Document JN4mqQvdvowdNVmqOKp7D9boB

Proven Results. Attachment 2 Analytical Report Air Sampling Fluorochemicai Report DuPont Washington Works - Air Sampling Program Round 2 Exygen Research Report No. L0001308 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 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 1 of 7 3058 Research Drive State College, PA 16801, USA 0000 T: 800.281.3219 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 OYS 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. Fractions A and B were extracted with 1 mL of methanol. Fraction C was not analyzed but saved for possible future analysis. Perfluorodecanoic Acid (CIO Acid) was added as a surrogate spike to each fraction prior to extraction. Instrument 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 000083 Results Summary Request # Air Volume Sampled (L) C8 Acid (mg/m3) WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS1-E2 C WWK-A-AMS1-E2 (Total) 1475 1475 1475 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS2-E2 A WWK-A-AMS2-E2 B WWK-A-AMS2-E2 C WWK-A-AMS2-E2 (Total) 1468 1468 1468 0.0009 < 0.00007 NA 0.0009 WWK-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-EMS3-E2 C WWK-A-EMS3-E2 (Total) 1462 . 1462 1462 0.0009 < 0.00007 NA 0.0009 WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A-AMS4-E2 C WWK-A-AMS4-E2 (Total) 1437 1437 1437 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS5-E2 A WWK-A-AMS5-E2 B WWK-A-AMS5-E2 C WWK-A-AMS5- E2 (Total) 1456 1456 1456 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B WWK-A-AMS6-E2 C WWK-A AMS6-E2 (Total) 1422 1422 1422 < 0.00007 < 0.00007 NA <0.00014 NA - Not Analyzed. B fraction was below the quantitation limit, therefore the backup fraction does not require analysis. 1. "<" is defined as not detected at or above the reported level. 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 (not analyzed) ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 3 of 7 000084 ? I t I; i s. |. ? 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 (60 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) 503 C8 Acid (percent recovery 101 Blanks Request # WWK-A-AMSFBLK-E2 A WWK-A-AMSFBLK-E2 B Voi. Of Air (L) 0 0 C8 Acid (uq/fraction) <0.10 <0.10 000085 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-E2 A WWK-A-AMSFBLK-E2 B WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS2-E2 A WWK-A-AMS2-E2 B WWK-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A-AMS5-E2 A WWK-A-AMS5-E2 B WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B Control Spike A Control Spike B Amount Spiked (PPb) 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 Amount Recovered (PPb) 644 329 707 392 666 405 666 396 697 403 732 437 763 375 612 392 Percent Recovery (%) 129* 66* 141* 78 133* 81 133* 79 139* 81 146* 87 153* 75 122 78 * Surrogate recovery outside of advisory range ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 0000S6 Calculations Request # WWK-A-AMSFBLK-E2 A WWK-A-AMSFBLK-E2 B WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS2-E2 A WWK-A-AMS2-E2 B WWK-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A-AMS5-E2 A WWK-A-AMS5-E2 B WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B Control Spike A Control Spike B Vol. Of Air (L) 0 0 1475 1475 1468 1468 1462 1462 1437 1437 1456 1456 1422 1422 0 0 C8 Acid (raw-ppb) < 10 < 10 <10 <10 1340 <10 1266 <10 < 10 <10 49 <10 <10 <10 454 49 C8 Acid (ug/fraction) <0.10 <0.10 <0.10 <0.10 1.3 <0.10 1.3 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 0.45 <0.10 C8 Acid (mg/m3) < 0.00007 < 0.00007 0.0009 < 0.00007 0.0009 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 AT T. DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGENRESEARCH Example Calculation For sample WWK-A-AMS2-E2 A C8 Acid, = [1340 ng/ml of C8 Acid x (1 ml) x (1 ug / 1000 ng) x (1 mg / 1000 ug) ] / [(1468 L) x (1 m3 / 1000 L)] = 0.0009 mg / m3 Signatures Other Lab Members Contributing to Data James Miller Date Date ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 7 000088 I1 Table 1. Login Information / Field Data Sample ID Exygen Lab ID Date Received Description WWK-A-AMSFBLK-E2 A WWK-A-AMSFBLK- E2 B WWK-A-AMSFBLK-E2 C WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS1-E2 C WWK-A-AMS2-E2 A WWK-A-AMS2-E2 B WWK-A-AMS2-E2 C WWK-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-AMS3-E2 C WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A-AMS4-E2 C WWK-A-AMS5-E2 A WWK-A AMS5-E2 B WWK-A-AMS5-E2 C WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B WWK-A AMS6-E2 C Control Spike A Control Spike B Control Spike C L0001308-1 L0001308-2 L0001308-3 L0001308-4 L0001308-5 L0001308-6 L0001308-7 L0001308-8 L0001308-9 L0001308-10 L0001308-11 L0001308-12 L0001308-13 L0001308-14 L0001308-15 L0001308-16 L0001308-17 L0001308-18 L0001308-19 L0001308-20 L0001308-21 L0001308-22 L0001308-23 L0001308-24 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 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 1475 1475 1475 1468 1468 1468 1462 1462 1462 1437 1437 1437 1456 1456 1456 1422 1422 1422 0 0 0 J 000089 000090 009 Table 2. Chain of Custody Sample ID WWK-A-AMSFBLK-E2 A WWK-A-AMSFBLK-E2 B WWK-A-AMSFBLK-E2 C WWK-A-AMS1-E2 A WWK-A-AMS1-E2B WWK-A-AMS1-E2C WW K-A-AMS2-E2 A WWK-A-AMS2-E2 B WWK-A-AMS2-E2 C WW K-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-AMS3-E2 C WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A-AMS4-E2 C WWK-A-AMS5-E2 A WWK-A AMS5-E2 B WWK-A-AMS5-E2 C WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B WWK-A AMS6-E2 C Control Spike A Control Spike B Control Spike C Date Collected 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 11/12/03 NA NA NA Date Received at Exygen 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 11/13/03 Date Extracted by Exygen Date Analyzed by Exygen 11/20/03 11/20/03 NA 11/20/03 11/20/03 NA 11/20/03 11/20/03 NA 11/20/03 11/20/03 NA 11/20/03 11/20/03 NA 11/20/03 11/20/03 NA 11/20/03 11/20/03 NA 11/20/03 11/20/03 NA 11/20-11/21/03 11/20-11/21/03 NA 11/20-11/21/03 11/20-11/21/03 NA 11/20-11/21/03 11/20-11/21/03 NA 11/20-11/21/03 11/20-11/21/03 NA 11/20-11/21/03 11/20-11/21/03 NA 11/20-11/21/03 11/20-11/21/03 NA 11/20-11/21/03 11/20-11/21/03 NA 11/20-11/21/03 11/20-11/21/03 NA ANALYTICAL DATA REVIEW SHEET LC/MS Analyst R . . M i l 2_ g- Sigriature/Date Reviewed by 2/ / & / S Signature/Date '/ */ *r 0010 000091 Sequence: C:\HPCHEM\1\SEQUENCE\112003.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 Vial 3 STD 250 ppb 5 Vial 4 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 L0001308-22 11 Vial 12 L0001308-23 12 Vial 13 L0001308-1 13 Vial 14 L0001308-2 14 Vial 15 L0001308-4 15 Vial 16 L0001308-5 16 Vial 17 L0001308-7 17 Vial 18 L0001308-8 18 Vial 19 L0001308-10 19 Vial 20 L0001308-11 20 Vial 4 STD 500 ppb 21 Vial 92 Solvent blank 22 Vial 21 L0001308-13 23 Vial 22 L0001308-14 24 Vial 23 L0001308-16 25 Vial 24 L0001308-17 26 Vial 25 L0001308-19 27 Vial 26 L0001308-20 28 Vial 4 STD 500 ppb 29 Vial 92 Solvent blank 30 Vial 1 STD 50 ppb 31 Vial 2 STD 100 ppb 32 Vial 3 STD 250 ppb 33 Vial 4 STD 500 ppb 34 Vial 5 STD 750 ppb 35 Vial 6 STD 1000 ppb 36 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 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Sample Calib Calib Calib Calib Calib Calib Calib Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Calib Calib Calib Calib Calib Calib Calib Calibration Part: Line Location SampleName Method CalLev Update RF Update RT Interval 2 Vial 1 STD 50 ppb 3 Vial 2 STD 100 ppb 4 Vial 3 STD 250 ppb 5 Vial 4 STD 500 ppb 6 Vial;- 5 STD 750 ppb 7 Vial 6 1 STD 1000 ppb 8 Vial 7 STD 1500 ppb 30 Vial 1 STD 50 ppb 31 Vial 2 STD 100 ppb 32 Vial 3 STD 250 ppb 33 Vial 4 STD 500 ppb 34 Vial 5 STD 750 ppb 35 Vial 6 STD 1000 ppb 36 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 LCMS3 11/20/03 4:31:48 PM jmiller 1 Replace Average 2 Replace Average 3 Replace Average 4 Replace Average 5 Replace Average 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 0 011 0 0 0 0 9 2 Page 1 of 2 Sequence: C:\HPCHEM\1\SEQUENCE\112003.S LCMS3 11/20/03 4:31:48 PM jmiller ? 0012 0 0 0 0 9 3 Page 2 LC/MS SYSTEM AND OPERATING CONDITIONS Client: Dupont EXYGEN STUDY: L00013Q8 Instrument: Hewlett-Packard 1100 LC/MSD (LC/MS 3) API-ES Interface - Negative SIM mode Nitrogen: 10 L/min at 300C Fragmentor: Variable; Vcap: 3500V Computer: Hewlett-Packard Kayak workstation Software: Microsoft 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 Thermostat HP G 1946A 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 Water HPLC grade Methanol Time %A 0.0 70 6.0 10 10.0 10 10.0 STOP Post Time = 4 min. Total run time = 14 min. Flow Rate: 0.3 mL/min Injected Volume: 5 pL %B 30 90 90 STOP Page 1 of 2 o 13 000094 Ions monitored: Analyte C8 Acid (PFOA) C10 Surrogate Ion (m/z) 369 469 Extraction Date: November 20, 2003 Analyst: James R. Miller Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039, FAX: (814) 231-1580 Page 2 of 2 004 000095 Instrument : LCMS3 Wed Nov 12 08:47:10 2003 G1946: API_ES Negative mode Page 1 of 3 Ao 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 0.3 100 -i 60 - 40 - 20 - 0 --`-J i I-----r---- 1-----1---- 1-- --i-----1----- [---- 1-----1-----/ 500 1000 1500 2000 2500 m/z gf Abund 113.01 64976 601.98 48816 1034.05 148800 1633.95 487296 2233.95 1021824 Rei 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 000096 G1946: API_ES Negative mode Instrument : LCMS3 /Lfs Page 2 of 3 Wed Nov 12 08:47:10 2003/^' '`V*? C:\HPCHEM\1\194 6TUNE\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 0016 000097 Gl946: API_ES Negative mode Instrument : LCMS3 /W, iy Page 3 of 3 Wed Nov 12 08:47:10 2003 f f 1' 1 /'VJ C:\HPCHEM\1\194 6TUNE\ATUNES.TUN 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 j 0 7 000098 !..M.ethod C:\HPCHEM\1\METHODS\112003.M r' Calibration Table Calib. Data Modified Thursday, January 08, 2004 2:45:39 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 [min] Sig Amount Area Amt/Area Ref Grp Name [ppb] 1---------- 1---------- 7.237 1 1 50.00000 2.06063e4 2.42644e-3 2 100.00000 4.03552e4 2.47800e-3 3 250.00000 1.05844e5 2.36198e-3 4 500.00000 2.01381e5 2.48286e-3 5 750.00000 2.83374e5 2.64668e-3 6 1000.00000 3.74570e5 2.66973e-3 7 1500.00000 5.30698e5 2.82646e-3 8.005 2 1 50.00000 3.00000e4 1.66666e-3 2 100.00000 5.87547e4 1.70199e-3 3 250.00000 1.53 014e5 1.63384e-3 4 500.00000 2.90758e5 1.71964e-3 5 750.00000 4.07335e5 1.84124e-3 6 1000.00000 5.37103e5 1 .86184e-3 7 1500.00000 7.56846e5 1.98191e-3 1 1 C8 Acid CIO Surrogate More compound-specific settings: Compound: C8 Acid Time Window From 7.064 min To 8.065 min Compound: CIO Surrogate Time Window : From 7.808 min To 8.614 min Peak Sum Table ***No Entries in table*** 00414 1/8/04 2:48:28 PM jmiller OV 0018 000099age 1of 2 Method C:\HPCHEM\1\METHODS\112003.M Calibration Curves C8 Acid at exp. RT: 7.237 MSD1 369, EIC=368.7:369.7 Correlation: 0.99864 Residual Std. Dev.: 10680.87214 Formula: y = mx + b m: 353.21288 b: 12999.22280 x: Amount[ppb] y : Area CIO Surrogate at exp. RT: 8.005 MSD1 469, EIC=468.7:469.7 Correlation: 0.99837 Residual Std. Dev.: 16687.58942 Formula: y = mx + b m: 503.56527 b: 20573.54985 x: Amount[ppb] y : Area '00414 1/8/04 2:48:28 PM jmiller *Y 0019 OOOlQfte 2 of 2 Sample Name:STD 50 ppb Sample Info:Warm up Data file :C:\HPCHEM\1\DATA\FC000001. D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 4:41:30 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000001.D) API-ES, Neg, SIM, Frag: Var 7.256- C8 Acid 2500 2000 1500- 1000 500- 1 1 1 1 5 pi 'MSD1 469, EIC=468.7:469.7 (FC000001 .D) API-ES, Neg, SIM, Frag: Var 4500 8.042- C10 Surrogate, 4000 3500 3000- 2500 r 2000 "i 1500 1000 500- 1 1 1--- '--- 1-- 24 i--- 1 i i--- 1--- 1--- 1--- '--- r 6 8 min Compound Amount (ng/mL) R.T. Area Signal S18 Acid 26.66 :10 Surrogat 28.77 7.256 8.042 22415 35062 MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 0 PC00414 *** End of Report *** Thu, 8. Jan. 2004 04:20:20 pm 02 Page 1 of 1 000101 Sample Name:STD 50 ppb [*"" Sample Info: Data file :C:\HPCHEM\1\DATA\FC000002.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 4:57:02 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method . Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000002.D) API-ES, Neg, SIM, Frag: Var r! 7.228- C8 Acic 2500|.j i nk' s 1 2000- 1500- 1 2 1 1 5 pi 1000- 500-- _________ L. ' ' ', . . j . . -r | r i 246 'MSD1 469, EIC=468.7:469.7 (FC000002.D) API-ES, Neg, SIM, Frag: Var 'i ' ' ' I 8 min 4000 8.012- C10 Surrogate, 3500 H 3000 2500 2000 1500- 1000 500 0-1 i Compound Amount (ng/mL) R.T. 23 Acid 22.42 l0 Surrogat 19.93 7.228 8.012 Area 20919 30608 LL D o min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 >000414 *** End of Report *** Thu, 8. Jan. 2004 04:20:50 pm 02 ! Page 1 of 1 000102 Sample Name:STD 100 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000003.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 5:12:37 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METH0DS\112 003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000003.D) API-ES, Neg, SIM, Frag: Var 7.229- C8 Acid 4000- 1 3 2 1 5 pi 3000- 2000- 1000- o- 1' 1r 111i 111i 1 246 *MSD1 469, EIC=468.7:469.7 (FC000003.D) API-ES, Neg, SIM, Frag: Var i ____________ - ____________________ 11r 111I 8 min 7000 J 8.014- C10 Surrogate 6000 -j 5000 4000 3000- 2000 i 1000 j : o- Compound Amount (ng/mL) R.T. *8 Acid 78.98 10 Surrogat 77.98 7.229 8.014 -CD - CM Area 40896 59840 JV ' 1i 1 8 1 1r min Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 s \ PC00414 *** End of Report *** Thu, 8. Jan. 2004 04:21:44 pm 0022 Page 1 of 1 000103 Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000004.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 5:28:08 PM Seq Line Vial No. Inj . N o . Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEMX1\METHODS\112003.M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000004.D) API-ES, Neg, SIM, Frag: Var 12000- 7.235- C8 Acid. 10000- 8000- 6000- 4000- 2000- 1 4 3 1 5 pi --I----------- r~ *MSD1 469, EIC=468.7:469.7 (FC000004.D) API-ES, Neg, SIM, Frag: Var 17500- 8.013- C10 Surrogate, 15000- 12500- 10000^ 7500 -j 5000 J 2500- o-t min Compound Amount (ng/mL) R.T. *8 Acid 263.53 10 Surrogat 262.83 7.235 8.013 Area 106083 152925 Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 04:22:30 pm 0023 Page 1 of 1 000104 Sample Name:STD 500 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\FC000005.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 5:43:40 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method --. Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\112003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. ... *MSD1 369, EIC=368.7:369.7 (FC000005.D) API-ES, Neg, SIM, Frag: Var 7.241 - C8 Aclc -- 20000 - 15000- ... 10000- 1 5 4 1 5 pi 5000- o- ''' 1' 2 ' ' 1' ' 1 I 46 *MSD1 469, El0=468.7:469.7 (FC000005.D) API-ES, Neg, SIM, Frag: Var yl ' _ rT > 8 35000 ^ 8.017 - C10 Surrogate _ r. f min -- 30000 ^ 25000 20000 - 15000- 10000- 5000 - 0 -,. T , -p- . , 24 Compound Amount (ng/mL) R.T. ,Z3 Acid 527.92 10 Surrogat 532.32 7.241 8.017 n Area 199467 288630 i 1' 6 _ L ___________________ ' 't 8 r min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 I[ PC00414 *** End of Report *** Thu, 8. Jan. 2004 04:23:18 pm 024 Page 1 of 1 000105 Sample Name:STD 750 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\FC000006.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 5:59:20 PM Seq Line Vial No. Inj . No . Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODSU12003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000006.D) API-ES, Neg, SIM, Frag: Var 30000 - 7.220- C8 Acid 25000 - 20000 H 15000- 10000- 5000- 0~T~ 4 *MSD1 469, EIC=468.7:469.7 (FC000006.D) API-ES, Neg, SIM, Frag: Var 7.996- C10 Surrogata 40000- 30000 - 20000 - 10000- 1 6 5 1 5 pi --1----------- 1- Compound Amount (ng/mL) R.T. 8 Acid 750.22 10 Surrogat 752.85 7.220 7.996 Area 277987 399682 Signal MSD1 369, EIC=3 68.7:369.7 MSDl 469, EIC=468.7:469.7 i-- PC00414 *** End of Report *** Thu, 8. Jan. 2004 04 :24 :04 pm 0025 Page 1 of 1 000106 Sample Name:STD 1500 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\FC000008.D Injection Date Acq Operator Instrument .. Dilution 11/20/03 jmiller PC00414 1 6:30:33 PM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method -- Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\112003.M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000008.D) API-ES, Neg, SIM, Frag: Var 7.236- C8 Acid 50000 - 1 8 7 1 5 pi 40000 - 30000 - 20000 - 10000- MSD1 469, EIC=468.7:469.7 (FC000008.D) API-ES, Neg, SIM, Frag: Var 90000 8.026- C10 Surrogate 80000 i 70000 60000 50000 40000 30000 20000 10000 - i 0 1 1 1 1 1 1--2 1 4 I--- 1 ' m | ' > ' r 6 8 min ompound Amount (ng/mL) R.T. Area Signal eg Acid 1445.01 -0 Surrogat 1444.38 7.236 8.026 523394 747916 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 'C00414 *** End of Report *** Thu, 8. Jan. 2004 04:25:19 pm 0027 Page 1 of 1 000107 Sample Name:Solvent blank Sample Info : Data file :C:\HPCHEM\1\DATA\FC000009.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 6:46:01 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method ' Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:46:06 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 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 04:26:06 pm 0028 Page 1 of 1 000108 Sample Name:L0001308-22 Sample Info : 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11337194\A370560\FC000010.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 7:01:33 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 10 11 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORVI1337194\A370560\FC000010.D) API-ES, Neg, SIM, Frag: Var 16000- 7.221 - C8 Acid 14000 12000- 10000- 8000 6000- 4000 J 2000 od *MSD1 469, EIC=468.7:469.7 (CHEMSTORM1337194\A370560\FC000010.D) API-ES, Neg, SIM, Frag: Var 30000 - 7.995- C10 Surrogatesi 25000 - 20000 - 15000- 10000- 5000-I 0- Compound Amount (ng/mL) R.T. Z8 Acid 453.59 10 Surrogat 612.12 7 .221 7 .995 Area 173212 328815 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 * End of Report *** Thu, 8. Jan. 2004 03:11:12 pm 0029 Page 1 of 1 000109 Sample Name:LOOO1308-23 Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11337379\A373312\FCOOOOil.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 7:17:05 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : 11 12 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11337379\A373312\FC000011.D) API-ES, Neg, SIM, Frag: Var 3500 H 7.227- C8 Acid 1 3000 2500- 2000 J 1500 1000 5 0 0 -| 0 __ T8_________ MSD1 469, EIC=468.7:469.7 (CHEMSTORU1337379\A373312\FC000011.D) API-ES, Neg, SIM, Frag: Var 25000 - 8.015- C10 Surrogate, 20000 15000- 10000- 5000- c ompound 1 2 Amount (ng/mL) 1 1--- 1-- 4 R.T. -)--- '--- '---i i 1 68 Area Signal 1--- 1--- r min 8 Acid 48.98 10 Surrogat 391.61 7.227 8.015 30300 217774 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:12:27 pm 03G Page 1 of 1 OOOllO Sample Name:L0001308-l Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\11337644\A376064\FC000012.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 7:32:42 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method -. Last Changed FC8-10 .M C :\HPCHEMN1\METHODS U12003.M 1/8/04 02:45:39 pm 1 12 13 1 5 pi Compound Amount (ng/mL) R.T. "8 Acid 0.00 10 Surrogai 644.03 0.000 8.021 Area 0 344887 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:13:07 pm 0031 Page 1 of 1 000111 Sample Name :L0001308-2 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11337804\A378880\FC000013.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmi H e r PC00414 1 7:48:16 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:45:39 pm 1 13 14 1 5 pi Compound Amount (ng/mL) R.T. --8 Acid 0.00 10 Surrogat 328.79 0.000 7.997 Area 0 186139 Signal MSD1 369, EIC=3 68.7:3 69.7 MSD1 469, EIC=468.7:469.7 7C00414 *** End of Report *** Thu, 8. Jan. 2004 03:13:31 pm 0032 Page 1 of 1 000112 Sample Name:L0001308-4 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11337966\A381760\FC000014.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 8:03:50 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm 1 14 15 1 5 pi Compound Amount (ng/mL) R.T. -8 Acid 0.00 10 Surrogat 707.26 7.219 8.003 Area 5564 376727 Signal MSD1 369, EIC=3 68.7:3 69.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:14:07 pm 0035 Page 1 of 1 000113 Sample Name :L0001308-5 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11338127\A385024\FC000015.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 8:19:26 PM Seq Line Vial No. Inj . No . Inj. Voi. : : : : Acq. Method Analysis Method -- * Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm 1 15 16 1 5 pi Compound Amount (ng/mL) R.T. " 8 Acid 0.00 10 Surrogat 392.49 0.000 8.018 Area 0 218217 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:14:59 pm 0 34 Page 1 of 1 000114 Sample Name :L0001308-7 Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11338314\A387648\FC000016.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 8:35:04 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 16 17 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:45:39 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11338314\A387648\FC000016.D) API-ES, Neg, SIM, Frag: Var 7.234 - C8 Acid 40000 - 30000 - 20000 - 10000- 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM1338314\A387648\FC000016.D) API-ES, Neg, SIM, Frag: Var 40000 - 8.018- C10 Surrogate 35000 - 30000 - 25000 - 20000 ^ 15000- 10000d 5000- 0- 1 _L Compound Amount (ng/mL) R.T. "8 Acid 1339.98 10 Surrogat 666.04 7.234 8.018 Area 486298 355969 Signal MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:15:51 pm 35 Page 1 of 1 000115 Sample Name:L0001308-8 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11338477\A390656\FC000017.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 8:50:40 PM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm LC/MS analysis of perfluorooctanoic acid. 1 17 18 1 5 pi 3 Acid 0.00 l0 Surrogat 405.08 7.240 8.012 7681 224557 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 >C00414 *** End of Report *** Thu, 8. Jan. 2004 03:17:16 pm 0036 Page 1 of 1 000116 Sample Name:L0001308-10 Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11338658\A393600\FC000018.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 9:06:20 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : 18 19 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11338658\A393600\FC000018.D) API-ES, Neg, SIM, Frag: Var 7.244 - C8 Acid 40000 - 30000 - 20000 - 10000- 0-- *MSD1 469, EIC=468.7:469.7 (CHEMSTORYI1338658\A393600\FC000018.D) 1 ~r 8 API-ES, Neg, SIM, Frag: Var 40000- 8.015- C10 Surrogate 35000 -j 30000 - 25000 - 20000 - 15000 -; 10000^ 5000 -j 0- 11111 -[--- 1--- '--- 1 1 ' 1 1 1 246 8 min ompound Amount (ng/mL) R.T. Area Signal --8 Acid 1266.20 10 Surrogat 666.34 7.244 8.015 460236 356121 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03 :18 :01 pm 0037 Page 1 of 1 000117 Sample N a m e :L0001308-11 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\1133 8818\A3 95840\FC000019 .D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 9:21:59 PM Seq Line Vial No. Inj . N o . Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:45:39 pm 1 19 20 1 5 pi Compound Amount (ng/mL) R.T. 8 Acid 0.00 10 Surrogat 396.07 7.236 8.004 Area 5278 220023 Signal MSDl 369, EIC=368.7 :369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:19:17 pm 0038 Page 1 of 1 000118 Sample Name:STD 500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11339001\A398848\FC000020.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 9:37:33 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\112 003 .M 1/8/04 02:45:39 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11339001\A398848\FC000020.D) API-ES, Neg, SIM, Frag: Var 7.238- C8 Acid 20000 - 15000- 10000- 5000- _____________ _____________ H_____________ O_____________ O__________ MSD1 469, EIC=468.7:469.7 (CHEMSTORU 1339001\A398848\FC000020.D) API-ES, Neg, SIM, Frag: Var 35000 - 8.008- C10 Surrogate mm 30000 - 25000 - 20000 - 15000- 100007 5000 J 0- Compound Amount (ng/mL) R.T. 8 Acid 542.63 10 Surrogat 546.18 7.238 8.008 Area 204664 295610 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:20:06 pm 0039 Page 1 of 1 000119 Sample Name :Solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11339162\A401344\FC000021.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 9:53:02 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method -* Last Changed FC8-10.M C :\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm 1 21 92 1 5 pi Compound Amount (ng/mL) R.T. 0 Acid 0.00 L0 Surrogat 0.00 7.238 0.000 Area 477 0 Signal MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:20:53 pm 0040 Page 1 of 1 000120 Sample Name :L0001308-13 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11339324\A404096\FC000022-D 1 ,SJB Acid 0.00 10 Surrogat 696.93 7.222 8.002 2273 371523 MSD1 369, EIC=3 68.7:3 69.7 MSDl 469, EIC=468.7:469.7 [ PC00414 *** End of Report *** 004 i Thu, 8. Jan. 2004 03 :22 :14 pm Page 1 of 1 000121 Sample Name:L0001308-14 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11339485\A406464\FC000023.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 10:24:08 PM Seq Line Vial No. Inj . N o . Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\112003 .M 1/8/04 02:45:39 pm 1 23 22 1 5 pi Compound Amount (ng/mL) R.T. 3 Acid 0.00 L0 Surrogat 403.03 0.000 8.002 Area 0 223526 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 >C00414 *** End of Report *** Thu, 8. Jan. 2004 03:22:56 pm 0042 Page 1 of 1 000122 Sample Name :L0001308-16 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11339647\A409408\FC000024.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 10:39:44 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm 1 24 23 1 5 pi Compound Amount (ng/mL) R.T. .08 Acid 49.31 10 Surrogat 732.49 7.224 8.004 Area 30418 389428 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:24:08 pm u043 Page 1 of 1 000123 Sample Name :L0001308-17 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11339761\A411904\FC000025.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 10:55:20 PM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method ... Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm 1 25 24 1 5 pi lompound Amount (ng/mL) R.T. C,8 Acid 0.00 L0 Surrogat 436.81 7.218 8.000 Area 670 240538 Signal MSDl 369, EIC=3 68.7:3 69.7 MSDl 469, EIC=468.7:469.7 >C00414 *** End of Report *** U044 Thu, 8. Jan. 2004 03 :27 :25 pm Page 1 of 1 000124 Sample Name:L0001308-19 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11339850\A414784\FC000026.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 11:10:54 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEMX1\METH0DS U12003.M 1/8/04 02:45:39 pm 1 26 25 1 5 pi Zompound Amount (ng/mL) R.T. "3 Acid 0.00 L0 Surrogat 763.22 7.228 8.006 Area 7461 404905 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** U045 Thu, 8. Jan. 2004 03:37:42 pm Page 1 of 1 000125 Sample Name:L0001308-20 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11339937\A417664\FC000027.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 11:26:30 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEMN1\METHODS\112003.M 1/8/04 02:45:39 pm 1 27 26 1 5 pi Compound Amount (ng/mL) R.T. a.3 Acid 0.00 10 Surrogat 374.67 0.000 8.002 Area 0 209243 Signal MSD1 369, EIC=3 68.7:3 69.7 MSD1 469, EIC=468.7:469.7 ?C00414 *** End of Report *** Thu, 8. Jan. 2004 03:38:31 pm U46 Page 1 of 1 00l2e Sample Name:STD 500 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11340049\A420608\FC000028.D Injection Date Acq Operator Instrument Dilution 11/20/03 jmiller PC00414 1 11:42:04 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : 28 4 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm LC/MS analysis of perfluorooctanoic acid. MSD1 369, EIC=368.7:369.7 (CHEMSTORY11340049\A420608\FC000028.D) API-ES, Neg, SIM, Frag: Var 22500 7.221 - C8 Acic 20000 -j 17500 15000 12500 10000 7500 5000 r] 2500 0 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1340049\A420608\FC000028.D) API-ES, Neg, SIM, Frag: Var 8.003- C10 Surrogate* min 30000 - 25000 - 20000 H 15000- 10000- 5000- 0- ii :ompound Amount (ng/mL) R.T. CIS Acid 504.95 .0 Surrogat 511.66 7.221 8.003 Area 191355 278229 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 1 'C00414 *** End of Report *** (J047 Thu, 8. Jan. 2004 03:39:13 pm Page 1 of 1 000127 Sample Name:Solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11340137\A423616\FC00002 9.D Injection Date Acg Operator Instrument Dilution 11/20/03 jmiller PC00414 1 11:57:31 PM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm 1 29 92 1 5 pi Compound Amount (ng/mL) R.T. Acid 0.00 .0 Surrogat 0.00 7.240 0.000 Area 325 0 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 'C00414 *** End of Report *** Thu, 8. Jan. 2004 03:40:19 pm 0 48 Page 1 of 1 000128 Sample Name:STD 50 ppb * Sample Info : Data file :C :\HPCHEM\1\DATA\FC000030.D Injection Date Acq Operator Instrument Dilution 11/21/03 jmiller PC00414 1 12:13:02 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000030.D) API-ES, Neg, SIM, Frag: Var 2500- 7.244- C8 Acid 2000- 1500- 1000- 500- 1 30 1 1 5 ul 3500 MSD1 469, EIC=468.7:469.7 (FC000030.D) API-ES, Neg, SIM, Frag: Var 8.007- C10 Surrogate min 3000 2500 H 2000 1500H 1000 500 H --- !--- ,--1--- --- 1--1--- --- 1- l 1 -- ,--- ,--- 1--- .--- 1--- --- r 2 4 6 8 min Compound Amount (ng/mL) R.T. Area Signal 7.8 Acid 20.75 L0 Surrogat 17.57 7.244 8.007 20329 29419 MSDl 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 049 04:33:53 pm Page 1 of 1 000129 Sample Name:STD 100 ppb Sample Info : Data file :C:\HPCHEM\1\DATA\FC000031.D Injection Date Acq Operator Instrument Dilution 11/21/03 jmiller PC00414 1 12:28:34 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000031 .D) API-ES, Neg, SIM, Frag: Var 7.241 - C8 Ado i 4000- 1 31 2 1 5 pi 3000- 2000- 1000- 0 -- MSD1 469, EIC=468.7:469.7 (FC000031 .D) API-ES, Neg, SIM, Frag: Var 7000 8.008 - C10 Surrogate 6000 5000- 4000- 3000 2000 1000-1 0 min Compound Amount (ng/mL) R.T. "8 Acid 75.92 L0 Surrogat 73.67 7.241 8.008 Area 39814 57670 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 ?C00414 *** End of Report *** Thu, 8. Jan. 2004 04 :38 :25 pm L Page 1 of 1 000130 Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000032.D Injection Date Acq Operator Instrument Dilution 11/21/03 jmiller PC00414 1 12:44:06 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. ' MSD1 369, EIC=368.7:369.7 (FC000032.D) API-ES, Neg, SIM, Frag: Var 12000- 7.240- C8 Acid 10000 8000- 6000- 4000- 2000- 1 32 3 1 5 pi *MSD1 469, EIC=468.7:469.7 (FC000032.D) API-ES, Neg, SIM, Frag: Var 8 17500- 8.007 - C10 Surrogate min 15000- 12500 -j 10000- 7500- 5000- 2500 -j 0-- Compound Amount (ng/mL) R.T. -8 Acid 262.18 10 Surrogat 263.18 7.240 8.007 Area 105604 153103 min Signal MSD1 369, EIC=3 6 8 .7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 04:38:54 pm 51 Page 1 of 1 noOl31 Sample Name:STD 500 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000033.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 11/21/03 jmiller PC00414 1 12:59:38 AM Seq Line Vial No. Inj. No. Inj. Vol. FC8-10,M 1 C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:46:06 pm : : : : LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000033.D) API-ES, Neg, SIM, Frag: Var 7.238- C8 Acic 20000 - 1 33 4 1 5 pi 15000- 10000- 5000- 0-- *MSD1 469, ElC=468.7:469.7 (FC000033.D) API-ES, Neg, SIM, Frag: Var 35000 8.008- C10 Surrogate 30000 25000 20000 15000- 10000^ 5000- 0 --- !--- ,---.--- '--- j- --!--- 1--- 1---1--- [--- 1--- 1--- 1--- r 2 4 6 8 min ompound Amount (ng/mL) R.T. Area Signal VS Acid 538.75 L0 Surrogat 540.77 7.238 8.008 203294 292886 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 3C00414 *** End of Report *** Thu, 8. Jan. 2004 04:39:29 pm U52 Page 1 of 1 000132 Sample Name:STD 750 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000034.D Injection Date Acg Operator Instrument Dilution 11/21/03 jmiller PC00414 1 1:15:13 AM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000034.D) API-ES, Neg, SIM, Frag: Var 7.238 - C8 Acid 30000 - 25000 20000 - 15000- 10000- 5000- 0-h *MSD1 469, EIC=468.7:469.7 (FC000034.D) API-ES, Neg, SIM, Frag: Var 8 50000-j 8.014 - C10 Surrogate, 40000- 30000 - 20000 - 10000- 1 34 5 1 5 pi min :ompound 1 2 Amount (ng/mL) 1--- 1 i-- --,--- --- !------ 146 ' R.T. Area --- 1--- 1--- ,---- ,---8 min Signal ZB Acid 780.73 LO Surrogat 783.24 7.238 8.014 288762 414987 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 'C00414 *** End of Report *** Thu, 8. Jan. 2004 04:39:59 pm U055 Page 1 of 1 000133 Sample Name:STD 1000 ppb Sample Info : 1 Data file :C:\HPCHEM\1\DATA\FC000035.D Injection Date Acq Operator Instrument Dilution 11/21/03 jmiller PC00414 1 1:30:48 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 35 6 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\112003 .M 1/8/04 02:46:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000035.D) API-ES, Neg, SIM, Frag: Var 40000 / 7.235- C8 Acic 35000 30000 / 25000 / 20000 / 15000 / 10000/ 5000/ 0 J v_ , . . , . T . -| T I i 1 i 1 1 2468 *MSD1 469, EIG=468.7:469.7 (FC000035.D) API-ES, Neg, SIM, Frag: Var : 8.003 - C10 Surrogate 1^ 1r min 50000 40000 : 30000 ^ 20000 ; 10000^ r 1' 11i' 1- - - - - - 1 i- - - - - 1- - - - - - - '- - - - - - 1- - - - - - 1- - - - - 1- - - - - - - 1- - - - - - 1- - - - - - 1- - - - - 1- - - - - - - 1- - - - - - 1- - - - - - r ____________________________ 2__________________4__________________6__________________8________________min Compound Amount (ng/mL) R.T. Area Signal "*8 Acid 1034.12 10 Surrogat 1039.70 7.235 8.003 378265 544129 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** u D54 Thu, 8. J a n . 2004 04:40:31 pm Page 1 of 1 000134 Sample Name:STD 1500 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11336955\A367936\FC000036.D Injection Date Acq Operator Instrument Dilution 11/21/03 jmiller PC00414 1 1:46:24 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 36 7 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\112003.M 1/8/04 02:45:39 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1336955\A367936\FC000036.D) API-ES, Neg, SIM, Frag: Var 60000 - 7.235 - C8 Acid, 50000 - 40000 - 30000 - 20000 - 10000- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1336955\A367936\FC000036.D) API-ES, Neg, SIM, Frag: Var 9000080000 -j 8.003 - C10 Surrogate. ] min 70000 - 60000 - 50000 - 40000 - 30000 20000 10000j 0- mm Compound Amount (ng/mL) R.T. Area Signal --3 Acid 1486.37 L0 Surrogat 1479.86 7.235 8.003 538003 765777 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Thu, 8. Jan. 2004 03:10:41 pm 055 Page 1 of 1 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 .ogin Login #: L0001308 > 1,418 Project: P0000419 Project Storage: Submitted By: Michael D. Aucoin Status: Unreceived Login Type: Immediate Receipt of Samples Started: T Date Start: 11/14/2003 8:43:13AM Due Date: 11/28/2003 Received Date: 11/14/2003 Received By: AMMERMAN, MARK Spread Sample: Label: Project Title/Typej Conform COC Sample: Conform COC: Conform Sample: Conform Request: True True True True Login Notes: Conform Notes: Package PK0001882 Carton Packages / Containers Mail Date / Condition Shipper /_ID Temp. Control / Temperat 11/13/2003 2:00:14PM Package & Contents Uncompromised FEDEX 8363913020070200 RT 0.00 Direction / Handled By RECEIVED AMMERMAN, MARK Container # Gross Weight C0019829 7.2 g C0019830 7.2 g COOt9831--------- ------ 7:2-g~ C0019832 7.2 g C0019833 7.2 g G0949834---------------7.2 g - C0019835 7.2 g C0019836 7.2 g 6001083?-------------- ^ T ~ C0019838 7.2 g C0019839 7.2 g 69019840---------------TtS-O- C0019841 7.2 g C0019842 7.2 g C0010843---------------f i t r C0019844 7.2 g C0019845 7.2 g 60010846--------------- C0019847 7.2 g C0019848 7.2 g CO019FUS-------------- 7& g- C0019850 7.2 g COO19851 7.2 g 60019832------ ------- 7.2 g - pH Miscellaneous Item Key None 11/14/2003 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 Mfg. Lot ICOC Description 0056 Report Version: Nov 13 2003 4:51PM Page 1 of 5 Instance: 0003t^ Mfg. ID R0072755 R0072755 Sample ID L0001308-0001 L0001308-0002 -feeootaoo 0 0 0 3 L0001308-0004 L0001308-0005 L0001300^0008L0001308-0007 L0001308-0008 L00Q13Q8 0000" L0001308-0010 L0001308-0011 L0001000^0012 L0001308-0013 L0001308-0014 -LOO&iaOfl 0048-- L0001308-0016 L0001308-0017 LQQ01300 00<HK L0001308-0019 L0001308-0020 i nnniofi nnn L0001308-0022 L0001308-0023 ' 'vT11ff nnnt" 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-E2 A WWK-A-AMSFBLK-E2 B WWK-A-AMCrDLK'*Gg-0 WWK-A-AMS1-E2 A WWK-A-AMS1-E2 B WWK-A-AMS1 E2 C WWK-A-AMS2-E2 A WWK-A-AMS2-E2 B WWK A AMS2 E2G-- WWK-A-AMS3-E2 A WWK-A-AMS3-E2 B WWK-A-AMS3-E2 G WWK-A-AMS4-E2 A WWK-A-AMS4-E2 B WWK-A"AM04-E G WWK-A-AMS5-E2 A WWK-A-AMS5-E2 B WWK-A-AMG5-E2 e WWK-A-AMS6-E2 A WWK-A-AMS6-E2 B WWK-A-AMQG-E3-CControl 1 A Control 1 B Control 1-6-------------' fJa O Date Sampled Date Received f e t . t r 01^_ 11/13/2003 A B ovAy. 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 11/13/2003 Date Due 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/28/2003 11/14/2003 Login.rpt 0057 Report Version: Nov 13 2003 4:51PM Page 2 of 5 Instance: R0072755 " L0001308-0001 Container C0019829 / Other / NONE L0001308-0002 Container C0019830/Other/NONE - L0001308-0003 Container C0019831 / Other/NONE L0001308-0004 Container C0019832/O ther/NO NE L0001308-0005 Container C0019833/ Other/ NONE L0001308-0006 Container C0019834/O ther/NO NE L0001308-0007 Container C0019835/Other/NONE L0001308-0008 Container C0019836/Other/NONE L0001308-0009 Container CO019837 / Other / NONE L0001308-0010 Container C0019838/O ther/NO NE L0001308-0011 Container C0019839/Other/NONE L0001308-0012 Container 11/14/2003 Login.rpt Login Bottles Method Method Method Method Method Method Method Method Method Method Method Method --- u058 Report Version: Nov 13 2003 4:51PM Page 3 of 5 Instance: ocoue R0072755 C0019840/ Other /NONE r L0001308-0013 Container C0019841 / Other/NONE L0001308-0014 Container C0019842/Other/NONE L0001308-0015 Container CO019843 / Other / NONE " l.0001 308-0016 Container ~ CO019844 / Other / NONE L0001308-0017 f" Container i C0019845/O ther/NO NE ***L00013 0 8 - 0 0 1 8 Container CO019846/ Other /NONE L0001308-0019 Container C0019847/O ther/NO NE L0001308-0020 Container CO019848 / Other / NONE \0001308-0021 Container " * C0019849 / Other / NONE L0001308-0022 Container C0019850 / Other / NONE -L0001308-0023 Container CO019851 / Other/NONE l L0001308-0024 Container C0019852/Other/NONE _ 11/14/2003 Login.rpt Method Method Method Method Method Method Method Method Method Method Method Method u059 Report Version: Nov 13 2003 4:51PM Page 4 of 5 Instance: n/'l 4 R0072755 R0072755 11/14/2003 Login.rpt Report Version: Nov 13 2003 4:51PM Page 5 of 5 QJ Instance: R0072755 OCCl4 R0072755 Composite Number of Containers 00014jf CHAIN OF CUSTODY/ANALYSIS REQUEST FORM RESEARCH 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 _____ PROJECT INFORMATION ANALYSES REQUESTED Client (name & address): h D QvW \ /Od&ViA.(\iX\o1A \ p~<^r\S u Phone: C 'bQft) ^ 'X- \ W0^ Fax: ' Sampler: fZOC 356? Project Manager (Name & E-mail Address): rY\ Project Name: ^ (V \f RO. #: Quotation #: r\ l\<\ \ \ r^ O Please fill o u t this form completely to ensure correct analysis an d proper h a n d lin g o f y o u r sam ples. rQ SAM PLE ANALYSIS xExyLIM S# Client Sample Identification Collection Collection Date Time Orwt \j0\O\~ Pr ' Pr (ALV.*(D M iqlf 7* lO\AjVs"fV-'Pr'VXSV VOvAJK - f t r HfVp/VS2>- p/7 J L fcl jL TT 1/0 V(Y\S>^' 1 vJ 'hrft-- s i___ \Zh f iCfrSih Z 2 Specify Matrix Com m ents 1 PrX 'rCeAib ^ W V . \ fv;r V ) peer _L PRC fRC LAB USE ONLY CHAIN OF CUSTODY Relinquished by D a te T im e C ooler ID # fio ec* U, Cooler Temp. (C) xi xO x 'T / M/2I1& tv/7 OTHER INFORM ATIO N II 1 . i _ _ i _ _ I _ _ _ I _ _ f JI 1 4- ** jL A y % PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: CD Sample results only I I Add case narrative CD Add quality control summary CD Add calibration summary CD Add raw data Other L _ r! ,,I. DCV.3-0J? Proven Results. 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