Document 5b49VMKo9O8DEY40wDjmXrEjV

Proven Results. Attachment 2 Analytical Report Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 1 Exygen Research Report No. L0001277 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Michael D Aucoin URS Corporation Barley Mill Plaza Building 27 Room 1260 Lancaster Pike and Rt 141 Wilmington, DE 19805 27s* 'CD -< T> rn rv> " D o eo ~i m 3? 9? cn UD ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 1 of 7 ooooos J & 33055;8 Research Drive VState College, PA 16801, USA T: 800.281.3219 F: 814.272.1019 exygen.com Summary Seven solid media samples were received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. The media represent samples of air collected on OVS tubes. Please see Table 1 for a completed listing of samples received and field air volumes collected. The samples were analyzed for Perfluorooctanoic Acid (C8 Acid) using liquid chromatography / mass spectrometry (LCMS). The method employed is entitled "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in OVS Airtubes by LCMS" (James Miller, Exygen Research, February 17, 2003). The OVS tubes were separated into three fractions for specific fluorochemical analysis. Fraction A consisted of the filter, backing material and plastic ring. Fraction B contained the first bed of XAD resin and the PUF backing. Fraction C contained the second bed of XAD resin and PUF backing. The fractions were extracted with 1 mL of methanol. Perfluorodecanoic Acid (CIO Acid) was added as a surrogate spike to each fraction prior to extraction. Instmment operating conditions can be found at the beginning of each analytical run. Raw instrument data is given in Appendix A. Chain-of-custody information can be found in Appendix B . ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 2 of 7 000009 Results Summary Request # WWK-A-AMS1-E1 A WWK-A-AMS1-E1 B WWK-A-AMS1-E1 C WWK-A-AMS1-E1 (Total) Air Volume Sampled (L) 1407 1407 1407 WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS2-E1 (Total) 1410 1410 1410 WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-EMS3-E1 C WWK-A-EMS3-E1 (Total) 1418 1418 1418 WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS4-E1 (Total) 1397 1397 1397 WWK-A-AMS5-E1 A WWK-A-AMS5-E1 B WWK-A-AMS5-E1 C WWK-A-AMS5-E1 (Total) 1418 1418 1418 WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A-AMS6-E1 C WWK-A AMS6-E1 (Total) 1482 1482 1482 1. "<" is defined as not detected at or above the reported level. C8 Acid (mg/m3) < 0.00007 < 0.00007 < 0.00007 <0.00014 0.00007 < 0.00007 < 0.00007 0.00007 0.00008 < 0.00007 < 0.00007 0.00008 < 0.00007 < 0.00007 < 0.00007 <0.00014 < 0.00007 < 0.00007 < 0.00007 <0.00014 < 0.00007 < 0.00007 < 0.00007 <0.00014 2. Sample results have not been corrected for blank results or control spike recoveries. 3. Please note the following descriptions of the OVS sample tube fractions: Fraction A B C Fraction Description Frit Extract 1st set beads extract 2nd set beads extract ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 3 of 7 000010 OC Data LCS Please note: One control sample was spiked with each perfluorooctanoic acid to give a final concentration of 500 ppb. Air was pulled through the tube at a rate of 1-liter per minute for one hour (480 liters of air). The fractions were separated and analyzed. The acceptable range for control recovery is 75-125%. Request # Control 1 C8 Acid (amount spiked - ppb) 500 C8 Acid (amount recovered - ppb) 509 C8 Acid (percent recovery 102 Blanks Request # WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C Voi. Of Air (L) 0 0 0 C8 Acid (uq/fraction) <0.10 <0.10 <0.10 000011 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 4 of 7 Surrogates A surrogate spike (CIO Acid) was added to all OVS tubes to give a final concentration of 500 ppb in the extract. Surrogate spike recoveries are given in the following table. There are no set criteria for surrogate spike recoveries. Advisory ranges are 75-125%. Sample # WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C WWK-A-AMS1-E1 A WWK-A-AMS1 -E1 B WWK-A-AMS1-E1 C WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-AMS3-E1 C WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS5-E1 A WWK-A-AMS5-E1 B WWK-A-AMS5-E1 C WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A-AMS6-E1 C Control Spike A Control Spike B Control Spike C Amount Spiked (ppb) 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 1000 * 500 500 Amount Recovered (PPb) 663 345 393 561 384 359 668 423 411 691 417 418 774 384 382 643 358 407 825 397 442 1196 349 385 Percent Recovery (%) 133 ** 69 ** 79 112 77 72 ** 134 ** 85 82 138 ** 83 84 155 ** 77 76 129 ** 72 ** 81 165 ** 79 88 120 70 ** 77 * The control spike A Fraction was inadvertently spiked twice with surrogate. The surrogate concentration for this sample is therefore 1000 ppb. ** Surrogate recovery outside of advisory range. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 000012 Calculations Request # WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C WWK-A-AMS1-E1 A WWK-A-AMS1-E1 B WWK-A-AMS1-E1 C WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-AMS3-E1 C WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS5-E1 A WWK-A-AMS5-E1 B WWK-A-AMS5-E1 C WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A-AMS6-E1 C Control Spike A Control Spike B Control Spike C Vol. Of Air (L) 0 0 0 1407 1407 1407 1410 1410 1410 1418 1418 1418 1397 1397 1397 1418 1418 1418 1482 1482 1482 0 0 0 C8 Acid (raw-ppb) <10 <10 < 10 <10 <10 <10 101 <10 <10 105 <10 < 10 < 10 < 10 <10 <10 <10 <10 <10 < 10 < 10 509 <10 <10 C8 Acid (ug/fraction) <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 0.10 <0.10 <0.10 0.11 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 0.51 <0.10 <0.10 C8 Acid (mg/m3) < 0.00007 < 0.00007 < 0.00007 0.00007 < 0.00007 < 0.00007 0.00008 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 000013 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 7 Example Calculation For sample WWK-A-AMS2-E1 A C8 Acid, = [101 ng/ml of C8 Acid x (1 ml) x (1 ug / 1000 ng) x (1 mg / 1000 ug) ] / [(1410 L) x (1 m3 / 1000 L)] = 0.00007 mg / m3 Signatures co L Paul Connolly, LCMS Team Leader /] Date Other Lab Members Contributing to Data James Miller Date ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 7 000014 000015 Table 1. Login Information / Field Data Sample ID Exygen Lab ID Date Received Description WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C WWK-A-AMS1-E1 A WWK-A-AMS1-E1 B WWK-A-AMS1-E1 C WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-AMS3-E1 C WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS5-E1 A WWK-A AMS5-E1 B WWK-A-AMS5-E1 C WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A AMS6-E1 C Control Spike A Control Spike B Control Spike C L0001277-1 L0001277-2 L0001277-3 L0001277-4 L0001277-5 L0001277-6 L0001277-7 L0001277-8 L0001277-9 L0001277-10 L0001277-11 L0001277-12 L0001277-13 L0001277-14 L0001277-15 L0001277-16 L0001277-17 L0001277-18 L0001277-19 L0001277-20 L0001277-21 L0001277-22 L0001277-23 L0001277-24 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Air Volume Sampled (L) 0 0 0 1407 1407 1407 1410 1410 1410 1418 1418 1418 1397 1397 1397 1418 1418 1418 1482 1482 1482 0 0 0 9T0000 Table 2. Chain of Custody Sample ID WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C WWK-A-AMS1-E1 A WWK-A-AMS1-E1 B WWK-A-AMS1-E1 C WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-AMS3-E1 C WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS5-E1 A WWK-A AMS5-E1 B WWK-A-AMS5-E1 C WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A AMS6-E1 C Control Spike A Control Spike B Control Spike C Date Collected 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 11/5/03 NA NA NA Date Received at Exygen 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 11/7/03 Date Extracted by Exygen 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 11/17/03 Date Analyzed by Exygen 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 11/17-11/18/03 ANALYTICAL DATA REVIEW SHEET LC/MS Analyst V#/n /n Reviewed by ej-- Signature /Date Of o / / ^ ^Sfgnature/Date m oi o OOOO/i " Sequence : C :\HPCHEM\1\SEQUENCE\111703.S Sequence Table: Method and Injection Info Part: Line Location SampleName Method Inj SampleType InjVolume DataFile 1 Vial 1 STD 50 ppb 2 Vial 1 STD 50 ppb ` 3 Vial 2 STD 100 ppb ' 4 5 Vial 3 Vial 4 STD 250 ppb STD 500 ppb 6 Vial 5 STD 750 ppb 7 .Vial 6 STD 1000 ppb 8 Vial 7 STD 1500 ppb 9 Vial 92 Solvent blank 10 Vial 11 L0001277-22 11 Vial 12 L0001277-23 12 Vial 13 L0001277-24 13 Vial 14 L0001277-1 14 Vial 15 L0001277-2 15 Vial 16 L0001277-3 16 Vial 17 L0001277-4 17 Vial 18 L0001277-5 18 Vial 19 L0001277-6 19 Vial 20 L0001277-7 20 Vial 4 STD 500 ppb 21 Vial 92 Solvent blank 22 Vial 21 L0001277-8 23 Vial 22 L0001277-9 24 Vial 23 L0001277-10 25 Vial 24 L0001277-11 26 Vial 25 L0001277-12 27 Vial 26 L0001277-13 28 Vial 27 LQ001277-14 29 Vial 28 L0001277-15 30 Vial 29 L0001277-16 31 Vial 30 L0001277-17 32 Vial 4 STD 500 ppb 33 Vial 92 Solvent blank 34 Vial 31 L00012773-18 35 Vial 32 L0001277-19 36 Vial 33 L0001277-20 37 Vial 34 L0001277-21 38 Vial 4 STD 500 ppb 39 Vial 92 Solvent blank 40 Vial 1 STD 50 ppb 41 Vial 2 STD 100 ppb . 42 Vial 3 STD 250 ppb 43 Vial 4 STD 50 ppb 44 Vial 5 STD 750 ppb 45 Vial 6 STD 1000 ppb 46 Vial 7 ' STD 1500 ppb FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 'FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 1 Sample 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib , Calibration Part: Line Location SampleName Method CalLev Update RF Update RT Interval 2 Vial 1 3 Vial 2 4 Vial 3 5 Vial 4 6 Vial 5 STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 .CMS3 11/17/03 4[:58 :38 PM jmiller 4>& "/'Vo,' 1 Replace Average 2 Replace Average 3 Replace Average 4 Replace Average 5 Replace Average 0 11 000017 of 2 Sequence : C: \HPCHEM\1\SEQUENCE\111703 .S Line Location SampleName Method CalLev Update RF Update 1 7 Vial 6 8 Vial 7 40 Vial 1 41 Vial 2 42 Vial 3 43 Vial 4 44 Vial 5 45 Vial 6 46 Vial 7 STD 1000 ppb STD 1500 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 6 Replace Average 7 Replace Average 1 Average Average 2 Average Average 3 Average Average 4 Average Average 5 Average Average 6 Average Average 7 Average Average iCMS3 11/17/03 4:58:38 PM jmiller u 01 2 OOOOIS Page 2 of 2 LC/MS SYSTEM AND OPERATING CONDITIONS Client: Dupont EXYGEN STUDY: L0001277 Instrument: Hewlett-Packard 1100 LC/MSD (LC/MS 3) API-ES Interface - Negative SIM mode Nitrogen: 10 L/m in at 300C Fragmentor: Variable; Vcap: 3500V Computer: Hewlett-Packard Kayak w orkstation Software: M icrosoft Windows NT 4.0 Agilent ChemStation Version A.08.03 HPLC Equipment: HP G1379A Solvent Degasser HP G1311A Quaternary Pump HP G1313A Autosampler HP G1316A Column Therm ostat HP G1946A MSD HPLC Column: Column Temp.: Mobile Phase (A): Mobile Phase (B): Thermo Hypersil-Keystone Betasil C18, 30 x 2.0 mm x 3pm 35 C 2mM Ammonium acetate in OmniSolv W ater HPLC grade Methanol T im e %A 0.0 70 6.0 10 10.0 10 10.0 STOP Post Time = 4 min. T otal run tim e = 14 min. Flow Rate: 0.3 m L/m in Injected Volume: 5 pL %B 30 90 90 STOP Page 1 of 2 00:3 000019 Ions m onitored: Analyte C8 A dd (PFOA) C10 Surrogate Ion (m/ z ) 369 469 Extraction Date: November 17, 2003 Analyst: James R. M iller "/"/v Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039, FAX: (814) 231-1580 Page 2 of 2 oou 000020 Instrument : LCMS3 Wed Nov 12 08:47:10 2003 G1946: API_ES Negative mode . Page 1 of 3 fa C:\HPCHEM\1\1946TUNE\ATUNES.TUN Scan: 50.00 - 3000.00 Samples: 8 Thresh: 0 Step: 0.10 29501 peaks Base: 2233.95 Abundance: 1021824 F Raw,Gauss 0.3 m/z gf Abund 113.01 64976 601.98 48816 1034.05 148800 1633.95 487296 2233.95 1021824 Rel Abund 100.00 75.13 229.01 749.96 1572.62 Iso m/z 113.99 602.85 1035.05 1634.85 2234.95 Iso Abund Iso Ratio 1450 2.23 6177 12.65 34384 23.11 177792 36.49 506496 49.57 0015 000021 G1946: API_ES Negative mode Instrument : LCMS3 (Lp),,/ Page 2 of 3 Wed Nov 12 08:47:10 2003/^' C:\HPCHEM\1\1946TUNE\ATUNES.TUN Mode: API -ES Polarity: NEG Fragment Skim2 Lensl Lens2 Iris Gain VAR WidthGain -128 6.0 WidthOffs VAR -4.0 MassGain- 36.15 21 MassOffs VAR 176 Energy 5.0 OpolPeak 300 OpolKnee 316 2.0 QuadDC 0.00 EMV VCap Status: CapCur ChamCur 2068 Samples 8 4000 Averages 1 StepSize 0.10 71 DryingGas 6.0 1.06 Gas Temp 300 Quad Temp 99 Neb Pres 20 UCli6 000022 G1946: API ES Negative mode Mass Offset Dynamic Parameter Ramp Mass 112.99 1633.95 Setting 0.56 0.56 Mass 601.98 2233.91 Setting 0.62 0.56 Mass 1033.99 Setting 0.64 UO'i 7 000023 Method C:\HPCHEM\1\METHODS\111703.M Calibration Table Calib. Data Modified Tuesday, January 06, 2004 3:42:40 PM Calculate Based on External Standard Peak Area Rel. Reference Window Abs. Reference Window Rel. Non-ref. Window Abs. Non-ref. Window Uncalibrated Peaks Partial Calibration Correct All Ret. Times 5.000 % 0.000 min 5.000 % 0.000 min not reported Yes, identified peaks are recalibrated No, only for identified peaks Curve Type Origin Weight Linear Ignored Equal Recalibration Settings Average Response Average Retention Time Average all calibrations Floating Average New 75% Calibration Report Options : Printout of recalibrations within a sequence: Calibration Table after Recalibration Normal Report after Recalibration If the sequence is done with bracketing: Results of first cycle (ending previous bracket) Signal 1: MSD1 369, EIC=368.7 :369.7 Signal 2: MSD1 469, EIC=468.7 :469.7 RetTime Lvl Amount Area [min] Sig [ppb] 11 11 | 1 7.277 1 1 50.00000 2.14132e4 2 100.00000 4.05086e4 3 250.00000 1.05354e5 4 500.00000 2.02487e5 5 750.00000 2.93093e5 6 1000.00000 3.82075e5 7 1500.00000 5.51002e5 8.040 2 1 50.00000 3.07352e4 2 100.00000 5.72000e4 3 250.00000 1.48856e5 4 500.00000 2.88926e5 5 750.00000 4.15738e5 6 1000.00000 5.40429e5 7 1500.00000 7.75202e5 Amt/Area I1 2.33501e-3 2.46861e-3 2.37295e-3 2.46930e-3 2.55892e-3 2.61729e-3 2.7223le-3 1 ,62680e-3 1.74825e-3 1.67947e-3 1.73055e-3 1.80402e-3 1 .85038e-3 1 .93498e-3 Ref Grp Name 1 C8 Acid 1 CIO Surrogate More compound-specific settings: Compound: C8 Acid Time Window From 7.105 min To 8.105 min Compound: CIO Surrogate Time Window : From 7.844 min To 8.649 min Peak Sum Table ***No Entries in table*** :00414 1/6/04 3:43:01 PM jmiller^<?7 ^ i U0 8 000024 Page 1o2 Method C:\HPCHEM\1\METHODS\111703.M Calibration Curves C8 Acid at exp. RT: 7.277 MSD1 369, EIC=368.7:369.7 Correlation: 0.99921 Residual Std. Dev.: 8441.61320 Formula: y = mx + b m: 366.65986 b: 10613.38950 x : Amount[ppb] y : Area CIO Surrogate at exp. RT: 8.040 MSD1 469, EIC=468.7:469.7 Correlation: 0.99897 Residual Std. Dev.: 13553.16277 Formula: y = mx + b m: 516.25884 b: 16373.12175 x: Amount[ppb] y : Area :00414 1/6/04 3:43:01 PM jmiller 0019 000025page 2of 2 Run# PCOflotaQ) jo F^oooo Sample Name:STD 50 ppb Sample Info-.Warm up Data file :C :\HPCHEM\l\DATA\Chemstor\11238833\A45120\FC000001.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 5:03:37 PM Seq Line Vial N o . Inj.No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 1 1 1 1 5 pi ra JS is Compound Amount (ng/mL) R.T. ,*"*8 Acid 32.29 10 Surrogat 28.95 7.281 8.048 Area 22453 31319 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 03:43:13 pm 0020 Page 1 of 1 000026 Sample Name:STD 50 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11238922\A49152\FC000002.D Injection Date Acq Operator Instrument - Dilution Acq. Method Analysis Method Last Changed 11/17/03 jmiller PC00414 1 5:19:09 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42 :41 pm 2 1 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1238922\A49152\FC000002.D) API-ES, Neg, SIM, Frag: Var 7.273 - C8 Acid 2500- 2000 - 1500- 1000 500- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1238922VA49152\FC000002.D) API-ES, Neg, SIM, Frag: Var 8.036 - C10 Surrogate 3500 30002500 J 2000 1500 1000 500 H 0 min Compound Amount (ng/mL) R.T. "S Acid 32.27 L0 Surrogat 28.92 7.273 8.036 Area 22445 31303 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 i 3C00414 *** End of Report *** Tue, 6. Jan. 2004 03:48:23 pm 0021 Page 1 of 1 000027 Sample Name:STD 100 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11239011\A51648\FC000003.D Injection Date Acq Operator Instrument - Dilution 11/17/03 jmiller PC00414 1 5:34:40 PM Seq Line Vial No. Inj . No. Inj. Voi. : : : : Acq. Method Analysis Method ~ Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 3 2 1 5 pi *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1239011\A51648\FC000003.D) API-ES, Neg, SIM, Frag: Var 5000- 7.271 - C8 Acic 4000- 3000- 2000- 1000- - 0- 1 1 1 ' I ` 1 1 I 1 246 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1239011\A51648\FC000003.D) i ,/ ' 1 -- ,--------1--------1--------1---------------- r 8 min API-ES, Neg, SIM, Frag: Var 7000- 8.045- C10 Surrogata 6000- 5000 -j 4000- 3000- 2000- 1000- 0-I 1 --------1-------- 1----- ,--------1--------r ~ , 24 ---- !--------,--------1------- 1 1 1 ' 68 11 min Compound Am ount (n g /m L ) R.T. A rea S ig n a l *" *8 A c i d 83.07 10 S u rro g a t 7 9 . 6 6 7.271 8.045 41070 57499 MSDl 369, E IC = 3 6 8 . 7 : 3 6 9 . 7 MSD1 4 6 9 , E I C = 4 6 8 . 7 : 4 6 9 . 7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 03 :48 :59 pm ^9 Page 1 of 1 000028 Sample Name:STD 250 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11239100\A54080\FC000004.D Injection Date Acg Operator Instrument - Dilution 11/17/03 jmiller PC00414 1 5:50:13 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : 4 3 1 5 pi Acq. Method Analysis Method * Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1239100\A54080\FC000004.D) API-ES, Neg, SIM, Frag: Var 12000- 7.2 79- C8 Acid j 10000- 8000- 6000- 4000- 2000- 0- l 1 , ,,r 2 r 1^ 1 i 1 ' ` 1 ' 1 1 1 4 6 S min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1239100\A54080\FC000004.D) API-ES, Neg, SIM, Frag: Var I l 8.047 - C10 Surrogate 17500- ! 15000 12500 -J 10000 7500 -j 5000 -j ..... 2500 -j : 0" r 1 1 r^ 2 11 1 4 Compound Amount (ng/mL) R.T. "Q Acid 264.15 10 Surrogat 260.15 7.279 8.047 ' 11 Area 107467 150676 iI 1 111111 6 8 min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 [ ?C00414 *** End of Report *** Tue, 6. Jan. 2004 03:49:32 pm 02 3 Page 1 of 1 000029 Sample Name:STD 500 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11239189\A56384\FC000005.D Injection Date Acq Operator Instrument r-- Dilution 11/17/03 jmiller PC00414 1 6:05:48 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method " Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 5 4 1 5 pi *MSD1 369, EIC=368.7:369.7 (CH EMSTORM 1239189\A56384\FC000005.D) API-ES, Neg, SIM, Frag: Var 7.2 76- C8 Acid 20000 - 15000- 10000- 5000- o-- _____________ ^ 5_____________ D_____________ O_________ *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\11239189\A56384\FC000005.D) API-ES, Neg, SIM, Frag: Var 35000 - 8.043 - C10 Surrogata 30000 - 25000 - 20000 - 15000- 10000- 5000- o-j-, | ---1--- 1- * 2 1 -1--- --- 1--- i--- '-- ----1---1--------1--- 1--- --- 1--- r 4 6 8 min Compound Amount (ng/mL) R.T. Area Signal "'3 Acid 533.05 L0 Surrogat 539.02 7.276 8.043 206063 294645 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 [ ?C00414 *** End of Report *** Tue, 6. Jan. 2004 03:51:34 pm 024 Page 1 of 1 000030 Sample Name:STD 750 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11239278\A59328\FC000006.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 6:21:21 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : Acq. Method Analysis Method * Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 6 5 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORYI 1239278\A59328\FC000006.D) API-ES, Neg, SIM, Frag: Var 35000 7.271 - C8 Add 30000 25000- 20000 J 15000 10000-1 5000 0-t _L *MSD1 469, EIC=468.7:469.7 (CHEMSTORY11239278\A59328\FC000006.D) API-ES, Neg, SIM, Frag: Var 50000 -| 8.032- C10 Surrogate, min 40000 30000 20000 - 10000- | r-- 1 ' 1 ----------1 --- -!---1------ ,--- 1-- ^ ! , , i--- r 2 4 6 8 min ompound Amount (ng/mL) R.T. Area Signal *>3 Acid 790.26 L0 Surrogat 785.82 7.271 8.032 300368 422062 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 C00414 *** End of Report *** Tue, 6. Jan. 2004 03:52:03 pm U025 Page 1 of 1 000031 Sample Name:STD 1000 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11239367\A62272\FC000007.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 11/17/03 jmiller PC00414 1 6:36:56 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : FC8-10.M C:\HPCHEM\1\METHODS\111703 .M 1/6/04 03:42:41 pm 7 6 1 5 Ul LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1239367\A62272\FC000007.D) API-ES, Neg, SIM, Frag: Var 45000 7.280- C8 Acid 40000 d 35000 30000 - 25000 -i 20000 "i 15000 10000 5000 0 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1239367\A62272\FC000007.D) API-ES, Neg, SIM, Frag: Var 60000 - 8.047 - C10 Surrogate 50000 ^ 40000- 30000 20000 - 10000- 0-- [--- 1- 1 ' 1 -!--- 1 i- 1 2 46 8 min Compound Amount (ng/mL) R.T. Area Signal Acid 1037.06 LO Surrogat 1034.57 7.280 8.047 390861 550477 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 'C00414 *** End of Report *** Tue, 6. Jan. 2004 0026 03:52:40 pm Page 1 of 1 000032 Sample Name:STD 1500 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11239456\A64768\FC000008.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 6:52:34 PM Seq Line Vial N o . Inj . No . Inj. Voi. : : : : 8 7 1 5 pi Acq. Method Analysis Method Last Changed FC8-10-M C :\HPCHEM \1\METHODS U11703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11239456\A64768\FC000008.D) API-ES, Neg, SIM, Frag: Var 60000 - 7.265 - C8 Acid, 50000 - 40000 - 30000 H 20000 - 10000H 0- L *MSD1 469, EIC=468.7:469.7 (CHEMSTORVI1239456\A64768\FC000008.D) API-ES, Neg, SIM, Frag: Var 8.037- C10 Surrogate. 80000- 60000 - 40000 - 20000- 1 1------------ 1 I '----- 1 1------------1-- 24 Compound Amount (ng/mL) R.T. 8..... Acid 1516.67 10 Surrogat 1509.46 7.265 8 . 037 ------ !------------1------------ ---------- H------------ 1------------ 1------------ '------------'----------- T 6 8 min Area Signal 566716 795645 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 03:53:04 pm 02 7 Page 1 of 1 000033 Sample NameSolvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11239542\A67136\FC000009.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 7:08:03 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\111703,M 1/6/04 03:42:41 pm 1 9 92 1 5 pi Compound Amount (ng/mL) R.T. 8 Acid 0.00 10 Surrogat 0.00 0.000 0.000 Area 0 0 Signal MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 03 :53 :37 pm 0028 Page 1 of 1 000034 Sample Name :LO001277-22 Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11239629\A69376\FC000010.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 11/17/03 jmiller PC00414 1 7:23:35 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 10 11 1 5 y.1 LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1239629\A69376\FC000010.D) API-ES, Neg, SIM, Frag: Var 7.252- C8 Acid 20000 - 15000- 10000- 5000- 0-- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1239629\A69376\FC000010.D) API-ES, Neg, SIM, Frag: Var 70000 - 8.019- C10 Surrogate 60000 - 50000 - 40000- 30000 - 20000 - 10000 -j 0- L min Compound Amount (ng/mL) R.T. "3 Acid 509.00 L0 Surrogat 1195.66 7.252 8.019 Area 197244 633642 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 9C00414 *** End of Report *** Tue, 6. Jan. 2004 03:54:52 pm 0029 Page 1 of 1 000035 Sample Name-.L0001277-23 Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11239718\A71872\FC000011.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 11/17/03 jmiller PC00414 1 7:39:07 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 11 12 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1239718\A71872\FC000011.D) API-ES, Neg, SIM, Frag: Var 1400 7.253- C8 Acic 1200- 1000 800- 600 400- 200 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1239718\A71872\FC000011 ,D) API-ES, Neg, SIM, Frag: Var 8.029- C10 Surrogate min 20000 - 15000- 10000 - 5000 Compound Amount (ng/mL) '"3 Acid 0.20 LO Surrogat 348.96 R.T. 7.253 8.029 Area 10688 196528 O o min Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 ?C00414 *** End of Report *** Tue, 6. Jan. 2004 03:57:43 pm Q3 Page 1 of 1 000036 ,,,, Sample Name:L0001277-24 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11239807\A75136\FC000012.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 11/17/03 jmi H e r PC00414 1 7:54:41 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 12 13 1 5 pi "" 8 Acid 0.00 10 Surrogat 385.38 7.258 8.028 423 215328 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 03:58:20 pm 0 0 3! Page 1 of 1 000037 Sample Name :L0001277-1 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11239894\A78016\FC000013.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 8:10:16 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 13 14 1 5 pi "3 Acid 0.00 LO Surrogat 663.10 0.000 8.027 0 358705 MSD1 369, E I C = 3 6 8 .7:369.7 MSD1 469, E I C = 4 6 8 .7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 03:59:15 pm u032 Page 1 of 1 000038 ,,,, Sample Name :L0001277-2 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11239980\A80704\FC000014.D Injection Date Acg Operator Instrument Dilution 11/17/03 jmiller PC00414 1 8:25:51 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acg. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 14 15 1 5 pi Compound Amount (ng/mL) R.T. '8 Acid 0.00 10 Surrogat 345.43 0.000 8.034 Area 0 194702 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:00:01 pm 0035 Page 1 of 1 000039 Sample Name:L0001277-3 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11241121\A107200\FC000015.D 1 '8 Acid 0.00 10 Surrogat 393.12 0.000 8.036 0 219326 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** U34 Tue, 6. Jan. 2004 04:18:21 pm Page 1 of 1 000040 Sample Name :L0001277-4 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11240172\A83200\FC000016.D Injection Date Acg Operator Instrument Dilution 11/17/03 jmiller PC00414 1 8:57:08 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 1 16 17 1 5 pi Compound Amount (ng/mL) R.T. -- 8 Acid 0.00 10 Surrogat 561.20 7.277 8.050 Area 3198 306099 Signal MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:00:35 pm U035 Page 1 of 1 000041 Sample Name:L0001277-5 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11240259\A86208\FC000017.D Injection Date Acg Operator Instrument Dilution 11/17/03 jmiller PC00414 1 9:12:46 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\111703 .M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 17 18 1 5 pi '8 Acid 0.00 10 Surrogat 384.05 0.000 8.056 0 214641 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:01:14 pm 0036 Page 1 of 1 000042 Sample Name:L0001277-6 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11241207\Al09504\FC000018.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 9:28:24 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 1 18 19 1 5 vl Compound Amount (ng/mL) R.T. 8 Acid 0.00 10 Surrogat 358.95 0.000 8.047 Area 0 201686 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:19:05 pm U037 Page 1 of 1 000043 Sample Name:L0001277-7 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11240455\A88704\FC000019.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 11/17/03 jmiller PC00414 1 9:44:00 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 19 20 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1240455\A88704\FC000019.D) API-ES, Neg, SIM, Frag: Var 5000- 7.280- C8 Acid 4000- 3000 2000- 1000- ` MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1240455\A88704\FC000019.D) APl-ES, Neg, SIM, Frag: Var 40000 - 8.047 - C10 Surrogata 35000 - 30000 - 25000 - 20000 -j 15000- 10000- 5000 0- Compound Amount (ng/mL) R.T. "8 Acid 100.51 10 Surrogat 668.26 7.280 8.047 Area 47465 361371 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PCO0414 *** End of Report *** Tue, 6. Jan. 2004 04:05:41 pm 3 Page 1 of 1 000044 Sample Name:STD 500 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11240544\A93120\FC000020.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 9:59:36 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : 20 4 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1240544\A93120\FC000020.D) API-ES, Neg, SIM, Frag: Var 7.280 - C8 Ade 20000 - 15000- 10000- 5000- o- L _ ' ' r ! 1^ 2 ' 1 1' 11 ' 11 1 1 1 r 4 6 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM1240544\A93120\FC000020.D) API-ES, Neg, SIM, Frag: Var 35000 -j 8.042 - C10 Surrogate, 30000- 25000 - 20000 - 15000- 10000-1 5000- 0... 1--------1 -,--- --- J 24 Compound Amount (ng/mL) R.T. "8 Acid 520.33 10 Surrogat 522.49 7.280 8.042 Area 201399 286112 1 1 * --|--------1--------'--------1--------1--------r 6 8 min Signal MSDl 369, EIC=3 68.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04 :12 :46 pm UQ39 Page 1 of 1 000045 Sample NameSolvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11240630\A95488\FC000021.D 1 " :8 Acid 0.00 10 Surrogat 0.00 0.000 0.000 0 0 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 i PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:13:26 pm 0 4 0 Page 1 of 1 000046 Sample Name:L0001277-8 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11240717\A97920\FC000022.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 10:30:34 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METH0DS\1117 03.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 22 21 1 5 pi 8 Acid 0.00 10 Surrogat 422.67 7.287 8.040 706 234578 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 I. *** End of Report *** PC00414 Tue, 6. Jan. 2004 04:13:53 pm 004 1 Page 1 of 1 000047 Sample Name :LO001277-9 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11240804\A100224\FC000023.D Injection Date Acq Operator Instrument Dilution 11/17/03 jmiller PC00414 1 10:46:05 PM Seq Line Vial N o . Inj . No . Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 23 22 1 5 ul 8 Acid 0.00 10 Surrogat 411.43 0.000 8.047 0 228775 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 [ PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:14:23 pm 42 Page 1 of 1 000048 Sample Name:L0001277-10 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11240910\A102464\FC000024.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 11/17/03 jmiller PC00414 1 11:01:41 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 24 23 1 5 pi 8 Acid 105.39 10 Surrogat 690.57 7.277 8.042 49256 372888 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:17:01 pm 0043 Page 1 of 1 000049 Sample Name :L0001277-11 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11240999\A105024\FC000025.D Injection Date Acg Operator Instrument Dilution 11/17/03 jmiller PC00414 1 11:17:16 PM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 25 24 1 5 pi *8 Acid 0.00 10 Surrogat 416.87 7.260 8.025 788 231588 MSDl 369, EIC=3 68.7:3 69.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:17:44 pm U0 44 Page 1 of 1 000050 Sample Name :L0001277-12 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11241293\Alll808\FC000026.D Injection Date Acq Operator Instrument " Dilution 11/17/03 jmiller PC00414 1 11:32:53 PM Seq Line Vial N o . Inj. No . Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 26 25 1 5 pi *":8 Acid 0.00 :10 Surrogat 418.17 0.000 8.036 0 232258 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:19:27 pm Q0 45 Page 1 of 1 000051 Sample Name:L0001277-13 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11241381\All4112\FC000027.D Injection Date Acq Operator Instrument * Dilution 11/17/03 jmiller PC00414 1 11:48:28 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 1 27 26 1 5 y.1 Compound Amount (ng/mL) R.T. 8 Acid 0.00 10 Surrogat 773.81 7.254 8.030 Area 3012 415861 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:20:00 pm u046 Page 1 of 1 0000S2 Sample Name:L0001277-14 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11241489\All6416\FC000028.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 12:04:04 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METH0DS\1117 03 .M 1/6/04 03:42:41 pm 1 28 27 1 5 pi Compound Amount (ng/mL) R.T. '8 Acid 0.00 10 Surrogat 384.24 0.000 8.033 Area 0 214743 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 l _____________________________________________________________ *** End of Report *** 0047 1 PC00414 Tue, 6. Jan. 2004 04:20:46 pm Page 1 of 1 0000S3 Sample Name:L0001277-15 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11241575\A118720\FC000029.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 12:19:40 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEMX1\METHODS\111703.M 1/6/04 03:42:41 pm 1 29 28 1 5 pi Compound Amount (ng/mL) R.T. J8 Acid 0.00 :10 Surrogat 381.84 0.000 8.031 Area 0 213502 Signal MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:21:21 pm 0048 Page 1 of 1 000054 ... Sample Name-.L0001277-16 Sample Info: Data file :C:\HPCHEM\1\DATA\Chemstor\11241687\Al20896\FCO00030.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 12:35:16 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 1 30 29 1 5 pi Compound Amount (ng/mL) R.T. 8 Acid 0.00 10 Surrogat 643.49 7.254 8.030 Area 3244 348580 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** 0049 Tue, 6. Jan. 2004 04:22:03 pm Page 1 of 1 000055 . Sample Name:L0001277-17 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11241774\A123200\FC000031.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 12:50:54 AM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703 .M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 31 30 1 5 pi " 8 Acid 0.00 !10 Surrogat 357.88 0.000 8.047 0 201132 MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:22 :38 pm u 0 b Page 1 of 1 000056 Sample Name:STD 500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11241882\A125376\FC000032.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 1:06:28 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703 .M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 32 4 1 5 pi *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1241882\A125376\FC000032.D) API-ES, Neg, SIM, Frag: Var 7.281 - C8 Acid 20000 15000- 10000- 5000- 8 MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1241882\A125376\FC000032.D) API-ES, Neg, SIM, Frag: Var 35000- 8.0 48- C10 Surrogate. 30000 - 25000 20000 15000- 10000 5000 0 1'11r 24 Compound Amount (ng/mL) R.T. 'l8 Acid 512.90 !10 Surrogat 520.70 7.281 8.048 Area 198672 285188 1 * , i----------- --- 1--- --- r 6 8 min Signal MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 005 04:22:53 pm Page 1 of 1 000057 Sample Name:Solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11241968\A127680\FC000033 .D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC 00414 1 1:21:57 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 1 33 92 1 5 pi Compound Amount (ng/mL) R.T. ':8 Acid 0.00 :10 Surrogat 0.00 0.000 0.000 Area 0 0 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 ! I PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:23:33 pm 0052 Page 1 of 1 000058 Sample Name :L0001277-18 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11242332\A136576\FC000034.D 1 18 Acid 0.00 :10 Surrogat 407.14 0.000 8.059 0 226562 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:25:54 pm u 055 Page 1 of 1 000059 Sample Name:L0001277-19 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\11242073\A129920\FC000035.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 1:53:03 AM Seq Line Vial No. Inj. No. Inj. Voi. : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm 1 35 32 1 5 pi Compound Amount (ng/mL) R.T. '*5 Acid 0.00 10 Surrogat 825.29 7.278 8.042 Area 2628 442438 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:24:17 pm 0054 Page 1 of 1 000060 Sample Name:L0001277-20 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11242160\A132160\FC000036.D Injection Date Acg Operator Instrument Dilution 11/18/03 jmiller PC00414 1 2:08:39 AM Seq Line Vial No. Inj.No. Inj . Voi. : : : A c q . Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\111703 .M 1/6/04 03:42:41 pm 1 36 33 1 5 pi Compound Amount (ng/mL) R.T. "8 Acid 0.00 10 Surrogat 396.83 0.000 8.050 Area 0 221239 Signal MSDl 369, EIC =368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:24:48 pm 55 Page 1 of 1 000061 Sample Name:L0001277-21 [ Sample Info: 1 Data file :C :\HPCHEM\1\DATA\Chemstor\11242246\A134400\FC000037.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 2:24:16 AM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. 1 37 34 1 5 pi *"'8 Acid 0.00 10 Surrogat 442.08 0.000 8.048 0 244599 MSD1 369, EIC=3 68.7:3 69.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:25:23 pm 0056 Page 1 of 1 000062 Sample Name:STD 500 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11242420\A138752\FC000038.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 2:39:51 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 38 4 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METH0DS\111703 .M 1/6/04 03:42:41 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1242420\A138752\FC000038.D) API-ES, Neg, SIM, Frag: Var 7.279- C8 Acid 20000 - 15000- 10000- 5000- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1242420VA138752\FC000038.D) API-ES, Neg, SIM, Frag: Var 35000 8.043- C10 Surrogate 30000 - 25000 20000 - 15000- 10000 5000 0 -f- Compound Amount (ng/mL) R.T. "8 Acid 524.51 10 Surrogat 531.10 7.279 8.043 Area 202929 290556 Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7 :469.7 i PC00414 *** End of Report *** U57 Tue, 6. Jan. 2004 04:26:19 pm Page 1 of 1 000063 Sample Name:Solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11242523\A141056\FC000039 .D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 2:55:17 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\111703 .M 1/6/04 03:42:41 pm 1 39 92 1 5 pi Compound Amount (ng/mL) R.T. ~8 Acid 0.00 10 Surrogat 0.00 0.000 0.000 Area 0 0 Signal MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:26:59 pm 0058 Page 1 of 1 000064 Sample Name:STD 50 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11242610\A676032\FC000040.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 3:10:50 AM Seq Line Vial N o . Inj. No. Inj . V o i . : : : : 40 1 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METH0DS\1117 03 .M 1/6/04 03:42:52 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORU 1242610\A676032\FC000040.D) API-ES, Neg, SIM, Frag: Var 2500 7.2 79- C8 Acid 2000- 1500- 1000- 500- *MSD1 469, EIC=468.7:469.7 (CHEMSTORU1242610\A676032\FC000040.D) API-ES, Neg, SIM, Frag: Var 8.040- C10 Surrogate. 3500- mtn 3000 -i 2500- 2000- 1500- 1000-j 500- 0- Compound Amount (ng/mL) R.T. *8 Acid 26.78 10 Surrogat 26.72 7.279 8.040 Area 20433 30167 ~T min Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:42:37 pm 059 Page 1 of 1 000065 Sample Name:STD 100 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11242717\A678080\FC000041.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 3:26:22 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 41 2 1 5 ul Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1 \METHODS U11703.M 1/6/04 03:42:52 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11242717\A678080\FC000041.D) API-ES, Neg, SIM, Frag: Var 7.271 - C8 Acid 4000- 3000- 2000- 1000- 0-L *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\11242717\A678080\FC000041.D) API-ES, Neg, SIM, Frag: Var 7000- 8.029 - C10 Surrogate: min 6000- 5000 J 4000- 3000- 2000- 1000- 0- Compound Amount (ng/mL) R.T. '"8 Acid 80.11 10 Surrogat 78.50 7.271 8.029 Area 39986 56901 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:43:16 pm QQ Page 1 of 1 000066 Sample Name:STD 250 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11242806\A679872\FC000042.D Injection Date Acg Operator Instrument Dilution 11/18/03 jmiller PC00414 1 3:41:57 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 42 3 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:52 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1242806\A679872\FC000042.D) API-ES, Neg, SIM, Frag: Var 12000- 7.277- C8 Add 10000- 8000- 6000- 4000- 2000- 0J 1. , | i ' r 1^ 246 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1242806\A679872\FC000042.D) L , | r. , 8 API-ES, Neg, SIM, Frag: Var r mi n 18000j 8.040- C10 Surrogate 16000 j 14000- -- 12000j 10000j 8000 6000 j 4000 j 2000 j 01 1 1 i 1 1 1 i T rn 246 j 1 __________________ 1 !^ 8 ^T min Compound Amount (ng/mL) R.T. Area Signal ":8 Acid 252.62 '10 Surrogat 253.10 7.277 8.040 103241 147036 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:44:03 pm U U6 ! Page 1 of 1 000067 Sample Name:STD 500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11242895\A681664\FC000043.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 3:57:31 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 43 4 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:52 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORVt 1242895\A681664\FC000043.D) APl-ES, Neg, SIM, Frag: Var 7.278 - C8 Add 20000 - 15000- 10000- *MSD1 469, EIC=468.7:469.7 (CHEMSTORYI1242895\A681664\FC000043.D) APl-ES, Neg, SIM, Frag: Var 35000 8.043- C10 Surrogata 30000 25000 20000 - 15000- 10000 5000 0 Compound Amount (ng/mL) R.T. "8 Acid 513.55 10 Surrogat 516.86 7.278 8.043 Area 198911 283206 Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:44:44 pm Q6 Page 1 of 1 000068 Sample Name:STD 750 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11242984\A683392\FC000044 .D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 4:13:05 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 44 5 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\111703 .M 1/6/04 03:42:52 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1242984\A683392\FC000044.D) API-ES, Neg, SIM, Frag: Var 7.283 - C8 Acid 30000 - 25000 - 20000 - 15000- 10000- 5000- 0- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1242984\A683392\FC000044.D) API-ES, Neg, SIM, Frag: Var 50000 - 8.043 - C10 Surrogate. 40000 - 30000 20000 - 10000- Compound Amount (ng/mL) R.T. `8 Acid 750.57 HO Surrogat 761.33 7.283 8.043 Area 285817 409414 Signal MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:45:38 pm 0063 Page 1 of 1 000069 Sample Name:STD 1000 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11243073\A685120\FC000045.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 4:28:42 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : 45 6 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METH0DS\111703.M 1/6/04 03:42:52 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11243073\A685120\FC000045.D) API-ES, Neg, SIM, Frag: Var 40000 - 7.277- C8 Acid 35000 - 30000 -j 25000 -j 20000 - 15000- 10000- 5000- 0- 8 MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1243073\A685120\FC000045.D) API-ES, Neg, SIM, Frag: Var 60000 8.052- C10 Surrogate 50000 - 40000- 30000 20000 - 10000 0 Compound Amount (ng/mL) R.T. .'8 Acid 989.14 :10 Surrogat 995.64 7.277 8.052 Area 373290 530381 Signal MSD1 369, EIC=3 68.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Tue, 6. Jan. 2004 04:46 :08 pm U6 4 Page 1 of 1 000070 Sample Name:STD 1500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11243162\A687232\FC000046.D Injection Date Acq Operator Instrument Dilution 11/18/03 jmiller PC00414 1 4:44:21 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 46 7 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\111703.M 1/6/04 03:42:52 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11243162\A687232\FC000046.D) API-ES, Neg, SIM, Frag: Var 60000 - 7.279 - C8 Aci. 50000 - 40000 - 30000 - 20000 - 10000- 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORY11243162\A687232\FC000046.D) API-ES, Neg, SIM, Frag: Var 90000 8.043- C10 Surrogate! 80000 - 70000 - 60000 - 50000 -j 40000- 30000 - 20000 - 100000- --- 1 1--- 1--- >-->--- --- 1 24 -1--- 6 1 1--- 1 i i .--- r 8 min Compound Amount (ng/mL) R.T. Area Signal 18 Acid 1425.56 :10 Surrogat 1430.26 7.279 8.043 533309 754759 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Tue, 6. J a n . 2004 uU65 04:46:49 pm Page 1 of 1 000071 Login #: L0001277> 1,387 Project: P0000419 Project Title/Type: Analysis of PFOA in OVS Tubes / ROUTINE Project Storage: Submitted By: Michael D. Aucoin ' Status: Unreceived Login Type: Immediate Receipt of Samples Started: Date Start: T 11/7/2003 2:41:35PM Due Date: 11/21/2003 Received Date: 11/07/2003 Received By: ROBB, SHAWN Spread Sample: Label: Login Notes: Conform Notes: " Conform COC Sample: Conform COC: Conform Sample: Conform Request: True True True True Package PK0001842 Carton Packages / Containers Mail Date / Condition Shipper /J D Temp. Control / Temperai 11/7/2003 10:40:51PM Package & Contents Uncompromised FEDEX 8363913020300200 NONE Direction / Handled By RECEIVED ROBB, SHAWN Container # C0018656 C 0 0 18657 C0018658 C 0 0 18659 C 0 0 18660 C0018661 C 0 0 18662 C 0 0 18663 COO18664 C0018665 C0018666 C 0 0 18667 COO18668 COO18669 COO18670 COO18671 COO18672 C0018673 C0018674 COO18675 COO18676 COO18677 COO18678 COO18679 Gross Weight 7.2 g 7.1 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g RM Miscellaneous Item Key None - 11/7/2003 Login.rpt Container Type Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Preservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE ICOC Description 0066 Report Version: Oct 23 2003 9:55AM Page 1 of 5 Mfg. Lot Mfg. ID Instance: R0072027 0 0 0 0 7 2 R0072027 ogm Sample ID L0001277-0001 L0001277-0002 L0001277-0003 L0001277-0004 L0001277-0005 L0001277-0006 L0001277-0007 L0001277-0008 L0001277-0009 L0001277-0010 L0001277-0011 L0001277-0012 L0001277-0013 L0001277-0014 L0001277-0015 L0001277-0016 L0001277-0017 L0001277-0018 L0001277-0019 L0001277-0020 L0001277-0021 L0001277-0022 L0001277-0023 L0001277-0024 Matrix GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS Fraction OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes Samples Sample WWK-A-AMSFBLK-E1 A WWK-A-AMSFBLK-E1 B WWK-A-AMSFBLK-E1 C WWK-A-AMS1-E 1 A WWK-A-AMS1-E1 B WWK-A-AMS1-E1 C WWK-A-AMS2-E1 A WWK-A-AMS2-E1 B WWK-A-AMS2-E1 C WWK-A-AMS3-E1 A WWK-A-AMS3-E1 B WWK-A-AMS3-E1 C WWK-A-AMS4-E1 A WWK-A-AMS4-E1 B WWK-A-AMS4-E1 C WWK-A-AMS5-E1 A WWK-A-AMS5-E1 B WWK-A-AMS5-E1 C WWK-A-AMS6-E1 A WWK-A-AMS6-E1 B WWK-A-AMS6-E1 C CONTROL A CONTROL B CONTROL C Date Sampled Date Received 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 Date Due 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 * 11/7/2003 Login.rpt U0 67 Report Version: Oct 23 2003 9:55AM Page 2 of 5 Instance: 000073 R0072027 R0072027 L0001277-0001 Container / /C0018656 Other NONE L0001277-0002 r Container C 0 01 865 7/O th e r/N O N E L0001277-0003 Container C 0 0 1 865 8/O th e r/N O N E L0001277-0004 Container C 0 01 865 9/O th e r/N O N E - L0001277-0005 Container C0018660/O ther/N O N E L0001277-0006 Container C0018661 / O ther/N O N E L0001277-0007 Container C0018662/ Other /N O N E L0001277-0008 Container C 0 01 8 6 6 3 /O th e r/N O N E L0001277-0009 Container C0018664/O ther/N O N E LOO01277-0010 Container C 0 01 8 6 6 5 /O th e r/N O N E L0001277-0011 Container C 0 01 866 6/O th e r/N O N E L0001277-0012 Container ` 11/7/2003 Login.rpt ogin Bottles Method Method Method Method Method Method Method Method Method Method Method Method U0 68 Report Version: Oct 23 2003 9:55AM Page 3 o f5 Instance: 000074 R0072027 R0072027 C0018667 / Other / NONE L0001277-0013 Container C0018668/O ther/N O N E L0001277-0014 Container C0018669/O th er/N O N E L0001277-0015 Container C 0 01 8 6 7 0 /O th e r/N O N E L0001277-0016 Container C0018671 / O ther/N O N E L0001277-0017 Container C0018672/ Other/ NONE L0001277-0018 Container C 0 01 8 6 7 3 /O th e r/N O N E L0001277-0019 Container C0018674 / Other / NONE L0001277-0020 Container C 0 01 8 6 7 5 /O th e r/N O N E L0001277-0021 Container C0018676/ Other/ NONE L0001277-0022 Container C 0 01 8 6 7 7 /O th e r/N O N E L0001277-0023 Container C 0 01 867 8/O th e r/N O N E L0001277-0024 Container 11/7/2003 Login.rpt Method Method Method Method Method Method Method Method Method Method Method Method Report Version: Oct 23 2003 9:55AM Page 4 of 5 U0 69 Instance: R0072027 0 0 0 0 7 5 R0072027 C0018679/Other/NONE 11/7/2003 Login.rpt Report Version: Oct 23 2003 9:55AM Page 5 of 5 U070 Instance: R0072027 0 0 0 0 7 6 R0072027 T CHAIN OF CUSTODY/ANALYSIS REQUEST FORM SEARCH Exygen Research Sample Receiving * 3 1 1 7 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com I| Page ___o f I PROJECT IN FO R M A TIO N ANALYSES REQUESTED Client (nam e & address): A M aa )*. b rJr VA/* kW. \es\ Phone: Fax: S am p ler: (3 0%) ^ So j i^tQ JW V\K JPrM ), Project M an ag er (N am e & E-mail Address): A v k c A l. co.Vx Project Nam e: RO. # : 4V Q uotation # : , rv S r^aadA. rJ J Please fill out this form completely to ensure correct analysis and proper handling of your samples. rA !T Composite Number of Containers SAMPLE ANALYSIS Collection Collection _fQd ExyLIMS# Client Sample Identification pate Time O W w k - A - A /*5 P B U < - 1 T 0U>33 w w k-A -V K 1-E 1 05H5 x 0551 / A m t ,- EJ- 0033 X ooa w v K ' A- A^ 5 5 ' E4. W W K - A ' A M 5 ' ELI C. -6rt'b's / O LAB USE ONLY ^<3 esz\ 2 7 )U l5 2 L - CHAIN OF CUSTODY Specify Matrix I At I I Ate l A;r 1 A ir 1 A> \ Ar Comments BLaI* * Cooler ID # . f\A A4Cooler Temp. (C) Relinquished by Date Time Received by Date Time Jli! j"ff\ivis' tyff 1* .01 %e?C> 1L J L ,,T * r J /M V ..... ----f --i ----- tlj j/o /o ty OTHER INFORM ATION E v a ,+ 1 LAB USE ONLY < V-> X. y X X X X 2<_ PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: Sample results only I I Add case narrative I I Add quality control summary I I Add calibration summary HD Add raw data Other 000077 REV. 3 - 0 2 DuPont Washington Works Air Sampling Program Sampler(s): SO, AC RK, LK FedEx Airbill #: 1 K 3 W j ^ 0 3 0 Event Number Event 1 Pump # 669842 669908 669878 669831 669769 669865 Hours 0 1 2 3 4 Station# MS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes 0 60 120 180 240 WWK-A-AMS1-E1 WWK-A-AMS2-E1 WWK-A-AMS3-E1 WWK-A-AMS4-E1 WWK-A-AMS5-E1 WWK-A-AMS6-E1 Hours 5 6 7 8 9 Calibration (pre) i M i l j.001 ll"5-4> ).o i 1 o iz . l.O ll Loti I.e lO Minutes 300 Hours 10 360 11 420 12 480 13 540 14 s ta rttim e S U stop Time 5JK 7O C o fn l a iilJtL...m w T 05^t o i*.W b 0.!TV3 0^43 Minutes 03\ 's O I slJ Hours Minutes 600 15 900 660 16 960 720 17 1020 780 18 1080 840 19 1140 Calibration (post) h o A u a i .... 0 ,^ 6 1 0 0 C0O Hours 20 21 22 23 24 h i b Total volume i4 ; ^ I N .9 - 1 ra aq 143 1 3 ^ ^1-5 Minutes j.v " '" 1200 1 7 1260 1320 1380 1440 Field Blank: WWK-K-AMSFBLK-E1 yes or no Weather: M lf -j \\v*rs\*f'A S j SAFER operational: Comments: oc . JE5. yes or no 000078 11/4/2003 Page 1 of 1 airdatal .xls Washington Works No Charge Shipper Ship To: Exygen Research 3058 Research Drive State College, PA 16801 Attn: Shawn Robb or John Flaherty 814-272-1039 Date: 10/27/2003 NCS # : 38-200304715 Routing: FED EX ( SEE ABOVE ACCT) F. O. B.: COLLECT Date Shipped: B / L: Phone Number: Quantity 1 Product Code / Description Box containing glass sample tubes for analysis W eight 10 Units lbs. Freight Class: TUBES, GLASS, NOI. Originator: Crane, Alison A Cost Code: 7035-507483-862200 Purchase Order #: Value fo r Customs: Dimensions: Ship From: Stores Status: Phone: 4448 Hazardous Shipment? No O Yes MSDS Sheets Required? No O Yes Material Class: Corrosive Flammable Toxic Other Shipping # : u073 000079 Special Instructions: This N-C-S will cover 6 shipments beginning 10/30/03. > > > Will deliver package to Stores with completed FEDEX Bill. CRG Account Number 2230-5551-6. Weekend samples will be delivered directly to FEDEX. < < < < Comments: U074 000080 S USA A irb ill Express S B tB llB O S O O Company f)up>A Address Ho Je C& b i-City 7 ^ / N 2 YourInternal BillingReference 3 To Recipient's Name ________ r r e . mil'M tate Po&d Dep|/RoDf/Surte/RQom zip <3-01%I M } , 7 .0 0 0 0 3 Phone 6H 331- S033 Company PrS>^r(lo Address I H "? l^SrWflt To "HOLD" at FedEx Station, printFedEx address. \ `' ' ' Address We cannot delivertoP.Q. boxesisP.O. ZJP codes. 000081 Recipients Copy 4a Express Package Serine Packagesupto 150lbs. Delivery commitment may be later in suite areas. FedEx Priority Overnight Next business morning [ 1 FedEx Standard Overnight \ Next business afternoon \. I I FedEx First Overnight 1-- 1 EEaarrlliieessttnneexxttbbuussiinneessssmmoorrnniinngg deliveiy to select locations C 3 FedEx 2 0 ay j FedEx Express Saver Second business day 1 Third business day |--------- FedExEnvelODerattnotavailable.Miimum|Y^a.nnc.p0unc| fate ---------- 4b ExpressFreightSeivice \ : I ] FedEx 1Day Freight* I-- I Next business Jay * Call tor Confirmation: . I I ^dEx2Day Freight Stand business day Packages over150lbs. Delivery commitmentmay be later in some areas. | I FedEx 3Day Freight I-- I Third business day 5 Packaging * Declared value ltnwt S500 F I FedEx Envelope* D FedExPak* IncisteiFedEx^mallPak, FedEx LargePak, and FedEx Sturdy Pak '^OtOtther 6 Special Handling IncItHtbFedEx address in Section 3. ,, S A ltM A Y D elivery !___| Avaiabte oniyfor FedEx Priority Overnight and FedEx 2Day to selectZIP codes I-- ^HOLD ^W eekday at FedExlocation Not available for 'edEx fitst Overnight Does th is shipm ent contain dangerous g ods? ------------- One box must be checked. -- -------- I-- i HOLD S a tu rd a y I__ ! a t FedEx Location Available onlyter FedEx Priority Overnight and FedEx2Dayto select locations i No YesAs per attached PL JI YfSheipsper Declaration Shipper's Declaration not remol El1"Drylce.9,UN ^ __ Dangerous Goods including Dry Icel'cannot be shipped in FedExgckaginy. I I Cavgi.,Aircraft Only 7 Payment [ X Sender I JRecipient . | Thin Party Acct No. in Section v r, ------- \ ' ObtainRecip. J lrtN o . | | Credit Card L J ^h /C he ck By signing you authorize ustod8liv8rthis shipment w ithout obtaining a ^nature and agree-to indemnify and hold us harmless from any resulting claim s.' Questions? Visit our Web site at fedex.com o r call 1.8Q0.Go.FedEx 800.463.3339. < Bav. DatB 10/1)1Part #T57B121994--^X31 FadEx*PRlNTED IN U.S.A WCSL02 . . . I CD 3