Document aJBE6kqrEbqVQogGED8qLNGmB

Attachment 2 Analytical Report Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 5 Exygen Research Report No. L0001400 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 i\5 CO Cp cn CO 1 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 1 of 7 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. Sample WWK-A-AMS4-E5 had sampler problems during collection. No results are reported for this sample. 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 000206 Results Summary Request # WWK-A-AMS1-E5 A WWK-A-AMS1-E5 B WWK-A-AMS1-E5 C WWK-A-AMS1-E5 (Total) Air Volume Sampled (L) 1480 1480 1480 C8 Acid (mq/m3) < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS2-E5 A WWK-A-AMS2-E5 B WWK-A-AMS2-E5 C WWK-A-AMS2-E5 (Total) 1459 1459 1459 0.0007 < 0.00007 NA 0.0007 WWK-A-AMS3-E5 A WWK-A-AMS3-E5 B WWK-A-EMS3-E5 C WWK-A-EMS3-E5 (Total) 1460 1460 1460 0.0007 < 0.00007 NA 0.0007 WWK-A-AMS5-E5 A WWK-A-AMS5-E5 B WWK-A-AMS5-E5 C WWK-A-AMS5-E5 (Total) 1462 1462 1462 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS6-E5 A WWK-A-AMS6-E5 B WWK-A-AMS6-E5 C W W K-AAMS6-E5 (Total) 1479 1479 1479 < 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 Fraction Description A Frit Extract B 1st set beads extract C 2nd set beads extract (not analyzed) ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 3 of 7 000207 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) 508 C8 Acid (percent recovery 102 Blanks Request # WWK-A-AMSFBLK-E5 A WWK-A-AMSFBLK-E5 B Voi. Of Air (L) 0 0 C8 Acid (uq/fraction) <0.10 <0.10 000208 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-E5 A WWK-A-AMSFB LK-E5 B WWK-A-AMS1-E5 A WWK-A-AMS1-E5 B WWK-A-AMS2-E5 A WWK-A-AMS2-E5 B WWK-A-AMS3-E5 A WWK-A-AMS3-E5 B WWK-A-AMS5-E5 A WWK-A-AMS5-E5 B WWK-A-AMS6-E5 A WWK-A-AMS6-E5 B Control Spike A Control Spike B Amount Spiked (ppb) 500 500 500 500 500 500 500 500 500 500 500 500 500 500 Amount Recovered (ppb) 558 295 500 319 490 334 482 289 496 315 488 317 552 331 * Surrogate recovery outside of advisory range. Percent Recovery (%) 112 59* 100 64* 98 67* 96 58* 99 63* 98 63* 110 66* ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 000209 Calculations Request # WWK-A-AMSFBLK-E5 A WWK-A-AMSFBLK-E5 B WWK-A-AMS1-E5 A WWK-A-AMS1-E5 B WWK-A-AMS2-E5 A WWK-A-AMS2-E5 B WWK-A-AMS3-E5 A WWK-A-AMS3-E5 B WWK-A-AMS5-E5 A WWK-A-AMS5-E5 B WWK-A-AMS6-E5 A WWK-A-AMS6-E5 B Control Spike A Control Spike B Vol. Of Air (L) 0 0 1480 1480 1459 1459 1460 1460 1462 1462 1479 1479 0 0 C8 Acid (raw-ppb) <10 <10 < 10 < 10 1020 < 10 1074 <10 <10 < 10 <10 < 10 508 <10 C8 Acid (ug/fraction) <0.10 <0.10 <0.10 <0.10 1.0 <0.10 1.0 <0.10 <0.10 <0.10 <0.10 <0.10 0.51 <0.10 C8 Acid (mg/m3) < 0.00007 < 0.00007 0.0007 < 0.00007 0.0007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 000210 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 7 Example Calculation For sample WWK-A-AMS2-E5 A C8 Acid, = [1020 ng/ml 1000 L)] of C8 Acid X (1 ml) X (1 ug/ 1000 ng) X (1 mg / 1000 ug) ] / [(1459 L) x (1 m3 / = 0.0007 mg / m3 Signatures 1 Paul Connolly, LCMS Team Leader a. mfL Oohn M. Flaherty, Vice President Other Lab Members Contributing to Data James Miller M2-S7<7 4 Date Date ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 7 000211 000212 Table 1. Login Information / Field Data Sample ID Exygen Lab ID Date Received Description WWK-A-AMSFBLK-E5 A WWK-A-AMSFBLK-E5 B WWK-A-AMSFBLK-E5 C WWK-A-AMS1-E5 A WWK-A-AMS1-E5B WWK-A-AMS1-E5C WWK-A-AMS2-E5 A WWK-A-AMS2-E5 B WWK-A-AMS2-E5 C WW K-A-AMS3-E5 A WWK-A-AMS3-E5 B WWK-A-AMS3-E5 C WWK-A-AMS5-E5 A WWK-A AMS5-E5 B WWK-A-AMS5-E5 C WWK-A-AMS6-E5 A WWK-A-AMS6-E5 B WWK-A AMS6-E5 C Control Spike A Control Spike B Control Spike C L0001400-1 L0001400-2 L0001400-3 L0001400-4 L0001400-5 L0001400-6 L0001400-7 L0001400-8 L0001400-9 L0001400-10 L0001400-11 L0001400-12 L0001400-16 L0001400-17 L0001400-18 L0001400-19 L0001400-20 L0001400-21 L0001400-22 L0001400-23 L0001400-24 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 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 Air Volume Sampled (L) 0 0 0 1480 1480 1480 1459 1459 1459 1460 1460 1460 1462 1462 1462 1479 1479 1479 0 0 0 000213 Table 2. Chain of Custody Sample ID WWK-A-AMSFBLK-E5 A WWK-A-AMSFBLK-E5 B WWK-A-AMSFBLK-E5 C WWK-A-AMS1-E5 A WWK-A-AMS1-E5B WWK-A-AMS1-E5 C WW K-A-AMS2-E5 A WWK-A-AMS2-E5 B WWK-A-AMS2-E5 C WWK-A-AMS3-E5 A WWK-A-AMS3-E5 B WWK-A-AMS3-E5 C WWK-A-AMS5-E5 A WWK-A AMS5-E5 B WWK-A-AMS5-E5 C WWK-A-AMS6-E5 A WWK-A-AMS6-E5 B WWK-A AMS6-E5 C Control Spike A Control Spike B Control Spike C Date Collected 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 11/30/03 NA NA NA Date Received at Exygen 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 12/2/03 Date Extracted by Exygen 12/11/03 12/11/03 NA 12/11/03 12/11/03 NA 12/11/03 12/11/03 NA 12/11/03 12/11/03 NA 12/11/03 12/11/03 NA 12/11/03 12/11/03 NA 12/11/03 12/11/03 NA Date Analyzed by Exygen 12/11 -12/12/03 12/11 -12/12/03 NA 12/11 -12/12/03 12/11 -12/12/03 NA 12/11 -12/12/03 12/11 -12/12/03 NA 12/11 -12/12/03 12/11 -12/12/03 NA 12/11 -12/12/03 12/11 -12/12/03 NA 12/11 -12/12/03 12/11 -12/12/03 NA 12/11 -12/12/03 12/11 -12/12/03 NA ANALYTICAL DATA REVIEW SHEET LC/MS es K A iA \ Analyst -7 ^ - Si^nature/Date Reviewed ^/ i 0010 000214 Sequence: C:\HPCHEM\1\SEQUENCE\121103.S Sequence Table: Method and Injection Info Part: Line Location SampleName "" Method Inj SampleType InjVolume DataFile 1 Vial 1 2 Vial 1 3 Vial 2 4 Vial 3 5 Vial 4 6 Vial 5 7 Vial 6 8 Vial 7 9 Vial 92 10 ' Vial 11 11 Vial 12 12 Vial 13 13 Vial 14 14 Vial 15 15 Vial 16 16 Vial 17 17 Vial 18 18 Vial 19 19 Vial 20 20 Vial 4 21 Vial 92 22 Vial 21 23 Vial 22 24 Vial 23 25 Vial 24 26 Vial 25 27 Vial 26 28 Vial 4 29 Vial 92 30 Vial 1 31 Vial 2 32 Vial 3 33 Vial 4 34 Vial 5 35 Vial 6 36 Vial 7 STD 50 ppb STD 50 ppbSTD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb Solvent'blank L0001400-22 L0001400-23 L0001400-1 L0001400-2 L0001400-4 L0001400-5 L0001400-7 L0001400-8 L0001400-10 L0001400-11 STD 500 ppb Solvent blank L0001400-13 L0001400-14 L0001400-16 L0001400-17 L0001400-19 L0001400-20 STD 500 ppb Solvent blank 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 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 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib Calibration Part: Line Location SampleName' j 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 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 12/11/03 4:46:58 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 000215 Page 1 of 2 Sequence: C:\HPCHEM\1\SEQUENCE\121103.S LCMS3 12/11/03 4:46:58 PM jmiller u 01 2 0 0 0 2 1 6 Page of 2 Method C :\HPCHEM\1\METHODS\121103.M Calibration Table I Ir Calib. Data Modified Calculate Based on Friday, January 09, 2004 4:06:50 PM 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) r Signal 1: MSD1 369, EIC=368.7 :369.7 i Signal 2: MSD1 469, EIC=468.7 :469.7 RetTime Lvl [min] Sig ! Amount [ppb] Area 7.470 8.337 1 l 50.00000 1.05075e4 2 100.00000 1.98922e4 3 250.00000 4.87715e4 4 500.00000 9.17117e4 5 750.00000 1.27971e5 6 1000.00000 1.65424e5 7 1500.00000 2.27786e5 2 1 50.00000 1.44995e4 2 100.00000 2.74226e4 3 250.00000 6.78299e4 4 500.00000 1.26927e5 5 750.00000 1.78723e5 6 1000.00000 2.29796e5 7 1500.00000 3.17153e5 Amt/Area Ref Grp Name 1 4.75851e-3 5.02709e-3 5.12594e-3 5.45187e-3 5.86069e-3 6.04507e-3 6.58513e-3 3.44841e-3 3.64663e-3 3.68569e-3 3.93926e-3 4.19645e-3 4.35168e-3 4.72958e-3 1 1 C8 Acid CIO Surrogate More compound-specific settings: Compound: C8 Acid Time Window : From 7.298 min To 8.298 min Compound: CIO Surrogate Time Window From 8.141 min To 8.946 min Peak Siam Table ***No Entries in table*** \ C00414 1/9/04 4:07:56 PM jmiller uO'i 3 000217 Page 1 of 2 Method C:\HPCHEM\1\METHODS\121103.M Calibration Curves r C8 Acid at exp. RT: 7.470 MSD1 369, EIC=368.7:369.7 Correlation: 0.99699 Residual Std. Dev.: 6799.05760 Formula: y = mx + b m: 151.06015 b: 9309.20748 x: Amount[ppb] y : Area CIO Surrogate at exp. RT: 8.337 MSD1 469, EIC=468.7 :469.7 Correlation: 0.99705 Residual Std. Dev.: 9386.65381 Formula: y = mx + b m: 210.42896 b: 12724.42953 x: Amount[ppb] y : Area C00414 1/9/04 4:07:56 PM jmiller 7 ay U0 !4 000218 Page 2 of 2 LC/MS SYSTEM AND OPERATING CONDITIONS Client: Dupont EXYGEN STUDY: L0001400 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 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 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 Time %A 0.0 70 6.0 10 10.0 10 10.0 STOP Post Time = 4 min. Total run tim e = 14 min. Flow Rate: 0.3 mL/min Injected Volume: 5 pL %B 30 90 90 STOP Page 1 o f 2 ; i fs ' r UU ;S 000219o Instrument : LCMS3 Tue Dec 02 09:17:46 2003 G1946: API_ES Negative mode Page 1 of 3 C:\HPCHEM\1\1946TUNE\ATUNES.TUN 4 Scan: 50.00 - 3000.00 Samples: 8 Thresh: 0 Step: 0.10 29501 peaks Base: 2233.95 Abundance: 1314304 F Raw,Gauss 0.3 100 -i 40 20 - -- 1-- 1-- r--,-- r--1-- -- .-- 1-- r-- r 500 1000 1500 1i 2000 1-- r-' |` 2500 m/z gf Abund 113.00 61000 601.99 21664 1033.97 210944 1633.95 695552 2233.95 1314304 Rel Abund 100.00 35.51 345.81 1140.25 2154.60 Iso m/z 114.02 602.99 1034.95 1634.95 2234.95 Iso Abund Iso Ratio 1982 3.25 4281 19.76 44120 20.92 256896 36.93 652160 49.62 0017 G002rr Instrument : LCMS3 Tue Dec 02 09:17:46 2003 G1946: API_ES Negative mode Page 2 of 3 C :\HPCHEM\1\19 46TUNE\ATUNES.TUN Mode: API--ES Polarity: NEG Fragment Skim2 Lensl Lens2 Iris Gain VAR. WidthGain -128 6.0 WidthOffs VAR -4.0 MassGain- 36.25 19 MassOffs VAR 240 Energy 5.0 OpolPeak 300 OpolKnee 316 3.0 QuadDC 0.00 EMV VCap Status: CapCur ChamCur 2164 Samples 8 4000 Averages 1 StepSize 0.10 63 DryingGas 6.0 1.02 Gas Temp 300 Quad Temp 99 Neb Pres 20 0 18 00022r Instrument : LCMS3 Tue Dee 02 09:17:46 2003 Gl946: API_ES Negative mode Page 3 of 3 C:\HPCHEM\1\1946TUNE\ATUNES.TUN Mass Offset 2.00-, 1.00 0.00 - - 1.00 - Dynamic Parameter Ramp 500 Mass 112.99 1633.95 1000 1500 Setting 0.56 0.63 Mass 601.98 2233.91 Setting 0.67 0.56 2000 Mass 1033.99 2500 Setting 0.64 3000 0019 000223 Run# FCOGo \ To F C obao^ t Sample Name:STD 50 ppb i Sample Info:Warm up i Data file :C :\HPCHEM\1\DATA\FC000001.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 4:50:48 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\ 1\METHODSM21103 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000001 .D) API-ES, Neg, SIM, Frag: Var 7.476 - C8 Acid 180016001400- 1200- 1000800600 -j 400200- 1 1 1 1 5 pi *MSD1 469, EIC=468.7:469.7 (FC000001 .D) API-ES, Neg, SIM, Frag: Var 2500- 8.355- C10 Surrogate 2000- 1500- 1000- 500- Compound Amount (ng/mL) R.T. 8 Acid 23.08 10 Surrogat 20.32 7.476 8.355 Area 12796 17000 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 4~ 0 3 ( PC00414 * * * End of Report *** Fri, 9. Jan. 2004 04:51:49 pm 020 Page 1 of 1 000224 Sample Name:STD 50 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\FC000002 .D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 5:06:19 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method . Last Changed FC8-10 .M C : \HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000002.D) API-ES, Neg, SIM, Frag: Var 7.465- C8 Add, 1600- 1400 1200- 1000- 800 600 400 200 2250 MSD1 469, EIC=468.7:469.7 (FC000002.D) API-ES, Neg, SIM, Frag: Var 8.3 34- C10 Surrogate 2000 1750 1500 1250- 1000 ^ 750 500 d 250 1 2 1 1 5 pi min Compound Amount (ng/mL) R.T. C'S Acid 14.95 .0 Surrogat 14.07 7.465 8.334 Area 11567 15685 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 'C00414 *** End of Report *** Fri, 9. Jan. 2004 04:52:42 pm 0 021 Page 1 of 1 0002 Sample Name:STD 100 ppb Sample Info : Data file :C:\HPCHEM\1\DATA\FC000003.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmi H e r PC00414 1 5:21:50 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000003.D) API-ES, Neg, SIM, Frag: Var 3000 7.463- C8 Acid, 2500- 2000 1500- 1000 J 500- 1 3 2 1 5 pi *MSD1 469, EIC=468.7:469.7 (FC000003.D) API-ES, Neg, SIM, Frag: Var 4000- 8.336 - C10 Surrogate 3500- 3000- 2500 -j 2000- 1500 - 1000- 500- 0 -L Compound Amount (ng/mL) R.T. "8 Acid 80.30 10 Surrogat 78.24 7.463 8.336 Area 21439 29188 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 i PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:53 :23 pm 0022 Page 1 of 1 0002 Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000004.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 5:37:30 PM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000004.D) API-ES, Neg, SIM, Frag: Var 7000- 7.461 - C8 Acid 6000- 5000 H 4000- 3000- 2000- 1000- 0- *MSD1 469, EIC=468.7:469.7 (FC000004.D) ~i--- 1--- r_ 6 API-ES, Neg, SIM, Frag: Var 10000-| 8.335 - C10 Surrogate 1 4 3 1 5 pi 8000- 6000- 4000- 2000- 1111i 24 ompound Amount (ng/mL) R.T. ^3 Acid 280.46 10 Surrogat 277.18 7.461 8.335 -j--- 16 '11111 8 min Area Signal 51676 71051 MSDl 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:54:14 pm U023 Page 1 of 1 000227 Sample Name:STD 500 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000005.D Injection Date Acq Operator Instrument ' Dilution 12/11/03 jmiller PC00414 1 5:53:04 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method - Last Changed FC8-10.M C :\HPCHEM\1\METHODS\121103-M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000005.D) API-ES, Neg, SIM, Frag: Var 7.459 - C8 Acid 12000- 1 5 4 1 5 pi 10000- 8000- 6000- 4000- 2 0 0 0 -I 0- " *MSD1 469, EIC=468.7:469.7 (FC000005.D) API-ES, Neg, SIM, Frag: Var 18000- 8.338- C10 Surrogate. 16000 14000H 12000 10000 8000 6000- 4000 J 2000 0-f min mm Compound Amount (ng/mL) R.T. Area Signal -a8 Acid 584.62 10 Surrogat 570.55 7.459 8.338 97622 132785 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:54:56 pm u 024 Page 1 of 1 000278 Sample Name:STD 750 ppb Sample Info: 1 Data file :C:\HPCHEM\1\DATA\FC000006.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 6:08:41 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. "",w *MSD1 369, EIC=368.7:369.7 (FC000006.D) API-ES, Neg, SIM, Frag: Var 17500- 7.471 - C8 Ade 6 5 1 5 pi 15000- 12500- 10000j -- 7500 -j 5000 -j * 2500 -j o' , , 11' T1' ' 111 2 46 *MSD1 469, EIC=468.7:469.7 (FC000006.D) API-ES, Neg, SIM, Frag: Var ' l1 i 111j 8 min 25000 - 8.338- C10 Surrogate 20000 - 15000- 10000- 5000- Compound 1 2 Amount {ng/mL) l 4 R.T. " 8 Acid 829.82 10 Surrogat 828.56 7.471 8.338 1T 11 1 1 6 Area s___ 1 III, 8 mi n Signal 134661 187078 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 f PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:55:23 pm u 025 Page 1 of 1 000229 r! Sample Name:STD 1000 ppb Sample Info: i Data file :C:\HPCHEM\1\DATA\FC000007 .D Injection Date Acq Operator Instrument r *. Dilution 12/11/03 jmiller PC00414 1 6:24:17 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method . Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. j *MSD1 369, EIC=368.7:369.7 (FC000007.D) API-ES, Neg, SIM, Frag: Var 7.461 - C8 Acid 20000 - 1 7 6 1 5 pi 15000- 10000- 5000- - 0 1' ' 1 11' I 24 ^ 11 6 *MSD1 469, EIC=468.7:469.7 (FC000007.D) API-ES, Neg, SIM, Frag: Var LU 11 1 8 30000 - r i 25000 -J 8.335 - C10 Surrogate --, r min 20000 ^ 15000 -J 10000 ^ 5000 - ,,, Compound 1' '1 2 Amount (ng/mL) 1 4 R.T. '8 Acid 1069.28 10 Surrogat 1059.33 7.461 8.335 11 Area 170834 235638 i' 6 1 A__ 1 8 _ 11 min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 i PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:55:42 pm U02 6 Page 1 of 1 000230 Sample Name :STD 1500 ppb Sample Info : Data file :C :\HPCHEM\1\DATA\FC000008.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 6:39:52 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\12110 3 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000008.D) API-ES, Neg, SIM, Frag: Var 30000 - 7.448 - C8 Acid 1 8 7 1 5 pi 25000 - 20000 - 15000- 10000 ^ 5000 0-- J_1 *MSD1 469, EIC=468.7:469.7 (FC000008.D) API-ES, Neg, SIM, Frag: Var 45000 t 8.321 - C10 Surrogatei 40000- 35000 -j 30000 - 25000 r 20000 -j 15000 100005000 -j 0- -- 1--- 1--- ,--- ,--- ,-- 24 J .L -- i--- 1--- '----T | . i i--- r 6 8 min ompound Amount (ng/mL) R.T. Area Signal 3 A c id 1502.72 L0 Surrogat 1492.75 7.448 8.321 236310 326842 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 ?C00414 *** End of Report *** Fri, 9. Jan. 2004 04:56:02 pm U027 Page 1 of 1 0002.71 Sample Name:Solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11570338\A845120\FC000009 .D Injection Date Acq Operator Instrument ,,. Dilution 12/11/03 jmiller PC00414 1 6:55:21 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method .. Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103.M 1/9/04 ' " 04:06:51 pm 1 9 92 1 5 pi Compound Amount (ng/mL) R.T. S Acid 0.00 10 Surrogat 0.00 0.000 0.000 Area 0 0 Signal MSD1 369, EIC=3 68.7:3 69.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:07:36 pm 0028 Page 1 of 1 000232 Sample Name :LO001400-22 Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11570425\A847488\FC000010 .D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 12/11/03 jmiller PC00414 1 7:10:52 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : FC8-10 .M C:\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm 10 11 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1570425\A847488\FC000010.D) API-ES, Neg, SIM, Frag: Var 12000- 7.464 - C8 Acid 10000 8000- 6000 4000 2000- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1570425\A847488\FC000010.D) API-ES, Neg, SIM, Frag: Var 8.333- C10 Surrogate 1600014000- 1200010000- 800060004000 2000 -j 0-- Compound Amount (ng/mL) R.T. "*8 Acid 507.80 10 Surrogat 551.50 7.464 8.333 Area 86017 128777 Signal MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:08:40 pm 029 Page 1 of 1 000233 Sample Name :L000140Q-23 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11570512\A849856\FC000011.D 1 3-3 Acid 0.00 LO Surrogat 331.09 7.466 8.334 3984 82394 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7 :469.7 >000414 *** End of Report *** Fri, 9. Jan. 2004 04:09:24 pm J3 Page 1 of 1 000234 Sample Name:L0001400-1 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11570627\A851712\FC000012.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 12/11/03 jmiller PC00414 1 7:42:01 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : FC8-10.M C :\HPCHEM\1\METHODS\12110 3 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. 1 12 13 1 5 pi -~8 Acid 0.00 10 Surrogat 558.27 0.000 8.336 0 130201, MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:10:19 pm u051 Page 1 of 1 00235 Sample Name:L0001400-2 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11570714\A854912\FC000013.D 1 Acid 0.00 10 Surrogat 295.48 0.000 8.346 0 74902 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7 :469.7 S PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:18:39 pm U032 Page 1 of 1 000236 Sample N a m e :L0001400-4 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\11570831\A857088\FC000014.D 1 ~*8 Acid 0.00 10 Surrogat 500.35 7.489 8.357 880 118012 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:11:28 pm 0 3 Page 1 of 1 000237 Sample Name:L0001400-5 Sample Info : Data file :C :\HPCHEM\1\DATA\Chemstor\11570979\A859264\FC000015.D 1 *8 Acid 0.00 :10 Surrogat 319.07 7.465 8.332 1218 79866 MSDl 369, EIC=368.7 :369.7 MSDl 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:13:29 pm U034 Page 1 of 1 000238 Sample Name :LOO014OO-7 Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11571097\A861056\FC000016.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 8:44:20 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 16 17 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1571097\A861056\FC000016.D) API-E S, Neg, SIM, Frag: Var 7.463- C8 Acid 17500 j 15000 / 12500 j 10000 -J 7500 5000 -j 2500 -j o-------I-------- 1--------1 I--------1-------- 1 ' 1 1 1 !--------1 1 2 46 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1571097\A861056\FC000016.D) / 1' 11 11 1 8 min API-ES, Neg, S M, Frag: Var 16000 ^ 8.336 - C10 Surrogate 14000 12000 ^ 10000^ 8000 6000 4000 ^ 2000 -j 0- ^ 11111 2 Compound Amount (ng/mL) 111 4 R.T. 1' 1 Area 1 6 J. 1 8 ' 1 1 Signal 11 min 8 Acid 1020.01 10 Surrogat 489.74 7.463 8.336 163392 115779 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:14:06 pm 35 Page 1 of 1 000239 Sample Name:L0001400-8 Sample Info: ,, Data file :C:\HPCHEM\l\DATA\Chemstor\11573431\A881472\FC000017.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 8:59:56 PM Seq Line Vial No. Inj. No. Inj. Voi. 17 18 1 Ul "8 Acid 0.00 '10 Surrogai 333.91 7.471 8.338 1743 82989 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7 :469.7 I PC00414 *** End of Report *** Fri, 9. Jan. 2004 04 :25 :41 pm U36 Page 1 of 1 00040 Sample Name:L0001400-10 Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11571274\A863680\FC000018.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 9:15:38 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : 18 19 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1571274\A863680\FC000018.D) API-E S, Neg, SIM, Frag: Var 20000 -j 7.4 56- C8 Acid 17500 ; 15000 j 12500j 10000j 7500 j 5000 r 2500 -j J o,--------,--------1--------[----------------1--------1 j--------'--------'--------1--------1--------1 246 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1571274\A863680\FC000018.D) '------- 1--------!----- ` 8 1 API-ES, Neg, S IM, Frag: Var i min 16000 i 8 .3 28- C10 Surrogate 14000 ^ 12000- 10000- 8000 -j 6000 4000 -j 2000 0- Compound , i , ! i i i i i ' 111 246 Amount (ng/mL) R.T. Area : ' i II., 8 mi n Signal *"3 Acid 1074.05 L0 Surrogat 482.44 7.456 8.328 171556 114243 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:15:37 pm 0037 Page 1 of 1 cocr4i Sample N a m e :L0001400-11 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11573 621\A883264\FC000019.D 1 8 Acid 0.00 10 Surrogat 289.37 7.453 8.326 792 73617 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 i PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:26:15 pm 0038 Page 1 of 1 ooor Sample Name:STD 500 ppb I""' Sample Info : i Data file :C:\HPCHEM\l\DATA\Chemstor\11571392\A865664\FC000020.D 1 Injection Date Acq Operator Instrument ... Dilution 12/11/03 jmiller PC00414 1 9:46:52 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 20 4 1 5 pi Acq. Method Analysis Method -- Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11571392\A865664\FC000020.D) API-ES, Neg, SIM, Frag: Var 12000- 7.466- C8 Acid, 10000- 8000- 6000- 4000- 2000- 16000 8 MSD1 469, EIC=468.7:469.7 (CHEMSTORYI 1571392\A865664\FC000020.D) API-ES, Neg, SIM, Frag: Var 8.334- C10 Surrogate 14000 12000 10000- 8000 6000 J 4000 2000 0-t ./ I Compound Amount (ng/mL) R.T. a8 Acid 504.97 10 Surrogat 516.19 7.466 8.334 Area 85590 121345 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:16:03 pm 0039 Page 1 of 1 000243 Sample Name:Solvent blank Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11571450\A867456\FC000021.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 10:02:21 PM Seq Line Vial No. Inj. No. Inj. Voi. 1 21 92 1 5 pi -*8 Acid 0.00 10 Surrogat 0.00 0.000 0.000 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:16:42 pm U4 Page 1 of 1 GOO Sample Name :L0001400-13 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11571627\A869120\FC000022.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 10:17:54 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method r-- Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm 1 22 21 1 5 pi Compound Amount (ng/mL) R.T. "-8 Acid 0.00 10 Surrogat 475.71 7.455 8.321 Area 8496 112827 Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:19:56 pm 004! Page 1 of 1 GC0245 Sample Name :L0001400-14 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11571685\A871296\FC000023.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 10:33:26 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm 1 23 22 1 5 pi Compound Amount (ng/mL) R.T. -8 Acid 0.00 10 Surrogat 402.62 0.000 8.326 Area 0 97448 Signal MSD1 369, EIC=3 68.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:20:44 pm 42 Page 1 of 1 COO Sample N a m e :L0001400-16 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11571858\A873664\FC000024.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 10:49:00 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm 1 24 23 1 5 pi Compound Amount (ng/mL) R.T. 8 Acid 0.00 10 Surrogat 495.67 0.000 8.338 Area 0 117027 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC 00414 *** End of Report *** Fri, 9. Jan. 2004 04:21:32 pm 0043 Page 1 of 1 000247 Sample Name:L0001400-17 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11573758\A885056\FC000025.D 1 -8 Acid 0.00 10 Surrogat 314.60 0.000 8.328 0 78926 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:27:26 pm 0 44 Page 1 of 1 000248 Sample Name:L0001400-19 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11572016\A875456\FC000026.D Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 11:20:07 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm 1 26 25 1 5 pi Compound Amount (ng/mL) R.T. *"8 Acid 0.00 10 Surrogat 488.18 0.000 8.311 Area 0 115451 Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:22:38 pm 0045 Page 1 of 1 000249 Sample N a m e :L0001400-20 Sample Info: ` Data file :C:\HPCHEM\l\DATA\Chemstor\11573838\A886848\FC000027.D ! Injection Date Acq Operator Instrument Dilution 12/11/03 jmiller PC00414 1 11:35:43 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method <*'- Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. 1 27 26 1 5 pi n>8 Acid 0.00 10 Surrogat 317.36 0.000 8.342 0 79506 MSD1 369, EIC=3 68.7:3 69.7 MSD1 469, EIC=468.7:469.7 PCO 0414 *** End of Report *** Fri, 9. Jan. 2004 04:28:17 pm 0046 Page 1 of 1 000 Sample Name:STD 500 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11572095\A877760\FC000028.D Injection Date Acq Operator Instrument r- Dilution 12/11/03 jmiller PC00414 1 11:51:16 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 28 4 1 5 pi Acq. Method Analysis Method *"* Last Changed FC8-10.M C :\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORV11572095\A877760\FC000028.D) API-ES, Neg, SIM, Frag: Var 12000- 7.477- C8 Aci 10000- 8000 6000 4000- 2000- _________________________________________________________________________ 1__i____ ,____________________ , . 1 , , ^ 11 1i 1' ' ' 1 , 1r 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORY11572095\A877760\FC000028.D) API-ES, Neg, SIM, Frag: Var 16000 8.345- C10 Surrogate 14000 12000 2000 L_ , , 1--------1--------1--------1--------1--------1--------1--------1-------- 1--------1--------1--------1-------- 1--------1-------- 1-------- 1-------- 1--------r Compound Amount (ng/mL) R.T. ~8 Acid 519.38 10 Surrogat 524.15 7.477 8.345 Area 87767 123021 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:24:29 pm 0047 Page 1 of 1 000251 Sample NameSolvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11572153\A879744\FC000029.D Injection Date Acq Operator Instrument Dilution 12/12/03 jmiller PC00414 1 12:06:43 AM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. 1 29 92 1 5 pi "`*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 PCO0414 *** End of Report *** Fri, 9. Jan. 2004 04:24:59 pm J043 Page 1 of 1 oocn2 Sample Name:STD 50 ppb Sample Info : Data file :C :\HPCHEM\1\DATA\FC000030.D Injection Date Acq Operator Instrument Dilution 12/12/03 jmiller PC00414 1 12:22:15 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000030.D) API-ES, Neg, SIM, Frag: Var 1400- 7.465- C8 Acid, 1200 1000 H 800 600- 400- 200- 30 1 1 5 pi MSD1 469, EIC=468.7:469.7 (FC000030.D) API-ES, Neg, SIM, Frag: Var 2000 8.337- C10 Surrogate 1750-1 1500 1250 1000 750 H 500 250 H -- 11 24 Compound Amount (ng/mL) R.T. Acid 1.01 10 Surrogat 2.64 7.465 8.337 Area 9462 13279 1--- 1-- 6 i i , i--- r 8 min Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:56:47 pm 0049 Page 1 of 1 00025 $ Sample Name:STD 100 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000031.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 12/12/03 jmi H e r PC00414 1 12:37:48 AM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : FC8-10 .M C:\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000031 .D) API-ES, Neg, SIM, Frag: Var 2500 - 7.486- C8 Acid 2000- 1500- 1000- 500- 1 31 2 1 5 pi MSD1 469, EIC=468.7:469.7 (FC000031 .D) API-ES, Neg, SIM, Frag: Var 3500- 8.352- C10 Surrogate 3000- 2500 2000 H 1500 1000- 500 0- Compound Amount (ng/mL) R.T. "* 8 Acid 60.25 10 Surrogat 61.32 7.486 8.352 Area 18411 25628 Signal MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:57:34 pm 5 Page 1 of 1 000 Sample Name:STD 250 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\FC000032.D Injection Date Acq Operator Instrument Dilution 12/12/03 jmiller PC00414 1 12:53:19 AM Seq Line Vial N o . Inj . No . Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000032.D) API-ES, Neg, SIM, Frag: Var 6000- 7.481 - C8 Acid 5000- 4000- 3000- 2000- 1000- 1 32 3 1 5 pi , , T| >' ' | ' ' 1 ' 1I i i i 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (FC000032.D) API-ES, Neg, SIM, Frag: Var 9000 r 8.344 - C10 Surrogate 8000 7000 6000- A______. ... h , , i--------1--------1--------1--------1--------1--------1--------1--------1--------1--------1--------1--------1--------1--------1--------'-------- 1--------r Compound Amount (ng/mL) R.T. ~8 Acid 242.01 10 Surrogat 246.13 7.481 8.344 Area 45867 64518 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC 00414 *** End of Report *** Fri, 9. Jan. 2004 04:58:08 pm 005 I Page 1 of 1 000255 Sample Name:STD 500 ppb Sample Info : Data file :C:\HPCHEM\1\DATA\FC000033.D Injection Date I Acq Operator Instrument -- . Dilution 12/12/03 jmiller PC00414 1 1:08:55 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method *"* Last Changed F C 8 - 1 0 .M C :\HPCHEM\1\METHODS\121103.M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000033.D) API-ES, Neg, SIM, Frag: Var 12000- 7.469- C8 Acic 10000- 1 33 4 1 5 pi 8000- 6000- 4000- 2000- 0- ... l , , ,- , . 1 ' 1 ' 1 1 ' 1 1 1 1 I 2 4 6 8 mi n *MSD1 469, EIC=468.7:469.7 (FC000033.D) API-ES, Neg, SIM, Frag: Var . 16000 8.337- C10 Surrogate 14000 ^ 12000 ^ 10000-^ 8000 -j 6000 -; 4000 i 2000 -j 0, , I 1' ' 1 24 11 1 1 6 ___ 1 1 1 1r 8 min Compound Amount (ng/mL) R.T. Area Signal 8 Acid 506.37 10 Surrogat 514.88 7.469 8.337 85802 121069 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 1 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:58:28 pm 0052 Page 1 of 1 000256 Sample Name:STD 750 ppb Sample Info: 1 Data file :C :\HPCHEM\1\DATA\FC000034.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 12/12/03 jmiller PC00414 1 1:24:30 AM Seq Line Vial N o . Inj. No. Inj. Voi. : : : FC8-10.M C :\HPCHEM\ 1\METHODS U 2 1103.M 1/9/04 04:06:51 pm 34 5 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000034.D) API-ES, Neg, SIM, Frag: Var 16000- 7.449- C8 Ade 14000- 12000 ^ 10000-; 8000 - 6000- 4000 ^ 2000 ^ 0 - . t - r r 1 1 2 __ ............ n 1i 46 1 *MSD1 469, EiC=468.7:469.7 (FC000034.D) API-ES, Neg, SIM, Frag: Var _u _L___ 1 1 i 8 --------- 1 8.323- C10 Surrogate ir min 20000 - 15000- 10000- 5000- - 0 Compound 1. T ' 2 Amount (ng/mL) 1 '1 4 R.T. -R8 Acid 741.24 10 Surrogat 749.15 7.449 8.323 '1' Area 121281 170367 1 I 1 11 1 ' 1 1 i 6 8 min Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:58:45 pm 055 Page 1 of 1 000257 Sample Name:STD 1000 ppb Sample Info : Data file .-C:\HPCHEM\1\DATA\FC000035.D Injection Date Acq Operator Instrument Dilution 12/12/03 jmiller PC00414 1 1:40:04 AM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121103 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000035.D) API-ES, Neg, SIM, Frag: Var 20000 ^ 7.474- C8 Aci' 17500- 15000- 12500- 10000 t 7500- 5000- 2500 r 0- 1 *MSD1 469, EIC=468.7:469.7 (FC000035.D) API-ES, Neg, SIM, Frag: Var 8 30000 - 8.340 - C10 Surrogate 25000 - 20000 - 15000- 10000- 5000- 1 35 6 1 5 pi Compound Amount (ng/mL) R.T. 8 Acid 997.65 10 Surrogat 1003.81 7.474 8.340 . Area 160014 223954 Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 *** End of Report *** PC00414 Fri, 9. Jan. 2004 04:59:03 pm o U54 Page 1 of 1 000258 Sample Name:STD 1500 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000036.D Injection Date Acq Operator Instrument Dilution 12/12/03 jmiller PC00414 1 1:55:40 AM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEMX1\METHODS\12110 3 .M 1/9/04 04:06:51 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000036.D) API-ES, Neg, SIM, Frag: Var 30000 - 7.467- C8 Acid 25000 - ^20000 15000 ^ 10000J 5000- 1 36 7 1 5 pi *MSD1 469, EIC=468.7:469.7 (FC000036.D) 40000 - API-ES, Neg, SIM, Frag: Var 8.334- C10 Surrogate 35000 ^ 30000 ~ 25000 20000 - 15000- 10000J 5000- 0- - 1 11111 2 1- 4 -----!---------,--- ,--6 111 1f 8 min Compound Amount (ng/mL) R.T. Area Signal *8 Acid 1389.86 10 Surrogat 1400.66 7.467 8.334 219262 307464 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 04:59:21 pm u U55 Page 1 of 1 000259 3058 Research Drive State College, PA 16801 .ogin Phone: 814-272-1039 Fax: 814-231-1580 Login #: 1510 Project: P0000419 Project Storage: Company Name: DuPont de Nemours & Co, Inc. Submitted By: Michael D. Aucoin Status: Un received Login Type: Immediate Receipt of Samples Started: T Date Start: 12/02/2003 Due Date: 12/16/2003 Received Date: 12/02/2003 Received By: AMMERMAN, MARK Spread Sample: Label: Project Title/Type: Analysis of PFOA in OVS Tubes / ROUTINE Exygen SD/PI: MILLER, JAMES Login Notes: Conform Notes: Conform COC Sample: Conform COC: Conform Sample: Conform Request: True True True True Package PK0001982 Carton Packages / Containers Mail Date / Condition Shipper/ ID 12/2/2003 10:30:09PM Package & Contents Uncompromised FEDEX 8363913019710200 Temp. Control/Temp. None 23.3 Direction / Handled By RECEIVED AMMERMAN, MARK C ontainer # C0020357 C0020358 C0020359 C0020360 C0020361 C0020362 C0020363 C0020364 C0020365 C0020366 C0020368 C0020369 C0020370 C0020371 C0020372 C0020373 C0020374 C0020375 C0020376 C0020377 C0020378 C0020379 C002Q380 C0020381 Gross W eight 7.2 g 7.2 g 7.2 g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g 7.3 g 7.3 g 7.3 g 7.2 g 7.2 g 7.2 g 7.1 g 7-1 g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g pH 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 Mfg. ID 12/12/2003 Login.rpt U56 Report Version: Dec 12 2003 11:28AM Page 1 of 5 Instance: 000260 R0076077 R0076077 Login #: 1510 Project: P0000419 Project Storage: Company Name: DuPont de Nemours & Co, Inc. Submitted By: Michael D. Aucoin Status: Unreceived Login Type: Immediate Receipt of Samples Started: T Date Start: 12/02/2003 Due Date: 12/16/2003 Received Date: 12/02/2003 Received By: AM MERMAN, MARK Spread Sample: Label: Project Title/Type: Analysis of PFOA in OVS Tubes / ROUTINE Exygen SD/PI: MILLER, JAMES Login Notes: Conform Notes: Conform COC Sample: Conform COC: Conform Sample: Conform Request: True True True True Package Carton M iscellaneous Item Key None Packages / Containers Mail Date / Condition Shipper /JD ICOC Temp. Control/Temp. Description Direction / Handled By Sample ID L0001400-0001 L0001400-0002 LOO01400-0003 L0001400-0004 L0001400-0005 L0001400-0006 L0001400-0007 L0001400-0008 L0001400-0009 L0001400-0010 L0001400-0011 L0001400-0012 L0001400-0013 L0001400-0014 L0001400-0015 L0001400-0016 L0001400-0017 L0001400-0018 L0001400-0019 L0001400-0020 L0001400-0021 LOOO1400-0022 L0001400-0023 L0001400-0024 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-AMSFLBK-E5 A WWK-A-AMSFLBK-E5 B WWK-A-AMSFLBK-E5 C WWK-A-AMS1-E5 A WWK-A-AMS1-E5 B WWK-A-AMS1-E5 C WWK-A-AMS2-E5 A WWK-A-AMS2-E5 B WWK-A-AM S2-E5 C WWK-A-AMS3-E5 A WWK-A-AMS3-E5 B WWK-A-AMS3-E5 C WWK-A-AMS4-E5 A WWK-A-AMS4-E5 B WWK-A-AMS4-E5 C WWK-A-AMS5-E5 A WWK-A-AMS5-E5 B WWK-A-AMS5-E5 C WWK-A-AMS6-E5 A WWK-A-AMS6-E5 B WWK-A-AMS6-E5 C Control 1 A Control 1 B Control 1 C Date Sampled Date Received 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 11/30/2003 12/02/2003 12/02/2003 12/02/2003 12/02/2003 Date Due 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/16/2003 12/12/2003 Login.rpt J05/ Report Version: Dec 12 2003 11:28AM Page 2 of 5 Instance: 000261 R0076077 R0076077 L0001400-0001 C ontainer C0020357 / Other / NONE L0001400-0002 C ontainer C0020358/ Other /N O N E , L0001400-0003 C ontainer C0020359 / Other / NONE L0001400-0004 C ontainer C0020360 / Other / NONE L0001400-0005 C ontainer C0020361 / O ther/N O N E L0001400-0006 C ontainer . , C0020362 / Other / NON E L0001400-0007 C ontainer C0020363/Other/NONE -L 000 1400-0008 C ontainer 00020364/ Other /N O N E L0001400-0009 C ontainer 00 02 03 65/O ther/NONE L0001400-0010 C ontainer 00 02 03 66/O ther/NONE L0001400-0011 C ontainer ... C0020368 / Other / NONE L0001400-0012 C ontainer .... 12/12/2003 Login.rpt Bottles M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod , u U00 M ethod Report Version: Dec 12 2003 11:28AM p age 3 of 5 Instance: R0076077 (00262 R0076077 C0020369 / Other / NONE L0001400-0013 Container C0020370/Other/NONE L0001400-0014 Container C0020371 / O th er/N O N E L0001400-0015 Container C0020372/Other/NONE L0001400-0016 Container C0020373 / Other / NONE L0001400-0017 Container C0020374 / Other / NONE 'L0001400-0018 Container C0020375/Other/NONE L0001400-0019 Container C0020376/ Other /N O N E L0001400-0020 Container C0020377/Other/NONE L0001400-0021 Container ` C0020378 / Other / NONE L0001400-0022 Container C0020379 / Other / NONE L0001400-0023 Container C0020380/Other/NONE L0001400-0024 Container C0020381 / O th e r/N O N E 12/12/2003 Login.rpt Method Method Method Method Method Method Method Method Method Method Method Method UU59 Report Version: Dec 12 2003 11:28AM Page 4 of 5 Instance: 000263 R0076077 LoginfW* 12/12/2003 Login.rpt U060 Report Version: Dec 12 2003 11:28AM p age 5 o '5 Instance: R0076077 000264 R0076077 CHAIN OF CUSTODY/ANALYSIS REQUEST FORM RESEARCH Exygen Research Sample Receiving * 3117 Research Drive State College, PA 16801, U SA T: 814.231.8032 F: 814.231.1580 exygenresearch.com Page \ l of i PROJECT INFORMATION ANALYSES REQUESTED Client (name & address): P l-0 (^iY \ o. , 0. Phone: Fax: Sampler: vA ,j R . \4 o m flJ A \ L*K$,rCXXiA Project Manager (Name & E-mail Address): ffw W . n u Q ^ A Project Name: 0 rs f W o o ^ p \ ir ^ \ \f\)9vC<uvO RO. # : * <T ) <0 Q uotation#: I l/) C- o c o Please fill out this form com plete ly to ensure correct analysis and proper handling of your samples. C om p o site Num ber of C o n tain ers SAMPLE ANALYSIS ExyLIMS# Client Sample Identification Colle ction Collection ite Time -fkQd. O vooM V- P r e t a x e f Liis-1|0^ DklaO y * vovO ^-P iA PriY \S9.-efS f t m s *> V \0 y H V ` PrfTK 4 - E S b V.v5 * oW }o % v jv o ic - -iv m S -e s ' V O W K rfV - \o r 5 \SlD0 * 0\5^\ * A A -A / 1 LAB USE ONLY Specify M atrix Comments \ PtTT \ fW Kx c V>kc > \ (W A 'r Q Ncwvk-- CHAIN OF CUSTODY Relinquished by /Kn . 1 . . 1/ n Date Time 11 -- liso Cooler ID # / l'ic Received cby l J f e y#/ ^ / 7' /" lit Cooler Temp. (C) Date 1 Time iomd? y. -J//./tr*&vT /o f* OTHER INFORMATION LAB USE ONLY V\AA fI o D D y % y y S * PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: I I Sample results only I I Add case narrative HU Add quality control summary HU Add calibration summary CDI I Add raw data Other ___ REV. 3-0? Sam plers): LK, R EK DuPont W ashington W orks Air Sam pling Program FedEx Airbill #: ] Event Number Event 5 1 669842 669908 669878 669901 669769 669848 Hours 0 1 2 3 4 A M S-1 AM S-2 A M S-3 AM S-4 A M S-5 A M S-6 Minutes 0 60 120 180 240 W W K-A-AMS1-E5 W W K-A -A M S2-E5 W W K-A -A M S3-E5 W W K-A -A M S4-E5 W W K-A -A M S5-E5 W W K-A -A M S6-E5 Hours 5 6 7 8 9 1.019 1.011 1.013 1.013 1.018 1.017 Minutes 300 360 420 480 540 29-Nov 29-Nov 29-Nov 29-Nov 29-Nov 29-Nov Hours 10 11 12 13 14 0547 0550 0550 0558 0540 0605 Minutes 600 660 720 780 840 30-Nov 30-Nov 30-Nov 30-Nov 30-Nov 30-Nov Hours 15 16 17 18 19 0630 0615 0615 0640 0600 0649 Minutes 900 960 1020 1080 1140 Field Blank: yes WWK-K-AMSFBLK-E5 yes or no Weather: 11/29= Temperature about 30 degrees, with light snow. 11/30 = Temperature about 32 degrees, and clear. 0.9162 1.013 1.077 1.19 1.015 1.022 Hours 20 21 22 23 24 1480 1459 1460 957* 1462 1479 Minutes 1200 1260 1320 1380 1440 S A F E R operational: yes yes or no ] Comments: Total minutes column is the reading from the monitor counter. * Pum p A M S-4 had an intake fault icon on the display and had stopped running at 957 minutes. W hen brought back for post calibration pump w ould run for 10 to 15 seconds with a flow of 1.190 and then stop again with the fault icon s h o w i n g . ___________________________________________ W O C O CM \> CD D 12/1/03 Page 1 of 2 airdataevent5 I i 1 From USA A irbill f l 3 b 3 H 3 o i * mExpress FedEx Tracking Number Date i a l 0 \ | 0 3 3 4"'. :Q ^_Sender's Name C\ ) vm q Phone -3 oj Company \N O ,i 7 O/'"' \ o (Vi-- Address :^r.^ sflQ /^nVcg-t k 0 . r """ * -- Deptyfloor/Suite/Room City U 2 Your Internal Billing Reference <A State 1 - 0 z,p . Q \ , \ % \ ^ \s o. Z) ' ^,-.tJsiru*i o . t\ V\ ( ( _ _ ' ( _3 To Recipient's Name O \V V '1 l A - \ ~ ^ \P h o n e K i ] " 7 ^ P j- Company V \ ;^ \j\ ...,e ; \ : 1 A . ) s k c ^ < r \ & Address " .\i -V-' To 'HOLD' at FedEx locattiomn, porinti FedEx address. 7 Address \ i v> \ - A ^\rC^- T" WWeeccaannnoottddeelilvievertrotoP.P..H dopes or P.0. ZIP codes. (Lz)'<Z\jd Recipient's Copy 4a Express Package Service .dEx Priority Overnight Next business morning I I FedEx Standard Overnight 1-- 1 Next business afterpoon Packagesup to 15Qlbs. trycommitment maybe later in some areas. 1 | FedEx First Overnight -- Earliescnext business rrraming deliveryto select locations I j FedEx 2Day Q FedEx Express Saver Second business day Third business day t FedEx Envelope rate not available. Minimum charge: Qne-pound rate 4b Express Freight Service Packages over IS) lbs. Delivery commitment maybe laterinsome areas. ! j FedEx 1Day Freight* l-- 1 Nextbusiness dos I I FedEx 2Day Freight I-- I Second business day ) I FedEx 3Day Freight i-- ' Third business day * Call lorConfirmabon: 5 Packaging I I FedEx Envelope4 FedEx Pak* Includes FedEx SmaH Pak, FedEx Large Pak, and FedEx Sturdy Pak * Declared value limit$500 X Other 6 Special Handling Include FedEx address in Section 3. -, S A T U R D A Y D e liv e ry |___j AvailableonlyforFedExPnrnty Overnightami FedEx 2Day to select ZIP codes H HOLD W eekday I__ I at FedEx Location Not available for FedEx FirstOvernight D oes tin s shipm ent tontain dangerous goods? ------------- One box rust be checked. ------------ -- 1No * ", jY.neySjj/oia auyu nutiBrunei!k i-- i Yes kouaiAsperattaclsd |___| Shipper's Declaration Shipper's Dedataon nof required I-- i HOLDSaturday I__ I at FedEx Location Available ontytor FedEx PriorityOvernight and FedEx2Dayto select locations I 1 Dry Ice I-- I QDrylice, 9.UN 1845- Dangerous Goods (including Dry Ice) armorbe shipped in FedEx packaging. I I Cargo A ircraft Only 7 Payment Billto: _ . -- -- ------ EnterFedExA c c i No. or CreditCard No. below. -- ["IObtainRectp. ! -- 1AcctNo. lender j I Recipient Acct No. in Secbon | Third Party Q Credit Card | 1Cash/Check 65 Total Packages TotalW eight Total D eclared Value* _ i-- 4 l``$ .00 tOur liability is limited to $100 unless you declarty higher value. See back for details. 8 Release Signature Sign to authorizeiJehmy rtthouiobtaining signature. Ey signing you authorize us to deliver this shipment wthout obtaining a signature aid agree to indemnify and hold us harmless from any-esulting claims. , O u e stio n s?V isito u rW e b $ ite a tfe ie x .c o m 0- call 1.800.Go.FedEx 800.463.3333. lev Date 10/01Part #I576121994-2001 FedExPRINTED IN U5.A. WCSLG2 Total Q iarges