 Research Drive, State College, PA 16801 000264 --------- ----- --- ---P-F ---- Quantify Sample Report `d Study No.: L34910, Set No .:000603A, Ext.Date:07/31 6L 08/06/03, Analyst:K.Risha Page 20 Sarqle List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\MasslyPx\Fluorochemicala.PRO\S~leDB\O~O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Maaslynx\Fluorochemica~s.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: ----~--------~_-_-__ Thu Aug 07 12:49:56 2003 ~---------__-----------___ Name: 000603A-1020 Text : ------------_ L: C8 Sulfonate (PFOS) L3491 O-1 2 Rep, DF=l 00 080603A-1020 10 i , %- Sm (Mn, 2x3) 9.32 1187? 06-Aug-2003 21:50:16 E/MS/MS #6 MRM of 4 Channels ES499 > 99 5.29e4 Area Exygen Research, 3058 Research Drive, State College, PA 16801 000265 Quantify Sample Report ,4 Study No.:L34910, Set No.. *080603A, Ext.Date:07/31 6r 06/06/03, Analyst:R.Risha Page 21 Saqple List: Last modified: Method: Last modified: Job Code: P:\Data\LQISMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSUS6\Uasslynx\Fluorochernica~s.PRO\MetbDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: --e--w-- Thu Aug 07 12:49:56 2003 -__-_-----____----________I_ --- -------e--e------_ Name: Text: 080603A-1021 : C8 Sulfonate (PFOS) -3491 O-l 5, DF=lOO 180603A-1021 Sm (Mn, 2x3) 1 06-Aug-2003 22:12:03 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.84e4 Area 2.00 4.00 6.00 8.00 10.00 Time 1 Exygen Research, 3056 Research Drive, State College, PA 16801 000266 -- ---I- Quantify Sample Report ,,& Study No.:L34910, Set No.: 080603A, Ext.Date:O7/31 -& 08/06/03, -Analyst:K.Risha --Page 22 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L(IMSMS6\blasslynx\Fluoroch~ca~s.PRO\S~leDB\O80603A Thu Aug 07 08:12:08 2003 P:\Data\LQbSMS6\Masslynx\Fluorochemicals.PRO\~et~B\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Brinted: Thu Aug 07 12:49:56 2003 --------l--------_______________II_ ---v-------e-- m---s- Neme: 080603A-1022 Text: 1: C8 Sulfonate (PFOS) L34910-13, DF=lOO 080603A-1022 10 Sm (Mn, 2x3) 9.36 14257 06-Aug-2003 22:33:4t LC/MS/MS #E MRM of 4 Channels ES499 > 9s 6.13e4 Area Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000267 -----__ ------------- P--e----- ----- Quantify Sample Report 'lu, StUaY No.:L34910, Set NO.: 0806031, F+xt.Date:07/31 h 00/06/03, Analyst:K.Riaha Page a3 SaxDQla List: Last modified: Method: Last modified: Job Code: P:\Data\M3MSMS6\Masslynx\Fluorochamieals.PRO\S~l~DB\O6O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 ----__-----------1-___________I________ ----_--I_P----_ Name: 080603A-1023 Text : ,: C8 Sulfonate <CO72503-4,250 (PFOS) q/L Standard 180603A-1023 10 7 % 1 Sm (Mn, 2x3) 9.34 10803 06-Aug-2003 22:55:23 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.85e4 Area 0 ,`,,~,`,,,,I,`,,~,,,,,,`,,,,,,,,,',',,,",,' Time 2.00 4.00 6.00 8.00 10.00 Exypen Research, 3058 Research Drive, State College, PA 16601 000X8 Quantify Sample Report w Study No.:L34910, Set No.. *0806033, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 24 Sample List: Last modified: Method: Last modified: Job Coda: P:\Data\LCmaSWS6\r#assl~\Fluoroch~ca~s.PRO\S~leDB\O6O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MetbDB\PFoS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 000603A-1024 Text : 1: Cl3 Sulfonate XCO72503-5,500 (PFOS) rig/L Standard' 080603A-1024 100- Sm (Mn, 2x3) %- 06-Aug-2003 23:17:07 K/MS/MS #6 MRM of 4 Channels ES499 > 991 9.98e4 Area BJWgen Research, 3058 Research Drive, State College, PA 16801 000269 ------ -- -- --s----e Quantify Sample Report `14 Study NO. : L34910, Set No.:O80603A, Ext.Date:O7/31 & 08/06/03, Analyst:K.Risha Page 25 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals~~RO\S~leDB\O8O6O3A Thu Aug 07 08:12:08 2003 P:\Data\LCM~S6\MsslyPx\FluorochemiB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: -_-_---------------------_____I__-----------___I------ Tbu Aug 07 12:49:56 2003 Name: 080603A-1025 Text : 1: ca Sulfonate (PFOSI XCO72503-6,lOOO r rig/L Standard )80603A-1025 100- Sm (Mn, 2x3) %- 06-Aug-2003 23:38:5: LC/MS/MS #f MRM of 4 Channels ES499 > 9s 1.91e5 Area Exygen Research, 3058 Research Drive, State College, PA 16801 000270 SECTION E _.--- - Sponsor Sody No: Exygcn Study No: Anslytc: Ions Mooit& Site: HA l.34910 PFOA 413 .>369 Lkcanrr Baker's Cnek RAW DATA REPORT Liil of Quaodutiw: bljdoa v01umaz M&X Sample Wei& Fii Volume: 50 PPt lSd. Soil 5.0 g J.OmL Set No: AdySC Inseum~n~ Extraction Aulyzcd Type: Daw: on: 080103.4 K&ml Rirhs LCMSMS 86 om1m3 o&urn3 xCO72503-0 XCOR503.I xCm2So3.2 xCO72503-3 XCO72.503~ xCu72503-5 XCO72M3-6 SpXlSO~ m Sample COdC cs cs cs cs cs c-s cs RWr NO. 080103A-2001 080103A-2002 080103A-2CO3 OB0103A-2lXM 080103A-2005 080103A-UXM 080103A-2007 Std. COnC. (ppt) 0 25 50 loo 250 500 IWO Dhtion Facux Peak hrcp 333 9882 17917 34827 78794 171634 315768 .-JYW Pound (PPO Amount Added @PC) RCCOVCIy (5) Adytc Found (p9b) Mcfhanol Wash l&agent Blmk C 080103A-2008 C 080103A.2009 525 1 518 ND Reagent Spk A LCS 080103A-2010 I 18939 55.3 111 Reagent Spk B LCS 080103A.201 I 1 163063 536 107 xCO72503-I cs 080103A-2012 2.5 9820 L34910-5 Spk C km SED-M LF OSOIMA-2013 IO 157971 SIW 96 L34910-10 Spk D EC? SED-05 LF 080103A-2014 10 166134 J4bo 96 L34910-11 Spk E BC2 SE&M LF 080103A.24US 10 187666 6180 W L3491&20 Spk F Outf-oIl to P.ivw S.eD-2s LP 080103A-2016 LO 179090 ss90 91" *J xamso3-2 CT 080103A-2017 SO 18190 L34910.5 BC7 SEMU S 080103A-2018 1 llS4JI 377 3JY2 L34910.5 Rep BC2 SED-04 S 080103A-2019 1 82762 268 2.14 w910.IO EC-2 sBD4s S 080103A-20'20 1 19505s 642 5.14 I3491010 Rep BC2 SED-OS S 080103A-2021 1 1677826 551 4.4 I xco72503-3 xCO72503-4 cs 080103A-2022 Im 33920 cs 080103A4.723 250 79282 w49 lo-1 1 BClSED-06 S 080103A-2U24 1 473416 L34910-11 Rep BC2 SED-06 S 080103A.2OZ 1 463017 W49Wm outhll to River SD-25 s 080103A-2026 1 404m L34910-20 Rw w4910-21 OutN) lo Riva sm25 hrtfidl to Riircc SJiD4S Dup S 080103A-2027 S 080103A-mm I 301201 I 532619 xCfJ72503-5 x0372503-6 cs 080103A-2029 500 cs 080103A-2D30 Iwo 14ocm 273386 Andyfe Recovay Fcund (ppt) (%) = - (peak M _ irmccpt) I JIG+ L DF [adym fowd (pplMnalya foul amount ridded &l colltml (per) (ppc)l x 100 Standard hlaccpt Slope cat. Of Del. : Liacar (l/x - 2344.75 = 300.076 - 0.988097 weighted) Adyo Andytc Fmmd @pb) - (mdyrc found @PC) I volum cxerkd (0.04 L)] I wmpk weight (5 r) Feud (pph) dry weight * malytr found @pa) x (100% I tolll solids (%j) CS I Calibmimsm&ni C = Cootrol mmpk s I sample LF s Lab fadfkd luaplc FF - Fwd fortified sample LCS = l&omcey CMml spike Toid SOlidS (5) MY& Found (ppb) Dry Weight 69.96 69.96 69.54 69.54 60.41 60.41 63.27 63.27 61.43 *Sample requires dilution. See data %I 080103AR. "Sample was corrected using the data found in se 080103AR. %I# 000272 Spaua Study No: NA Baygcn Stxdy No: L34910 Adyle: PFEIS Ionr Monimredz 399 -> 80 Site: Dccaw Eakdr Gcck RAW DATA REPORT Limit of Qwldlalion: Injcclioo Volume: Matlil: Samplr Weight: Fiinl v01umc: JO PPl I5d. Soil 5.0 g 5.0 ld. Ss( No: A&SE inr-1 Exmcdoo Analyyml TpJ: Da: ml: 080103A ib.mRisha LCMSMS L6 o&mu3 oumm3 `t*( ww spoaror Svnpk Run ID ID Code No. xcu72.503-0 Xcw2JO3.I cs 080103A-2001 c-5 080103A.2002 xcm2s03.2 c-s 080103A-2m3 xcm?503.3 xcm2Jo3.4 cs OSOlMA-2W cs 080103A.2tW5 xcO72503.s XCW2503.6 cs 080103A.2OC'S cs 080103A-2007 Mclhawl Wnrh C 080103A-2008 Reagent Blank C 080103A-2009 ha&co1 Spk A LCS 080103A-2010 Rcagsel Spk B LCS 080103A.2011 X(372.503.I cs 080103A.2012 L34910-5 Spk C BC2 SED.04 LP 080103A-2013 t.34910.10 Spk D 0C2 SD-OS Lp 0@3103A-2014 W4910.11 SpkE BQ SED-06 LF 080103A-201S L34910.20 Spk F outfall lo River SD-25 LF 080103A-2016 XCO72N3-2 cs 080103A.2017 w4910-5 BQ SED-0.l s 080103A.2018 L349w5 Rep w4910.10 80 SED04 BCZ SEDJJS S 080103A.2019 S 080103A.2fYU l-34910.10 Rep EC2 sRD.05 S 080103A-2021 xcQmo3-3 cs 080103A.2022 xal72503-4 c-s 080103A.2023 L34910.l W4910-11 Rep L34910-20 L34910-20 Rep BC2 SE&O6 BC2 SBD-06 Oulfsll m Ri"rr SD-U outfall In RiversED-2s S 080103A-2024 s 080103A-2025 S 060103A-2026 S 080103A-2027 W4910-21 outfill to Riva SED-2.3 Dup s 080103A-2028 xcowo3-5 XClX?303.6 cs 080103A-2029 cs 080103A-2030 Anrlyts Rmvoly Faud @pt) = (peak uu (%) - ldyte . intmcpc) found I slop x OF (ppox,alyte found in cmmol amoonl added (ppd (pm)] x 100 Std. coot. Diluliocl (~0 Facta 0 25 SO 100 2so 3x3 loo0 I I 1 2s 10 10 10 10 50 I 1 I 1 100 254 1 I 1 1 I so0 Ica Peak Area 0 1572 3699 6481 Imo 31281 58308 0 0 3457 3lOw 176s 30746 32192 12334 32343 3449 4534 3439 10896 129% 6560 14801 111133 Iml3 23354 16649 36172 28497 54198 -Yw Found (PPO Amouol Added (pm) uewvcq (5) &Ye FOLM (wb) ND 52.0 104 533 107 5280 104 5530 107 5560 105 5560 103 70.8 0.5l 51.7 0.41 Ill2 1.45 218 1.75 308 2.46 321 2.61 399 3.19 282 2.26 623 4.98 D hwyll Slope cocf. Of DCL : Linear (l/x -476.906 - 57.3138 - 0.995587 wcighoxl) Told SOti& (5) 69.96 69.96 69.54 69.54 60.41 60.41 63.27 63.27 67.43 rrntlYlc htiylc l%uod (ppb) = [amlytc found fppt) I wlum exmctcd (O.o( L)j I rlmplo vcight (5 g) Found (ppb) dry weight I malytc fwnd (ppb) I (100% I total solids (%)) CS = Calihrathrfadud c = CcmVOl rdmp,o s - Sample LF I Lb fortified lT * Field tonilied LCS L Laboratory sampk sampk Cmtrol Spike CK=ChskSuodud M) - Notdetmmi=Rcspwob*wmOaod25pppc NQ - Not quuifipblc - Rcrponrr buwceo 25 ppt sod LOQ (SO ppt) Andy& bud (ppb) Weight 0.809 0.591 2.09 2.51 4.08 4.33 5.0s 357 7.39 . _--- --. 000273 Spama Shuiy No: Exypra SMy No: Adya: loal Mwitorcd: Site: NA L2-4910 PFOS 499 -2.99 tkcatur Baker's Creek RAW DATA REPORT Limit of Qllmliuliw: lnpcdaa Vdumc: Matrix Sampls weight Fiat Volume: SOPPf 15d. soil 5.0 g 5.0 mL sst NQ: AdYSC ltuhumsnc !2.xlr4ctioo Analy7.ui Type: Dus: w: OSOIMA Kyea Birha LChGMS #6 o&QLDY 08mu3 Std. Amlytc Amount Amlyle Total hYS= Smpk Rut2 COIIC. Dilutia Peak FOUIUI Added Recovery Found Solids ID xcu72503-p Xcu72503- I XCU7UO3-2 . , - . -5-M. . .`. I.. cc& Na. (ppt) Fmor Am (PPQ (PPO (%) hvb) (%) c.s 080103A-ux)l 0 0 cs 080103A-2002 25 : 1018 - cs 080103A-MO3 50' ton XCfJ72503-3 cs 080103A.hM loo 3701 xco72503-4 ci 080103A-2005 2.54 9370 xcO72.503-5 a 080103A.2006 mJ 19171 XCO72503-6 cs 080103A-2007 Iwo 37079 hlelhlnol WYh C 080103A-2008 0 Reap1 BIank C 000103A-2009 1 0 ND Resgcnc Spk A LCS 080103A-2010 I 2011 51.4 50 103 lbxgcnl Spk B LCS 080103A-2011 1 17583 4% 500 99 xc.m2503-1 a 080103A-2012 21 430 W4910-5 Spk C BC2 SE@04 LF 080103A.2Bl3 10 22078 6470 sow 93" U4910.10 Spk D BC2 SED-05 Lp 080103A-1014 10 26935 7620 moo 9r U4910-II SpkE BC2 SED06 LF 080103A.2015 IO 336383 . sow `*rs I.3491020 X072503-2 Spk F outfall m River SED-25 LP D80103A.2016 cs 080103A-U)l7 10 72248 JO 2'233 . 5Dw L349m5 BC-2 SEDM S 080103A-2018 1 60613 . 69.% l.34910.5 Rep ac2 SED-04 s 080103A.U)19 I 51074 . 69.96 L34910-IO X2 SE&OS s 080103A-2020 I 93844 . 6954 w491010 Rep Bc2 sED-05 s 080103A.2021 I 106350 . 69.54 xcum3-3 cs 080103A.2022 mJ 3634 xco72503-4 cs 080103A-2023 250 8WS l.34910.I I BQ SE&O6 s 080103A-2024 I 2354673 . 60.41 L34910-11 Rep BQ SED-M s 080103A-2025 I 1794353 . 60.41 w4910-20 Outfall to Rive? SEDU S 080103A-2026 I 418516 I 63.27 w4910.20 Rap OutfalI ra River SED-23 S 080103A-2027 I 287933 . 63.27 w4910-21 Outfall IO River SED-25 Dup S 080103A-2028 I 409821 l 67.43 xal72xl3.s cs 080103A~ZJl2Y ml 17108 XCO72503-6 cs 080103A.2030 Iwo 32192 Amlyu Rumuy Feud (ppt) m (psak vu - Qtmxpt) I slope I DP (%) P [andya found (pp+mtyte found in canml mouat dkd (ppt) (ppt)] x iW Jilaw&m InUerccp1 stqx Cd Off& : Lincy (l/x - 208.s43 I 35.0593 I 0.990916 weighted) A&w Aosly(c Found (ppb) i [amlyte fmmd (ppt] x ~oluma mknckd (0.04 L)I I sampk weight (5 g) Pod (ppb) dry weight - analytc found (ppb) x (I 00% I total solids (+)I CS - tXibnum C I Cmtml s -sample rurdud m~~plc LF = Lab fortified FP - Field fmirlcd LCS -L&oratory sample sample Cmtrol Spike CK I Check Sacdad ND I Noc&wcwd=RUpopl~bmv~~.Oa~d2Sppt NQ I Not quurtitiablc - Reaporuc bctwaa 2S ppt and LDQ (50 wt) mlylc Fwad (ppb) Dxy Weight `Sample %mplc requires dilution. See data ICI 080103AR. was corrcctcd using the data found in re( 080103AR. %a# 000274 Sponsor Study No: Exygco Study No: Adytc: Ions Mooitored: Site: NA L34910 FOSA 498 -> 78 Decatur Bakea's Creek RAW DATA REPORT Limit of Qwtitation: hjdon Volume: Manix: Sample Weighr Final Volume: 50 PP' IS pL Soil 5.0 g 5.0 mL Set No: AtlllYSi: InauumntTypc: Extraction Da@: Analyzed on: OBOlO3A Karen Rishs LCMSMS #6 08iO 1103 08102103 Std. ExY8a w Sample Code RUn COW NO. (ppt) xco72503a CS 080103A-2001 0 XCO72503-I cs OIOIO3A-2002 25 XCO72503-2 xco72503.3 cs 080103A-2003 50 cs 080103A-2004 loo xco72503-4 cs 080103A-2005 250 xco72503-5 XCO72503-5 cs 080103A-2006 500 cs 080103A-2W7 loo0 Metbanol Wash C 080103A-2008 Reagent Blank lla C 080103A-2009 Reagent Spk A "a LCS 080103A-2010 Reagent Spk B ns LCS 080103A.201 I XCO72503-I CS 080103A.2012 25 L34910.5 Spk C BC2 SED.04 LF 080103A-2013 L34910-10 Spk D BC2 SED-05 LF 080103A-2014 L34910-I I Spk E BCZ SED-06 LF 080103A-2015 L349lO-20 Spk F Outfall ID River SED-25 LF 080103A-2016 Vd XCO72503.2 L34910.5 BC2 SED-04 cs 080103A.2017 50 S 080103A-2016 L34910-5 Rep BC2 SED-04 S 080103A.2019 L34910-LO 6'22 SED-05 S 080103A.2020 L34910-IO Rep BC2 SED-05 S 080103A-2021 xco72503-3 cs 080103A.2022 loo xcci72503-4 cs 080103A-2023 250 L34910-I I BC2 SED-C.5 S 080103A-2024 L34910-I I Rep BCZ SED-06 S 080103A-2025 L34910.20 Outfall to River SED-25 s 080103A-2026 L349lO-20 Rep Outfall to River SED-25 s 080103A-2027 w4910-21 Ouffall to River SED-2S Dup S 080103A-2028 XCO72503.5 CS 080103A-2029 500 XCO72503-6 CS 080103A.2030 loo0 Attslytc Found (pit) Rccovexy (%) = = @crk LTCP - imerccpt) [amlyte found / slope x DF (pptkmalytc found .mount added in control @pt) (pp~)J x IM) Analyte Antdytc Found @pb) = [analytc Found (ppt) x volume extracted (0.04 L)] I sample weight (5 g) Found (ppb) dzy weight = analy?c found (ppb) r ( ICOYI / total rolids (%)) CS - Calibr&nstandard c = Conholsample s - Sample LF -Lab fortified sample FF - Field fonilied wttplc LCS = Laboratory Control Spike Dilution FZiElQI 1 I I IO IO IO IO I 1 I I I 1 I I I PC& Area 0 3995 7728 IS082 36693 72894 137821 0 0 6150 65424 3817 79517 82212 155090 IO0640 7957 121882 133583 133763 191201 14698 34282 1215533 92977 I 412369 346884 357273 6723 I 1291 I8 Analytc FOund (ppt) Amount Added (ppt) RCCOVCTy (%) Adyte Found (ppb) ND 43.6 50 477 500 5810 5000 6010 5000 l 5cw 73 70 so00 894 961 982 . 87 9s 98 IO1 77" 7.15 7.84 7.86 &&rd CWP lntacept slaps Ccuf. Of Da. : Linear (I/x - 849.062 - 135.358 = 0.996863 weighted) TOtnl Solids (% 69.96 69.96 69.54 69.54 60.41 60.4 I 63.27 63.27 67.43 CK - Check Standard ND - Not detected = Reoponrc between 0 and 25 ppt NQ = Not quantifiable - Response bctwcm 25 ppt md LOQ (50 ppt) Analyie Found @pb) Dry Weight 10.2 Il.2 Il.3 - `Sample *Sample requires dilution. See data set 080103AR. was corrected using the data found in set 080103AR. Spreadsheet prepared by: 000275 Work Group-`VG46121 Analysis: Solid% Title: Send Date Prepared: 29- ID L34905-21 L34905-22 L34905-23 L34905-24 L34905-25 L34905-26 L34905-27 L34905-28 L3490523 L34905-30 L34910-5 L34910-10 L3491P11 L34910-20 L34910-21 L34921-1 Result 100 100 100 100 100 100 IO0 100 100 100 69.96 69.54 60.41 63.27 67.43 81.19 Product PERC SOLID PERCSOUD, PERCSOLID PERC SOLID PERC SOLID PERCSOLID PERC SOLID PERC SOLID PERCSOLID PERC SOLID PERC SOLID PERC SOUD PERCSOLID PERCSOLID PERC SOLID PERC SOLID Matrix SOUD SOLID SOUD SOLID SOLID SOLID SOLID SOLID SOUD SOLID SOLlD Soil0 SOLlD SOLID SOLID SOLID, DF MDLxDF I 0.01 I 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 1 0.01 CRDLxDF 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Flags The Collect Time Run Client ID OB-J&O3 0O:OO 24Jul-03 15% 200874 X33238-32-21 08-Jut-03 0O:OO 29-Jul-03 1534 200875 X33238-32-22 08-J&03 0O:OO 29-J&03 15:34 200876 X33238-32-23 OB-J&O3 0O:OO 29-Jul-03 1534 200077 X33236-32-24 OB-Jul-03 0O:OO 24Jul-03 15:34 200878 X33236-32-25 oaJul-03 0o:oo 29-J&03 15:34 200879 X3323632-26 08-J&03 0O:OO 29-Jul.03 15~34 200860 X33236-32-27 OB-Jul-03 0O:OO 29-Jul-03 15:34 200881 X33236-32-28 O&Jui-03 0O:OO 29-J&03 15% 200882 X33238-32-29 OB-Jul-03 0O:OO 29-J&03 15~34 200883 X33238-32-30 23-Jul-03 14% 24Jul-03 15% DC2 SED-04 21-Jul-03 14:15 29-Jul-03 15:34 BC2 SED-05 23-J&03 15:25 29-J&03 15% BC2 SED-06 23-J&03 16:15 29-Jut-03 15:34 OUTFALL TO RIVER SE525 23-J&03 16:15 24Jut-b3 15% OUTFALL TO RIVER SED-25 DUP 23-JuLD3 14:00 24Jul-03 15:34 BASR7-23 Print Date: 30-Jul-03 Page 1 of 1 Analyst: AJ < Work Analysis: Group: Solids * 46121 t Title: Data Date Prepared: 29-t r03 Analyst Initiate Date and Time Data Aquired (ctri+t) AJH 29-Ju1-03 1534 AJH 29-JulO3 16.06 AJH 30.J&f33 0834 CAL ID WG46121.1 WG46121-2 L34905-21 L3490522 L3490523 L34905.24 I L3490525 L-%905-26 L34905-27 L349ClS-28 L34905.23 I L3.490530 L34910-5 L34910-10 L34910-1 I CUENT ID MATRIX PAN ID MB PERC SOL10 1 SOLID 1 UP: L34910- PERC SCUD ) SOLID 2 74 X33238-3 PERC SOLID ) SOW 3 75 xwm-ah PERC SOLID I souo 4 76 X33238-3 PERC Sa.lO 1 sow 5 1 77 X33238-3b PERC SOLID ) SCUD 1 6 176 X33238-3b PERC SCUD 1 SOLID 1 7 PERC SOilD ] SOLID 8 PERC SOLID 1 SLXIO 9 81 X33238-3 PERC SOLID ) SOLID 10 82 X33238-3 PERC SOLID ) SOLM 11 1 83 X33236-3b PERC SOLID I SOLID i 12 I r I 6C2 SED.04 PERC SOLID ) SOCID 13 6C2 SE&OS PERC SOLID ) SOLID 14 EC2 SEDD6 PERC SOLID ] SOLID 1 15 PAN WEIGHT I.2578 1 2521 1 1 1 1 1 1 1 1 1.2512 1.2517 1 .i578 1 2574 12638 1.2556 (g) sAMPLE+PAN'gJ I I 1.2578 1 43.5159 2 2 2 2 2 2 I 2 I 39.8338 28 6584 I 34.2073 23.9616 1 20 0233 4.2022 DRIED SAMPLE 1 *PAN(g) IGNITED SAMPLE / +PAN(g) X Solids of X TVS / or%Ash ( 1.2578 31.9212 2 2 2 2 2 2 2 I 2 I 0 72.56 100 lco loo 1W 100 loo loo I 100 I I 28 246 I 20.3121 21.1653 I . 15.6246 13.9150 I 36481 I 69.96 69.54 I 60.4 1 63.27 67.43 81.19 I I I 1 Print Date: 06-Aug43 Page 1 of 1 E Exygen Study Number: nn4 EAKCH 3058 Research Drive State Cdlege, PA 16801 Internal Chain of Custody/Fortification L34910 Sheet Matrix: Phone: 814-272-1039 Fax: 814-231-1580 m w were removed from refrig Outfall to River SED-25 Dup L34910-21 5.0 AI1 samples were weighed on balance No. W Time C%?e InitiaIs & After weighing samples were re Time I.= InitiaIs &5 bxUnen~: 200 S of 250 mglmL sodium tiosulfatc was added to all sunpler kfmc Analysis Summary: Data Set: Data Set: Data Set: fio~03~ - rpikiag. Inilials/t)atc: Initials/Date: Initials/Date: Initials/Date: Set extraction/analysis data verified by: Date: g/hb July 26, 20011t)00278 1 d nma (. EAKC ti 3058 Research Drive Phone: 814-272-1039 State College, PA 1680 1 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: MATRIX: L34910 &! METHOD: ANALYTES: ExM-023-014's PFHS. PFOS. PFOA and PFOSA PROTOCOL NUMBER: m STEP 1: Add 5mL of methanol and shake by hand for -I minute STEP 2: Bring up to 40 mL with hypercarb filtered type I water STEP 3: Centrifuge for 10 minutes at -3OOO rpm STEP 4: Filter through glass acrodisc STEP 5: SPE colmnn clean up (omitting 40% wash) STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP I: LtXWMS analysis 0 STEP 8: LCfMS/MS reanalysis. 8 *Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluor~tancsulfonate (PFOS) and Pentadeeafluorooctanoic Acid (PFOA) in Soil COMMENTS: Final extracts stored in refrigerator 9 Initials: @ Date: 3 July 19,200114 Masslynx - Sample List Sample List: Printed: Fri AMJ 01 15:28:30 2003 Exygen STUDY NO. !--3!45(0 Page 1 Page Position: (1, 1) Vial File Name LIMS ID Client ID Sample Description Matrix Sample Type Conc(ng/L) 1 41 080103A-2001 -- - 2 42 080103A-2002 --_ - 3 43 080103A-2003 --- - 4 44 080103A-2004 --- - 080103h2005 _-- - f 1: 060103A-2006 -- - 080103A-2007 -_ - ii 080103A-2008 -- - 9 080 I 03A-2009 -- -_ 080103A-2010 -_- - :: 080103A-2011 I- - 42 080103A-ml2 ___ - :: 4 080103A-2013 -- - 080103A-2014 I_ - :: 2 080103A-2015 -- - 16 7 080103A-ml6 -_ - 17 43 080103A-2017 -_ - 18 080103A-2018 - 19 i 080103A-2019 ___ - 20 10 080103A-2020 -- - 21 11 080103A-2021 ___ - 22 44 080103A-2022 ___ - 23 45 080103A-2023 -_ - 24 12 080103A-2024 sm.. - 25 13 080103A-2025 __- - 14 080103A-2026 -- - z; 15 080103A-2027 -- - 28 16 080103A-2028 -- - 29 46 080103A-2029 -- - 30 47 080103A-2030 -- - XCO72503-0.0 nglL Standard -- Standard 0 XCO72503-I,25 rig/L Standard _- Standard 25 xCO72503-2, 50 nglL Standard -- Standard 50 xCo72503-3, 100 rig/L Standard - Standard loo XCO72503-4,250 nglL Standard - Standard 250 XCO72503-5,500 rig/L Standard Standard 500 XCO72503-6, 1000 t-g/L Standard -- Standard 1000 Methanol Wash - Blank -- Reaccent Blank -- Blank - Reagent Spk A. 50 nglL .- 100 Reagent Spk 6,500 ngR - :: 500 XCO72503-1,25 rig/L Standard -- Standard 25 L34910-5 Spk C. 5000 rig/L, DF=lO - QC 5000 L34910-10 Spk D,5000 rig/L, DF=lO -- 5000 L34970-11 Spk E, 5000 w/L, DF=lO - :: 5000 L34910-20 Spk F, 5000 rig/L. DF=lO -- QC 5000 XCO72503-2. 50 ~111 Standard - Standard 50 L34910-5 - -- Analyte - L3491.0-5 Rep -- Analyte - L34910-10 - Analyte - L34910-10 Rep - Analyte XCO72503-3, 100 rig/L Standard -- Standard lo0 XCO72503-4,250 nglL Standard - Standard 250 L34910-11. -- Analyte -- L34910-11 Rep - Anaiyte -- L3491 O-20 - Analyte -* L34910-20 Rep - Analyte -- L34910-21 - Analyte -_ XCO72503-5,500 rig/L Standard - Standard 500 XCO72503-6,lOOO ngll Standard -- Standard 1000 ConcB -_ ----_ -_ --_ -_ ---_-_ --.--- _----__ ---_ ConcC ___ -I -_-- _^_ -_--_--_-----I ---- Test ID DF 0 1 0 1 0 1 1 x 1 0 1 0 0 : 0 1 x : 0 1 10 : IO 0 0 ii 0 1 0 1 0 1 0 1 0 1 1 8 1 0 1 0 1 0 0 : 1 ii 1 0 1 t Masslynx - Sample List Sample List: Printed: Fri Aug 01 15:28:30 2003 MS Method HPLC Method MS Tune File Inj.Volume I C6 C8 SULF C8 ACID PFOSA 2 C6 C8 SULF CB ACID PFOSA 3 C6 C8 SULF C8 ACID PFOSA 4 C6 C6 SULF C6 ACID PFOSA 5 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA ; C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID F'FOSA : C6 C8 SULF C6 ACID PFOSA C6 C8 SULF C8 ACID PFOSA :`: C6 C8 SULF C8 ACID PFOSA 12 C6 C8 SULF C8 ACID PFOSA 13 C6 C6 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA :`: C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C6 ACID PFOSA :t C6 C8 SULF C8 ACID PFOSA 18 C6 C8 SULF C8 ACID PFOSA 19 C6 C8 SULF C8 ACID PFOSA 26 C6 C8 SULF C8 ACID PFOSA 21 C6 C8 SULF C8 ACID PFOSA 22 C6 C8 SULF C8 ACID PFOSA 23 C6 C8 SULF C8 ACID PFOSA 24 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF CB ACID PFOSA pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfhs water pfhs water pfbs water pfhs water pfbs water ppfbms swwaatteerr pmswater ppfbms swwaatteerr ppfbms swwaatteerr pmswater ppmrnsswwaatteerr ppfbms swwaatteerr pmswater pmswater pmswater pfbs water pfbs water Fluorochems 15 Fluorochems 15 Fluorochems Fluorochems :z Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems Fluorochems :: Fluomchems Fluorochems :55 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems f5 Fluorochems 15 Fluorochems 15 Fluorochems Fluerochems ;z Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Oxygen STUDY NO. " L3q'0 A t Page 2 Page Position: (2, 1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Soonsor Protocol No: NA Exveren S tudv No: L34910 Instrument: Micromass Quattro Ultima @C/MS/MS Unit #6) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC cohlmn: Genesis C-8,5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by: ' i 000282 w Scanning Method Report Method: Last Modified: C:\M?GSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 Printed: Fri Aug 01 15:29:10 2003 C8 SULF CS ACID PFOSA Solvent Delay ( mins ) : 0.00 Analog Channel Function : 1 4 : Unused MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Sets ) : 0.03 Span ( Daltons ) : 0.00 Start Time ( Mins ) : 0.00 End Time ( Mins ) : 12.00 Repeats : 1 Channel Parent Daughter Dwell (Sets) Co11 Energy (eV) Cone ( V ) 1 399.00 80.00 0.20 35 50 2 413.00 369.00 0.20 10 10 3 498.00 78.00 0.20 30 50 4 499.00 99.00 0.20 40 30 000283 Method Report Method File: Laat Modified: v Printed: c:\maeslynx\fluotochsmicals.pro\acqudb\pfbs Friday, August 01, 2003 15:20:36 Friday, August 01, 2003 15:29:16 HP1100 LC Pump Initial Conditions Solvents A% 90.0 B% 10.0 C% 0.0 D% 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Oven Temperature Right(OC) 0.300 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains S entries which are : Time A% B% C% D% 0.00 90.0 10.0 0.0 0.0 2.00 90.0 10.0 0.0 0.0 5.00 10.0 90.0 0.0 0.0 9.00 10.0 90.0 0.0 0.0 9.50 0.0 100.0 0.0 0.0 14.00 0.0 100.0 0.0 0.0 14.50 90.0 10.0 0.0 0.0 20.00 90.0 10.0 0.0 0.0 b@ HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contact1 Off On Off Off Off Off Contact2 Off Off Off On Off Off 'Contact3 Off Off Off Off On Off w Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300 Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(p1) Vial Number Conditions 200.0 200 0.50 20.00 15.0 69 Page 1 water Pressure 400 400 400 400 400 400 400 400 000284 1111 Tuning Method: Printed: Method Report C:\kWi.SLYNX\FZUOROCHEMICALS.PRO\ACQUDB\EWOROCHEMS Fri Aug 01 15:29:30 2003 Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set Rdbk 3.00 -2.93 20 -33 0.0 0.0 0.0 100 100 300 299 Rdbk OFF 3.3e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation V Set Rdbk 14.0 14.0 1.0 -2 36 15 19 2 40 14.0 14.0 2.0 650 -648 Rdbk 131.8 751.3 00028s ----- --------- Quantify Calibration Report \Icl, Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:X.Riaha Calibration: Last modified: Printed: ----___ P:\Data\LCWSMS6\blasslynx\Fluorochemicals.PRO\~~eDB\O8OlO3A Sun Aug 03 07:26:03 2003 Sun Aug 03 07:32:22 2003 ------_---- Compound 1 name: C8 Acid (PFOA) >oefficient of Determination: 0.988097 >alibration curve: 300.076 * x + 2344.75 qesponse type: External Std, Area 2urve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 3.16e5- ----- Page 1 Decatur BC Response- Oxygen Research, 3058 Research Drive, State College, PA 16801 ---___I_-- -------MI --- Quantify Calibration Report w Study No.:L34910, Set No.. -080103A, Ext.Date:08/01/03, Analyst:K.Risha Calibration: Last modified: Printed: ---- P:\Data\L~SWS6\Masslynx\Fluorochsmicals.P~\~~~DB\O80103A Sun Aug 03 07:26:03 2003 Sun Aug 03 07:32:22 2003 -- -_____---------_II------~~~~~~~~~ :ompound 2 name: C6 Sulfonate (PFHS) Coefficient of Determination: 0.995587 :alibration curve: 57.3138 l x + 476.906 Response type: External Std, Area :urve type: Linear, Origin: Exclude, Weighting: 5.83@4- l/x, Axis trans: None -- Page 2 Decatur BC X Response- Exygen Research, 3058 Research Drive, Stats College, PA 16801 0002~7 Quantify Calibration Report $,J Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:R.Risha Calibration: Last modified: Printed: P:\Data\L~SndS6\bssl~\F~uoroch~cals.PRO\~~eDB\O80103A Sun Aug 03 07:26:03 2003 SUA Aug 03 07:32:22 2003 :ompound 3 name: C8 Sulfonate (PFOS) >oefficient of Determination: 0.990916 Calibration curve: 35.0593 l x + 208.543 lesponse type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 3.71 e4 l/x, Axis trans: None Page 3 Decatur BC X Response Exygen Research, 3058 Research Drive, State College, PA 16801 000288 -__-_.___ --.-.-.-- ..-. -... ...-.- ..---- ----------- Quantify Calibration Report "4 Study No.: L34910, Set No.: 080103A, Ext.Data:08/01/03, Calibration: Last modified: Printed: - ----- P:\Data\LCM~S6\Massl~\FluorochemicaeDB\O8OlO3A Sun Aug 03 07:26:03 2003 Sun Aug 03 07:32:22 2003 ---____--__-----___-------- Analyst:R.Risha ------e--y------- Compound 4 name: PFOSA Coefficient of Determination: 0.996863 :alibration curve: 135.358 l x + 849.062 Response type: External Std, Area >urve type: Linear, Origin: Exclude, Weighting: 1.38e5 l/x, Axis trans.: None Page 4 Decatur BC Response 0(I-.0 Exygen Research, 3058 Research Drive, State College, . PA 16801 000289 ----- -v------w----w--- -------_------__I_ Quantify Sample Report Study No .:L34910, Set No.:080103A, E&.Date:08/01/03, Analyst:K,Risha Sample List: Last modified: Method : Last modified: Job Code: P:\Data\L~~6\~sslynx\Fluoroch~cals.PRO\S~1eDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicale\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 1 Decatur BC BC 080103 Name : 080103A-2001 Text: 1: C8 Acid (PFOA) XCO72503-0,O rig/L Standard 080103A-2001 Sm (Mn, 2x3) 2: C6 Sulfonate XCO72503-0,O @I I I .m, 2.00 4.00 (PFHS) rig/L Standard I I 6.00 02-Aug-2003 02:27:16 LC/MS/MS #6 MRM of 4 Channels ES413>369 2.00e4 Area 9.14 333 10.00 12.00 02-Aug-2003 02:27:16 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) XCO72503-0,O rig/L Standard 02-Aug-2003 02:27:16 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 11.36 11.75 962 0 ~..~,~~~~,.,,,,,,~,,~~,,,~,,~,,~,,,,~,,,~~~~,~~,~,~~,~,~,~~~Time 2.00 4.00 6.00 8.00 10.00 12.00 _ Oxygen Research, 3056 Research Drive, State College, PA 16801 000290 ---- ---------------------~ Quantify Sample Report ,,d Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:K.Risha Si?uaple List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\blasslynx\Fluoroch~cala.P~O\S~leDB\O6OlO3A Sun AUg 03 07:25:44 2003 P:\Data\LCMSWS6\Masslynx\Fluoroch~cals.~RO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 ------ Page 2 Decatur BC BC 080103 Name: 000103A-2001 Text : 4: PFOSA XCO72503-0, 0 rig/L Standard 080103A-2001 100-l Sm (Mn, 2x3) I 32-Aug-2003 02:27:1 t V LCNS/MS #IE MRM of 4 Channels ES- 9.79 498 > 7fc EXygen Research, 3058 Research Drive, Stats College, PA 16801 000291 ------ I__----- --------- Quantify Sample Report " 4 Study No.:L34910, Set No.:080103A, Rxt.Date:08/01/03, Analyst:K.Risha Sample List: Last madified: Method: Last modified: Job Code: P:\Data\LCMSblS6\WasslyPx\Fluorochemicals.PRO\S~leDB\O8OlO3A Sun Auq 03 07:25:44 2003 P:\Data\LCbISMS6\~ssl~\Fluorochsmica\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 --- Page 3 Decatur BC BC 080103 Name: 080103A-2002 Text : 1: C8 Acid (PFOA) lXCO72503-I,25 rig/L Standard 080103A-2002 10% Sm (Mn, 2x3) %- 9.13 98827 02-Aug-2003 02:49:04 LClMS/MS #6 MRM of 4 Channels ES413>369 5.84e4 Area `d 2: C6 Sulfonate (PFHS) XCO72503-1,25 rig/L Standard 080103A-2002 10 Sm (Mn, 2x3) % 4 3: C8 Sulfonate XCO72503-1,25 (PFOS) q/L Standard 080103A-2002 100- Sm (Mn, 2x3) %- 02-Aug-2003 02:49:05/ LCIMSNS #6 MRM of 4 Channels ES- 8.98 399 > 80 1579 9.29e3 Area - L^ Time 12.00 02-Aug-2003 02:49:05 LC/MS/MS #6 MRM of 4 Channels ES- 9.26 499 > 99 6.29e3 Area A 0 ,,l,71~~,.".,,,,.,,.,.,..~`,"`.,"","", 1 , 3 TyT-cy Time 2.00 4.00 6.00 8.00 10.00 12.00 , Exygen Research, 3058 Research Drive, State College, PA 16801 .-BIII""( -- ~,--- .^ -- 000292 ---- ----- ----- ------------_ Quantify Sample Report \& Study No.:L34910, Set No.: 080103A, Ext.Date:O8/01/03, Analyst:K.Risha Page 4 Ssmgls List: Last xmdified: Method: Last modified: Job Code: P:\Data\LCWSMS6\Masslynx\Fluorochemicals.PRO\S~leDR\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\L(3WSMS6\blasslynx\FluorochemicaR\Decatur Sun Au% 03 07:11:59 2003 Decatur BC BC 080103 Printed: --------------em Sun Aug Name: 000303A-2002 Text : 03 07:32:25 2003 ------- c-----------------_________ : PFOSA (CO72503-1,25 rig/L Standard 180103A-2002 10 Sm (Mn, 2x3) %3. 02-Aug-2003 02:49:05 LC/MS/MS #6 MRM of 4 Channels ES- 9.9C) 399! 498 > 78 2.1 le4 Area 01 2.00 4.00 6.00 8.00 10.00 12.00 l%YOen Research, 3058 Research Drive, State College, PA 16801 P-m------ -1_------- Quantify Sample Report w Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Aaalyst:X.Risha Sample List: Last modified: Method: Last modified: Job Coda: P:\Data\L~SMS6\Mssslyox\Fluoroch~cals.PRO\S~~eDR\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCEISMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: SUA Aug 03 07:32:25 2003 Page 5 Decatur BC BC 080103 Name : 080103A-2003 Text: 1: C8 Acid (PFOA) XCO72503-2,50 rig/L Standard 080103A-2003 lO& Sm (Mn, 2x3) %- 02-Aug-2003 03:10:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413>369 l.lle5 Area 2.00 4.00 w 2: C6 Sulfonate (PFHS) XCO72503-2,50 q/L Standard 080103A-2003 Sm (Mn, 2x3) , , . 1, , , , , , , 8.00 10.00 . , r , ,-y Time 12.00 02-Aug-2003 03:10:44 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 2.28e4 Area - ;: C8 Sulfonate KO72503-2,50 (PFOS) rig/L Standard )80103A-2003 10 Sm (Mn, 2x3) %j Time 12.00 7 02-Aug-2003 03:10:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 207: 1.28e4 Area Time 2.00 4.00 6.00 8.00 lo:oo 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000234 -- --- ------- ----------- w------m-- Quantify Sample Report \& Study No.:L34910, set NO.: 080103A, Ext.Date:08/01/03, AMllyst:K.Risha Page 6 SamQls List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSblS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O6~lO3A Sun Aug 03 07:25:44 2003 P:\Data\L~SMS6\Masslynx\Fluorochamica\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 060103 Printed: Sun Aug 03 07:32:25 2003 I--------------I-------------I_-----------------------__~_ NW: 000f03A-2003 Text : 4: PFOSA X072503-2,50 rig/L Standard 02-Aug-2003 03:10:44 LC/MS/MS #6 )80103A-2003 Sm (Mn, 2x3) 10 7 i %IO'~~~~,~~~~,~~~`,~".,.~`~,~~",~"','~,~,,~~~,',~ MRM 9.90 , 772E5 of 4 Channels ES498 > 78 4.01 e4 Area A- Time 2.00 4.00 6.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16,801 ------- p-w--- ----- -----v----m__ Quantify s-10 Report bf Study No.: Ll34910, set No .:080103A, Eact.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslyPx\Fluoroch~cals.PRO\S~~eDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\~SMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Rage 7 Decatur BC BC 080103 Name: 0801031-2004 Text : 1: C8 Acid (PFOA) XCO72503-3,100 rig/L Standard 080103A-2004 10 Sm (Mn, 2x3) 9.13 34827 02-Aug-2003 03:32:2d LCYMWMS #6 MRM of 4 Channels ES413>369 2.10e5 Area Time L 2.00 4.00 6.00 8.00 1o:oo 12:oo \d 2: c6 Sulfonate (PFHS) XC072503-3,100 rig/L Standard 080103A-2004 10 7 Sm (Mn, 2x3) 02-Aug-2003 03:32:2j LCJMWMS #6 MRM of 4 Channels ES- 8.98 399 > 80 6481 3.94e4 Area e Time L 2.00 4.00 6.00 8.00 10.00 12.00 : C8 Sulfonate (PFOS) KO72503-3, IO0 rig/L Standard 180103A-2004 10 ?I Sm (Mn, 2x3) % 02-Aug-2003 03:32:27 LCIMSMS #6 MRM of 4 Channels ES- 9.24 499 > 99 3701 2.21 e4 Area i %___-- Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000296 Quantify Sallqlle Report ,cf Study No.:L34910, Set No.. -000103A, Ext.Date:oa/ow03, A.ualyst:K.Risba Page 8 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQHSMS6\Masslynx\Fluoroch~cals.PRO\S~laDB\O8OlO3A Sun Aug 03 07:25:44 2003 B:\Data\L~SMS6\Maaslyax\Fluorochamicals.PRO\MethDB\Decatur Sun Aug 03 07x11:59 2003 Decatur BC BC 080103 Printed: ------ Sun Aug 03 07:32:25 2003 --------___l_ --------------_I__ -- - Name: 080103A-2004 Text : 4: PFOSA XCO72503-3,100 rig/L Standard 080103A-2004 loo- Sm (Mn, 2x3) %- 02-Aug-2003 03:32:2$ LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498>78 7.93e4 Area 0 `~~~,~"`,J~(~,1~~~,`~",~"(,"",~J'I,"","' , I I 1 t 1Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygtrn Research, 3058 Research Drive, State College, pA 16801 000297 Quantify Sarr~le Report w Study No.:L34910, Set No.. *080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 9 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L(2dSMS6\Masslynx\Pluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Mas8lynx\Fluorochamica~s.PRO\MethDB\Dscatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ------------_---------------_ Sun Aug 03 07:32:25 2003 -----_-------------- ---------I____ Nzuae: 080103A-2005 Text : 1: C8 Acid (PFOA) KC072503-4,250 rig/L Standard 080103A-2005 10 Sm (Mn, 2x3) 9.13 78794 02-Aug-2003 03:54:13/ LC/MS/MS #6 MRM of 4 Channels ES413>369 4.78e5 Area w 2: C6 Sulfonate XCO72503-4,250 (PFHS) rig/L Standard 080103A-2005 100- Sm (Mn, 2x3) %- 3: C8 Sulfonate [XCO72503-4,250 (PFOS) rig/L Standard 080103A-2005 Sm (Mn, 2x3) 8.98 15770 02-Aug-2003 03:54:13 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 9.57e4 Area 8 I I , . I I , I r I 1Time 10.00 12.00 02-Aug-2003 03:54:1 I LCNSNS #c MRM of 4 Channels ES- 499 > 99 5.56e4 Area Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000298 Quantify Sample Report +4 Study No.:L34910, set NO .:080103A, Ext.Dats:00/01/03, &aalyet:K.Risha Salqple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\MasslyPx\Fluorochemicals.PRO\S~leDB\O8DlO3A Sun Aug 03 07:25:44 2003 P:\Data\L(IMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 10 Decatur BC BC 080103 Name: Text: 000103A-2005 4L: PFOSA (CO72503-4,250 rig/L Standard 180103A-2005 10 "f %$ Sm IMn. 2x31 O'~~",~,",`~~`,`~~~,~~`~,~"`,,~~~,~"~,~~",~" 2.00 4.00 6.00 8.00 02-Aug-2003 03:54:1 Z LC/MS/MS #6 MRM of 4 Channels ES- 9.90 49% > 78 3669: I 1.95e5 Area I Time 12.00 RWgen Research, 3058 Research Drive, Stata Collage, PA 16801 000299 __1---- -- --- --------me- Quantify Simple Report N4 Study No.:L34910, Set No .:080103A, Fkt.Date:08/01/03, Analyst:X.Risha SasllDle List: Last modified: Method: Last modified: Job Code: P:\Data\LCW~S6\blassl~\Fluoroch~ca~s.PRO\S~leDB\O80103A Sun Aug 03 07:25:44 2003 P:\Data\L(lbiSMS6\Masslynx\FluorochemicaB\Decatur Sun Aug 03 07:11:59 2003 Page 11 Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 ----------------------------------------------------- ---w----w-- Name: 080103A-2006 Text : :-C8 Acid (PFOA) EO72503-5,500 rig/L Standard )80103A-2006 -loo- Sm (Mn, 2x3) %- 9.12 171634 02-Aug-2003 04:15:54j LCIMSIMS #6 MRM of 4 Channels ES413> 369 l,Ole6 Area 2: C6 Sulfonate XCO72503-5,500 2.00 4.00 (PFHS) rig/L Standard 080103A-2006 10 Sm (Mn, 2x3) 6.00 8.00 8.98 31281 02-Aug--2003 04:15:54/ LCNSNS #6 MRM of 4 Channels ES399 > 80 1.90e5 Area I, I,, / 10.00 (1, I r 7 Time 12.00 , 3: C8 Sulfonate (PFOS) XCO72503-5,500 rig/L Standard 02-Aug-2003 04:15:54 LC/MS/MS #6 080103A-2006 Sm (Mn, 2x3) MRM of 4 Channels ES- lo@4-1 i 9.24 19171 499 > 99 l.lle5 Area %1 A-?- Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16803 000300 Quantify Sample Report tiu' study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyet:K.Risha Sample List: Lant modified: Method: Last nmdif ied: Job Code: P:\Data\~SMS6\Massl~\Fluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 1003 P:\Data\LCMSMS6\Mssslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Pags 12 Decatur BC BC 080103 Name: 080103A-2006 Text : 4: PFOSA XCO72503-5,500 rig/L Standard 080103A-2006 1001 Sm (Mn, 2x3) %- 02-Aug-2003 04:15:54 LC/MS/MS #6 MRM of 4 Channels ES- 9.92 498 > 78 3.82e5 Area , , , , , , Time 10.00 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 000306 Quantify Sample Report vd Study No.:L34910, Set No.: 000103A, Ext.Date:08/01/03, Analyst:K.Risha Page 13 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\MasslWr\Fluorochermlcals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LQHSMS6\MasslyPx\FluorochsmicaleB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: -e-p- Sun Aug 03 07:32:25 2003 ~---------------------------- NallBB: 080103A-2007 Text: e----m- 1: CB Acid (PFOA) XCO72503-6,lOOO rig/L Standard 080103A-2007 lO& Sm (Mn, 2x3) %- 9.13 315768T 02-Aug-2003 04:37:34 LC/MS/MS #6 MRM of 4 Channels ES413>369 1.84e6 Area 0 ,~~,,,~,,,,~~~,,,,,,,~,~,~~,,,,,,,,~,,,,,,,,~,~,,,,,,,,,,,,Time 2.00 4.00 6.00 vii, 2: C6 Sulfonate (PFHS) XCO72503-6, 1000 rig/L Standard 080103A-2007 lOO- I Sm (Mn, 2x3) 8.00 6.98 10.00 12.00 02-Aug-2003 04:37:34 LC/MS/MS #6 MRM of 4 Channels ES- 399 > 80 3.49e5 Area 2.00 4.00 6.00 3: C8 Sulfonate XCO72503-6,1000 (PFOS) rig/L Standard 080103A-2007 loo- Sm (Mn, 2x3) %- %cIJ - ~,~,,,,,,~,,~~,,,,,,,,,,,,~.~~,~,~,,~~~~,~~~~,1(1:~~,..~~,~~~~1Time 2.00 4.00 6.00 8.00 9.25 37079 10.00 12.00 02-Aug-2003 04:37:34 LClMS/MS #6 MRM of 4 Channels ES- 499 > 99 2.12e5 Area 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000302 Quantify S-10 Report Study No .:L34910, Set No.:080103A, Kxt.Date:08/01/03, Analyst:K.Risha Page 14 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCblSMS6\blasslyPx\Fluoroch~cals.~RO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\L(1MSMS6\Maselyax\Fluorochamicalr Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: --------_I--------_______I Sun Aug 03 07:32:25 2003 --__------------ ------------____ Name: 080103A-2007 Text : 4: PFOSA XCO72503-6,1000 I / 080103A-2007 Sm I1nfh rig/L Standard (Mn, 2x3) 02-Aug-2003 04:37:34/ LC/MS/MS #6 MRM of 4 Channels ES- 9.92 _ 137821 498 > 78 7.22e5 Area , , , , , , , Time 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 .._"_I.,-_,.- 000303 Quantify Sample Report Study No .:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:X.Rieha Sam@0 List: Last modified: Method: Last modified: Job Code: P:\Data\LWSMS6\Masslynx\Fluorochemical~.~RO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Maeelynx\FluorochemicglsB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:2S 2003 Page 15 Decatur BC BC 080103 Name : 080103A-2008 Text: 1: C8 Acid (PFOA) Methanol Wash I0801 0314-2008 Sm (Mn, 2x3) II 10%(1i7J-W 01,,,,,,,,,,~,~~,,~~~I~,,,,,,~~,,~~,,~~~~,~~~~,~~~~1~~,~,~~~~1Time 2.00 4.00 6.00 2: c6 Sulfonate Methanol Wash (PFHS) 080103A-2008 Sm (Mn, 2x3) 9.15 525 I 8.00 I v 02-Aug-2003 04:59:21 LCNSIMS #6 MRM of 4 Channels ES- 413> 369 5.39e3 A Area ""\ 10.00 12.00 02-Aug-2003 04:59:21 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 O~,...,,...,....,,,..,..,.,.,..,~...,,...,....,....,~...,...,~Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate Methanol Wash (PFOS) 080103A-2008 Sm (Mn, 2x3) MRM of 4 Channels ES- Exygsn Research, 3058 Research Drive, State College, PA 16801 000304 Quantify Sample Report Study No .:L34910, Sot No.:080103A, Ext.Dats:08/01/03, AnalystrK.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\M4sslynx\Fluoroch~cals.PRO\S~l~DB\O8OlO3A Sun hug 03 07:25:44 2003 P:\Data\LCMSMS6\blasslynx\FluorochamicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: ---- Sun hug ------l----__-__------------~---- 03 Oi'r32:25 2003 Name: 080103A-2008 Text : .: PFOSA klethanol Wash 180103A-2008 100-I Sm (Mn, 2x3) Page 16 Decatur BC BC 080103 ----------a___ I -Aug-2003 04:59:2 LC/MS/MS # MRM of 4 Channels ES, 9.?3 498> 7t Oxygen Research, 3058 Research Drive, Stats College, PA 16801 000305 Quantify Sample Report Study No.:L34910, Set Nb .:080103A, Ext.Date:08/01/03, Analyst:K.Risha saIllQ1e List: Last modified: Method: Last modified: Job Code: P:\Data\LCMISMS6\bfasslyPx\Bluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 17 Decatur BC BC 080103 Name: 080103A-2009 Text : 1: C8 Acid (PFOA) Reagent Blank 080103A-2009 Sm (Mn, 2x3) 100-J b %- OW, .i-. , , , , Y., , ,,,, f: I, ,>Time 2.00 4.00 6.00 2: C6 Sulfonate Reagent Blank (PFHS) 02-Aug-2003 05:20:57 LC/MS/MS #6 MRM of 4 Channels ES413s369 1.71e4 Area 9.10 518 8.00 10.00 12.00 02-Aug-2003 05:20:57 I LC/MS/MS #6 MRM of4 Channels ES- %- 0 ,,,,,~,~,,,,,~,~~.,,~,~~r,~,~,,.~~,~.,~,.~~.r~~~~,~~~~,~~~~ITime 2.00 4.00 6.00 8.00 3: C8 Sulfonate Reagent Blank (PFOS) 080103A-2009 Sm(Mn,2x3) 10.00 12.00 _ 02-Aug-2003 O&20:57 LC/MS/MS #6 MRM of 4 Channels ES- 0 ,~,,,,,,,,,,~~,,,,,,,,,,r~~,~,~~~~,~~~~,,~,~,~~~.,,~~.r,~.,ITime 2.00 4.00 6.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 10.00 12.00 000306 Quantify Sample Report ,d Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~~S6\Masslynx\Fluorocb~ca~s.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LBrlSMS6\Masslynx\FluorochemiealB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 18 Decatur BC BC 080103 Name: 080103A-2009 Text: 4: PFOSA Reagent Blank 080103A-2009 Sm (Mn, 2x3) C2-Aug-2003 05.:20:57 LX/MS/MS #6 MRM of 4 Channels ES- 9.93 498 > 78 747 11.84 i O'~~~~,~`~~,~~~~,~~~~,~~~~,~~~~,,~,,,~,,,,,,,,,,.,,,,,,,,,,,,, 2.00 4.00 6.00 8.00 10.00 Time 12.00 ExVoen Research, 3058 Research Drive, Stat- College, PA 16801 ---------_ --I_-- ----e-1111-------__-- Quantify Saarplrr Report w Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~S6\bsslynx\Fluoroch~cals.PRO\S~leDB\O8O~O3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicala\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 19 Decatur BC BC 080103 Name: 080103A-2010 Text: 1: C8 Acid (PFOA) Reagent Spk A, 50 rig/L 080103A-2010 Sm (Mn, 2x3) 02-Aug-2003 05:42:42 LC/MS/MS #6 MRM of 4 Channels ES413>369 1.12e5 Area 1: C6 Sulfonate (PFHS) qeagent Spk A, 50 rig/L 180103A-2010 10 Sm (Mn, 2x3) Time 12.00 02-Aug.2003 05:42:42 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 345i I.9834 Area L 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) Reagent Spk A, 50 rig/L 080103A-2010 10 Sm (Mn, 2x3) 02-Aug-2003 05:42:44 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.21 e4 Area 2.00 4.00 Time 6.00 8.00 1o:oo 12100 J Oxygen Research, 3058 Research Drive, State College, PA 16801 000308 Quantify Sample Report w Study No.:L34910, Set No,: 080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSbIS6\~sslyPx\Fluoroch~cals.PRO\S~leDB\O80103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals\Decatur Sun Aug 03 07:ll:SS 2003 Printed: Sun Aug 03 07:32:25 2003 Page 20 Decatur BC BC 080103 Name: 080103A-2010 Text : : PFOSA leagent Spk A, 50 rig/L 180103A-2010 Sm (Mn, 2x3) -I % i , 02-Aug-2003 05:42:44 LCYMSIMS #6 MRM of 4 Channels ES- 9.90 498 > 78 675C 3.52e4 Area O'..,,,,,l',,,.`,`,~`,,l,`,.`,,,,',,,"',,',,.,',~ Time 2.00 4.00 6.00 8.00 10.00 12.00 -gOA Research, 3058 Research Drive, State College, PA 16801 000309 ----- --- v-e---- -----_ Quantify Sample Report q&J Study No.: L34910, Set No.:080103A, Ext.Data:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: irob Code: P:\Data\LQaSMS6\ManslyPx\FluorochemicalP\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\~SMS6\MasslyPx\Fluorochemicals.PRO\Met~B\Decatur Sun Aup 03 07:11:59 2003 Page 21 Decatur BC BC 080103 Printed: ----------------------- Sun Aug 03 07:32:25 2003 --M---w---- --w------_ Name : 080103A-2011 Text: L: C8 Acid (PFOA) Reagent Spk B, 500 ng./L 080103A-2011 Sm (Mn, 2x3) 9.15 163063 02-Aug-2003 06:04:24 LCiMS/MS #6 MRM of 4 Channels ES413 > 369 9.90e5 Area m Time I 2.00 4.00 6.00 8.00 10.00 12.00 !: C6 Sulfonate (PFHS) Reagent Spk B, 500 rig/L 02-Aug-2003 06:04:23/ 080103A-2011 10 Sm (Mn, 2x3) 6.99 31000 %- I: C8 Sulfonate (PFOS) qeagent Spk B, 500 rig/L 380103A-2011 `OO-4 %I-,I Sm (Mn, 2x3) 2.00 9.25 1758: I3L- 02-Aug-2003 06:04:23 LC/MS/MS #6 MRM of 4 Channels ES> 99 4991.05e5 Area Time 8.00 10.00 12.00 , Oxygen Research, 3058 Research Drive, State College, PA 16801 _II_ .._. ll--_------- - QOO31Q ---- ----- Quantify Sanr~le Report u Study No.:L34910, Set No .:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sampls List: Last modified: Method: Last modified: Job code: P:\Data\LCM~S6\Masslynx\Pluoroch~cals.PRO\S~l~D~\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCbl~S6\Masslynx\Fluorochsmicals.PRO\Met~B\D~catur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 22 Decatur BC BC 080103 Name: 080103A-2011 Text : 4: PFOSA Reagent Spk 8,500 rig/l 080103A-2011 100-j Sm (Mn, 2x3) %- 0%Aug-2003 06:04:23 LCNSNS #6 MRM of 4 Channels ES- 9.89 498> 78 3.52e5 Area 0 "","","","","","","","","", , I , 1 , , , ,Time 2.00 4.00 6.00 8.00 10.00 12.00 _ Exyrren Research, 3058 Research Drive, State College, PA 16801 .""-. ..- .._. "-.~--_-- ."- 000311 Quantify Sam&i Report 44 Study No.:L34910, Set No.. -080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 23 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCW~S6\~sslynx\FluorochamicaB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ------_---- Sun Aug 03 07:32:25 2003 --- ------------ ------- ------ Name: 080103A-2012 Text : 1: C8 Acid (PFOA) KC072503-1,25 rig/L Standard 080103A-2012 Sm (Mn, 2x3) . 02-Aug-2003 06:26:1 C LC/MS/MS #6 MRM of 4 Channels ES- I 9.14 413>369 982C I 5.69e4 Area \,& 2: C6 Sulfonate (PFHS) XCO72503-1,25 rig/L Standard 080103A-2012 lOO- Sm (Mn, 2x3) %- I v 10.00 Time 12.00 02-Aug-2003 06:26:1 C LC/MS/MS #6 MRM of 4 Channels ES- 8.99 399 > 80 1.13e4 Area 0 ,,,#.r* I , I . I . , I I I I I Time 2.00 4.00 6.00 8.00 10.00 12.00 _ 3: C8 Sulfonate XCO72503-1,25 (PFOSI rig/L Standard 080103A-2012 100- Sm (Mn, 2x3) %- 02-Aug-2003 06:26:1 t Lcnns/Ms #6 MRM of 4 Channels ES- 9.25 499 > 9s 5.93e3 Area rllwf 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report \\r~ Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:X.Xisha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluorochemicals.PXO\s~leDB\O~OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LQ3SWS6\~sslynx\Fluorochsmicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 24 Decatur BC BC 080103 Name: 0801031-2012 Text : 4: PFOSA XCO72503-1,25 rig/L Standard 080103A-2012 100- Sm (Mn, 2x3) %- 02-Aug-2003 06:26:1 t) LClMShlS #6 MRM of 4 Channels ES- 9.88 498 > 78 2.01e4 Area 0 "","","'1,"","'~,"","","","",", I , , , , , , , Time 2.00 4.00 6.00 8.00 10.00 12.00 me= Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report 9b*1/ Study No.:L34910, Set NO.: 080103A, EXt.Date:08/01/03, Analyst:R.Risha Sanlpls List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochsmicals.PRO\S~leDB\OSOlO3A Sun Aug 03 07:25:44 2003 P:\Data\L(SM~S6\~sal~\Fluorochemi\D~catur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 25 Decatur BC BC 080103 Name: 0801031-2013 Text : : C8 Acid (PFOA) -34910-5 Spk C, 5000 rig/L, DF=lO 380103A-2013 10 Sm (Mn, 2x3) 9.13 157971 02-Aug-2003 06:47:56j LC/MS/MS #6 MRM of 4 Channels ES- 413>369 9.32e5 Area !: C6 Sulfonate (PFHS) L34910-5 Spk C, 5000 rig/L, DF=lO 080103A-2013 10 ]# Sm (Mn, 2x3) % ,,,,,,,,,,,,,,,, I ,,,,,,,,,,,,,,,,,,,,,,,,,, 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) L34910-5 Spk C, 5000 rig/L, DF=lO 080103A-2013 100- Sm (Mn. 2x3) %- 0 ,,"~,,,,,,,,,,,,,~,,`,`,."`,"","","", 2.00 4.00 6.00 8.98 30746 02-Aug-2003 06:47:5 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.76e5 " Area 8.00 499 > 99 1.36e5 Area 1 c , I I I I , I I 1 Time 8.00 10.00 12.00 RW!Wn Research, 3058 Research Drive, State Collage, PA 16801 000324 Quantify Sample Report ,d Study No.:L34910, Set No.. *OBO103A, Ext.Date:08/01/03, Analyst:R.Risha Sample List: Last modified2 Method: Last modified: Job Coda: P:\Data\LCab~S6\blas8l~\Fluotochamicals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\L~SMS6\Masslynx\FluorochamicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 26 Decatur BC BC 080103 Name: 080103A-2013 Text : r: PFOSA -3491 O-5 Spk C, 5000 rig/L, DF=lO 180103A-2013 10 Sm (Mn, 2x3) % I i O'~~~,,`~~~,`~",~`,~,`~~~,~~~~,~~~~,~~,',~~~~,`~~ 2.00 4.00 6.00 8.00 02-Aug-2003 06:47:56 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 79517 , 498 > 78 4.18eS Area L10.00 lime 12.00 1 ExyOen Research, 3058 Research Drive, State College, PA 16601 0003l5 Quantify SamQls Report A,& Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\bsslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslyax\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 27 Decatur SC BC 080103 Name: Text: 080103A-2014 1: C8 Acid (PFOA) IL3491 O-1 0 Spk D, 5000 rig/L, DF=lO 080103A-2014 Sm (Mn, 2x3) %- 02-Aug-2003 07:09:35/ LCNSIMS #6 MRM of 4 Channels ES413> 369 9.88e5 Area 2.00 4.00 6.00 : C6 Sulfonate (PFHS) -34910-10 Spk D, 5000 rig/L, DF=lO 380103A-2014 loo- Sm (Mn, 2x3) 8.00 8.98 3219: 2 10.00 12.00 _ 02-Aug-2003 07:09:3!j LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.89e5 Area L 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) 134910-10 Spk D, 5000 rig/L, DF=lO 080103A-2014 lOO- Sm (Mn, 2x3) %- 0 ,~,,,,,,,,,,,,,~,,~,,,,,,,,,,,,,,,,~,,,,,,,,,~,,,,,,,,,,,.lTime ! 2.00 4.00 6.00 A-8.00 10.00 Time 12.00 9.25 _ 26935 02-Aug-2003 07:09:35 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.62e5 Area 8.00 10.00 12.00 %Wen Research, 3058 Research Drive, State College, PA 16801 00032.6 Quantify Sample Report \J Study No.:L34910, Set No.: 080103A, E&.Date:08/01/03, Analyst:K.Risha Page 28 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluoroch~cal~.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LBISMS6\Masslynx\Fluorochemicalscatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Rug 03 07:32:25 2003 ----- ----------I_---- -------------_- ----- Name: 0801031-203.4 Text : 4: PFOSA -3491 O-l 0 Spk D, 5000 rig/L, DF=lO 180103A-2014 Sm [Mn. 2x3) I . r 02-Aug-2003 07:09:36 LCNSIMS #6 MRM of 4 Channels ES- 9.09 8221; ! 498 > 78 4.27e5 Area O'.,.,,,,~,,,,`.,.,..,,.,,,,,.,,,,,,,,',,,',,,,l.~ L- Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sax&s Report t& Study No.:L34910, Set NO.: 080103A, mct.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQHSMS6\~sslyax\Pluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\FluorochamicalsB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 29 Decatur BC BC 080103 Name: 080103A-2015 Text : * C8 Acid (PFOA) -34910-l 1 Spk E, 5000 rig/L, DF=lO 380103A-2015 10 Sm (Mn, 2x3) 0x2 1 2.00 4.00 6.00 \14 2: C6 Sulfonate (PFHS) L34910-11 Spk E, 5000 rig/L, RF=10 080103A-2015 lOO- Sm(Mn,2x3) %- 9.13 18766t 5 02-Aug-2003 07:31 :17 LC/MS/MS #6 MRM of 4 Channels ES413> 369 l.lle6 Area L-_- 8.00 10.00 Time 12:oo 02-Aug-2003 07:31: 17 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399> 80 1 .SOe5 Area 2.00 4.00 6.00 : C8 Sulfonate (PFOS) -34910-l 1 Spk E, 5000 rig/L, DF=lO )80103A-2015 10 Sm (Mn, 2x3) 8.00 9.27 33638: 10.00 12.00 J 02-Aug-2003 07:31 :17 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.9566 Area mgen Research, 3056 Research Drive, State Collage, PA 16601 "--^...-.1- -..- -.- --------_ ------- -------------__-- Quantify Sample Report ,,& Study No.:L34910, Set No.. -080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 30 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\~ss~ynx\Fluoroch~cals~PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 ----------------__I-----------___________I_ -------------___-_ Name: 080103A-2015 Text : I: PFOSA -34910-I 1 Spk E, 5000 g/L, DF=lO 380103A-2015 10 7 % -i Sm (Mn, 2x3) 02-Aug-2003 07:31 :l' LC/MS/MS #I MRM of 4 Channels ES- 9.88 15509t 3 498 > 71 7.93e! Are: O',,,`,~.",.,~`,,.",,,`,,`,~`,.".,,,,',,',,,,,, L. Time t 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ooam9 Quantify Sanlple Report w Study No.:L34910, Set No. :080103A, Ext.Date:08/01/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\~S6\Masslynx\Fluorochamicals.PRO\S~leDB\O6OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LQHSMS6\Masslyax\Fluorochemicalsr Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 31 Decatur flC BC 080103 Name: 000103A-2016 Text : 1: CB Acid (PFOA) L34910-20 Spk F, 5000 rig/L, DFdO 080103A-2016 loo- Sm (Mn, 2x3) %- 9.13 1790901 02-Aug-2003 075254 LCIMSNS #6 MRM of 4 Channels ES413> 369 1.02e6 Area 0 ,,,.;7-..,,~...,~,..,,~~,,...~,.~~.,..~.,~..~~~.~,..~.,.~.~,Time 2.00 4.00 6.00 : C6 Sulfonate (PFHS) -3491 O-20 Spk F, 5000 rig/L, DF=lO 180103A-2016 `O(+ Sm (Mn, 2x3) 8.00 8.96 3234: 10.00 12.00 02-Aug-2003 07:52:54 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.91e5 Area O',,`,,,,~,,,,,,,`,,`,,.~`,,,",`,',,",,,,,'~ L 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) L34910-20 Spk F, 5000 rig/L, DF=Y 0 080103A-2016 100- Sm (Mn, 2x3) %- 8.00 9.25 ,,I, , 10.00 b - 1 Time 12.00 02-Aug-2003 07:52:54 LCIMSIMS #6 MRM of 4 Channels ES499 > 99 4.1385 Area , I , I , . . I j 1 Time 10.00 12.00 Oxygen Research, 3056 Research Drive, State College, PA 16801 000320 Quantify Sample Report ,14 Study No.:L34910, Set No.. l 080103A, Ext.Date:08/01/03, Analyst:K.Risha SamQle List: Last modified: Method: Last modified: Job Code: P:\Data\M3HSMS6\nbasslynx\Fluoroch~cals.PRO\S~~aDB\O8OlO3A Sun Rug 03 07:25:44 2003 P:\Da~a\LCMSIS6\Masslyrur\FluorochamicalS.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: -------A-- Sun Aug 03 07:32:25 2003 ----------__-------~---- Name: Text: 0801031-2016 Page 32 Decatur EC EC 080103 --- tL34910-20 Spk F, 5000 rig/L, DF=IO 080103A-2016 lOO- Sm (Mn, 2x3) %- 02-Aug-2003 075254 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 z 78 5.19e5 Area , , , , , I , , , Time 10.00 12.00 Oxygen Research, 3058 Research Drive, State Collage, PA 16801 w-w---- -------- ----- --- Quantify Sample Report -,+, Study No.:L34910, Set No.: 080103A, Ext.Dats:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Coda: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~~eDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochesnicals.PRO\Mat~B\D~catur Sun Aug 03 07:11:59 2003 Printed: e---e------ Sun Aug 03 07:32:25 2003 ------------------------~-_- Nams: 0801031-2017 Text : 1 : C8 Acid (PFOA) (CO72503-2,50 rig/L Standard 180103A-2017 10 9 Sm (Mn, 2x3) 9.13 181901 ---m-m- page 33 Decatur BC BC 080103 02-Aug-2003 08:14:41 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 1 .lOe5 Area 2.00 4.00 6.00 8.00 `IlId 9I: C6 Sulfonate i : KO72503-2,50 (PFHS) rig/L Standard 180103A-2017 10 Sm (Mn, 2x3) 02-Aug-2003 08:14:41/ LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 3449 2.06e4 Area 2.00 4.00 6.00 i: C8 Sulfonate KC072503-2,50 (PFOS) rig/L Standard 080103A-2017 `Oo7 % 1 Sm (Mn, 2x3) 02-Aug-2003 08:14:41 LCIMSNS #6 MRM of 4 Channels ES- 9.24 499 z 99 2233 1.34e4 Area I_;;, - 10.00 Time 12.00 -en Research, 3058 Research Drive, Stata College, PA 16801 088322 -- QUantify Sample Study No .:L34910, -------------_ Report Set No.:080103A, Ext,Dats:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\blasslynx\Fluor4ch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\~t~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 w--m-- ------- ------ -w--I__----p_ Name: 080103A-2017 Text : 4: PFOSA (XCO72503-2,50 rig/L Standard 080103A-2017 Sm (Mni 2x3) Page 34 Decatur BC BC 080103 02-Aug-2003 08: 14:41[ LC/MS/MS #6 MRM of 4 Channels ES498 > 78 4.1 Oe4 Area Time 12.00 Oxygen Research, 3058 Research Drive, State College, PA 36801 ."_ ----- 000323 ----- -I_------- Quantify Sample Report \& Study No.:L34910, Set No.: 080103A, Ext.Data:08/01/03, Analyst:X.Risha Page 35 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Msssl~\Fluoroch~cals.PRO\S~leDB\O~DlO3A Sun Aug 03 07:25:44 2003 P:\Data\L~~S6\~sslyIw\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:ll:SS 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 -------___ --------------------------------~---- ------ Name: 080103X-2018 Text : 1: C8 Acid L3491 o-5 (PFOA) 180103A-2018 10 Sm (Mn, 2x3) 9.15 115451 02-Aug-2003 08:36:27 LC/MS/MS #6 MRM of 4 Channels ES413>369 6.67e5 Area i 2.00 4.00 6.00 8.00 !: C6 Sulfonate L3491 o-5 (PFHS) 02-Aug-2003 08:36:2 080103A-2018 Sm (Mn, 2x3) 10 8.98 4534 2.00 4.00 6.00 8.00 10.00 12.00 I 3I: C8 Sulfonate -3491 o-5 (PFOS) )80103A-2018 Sm (Mn, 2x3) 9.27 1.. 60613 02-Aug-2003 08:36:2? LC/MS/MS #6 MRM of 4 Channels ES499358A>ere59a9 Time 2.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 'cc 000321 -w---_II -----A --1_- -v---1_-- ---- Quantify Sample Report \Ir, Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:X.Riaha Page 36 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~~S6\bssl~\Fluoroch~cals.P~\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\MasslyPx\Fluorochemicals\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: --WV-- Sun Aug 03 07:32:25 2003 -------------------------------- Name: Text: 0801031-2018 --_-_-- ---- : PFQSA -3491 o-5 380103A-2018 Sm (Mn, 2x3) 9.90 12188: 02-Aug-2003 08:36:2; LC/MS/MS #f MRM of 4 Channels ES- 496> 7E 2 6.28e5 Area I Time 12.00 Exyoen Research, 3058 Research Drive, State College, PA 16801 Quantify sml.9 Rsport \ulJI Study No.:L34910, Set No .:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Wethod: Last modified: Job Code: P:\Data\LCM~S6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCblSMS6\Masslynx\FluorochemicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: -m--v- Sun Aug 03 07:32:25 -------------- 2003 -m---e--- -------m Name: 080103A-2019 Text : 1: C8 Acid (PFOA) rI-3491 O-5 Rep I (180103A-2019 Sm (Mn, 2x3) lOO-4 `2 , %1 I I- %& 2: C6 Sulfonate L3491 O-5 Rep (PFHS) 080103A-2019 Sm (Mn, 2x3) Page 37 Decatur BC BC 080103 02-Aug-2003 08:58:12 LC/MS/MS #6 MRM of 4 Channels ES- 413>369 4.81e5 Area Time 12.00 _ 02-Aug-2003 08:58:12 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.09e4 Area 3 : C8 Sulfonate -3491 O-5 Rep (PFOS) 380103A-2019 Sm (Mn, 2x3) 9.25 51074 Time 12.00 ~ 02-Aug-2003 08:58:12 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.06e5 Area , , , , , , , , , , , `Time 10.00 12.00 -gOa Research, 3058 Research Drive, State College, PA 16801 WO3Xi . "_ _-_.--- -.-. ._ --.-- _ ._-,,__ "--_ . quantify saxuple Report ,& study NO.:L34910, Sat No.: 060103A, Ext.Date:06/01/03, Analyst:K.Risha page 38 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Massl~\Fluoroc~cals.PRO\S~leDB\OSOlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCM~S6\Masslynx\Fluoroch~cals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: v----e- Sun Aug _I_-----__----------------------------_-- 03 07:32:25 2003 Name: 0801031-2019 Text : 4: PFOSA L3491 o-5 Rep I(180103A-2019 Sm (Mn, 2x3) 9.88 13358: 02-Aug-2003 08:58:1: LCYMWMS #1 MRM of 4 Channels ES- 498 > 7t 3 6.93e! Are: 2.00 4.00 I Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 008327 --- ----_- -------- --------- Quantify Sample Report w Study No.:L34910, Set No.. -080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 39 Sample List: Laat modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Wasslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3A sun Aug 03 07:25:44 2003 P:\Data\LCWSblS6\Wasslynx\BluorochemfcslB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 --m-e--------- ---------------------------------_- --- Name: 080103A-2020 Text : .: C8 Acid (PFOA) -3491 o-1 0 380103A-2020 lo? Sm (Mn, 2x3) 02-Aug-2003 09: 19:59 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 1.13e6 Area 2.00 4.00 6.00 8.00 10.00 12.00 )* C6 Sulfonate i3491 o-1 0 (PFHS) 02-Aug-2003 09:19:5 080103A-2020 10 Sm (Mn, 2x3) 8.97 10896 Area v Time / 2.00 4.00 6.00 8.00 10.00 12.00 I 3: C8 Sulfonate L3491 o-1 0 (PFOS) ,080103A-2020 IOO- Sm (Mn, 2x3) %- 02-Aug-2003 09:19:5I LCiMSlMS #E MRM of 4 Channels ES499 > 99 5.38e5 Area , I I I l , I ( I ,lTime 10.00 12.00 Eyygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report w Study No.:L34910, Set No.. l 080103A, E%t.Date:08/01/03, Aualyst:K.Rieha Santpls List: Last modified: Method: Last modified: Job Code: P:\Data\LC41~S6\bsslylur\Fluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCM~S6\Massl~\Fluoroch~cals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 40 Decatur BC BC 080103 Name: 080103A-2020 Text : 4: PFOSA L3491 (J-1 0 080103A-2020 100- Sm (Mn, 2x3) %- 02-Aug-2003 09:19:59 LWMWMS #6 MRM of 4 Channels ES- 9.91 _ 133763 498 > 78 6.89e5 Area 1 t I , r I , , 1 Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000329 ------ Quantify Sample Report ,4 Study No.rL34910, Set No.. *000103A, Ext.Date:08/01/03, --Analy8t:K.Risha -Page 41 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQb~S6\Maasl~\Fluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\L~SMS6\Ma~al~\FluorochamicaB\Decatux Sun Aug 03 07:11:59 2003 Decatur SC BC 080103 Printed: ---- Sun Aug 03 07:32:25 2003 ----------_---------A-- Name: 080103A-2021 Text : ----__l--------_--_ --me------- : C8 Acid (PFOA) -3491 O-l 0 Rep )80103A-2021 10 Sm (Mn, 2x3) 9.13 16782 6 02-Aug-2003 09:41:4j LC/MS/MS #6 MRM of 4 Channels ES413>369 9.66eS Area : C6 Sulfonate -3491 O-l 0 Rep (PFHS) )80103A-2021 lo& Sm (Mn, 2x3) I 8.98 1299s Time 12.00 02-Aug-2003 09:41:47 LWMWMS #6 MRM of 4 Channels ES399 > 80 7.94e4 Area 2.00 4.00 6.00 8.00 3: C8 Sulfonate IL3491 O-l 0 Rep (PFOS) 02-Aug-2003 09:41:47/ 080103A-2021 `Oo-2 Sm (Mn, 2x3) 2.00 4.00 6.00 8.00 10.00 E%ygen Research, 3058 Research Drive, State College, PA 16801 12.00 ---------___-__1--___I----------- Quantify Sanlple Report ,4 Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, ?tnalyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\bssl~\Fluoroch~ca~s.PRO\S~leDB\O60103A Sun Aug 03 07:25:44 2003 P:\Data\L~SMS6\Mrrssl~\~luorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 -- Page 42 Decatur BC BC 080103 Name : 000103A-2023 Text : 4: PFOSA L3491 O-l 0 Rep 080103A-2021 loo- Sm (Mn, 2x3) %- 02-Aug-2003 09:41:47 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 191201 498> 78 9.92e5 Area 0 ~,,,,,,~,,~,,,,,,,,,,~~~,~,,,,,~,,,~~~~,~~~~,.~~~~~~~,~~~,;Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000331 Pm------- -- m-v-- Quantify Sample Report `NY Study No .:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L(=blSMS6\Massl~\Fluoroch~ca~s.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicsls.PRO\Met~B~Dacatur Sun Aug 03 07:11:59 2003 Page 43 Decatur RC BC 080103 Printed: Sun Aug 03 07:32:25 2003 -me-- ----------- ----------cI_------------- --- Name: Text: 080103A-2022 : CB Acid (PFOA) (CO72503-3, 100 rig/L Standard )80103A-2022 lo9 Sm (Mn, 2x3) % 02-Aug-2003 10:03:27j LC/MS/MS #6 MRM of 4 Channels ES- 9.15 413> 369 2.02e5 Area i 2.00 4.00 10.00 Time 12.00 !: C6 Sulfonate KO72503-3,100 (PFHSI rig/L Standard 380103A-2022 10 Sm (Mn, 2x3) 02-Aug-2003 10:03:27j LChK/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 656C 3.80e4 Area 2.00 4.00 6.00 8.00 3: C8 Sulfonate XCO72503-3,100 (~~0s) rig/L Standard 080103A-2022 10 Sm (Mn, 2x3) 02-Aug-2003 10:03:2? LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 3634 2.23e4 Area 2.00 4.00 6.00 L-;, Time 12.00 RJWWn Rssawch, 3058 Research Drive, Stats Collage, PA 16801 QOO332 -------------PI- ---- Quantify Sample Report q,d Study No. :L34910, Set No.: 080103A, Ext.Date:08/01/03, kralyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSWS6\Masalynx\Fluoroch~cals~PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 -Page 44 Decatur BC BC 080103 Name: 0801031-2022 Text : 4: PFOSA IXCO72503-3, 100 rig/L Standard 080103A-2022 lOO- Sm (Mn, 2x3) %- 02-Aug-2003 10:03:27j LC/MS/MS #6 MRM of 4 Channels ES- 9.90 _ 14698 498 > 78 7.86e4 Area 0 "","l',"","","","","","","","' Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 -------e---P- --- ---- ---- Quantify Sample Report w Study No. :L34910, Set No .:080103A, Bxt.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\Lc=MSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\OSOlO3A sun hug 03 07:25:44 2003 P:\Data\LcZIISMS6\Massl~\Fluoroch~cals.PRO\MethDB\Decatur sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 45 Decatur BC BC 080103 Name: Text: 080103A-2023 1: C8 Acid (PFOA) XCO72503-4,250 rig/L Standard 080103A-2023 Sm (Mn, 2x3) lOO- 9.13 %- 1 0 "8 r,= * ,,r f 8 ,(I 2.00 r I I,8 8 n ,,I 4.00 r 8 I,`) 6.00 8 ,,I'# tJ 2: C6 Sulfonate (PFHS) XCO72503-4,250 rig/L Standard 080103A-2023 100- Sm (Mn, 2x3) (,)`I r 8.98 %- 02-Aug-2003 10:25:1 C LC/MS/MS #6 MRM of 4 Channels ES- 413>369 4.72e5 Area , , , I , , I a I , Time 10.00 12.00 02-Aug-2003 10:25:1 C LC/MS/MS #6 MRM of 4 Channels ES399 > 80 9.02e4 Area * o- ~"`,`."`,"")`.","","","","", , I I I 1 , , I 1 . 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 I 1: C8 Sulfonate #CO72503-4,250 (PFOS) rig/l Standard 080103A-2023 Sm (Mn, 2x3) 02-Aug-2003 10:25:1 C LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 8965 5.15e4 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 wgen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report w Study No.:L34910, Set No.: 080103A, Ekt.Date:08/01/03, Analyst:K.Risha Page 46 SamOle List: Last modified: Method: Last modified: Job Code: P:\Data\LOMS~S6\~ssl~\Fluorochemicals.PxO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LWSMS6\Masslynx\FluoroChsmicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 ---- --------------------------- --- --es---_ -- Name : 080103A-2023 Text: 4: PFOSA IXCO72503-4,250 rig/L Standard 080103A-2023 Sm (Mn, 2x3) 02-Aug-2003 10:25:1( LCIMSNS #f MRM of 4 Channels ES- 2.00 4.00 6.00 8.00 10.00 12.00 ExyrJen Research, 3058 Research Drive, State College, PA 16801 Q00335 -- --------- --------------------- Quantify Sruqple Report \d Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\bs8l~\Fluoroch~cals.PRO\S~leDB\OSOlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCbIS~B\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Naalm : 0801031-3024 Text: Page 47 Decatur BC BC 080103 )80103A-2024 10 Sm (Mn, 2x3) 9.12 47341r 5 02-Aug-2003 t 0:47:04 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 2.88e6 Area i-- Time L 2.00 4.00 6.00 8.00 10.00 12100 U& 2: C6 Sulfonate L3491 o-1 1 (PFHS) 080103A-2024 100- Sm (Mn, 2x3) %- 02-Aug-2003 10:47:05 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 1.03e5 Area 0 "","","",`11',"","","",`l","' , , I 1 , , , , 1 Time 1 2.00 4.00 6.00 8.00 10.00 12.00 : C8 Sulfonate -3491 o-1 1 (PFOS) )80103A-2024 Sm (Mn, 2x3) 9.25 3-235467: 02-Aug-2003 10:47:04 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.27e7 Area O1,,,,,,,,,,,,,,,,~~,,~,~,~,,,,,~,,.,,,,,,,,,,,St,.,..,.,.,,,,Time 2.00 4.00 6.00 8800 10.00 12.00 Exygsn Research, 3058 Research Drive, State College, PA 16801 ,-1 -.--. -- -------_-_ --u---w- ---- Quantify Sample Report 14 Study No.:L34910, Set No.: 080103A, Ext.Date:06/01/03, Analyet:IC.Xisha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cala.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Name: 08010311-2024 Text : Page 46 Decatur BC BC 060103 L3491 o-1 1 080103A-2024 100- Sm (Mn, 2x3) %- 02-Aug-2003 10:47:05! LC/MS/MS #6 MRM of 4 Channels ES- 9.90 1215533 498 > 78 6.18e6 Area 0 ~,~~,l~/(,~rll,~ll.,~I'I,I.II,)I)/,IIIr,llll,lll Time 2.00 4.00 6.00 a.00 10.00 12.00 ExVgen Research, 3058 Research Drive, State collage, PA 16601 000337 Quantify Sample Report ,,, Study No. zL349l.0, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 49 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCblSMS6\Masslynx\Pluoroch~cals.PRO\S~l~DB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\~et~B\Decatur Sun Auu 03 07:11:59 2003 Decatur BC BC 080103 Printed: --e---w------ Sun Aug 03 07:32:25 -__----- 2003 ------- --w---_-----P Name: 0801031-2025 Text : 1,: CB Acid (PFOA) -3491 O-1 1 Rep 180103A-2025 1007 Sm(Mn,2x3) %- 9.12 463017 02-Aug-2003 11:08:44) LC/MS/MS #6 MRM of 4 Channels ES413>369 2.77e6 Area q& 2: C6 Sulfonate (PFHS) L3491 O-1 1 Rep 080103A-2025 I 10 01 Sm (Mn, 2x3) I 8.96 Time 12.00 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of 4 Channels ES399>80 1.09e5 Area 3: CB Sulfonate L3491 O-1 1 Rep (PFOS) 080103A-2025 Sm t.Mn.2~3) , 02-Aug-2003 11:08:4~ LC/MS/MS #t MRM of 4 Channels ES- 9.26 499 > 95 1 .OOei Are: , I I I I , I I 1Time 2.00 4.00 6.00 8.00 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 -------- ------v--m ----~----------- ---me-- Quantify Sample Report ,,ul Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 50 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCblSMS6\~ssl~\Fluoroch~cals.PRO\S~le~\OBOlO3A Sun Aug 03 07:25:44 2003 P:\Data\L~fl3S6\Masslynx\Fluorochemicat~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC EC 080103 Printed: Sun Aug 03 07:32:25 2003 ------- ----------------------~ w----w-- -----------P--_ Name: 0801031-2025 Text : 4: PFOSA (L3491 O-l 1 Rep 080103A-2025 lOc- Sm (Mn, 2x3) %- 02-Aug-2003 11:08:4d LC/MS/MS #6 MRM of 4 Channels ES- 9.87 929771-- 4982.78 4.73e6 Area 0 `~,~,~`~~,~~`~,.~~,,~,,,,,,,,,,,,,,,,,,,,,,,,,,,c....,.,,,, 2.00 4.00 6.00 a.00 1 oloo Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 "I. -l-.,. ". _,1.,,,1-111"----1 .-- --- ------ --------- ------ __----~----_ Quantify Sample Report Study No.: L34910, Set No .:080103A, Ea&.Date:08/01/03, Analyst:K.Risha SaIlple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\SamgleDB\O80103A Sun Aug 03 07:25:44 2003 P:\Data\LQ3SMS6\Masslynx\Fluorochsmicals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 51 Decatur BC BC 080103 Name: 0801031-2026 Text : 1: C8 Acid (PFOA) L3491 O-20 080103A-2026 lOO- Sm (Mn, 2x3) %- 9.12 4042097 02-Aug-2003 11:30:2d LC/MS/MS #6 MRM of 4 Channels ES413>369 2.37e6 Area 0 ,,,,,,~,,,,,,,,,,,,,,,,,,,,,,,,,,.,,,,,,,,,,~~,~,,,,,,,,,,rTjme 2.00 4.00 6.00 2: C6 Sulfonate L3491 O-20 (PFHS) 080103A-2026 loo- Sm (Mn, 2x3) %- 8.00 8.96 10.00 12.00 02-Aug-2003 11:30:26 IX/MS/MS #6 MRM of 4 Channels ES399 > 80 1.41 e5 Area 0 `.`I~~`~,~`/(/,~~./`~,,,~~~./"~`,",~, , , I , . I 1Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate L3491 O-20 (PFOS) 080103A-2026 10 Sm (Mn, 2x3) 9.25 418516 02-Aug-2003 11:30:26 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.35e6 I 2.00 4.00 6.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 10.00 12.00 000340 -- ---------w- ----m-P ----w--m- Quantify Sample Report Study No.:L34910, Set No .:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 52 Samgla List: Laot modified: Method: Last modified: Job Code: P:\Data\LCM~S6\bIasslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\~sslynx\Fluorochgmica\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 --------------------- ------ ----- ------ ----- Name: 06010311-2026 Text : : PFOSA .3491 O-20 )80103A-2026 Sm (Mn, 2x3) 02-Aug-2003 11:30:26 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 i341236: 4928.1A>Ore7ea86 Time Oxygen Research, 3050 Research Drive, State College, PA 16801 000341 -- -e---p ----- ------ e-v-- ------ Quantify Sample Report vd Study No.:L34910, Set No .:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 53 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQH~6\Maselynx\Fluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\L~SMS6\Massl~\Fluoroch~cals.PRO\~at~B\Dacatur Sun Aug 03 07:11:59 2003 Decatur Be BC 080103 Printed: ------- Sun Aug 03 07:32:25 2003 ---__------------------~ -_----^------------_--_-____ Name: 080103A-2027 Text : ,: C8 Acid (PFOA) -3491 O-20 Rep 380103A-2027 10 % 1 Sm (Mn, 2x3) L \clr) 2: C6 Sulfonate L3491 O-20 Rep 2.00 (PFHS) 080103A-2027 lOO- Sm (Mn, 2x3) %- 9.13 30120' 1. 02-Aug-2003 1152: 11 LCIMSIMS #6 MRM of 4 Channels ES- 413>13.7669e6 Area 8.00 8.97 10.00 Time 12.00 02-Aug-2003 11:52:11 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 9.68e4 Area 0 "","","","","","","","","","",""I"", Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate 113491 O-20 Rep (PFOS) 080103A-2027 1001 Sm (Mn, 2x3) %- 02-Aug-2003 11:52:11/ LCMNMS #6 MRM of 4 Channels ES499 > 99 1.68e6 Area 0 "","","","","","","",""I"" , I , , , I , 1 , I Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 QUO34~2 ---- ----------------L---I_-- --------- Quantify Sample Report \& Study No.:L34910, Set No.: 080103A, Ext.Date:08/01/03, Analyst:R.Risha Page 54 Sanrple List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\MasslyPx\Fluoroch~ca~s.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\L~SMS6\Massl~\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 -----111-----e- ------_-------------- --- Name: 080103A-2027 Text : : PFOSA -3491 O-20 Rep )80103A-2027 100- Sm (Mn, 2x3) %- 0%Aug-2003 71:52:111 LCYMWMS #6 MRM of 4 Channels ES- 9.08 346884 498> 78 1.78e6 Area 0 ,~,,,,,,,,,,,,,,~,,,,,,,,,,,,,,,,,,,,,,,,,,,,,1.~ Time 2.00 4.00 6.00 8.00 10.00 12.00 wgen Research, 3058 Research Drive, State College, PA 1680% WQ34-3 ---w----m- ------------ P-B-- ----- Quantify Sample Report \d Study No.:L34910, Set No.: 000103A, Ext.Date:08/01/03, A.nalyst:K.Rislha Page 55 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SblS6\Mas~~\Fluoroch~cala.PXO\S~l~DX\O8OlO3A Sun Aug 03 07:35:44 2003 P:\Data\L~SbIS6\Masslynx\FluorochemiB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ---__-- Sun Aug 03 07:32:25 --------------e-w- 2003 ------------------- Name: 080103A-2028 Text : .: C8 Acid -3491 o-21 (PFOA) 180103A-2028 10 Sm (Mn, 2x3) % 9.13 53261: 3 02-Aug-2003 12:13:52/ LCIMSNS #6 MRM of 4 Channels ES413>369 3.15e6 Area : !: C6 Sulfonate L3491 o-21 (PFHS) 080103A-2028 Sm (Mn, 2x3) L. 8.00 10.00 Time 12.00 8.98 36172` 02-Aug-2003 12:13:523 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.1 le5 Area 2.00 4.00 6.00 8.00 3: C8 Sulfonate L3491 O-21 (PFOS) 080103A-2028 Sm (Mn, 2x3) 9.25 40962 02-Aug-2003 12:13:5: LC/MS/MS #( MRM of 4 Channels ES- 499 > 9! 2.39et Are; , I I c I , I s t I 7 Time 10.00 12.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 -------------B-P- ---- --------_ Quantify Sample Report qrrr, Study No.:L34910, Set No.: 080103A, Ea&.Date:08/0l./03, Analyst:K.Risha Sample List: Last modified: Wethod: Last modified: Job Code: P:\Data\~SMS6\Mass~~\Fluoroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LQ3SMS6\Maeslynx\FluorochamicalsB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 56 Decatur BC BC 080103 Name: 080103A-2028. Text : 4: PFOSA L3491 o-21 080103A-2028 lOO- Sm (Mn, 2x3) %- 02-Aug-2003 12:13:52 LCYMWMS #6 MRM of 4 Channel8 ES- 9.87 498 > 78 1.82e6 Oxygen Research, 3058 Research Drive, State College, PA 16801 Quantify Saqle Report w Study No.:L34910, Set No.: 080103A, Eact.Date:08/01/03, Ana1yst:K.Rish.a Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massl~\Fluoroch~ca~s.PRO\S~leDB\~80103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\FluorochamicalsB\Decatur Sun Aug 03 07:1X:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 57 Decatur BC BC 080103 Name: 080103A-2029 Text : 1: c8 Acid (PFOA) l>(CO72503-5,500 rig/L Standard 080103A-2029 1 oo- Sm (Mn, 2x3) %- 9.13 _ 140009 02-Aug-2003 12:35:3! LC/MS/MS #( MRM of 4 Channels I%413 > 36! 8.49el Are: 0 ,,,~,`;;,~,,,,,,,,,,,~~,,i,,~,,~~~~,,,~~,~~~~~~,~i~~~~,,~,,,Time 2.00 4.00 6.00 \wlr' 2: C6 Sulfanate IXCO72503-5,500 (PFHS) rig/L Standard 080103A-2029 lOO- Sm (Mn, 2x3) %, 8.00 8.98 10.00 12.00 J 02-Aug-2003 12:35:34 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.72e5 Area : C8 Sulfonate :CO72503-5,500 (PFOS) rig/L Standard 80103A-2029 Sm (Mn, 2x3) 9.24 17108 02-Aug-2003 12:35:39 LC/MS/MS #6 MRM of 4 Channels ES499 z 99 1.02e5 Area VI&-- A-- 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Time 12.00 ] 000346 -w-p--- ----------------------------------~--__I_--- Quantify Sample Report ,& Study No. : L34910, Set No.:080103A, Eact.Date:08/01/03, Analyst:K.Risha Page 58 Salnple List: Lallt modified: Method: Last modified: Job Code: P:\Data\LCWSMS6\~sslyPx\Fluorochamicals.PRO\S~leDB\O80103A Sun Aug 03 07:25:44 2003 P:\Data\L~SMS6\Masslylur\FluorachamicB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: m-v--- Sun Auq ------- Name: 080103A-2029 Text : 03 07:32:25 2003 --_---------------- -- --e--M-_ i: PFOSA (CO72503-5,500 rig/L Standard 38010319-2029 10 "i i % i Sm (Mn, 2x3) o"~~`,~`~~,~,~~,~`~`,~~",~~~`,`~~'r'~'~,'~'~,~~r 2.00 4.00 6.00 02-Aug-2003 12:35:39( LC/MS/MS #6 MRM of 4 Channels ES- 9.88 6723' I 498 > 78 3.54e5 Area L Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ---m-v- --------- ------- ---- --- Quantify Sample Report ,w Study No.:L34910, Set No.: oa0103A, Ext.Dats:08/01/03, Analyst:K.Risha Page 59 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~ca~s.PRO\s~leDB\OaOlO3A Sun Aug 03 07:25:44 2003 P:\Data\LQ3SMS6\Masslynx\FluarochemicalaB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: ------__-I_-_ Sun Aug 03 07:32:25 ------- 2003 ---------__-------- -----l-----_l__ Name: 080103A-2030 Text : 1: CB Acid (PFOA) XCO72503-6,1000 rig/L Standard I080103A-2030 10 Sm (Mn, 2x3) 9.12 273386 02-Aug-2-003 12:57:2d LCMWMS #6 MRM of 4 Channels ES- 413>369 1.66e6 Area llu7 2: C6 Sulfonate XCO72503-6,lOOO (PFHS) rig/L Standard 080103A-2030 lOO- Sm (Mn, 2x3) %- L Time 12.00 8.98 _ 54198 02-Aug-2003 12:57:26 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 3.29e5 Area : C8 Sulfonate (CO72503-6,1000 (PFOS) rig/L Standard 380103A-2030 10 Sm (Mn, 2x3) % y/ 2.00 4.00 6.00 02-Aug-2003 12:57:26 LCIMSIMS #6 MRM of 4 Channels ES499 > 99 1.91e5 Area Exygen Research, 3058 Research Drive, State College, PA 16801 ..*- .-. ._-.-._--.""",,I-,__..,~ _--- .".__ Quantify Saalple Report ,J Study Na.:L34910, Set No.: 080103A, Ext.Date:08/01/03, ?umlyst:K.Risha Page 60 Sample List: Last modified: Method: Last modified: Job Code: ~:\Data\L~SMS6\Mssslynx\Fluaroch~cals.PRO\S~leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\L~SMS6\MasoLynx\Fluorochsmicalp.PRO\Met~B\Decatur Sun Aug 03 07:11:59 3003 Decatur EC BC 080103 Printed: ---------- Sun Aug 03 07:32:25 ---__------ NBlM: 080103A-2030 Text: 2003 ------------~-----------------_---- 4: PFOSA IXCO72503-6,lOOO rig/L Standard 080103A-2030 100- Sm (Mn, 2x3) %- 02-Aug-2003 12:57:26j LX/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 6.85e5 Area 0 "","","","","","",",`,"","`,,".`,",,,"", Time L 2.00 4.00 6.00 8.00 10.00 12.00 Eqgen Research, 3058 Research Drive, State College, PA 16801 -.-_--I.-. _ ooow9 spwsoc study No: Exypcn Study No: .bdytC: lms MoniIMcd: She: NA L34910 PFOA 413 -r369 Dccvur B&u's Creek RAW DATA REPORT Lid of QuaIuition: l+ction Volume: Ma& Sample weigh Fii v01urnc: 50 PPI IS& soil 5.Og 5.0 mL S.StNo: A&SC Lnrbummt Exuacdon Adyzsd Type: Date: w: 080103AR Karen Rirha LCMSMS #6 08mlrn3 081'34M3 l%YpCU m xCJ372503-a xc.o72503-1 spoolor m Run NO. cs 080103AR-301 cs 080103AR-302 Std. *a Am0uol bYW TOW COIIC. Dilution Puk Pwnd Added Rccmciy Found SOtid. (pp1) Factor hma (PEN) (PPO 6) (ppb) (%) 0 672 25 13717 XUY72503.2 xCO7u03.3 cs 080103AR-303 50 29040 cs 080103AR-304 1W 51582 xco72503-4 XCU72.503.5 cs 080103AR-305 2.50 cs 080103AR.3% so0 113798 242355 XCO72503.6 L34910.I 1 Spk E L34910.I 1 Spk E L34910-20 Spk P BCZSED-06 EC-2 SED-06 Outfall to River SED-Ls cs 080103AR-307 LP 080103AR-308 LF 080103AR.309 LP 080103AR-310 469994 369 1 l . 5ooo 29373 L. 5ooo 28261 .* moo L34910.5 BC2 SED-04 S 080103AR.311 18223 l * 69.96 L34910-5 Rep EC2 SED-04 s 080103AR.312 14512 .* 69.% u4910.10 BC2 SED-05 s 080103AR.313 32594 l * 69.54 U491QIO Rep BC2 SED-05 S 080103ASb314 31062 .* 6954 xCO72503-1 cs 080103Alb315 12807 bv XCO72.503-2 cs 080103AR.316 25414 L34910-I I BC2 SED-06 s 080103AR.317 9410 *. 60.41 L34910-11 Rep BC2 SED-06 S 080103AR.318 9587 . . 60.41 L34910-1 I EC2 SD-06 S 080103AR.319 80473 1780 14.24 60.41 u4910-11 Rep w4910-20 L34910.20 Rep BC2 SED-06 OulfaB lo River SED-2.5 Odd1 to River SED-25 s 080103AR.320 s 080103AR-321 S 080103AR.322 76840 1700 7081 .* 5379 .* 13.M) 60.41 63.27 63.27 x(x72503-3 cs 080103AR-323 41160 xCu72503-4 cs 080103AR-324 96206 W491C-20 Outfall IO Rivu S@D-2.i S 080103AR-325 61092 134a IO.72 63.27 W49lDzo RqJ W491021 L34910-21 Outfall co Rivn SED-25 Outfill to Rhr SEWI5 Dup outfall IO River SED-25 Dup S 080103AR.326 s 080103AR-327 S 080103AIG328 44037 949 10169 l 99240 2210 739 63.27 67.43 17.68 67.43 xm72503-5 cs 080103AIG329 215048 xa7uo3-6 cs 080103AR-330 4c6254 Standvd IIWCC~~ Slop Cd. Of Da. : Linw (l/x P 2443.00 - 438.457 = 0.990236 weighti) hnplylc Fcucd @pb) 1 halyW found (pp0 x volume extracted (0.04 L)] I sample weight (5 g) hdyte Fwad (ppb) dry weight = maly(c found (ppb) I (lGU% I total solids (R)) CS - Calibration nandndud c - cmlml s = sample wmple LF = Lab fortified PF = Fwld fort&d LCS * Laborntay sample sample Gxuol Splkc CK = Check Stiard ND I NIX detected NQ = Nor quantifiable * Rerpmsc betwan 0 and 2.5 pp' * Raponse bctwcc2.n5 ppl UMI LCQ (50 pal) A=JYE Found @pb) Dry WciglM 23.6 225 16.9 w 12.0 26.2 **Sample was analyzed with scvaai dilution facmn in onier to accommcda~c all compounds. The appmprialc rwulu we rcponcd. 000350 SpmwxStudyNo: Exy@a Study No: Al&B: l0n.l Monitored: Site: NA L34910 PFOS 499.>PP Dccahu Bakefs CIcck RAW DATA REPORT ' Limit of Quautition: Injjstioo Volume: MlUk Sample Wcighc Fmxl Votumc: so PPl IS& Soil -5.0 g 5.0 mL kt No: AdYSC hbuaKn1 extlacdon Adyzcd Type: Dam: w: 080103hR lcareo Rilha LCMSMS 16 08sJlrn3 08&4/03 EXYpeD D xCO72503-0 xCO72503-I xc07u03.2 xco72503-3 xCu72503-4 xco72503-s XCO72503-6 U4910-11 SpkE (34910.1lSpkE I34910-20 Spk F u4910.5 u4910-5 Rep L34910-10 U4910.10 Rep XC072503- I XCO72.503-2 w4910-II WPIO-11 Rep w4910-II L34910-II Rep L349lc-20 L34910-20 Rep X0372503-3 xCO72503-4 W910.20 w4910-20 Rep U491@21 L349Lc-21 xCO72503-s Xu)72503-6 Spoo= ID BC2 SED-06 BC2 SEDW `&fall LO River SED-25 BC2 SED-04 acz sm.04 ac2 sm.OS EC2 SED-05 BCZSED-06 aa SED-06 BCZ SED-06 BC2 SED-06 Outfall to River SED-2S ouu-dl to River sell-25 Sample c.z& cs cs cs cs cs cs cs LF LF LF s s S S cs cs S S s s S s c.s cs S S s s l-3 cs RU NO. 080103AR-301 080103AR-302 080103AR-303 080103AR.304 080103AR.305 080103AR-306 080103AR-307 080103AR.308 080103AR.309 080103AR-310 080103AR~311 080103AR.312 080103AR-313 080103AR-314 080103AR.315 080103AR.316 080103AR-317 080103AR-318 080103AR.319 080103AR-320 OS0103AR.37.L 080103AR-322 080103AR.323 080103AR.324 080103AIb325 080103Ah326 080103AR.327 080103AR-328 080103AR.329 080103AR-330 Std. Adp AUUUUI Adylc Twd cont. Dilution Rak FOUOd Added Rccovuy Found Soli& (ppt) Fxtw Area CPPO @PO (W (pph) (70) 0 0 2s 1442 50 3003 Nil 5613 250 11976 SW 2.5896 AadyrC &Jnd (Ppb) Dry Weight loo0 51730 low 5387 100 51842 so00 ** SW0 ml 9506 19lM 5ooo II4 10 9121 1830 14.64 69.96 20.9 10 7449 1490 11.92 69.96 17.0 10 14012 2850 22.80 69.54 32.8 10 15401 31M 2s.w 69.54 36.0 7.5 1301 50 2860 100 66379 100 48118 M 10 526238 l * 10 390663 l . 60.4 I 60.41 60.41 60.41 104 6714 13400 107.20 63.27 I69 loo 4609 9010 loo 4445 72.08 63.27 114 2.w 11649 10 63108 . . IO 45122 .* 63.27 r 63.27 100 8701 17500 10 Bow3 . . 140.00 67.43 208 67.43 500 24473 IcaJ 44784 Analy~ Recavuy Found (pp') = (pwk arw . intercept) I slope x DF (57) i Iadyte found (ppthnalytc fowd in CWiTOl (ppl)] amount added (ppt) x 100 S&i&&&w Intcrccp~ Slope Cosf. Of Del. : Limu (I/x I 254.789 = 48.3413 - 0.991571 weighted) AsrlyrC tiytc Found (ppb) = [analytc found (ppt) x volume extracted (0.04 L)] I sample weight (5 p) Found (ppb) dry weight I analyo found @pb) x (100% /total sc4idr (+)) CS = CJibradacl standard c 3 cantrcI1 ramplc s -.samplc LF = Lab fwtificd Pp = Field fonihcd LCS = Laboratory runplc ramp10 Control Spike CK = Uicck St+ndud ND I Notdstatrd = Rcrpcw ktwsen 0 aad 25 ppt NQ I Nor quantifiable - Response between 25 pp, lad LOQ (SO pp') Sponsor Shldy No: Exygcn Study No: Adytc: loos Monitored: Site: NA L34910 FOSA ea.>78 Decatur Bakda Creek RAWDATAREPORT Limit ofQwtitatioo: lnjtdioo Volume: Mst-ix: Sample Weight: Final volume: 50 PPt 15 pL Soil s.0 g S.OlllL Set No: Analyst: lnsbummt Type: Extrsction Date: Atlslymlo11: 080103AR Karen Riha LCMSMS #6 08/01/03 08/04/03 Exym SpOOSW Sample Run m m CC& No. xco72503-0 cs 080103.4R.301 xco72503-I cs 080103AR-302 XCO72SO3-2 cs 080103AR-303 XCO72503-3 cs 08OlO3AR-304 XC0725034 cs 080103.4R-305 XCO72503-5 CS 080103AR-306 XC0725036 cs 080103AR-307 W4910-11 Spk E BC2 SED-06 LF 080103AR-308 L34910-11 SpkE BC2 SED-06 LF 080103AR-309 L34910-20 Spk F Outfall to River SED-25 LF 080103AR-310 w4910.5 BC2 SED-04 S 080103AR-31 I L34910-5 Rep EC2 SED-04 S 080103AR-312 w4910-10 EC2 &ED-OS S 080103AR-313 L34910.lORep BC2 SED-05 S 080103AR-314 XCO72503-I cs 080103AR-315 XCO72503.2 CS OBOlO3AR-316 Qid Ll4910-II L349lO-I I Rep 0C2 SEDM BC2 SED-06 S 080103AR-317 S 080103M-318 L34910-II SC2 SED-C.5 s 080103AR-319 L34910-II Rep BC2 SED-W S 080103AR.320 L34910-20 Outid ta River SED25 S 080103AR-321 L349lQZO Rep Outfall (0 River SED-25 S 080103AR-322 XCO72503-3 cs 08OlO3AR-323 XC0725034 CS 080103AR-324 L34910-20 Outfall to River SED-25 S 080103AR-325 L34910-20 Rep Outfall to River SED-25 S 080103AR.326 w4910.21 Outfall to River SED-25 Dup S 080103AR-327 L349IO-21 Outtkll 10 Rivn SED-25 Dup S 080103AR.328 xca72503-5 cs OgOlO3AR-329 XCO72503-6 cs 080103AR-330 Analytc Found (ppt) - (peak area _ inracept) I slope x DF Recovery (%) - ,lardyte found @pl)-analytc found io contml (ppt)l x IO0 ~moont added @PI) Std. COUC. (PPO 0 25 50 100 250 500 1000 25 50 IO0 250 500 I000 Analyte Analyte Found (ppb) = [malytc found (ppt) x volume extracted (0.04 L)] I sample weigbt (5 6) Found (ppb) dry wcigbt = lnnlyte found (ppb) x (lCO?`a I total soli& (%)) CS = Calibrntion sundud c = cootroi sample s - Sample LF - Lab fortified sample FF - Field fortified sample LCS - Laboratory Control spike Aoalylc AnKJlmr Adyfe TOM DilUtiOll Peak Found Added RCCOVCIY Found Solids Factor Area (ppt) (ppt) x (ppb) (0% 0 5040 I0269 19684 45565 93155 179184 2308 5000 21870 5000 13524 .* 5000 16680 .I 69.96 I8189 .* 69.96 19503 l . 69.54 26862 I510 12.08 69.54 4380 a99 I 21988 60.41 16805 60.41 200293 l * 60.41 IS0384 . . 60.41 6516 .* 63.27 5371 ** 63.27 17628 40103 61447 3m 28.00 63.27 51717 2940 9119 .* 23.52 63.27 67.43 78207 4460 86063 167421 35.68 61.43 Standard w lntucepr Slops Chef. Of Dct. : Lincu (l/x = 610.451 = 174.067 - 0.996985 weighted) CK = Check Staodard ND = Not dcrectcd - Rsrpoow behvca 0 md 25 ppt NQ - Not quantifiable = Respmsc bctwcco 25 ppt and LOQ (50 ppt) Analyie F-xnd W-4 Dry Weight 17.4 44.3 37.2 52.9 **Sample -Sample was analmd with several diltttioo factors requircr reextmuion. Ssc data set 0806038. in order to accommodotc all compounds. The appropriate results arc rcportcd. 000352 Masslynx - Sample List Sampie List: Printed: Mon Aug 04 07:47:05 2003 --- &ygen STUDY NOa a -. Page 1 Page Position: (I, 1) Vial File Name LIMS ID Client ID Sample Description Matrix Sample Type Cone (rig/L) Cone B Cone C Test ID DF 2 1 41 080103AR-301 --- --- XCO72503-0. 0 rig/L Standard --- Standard " 0 2 42 080103AR-302 - -- XCO72503- 1. 25 m-r/L Standard -- Standard 3 43 080103AR-303 -- - XCO72503-2; 50 n$L Standard _-- Standard z 4 44 0801 03AR-304 -- -- XCO72503-3. 100 nglL Standard -- Standard 100 45 080103AR-305 - - XCO72503-4,250 ngiL Standard -- Standard 250 6" 46 080103AR-306 - - XCO72503-5.500 nglL Standard -- Standard 500 7 080103AR-307 - - XCO72503-6, 1000 ngR Standard -- Standard loo0 8 080103AR-308 -- - L34910-11 Spk E, 5ooO nglL, OF=1000 -- CC 5ooct 0801 03AR-309 - - L34910-11 Spk E, 5000 rig/L, OF=100 -- QC 5000 l"o 080103AR-310 -- -- L34910-20 Spk F, 5000 n&L, DF=lOO - QC 5000 11 080103AR-311 - - L34910-5, DF=lO - Analyte -- 12 080103AR-312 - - L34910-5 Rep, DF=lO - Analyte -- 080103AR-313 - -- L34910-lO.DF=lO - Analyte -_ :: 080163AR-314 -- - L34910-10 Rep, DF=lO - Analyte -_ 15 42 080103AR-315 - -- XCO72503-1,25 rig/L Standard - Standard 25 18 43 080103AR-316 - -- XCO72503-2, 50 @IL Standard - Standard 50 17 080103AR-317 - -- L34910-ll.DF=l60 - Analyte -- 18 080103AR-318 - - L34910-ll.Rep, DF=lOO - Analyie -- 080103AR-319 -- - L34910-11, DF=lO - Analyte m-w 2 080103AR-320 - - L34910-11 Reo. DF=lO - Analyte --- 12 080103AR-321 -- - L34910-20, Di~lOO -- Analyte -- z 13 080103AR-322 -- - L34910-29 Rep, DF=lOO _-- Analyte --- 080103AR-323 - - XCO72503-3. 100 rig/L Standard -- Standard 100 ;i 080103AR-324 - - XCO72503-4. 256 rig/L Standard -- Standard 250 25 14 080103AR-325 - - L34910-20. DF=lO --_ Analyte -I 26 15 0801 OJAR-326 - - L34910-20 Rep, OF=10 _- Analyte -- 27 16 080103AR-327 - -- L34910-21. DF=lOO -- Analyte -- 28 17 080103AR-328 - - L34910-21; DF=lO- ___ Analyte 29 080103AR-329 - -- XCO72503-5. 500 rig/L Standard -- Standard 500 30 "4; 080103AR-330 - - XCO72503-6. 1000 rig/L Standard - Standard 1000 --- 0 1 ___ -- 0 1 -- _- 0 1 _- - 0 1 -- --_ 0 1 -_ --_ 0 ___ -_- 0 : - --- 0 1000 -- --- 0 100 -.v --- 0 100 - --- 0 10 - --- -- _- x :: -- ___ 0 10 -- ___ 1 -- -- 8 1 -- ___ 0 100 - --- 0 100 - -- 0 IO - --- 0 10 -- 0 100 -- - 0 100 - - 0 1 - - 0 1 0 10 - - 0 10 - 0 -- - 0 :F? -- ..- 0 - 0 : Masslynx - Sample List Sample List: C:V\nASSLYNX\Fluorochemicals.PRO\SampleDt3~g66103AR 03 Printed: Man Aug 64 07:47:05 2003 --- Decatur BCSPL - MS Method 1 C6 C6 SULF C8 ACID PFOSA 2 C6 C8 SULF C8 ACID PFOSA 3 C6 C8 SULF C8 ACID PFOSA 4 C6 C8 SULF C8 ACID PFOSA 5 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA 7" C6 C6 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA 4" C6 CB SULF C8 ACID PFOSA IO C6 C8 SULF C9 ACID PFOSA 11 C6 C8 SULF C8 ACID PFOSA 12 C6 CB SULF C6 ACID PFOSA C6 C8 SULF C8 ACID PFOSA :: C6 C6 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA :i C6 C8 SULF C8 ACID PFOSA 17 C6 C6 SULF C8 ACID PFOSA 18 C6 C6 SULF C8 ACID PFOSA 19 C6 C8 SULF C8 ACID PFOSA 20 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA 2 C6 C8 SULF C8 ACID PFOSA 23 C6 C8 SULF C8 ACID PFOSA 24 C6 C8 SULF C8 ACID PFOSA 25 C6 C8 SULF C8 ACID PFOSA 26 C6 C8 SULF C8 ACID PFOSA 27 C6 CB SULF C8 ACID PFOSA 28 C6 C8 SULF C8 ACID PFOSA 29 C6 C8 SULF C8 ACID PFOSA 30 C6 C8 SULF C8 ACID PFOSA HPLC Method pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water MS Tune File Fluorochems Fluorochems Fluarochems Fluorochems Ftuorochems Fluorochems Fluorochems Fluorochems Fluorochems Ftuarochems Flucrochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Ffuorochems Fluomchems Fluorochems Inj.Volume 15 15 15 15 15 15 15 i: 15 iz 15 15 15 15 15 15 15 15 15 :55 15 :: 15 :"5 15 &ygen STUDY NC?. c3qqJ0 Page 2 Page Position: (2. 1) LC!/MS/MS SYSTEM AND OPERATING CONDITIONS Soonsor Protocol No: NA Exvgen Studv No: L349 IO Instrument: Micromass Quattro Ultima (IX/MS/MS Unit #6) Computer: Software: COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 138 1: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Mobile Phase (A) : Mobile Phase (B) : Genesis C-8,5 cm x 2.1 mm i.d. x 4 p (Oxygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (8 14) 272-1039 FAX: (8 14) 23 L-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by. * lip0!6/*3 "-_....- --._---.....--- 080355 Scanning Method Report fd Method: Last Modified: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 Thu Ju$ 31 16:23:50 2003 Printed: Mon Aug 04 07:47:13 2003 Page 1 C8 SULF C8 ACID PFOSA Solvent Delay ( mins ) : 0.00 ATlalog Function Channel : 1 4 : Unused MFN of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Sets ) : 0.03 Span ( Daltons ) : 0.00 Start Time ( Mins ) : 0.00 End Time ( Mins ) : 12.00 Repeats : 1 Channel Parent Daughter Dwell (Sets) Co11 Energy (eV) Cone ( V ) 1 399.00 80.00 0.20 35 50 2 413.00 369.00 0.20 10 10 3 498.00 78.00 0.20 30 50 4 499.00 99.00 0.20 40 33 Method Report Method File: Last Modified: C:\MASSLYNX\FLUOROCHEHICALS.PRO\ACQUDB\pfbs Monday, August 04, 2003 07x38:50 ,J Printed: Monday, August 04, 2003 07:47:18 u HP1100 LC Pump Initial Conditions Solvents A% 90.0 B% 10.0 C% 0.0 D% 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Oven Temperature Left(OC) Right (OC) 0.300 20.0 0 400 35.0 35.0 HP1100 LC Pump Qradient Timetable The gradient Timetable contains 8 entries which are : Time A% B% C% D% Flow 0.00 90.0 10.0 0.0 0.0 0.300 2.00 90.0 10.0 0.0 0.0 0.300 5.00 10.0 90.0 0.0 0.0 0.300 9.00 10.0 90.0 0.0 0.0 0.300 9.50 0.0 100.0 0.0 0.0 0.300 14.00 0.0 100.0 0.0 0.0 0.300 14.50 90.0 10.0 0.0 0.0 0.300 20.00 90.0 10.0 0.0 0.0 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contact1 Off On Off Off Off Off are : Contact2 Off Off Off On Off Off 'Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(pl) Vial Number Conditions 200.0 200 0.50 20.00 15.0 27 water Page 1 Pressure 400 400 400 400 400 400 400 400 000357 Tuning Method: Printed: Method Report C:\MASSLYNX\FLUOROCHEMICAtS.PRO\ACQUDB\FLUOROCHF,MS Mon Aug 04 07:47:28 2003 Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set Rdbk 3.00 -2.93 20 -16 0.0 0.0 0.0 100 100 300 299 Rdbk OFF 3.6e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 11 15 21 2 14 14.0 14.0 2.0 650 -647 Rdbk 134.7 765.9 000358 --- ------ Quantify Calibration Report Study No.: L34910, Set No.: 080103AR, ---- Ext.Date:08/01/03, aalyst:K.Risha Calibration: Last modified: Printed: -------w----v P:\Data\L~SMS6\Masslynx\Fluoroch~ca~8.P~O\~~eDB\O8OlO3~ Tue Aug 05 07:30:00 2003 'l'ue Aug 05 07:31:58 2003 --m-e----- >ompound 1 name: C8 Acid (PFOA) Coefficient of Determination: 0.990236 Calibration curve: 438.457 * x + 2443.00 qesponse type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 4.70e5 l/x, Axis trans: None ---_-----_ Page 1 Decatur BC X Response ~~,~~,,.~,,~~~.,~.~ 0.0 200.0 q, " ' ' , " , " ' ' , " " 1 " "1"' 400.0 600.0 800.0 8 IngIL 1000.0 WgOn Research, 3058 Research Drive, State College, PA 16801 000359 ---- -------__l---___I ------------- Quantify Calibration Report `U Study No .:L34910, Set No.:O80103AR, Ext.Date:08/01/03, Calibration: Last modified: Printed: ----- -------~_ P:\Data\L~SMS6\Masal~\Fluorochexrcic Tue Aug 05 07:30:00 2003 Tue Aug 05 07:31:58 2003 ----------- Axzalyst:K.Risha Compound 2 name: C6 Sulfonate (PFHS) :oefficient of Determination: 0.990051 :alibration curve: 77.0647 l x + 374.700 Response type: External Std, Area >urve type: Linear, Origin: Exclude, Weighting: 8.1584. 1 l/x, Axis trans: None -----------__ Page 2 Decatur BC -------___ X Response 0.0 Exygen Research, 200.0 400.0 600.0 3058 Research Drive, State College, PA 16801 800.0 rig/L 1000.0 --- ------- ------- --------------- Quantify Calibration Report w Study No.:L34910, Set No.. ~080103AR, Ea&.Date:08/01/03, Analyst:K.Rioha Calibratioq: Last modified: Printed: P:\Data\LQISMS6\Masslynx\Fluoroch~cals.PRO\~~eDB\O8OlO3~ Tue Aug 05 07:30:00 2003 'he Aug 05 07:31:58 2003 >ompound 3 name: C8 Sulfonate (PFOS) ;oefficient of Determination: 0.991571 >alibration curve: 48.3413 l x + 254.789 Response type: External Std, Area >urve type: Linear, Origin: Exclude, Weighting: 5.1704 l/x, Axis trans: None ------_- Page 3 Decatur BC Response O~,,,,,,,,,,,,,,,,,,,,~,~~r~~,~,~~~~,~~,~,~~'~,~~,~ln/L 0.0 200.0 400.0 600.0 Wgen Research, 3058 Research Drive, State College, PA 16801 800.0 1000. ? 0003Gl. Quantify Calibration Report p4 Study No.:L34910, Set No. :080103AR, Ext.Date:08/01/03, Analyst:K.Risha Calibration: Last modified: Printed: ------------------------ P:\Data\LChiSMS6\bsslynx\Fluoroch~cala.PRO\~~eDB\O8OlO3~ 'l'ue Aug 05 07:30:00 2003 'Pus Aug 05 07:31:58 2003 -------m---------- >ompound 4 name: PFOSA ;oefficient of Determination: 0.996985 ;alibration curve: 174.067 * x + 610.451 qesponse type: External Std, Area >urve type: Linear, Origin: Exclude, Weighting: 1.79eE l/x, Axis trans: None Page 4 Decatur BC Response 200.0 400.0 600.0 -en Research, 3058 Research Drive, State College, PA 16801 800.0 1000.0 ---_ PI--- ---m--m ----_ ------ Quantify Sample Report Study No.:L34910, Set No.: 080103AR, Ea&.Date:08/01/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LBISMS6\Wasslynx\Fluorochemicals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCbISMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 da Printed: Tue Aug 05 07:32:01 2003 Name : 080103AR-301 Text : 1: C8 Acid (PFOA) XCO72503-0,O rig/L Standard 080103AR-301 Sm (Mn, 2x3) r2: c6 Sulfonate XCO72503-0,O I I I II I I I~~#, I-I,I, 2.00 4.00 (PFHS) rig/L Standard 080103AFb301 Sm (Mn, 2x3) aII ,, 6.00 , , , , , , , ,c., 8.00 04-Aug-2003 08:35:x LC/MS/MS #6 MRM of 4 Channels ES413>369 4.35e4 Area 9.13 672 ,:,-Time 10.00 04-Aug-2003 08:35:5C LCIMSIMS #6 MRM of 4 Channels ES399 > 80 834 2.00 4.00 6.00 8.00 10.00 3: C8 Sulfonate (PFOS) XCO72503-0,O rig/L Standard 04-Aug-2003 08:35:5C LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.96e3 Oxygen Research, 3058 Research Drive, State College, PA 16801 QQQ3G3 Quantify Sample Report -lrl Study No.: L34910, Set No .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sanlple List: Last modified: Method: Last modified: Job Coda: P:\Data\L~SMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tue Aug OS 07:24:43 2003 P:\Data\L~SMS6\bsslynx\FluorochemicB\Decatur Sun Aug 03 07:11:59 2003 Page 2 Decatur BC BC 080103 Printed: l'ue Aug 05 07:32:01 2003 ------------------_____________________--~ Name: 080103AR-301 Text : ----___---___ 4: PFOSA XCO72503-0,O rig/L Standard 080103AFb301 Sm (Mn, 2x3) OC-Aug-2003 08:35:5C \I LC/MS/MS #6 MRM of 4 Channels ES- Exygen Research, 3058 Research Drive, State College, PA 16801 0003G4 ------ ----em-------------- ----------m-__ Quantify Sample Report Study No.: L34910, Set No.: 080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 3 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24x43 2003 P:\Data\LcMSMS6\Masslyax\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 -----------------__-----~----- ------__-- __------- Name : 080103AR-302 Text: : C8 Acid (PFOA) 3CO72503-1,25 rig/L Standard 380103AR-302 Sm (MI-I. 2x31 04-Aug-2003 08:57:29 LC/MS/MS #6 MRM of 4 Channels ES413> 369 8.44e4 Area !: C6 Sulfonate KC072503-1,25 (PFHS) rig/L Standard 080103AR-302 10 Sm (Mn, 2x3) Time 04"Aug-2003 08:57:29/ LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 2217 1.42e4 Area 2.00 4.00 6.00 3: C8 Sulfonate XCO72503-1,25 (PFOS) rig/L Standard 080103AR-302 10 Sm (.Mn. . 2x3) , %7 - O~,,,,,,,,,,~,,,,,,,,,,,,,,, 2.00 4.00 6.00 8.00 9.24 1442 10.00 I 04-Aug-2003 08:57:2$ LC/MS/MS #6 MRM of 4 Channels ES499 > 9s 9.02e? Area 8.00 10.00 Rxygen Research, 3058 Research Drive, State College, PA 16801 --- -- ___-... 000X5 Quantify Sanrple Report Study No.: L34910, Set No.:O80103AR, Ext.Dats:06/01/03, Analyst:K.Risha Szunple List: Last modified: Method: Last modified: Job Code: P:\Data\L~SblS6\Mssl~\Fluoroch~cals.PRO\S~leDB\O6OlO3~ !Cue Aug 05 07:24:43 2003 P:\Data\L~SP3S6\MsslyPx\FluaEochemic\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 4 Decatur BC BC 080103 Name: 080103AR-302 Text: 4: PFOSA XCO72503-1,25 rig/L Standard 080103AR-302 loo- Sm (Mn, 2x3) %- 04-Aug-2003 08:57:2d LCIMSIMS #6 MRM of 4 Channels ES- 9.92 5040-- 498 > 78 2.63e4 Area Exygen Research, 3058 Research Drive, State College, PA 16601 ---_------ w-e---- --------------I_--- - Quantify Sampla Report "4 Study No.: L34910, Set No.:O80103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyax\Pluorochemicals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:14:43 2003 P:\Data\L(3MSMS6\~ssl~\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:ll:SS 2003 Page 5 Decatur BC BC 080103 Printed: ----------__--------~~ Tue hug OS 07:32:01 2003 -a---------------e------s---- Name: 080103AR-303 Text : ----------_-_ 1: C8 Acid (PFOA) XCO72503-2,50 rig/L Standard 080103AR303 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 09:19:12 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413>369 1.67e5 Area 2.00 4.00 `4 2: C6 Sulfonate (PFHS) XCO72503-2,50 rig/L Standard 080103AFk303 Sm (Mn, 2x3) , , , , , , , , , , , , a , , , , , ,-Time 8.00 10.00 04-Aug-2003 09:i 9:12 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.81 e4 Area 3: C8 Sulfonate XCO72503-2,50 2.00 4.00 (PFOS) rig/L Standard 080103AR-303 100- Sm (Mn, 2x3) %- 8.00 9.27 Time 10.00 04-Aug-2003 09: 19: 12 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.63e4 Area 8 + , I I I I , r r t I Time 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 --- ~---___- ---_---I---------- ---------- Quantify Sample Report ,& Study No.:L34910, Set No.: 080103AR, Ekt.Date:08/01/03, Analyst:K.Risha Sanrple List: Last modified: Method: Last modified: Job Code: P:\Data\~:SMS6\Masslynx\Fluorocb~cals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07~24~43 2003 P:\Data\LCMSMS6\Maselynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 ---__ ----_ Page 6 Decatur BC BC 000103 Name : 080103AR-303 Text : 4: PFOSA XCO72503-2,50 rig/L Standard 080103AFb303 loo- Sm (Mn, 2x3) %- 04-Aug-2003 09:19:12 LCIMSNS #6 MRM of 4 Channels ES- 9.90 498 > 78 5.34e4 Area II ,I 10.00 I Time EWgen Research, 3058 Research Drive, State College, PA 16801 ---- -m--o- ---4----- -------I_------------- Quantify Sample Report \& Study No.:L349XO, Set No .:080103AR, Ext.Date:08/01/03, Analyst:IZ.Risha Page 7 Sam$Jle List: Last modified: Wethod: Last modified: Job Code: P:\Data\LCMSMS6\Massl~\~luoroc~~cala.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: -------------v-m- 'has Au% 05 07:32:01 Name: 080103JiR-304 Text : 2003 --___------ --------e-v-- : C8 Acid (PFOA) <CO72503-3, 100 rig/L Standard 380103AR-304 10 Sm (Mn, 2x3) 04-Aug-2003 09:41 :o LC/MS/MS # MRM of 4 Channels ES- 9.13 413>369 5158; 3.00e5 Area : v Time 2.00 4.00 6.00 8.00 10.00 2: C6 Sulfonate XCO72503-3,100 (PFHS) rig/L Standard 080103AFb304 10 Sm (Mn, 2x3) 04-Aug-2003 owl :od LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 8536 5.07e4 Area 2.00 4.00 6.00 8.00 10.00 3 : C8 Sulfonate 1 tCO72503-3,100 (PFOS) rig/L Standard (380103AR-304 10 01 % 1 Sm (Mn, 2x3) 04-Aug-2003 09:41:00 LCNWMS #6 MRM of 4 Channels ES- 9.2: 499 > 99 561: 3.18e4 Area -- 1 Time w 2.00 4.00 6.0~ 8.00 10.00 I WZTen R-earth, 3058 Research Drive, State College, PA 16801 000x9 Qwlntify Sample Report ud Study No.:L34910, Set No.: 080103X& Ext.Date:08/01/03, Analyst:K.Risha Page 8 Salnple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\~sslynx\Fluorochemical\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: -----_--_ Tue Aug 05 07:32:01 2003 __-_--__----___----------------~---------------------- Name : 080103AR-304 Text: ,: PFOSA KO72503-3,100 rig/L Standard 180103AR-304 10 Sm (Mn, 2x3) % 04-Aug-2003 09:41 :OC LC/MS/MS #6 MRM of 4 Channels ES- 9.92 19684 L 498 > 78 1.03e5 Area / , O",`,,,~,,,`,,,,~,ll,,`,,,.,,,,".,,,.,,,,',~,~,, 1. Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000370 Quantify Sample Report r Study No. :L34910, Set No.: 080103AR, Ext.Dats:08/01/03, I Analyst:K.Risha Page 9 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~ssl~\Fluoroch~cals.PRO\S~leD~~O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslyax\Fluoxoch~cals.PRO\Met~~\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Tue hug 05 07:32:01 2003 ~~~-~~----~---1----__~~-_-__-1_------------------~--~-----1----1 Name : 080103AR-305 Text: 1: C8 Acid (PFOA) XCO72503-4,250 rig/L Standard 080103AFb305 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 10:02:40 LC/MS/MS #6 MRM of 4 Channels ES413>369 6.66e5 Area @ ,,,,~,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,, I , , 1 G r I , r , I Time 2.00 4.00 6.00 8.00 10.00 J v 2: C6 Sulfortate (PFHS) XCO72503-4,250 rig/L Standard 080103AR-305 loo- Sm (Mn, 2x3) %- 04-Aug-2003 10:02:4C LCYMWMS #6 MRM of 4 Channels ES- 6.98 399 > 80 1.20e5 Area r A 0 /111,111,,1,,1,1111(1111,11/1/111~/1111, r I, rI I,I I Time 2.00 4.00 6.00 8.00 10.00 : C8 Sulfonate (CO72503-4,250 (PFOS) rig/L Standard )80103AR-305 IO j Sm (Mn, 2x3) 9.25 1197( 3 04-Aug-2003 10:02:4C LC/MS/MS #6 MRM of 4 Channels ES499 > 99 6.98e4 Area I Time Exygen Research, 3058 Research Drive, State College, PI 16801 000371 -- ------ -- -----___ - Quantify Sample Report w Study No.:L34910, Set No.: 080103AR, Ext.Date:08/01/03, Analyst:K.Ri.aha Page 10 SaluQle List: Last modified: Method: Last modified: Job Code: P:\Data\LWSMS6\ailsssl~\Fluoroch~cals.PRO\S~leDB\O8OlO3~ me Aug 05 07~24~43 2003 P:\Data\LQrlSMS6\Masslynx\Pluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11x59 2003 Decatur EC BC 080103 Printed: 'Pus Aug 05 07:32:01 2003 ----__-----------------------~-~-------~ -----A- __---- Name: 080103AR-305 Text : : PFOSA KO72503-4,250 rig/L Standard 180103AFL305 Sm (Mn, 2x3) 04-Aug-2003 10:02:4C LC/MS/MS #6 MRM of 4 Channels ES- 9.90 45565 i 498 > 78 2.39e5 Area i- Time 2.00 4.00 6.00 8.00 EXy!GWn Research, 3058 Research Drive, State College, PA 16801 e-------_- ------_-__- -Y-e---- -----------_ Quantify Sample Report 'lid Study No.: L34910, Set tio.:O80103AR, Ext.Date:08/01/03, Aualyst:K.Risha Page 11 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluaroch~cals.PRO\S~leDB\O8OlO3~ !tWe Aug 05 07:X:43 2003 P:\Data\LCMmS6\Wasslynx\Fluoroch~cals.RRO\~ethDB\~catur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Tus Aug 05 07:32:01 2003 ------------I_------------____I__- --------I_- ----__--_ Name: 080103AR-306 Text: .: C8 Acid (PFOA) l(CO72503-5,500 rig/L Standard 180103AR-306 IO 01 Sm (Mn, 2x3) 9.14 24235! 04-Aug-2003 10:24:22j LC/MS/MS #6 MRM of 4 Channels ES413 z 369 1.40e6 Area by 2: C6 Sulfonate [XCO72503-5,500 (PFHS) rig/L Standard 080103AR-306 -IO& Sm (Mn, 2x3) %- 0 llll,llll,lll,,ll,l,lllr,ll~l,~,,I,II,,/III 2.00 4.00 3: C8 Sulfonate XCO72503-5,500 (PFOS) rig/L Standard 080103AR-306 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 10:24:2d LC/MS/MS #6 MRM of 4 Channels ES- 8.97 399 > 80 2.48e5 Area , , , I , , , , , , , , Time 6.00 8.00 10.00 9.27 25896 04-Aug-2003 10324324 LC/MSlMS #6 MRM of 4 Channels ES499 > 99 1.52e5 Area Eacygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report 1~ Study No.:L34910, Set No.: 080103AR, Ext.Date:08/01/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\L(3MSMS6\Masslynx\FluorochsmicalB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 12 Decatur BC BC 080103 Name: 080103AR-306 Text : I4: PFOSA XCO72503-5,500 rig/L Standard 080103AFk306 1 oo- Sm (Mn, 2x3) %- 04-Aug-2003 10:24:2; LC/MSlMS #f MRM of 4 Channels ES- 9.90 498 > 78 4.79e5 Area @ ,,,,,,,~,,,,~,,~,~~~~~~~,,~~~~~~~~~~~~,i~~~~~ , , , , , , Time 2.00 4.00 6.00 8.00 10.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 ---0----e--s- -_---- -m--e Quantify Saxple Report hd Study No.: L34910, Set No .:080103AR, Ekt.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: iToh Code: P:\Data\L~SMS6\~sslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tus Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamieals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: -----__------------------ Tue Aug 05 07:32:01 2003 -------l_l-------------~---- Name: 080103AR-307 Text: .: C8 Acid (PFOA) YCO72503-6,1000 rig/L Standard 380103AFb307 10 % $ i Sm (Mn, 2x3) : 9.13 L4 46999, 2.00 4.00 8.00 : C6 SUlfOnate (CO72503-6,lOOO (PFHS) rig/L Standard 180103AR-307 10 Sm (Mn,`2x3) 8.96 8151( A---- Page 13 Decatur BC BC 080103 04-Aug-2003 10:46:08 LC/MS/MS #6 MRM of 4 Channels ES41322.693e669 Area Time 10.00 04-Aug-2003 10:46:08] LCIMSNS #6 MRM of 4 Channels ES399 > 80 4.74e5 Area 6.00 I3: C8 Sulfonate lXCO72503-6,lOOO (PFOS) rig/L Standard 080103AR-307 10 3 Sm (Mn, 2x3) 1 % Oi,,,,,,,,,~,,~,,,,~,,,,,,,~,,,,,,,,,~,,,,,,,,,~,~,~~~~,~~~~ 2.00 4.00 6.00 I p ' " I", r Time 8.00 10.00 9.25 51 730T 04-Aug-2003 10:46:08 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.90e5 Area Time 8.00 10.00 Oxygen Research, 3058 Research Drive, Stats College, PA 16801 000375 --v---e-- ------- -------------------_ -- Quantify Szunple Report Id Study No .:L34910, Set No.:O80103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyax\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tua Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Massl~\FluorochsmicalB\Decatur Sk Aug 03 07:11:59 2003 Page 14 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 -----------------------------------------------------~------- Name: Text: 080103Ub307 ,: PFOSA 3CO72503-6,1000 rig/L Standard 180103AFb307 10 03 % Sm (Mn, 2x3) 04-Aug-2003 10:46:04 LC/MS/MS #6 MRM of 4 Channels ES- 9.91 1791& i 498 > 78 9.27e5 Area i O'~.~~,~..`,~".,`...,`.`.,~~~~,`~","'~,'~.~,." I Time 2.00 4.00 6.00 8.00 Bxygen Research, 3058 Research Drive, State College, PA 16801 000376 Quantify Sample Report w Study No.rL34910, Set No.: 080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 15 S-10 List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Pluoroch~cals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSWS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 ------------------------B-------m-- -------- Name: Text: 080103AR-308 1: C8 Acid (PFOA) L34910-11 Spk E, 5000 rig/L, DF=lOOO 080103AFb308 lOO- Sm (Mn,. 2x3) I r %- 04-Aug-2003 11:07:51 LCIMSNS #6 MRM of 4 Channels ES- 9.13 413 > 369 2.44e4 Area \wl 2: C6 Sulfonate (PFHS) L3491 O-1 1 Spk E, 5000 rig/L, DF=lOOO 080103AFb308 lo& 7 %- Sm (Mn, 2x3) I 3 Time 10.00 04-Aug-2003 11:07:51 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 z 80 3SOe3 Area 0 l.l,lll.,II,I,I.I.,I.I., 2.00 3: C8 Sulfonate (PFOS) L3491 O-l 1 Spk E, 5000 rig/L, 4.00 DF=lOOO 080103AR-308 Sm (Mn, 2x3) I ,, I ,, r II,,, 6.00 c I ,, 8.00 I I ,, I I. ,'. I ,I Is IG Time 10.00 04-Aug-2003 11:07:51 LClMSiMS #6 MRM of 4 Channels ES499 > 99 3.29e4 Area Time Eacygen Research, 3058 Research Drive, State COllegO,.PA 16801 000377 ---------_I --------_I_- -------w---e- ------ Qwultify Sample Report $4 Study No.: L34910, Set No.:O80103AR, Ext.Date:08/01/03, A.nalyst:K.Riaha SanTpls List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\L~SMS6\Maaalynx\Fluorachamica\Met~B\D~catur Sun Aug 03 07:11:59 2003 Page 16 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 --------A--A--a---------m-----e---- -------I---____ Name: 080103AR-308 Text : 4: PFOSA -34910-l 1 Spk E, 5000 rig/L, DF=lOOO 180103AR-308 10 "i Sm (.Mn, 2x3). 04-Aug-2003 11:07:511 LC/MS/MS #6 MRM 9.90 230E; of 4 Channels ES- 498 > 78 . . 1.26e4 Area Oj I;;;- Time 2.00 4.00 6.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000378 we- ----- ----m--m--- ----- ---- Quantify Sanrple Report w Study No.:L34910, Set No.: 080103AR, Ra&.Date:O8/01/03, Analyst:X.Risha Page 17 Sample List: Last modified: Method: Last modified: Jab Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leD~\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 000103 Printed: ----w-w---_ Tue Aug 05 07:32:01 2003 ---_----------___I___ --we-- Name: 080103AR-309 Text: : C8 Acid (PFOA) -34910-11 SpkE,5000ng./L,DF=100 160103AFb309 10 Sm (Mn, 2x3) MRM of 4 Channels ES- 9.13 413 > 369 2937 1.82&i Area T 2.00 4.00 6.00 8.00 : C6 Sulfonate (PFHS) .34910-11 SpkE,5000ng/L,DF=lOO Time 1 ~60103AR-309 10 Sm (Mn, 2x3) MRM of 4 Channels ES399Bao 2.6ae4 Area 3: C8 Sulfonate (PFOS) L34910-11 SpkE,SOOOng/L,DF=lOO 060103AR-309 10 Sm (Mn, 2x3) 6.00 9.25 51842 6.00 a.00 Area Time Rxygen Research, 3058 Research Drive, State College, PA 16801 v-m-- -------- w------e--- ----- --------e---P-__ Quantify Sample Report ,,= Study No.:L34910, Set No.: 080103AR, Ext.Date:08/01/03, Analyst:X.Risha Page 18 Sample List: Last modified: Method: Last moUified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochsmicals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\Lc3MSMS6\Masslynx\Fluorochemicals.PRO\~ethDB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC EC 080103 Printed: Tue Aug 05 07:32:01 2003 -- ------------------__________I_________-_ Name: Text: 080103AR-309 : PFOSA .34910-l 1 Spk E, 5000 rig/L, DF=lOO MO1 03AR-309 10 Sm (Mn, 2x3) % 04-Aug-2003 11:29:3f LC/MS/MS #E MRM of 4 Channels ES- 9.87 2187C 1 498 > 78 1.12e5 Area 1 L Time Exygen Research, 3058 Research Drive, State College, PA 16801 000380 ----------__-------_-- -------e-w---- ----- Quantify Sample Report +, Sway NO .:L34910, Set No .:080103AR, Ext.Date:08/01/03, Aualyst:K.Risha Page 19 Stunple List: Last maifiea: Method: Last modified: Job code: P:\Data\L~SMS6\blasslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tus Aug 05 07:24x43 2003 P:\Data\LeMSMS6\~sslynx\Fluorochamicals.PRO\MetMB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: e----d- Tue Aug 05 07:32:01 2003 ---------------- ----------- Name : 080103AR-310 Text: -----------__--_- : C8 Acid (PFOA) -34910-20SpkF,5000nglL,DF=l00 180103AR-310 10 Sm (Mn, 2x3) 04-Aug-2003 11:51:14) LC/MS/MS#6 9.13 2826 MRM of 4 Channels ES413>369 1.66e5 Area 2.00 4.00 6.00 8.00 : C6 Sulfonate (PFHS) ,34910-20SpkF,5000ng/L,DF=lOO 380103AB310 10 Sm (Mn, 2x3) LC/MS/MS#6 MRM of 4 Channels ES- 8.96 399 > 80 433t 2.50e4 Area I( : C8 Sulfonate (PFOS) .34910-20SpkF,5000 ng/L,DF=lOO )80103AR-310 10 Sm (Mn, 2x3) 04-Aug-200311:51:1 MRM of 4 Channels ES499 > 99 5.36e4 Area Time Rxygsn Research, 3058 Research Drive, State College, PA 16801 0003Rl. Quantify Sample Report ,J Study No.:L34910, Set No.: 080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 20 Sample List: Last modified: Method: g;tCrdFfied: : P:\Data\LCMSMS6\MasslyPx\Fluorochemicals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\fluorochamicalsB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 -----_ -----_----_----~--~~~- _------- we--- ----- Name : 080103AR-310 Text : : PFOSA -3491 O-20 Spk F, 5000 rig/L, DFd 00 180103AFb310 Sm (Mn, 2x3) 10 "$ -1 % i i O'~~~~,~~~~,`~~~,~~~`,~"`,"~`,~~'~,"'~,~'~~,~', 2.00 4.00 6.00 8.00 04-Aug-2003 1151 :14j LC/MS/MS #6 MRM of 4 Channels ES- 9.90 13521 498 > 78 6.94e4 Area - r , Exygen Research, 3058 Research Drive, State College, PA 16801 00038Z ,,,-,, X,".,.l.- .._ --_-, _."I l-,.l-ll.- ,.._ ._-, .~l---ll -. -__-----------------ll-_--------- Quantify Sample Report '14 Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluoroch~cals~PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LQIISMS6\MasslyPx\FluorochemicalB\Decatur Sun Aug 03 07:11:!59 2003 --- Page 21 Decatur BC BC 080103 Printed: -----__ Tue Aug ----- Name: 080103AR-311 Text : 05 07:32:01 2003 ----------------w-m- ---------___ : C8 Acid (PFOA) -3491 O-5, DF=lO >80103AR-311 10 Sm (Mn, 2x3) , %-j i 4 2.00 04-Aug-2003 12:12:52 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 1.06e5 Area Time 10.00 !: C6 Sulfonate (PFHS) L34910-5, DF=lO 04-Aug-2003 12:12:5 380103AR-311 Sm (Mn, 2x3) 10 85.8916 I-~`~,~~,,.,,,~,,,,,,,,,,,~,,,,~,,,,,,,,,,,,~,~~,,,,,,~,..,..,, Time 2.00 4.00 6.00 8.00 10.00 RWgen Research, 3058 Research Drive, State College, PA 16801 -P-M--- ----------- -----------s---m- Quantify Sample Report ',d Study No.:L34910, Set No .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last nodified: Job Code: P:\Data\LCMGMS6\Massly\Fluoroch~cals.PRO\SampleDB\O80103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tus Aug 05 07:32:01 2003 --- Page 22 Decatur BC BC 080103 Name: 080103AR-311 Text : : PFOSA .3491 O-5, DF=lO 180103AFb311 10 Sm (Mn, 2x3) % 1 04-Aug-2003 12~1252 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 1668C ) 498 > 78 .8.67e4 Area O',,.,,"~,,`,,,,,,,`,"",,,,,,,`,,,,"',,',',,,,. IL- Time 2.00 4.00 6.00 8.00 10.00 Ewgen Research, 30.58 Research Drive, Stata college, PA 18801 000384 Quantify Sample Report Study No.: L34910, Set No .:080103AR, $4 Ext.Date:08/01/03, Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Ma~~l~\Fluoroch~cals.~~\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LQISMS6\Masslynx\PluorochsmiEalsB\Decatur Sun Aug 03 07:11:59 2003 Printed: ---- Tue Aug 05 07:32:01 ----_ -------- 2003 -w--e------- Name: 080103AR-312 Text : 1: C8 Acid (PFOA) IL3491 O-5 Rep, DF=lO 080103AR-312 Sm (Mn, 2x3) 2.00 2: C6 Sulfonate (PFHS) `u' L3491 O-5 Rep, DF=lO 080103AFb312 Sm (Mn, 2x3) Analyst:X.Risha Page 23 Decatur BC BC 080103 --- ----- 04-Aug-2003 12:34:34 LC/MS/MS #6 MRM of 4 Channels ES- 413r369 . 8.59e4 Area Time 3: C8 Sulfonate (PFOS) L3491 O-5 Rep, DFd 0 080103AFk312 Sm (Mn, 2x3) 1 Time 04-Aug-2003 12:34:3d MRM of 4 Channels ES9.24 7449 wgen Research, 3058 Research Drive, State College, PA 16801 60038s ------ __----- ----- ---1----------__ Quantify Sample Report Study No.:L34910, Set No .:080103AR, Ext.Dats:08/01/03, Analyst:K.Risha Page 24 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Wasslynx\Fluorochamicals.PRO\S~leDB\O~OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\FluorochemicalsB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 ------~--------~------------ --P---P--__ Name: 080103AR-312 Text : 4: PFOSA IL3491 O-5 Rep, DF=lO 080103AFb312 loo- Sm (Mn, 2x3) %- 04-Aug-2003 12:34:35( LC/MS/MS #6 MRM of 4 Channels ES- 9.87 498>78 9.40e4 Area Exygen Research, 3058 Research Drive, State College, PA 16801 0003f3G --v---s---- ------- --e--w--- Quantify Sample Report Study No.:L34910, w Set No.: 080103AR, Ext.Date:08/01/03, Analyst:K.Riaha SangZle Liat: P:\Data\L~S2HS6\bssl~\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Last modified:. Tue Aug 05 07:24:43 2003 Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 ---------_ Page 25 Decatur BC BC 080103 Name: 080103AR-313 Text : 1: C8 Acid (PFOA) L3491 O-1 0, DF=lO 080103AR-313 100- Sm (Mn, 2x3) %- 04-Aug-2003 12:56:21 LC/MS/MS #6 MRM of 4 Channels ES413> 369 1.86e5 Area 0--- I r I , I , , , , I , Time 2.00 4.00 6.00 8.00 10.00 ~ 2: C-.6 -S--u-l-fanate----- ,fP__F-H--S, 1 1.3491 O-l 0, DF=lO C)80103AR-313 lOO: Sm (Mn, 2x3) %- 040Aug-2003 12:56:2' LC/MS/MS #E MRM of 4 Channels ES- 8.96 1564- 399 > 8C 9.26eZ Are5 !- 3: C8 Sulfonate (PFOS) L3491 O-l 0, DF=lO 080103AR-313 loo- Sm (Mn, 2x3) %- 9.25 _ 14012 04-Aug-2003 12:56:21 LCIMSNS #6 MRM of 4 Channels ES499 > 99 8.15e4 Area Exygen Research, 3058 Research Drive, State College, PA 16801 000387 Quantify Sample Report Study No.: L34910, Set No.:O80103AR, Ext.Date:08/01/03, Analyst:K.Risha Sawple List: Last modified: Method: Last modified: Job Code: P:\Data\LCWSMS6\Masslynx\Fluorochemicals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\L~SMS6\Masslynx\FluorochemicaB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 26 Decatur BC BC 080103 Name : 080103AR-313 Text : 4: PFOSA L3491 O-1 0, DF=lO 080103AR-313 100- Sm (Mn, 2x3) %- 04-Aug-2003 12:56:21 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 I .Ol e5 Area Fxygen Research, 3058 Research Drive, Stats College, PA 16801 000388 ------------- --__--_------- ------7---- Quantify Sample Report Study No.: L34910, Set NO .:080103AR, Rxt.Date:08/01/03, Aualyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Mssl~\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCM~S6\Masslynx\Fluorochsmicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue hug OS 07:32:01 2003 Page 27 Decatur BC BC 080103 Name: 080103AR-314 Text : : C8 Acid (PFOA) -3491 O-l 0 Rep, DF=lO )80103AR-314 10 Sm (Mn, 2x3) 9.13 ,3106: 04-Aug-2003 13:18:lC LC/MShlS #6 MRM of 4 Channels ES413 > 369 1.85e5 Area 4 hLb= Time L 2.00 4.00 6.00 8.00 10.00 2: C6 Sulfonate (PFHS) `& L3491 O-l 0 Rep, DF=lO 080103AFb314 100-I Sm (Mn, 2x3) %- 04-Aug-2003 13:18:lC LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 1811 l.lOe4 Area 0 ,,,,1,,~,,.,,.,,,,,,,,.,,~,,,,,,,,,,,,,,,,, , - 7. , I I Time 2.00 4.00 6.00 8.00 10.00 : C8 Sulfonate (PFOS) -3491 O-l 0 Rep, DF=lO )80103AR-314 10 Sm (Mn, 2x3) 04-Aug-2003 13: 18: 1C LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.18e4 Area Rxygen Research, 3058 Research Drive, State College, PA 16801 QQ0389 -v-s--- ----------------I_____________ --v-v Quantify Sample Report Study No.: L34910, Set No.:O80103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 28 Sample List: Last modified: Method: Last modified: sob Code: P:\Data\L~SMS6\Ma~sl~\Fluorochamica~s.PRO\S~leDB\O8OlO3~ Tue hug 05 07:24:43 2003 P:\Data\L~SMS6\Masslynx\Fluorochamicals.P~\Met~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: -------- Tue Aug 05 07:32:01 2003 ------------------____I______ Name: 080103.m-314 Text: :: PFOSA -3491 O-l 0 Rep, DF=l 0 380103AR-314 10 "$ %d Sm (Mn. 2x3) I , -I 04-Aug-2003 13:18:1( LWMSIMS #E MRM of 4 Channels ES- 9.67 498>7E 2686: 1.41e5 Area Time , Exygen Research, 3058 Research Drive, State College, PA 16801 000390 ----------- --------- ----s-Y---- Quantify sample Report Study No.: L34910, Set No.:O80103AR, u Ext.Date:08/01/03, Sample List: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Last modified: Tus Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslyzuc\FluorochamicalB\Dacatur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: ---- -__-__ Tue Aug 05 07:32:01 2003 -----__-- ---------------__---------------------------- Name: Text: 080103AR-315 : C8 Acid (PFOA) (CO72503-1,25 rig/L Standard J80103AR-315 1001 % Sm (Mn, 2x3) ----__---__ Analyst:R.Risha Page 29 Decatur BC BC 080103 04-Aug-2003 13:39:58 LCIMSNS #6 MRM of 4 Channels ES413> 369 8.23e4 Area 0 !: c6 Sulfonate KC072503-1,25 (PFHS) rig/L Standard 380103AR-315 10 Sm (Mn, 2x3) Time 04-Aug-2003 13:39:5d LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 2099 1.27e4 Area f 0 ,..r,.-.,....,,..,,,..,,...,,,,..,....,,.,! 2.00 4.00 6.00 3: C8 Sulfonate : KCO72503-1,25 (PFOS) rig/L Standard 380103AR-315 10 9 Sm (Mn, 2x3) 8.00 T- 9.24 1301 10.00 1 04-Aug-2003 13:39:58 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 8.29e3 Area un 1 ,~~~,(~~`,~~~~,~~`~,`1~~,~~`~,~`1',"'~,'~~~/ I Time 2.00 4.00 6.00 8.00 10.00 Wgen Research, 3058 Research Drive, State College, PA 16801 000391 --w---m------- ------------------ --- Quantify Saqle Report Study No. : L34910, Set No.:O80103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 30 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicalst~B\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: -------__------ Tue Aug 05 07:32:01 2003 --------------l__- Name: 080103AR-315 Text: 4: PFOSA /XCO72503-1,25 rig/L Standard 080103AFb315 loo- Sm (Mn, 2x3) %- 04-Aug-2003 13:39:5d LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498>78 2.30e4 Area Oxygen Research, 3058 Research Drive, State College, PA 16801 Quantify S-10 Report Study No.:L34910, Set No .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Cd Sample List: P:\Data\L~S6\~ssl~\Fluoroch~cals.PRQ\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LQlmS6\Masslynx\Fluorocbemicals.PRO\~et~B\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job code: Page 31 Decatur BC BC 080103 Printed: ---4------e-- Tue Aug 05 ------____---- 07:32:01 2003 ---c-----------___--------- Name: 080103AR-316 Text : 1: C8 Acid (PFOA) XCO72503-2,50 ngJL Standard 080103AR-316 lOc-- Sm (Mn, 2x3) %- 9.12 254147 04-Aug-2003 1 14:01:43 LC/MSJMS #6 MRM of 4 Channels ES- 413>369 1.50e5 Area : C6 Sulfonate (CO72503-2,SO (PFHS) ngJL Standard 180103AFL316 10 "3 Sm (Mn, 2x3) 8.9Z j 421' 1 04-Aug-2003 14:01:44 LCIMSIMS #6 MRM of 4 Channels ES399 > 80 2.50e4 Area 2.00 4.00 6.00 : C8 Sulfonate (PFOS) (CO72503-2, 50 ngJL Standard )80103AR-316 10 Sm (Mn, 2x3) J i Ok..,...,,....,..`,,..`.,"..,.`.',...,, 2.00 4.00 6.00 % V 8.00 10.00 Time 1 I 7 04-Aug-2003 14:01:43 LCJMSJMS #6 9.2! i 286( I MRM of 4 Channels ES499 > 99 1.66e4 Area I___ Time 8.00 10.00 kygen Research, 3058 Research Drive, State College, PA 16801 0003!?3 -- -------------- ---------me - Quantify Sample Report Study No.rL34910, set NO .:080103AR, Eact.Date:08/01/03, Analyst:K.Risha Ud Sample List: P:\Data\LCM~S6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Page 32 Decatur BC EC 080103 Printed: -m-e-- Tue Aug 05 07:32:01 2003 -------------------_-~-_-------------_-_____ Name: 080103AR-316 Text : : PFOSA (CO72503-2,50 rig/L Standard 180103AR-316 10 Sm (Mn. 2x3) . . I % 3 04-Aug-2003 14:01:4I LCIMSIMS #f MRM of 4 Channels ES- 9.90 I 8991 498 > 7E 4.83e4 Arez o'~"~,`~`~,~`~~,~~~`,~;`~,`~",~~'~,'~",~'~~,~~~ Time 2.00 4.00 6.00 8.00 Rwgen Research, 3058 Research Drive, State College, PA 16801 000394 Quantify Sample Report Study No.: L34910, Set No.: 080103AR, Ext.Date:08/01/03, Analyst:K.Risha tic, Sample List: P:\Data\LCMSMS6\Masalynx\Fluoroc~~cals.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\EIaaslynx\Fluorochemicalr Last modified: Sun Aug 03 07:11:59 2003 irob Code: Printed: --- Tue Aug 05 07:32:01 2003 ------me------- ~---~---------------_ Name: 080103AR-317 Text : : C8 Acid (PFOA) .3491 O-1 1, DF=lOO )80103AR-317 Sm (Mn, 2x3) 9.11 10 941( -I Page 33 Decatur SC BC 080103 04-Aug-2003 14:23:2? LC/MS/MS #6 MRM of 4 Channels ES- 413 > 369 5.65e4 Area Time 2.00 4.00 6.00 8.00 1o:oo 2: C6 Sulfonate (PFHS) `& L3491 O-1 1, DF=l 00 080103AFb317 Sm (Mn. 2x3) 04-Aug-2003 14:23:2? LC/MS/MS #6 MAM of 4 Channels ES399 > 80 Oi.,.,,....,..,.,,...,.,,,,....,...~,....,....,..~.,~~.~,.~~. Time 2.00 4.00 6.00 8.00 10.00 3: C8 Sulfonate (PFOS) L3491 O-1 1, DF=lOO 080103AR-317 Sm (Mn, 2x3) 04-Aug-2003 14:23:2? LC/MSlMS #6 MRM of 4 Channels ES- 9.24 499 > 99 3.85e5 Area Exysen Research, 3058 Research Drive, State College, PA 16801 -------------__-----_---- ----e--------w----- -------- Quantify Sample Report study No.:L34910* Set No.:080103AR, Ea&.Date:08/01/03, Analyst:K.Risha \r, Sample List: P:\Data\LX=MSHS6\Masslyax\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Laet modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tus Aug 05 07:32:01 2003 Page 34 Decatur BC BC 080103 Name: 080103AR-317 Text: 4: PFOSA L3491 O-1 1, DF=lOO 080103AR-317 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 14:23:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 219887 498 > 70 1.09e.5 Area 0 "","",11","","","","`1,"","' I,1II I I 1 , , , I , Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ---------- -------- -------___ ------a--- Quantify Sample Report Study No .:L34910, Set No .:080103AR, Xxt.Date:08/01/03, ',d Analyst:X.Risha S~lei List: P:\Data\Lc3MSMS6\Masslyrur\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\~et~B\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Page 35 Decatur BC BC 080103 Printed: ---_- 'he Aug -~--------_- Name: 080103AR-318 Text : 05 07:32:01 2003 ----- -------_-m___ -I------____ 1: CS Acid (PFOA) IL3491 O-l 1 Rep, DF=lOO 080103AFb318 100- Sm (Mn, 2x3) %- 04-Aug-2-003 14:45:lj LCNSIMS #6 MRM of 4 Channels ES413>369 5.66e4 Area O';`,,,r,,,,,,,,,,,,,,,,,,,,~ 2.00 4.00 2: C6 Sulfonate (PFHS) w L3491 O-l 1 Rep, DF=lOO 080103AR-318 Sm (Mn, 2x3) ,II,Iq I,,! 6.00 ,I I 8.00 8.95 207 , , ,";`: 10.00 , , , , , , ,h Time 04-Aug-2003 14:45:17 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.56e3 Area 2.00 4.00 6.00 8.00 10.00 3: C8 Sulfonate (PFOS) L3491 O-l 1 Rep, DF=lOO 080103AFb318 10 i Sm (Mn, 2x3) 9.25 48518 04-Aug-2003 14:45:17 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.82e5 Area L Emen Research, 3058 Research Drive, State College, PA 16801 Time 000397 --_ .-. . .._-._. -.---- --.. - --s--p ---s---P----- ---_- --- Quantify Sample Report Study No.: L34910, Set No.:O80103AR, 'J Ext.Date:O8/01/03, Analyst:K.Risha Saznple List: P:\Data\LCMSMS6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug OS 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicalsr Last modified: Sun Aug 03 07:11:59 2003 Job Code: Page 36 Decatur BC BC 080103 Printed: ----------------b-----s Tue Aug Name: 080103AR-318 Text : 05 07:32:01 2003 ---------- ---_^---- -m-m---- : PFOSA -3491 O-l 1 Rep, DF=lOO 380103AR-318 Sm (Mn, 2x3) 10 "i J %10~.`.~,"~.,`~`.,."`,`...,~`~.,~~'.,~"','.'.,.~~ 2.00 4.00 6.00 8.00 04-Aug-2003 14:45:17 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 16405 0.63e4 Area 1. Time Ekygen Research, 3058 Research Drive, State College, PA 16801 000398 Quantify Sample Report Study No.: L34910, Set No .:080103AR, Ext.Date:08/01/03, Analyst:X.Risha Page 37 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cal~.PRO\S~leDB\O8OlO3~ Tus Aug 05 07:24:43 2003 P:\Data\LCM~S6\Masslynx\Fluorochemica\Decatur Sun Aug 03 07:11:59 2003 Decatur BC EC 080103 Printed: --------s-e--- Tus Aug 05 07:32:01 2003 ___--------------------- m-w-- --------- Name: 080103AR-319 Text : 1: C8 Acid (PFOA) iL3491 O-l 1, DF=lO `080103AR-319 IOO- Sm (Mn, 2x3) %- 9.11 _ 80473 04-Aug-2003 l&07:04 LC/MS/MS #6 MRM of 4 Channels ES413>369 4.67e5 Area !: C6 Sulfonate (PFHS) L3491 O-l 1, DF=l 0 080103AR-319 100- Sm (Mn, 2x3) %- 04-Aug-2003 15:07:04 LC/MS/MS #6 MRM of 4 Channels ES- a.95 399 > 80 1.36e4 Area 0 /, , I, I ,-. I,, .1), 2.00 3: C8 Sulfonate (PFOS) L3491 O-1 1, DF=lO . r I I,. 1 I., 4.00 1 I, I, F<", 6.00 / I I I, 8.00 080103AR-319 100- Sm (Mn, 2x3) 9.25 _ 526238 %- 10.00 ,-, , , , , Time 04-Aug-2003 15:07:04 LCIMSIMS #6 MRM of 4 Channels ES499 > 99 3.05e6 Area , , I , I I , I I I I Time 2.00 4.00 6.00 8.00 10.00 &Id Exygen Research, 3058 Research Drive, State College, PA 16801 000399 Quantify Sample Report ',d Study No .:L34910, Set No .:080103AlZ, Ext.Date:08/01/03, A.nalyst:K.Risha Sample List: Last modified: Method: Last nmdifiad: Job Code: P:\Data\L~SMS6\~sslynx\Fluoroch~cals.PRO\S~~eDB\O8OlO3~ Tua Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 38 Decatur EC BC 080103 Printed: --e-e------------ Tua Aug 05 07:32:01 2003 ----- -----__--------___ Name: 080103Xfi-319 Text: 4: PFOSA IL3491 O-l 1, DF=lO 080103AR-319 loo- Sm (Mn, 2x3) %- 04-Aug-2003 15:07:04/ LC/MS/MS #6 MRM of 4 Channels ES- 9.87 498 > 78 1 O.OOe5 Area 2 , , , , , , , Time 10.00 Exygen Research, 3058 Research Drive, State Collega, PA 16801 II- ______ __-___l----.--- 000400 Quantify Sample Report Study No.:L34910, Set No .:080103AX, Ext.Date:08/01/03, Analyst:X.Risha \r, Sample List: P:\Data\LCM~S6\Mas~lynx\Fluoroch~cals.P~\S~leDB\O8OlO3~ Last xuodified: Tue hug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemical9\Decatur Last modified: SW hug 03 07:11:59 2003 Job Code: Printed: Tue hug OS 07:32:01 2003 Page 39 Decatur BC BC 080103 Name: 080103AR-320 Text: 1: CB Acid (PFOA) L3491 O-l 1 Rep, DF=lO 080103AR-320 100- Sm (Mn, 2x3) %- 04-Aug-2003 15:28:46j LC/MS/MS #6 MRM of 4 Channels ES413>369 4.58e5 Area 0 "1',"","",""["","","","","" , , , , , , I , , , , Time 2.00 4.00 6.00 8.00 10.00 2: C6 Sulfonate (PFHS) 13491 O-1 1 Rep, DF=lO 080103AFb320 100- Sm (Mn, 2x3) %- 8.96 _ 2458 04-Aug-2003 1 15:28:46 LC/MS/MS #6 MRM of 4 Channels ES- 399 > 80 1.49e4 Area I: CB Sulfonate (PFOS) L3491 O-1 1 Rep, DFdO 04-Aug-2003 15:28:46 LC/MS/MS #6 080103AR-320 Sm (Mn, 2x3) MRM of 4 Channels ES- 10 % 1 9.25 390663 L 499 a- 99 2.30e6 Area Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 OoQ4Qa --w--w--___ ----w---s-- -------e----- --c----I__I Quantify Sample Report Study No. : L34910, Set No.:O80103AR, 44 Eatt.Date:08/01/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS6\Maaslynx\Fluorochamicals.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCHSMS6\Masslynx\Bluoroch~cals.PRO\Met~B\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Page 40 Decatur BC BC 080103 Printed: -m---_-v Tue Aug 05 07:32:01 2003 -_-_----__-----__--_______l___l-_ Name: 080103AR-320 Text: -7--e--w--__ : PFOSA -34910-l 1 Rep, DF=lO )80103AR-320 loo- Sm (Mn, 2x3) %- 04-Aug-2003 15:28:46 LC/MS/MS #6 MRM of 4 Channels ES- 9.87 i503ad c 498 r 78 7.59e5 Area 0- ~~~~,~~~~,~1~,,"~,(ll~~,'~~~,~~~~,~'~',~~'~,'~C i- Time L 2.00 4.00 6.00 8.00 10.00 E-en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No. : L34910, Set No .:080103AR, Ext.Date:oa/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCM~S6\MasSl~\FluOrocbemicalS.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMSS\Masslynx\Fluorochamical8.PRO\Met~R\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 41 Decatur BC BC 080103 Name: oaoio3sb321 Text : 1: C8 Acid (PFOA) L3491 O-20, DF=l 00 080103AR-321 loo- Sm (Mn, 2x3) %- 04-Aug-2003 15:50:25 LC/MS/MS #6 MRM of 4 Channels ES- 9.12 413 > 369 4.43e4 Area 2.00 2: C6 Sulfonate (PFHS) L3491 O-20, DF=lOO 080103AR-321 10 Sm (Mn, 2x3) I , I , , , . , , , , , ,\ Time 10.00 04-Aug-2003 1550324 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 334 2.23e3 Area 3: C8 Sulfonate (PFOS) L3491 O-20, DF=lOO 080103AR-321 Sm (Mn, 2x3) 04-Aug-2003 15:50:25 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.96e4 Area Time Oxygen Research, 3058 Research Drive, State College, PA 16801 QQQM?3 Quantify Sample Report Study No.:L34910, `id Set No .:080103AR, Ext.Date:00/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Dats\LCblSMS6\Masslynx\Fluoroch~cal8.PRO\S~leDB\O8OlO3~ !Pue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\FluarachamicarsB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 42 Decatur BC BC 080103 Name: 080103AR-321 Text : 4: PFOSA L3491 O-20, DF=lOO 080103AR-321 Sm (Mn, 2x3) 04-Aug-2003 15:50:2t LC/MS/MS #E MRM of 4 Channels ES498 > 78 3.40e4 Area Time Exygen Research, 3058 Research Drive, Stats College, PA 16801 000404 Quantify Sample Report Study No. : L34910, Set No.:O80103AR, ',d Ext.Date:O8/01/03, Analyst:R.Risha Sanrple List: P:\Data\LCMSMS6\Ma5slynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\MaSslynx\Fluoroch~cals.PRO\Met~B\Decatur Last modified: Job Code: Sun Aug 03 07:11:59 2003 Page 43 Decatur BC BC 080103 Printed: ----------me-----___ Tue Aug 05 07:32:01 2003 -_--__-_------ ----_-------___~ Name: 080103AR-322 Text : 1: C8 Acid (PFOA) IL3491 O-20 Rep, DF=i 00 080103AR-322 100- Sm (Mn, 2x3) %- 04-Aug-2003 16:12:Oij LC/MS/MS #6 MRM of 4 Channels ES413>369 3.44e4 Area O~,,,,,~,,,,,,,,.,~-;-rn-,,,,,,, , , , ,m Time 2.00 4.00 6.00 8.00 10.00 ,,& 2: C6 Sulfonate (PFHS) L3491 O-20 Rep, DF=lOO 080103AR-322 Sm (Mn, 2x3) 04-Aug-2003 16:12:07 LCIMSNS #6 MRM of 4 Channels ES- 8.93 399 > 80 2307 1.76e3 Area 2.00 4.00 6.00 8.00 3: C8 Sulfonate (PFOS) IL3491 O-20 Rep, DF=lOO 080103AR322 Sm (Mn, 2x3) / %P 2.00 4.00 6.00 8.00 ExyOen Research, 3058 Research Drive, State College, PA 18801 10.00 04-Aug-2003 16: 12:0-/1 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.76e4 Area 10.00 Time 080405 -v--m --w-v-- _------ -----------1___ Quantify Sample Report Study No .:L34910, Set No.:O80103~R, Ext.Date:08/01/03, '4 Analyst:K.Rlsha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Piassl~\Fluoroch~cals.RRO\S~leDE\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\L~SMS6\Maeslynx\FluorochemicalB\D~catur Sun Aug 03 07:11:59 2003 Page 44 Decatur BC BC 080103 Printed: Tus Aug 05 07:32:03 2003 --------~---------__-_-------,----------~-, Name: 080103AR-322 Text : -P--1----- 1: PFOSA -3491 O-20 Rep, DF=lOO 380103AR-322 10 7 %-j Sm (Mn, 2x3) . I 04-Aug-2003 16: 12:07 LC/MS/MS #6 MRM of 4 Channels ES- 9.9c ) 537' 498 > 78 2.09e4 Area Time 6.00 8.00 men Research, 3058 Research Drive, State College, PA 16801 --I-------------___---__l_______l_____---~ Quantify Sample Report Study No .:L34910, Set No.:O80103AR, Ext.Date:08/01/03, Analyst:K.Riaha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Maselynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Tue Aug OS 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Print sd : Tue Aug 05 07:32:01 2003 Name: 080103AR-323 Text: 1: C8 Acid (PFOA) ---- Page 45 Decatur BC BC 080103 080103AFb323 Sm (Mn, 2x3) MRM of 4 Channels ES- 2: C6 Sulfonate XCO72503-3,100 (PFHS) rig/L Standard 080103AR-323 Sm (Mn, 2x3) 3: C8 Sulfonate XCO72503-3,100 2.00 4.00 (PFOS) rig/L Standard 080103AR-323 Sm (Mn, 2x3) 04-Aug-2003 16:33:5C LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 4.74e4 Area 10.00 04-Aug-2003 16:m:sd LC/MS/i'vlS #6 MRM of 4 Channels ES499 > 99 Area Bxygen Research, 3958 Research Drive, State College, PA 16801 ---- ----------__I- -----I_------- Quantify Sample Report Study No .:L34910, Set No .:080103AR, Ext.Date:O8/01/03, Analyst:K.Risha 'W Sample List: ~:\Data\L~SMS6\~sslynx\Fluoroch~cals.PRO\S~leDB\O6OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\FluorochemicalsR\D~catur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tua Aug 05 07:32:01 2003 Page 46 Decatur BC BC 080103 Name: 080103AR-323 Text : : PFOSA (CO72503-3,100 rig/L Standard 180103AR-323 10 Sm (Mn, 2x3) % 1 i 04-Aug.2003 16:33:X LCYMSIMS #6 MRM of 4 Channels ES- 9.89 498 > 78 17621 9.3104 Area Oxygen Research, 3058 Research Drive, State College, PA 16801 ----I_-----~----I---I- s-m------ Quantify S-10 Report Study No.: L34910, Set No .:080103AR, Xxt.Date:08/01/03, Analyst:X.Risha '4 Smgls List: P:\Data\LCMSblS6\Masslyrur\$luoroch~cals.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:X:43 2003 Method: P:\Data\L~SMS6\Pssl~\FluorochamicR\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Page 47 Decatur BC BC 080103 Printed: -------m-P Tam Aug 05 07:32:01 -L_4--- Name: 080103AR-324 Text: 2003 ----M--P_- -- ----- 1: C8 Acid (PFOA) XCO72503-4,250 rig/L Standard 080103AFb324 loo- Sm (Mn, 2x3) %- 04-Aug-2003 16:55:35 LC/MS/MS #6 MRM of 4 Channels ES413>369 5.78e5 Area 0 ,,,,,~.,,,,,,,,,",,,.,,..,`,`,,`,,,",,,,, 2.00 4.00 6.00 8.00 1: C6 Sulfonate KO72503-4,250 (PFHS) rig/L Standard 180103Ak324 10 Sm (Mn, 2x3) 6.96 17041 04-Aug-2003 16:55:35] LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.05e5 Area 2.00 4.00 6.00 8.00 10.00 I: C8 Sulfonate KC072503-4,250 (PFOS) rig/L Standard 080103AFG324 Sm (Mn, 2x3) 9.24 1164Z 3 04-Aug-2003 16:55:35 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 6.79e4 Area IL-- 2.00 4.00 6.00 8.00 10.00 Fxygen Research, 3058 Research Drive, State College, PA 16801 Time oaa4e9 --------II____-__---_--------~----- -- Quantify Sample Report Study No .:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha %d Semple List: P:\Data\L~SMS6\Mssslynx\Pluoroch~cals.PRO\S~leDB\O8OlO3~ Last modified: me Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\~sslynx\Fluorochemicalt~B\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Page 48 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 --_--__--_____------------------------------------ -----e--m Name: 080103AR-324 Text : 4:: PFOSA r1l(CO72503-4,250 rig/L Standard 380103AR-324 10 Sm (Mn, 2x3) % 3 1 O'~~,~,~~~.,~~`~,~~",~~`~,~`~`,~~'.,'~~~I~"~I~~~ 2.00 4.00 6.00 04-Aug-2003 16:55:3d LC/MS/MS #6 MRM of 4 Channels ES- 9.89 4010: 3 498 > 78 2.14e5 Area L Time 8.00 Exygea Research, 3058 Research Drive, State College, PA 16801 QQQ410 Quantify Sample Report Study No.: L34910, Set N0.:060103AR, Ext.Date:08/01/03, Analyst:K.Risha yud Sample List: P:\Data\L~SMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Mssslynx\Fluorochemicals\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Page 49 Decatur BC BC 080103 Printed: ---_ `he --------_------- Aug 05 07:32:01 2003 --------------------- ---_--___ ---B---e_ Name: 080103AR-325 Text : 1: C8 Acid (PFOA) 13491 O-20, DF=lO 080103AR-325 10 Sm (Mn, 2x3) 0", i 9.11 61092 I 04-Aug-2003 17:17:2C LCYMWMS #6 MRM of 4 Channels ES413>369 3.65e5 Area ,00- "","","","","","","",""I A i 2.00 4.00 6.00 8.0 w 2: C6 Sulfonate (PFHS) 13491 O-20, DF=lO 080103AR-325 100- Sm (Mn, 2x3) 04-Aug-2003 17: 17:2 LC/MS/MS #6 o-~~`~,~`.`,~"`,`...,~~~~,".`,~~'~,'..','.~',~'~`,~`~~,`." 2.00 4.00 6.00 : C8 Sulfonate (PFOS) .3491 O-20, DF=lO 180103AFL325 IO Sm (Mn, 2x3) 8.00 10.00 9.24 65101 6 04-Aug-2003 17:17:2d LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.76e5 Area i-- Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.: L34910, Set No.:080103AR, 'W Ext.Date:08/01/03, Analyst:K.Risha Sample List: P:\Data\LCblSWS6\MasslyPx\Fluoroch~cal~.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\L~SMSb\~sslyPx\Pluoroch~cals.PRO\Met~B\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:03 2003 Page 50 Decatur BC BC 080103 Name: 080103AR-325 Text: 4: PFOSA IL3491 O-20, DE1 0 080103AR-325 loo- Sm (Mn, 2x3) %- 04-Aug-2003 17:17:26 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 3.12e5 Area Exygen Research, 3058 Research Drive, State College, PA 16801 ------------------------ --------- --------w------ Quantify San~le Report Study No.: L34910, Set No.:O00103A.R, Ext.Date:08/01/03, 'id Analyst:X.Risha Sample List: P:\Data\LCMSblS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O80103~ Last modified: Method: Last modified: Job Code: Tue Aug 05 07:24:43 2003 P:\Data\LWSMS6\Masslynx\Fluoroch~cals.P~O\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 51 Decatur BC BC 080103 Printed: 'Ibs Aug 05 07:32:01 2003 --- -------------------------- Name: 080103AR-326 Text: ------------- -------------___^_-__ : C8 Acid (PFOA) .3491 O-20 Rep, DF=lO )80103AR-326 IOO- Sm (Mn, 2x3) %- 9.12 _ 44037 04-Aug-2003 17:39:07 LC/MS/MS #6 MRM of 4 Channels ES413>369 2.64e5 Area 2.00 ~: C6 Sulfonate (PFHS) -3491 O-20 Rep, DF=lO 180103AR-326 1Och Sm (Mn, 2x3) 8 I I , ,v Time 6.00 8.00 10.00 04-Aug-2003 17:39:0 LCfMS/MS #6 %- 0 "~~,~~~`,`~~~,~"~I~"`,`~`~1~~~~1"'~I~'~'I'~~~l"~`~~"~ 2.00 4.00 6.00 : C8 Sulfonate (PFOS) -3491 O-20 Rep, DF=lO 180103AR326 10th Sm (Mn, 2x3) %- 8.00 9.24 10.00 04-Aug-2003 17:39:0+ LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.63e5 Area Wgen Research, 3058 Research Drive, State College, PA I.6801 Quantify Saalple Report study No.: L34910, Set No.: 080103JUi, Ext.Date:08/01/03, lur, Analyst:K.Riaha saup10 List: Last modified: Method: Last modified: P:\Data\LWSMS6\Masalynx\Fluorochemicals.PRO\S~leDB\O6OlO3~ !Pue Aug 05 07224~43 2003 P:\Data\L~SMS6\Masslypx\Fluoroch~cals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Page 52 Decatur BC BC 010103 Name: oao103AR-326 Text : 4: PFOSA L3491 O-20 Rep, DF=l 0 080103AFb326 lOO- Sm (Mn, 2x3) %- 04-Aug-2003 17:39:07 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498>78 2.62e5 Area 0 "","",`,","","","","","",l"`, I r I , I t Time 2.00 4.00 6.00 8.00 10.00 INygen Research, 3058 Research Drive, State College, PA 16801 00043.4 Quantify Sample Report Study No.: L34910, Set No.:O80103AR, ' '4 Ext.Date:08/01/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS6\Masslynx\Fluo~och~ca~s.PRO\S~leDB\O8OlO3~ Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\L(ZrlSblS6\bssl~\Fluoroch~cals.PRO\Met~B\Decatur Last modified: Sun Aug 03 07:11:59 2003 Job code: Page 53 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 -------------------------------- Name: 080103AR-327 Text : 1: C8 Acid (PFOA) I-3491 O-21, DF=lOO (180103AR-327 10 Sm (Mn, 2x3) 04-Aug-2003 18:00:4j LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 1016s 6.21e4 Area q,d 2: C6 Sulfonate (PFHS) IL3491 O-21, DF=lOO 080103Ak327 100- Sm (Mn, 2x3) %- Time 04-Aug-2003 18:00:47j LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 3.35e3 Area 3: ca Sulfonate (PFOS) L3491 O-21, DF=lOO 080103AR-327 Sm (Mn, 2x3) 04-Aug-2003 18:00:4? LCRvWMS #6 MRM of 4 Channels ES499 > 99 4.95e4 Area Time Ekygen Research, 3058 Research Drive, State College, PA 16801 00043.5 Quantify Sample Report Study No .:L34910, %d Set No.:O80103A?i, Ext.Date:08/01/03, Analyst:K.Risha SausQls List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~aslynx\Fluorocbemica !#.m Aug OS 07:24:43 2003 P:\Data\LCMSMS6\Massl~\Fluoroch~cals.PRO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Page 54 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 __~----------------------------~ ------------------- Name: 080103AR-327 Text : 4: PFOSA IL3491 O-21, DF=l 00 080103AR-327 Sm (Mn, 2x3) 04-Aug-2003 i&00:4: LCIMSNS #t MRM of 4 Channels ES498 > 7E 4.67eL Are2 Time J men Research, 3058 Research Drive, State College, PA 16801 ----."--- .__"__- --- Quantify Sample Report Study No. : L34910, Set No.:O80103AR, '14 &&.Date:08/01/03, Analyst:K.Rieha Sample List: P:\Data\LCbISMS6\Massl~\F~uoroch~cals.PRO\S~~eDB\OSOlO3~ Last modified: Method: Last modified: Job Code: Tue Aug 05 07:24:43 2003 P:\Data\L~SMS6\Masslynx\Fluorochemicals.PRO\Met~B\Decatur Sun Aug 03 07:11:59 2003 Page 55 Decatur BC BC 080103 Printed: -----m--e------ Tue Aug 05 07:32:01 2003 -------------------l_l-------ll------------- Name: 080103AR-328 Text : : C8 Acid (PFOA) .34910-21,DFdO )80103AR-328 10 Sm (Mn, 2x3) 9.16 9924( I 04-Aug-2003 18:22:28/ LCNWMS #6 MRM of 4 Channels ES413 > 369 5.73e5 Area 1 L Time 2.00 4.00 6.00 8.00 10.00 w 2: C6 Sulfonate (PFHS) [L34910-21, DF=lO 04-Aug-2003 18:22:2d 080103AB328 Sm (Mn, 2x3) LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.84e4 Area Time 10.00 04-Aug-2003 18:22:28! lOO- 9.28 %- Oxygen Research, 3058 Research Drive, State College, PA 16801 000419.7 ---_---_ ---_-------_ ----- ---------------- Quantify Sample Report Study No .:L34910, '4 Set No.:O80103A~, Ext.Date:08/01/03, Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorach~cals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07324343 2003 P:\Data\LCMSMS6\Masslynx\Fluoroch~cal8.?RO\~et~B\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug OS 07:32:01 2003 Name : 080103AR-328 Text: 4: PFOSA L3491 O-21, DF=l 0 080103AR-328 100- Sm (Mn, 2x3) %- Analyet:K.Risha -e---e--_ Page 56 Decatur BC BC 080103 04-Aug-2003 18:22:2d LC/MS/MS #6 9.87 78207 MRM of 4 Channels ES498 > 78 3.95e5 Area Exyoen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.: L34910, Set No.:080103AR, 'hd Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07:24:43 2003 P:\Data\LCMSMSS\Masslynx\Fluorochemicals.PRO\~et~R\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:.32:01 2003 Page 57 Decatur BC BC 080103 Name : 080103AR-329 Text : : CB Acid (PFOA) (CO72503-5,500 rig/L Standard )80103AR-329 10 Sm (Mn, 2x3) 3 9.15 21504E 04-Aug-2003 18:44:11] LC/MS/MS #6 MRM of 4 Channels ES413>369 1.26e6 Area 2.00 4.00 ,4 2: C6 Sulfonate XCO72503-5,500 (PFHS) rig/L Standard 080103AR-329 10 ] Sm (Mn, 2x3) % ,,",`,,,,"","`,,"`,,"`, 2.00 4.00 3: C8 Sulfonate (PFOS) IXCO72503-5, 500 rig/L Standard 080103AR-329 Sm (Mn, 2x3) 1000- "~`//"`,~`J~,"' `r ,,`,,"`,,' %- 2.00 4.00 6.00 8.00 10.00 8.99 _ 37183 04-Aug-2003 18:44:11 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.23e5 Area 1,,1 ,,,,,,/,,,, $ ,,,,,, I,,,(,, Time 6.00 8.00 10.00 I ,,,,,,,,, "19,,.,277,,q 04-Aug-2003 18:44:11 LC/MS/MS #6 MRM of 4 Channels ES- ,,,, y.f 6.00 8.bO 10.00 wgen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report study No.: L34910, Set No.:O80103AR, 'Id Rxt.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: P:\Data\LCMSMS6\~sslynx\FluorochemicalS.PRO\S~~eDB\O80103~ Tue Aug 05 07~124~43 2003 Method: Last modified: P:\Data\LCMSMS~6\Masslynx\Fluorochamica~s.PRO\MethD~\Decatur Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-329 Text: Page 58 Decatur BC BC 080103 X072503-5,500 rig/L Standard 180103AFk329 Sm (Mn. 2x31 04-Aug-2003 18:44:11 LCIMSIMS #6 MRM of 4 Channels ES- 498 > 78 I 4.48e5 Area A- Time Exyoen Research, 3058 Research Drive, State College, PA 16801 QQQ420 Quantify Sample Report Study No .:L34910, h@ set No.:O80103AR, Ext.Date:08/01/03, Sample List: P:\Data\LWSMS6\Masslynx\Fluorochemicale. Last modified: TLIS Aug 05 07:.24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\FluorachemicalsB\D~catur Last modified: Sun Aug 03 07:.11:59 2003 Job Code: Analyst:K.Risha Page 59 Decatur BC BC 080103 Printed: ----___ !l'ue Aug OS 07:32:01 2003 ------------_---------_-___ Name : 000103AR-330 Text : --s----p___ ---- ---- 1: C8 Acid (PFOA) KC072503-6,lOOO rig/L Standard 080103AR-330 10 %100, Sm (Mn, 2x3) 2.00 9.15 406254 " " I" " I" ''," " I 4.00 6.00 8.00 " L 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES413>369 2.39e6 Area Time 10.00 2: ~6 Sulfonate (PFHS) w XCO72503-6,lOOO rig/L Standard 080103AR-330 IOO- Sm (Mn, 2x3) ,,,`,,,,,,,,,,`,,,,,, 04-Aug-2003 19:05:5: LC/MS/MS #6 MRM of 4 Channels ES- 8.99 ::;`1 `,,,",,,`,' y%!f %- 0 ""I"","","" 2.00 4.00 6.00 8.00 10.00 3: C8 Sulfonate (PFOS) XCO72503-6,1000 rig/L Standard 180103AW330 10 9 Sm (Mn, 2x3) 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.57e5 Area 2.00 4.00 6.00 8 ."" I".L I Exygsn Research, 3058 Research Drive, State College, PA 16801 Time 2 000421 Quantify Saxqpls Report Study No.:L34910, b+' Set No .:080103AR, Ext.Date:08/01/03, Aaalyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\~sslynx\Fluorochemicals.PRO\S~leDB\O8OlO3~ Tue Aug 05 07::24:43 2003 P:\Data\LCMSMS6\Maeslynx\Fluoroch~cals.~RO\Met~B\Decatur Sun Aug 03 07::L1:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 60 Decatur BC BC 080103 Name: 080103JUi-330 Text : 4: PFOSA XCO72503-6,lOOO rig/L Standard 080103AR330 100- Sm (Mn, 2x3) %- 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 8.67e5 Area 10.00 , , , , . , Time Exygen Research, 3058 Research Drive, State College, PA 16801 800422 NA I34910 PFOS 499 -> 99 Decatur B&w's Creek RAW DATA REPORT Limit of Qumtitati~n: kjcctian Volume: MSTiX Sample Weight FIOJ Volume: Set No: AnnlYSC hruummt-rypc: Exbvtioa Date: AwJyzcd on: 081203A KuCn RidU LCMSMS % OWI M3 08113Ki3 Exygca m XC08 1103-O xco.91103-I XC081 103.2 Xcu8lO3-3 XC081 103.4 xcm31103.5 Xc081 103-6 MclhlDd WadI Reagent Blank Ru&nl Spk A Rsegenr Spk B L34910-11 SpkE L34910-I1 Spk B XC081 103-L XC081 103-2 Xc081 103-3 L34910. I1 w4910-11 Rep u4910-11 w4910-11 REp XC0611034 Xc081 103.5 xcO81103-6 spam 111 01 ml BC2 SED.06 BQ SED-06 BCZ SED-06 BQ SED-06 BQ SBD-06 BC2 SEII-& SUnpk RUII CC& No. es ORI203A.3001 0 cs OIil203A.3002 2.7 cs 081203A-3003 SO cs 081203A-MO4 100 cs 061203&3005 230 cs 09 1203A.3006 SO0 cs 081203A.3a)7 IWO C 081203A.3008 C 081203A.3W9 LCS 081203A-3010 LCS 081203A.3011 LF 081203A.3012 LF 081203A-3013 cs 061203A.3014 7.5 cs 081203A-3015 50 cs 081203A-3016 100 S 081203A.3017 S 081203A-3018 S 081203A.3019 S 08 1203A.3020 cs 081203A-3021 250 cs 0817D3A.3022 500 cs 081203A-3023 1000 halyle Rcfovay Pound (ppl) (%) a - (peak - - iuterccp~) I slope (amlyle found (ppt)-unllylc -c I DP found in conuol Xldlxf (PP0 (PPl)] I loo .hdytc Farad (ppb) = [.w.lyte hnd (ppt) x volume uuacti (0.04 L)I I sample wei& (S n) Analytc Found (ppb) dry weight = malyw found (ppb) x (1Wa I t-1 solid, ("k)) C-3 = Calibntiooruuxhl c = cwtrol lpmplc s -Sample LF 3 Lab fortifud FF = Picld fatihed LCS I Lnborwry ramp10 sampk Coauol Spike 0 909 IS% 3803 9700 19165 39020 0 0 ND 1963 49.2 21166 533 8541 21swI 91234 * 954 2208 4213 4378 1100&l 493s 124aoa 422% l 48356 I 11039 20668 39291 98 107 105 880.00 60.41 1460 99240 60.41 1640 60.4 I 60.41 CK . Ckck SMprd ND - Noc&kwedrRupumebcnv~0and~ppr NQ . Not quantifiable = Rcrponss bccwcco U ppt and LOQ (SO ppr) *Dilution wzu for PFOSA. Spawn Study No: Exygcn Study No: An+lC Ions Monitored: Site: NA L34910 FOSA 498 -,-a Dscatur B&a's Creek RAW DATA REPORT Limit of Qwmiutioo: Lnjsction Volume: Mabix: Smlpk Weight: Final Volume: $0 PPt 1SpL Soil 5.0 g 5.0 mL Set No: AMlYSC lmtmmat Extrsction Andy24 Type: Date: on: 081203A Klrm Risha LCMSMS #6 OWl2'03 OS/l 3:03 Wsm ID xcos I 103-o xcoEIlo3-I XC081 103-2 xc081 103.3 XC081 103-4 XCOBI 103-S XCOB 1103-5 Mcthnnol Wash Reagent Blaok Reagent Spk A Rupent Spk B L349 LO-1 I Spk E L349 IO-1 I Spk E w XCOBI 103-I XC08 I 103-2 XC08 1103.3 L34910-11 L34910.I I Rep L34910-II L34910-II Rep XC081 103-I XC081 103-s XC081 103-6 Sponsor ID I). 0~ Il. EC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 SED-06 Sample Code cs cs CS cs CS CS cs C C LCS LCS LF LF CS CS CS S S S S cs cs cs Run NO. 081203A33001 OSI203A-3002 081203A.3W3 OS I203A.3004 081203A.3OOS 081203A.3006 OBl203A-3007 081203A-3038 081203A-3009 081203A-3010 081203A-3011 081203A-3012 081203A-3013 0131203A-3014 081203A-3015 081203A-3016 081203A-3017 081203A-3018 081203A.3019 081203A.3020 081203A-3021 081203A-3022 081203A-3023 Anatyte Raovy Found @pt) -(PC& (X) - ww . iotacspt) Imalytc found J slope x DP (ppt)-wMyl. found in coatrol amount added @pt) (opt)l x IO0 std. COW. @pt) 0 23 SO loo 250 500 loo0 Dilution Factor I 1 I IOW 100 25 SO loo 1000 loo0 loo 100 250 so0 IO00 Peak Area 0 3s47 7692 lSS22 39080 7390s 145023 0 0 725s 72614 1141s 122331 4230 8197 16248 I446 1737 13834 l6OlS 41122 78848 149443 AJwe Found (ppt) Amourit Added (ppt) Recovery (%) AaPlytC Found @pb) ND 4J.S 50 91 481 SW 96 * IOWQO 812W IooooO n l . 8930 71.44 IWO0 83.20 2gmdad Cwp totempt Slope Cocf.OfDct.= : Line= (I/x - 434.455 = 150.037 0.998129 weighted) TOtd SOlidS (K) 60.41 60.41 60.41 60.41 hnrlyte An~lyte Found @pb) = [analyte found (ppt) x volume cxbwtcd (0.04 L)]! prmple weight (3 g) Pound @pb) dry weight - uralyrc found (ppb) x (I 00% I total solids (%)) CS = Wibntion c - Contxol s - Slmpk rtmdard umple LF - hb fortified FF - Field foltificd LCS - Laborwtory wnple sample Contxol Spike CK * Cheek Standud ND - Not dctated NQ = Not qwtitiablc - Response bctwcen 0 md ZS ppt = Rerpoose between 25 ppt md LOQ (SO ppt) *Dilution was for PFOS Spreadsheet prepared by: $$ , 08/29(03 A&t0 Fwnd (Ppb) Dry Weight 118 138 000&?4 E nTM EARCH 3058 Research Drive State College, PA 16801 Phone: 8 14-272- 1039 Fax: 814-231-1580 \J Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34,9 10 Matrix: &iJ ere removed from refrig All samples were weighed on balance No. 2 Time @m Date Initials m After wei hing samples were returned to re t-i erator No. ,?2 Time lLfzz6 Date &$& Initials L&E Comments: ZOOpL of 250 mghL sodium thiosulfate WII added to all samplesbefore spiking. Initials/Date: Analysis Summary: Data Set *1203A Data Set: - Data Set: + Initials/Date: Initials/Date: Initials/Date: Set extraction/analysis data verified by. . - 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 SAMPLE EXTRACTION ANIl ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: MATRIX: L34910 m METHOD: ANALYTES: ExM-023-014 Is PFHS. PFOS. PFOA and PFOSA PROTOCOL NUMBER: & *Client ID na na na BC2 SED-06 I BC2 SED06 BC2 SED-06 Exygen KD STEP STEP STEP STEP STEP STEP Dilutions STEP Dilutions STEP 1 2 3 4 5 6 WJmL) 7 (mUmL) 8 Reagent Blank I I I I I I 1 Reagent Spk A , f Reagent Spk B 1 L34910-11 Spk E 1 1 I I I &.l/;rLl/o 1 : 1 L34910-11 1\ ! I! \ 1 j ! ! I( ,/y(,o-yo , P).fd II - L34910-11 Rep \L \L w * JI J, ~~~v\*~@~p \v Reagents/ Materials LOl# Mabaa cl8 SPE 2-b w3 ILp7B2 NA GTlwaslwsa-crodisc I I STEP 4: Fiiter through glass acrodise STEP 5: SPE column clean up (omitting 40% wash) STEP 6: Final volume. fo 5 mL collected in 15 mL polypropolenc tubes STEP 7: LCXVWMS analysis STEP 8: LC/MS/MS reanalysis. *Initials and date under each step indicates the personnel that performed this step, $$ Method of Analysis for the Determination of PerfIuorooctauesulfonate (PFOS) and Pentadecafluorcoctanoic Acid (PFOA) in Soil COMMENTS: Final extracts stored in refrigerator .32 Initials: aDafez * July 19,2001/4 n04 i 30.58 Research IXve c Phone: 814-272-1039 AESCARCH State College, PA 16801 Fax: 814-231-1580 Protocol No.: None Method No.: s PREPARATION OF EXTRACTED CALIBRATION Exygen Study No.: Am&es: m PEfls, PFAS. PFOS. PFQd STANDARDS Matrix: Sample Vol: T~DC I Water" 4&1& Vertical arrows in a column indicate identical vafues. **This must be a unique number. Use this system: Extracted Calibration Sofn ID Samples removed fro-r I lkezer # -a Time: mm 40 mL of each sample measured using a ,p rnL graduated cylinder. After measuring, samples returned t-9 / freezer # Time: 6% Samples fortified: Initials/Date: / Eall/!V SPE clean-up (omitting 40% Wash): Initials/Date: ZE I Fiial ~olumc adjusted to 5 mL: Extracts placed in refrigetator # XL Initials/Date: PE I s Initials/Date: &G / I QG+ #: XCMSfDDl'Y-0,1,2,3. InitiaWDate: InitialsAIate: Initials/Date: etc. CEEl /a 05 1 fe / ' s STANDARD EXPIRATION Comments: *This type I water has been filtered through a hypercarb filter J$ Method of Analysis for the Determination of Petfluorooctaoe mlfooatc (PFOS), Pcrfluorocctane sulfonylamide (PFOSA). and Perfluorooctanoatc (poti) DATE! h Water 8f25/03 Q July la,2oolM Masslynx - Sample list Sample List: C:\MASSLYNX\Fluoroch Printed: Wed Aug 13 09:36:59 2003 Is,PRO\SampleD8\081203A Decatur EC.SPL --. Vial File Name LIMS ID Client ID Sample Description Matrix Sample Type Cone @g/L) Cone B ConcC Test ID DF I 08 1203A-3001 -- -_- 2 : 08 1203A-3002 -- _- 3 3 08 1203A-3003 -- -- 4 4 08 1203A-3004 -- ..- 5 5 081203A-3005 -- _- 6 6 08 1203A-3006 -- -- 08 1203A-3007 -- -- s' 9'2 08 1203A-3008 -- -- 9 11 08 1203A-3009 -- - 081203A-3n10 -- -- :: :; 081203A-3011 -- -- 12 14 081203A-3012 -- _I 13 I5 081203A-3013 -- - 2 081203A-3014 -- -- 2 3 081203A-3015 -- - 16 4 081203A-3016 -- - 17 16 081203A-3017 - - da 17 081203A-3018 -- - 19 18 081203A-3019 - - 20 19 081203A-3020 -- - 21 5 081203A-3021 - - 22 6 081203A-3022 - - 23 7 081203A-3023 - - XC081 103-O. 0 ng!L Standard --- XC081 103-I,25 nglL Standard --- XC081 103-2.50 ngtL Standard --- XC081 103-3. 100 rig/L Standard --_ XCO81103-4,250 rig/L Standard -- XC081 103-5,500 rig/L Standard - XC081 103-6, 1000 rig/L Standard -_ Methanol Wash -_ Reagent Blank _-- Reagent Spk A, %I nglL -_- Reagent Spk B, 500 nglL _-- L34920-11 Spk E, 100000 nglL. OF=1000 --- L34910-11 Spk E. 100000 rig/L, DF=lOO --- XCO81103-1.25 nglL Standard -- XC081 103-2,50 ngR Standard _-- XC081 103-3, 100 rig/L Standard -- L34910-11,0F=1000 -- L3491 O-l 1 Rep, DF=lOOO - L34910-II. DF=lOO -- L3491 O-1 I Rep, DF=lOO -- XC081 103-4,250 rig/L Standard -- XC087 103-5.500 rig/L Standard _- XC081 103-6, 1000 nglL Standard -- Standard Standard Standard Standard Standard Standard Standard Blank Blank SC :: gt%dard Standard Standard Analy-te Analyte Analyte Analyte x5 50 100 250 500 1000 _-- 50 500 100000 100000 2 100 --- 250 500 1000 -- - -- -- -_ -- -_ -- -- c-- -- -- -- --- -- -- -- -_- -- - -- -- -- - -_ --_ - --- -- - -- - -- - -- - -- - -_ - - - 0 0 : 0 1 1 8 1 1 00 1 0 1 0 1 n i 0" 1 0 1000 0 100 I : I 1 a0 1000 0 1000 0 100 0 loo 0 I 0 1 0 1 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroch Printed: Wed Aug 13 093659 2003 als.PRO\SampteDB\O81203A bf$!jbs Decatur BCSPL MS Method HPLC Method MS Tune File Inj.Volume 1 C6 C8 SULF C8 ACID PFOSA 2 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA : C6 C8 SULF C8 ACID PFOSA 5 C6 C8 SULF C8 ACID PFOSA 6 C6 C8 SULF C8 ACID PFOSA 7 C6 C8 SULF C8 ACID PFOSA 8 C6 C8 SW-F C8 ACID PFOSA 9 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF 26 ACiD PFOSA :I: C6 C8 SULF C8 ACID PFOSA 12 C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA :1 C6 C8 SULF C8 AClD PFOSA C6 C8 SULF C8 ACID PFOSA :i C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA :3 C6 C8 SULF CB ACID PFOSA 19 C6 C8 SULF C8 ACID PFOSA 20 C6 C8 SULF CB ACID PFOSA 21 C6 C8 SULF C8 AClD PFOSA 22 C6 C8 SULF C8 ACID PFOSA 23 C6 C8 SULF C8 ACID PFOSA pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water PfbS Wi3t8r pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water Fluorochems 15 Fluorochems Fluorochems :z Fluomchems 15 Fluorochems Fluorochems ;z Fluorochems 15 Fluorochems 15 Fluorochems 15 Fiuorochems i5 Fluorochems 15 Fluorochems 15 Fluorochems Fiuorochems :; Fluorochems Fluorochems :z Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 Fluorochems 15 ExVgen STUDY NO; !-SW 10 .' . I Page 2 Page Position: (2, 1) LUMSI'MS SYSTEM AND OPERATING CONDITIONS SDonsor Protocol No: If?& Exvg;en Studv No: L34910 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: COMPAQ Professional Workstation AK?00 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HT'LC Equipment: .Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC coh.uM: Genesis C-8,5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 74A) (JONJZSCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 12mM Ammonium Acetate in Type I Water Methanol Analyst: IKaren Risha IExygen Research 3058 Research Drive, State College, PA 16801 I?hone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the lmasslynx software program. The pages contain the instrument settings used fbr the analysis of this data set. All Handwritten Peak D's by: glp$6~~3 Scanning Method Report lul, Method: Last Modified: C:\MASSLYNX\E-LUOROCHECALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 Page 1 C8 SULF C8 ACID PFOSA Printed: Solvent Wed Aug 13 09:37:33 2003 Delay ( mins ) : a.00 N5]1310 v ' halog Function Channel : 1 4 : Unused MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Sets ) : 0.03 Span ( Daltons ) : 0.00 Start Time ( Mins ) : 0.00 End Time ( Mins ) : 12.00 Repeats : 1 Channel Parent Daughter Dwell (Sets) Co11 Energy (eV) Cone ( V ) 1 399.00 80.00 0.20 35 50 2 413.00 369.00 0.20 10 10 3 498.00 18.00 0.20 30 50 4 499.00 99.00 0.20 40 30 Method Report Method Pile: Last Modified: C:\mSSLYNX\FLUOROCHEMICALS.PRO\ACQUUEi\pfbs Wednesday, August 13, 2003 09:25:46 Printed: 'ad Wednesday, August 13, 2003 09:37:56 HP1100 LC Pump Initial Conditions Solvents A% 90.0 8% 10.0 C% 0.0 D% 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Oven Temperature Right(OC) 0.300 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time A% B!k C% 0.00 90.0 10 .o 0.0 2.00 90.0 10.0 0.0 5.00 10.0 90.0 0.0 9.00 10.0 90 .o 0.0 9.50 0.0 100.0 0.0 14.00 0.0 1OO"O 0.0 14.50 90.0 10.0 0.0 20.00 90.0 10.0 0.0 D% Flow 0.0 0.300 0.0 0.300 0.0 0.300 0.0 0.300 0.0 0.300 0.0 0.300 0.0 0.300 0.0 0.300 '*r'HPllOO LC Pump External Event Timetable The Timetable contains 6 entries which Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contact1 Off On Off Off Off Off are : Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(@) Vial Number Conditions 290.0 200 0.50 20.00 15.0 47 Page 1 water Pressure 400 400 400 400 400 400 400 400 _ .I--t.. .~,Y_ -_... .- Tuning Method Report '4 Method: C:\MASSLYNX\E~UOROCHEMXCALS.PRO\ACQUD~~\E'LUOROCHEMS Printed: Wed Aug 13 09:37:50 2003 Page 1 . \d Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set Rdbk 3.00 -2.93 20 -42 0.0 0.0 0.0 100 100 300 299 Rdbk OFF 3.5e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set 14.0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650 Rdbk 132.1 755.7 Rdbk 26 38 29 -648 _--_" __II__ --IIxI--" --a-- -------------___l_------ e-----w__ Quantify Calibration Report Study No.:L34910, Set No .:081203A, lWt.Date:08/12/03, Analyst:R.Risha 14 Calibration: P:\Data\LCM~S6\Wasslynx\Bluorochemicals.PRO\~~eDB\O8l2O3A Last modified: Man Aug la 10:47:18 2003 Printed: MOn AUg 18 10:50:24 2003 m-----m-- ------------e--- ------------ 1C>ompound 1 name: C8 Sulfonate (PFOS) C;oefficient of Determination: 0.998540 C:alibration curve: 39.6727 * x + 10.4732 FResponse type: External Std, Area C;urve type: Linear, Origin: Exclude, Weighting: 3.97e4- l/x, Axis trans: None --A--- Page 1 Decatur BC Response 1I-S0 ( 3 ,`I ",""2/,"`0I 0.0 400.0 I'# ~l'~"l'+~n 600.0 I - 3 ~`I-8~~00.0 Oxygen Research, 3058 Research Drive, State College, PA 16801 r I ,' (`1 rig/L 1000.0 . ..- -- ..- __.---_1_-.-.-- . -- __---_-... _---- -- I_-------c-----I_--__l__l____ ---- --------_-__ Quantify Calibration Report Study No.:L34910, Set No .:081203X, Fzt.Date:08/12/03, Analyst:K.Risha Calibration: Last modified: Printed: ----------- P:\Data\LCblSMSS\Masslynx\Fluoroch~ca~s.PRO\~~eDB\O81203A Mon Aug 18 10:47:18 2003 Mon Aug 18 10:50:24 2003 -----we -____---- -------------___ :ompound 2 name: PFOSA :oefficient of Determination: 0.9981213 ;alibration curve: 150.037 * x + 434.455 lesponse type: External Std, Area h-ve type: Linear, Origin: Exclude, Weighting: 1.50eZ I- l/x, Axis trans: None Page 2 Decatur RC Response 0,' 7 r 0 I' " `I ' r 11 I f 3 I z ' 8 8 11 0.0 200.0 400.0 e 5 I""(' 600.0 #`II", `I,`, 800.0 Exygen Research, 3058 Research Drive, State College, PA 16801 / I rig/L 1000.0 -- -_---- ----------c_---- ----- -----------------____ Quantify Saa~~~le Report Study No.: L34910, set NO .:081203A, Ext.Dats:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\M1M~S6\Masslynx\Fluoroch~cals.PRO\S~leDB\O81203A Man Aug 18 10:47:09 2003 P:\Data\LCHSMS6\~sslynx\Fluorochemicals.P~O\Met~B\PFOS Mon Aug 11 09:49:08 2003 Yon Aug 18 10:50:26 2003 Page I Decatur BC and PFOSA 081103 Name : 081203A-3001 Text: 1: CB Sulfonate (PFOS) XC081 103-0,O rig/L Standard 081203A-3001 Sm (Mn, 2x3) 13-Aug-2003 14:43:39 LCYMSNS #6 d MRM of 4 Channels ES- 2.00 4.00 6.00 8.00 10.00 v 2: PFOSA XC081 103-0,O rig/L Standard Aug-2003 14:43:3 081203A-3001 Sm (Mn, 2x3) h;lRM of 4 Channels ES- Exygen Research, 3058 Research Driva, State College, PA 16801 A----- ----_- --------_ -----------_1---_____-_-___ Quantify Sample Report Study No.:L34910, Sat No .:081203A, Sxt.Date:08/12/03, Analyst:R.Riaha sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~ca~s.PRO\S~leDB\O8l2O3A Man Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFoS Mon Aug 11 09:49:08 2003 Printed: Hon Aug 18 10:50:26 2003 Page 2 Decatur BC and PFOSA 081103 Name: 081203A-3002 Text : 1: C8 Sulfonate (PFOS) XC081 103-1,25 rig/L Standard 081203A-3002 lOO- Sm (Mn, 2x3) 13-Augc2003 15:05:11 LCIMSIMS #6 MRM of 4 Channels ES- %- O~.,,,,,,,`~,,,,,,,,,..,,,,.,`.,.,,,'.,,,',,,',,,,l,,,,,,, 2.00 4.00 6.00 8.00 10.00 v 2: PFOSA XC081 103-1,25 rig/L Standard 081203A-3002 Sm (Mn, 2x3) 13-Aug-2003 15:05:11 LC/MS/MS #6 MRM of 4 Channels ES498 > 78 1.79e4 Area Time 2.00 4.00 6.00 8.00 10.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 ----P --------------e--w- ----- Quantify Sax&e Report Study No .:L34910, Set No.:O81203A, Ext.Dats:08/12/03, Analyst:K.Riaha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluarochemicals.PRO\S~leDB\O9l2O3~ Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\bIethDB\PFOS Man Aug 11 09:49:08 2003 Printed: Man Aug 18 10:50:26 2003 ----- Page 3 Decatur BC and PFOSA 081103 Name: OB1203A-3003 Text: 1: C8 Sulfonate (PFOS) XC081 103-2,50 rig/L Standard 081203A-3003 lOO- Sm (Mn, 2x3) %- 9.35 1 89tj7 13-Aug-2003 15:26:51 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1 .OOe4 Area 1 01--,,,~,~,,,,,,,,,,,,,.,,,~,,,,,,,,,~,,,,~Time 2.00 4.00 6.00 8.00 10.00 2: PFOSA XC081 103-2,50 rig/L Standard 081203A-3003 10 Sm (Mn, 2x3) % 13-Aug-2003 15:26:51 LC/MS/MS #E MRM of 4 Channels ES- 9.9f 498>7E 769: 3.73e4 Area i Time Exygen Research, 3058 Research Drive, State College, PA 16801 000439 --------------m----m- -_---- ------ ------ Quantify Sample Report Study No.: L349l.0, Set No. : 081203A, Ext.Date:O8/12/03, Analyst:K.Risha Cd Sample List: P:\Data\LCMSMS6\~sslynx\Fluorochemical8.PRO\S~leDB\O8l2O3A Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCIGMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Last modified: Man Aug 11 09:49:08 2003 Job Code: Printed: Non Aug 18 10:50:26 2003 Page 4 Decatur BC and PFOSA 081103 Name: 081203A-3004 Text : 1: C8 Sulfonate XC081 103-3,100 (PFOS) rig/L Standard 081203A-3004 10 % 1 Sm (Mn, 2x3) 0 "","","l',"","","",""l""I""I' I 2.00 4.00 6.00 r2: PFOSA `url XC081 103-3, 100 rig/L Standard 081203A-3004 10 Sm (Mn, 2x3) I%%.% 13-Aug-2003 15:48:3 9.33 3803 2.18e4 Area - -- Time 8.00 10.00 l3-Aug-2003 l5:48:30 LC/MS/MS #6 MRM of 4 Channels ES- 9.95 15522 498 > 78 7.50e4 Area I b Time / 00 Exygen Research, 3058 Research Drive, State College, PA 16801 000440 --_e-- ---------------_----~ -p-w-- --__-__-- Quantify Sample Report Study No.: L34910, Set No .:081203A, `d Ext.Date:08/12/03, Analyst:K.Risha Sample List: P:\Data\L~SMS6\b~sl~\Fluoroch~cal~.PRO\S~leDB\Oal2o3A Last modified: Moon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluoroch~cal=.PRO\Met~B\P~OS Last modified: Mon Aug 11 09:49:08 2003 Job Code: Page 5 Decatur BC and PFOSA 081103 Printed: MOn Aug 18 10:50:26 2003 --------------------.-----~-------------- Name : 081203A-3005 Text : I--------_------_w_ 1: C8 Sulfonate XC081 103-4,250 (PFOS) rig/L Standard 08 1203A-3005 Sm (Mn, 2x3) 13-Aug--2003 16:10:151 LCNShlS'#6 MRM of 4 Channels ES- 9.35 499 > 99 5.54e4 Area 2: PFOSA `W IXCO81103-4,250 rig/L Standard 081203A-3005 Sm (Mn, 2x3) %- 13-Aug-2003 16:iO:lfjl LC/MS/MS #6 MRM of 4 Channels ES- 390.9850-- 498 > 78 1.88e5 Area Oxygen Research, 3058 Research Drive, State College, PA 16801 -----------------------~ Quantify Saarple Report Study No .:L34910, Set No .:081203A, Ext.Date:O8/12/03, Nd Sample List: P:\Data\L~~S6\Wlsslynx\Fluoroch~ca~s.PRO\S~leDB\O81203A Last modified: Man Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masalynx\Fluorocharnica~s.PRO\MethDB\PFOS Last modified: Man Aug 11 09:49:08 2003 Job Code: Printed : Man Aug 18 10:50:26 2003 Name: 0812031-3006 Text : 1: C8 Sulfonate XC081 103~5,500 (PFOS) rig/L Standard 081203A-3006 Sm (Mn, 2x3) v--w------ Analyst:K.Rirha Page 6 Decatur RC and PFOSA 081103 13-Aug-2003 16:32:0 2.00 4.00 6.00 8.00 2: PFOSA XCO81103-5,500 rig/L Standard 081203A-3006 lOO- Sm (Mn, 2x3) %- 130Aug-2003 16:32:0tj LC/MS/MS #6 MRM of 4 Channels ES- 9.95 498 > 78 3.53e5 Area 0 ~ll`,,~~~,",~,~.`~,,~,~,,,-~,"~~/~"~,~"r, , I I 1 Time 2.00 4.00 6.00 8.00 10.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 ------------------------- ----------_l__ Quantify Sample Report Study No.:L34910, Set No .:081203A, Ext.Date:08/12/03, Analyst:K.Riaha Saarple List: Last modified: Method: Last modified: Job Code: P:\Data\LMSMS6\Massl~\Fluo~ochamicals.PRO\S~laDB\O8l2O3A Man Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Man Aug 11 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 __-__-___~~---~-~-~----~--____-_--~~~~~~-~-~~~-----~~ Name: 081203A-3007 Text : 1: C8 Sulfonate (PFOS) XC081 103-6, 1000 rig/L Standard 081203A-3007 100- Sm (Mn, 2x3) ,1,,1 [,,,,(, 9.33 ~~~,,Lr~,,,3~~~~ %- ----- Page 7 Decatur BC and PFOSA 081103 ----------__ 13-Aug-2003 16:53:41 LCIMSIMS #6 MRM of 4 Channels ES- 0 "","","","" 2.00 4.00 6.00 8.00 10.00 2: PFOSA XC081 103-6,lOOO rig/L Standard 081203A-3007 100- Sm (Mn, 2x3) %- 13-Aug-2003 16:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 :, 78 1 45023T 6.91e5 Area * I I a , I a - Time 6.00 8.00 10.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 -- ----- ___---l-l__-- --- Quantify Sample Report Study No .:L34910, Set No.:081203A, Ea&.Date:08/12/03, Analyst:K.Risha Sam&Jle List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Wasslynx\Fluoroc~~cals.PRO\S~leDB\O8l2O3A Man Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem.icals.PRO\MethDB\PFOS Mon Aug 11 09:49:08 2003 Printed: -___-_-___--_- Mon Aug -__- 18 10:50:26 ------__-----I--------- 2003 Name: 081203A-3008 Text : 1: C8 Sulfonate Methanol Wash (PFOS) 081203A-3008 Sm (Mn, 2x3) --m--- Page 8 Decatur BC and PFOSA 081103 -------m---e 13-Aug-2003 17:15:22 LC/MS/MS #6 MRM of 4 Channels ES10.47 11.23 4gg>gg 944 2: PFOSA Methanol Wash 081203A-3008 Sm (Mn, 2x3) I v - 1+Aug-2003 17:15:22/ LCiMSiMS #6 MRM of 4 Channels ES- 9;\96 498 > 76 I 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0004"-4 Quantify Sample Report Study No.: L34910, Set No.: 081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LQISMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8~2O3A Mon Aug 18 10:47:09 2003 P:\Data\LCWSMIS6\Massl~\Fluoroch~cals.PRO\Met~B\PFOS Mon Aug 11 09:49:08 2003 Printed: Man Aug 18 10:50:26 2003 Page 9 Decatur BC and PFOSA 081103 Name: 081203A-3009 Text : 1: C8 Sulfonate Reagent Blank (PFOS) 081203A-3009 Sm (Mn, 2x3) 13-Aug-2003 17:36:58 LC/MS/MS #6 MRM of 4 Channels ES- c Time 2.00 4.00 6.00 8.00 10.00 2: PFOSA 0 ~~~~,11~1,11~1/~~11,II..,II,I,III.,~III,,III(,,,,,,,,,,,,/, 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 om4n5 Quantify SangAe Report Study No.: L34910, Set No.: 081203A, Ext.Date:OI3/12/03, Salnple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\blasSl~\Fluorocbemicals.PRO\S~leDB\O8l2O3A Man Aug la 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MetbDB\PFOS Mon Aug 11 09:49:08 2003 Printed: MOA Aug 18 10:50:26 2003 Nm: 081203A-3010 Text : Analyst:K.Risha Page 10 Decatur BC and PFOSA 081103 2: PFOSA Reagent Spk A, 50 rig/L 081203A-3010 10 ,_- Sm (Mn, 2x3) % 13-Aug-2003 17:58:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 3.57e4 Area Time 2.00 4.00 6.00 8.00 10.00 Oxygen Research, 3058 Research Drive, State College, PA 16801 -- w-4---__I v-----e-----_-_ ---------- Quantify Sarqple Report Study No.: L34910, Set No .:081203A, Ext.Date:O8/12/03, Analyst:K.Risha Page 11 S~lS List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\SampleDB\O81203A Man Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\FluorochemicalB\PFOS Man Aug 11 09:49:08 2003 Decatur BC and PFOSA 081103 Printed: Won Aug 18 .X0:50:26 2003 -- -----------__------~------------------- Name: 081203A-3011 Text : -v---4----_____ 1: C8 Sulfonate ; (PFOS) 081203A-3011 10 Sm (Mn, 2x3) 9.36 21166 13-Aug-2003 18:20:23/ LC/MS/MS #6 MRM of 4 Channels ES499 199 1.12e5 Area w 2: PFOSA Reagent Spk B, 500 rig/L 081203A-3011 100- Sm (Mn, 2x3) %- I Time 1%Aug-2003 18:20:23 LC/MS/MS #6 MRM of 4 Channels ES- 9.97 498 > 78 3.5le5 Area I ' ' Time Exygen Research, 3058 Research Drive, State College, PA 16801 0004a7 -------- ---- ---- -- Quantify Sasqqle Report Study No.: L34910, Set No .:083203A, bJ Ext.Date:08/12/03, Analyst:K.Riaha Samiple List: ~:\Data\~~SMS6\Masslynx\Fluoroch~cals.PRO\S~leDB\O8l2O3A Last modified: MOP Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\MetbDB\PFOS Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 ---a-__ Page 12 Decatur BC and PFOSA 081103 Name : 081203A-3012 Text : 1: C8 Sulfonate (PFOS) ,L34910-11 Spk E, 100000 rig/L, DF=lOOO `081203A-3012 Sm (Mn, 2x3) 13-Aug-2003 18:42:04 LC/MS/MS #6 MRM of, 4 Channels ES499 > 99 4.55e4 Area 2.00 4.00 6.00 u ~3~~~~~ 1 Spk E, 100000 rig/L, DF=lOOO 081203A-3012 lOO- Sm (Mn, 2x3) %- Time 8.00 10.00 13-Aug-2003 18:42:04 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 11415 5.23e4 Area Oxygen Research, 3058 Research Drive, State College, pA 16801 --- -----_l_ --------_----l_---l-------- Quantify Sas@e Report Study No .:L34910, Sat No.:081203A, '4 Ext.Date:08/12/03, Analyst:X.Risha Sample List: P:\Data\LCEISMS6\Nasslynx\Fluaroch~cals.PRO\S~leDB\O8l2O3A Last modified: MOP Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\MasslyPx\Fluoroche.micals.PRO\MeithDB\PFOS Last modified: Man Aug 11 09:49:08 2003 Job Code: Printed: Man Aug 18 10:50:26 2003 ---e-e- Page 13 Decatur BC and PFOSA 081103 Naxm: 0812031-3013 Text : L: C8 Sulfonate (PF0.S) L34910-11 Spk E, 100000 rig/L, DF=lOO 081203A-3013 10 Sm (Mn, 2x3) % " 2.00 4.00 6.00 13-Aug-2003 19:03:46 LC/MS/MS #6 MRM of 4 Channels ES- 9.36 499 > 99 91234 4.77e5 Area 8.00 : PFQSA -34910-l 1 Spk E, 100000 rig/L, DF=lOO 381203A-3013 10 7 -1 % Sm (,Mn. . 2x3)a i ~`,",,,,,`,`,",`,,`,,,,,,"`,,~`,',,"'I,",I',, 2.00 4.-00 6.00 13-A~2003 19:03:4C LC/MS/MS #6 MRM of 4 Channels ES- 9.98 12233 I 498 > 78 5.76e5 Area I 8.00 1 0.00 Time - Eaqgen Research, 3058 Reseazch Drive, State College, PA 16801 ,_.-,_ ...-_".._-.-l*-l~.l-.,-.- 111-- ------_I_ stucly NO .:L34910, Set No.:O81203A, b Ext.Date:O8/12/03, Analyst:K.Risha Sample List: P:\Data\LCblSMS6\Masslynx\Fluoroch~cals.PRO\S~ieDB\O81203A Last modified: MOA Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochexkala.PRO\MathDB\PFOS Last modified: MOA Aug 11 09:49:08 2003 Job Code: Printed: MOA Aug 18 10:50:26 2003 ------ e--------------_---____c_ ---- Name: 0812031-3014 Text : 1: C8 Sulfonate (PFOS) XC081 103-l) 25 rig/L Standard 081203A-3014 100- Sm (Mn, 2x3) --- Pags 14 Decatur BC and PFOSA 081103 ------- %- n 0 , I, ,,, , ,,, , , , t ,, , , , , , , , , , , St ,a I r II 2.00 4.00 6.00 ,11311 2: PFOSA XC081 103-1,25 rig/L Standard 081203A-3014 100-l Sm (Mn, 2x3) I I I II t / 8.00 I, I I a I, r I I ,, , . I I Time 10.00 13-Aug-2003 19:25:2 LCIMSIMS #6 %- -gem Research, 3058 Research Drive, State College, PA 16801 -_I_-_--_-_-----__----~---_-_c_------------ Quantify Sample Report Study No.: L34910, Set No.: 081203A, Ext.Date:09/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L~SMS6\Masslynx\FluoroCh~ca~s.PRO\S~leDB\O91203A Man Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\Met~B\PFOS Mon Aug 11 09:49:08 2003 Printed: Man Aug la 10:50:26 2003 -- Page 15 Decatur BC and PFOSA 081103 Name: 0812031-301.5 Text : L: C8 Sulfonate (PFOS) XC081 103-2,50 rig/L Standard 081203A-3015 10 Sm (Mn, 2x3) 13-Aug-2003 19:47:12 LC/MS/MS #6 MRM of 4 Channels ES- 9.36 499 > 99 2208 1.24e4 Area " 2: PFOSA XC081 103-2,50 rig/L Standard 081203A-3015 Sm (Mn, 2x3) 1__;_ Time 13-Aug-2003 19:47:12 LC/MS/MS #6 MRM of 4 Channels ES498 > 78 3.75e4 Area Time Oxygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.: L34910, Set No.:081203A, F.xt.Dats:08/12/03, Analyst:K.Risha 'Iled Sample List: P:\Data\LCMSMS6\Masslyax\Fluorochemicals~eDB\O81203A Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCbiSMS6\Masslynx\Fluorochemicals.PRO\Met~B\PFOS Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: _--- Mon Aug --_--I___-____--I----T----------------_--I 18 10:50:26 2003 Name : 081203A-3016 Text : 1: C8 Sulfonate XC081 103-3,100 (PFOS) rig/L Standard 081203A-3016 10 Sm (Mn, 2x3) 9.36 421: I1- Page 16 Decatur BC and PFOSA 081103 --- 13-Aug-2003 20:08:511 LIZ/MS/MS #6 MRM of 4 Channels ES499 > 99 2.30e4 Area 'r, 2: PFOSA XC081 103-3, 100 rig/L Standard 081203A-3016 lOO- Sm (Mn, 2x3) %- Time 10.00 13-Aug-2003 20:08:51 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 7.75e4 Area I 10.00 I , I r I I Time Exygen Research, 3058 Research Drive, State College, PA 16801 000452 -----me--- ----___- ---_----- Quantify Saq~le Report Study No.:L34910, Set No.: 081203A, Ext.Date:08/12/03, Analyst:K.Risha v Sample List: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~~leDB\O8l2O3A Last modified: Man Aug 18 10:47:09 2003 Method: P:\Drlta\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\PFOS Last modified: Man Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 --- e-e- Page 17 Decatur RC and PFOSA 081103 Name: 0812031-3017 Text: 1: C8 Sulfonate (PFOS) 13-Aug-2003 20:30:33 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.39e4 Area 0-,,,,,,~,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,;~ 2.00 4.00 6.00 8.00 2: PFOSA `d IL3491 O-l 1, DF=l 000 081203A-3017 Sm (Mn. 2x3) 1 13-Aug-2003 20:30:3 K/MS/MS #6 MRM of 4 Channels ES- Oxygen Research, 3058 Research Drive, State College, PA 16801 000453 ----- -__-----------_----_c___ -----__ Quantify Sample Report ,'I& Study No.: L34910, Set No.: 081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\S~~eDB\O81203A Mon Aug 18 10:47:09 2003 P:\Data\L~SMS6\~asslynx\Fluoroch~cals.PRO\Met~B\PFOS Mon Aug 11 09:49:08 2003 Printed: Man Aug 18 10:50:26 2003 -----_ Page 18 Decatur BC and PFOSA 081103 mine : 081203A-3018 Text : 1: C8 Sulfonate (PFOS) I134910-l 1 Rep, DF=lOOO 381203A-3018 `OO-4 Sm (Mn, 2x3) 13-Aug-2003 20:52:12 LC/MS/MS #6 MRM of 4 Channels ES- 9.35 499 > 99 4935 2.74e4 Area L 2: PFOSA IL3491 O-l 1 Rep, DF=lOOO 081203A-3018 100- Sm (Mn, 2x3) %- L Time 13-Aug-2003 20:52:12 LC/MS/MS #6 MRM of 4 Channels ES- -L19:-7.9367 498.70>e378 Area 0 ,.,.,.,..,,`..,,,,,,....,.,.,,.".,,.'..,.,,., Time 2.00 4.00 6.00 8.00 10.00 -en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.: L34910, Ilru' Set No .:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\S~leDB\081203A Won Aug 18 10:47:09 2003 Wethod: P:\Data\L~SMS6\Masslynx\Fluorochamical\PFOS Last modified: Mea Aug 11 09:49:08 2003 Job code: Printed: Yon Aug 18 10:50:26 2003 Page 19 Decatur BC and PFOSA 081103 Name: 081203A-3019 Text : 1: '28 Sulfa& (PFOS) L34910-11, DF=lOO ? - -. ...'k" " :' . L 081203A-3019 I inh, I `""i 7 % j Sm (Mn, 2x3) . . 13-Aug-2003 21:13:5 9.34 499 > 99 2.24e5 Area w 2: PFOSA L3491 O-l 1, DF=l 00 08120314-3019 Sm (Mn, 2x3) 100- %- 13-Aug-2003 21:13:55 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 138347 498 > 78 6.48e4 Area Oxygen Research, 3058 Research Drive, State College, FA 16801 880455 Quantify Sample Report Study No.: L34910, Set No.: OBl203A, hd Ext.Date:08/12/03, Analyst:X.Risha Sample List: P:\Data\L~SMS6\MasslynX\Fluoroch~cals.PRO\S~leDB\O8l2O3A Last modified: Man Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\WethDB\PFOS Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 _----________-_--_____________________----- Name: 081203A-3020 Text : 1: C8 Sulfonate (PFOS) L3491 O-l 1 Rep, DF=lOO 081203A-3020 Sm (Mn, 2x3) 100- 9.36 %- Page 20 Decatur BC anc PFOSA 081103 13-Aug-2003 21:35:42 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.51e5 Area 0 1111/11~1,1111,1111,1111,1111,1111,11/1]1~ 2.00 4.00 6.00 2: PFOSA w L34910-17 Rep, DFdOO 081203A-3020 10 3 %- Sm (Mn, 2x3) 8.00 10.00 13-Aug-2003 21:35:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.98 498 > 78 7.31e4 Area 0 "","","",""1"",`,","","","", , . I I Time 2.00 4.00 6.00 8.00 10.00 Ekygen Research, 3058 Research Drive, State College, PA 16801 000456 Quantify Sample Report Study No.: L34910, Set No.: 081203A, Ext.Date:08/12/03, Analyst:K.Risha 'U Saxnple List: P:\Data\LCMSMS6\Maaslynx\Fluorochemicals.PRO\S~leD~\O81203A Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Met~B\PFOS Last modified: Mon Aug 11 09:49:08 2003 Job Code: Page 21 Decatur BC and PFOSA 081103 Printed: Man Aug I.8 10:50:26 2003 -__-_l----_-__----______I_____ -------w-e--- ---------_-__- Name : 081203A-3021 Text : 1: C8 Sulfonate XC081 103-4,250 (PFOS) rig/L Standard 081203A-3021 lOO- Sm (Mn, 2x3) %- 13-Aug-2003 21:57:23 LCYMSIMS #6 MRM of 4 Channels ES499 > 99 5.85e4 Area 2: PFOSA `N& XC081 103-4,250 rig/L Standard 081203A-3021 lOO- Sm (Mn, 2x3) %- , 10.00 I , I I Time 13-Aug-2003 21:57:23 LCNWMS #6 MRM of 4 Channels ES- 9.98 411227 498>78 1.97eS Area 0 ~`~~,~`~~,~"~,~~`~I~~"l~~~`l"~`l~~~'l"~'/~'~ , I I Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.: L34910, Set No.:Oa1203A, "lr/ mt.Date:oa/12/03, Analyet:K.Risha Sanyrle List: P:\Data\L~SMS6\Wrsslyax\Fluoroch~cals.PRO\S~leDB\D8l2O3A Last modified: Non Rug la 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\FluorochamicalPB\PFOS Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Man Aug 18 10:50:26 2003 Page 22 Decatur BC and PFOSA 081103 Name: 00120331-3022 Text : 1: C8 Sulfonate XC081 1034,500 (PFOS) rig/L Standard 081203k3022 Sm (Mn, 2x3) 13-Aug-2003 22:19:Oq LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.09e5 Area ,& 2: PFOSA XC081 103-5, 500 rig/L Standard 081203A-3022 lo& Sm (Mn, 2x3) 13-Aug-2003 22:19:0 LC/MS/MS #6 MRM of 4 Channels ES- %- ~~.,.`,,`..,,...,`." 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 ------ -------------------c_ -----__I--- -----e-- Quantify Sample Report Study No.: L34910, Set No .:OB1203A, Ext.Date:O8/12/03, Analyst:K.Risha pw Sample List: P:\Data\LCMSMS6\Masslynx\Fluoroch~cals.PRO\Samp~eDB\OB1203A Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\FluorochemicalsB\PFOS Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 ---- Page 23 Decatur BC and PFOSA 081103 Name: 0832031-3023 Text: 1: C8 Sulfonate (PFOS) XC081 103-6, 1000 rig/L Standard 081263A-3023 lOO- 7 %- Sm (Mn, 2x3) 13-Aug-2003 22:40:47 LC/MS/MS #6 MRM of 4 Channels ES- 9.36 499 > 99 2.13e5 Area 0 Ilrl,llll,~lll,,ll~,l~~l,llll/llll(l,l/,llI I, , , , , , , Time 2.00 4.00 6.00 8.00 10.00 2: PFCISA XC081 103-6,1000 rig/L Standard 081203A-3023 100- Sm (Mn, 2x3) 13-Aug-2003 22:40:4 LC/MS/MS #6 MRM of 4 Channels ES- %- 0 !`r',/!r,,"r*,rr*I 2.00 4.00 6.00 8.00 10.00 J Oxygen Research, 3058 Research Drive, State College, PA 16801 9/19/2003 Project: E03-0561 3MENVIR ONMINMLLMORATORY FinaIRcpolt 1 of3 Requester: Schnobrich, Dana M (223-lN-08) Department: 530711 Project Number: 0022674449 Date Received: 6/26/2003 Project Description: Decatur Bakers Creek Comments: #2 Surface Water and Sediment Completion Date: g/2/2003 Project Lead: Jess S. Eldridge Phone Number: 65 l-778-5233 Email Address: jseldridge@nmm.com Statement of Accuracy: Based on results of field spikes, laboratory spikes, field blank spikes, and laboratory control spikes, the analytical accuracy for all compounds is f 30%. Exceptions for the water samples are as follows: BC2 SW-04 high spike (PFOA 57%, PFOS - 62%, FOSA - 58%), BC2 SW-05 high spike (PFOA - 66%, FOSA - 400/a), BC2 SW-06 high spike (FOSA - 609/)), Outfall to River SW-25 (FOSA - 58%). Also, several low spike samples showed unacceptable recoveries in cases where the spiking concentration was comparable or below the inherent sample concentration. However, all laboratory control spikes, laboratory matrix spikes, and all other field spikes showed recoveries between 70% and 130% for all compounds. The accuracy for the sediment samples is based upon laboratory spike recoveries, all of which were between 70% and 130% for all compounds. Sediment sample results are reported as received. Results reported as dry weight are available in the Exygen report. REVISED REPORT: BGJ-Pace-9/19/03 Due to schedule changes, the original sample dates entered were revised to relect the actual collection dates. Pace Field Sampling Event - Complete 3M Sample Number E03-0561-49786 sampled Date 7l2 xxO3 Ii&! EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49787 PFOS by ESMS PFHS FOSA PFOA 9i21i2003 Sample Description BC2 SW-04 PFOS PFHS FOSA PFOA BC2 SW-04 DUP EXYGEN JXYGEN EXYGEN EXYGEN E03-0561-49788 EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49789 L&E EXYGEN EXYGEN PFOS by ESMS PFHS FOSA PFOA 7l23L2003 ical Methpd PFOS by ESMS PFHS FOSA PFOA 7Lw2003 PFOS by ESMS PFHS PFOS PFHS FOSA PFOA BC2 SED-04 m PFOS PFHS FOSA PFOA BC2 SW-OS PFOS PFHS 11.5 ng/mL 0.896 n&L 1.39 nahL 4.21 I&& 8.25 ng/mL 0.571 ng/mL 0.790 n@nL 2.54 ng/mL 14.6 rig/g 0.566 rip/g 7.15 rig/g 3.02 n#g 1.67 ng/mL 0.155 n@nL EL Oualifinr 0.05 0.05 0.05 0.05 BL - 0.05 0.05 0.05 0.05 EL OUlliripr 0.4 0.4 0.4 0.4 EL Ourliner 0.05 0.05 Project: E03-0561 (cont.) 3M Sample Number E03-0561-49789 (cont.) I&! EXYGEN EXYGEN E03-0561-49790 FOSA PFOA SampledDate 7/21/2003 7m2003 EXYGEN EXYGEN EXYGEN EXYGEN 303-0561-49791 LAB EXYGEN EXYGEN JXYGEN EXYGEN E03-056149792 PFOS by ESMS PFHS FOSA PFOA 7nv2003 m PFOS by ESMS PFHS FOSA PFOA 7n3mo3 I& EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49793 PFOS by ESMS PFHS FOSA PFOA 7n3noo3 LBB EXYGEN EXYGEN EXYGEN EXYGECN E03-0561-49794 PFOS by ESMS PFHS FOSA PFOA 7r2312003 EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49795 PFOS by ESMS PFHS FOSA PFOA 7i23i2003 La EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49796 PFOS by ESMS PFHS FOSA PFOA 7m2003 LAE EXYGEN FXYGEN EXYGEN PFOS by ESMS PFHS FOSA Sample Description BC2 SW-05 FOSA PFOA BC2 SW-05 DUP PFOS PFHS FOSA PFOA BC2 SED-05 PFOS PFHS FOSA PFOA BC2 SW-06 PFOS PFHS FOSA PFOA BC2 SW-06 DUP Comnonentr PFOS PFHS FOSA PFOA BCZ SED-06 PFOS PFHS FOSA PFOA Outfall to River SW-25 cPFOS PFHS FQSA PFOA Outfall to River SW-25 DUP PFOS PFHS FOSA 0. I46 ng/mL 0.591 nghL 4.33 nghL 0.377 nghd 0.389 ng/ti I .56 nghnL 22.8 ndg 1.45 rig/g 7.86 rig/g 5.14 ngtg 26.1 nghd 6.06 nghnL 2.43 nghL 12.1 n&nL 25.1 nghd 5.87 nghL 2.57 nghL 11.6n&nL 880 rip/g 2.46 rig/g 71.4 ndg 14.2 nglg 31.2 n&L 7.66nghL 3.26 nghL 15.8 n&L 30.8 n&L 6.77 nghL 3.28nghL l3L Oualirtrr 0.05 0.05 EL. Oualiner 0.05 0.05 0.05 0.05 EL - 0.4 0.4 0.4 0.4 BL Oualiner 0.05 0.05 0.05 0.05 BL Dualinrr 0.05 0.05 0.05 0.05 BL - 0.4 0.4 0.4 0.4 EiL Dulllifrcr 0.05 0.05 0.05 0.05 BL Oullifier 0.05 0.05 0.05 _a---." .,- .__.~_ .---." ,... _._1.".1_."_ -- -_ 9/19/2003 3MENVIR 0NMENTAL,LABOFL4'-K)RY Final Report Project: E03-0561 (cont.) 3M Sample Number E03-0561-49796 L&l EXYGEN E03-0561-49797 (cont.) PFOA sampled Date 7i23i2003 7L23/2003 Sample Description Outfall to River SW-25 DUP PFOA Outfall To River SED-25 UE EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49813 PFOS by ESMS PFHS FOSA PFOA 7i23l2003 PFOS PFHS FOSA PFOA Outfall to River SED-25 DUP LAB EXYGEN EXYGEN FXYGEN EXYGEN E03-0561-59479 LBB EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-59480 PFOS by ESMS PFHS FOSA PFOA 712V2003 s PFOS by ESMS PFHS FOSA PFOA ll2V2QO3 PFOS PFHS FOSA PFOA Field ControbTravel Blank PFOS PFHS FOSA PFOA Equipment Blank -Pump LAE EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-59481 LAB EXYGEN EXYGEN EXYGEN EXYGEN PFOS by ESMS PFHS FOSA PFOA 7/21/2003 PFOS by ESMS PFHS FOSA PFOA m PFOS PFHS FOSA PFOA Equipment Blank - Dredge ComDonentr PFOS PFHS FOSA PF0,4 14.4 nghL 107 ndg 3.19 nglg 28.0 rig/g 10.7 rig/g 140 rip/g 4.98 nglg 35.7 rig/g 17.7 ndg ND nghL ND llghL ND nghL ND n&L ND nghL ND nghnL ND nghL ND ng/mL ND nghL ND n&L ND nghL ND nghL 3 of3 a OuPlifier 0.05 BL Oualirier 0.4 0.4 0.4 0.4 BL Olaliner 0.4 0.4 0.4 0.4 EL Ovalifier 0.05 0.05 0.05 0.05 BL !ilulmc 0.05 0.05 0.05 0.05 BL OuPliner 0.05 0.05 0.05 0.05 Project Lead Review: Date: 9// 9/os