Document ppRZM3ypzK2yzbk577ZMq1Yk7

Precise Research. Proven Results. Attachment 2 ^Bzz^r/77-^ Analytical Report Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 11 Exygen Research Report No. L0001668 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 Summary Seven solid media samples were received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. The media represent samples of air collected on OVS tubes. Please see Table 1 for a completed listing of samples received and field air volumes collected. The samples were analyzed for Perfluorooctanoic Acid (C8 Acid) using liquid chromatography / mass spectrometry (LCMS). The method employed is entitled "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in OVS Airtubes by LCMS" (James Miller, Exygen Research, February 17, 2003). The OVS tubes were separated into three fractions for specific fhiorochemical 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 ran. 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 C00516 Results Summary Request # WWK-A-AMS1-E11 A WWK-A-AMS1-E-11 B WWK-A-AMS1-E11 C WWK-A-AMS1-E11 (Total) WWK-A-AMS2-E11 A WWK-A-AMS2-E11 B WWK-A-AMS2-E11 C WWK-A-AMS2-E11 (Total) WWK-A-AMS3-E11A WWK-A-AMS3-E11 B WWK-A-EMS3-E11 C WWK-A-EMS3-E11 (Total) WWK-A-AMS4-E11 A WWK-A-AMS4-E11B WWK-A-AMS4-E11 C WWK-A-AMS4-E11 (Total) WWK-A-AMS5-E11 A WWK-A-AMS5-E11 B WWK-A-AMS5-E11C WWK-A AMS5-E11 (Total) WWK-A-AMS6-E11 A WWK-A-AMS6-E11 B WWK-A-AMS6-E11 C WWK-A AMS6-E11 (Total) Air Volume Sampled (L) 1398 1398 1398 1448 1448 1448 931 931 931 1424 1424 1424 1402 1402 1402 1434 1434 1434 C8 Acid (mg/m3) < 0.00007 < 0.00007 NA <0.00014 < 0.00007 < 0.00007 NA <0.00014 < 0.0001 < 0.0001 NA < 0.0002 < 0.00007 < 0.00007 NA <0.00014 0.0003 < 0.00007 NA 0.0003 < 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 G0 0 5 1 7 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) 509 C8 Acid (percent recovery 102 Blanks Request # WWK-A-AMSFBLK-E9 A WWK-A-AMSFBLK-E9 B Voi. Of Air (L) 0 0 C8 Acid (uq/fraction) <0.10 <0.10 O o o rS l ATT. DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH C0 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-E11 A WWK-A-AMSFBLK-E11 B W WK-A-AMS1-E11 A WWK-A-AMS1-E11 B W WK-A-AMS2-E11 A W WK-A-AMS2-E11 B W WK-A-AMS3-E11 A W WK-A-AMS3-E11 B W W K -A -A M S 4-E11 A W WK-A-AMS4-E11 B W WK-A-AMS5-E11 A WWK-A-AMS5-E11 B W WK-A-AMS6-E11 A WWK-A-AMS6-E11 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) 479 360 498 564 497 583 517 580 519 569 520 592 524 584 532 347 Percent Recovery (% ) 96 72* 100 113 99 117 103 116 104 114 104 118 105 117 106 69* * Surrogate recovery outside of advisory range. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 C C 05.9 Calculations Request # WWK-A-AMSFBLK-E11 A WWK-A-AMSFBLK-E11 B WWK-A-AMS1 -E11 A WWK-A-AMS1 -E11 B WWK-A-AMS2-E11 A WWK-A-AMS2-E11 B WWK-A-AMS3-E11 A WWK-A-AMS3-E11 B WWK-A-AMS4-E11 A WWK-A-AMS4-E11 B WWK-A-AMS5-E11 A WWK-A-AMS5-E11 B WWK-A-AMS6-E11 A WWK-A-AMS6-E11 B Control Spike A Control Spike B Voi. Of Air (L) 0 0 1398 1398 1448 1448 931 931 1424 1424 1402 1402 1434 1434 0 0 C8 Acid (raw-ppb) < 10 < 10 < 10 <10 <10 < 10 10 <10 <10 <10 434 <10 <10 <10 509 < 10 C8 Acid (ug/fraction) <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 0.43 <0.10 <0.10 <0.10 0.51 <0.10 C8 Acid (mg/m3) < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.0001 < 0.0001 < 0.00007 < 0.00007 0.0003 < 0.00007 < 0.00007 < 0.00007 a & ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH 01 o?0 Page 6 of 7 Example Calculation For sample WWK-A-AMS5-E11 A C8 Acid, [434 ng/ml of C8 Acid x (1ml) x (1 ug /1000 ng) x (1 mg /1000 ug) ] / [(1402 L) x (1 m3 / 1000 L)] 0.0003 mg / m3 Signatures ohn M. Flaherty, Vice President Other Lab Members Contributing to Data James Miller ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 7 ANALYTICAL DATA REVIEW SHEET LC/MS fc. Hch Analyst J7 /y} ff) f/g j x & i y Reviewed by S ta tu re /D a te q/ W /Signature/Date ' U0Q8 Cn o LC/MS SYSTEM AND OPERATING CONDITIONS Client: Dupont EXYGEN STUDY: L0001668 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 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 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 j Uu9 G0 0 5 2 3 Instrument : LCMS3 Wed Jan 07 09:11:11 2004 G1946: API_ES Negative mode Page 1 of 3 C :\HPCHEM\1\194 6TUNE\ATUNES.TUN Scan: 50.00 - 3000.00 Samples: 8 Thresh: 0 Step: 0.10 29501 peaks Base: 2233.85 Abundance: 1132032 F Raw,Gauss 0.3 100 -, 80 - 60 - 20 - 1 '-- r--,-- >-- -i---- 1-- ' r 1 1.r. 500 1000 1500 11 2Q00 `11 2500 m/z gf Abund 112.99 80352 602.00 21400 1034.05 197568 1633.95 610624 2233.85 1132032 Rei Abund 100.00 26.63 245.88 759.94 1408.84 Iso m/z 113.98 602.99 1034.95 1634.95 2234.85 Iso Abund Iso Ratio 1768 2.20 3222 15.06 43112 21.82 217216 35.57 550720 48.65 0 ! 1 C005?5 Instrument : LCMS3 Wed Jan 07 09:11:11 2004 G1946: API_ES Negative mode Page 2 of 3 C:\HPCHEM\1\1946TUNE\ATUNES.TUN Mode: API -ES Polarity: NEG Fragment Skim2 Lensl Lens2 Iris Gain VAR WidthGain -128 6.0 WidthOffs VAR -4.0 MassGain-36.30 18 MassOffs VAR 272 Energy 5.0 OpolPeak 300 OpolKnee 316 3.0 QuadDC 0.00 EMV VCap Status: CapCur ChamCur 2358 Samples 8 4000 Averages 1 StepSize 0.10 55 DryingGas 6.0 0.82 Gas Temp 300 Quad Temp 99 Neb Pres 20 t y uG ! 2 CCO526 Instrument : LCMS3 Wed Jan 07 09:11:11 2004 G1946: API_ES Negative mode Page 3 of 3 C:\HPCHEM\1\1946TUNE\ATUNES.TUN Vl:' Mass Offset Dynamic Parameter Ramp Mass 112.99 1633.95 Setting 0.56 0.61 Mass 601.98 2233.91 Setting 0.62 0.56 Mass 1033.99 Setting 0.63 00 I3 C005^7 Sequence: C:\HPCHEM\1\SEQUENCE\012204 .S Sequence Table: Method and Injection Info Part: Line Location SampleName Method Inj SampleType InjVolume DataFile 1 Vial 1 STD 50 ppb FC8-10 __ 2_ Vial J.__ STD _5.Q ppb_______ FC8-10 3 Vial 2 STD 100 ppb FC8-10 4 Vial 3 STD 250 ppb FC8-10 5 Vial 4 STD 500 ppb FC8-10 6 Vial 5 STD 750 ppb FC8-10 7 Vial 6 STD 1000 ppb FC8-10 8 Vial 7 STD 1500 ppb FC8-10 9 Vial 92 solvent blank FC8-10 10 Vial 11 L1668-22 FC8-10 11 Vial 12 L1668-23 FC8-10 12 Vial 13 L1668-1 FC8-10 13 Vial 14 L1668-2 FC8-10 14 Vial 15 L1668-4 FC8-10 15 Vial 16 L1668-5 FC8-10 16 Vial 17 L1668-7 FC8-10 17 Vial 18 LI 668-8 FC8-10 18 Vial 19 L1668-10 FC8-10 19 Vial 20 LI 668-11 FC8-10 20 Vial 4 STD 500 ppb FC8-10 21 Vial 92 solvent blank FC8-10 22 Vial 21 L1668-13 FC8-10 23 Vial 22 L1668-14 FC8-10 24 Vial 23 L1668-16 FC8-10 25 Vial 24 L1668-17 FC8-10 26 Vial 25 L1668-19 FC8-10 27 Vial 26 L1668-20 FC8-10 28 Vial 4 STD 500 ppb FC8-10 29 Vial 92 solvent blank FC8-10 30 Vial 1 STD 50 ppb FC8-10 31 Vial 2 STD 100 ppb FC8-10 32 Vial 3 STD 250 ppb FC8-10 33 Vial 4 STD 500 ppb FC8-10 34 Vial 5 STD 750 ppb FC8-10 35 Vial 6 STD 1000 ppb FC8-10 36 Vial 7 STD 1500 ppb 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 Method CalLev Update RF Update RT Interval 2 Vial 1 3 Vial 2 4 Vial 3 5 Vial 4 6 Vial 5 7 Vial 6 8 Vial 7 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 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 1/22/04 4: 28: 51 PMi jmiller 7 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 !4 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 -3 P, vv r Sequence : C:\HPCHEM\1\SEQUENCE\012204 .S iCMS3 1/22/04 4:28:51 PM jmiller ? uO 0 Page 2 of 2 ccor.na Method C:\HPCHEM\1\METHODS\012204.M Calibration Table Calib. Data Modified Thursday, February 26, 2004 10:08:53 AM 1 Calculate Based on External Standard Peak Area I Rel. Reference Window ' Abs. Reference Window Rel. Non-ref. Window Abs _ Non-ref. Window Uncalibrated Peaks Partial Calibration Correct All Ret. Times 5.000 % 0.000 min 5.000 % 0.000 min not reported Yes, identified peaks are recalibrated No, only for identified peaks Curve Type Origin Weight Linear Ignored Equal Recalibration Settings Average Response Average Retention Time Average all calibrations Floating Average New 75% Calibration Report Options : Printout of recalibrations within a sequence: Calibration Table after Recalibration Normal Report after Recalibration If the sequence is done with bracketing: Results of first cycle (ending previous bracket) Signal 1 : MSD1 369, EIC= 368.7:369.7 Signal 2 : MSD1 469, EIC= 468.7:469.7 RetTime Lvl Amount Area [min] Sig [ppb] -------I - I - I 7.238 1 1 50.00000 ^2.54854e4 2 100.00000 5.21298e4 3 250.00000 1.38928e5 4 500.00000 2.68105e5 5 750.00000 3.95712e5 6 1000.00000 5.07448e5 7 1500.00000 7.25598e5 8.109 2 1 50.00000 7.14014e4 2 100.00000 1.43567e5 3 250.00000 3.67689e5 4 500.00000 6.92756e5 5 750.00000 1.00164e6 6 1000.00000 1.26065e6 7 1500.00000 1.75606e6 Amt/Area ^1.96191e-3 1.91829e-3 1.79949e-3 1.86494e-3 1.89532e-3 1.97064e-3 2.06726e-3 7.00266e-4 6.96541e-4 6.79922e-4 7.21754e-4 7.48773e-4 7.93240e-4 8.54185e-4 Ref Grp Name 1 C8 Acid 1 CIO Surrogate More compound-specific settings: Compound: C8 Acid Time Window : From 7.066 min To 8.067 min Compound: CIO Surrogate Time Window : From 7.913 min To 8.718 min Peak Sum Table ***No Entries in table*** C00414 2/26/04 10:10:50 AM jmiller 0 016 Method C:\HPCHEM\1\METHODS\012204.M Calibration Curves C8 Acid at exp. RT: 7.238 MSD1 369, EIC=3 68.7:369.7 Correlation: 0.99866 Residual Std. Dev.: 14581.78795 Formula: y = mx + b m: 485.91764 b: 13835.67745 x: Amount[ppbl____________ y: Area CIO Surrogate at exp. RT: 8.109 MSD1 469, EIC=468.7 :469.7 Correlation: 0.99690 Residual Std. Dev.: 53527.29878 i Formula: y = mx + b m: 1170.89142 b: 62080.82414 x: Amount[ppb] y: Area 300414 2/26/04 10:10:50 AM jmiller U0 : / Page 2 of 2 ooosn i Sample Name:STD 50 ppb Sample Info:Warm Up Injection Data file :C :\HPCHEM\l\DATA\Chemstor\12087705\A521536\FC000001.D 1 C8 Acid -- CIO Surrogate 26327.43 76333.71 25.71 12.17 7.261 8.134 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:12:17 am U0 18 Page 1 of 1 c corroo Sample Name:STD 50 ppb Sample Info : Data file :C :\HPCHEMU\DATA\Chemstor\12080405\A589376\FC000002.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 4:53:38 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method FC8-10 .M Analysis Method : C:\HPCHEM\1\METHODS\012204.M ... Last Changed : 2/26/04_____________ 10:08:53 am 2 1 1 5 pi 1 Compound Name C8 Acid -CIO Surrogate Area 26027.72 74031.62 Amount 25.09 10.21 Meas. Ret. T Signal Desc. 7.246 8.116 MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 10:09:41 am Q !9 Page 1 of 1 C0 0 5 3 3 Sample Name:STD 100 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12080464\A591808\FC000003.D 1 C8 Acid ,,CIO Surrogate 53601.73 148148.97 81.84 73.51 7.246 8.116 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 1 PC00414 Thu, 26. Feb. 2004 10:13:00 am Q02Q Page 1 of 1 C- 0 0 5 3 4 Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12080548\A593984\FC000004.D 1 C8 Acid ,,CIO Surrogate 142444.72 376511.78 264.67 268.54 7.237 8.105 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:13:41 am 0 0 21 Page 1 of 1 0 705.75 Sample Name:STD 500 ppb Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\12080667\A596224\FC000005.D 1 C8 Acid CIO Surrogate 270860.69 703836.19 528.95 548.09 7.232 8.104 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 Q22 10:14:18 am Page 1 of 1 009536 Sample Name:STD 750 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12088166\A532672\FC000006.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/22/04 jmi H e r PC00414 1 5:55:53 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : FC8-10.M C :\HPCHEMN1\METHODS\012204.M 2/26/04 10:08:53 am LC/MS analysis of perfluorooctanoic acid. 6 5 1 5 pi 1 C8 Acid ,,.CIO Surrogate 397814.34 1009547.12 790.21 809.18 7.226 8.102 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 02 3 10:15:15 am Page 1 of 1 CO0 5 3 7 Sample Name:STD 1000 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12088281\A534720\FC000007.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 6:11:29 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method FC8-10.M Analysis Method : C:\HPCHEM\1\METHODS\012204.M Last Changed : 2/26/04______________10:08:53 am 7 6 1 5 pi 1 Compound Name C8 Acid CIO Surrogate Area 514972.75 1274229.88 Amount 1031.32 1035.24 Meas. Ret. T Signal Desc. 7.235 8.108 MSD1 369, EIC =368.7 :369.7 MSD1 469, EIC=468.7 :469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 0024 10:15:59 am Page 1 of 1 CC0538 Sample Name:STD 1500 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12080979\A602816\FC000008.D Injection Date | Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/22/04 jmiller PC00414 1 6:27:05 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : FC8-10 .M C :\HPCHEM\1\METHODS\012204 .M 2/26/04 10:08:53 am LC/MS analysis of perfluorooctanoic acid. 8 7 1 5 ul 1 C8 Acid ,C10 Surrogate 737835.69 1784410.75 1489.96 1470.96 7.237 8.105 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 ?C00414 Thu, 26. Feb. 2004 10:16:50 am U 'o Page 1 of 1 c00539 Sample Name:solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12088595\A539136\FC000009.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 6:42:34 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\l\METHODS\012204.M 2/26/04 10:08:53 am LC/MS analysis of perfluorooctanoic acid. 9 92 1 5 pi 1 C8 Acid ,,,,CIO Surrogate 0.00 2059.66 0.00 0.00 0.000 8.108 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 >C00414 Thu, 26. Feb. 2004 026 10:18:53 am Page 1 of 1 C0 0 5 4 0 Sample Name:L1668-22 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12088763\A541184\FC000010.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 6:58:07 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method FC8-10 .M Analysis Method : C:\HPCHEM\1\METHODS\012204.M Last Changed : 2/26/04______________10:08:53 am 10 11 1 5 pi 1 Compound Name C8 Acid CIO Surrogate Area 261058.59 684950.62 Amount 508.78 531.96 Meas. Ret. T Signal Desc. 7.232 8.104 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 UU27 10:20:04 am Page 1 of 1 C00543. Sample Name :L1668-23 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\12088932\A543360\FC000011.D 1 C8 Acid -CIO Surrogate 16576.66 468416.38 5.64 347.03 7.239 8.111 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 28 10:21:21 am Page 1 of 1 000542 Sample Name:Ll668-1 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12089100\A545408\FC000012.D 1 C8 Acid ,,CIO Surrogate 3786.80 623131.69 0.00 479.17 7.234 8.110 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 [ PC00414 Thu, 26. Feb. 2004 10:21:58 am 029 Page 1 of 1 000543 Sample Name:L1668-2 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12089269\A547456\FC000013.D 1 C8 Acid ..10 Surrogate 3055.95 483225.03 0.00 359.68 7.234 8.108 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 ,I ,, ?C00414 Thu, 26. Feb. 2004 10:22:41 am Page 1 of 1 C^05A4 Sample Name:L1668-4 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\12089437\A549632\FC000014.D Injection Date Acq Operator Instrument _ Dilution 1/22/04 jmiller PC00414 1 8:00:24 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method r-- Last Changed FC8-10.M C :\HPCHEM\1\METHODS\012204.M 2/26/04 10:08:53 am 14 15 1 5 pi 1 Compound Name C8 Acid CIO Surrogate Area 4345.78 645270.00 Amount 0.00 498.07 Meas. Ret. T Signal Desc. 7.231 8.106 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** ?C00414 Thu, 26. Feb. 2004 UQ3 ! 10:24:18 am Page 1 of 1 C O O r;/! K Sample Name :L1668-5 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12089605\A551680\FC000015.D 1 C8 Acid -CIO Surrogate 4645.49 722482.75 0.00 564.02 7.237 8.116 *** End of Report *** MSD1 369, EIC =368.7:369.7 MSD1 469, EIC=468.7:4 6 9 . 7 ! PC00414 Thu, 26. Feb. 2004 10:24:53 am uUoZ Page 1 of 1 0 0 0 5 4 .6 Sample Name:L1668-7 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\1208980 0\A554112\FC000016.D "" Injection Date Acq Operator Instrument , . Dilution f : 1/22/04 : jmiller : PC00414 :1 8:31:39 PM Seq Line Vial No. Inj . No. Inj . Voi. : : : : 16 17 1 5 pi 1 C8 Acid .,,CIO Surrogate 18158.58 643424.06 8.90 496.50 7.242 8.112 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC =468.7:469.7 I, PC00414 Thu, 26. Feb. 2004 10:25:47 am 0033 Page 1 of 1 C0 0 5 4 .7 Sample Name:LI668-8 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12089968\A556032\FC000017.D 1 C8 Acid CIO Surrogate 4804.49 744889.56 0.00 583.15 7.240 8.110 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 i" I I- [ PC00414 Thu, 26. Feb. 2004 u 3 4 10:26:36 am Page 1 of 1 Sample Name :L1668-10 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\12090137\A558272\FC000018.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 9:02:55 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 18 19 1 5 pi Acq. Method Analysis Method L ast C h a n g e d __ FC8-10.M C :\HPCHEM\1\METHODS\012204.M 2/26/04______________10:08:53 am LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM2090137\A558272\FC000018.D) 2500 API-ES, Neg, SIM . Frag: Var 7 .2 3 5 - C8 Acid 2000- 1500- 1000 500- X- MSD1 469, EIC=468.7:469.7 (CHEM STO RM 2090137\A558272\FC000018.D ) API-ES, Neg, SIM, Frag: Var 8 .1 1 2 - C10 Surrogate 80000 60000 40000 - 20000 1 .' Compound Name C8 Acid -CIO Surrogate ---- !---- ,---- -- -,---- 1---- ,--- ' 24 '1 6 Area Amount Meas. Ret. T 1j i1 8 Signal D e s c . i min 18462.77 667939.62 9.52 517.43 7.235 8.112 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 ** End of Report ** I PC00414 Thu, 26. Feb. 2004 U35 10:27:58 am Page 1 of 1 CO0 5 1 9 Sample Name :L1668-11 (*" Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\12090306\A560448\FC000019.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 9:18:34 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method FC8-10.M Analysis Method : C:\HPCHEM\1\METHODS\012204.M Last Changed____ : 2/26/04_____________ 10:08:53 am LC/MS analysis of perfluorooctanoic acid. 19 20 1 5 pi 1 C8 Acid ,,,,CIO Surrogate 4648.05 741114.31 0.00 579.93 7.240 8.111 I ===================================================== *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 9C00414 Thu, 26. Feb. 2004 10:29:12 am U036 Page 1 of 1 C00550 Sample Name:STD 500 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12090474\A562368\FC000020.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 9:34:09 PM Seq Line Vial No. Inj . No . Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\012204.M 2/26/04 10:08:53 am 20 4 1 5 pi 1 Compound Name C8 Acid *C10 Surrogate Area 266118.88 688464.50 Amount 519.19 534.96 Meas. Ret. T Signal Desc. 7.239 8.110 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 10:29:46 am U037 Page 1 of 1 CO0 5 5 1 Sample Name:solvent blank Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\12090696\A564608\FC000021.D Injection Date : 1/22/04 Acq Operator : jmiller Instrument : PC00414 , Dilution :1 9:49:37 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 21 92 1 5 pi 1 C8 Acid ,,4310 Surrogate 0.00 1266.68 0.00 0.00 0.000 8.117 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC =468.7 :469.7 !" [ PC00414 Thu, 26. Feb. 2004 UU38 10:30:23 am Page 1 of 1 Co g r r o Sample N a m e :L1668-13 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12090837\A566720\FC000022.D Injection Date Acq Operator Instrument ^ Dilution 1/22/04 jmiller PC00414 1 10:05:14 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\012204 .M 2/26/04_____________ 10:08:53 am LC/MS analysis of perfluorooctanoic acid. 22 21 1 5 ul 1 C8 Acid ,,,,CIO Surrogate 5714.06 669559.87 0.00 518.82 7.241 8.113 *** End of Report *** MSD1 369, EIC =368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:31:13 am U39 Page 1 of 1 C00553 Sample Name :LI668-14 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\12091032\A568704\FC000023.D 1 C8 Acid -- CIO Surrogate 4615.60 728402.94 0.00 569.07 7.227 8.103 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:31:46 am U4 Page 1 of 1 C0 0 5 5 4 Sample Name :L1668-16 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12091175\A571008\FC000024.D Injection Date Acq Operator Instrument , Dilution 1/22/04 jmiller PC00414 1 10:36:21 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 24 23 1 5 pi Acq. Method Analysis Method Last C h a n g e d _ FC8-10.M C:\HPCHEM\1\METHODS\012204 .M 2/26/04 _________ 10:08:53 am LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORVI2091175\A571008\FC000024.D) 30000 API-ES, Neg, SIM, Frag: Var 7.233 - C8 Acid 25000 - 20000 - 15000 10000 5000 MSD1 469, EIC=468.7:469.7 (CHEMSTORYI2091175\A571008\FC000024.D) API-ES, Neg, SIM, Frag: Var 8 8 .1 0 8 - C10 Surrogate 80000 60000 40000 - 20000 - 1 Compound Name C8 Acid ,,C10 Surrogate Area 224633.11 670680.00 Amount 433.81 519.77 Meas. Ret. T Signal Desc. 7.233 8.108 MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 10:32:33 am U 04 Page 1 of 1 C00555 Sample Name:L1668-17 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12091264\A573120\FC000025.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmi H e r PC00414 1 10:51:57 PM Seq Line Vial No. Inj. No. Inj. Voi. 25 24 1 5 pi 1 C8 Acid CIO Surrogate 6979.76 755673.00 0.00 592.36 7.242 8.116 '* End of Report MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:36:14 am 0042 Page 1 of 1 C0 0 5 5 6 Sample Name :L1668-19 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12091353\A575168\FC000026.D "" Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 11:07:32 PM Seq Line Vial No. Inj . N o . Inj. Vol. : : : : Acq. Method FC8-10.M Analysis Method : C:\HPCHEM\1\METHODS\012204.M Last Changed____ : 2/26/04______________ 10 :08 :53 am LC/MS analysis of perfluorooctanoic acid. 26 25 1 5 pi 1 C8 Acid .CIO Surrogate 4094.76 675171.81 0.00 523.61 7.245 8.116 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7 :469.7 S PC00414 Thu, 26. Feb. 2004 0043 10:36:59 am Page 1 of 1 C0 0 5 5 7 Sample Name:L1668-20 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12091442\A577280\FC000027.D 1 C8 Acid CIO Surrogate 4583.95 746394.00 0.00 584.44 7.241 8.114 *** End of Report *** MSDl 369, EIC =368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:37:50 am U44 Page 1 of 1 C00558 Sample Name:STD 500 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\12091531\A579328\FC000028 .D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 11:38:43 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 28 4 1 5 pi Acq. Method FC8-10.M Analysis Method : C:\HPCHEM\1\METHODS\012204.M Last Changed____ : 2/26/04______________10:08:53 am LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEM STO R\12091531\A 579328\FC000028.D) API-ES, Neg, SIM , Frag: t/ar 35000 -j 7.236- C8 Add 30000 25000 j 20000 j 15000 -j 10000 j 5000- o- -, .1 T1T J* J` 1 1 1 1 1 i-----------r 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (C H E M S T O R U 2091531 \A579328\FC000028.D) API-ES, Neg, SIM , Frag: Var 8 .1 1 2 - C 10 Surrogate 80000- 60000- 40000- 20000- 11 Compound Name 1 2 11 Area r 1 11 1T ^ 46 Amount Meas. Ret. T Ji l ` 1I 8 Signal Desc. min C8 Acid CIO Surrogate 262699.81 676727.56 512.15 524.94 7.236 8.112 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7 :469.7 *** End of Report *** [ PC00414 Thu, 26. Feb. 2004 10:39:50 am U45 Page 1 of 1 CO0559 Sample Name :solvent blank Sample Info: I Data file :C:\HPCHEM\l\DATA\Chemstor\12091618\A581376\FC000029.D 1 C8 Acid -CIO Surrogate 0.00 1524.46 0.00 0.00 0.000 8.114 *** End of Report *** MSDl 369, EIC =368.7 :369.7 MSDl 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 U4 6 10:40:22 am Page 1 of 1 C0 0 5 6 0 Sample Name:STD 50 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12082179\A650816\FC000030.D Injection Date Acq Operator Instrument Dilution 1/23/04 jmiller PC00414 1 12:09:44 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method FC8-10.M Analysis Method : C:\HPCHEM\1\METHODS\012204.M r>,, Last Changed : 2/26/04______________10:08:53 am LC/MS analysis of perfluorooctanoic acid. 30 1 1 5 pi 1 C8 Acid CIO Surrogate 24847.55 70223.10 22.66 6.95 7.237 8.111 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 i.TM,. PC00414 Thu, 26. Feb. 2004 10:41:01 am uU47 Page 1 of 1 C0 0 5 6 1 Sample Name:STD 100 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12082231\A652800\FC000031.D 1 C8 Acid -,C10 Surrogate 50641.38 140791.94 75.74 67.22 7.237 8.114 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:42:43 am U0 48 Page 1 of 1 C005G2 Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12082266\A654848\FC000032.D 1 C8 Acid .CIO Surrogate 135673.20 362435.00 250.74 256.52 7.238 8.111 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC =468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:44:26 am 0 0 49 Page 1 of 1 C00563 Sample Name:STD 500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\12092002\A590208\FC000033.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/23/04 jmiller PC00414 1 12:56:24 AM Seq Line Vial No. Inj. No. Inj. Vol. : : : : FC8-10 .M C:\HPCHEM\1\METHODS\012204.M 2/26/04 10:08:53 am 33 4 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEM STO R\12092002\A590208\FC000033.D) API-ES, Neg, SIM , Frag: Zar 7 .2 4 5 - C8 Acid 35000 - 30000 j 25000 -j 20000 ^ V-,, 15000 10000^ 5000 !-<mTM 01 , , - 1 1 ' 1 T 1^ I 1 1 1 1 1---- r 2 4 6 8 min *MSD1 469, El0=468.7:469.7 (CHEM STO R\12092002\A 590208\FC000033.D) API-ES, Neg, SIM , Frag: Var 8 .1 1 3 - C10 Surrogate 80000 - 60000- 40000 - 20000 - , Compound Name C8 Acid -- CIO Surrogate ,,.i 2 Area 265541.34 682697.50 ,iri1 46 Amount Meas. Ret. T l1 i i f- 1 1 8 Signal Desc. 1I min 518.00 530.04 7.245 8.113 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 10:45:11 am Q5 Page 1 of 1 CC05fi4 Sample Name:STD 750 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12092091\A592256\FC000034 .D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/23/04 jmi H e r PC00414 1 1:12:01 AM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : FC8-10.M C:\HPCHEM\1\METHODS\012204.M 2/26/04 10:08:53 am LC/MS analysis of perfluorooctanoic acid. 34 5 1 5 pi 1 C8 Acid ,,CIO Surrogate 393610.00 993731.13 781.56 795.68 7.236 8.103 *** End of Report *** MSD1 369, EIC =368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 10:45:45 am U5 1 Page 1 of 1 0-^0565 Sample Name:STD 1000 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12092180\A594368\FC000035.D Injection Date Acg Operator Instrument Dilution 1/23/04 jmiller PC00414 1 1:27:37 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method FC8-10.M Analysis Method : C:\HPCHEM\1\METHODS\012204.M :-i, Last Changed____ : 2/26/04______________10:08:53 am LC/MS analysis of perfluorooctanoic acid. 35 6 1 5 pi 1 C8 Acid ,,.CIO Surrogate 499924.22 1247075.87 1000.35 1012.05 7.238 8.115 *** End of Report *** MSD1 359, EIC =368.7:369.7 MSD1 469, EIC =468.7:469.7 ! PC00414 Thu, 26. Feb. 2004 10:46:12 am u 0 5. Page 1 of 1 COQSfiG Sample Name:STD 1500 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12087617\A519552\FC000036.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/23/04 jmiller PC00414 1 1:43:15 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : FC8-10 .M C:\HPCHEM\1\METHODS\012204.M 2/26/04 10:08:53 am 36 7 1 5 pi 1 Compound Name C8 Acid CIO Surrogate Area 713993.87 1732682.13 Amount 1440.90 1426.78 Meas. Ret. T Signal Desc. 7.239 8.108 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 10:46:54 am U053 Page 1 of 1 G00567 (. 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 H Fax: 814-231-1580 r #: Project: P0000419 Conform COC: True f Project Storage: ----------------------------------------------------------------------------------- Conform Sample :----------- True Company Name: DuPont de Nemours & Co, Inc. Conform Request: True Submitted By: Michael D. Aucoin Login Type: Immediate Receipt of Samples Started: T Date Start: 01/19/2004 Due Date: 02/02/2004 Received Date: 01/17/2004 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: Package PK0002257 Carton Packages / Containers Mail Date / Condition S h ip p e r/ ID 1/17/2004 12:00:56PM Package & Contents Uncompromised FEDEX 8363912984560200 Temp. Control/Temp. None 23.3 Direction / Handled By R E C E IV E D AMMERMAN, MARK Container # C0026159 , C0026160 C0026161 C0026162 C0026163 C0026164 C0026165 C0026166 C0026167 C0026168 C0026169 C0026170 C0026171 C0026172 C0026173 CD026174 C0026175 C0026176 C0026177 C0026178 C0026179 C0026180 C0026181 C0026182 Gross W eight 6.3 g 6.3 g 6.3 g 6.1 g 6.1 g 6.1 g 6.3 g 6.3 g 6.3 g 6.1 g 6.1 g 6.1 g 6.2 g 6.2 g 6.2 g 6.2 g 6.2 g 6.2 g 6.1 g 6.1 g 6.1 g 6.3 g 6.3 g 6.3 g pH M iscellaneous Item Key None 1/19/2004 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 Description Preservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE ICOC U 0 54 R e p o rt V ersio n : D e c 22 2003 10:44AM Page 1 of 4 M fg. Lot Instance: Mfg. ID R0080976 R0080976 Login Sample ID L0001668-0001 L0001668-0002 . L0001668-0003 L0001668-0004 L0001668-0005 L0001668-0006 L0001668-0008 L0001668-0009 L0001668-0010 L0001668-0011 L0001668-0012 L0001668-0013 .... L0001668-0014 L0001668-0015 L0001668-0016 L0001668-0017 L0001668-0018 L0001668-0019 L0001668-0020 L0001668-0021 L0001668-0022 L0001668-0023 L0001668-0024 Matrix GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS 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 Samples Sample WWK-A-AMSFBLK-E11 A WWK-A-AMSFBLK-E11 B WWK-A-AMSFBLK-E11 C WWK-A-AMS1 -E11 A WWK-A-AMS1-E11 B W W K-A-AM S 1-E 11 C WWK-A-AMS2-E11 B WWK-A-AMS2-E11 C WWK-A-AMS3-E11 A WWK-A-AMS3-E11 B WWK-A-AMS3-E11 C WWK-A-AMS4-E11 A WWK-A-AMS4-E11 B WWK-A-AMS4-E11 C WWK-A-AMS5-E11 A WWK-A-AMS5-E11 B WWK-A-AMS5-E11 C WWK-A-AMS6-E11 A WWK-A-AMS6-E11 B WWK-A-AMS6-E11 C Control 1 A Control 1 B Control 1 C Date Sampled Date Received 01/16/2004 01/17/2004 01/16/2004 01/17/2004 01/16/2004 01/17/2004 01/16/2004 01/17/2004 01/16/2004 01/17/2004 01/16/2004 m /ie/onn/1 01/17/2004 rH /1 7 /o n n x 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/16/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 Date Due 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 m inom n* 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 1/19/2004 Login.rpt U 0 55 Report Version: Dec 22 2003 10:44AM Page 2 of 4 Instance: 009569 R0080976 R0080976 L0001668-0001 Container C 0026159/ Other /N O N E L0001668-0002 Container C0026160 / Other / NONE L0001668-0003 Container C 0026161 / O th e r/N O N E "L0001668-0004 Container C 0026162/O ther/N O N E L0001668-0005 r,,>. Container C 0026163/ Other /N O N E L0001668-0006 Container C0026164 / Other / NONE L0001668-0007 Container ... C 0026165/O ther/N O N E L0001668-0008 Container C 0026166/ Other /N O N E ,,L0001668-0009 Container C 0026167/O ther/N O N E L0001668-0010 Container - C 0026168 / Other / NO NE L0001668-0011 Container C 0026169/ Other /N O N E - L 0 0 0 1 668-0012 Container C002617 0 /O th er/N O N E _ 1/19/2004 Bottles Method Method Method Method Method Method Method Method Method Method Method Method u 0 b6 Report Version: Dec 22 2003 10:44AM Instance: R0080976 R0080976 L0001668-0013 Container C0026171 / O ther/N O N E Login Method L0001668-0014 Container C 0026172/ Other / NONE Method L0001668-0015---------------------------------------------------------------- Container C 0026173/O ther/N O N E Method L0001668-0016 Container C 0026174/O ther/N O N E Method L0001668-0017 Container C 0026175/O ther/N O N E Method L0001668-0018 Container C0026176 / Other / NONE Method L0001668-0019 Container C 0026177/O ther/N O N E Method L0001668-0020 Container C0026178/ Other/ NONE Method L0001668-0021 Container -- 0 0 0 2 6 1 7 9 /O ther/N O N E Method L0001668-0022 Container C 0026180/ Other /N O N E Method --L0001668-0023 Container C0026181 / Other / NONE Method L0001668-0024 Container -- C 0026182/O ther/ NONE Method 1/19/2004 Login.rpt JU57 Report Version: Dec 22 2003 10:44AM Page 4 of 4 Instance: c R0080976 R0080976 CHAIN OF CUSTODY/ANALYSIS REQUEST FORM 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 II P a g e __ _ o f _ J ___ Sam plers): SO, RK, LK DuPont Washington Works Air Sampling Program FedEx Airbill #: 836391298456 Event Number 669842 669908 669901 669890 669796 669865 Hours 0 1 2 3 4 AMS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes 0 60 120 180 240 WW K-A-AM S1-E11 WWK-A-AMS2-E11 WWK-A-AMS3-E11 WW K-A-AM S4-E11 WWK-A-AMS5-E11 WWK-A-AMS6-E11 Hours 5 6 7 8 9 0.9970 1.0160 1.0200 1.0180 1.0210 1.0150 Minutes 300 360 420 480 540 Field Blank: yes WWK-K-AMSFBLK-E11 yes or no Weather: 1/15 Cold, aljout 27 F, snow flurries, windy 1/16 Cold, bout 18 F, clear, breezy 15-Jan 15-Jan 15-Jan 15-Jan 15-Jan 15-Jan Hours 10 11 12 13 14 0700 0625 0627 0632 0638 0647 Minutes 600 660 720 780 840 16-Jan 16-Jan 16-Jan 16-Jan 16-Jan 16-Jan Hours 15 16 17 18 19 0620 0635 0637 0658 0645 0722 Minutes 900 960 1020 1080 1140 0.9794 0.9739 1.0130 1.0140 0.9687 1.0330 Hours 20 21 22 23 24 Event 11 1398 1448 ` 931 1424 1402 1434 Minutes 1200 1260 1320 1380 1440 SAFER operational: yes yes or no Comments: Total minute s column is the reading from the monitor counter. * AMS-3 was still running when we collected the sample after about 1410 minutes, but the counter only read 931 minutes. CO r LC O c o Os L-O *111J ---\ f 1/16/2004 Page 1 of 2 airdataeventl 1 C ^0574 DuPont Washington Works Air Sampling Program Sampler(s): SO, RK, LK FedEx Airbill #: 836391298456 Event Number 669842 669908 669901 669890 669796 669865 Hours 0 1 2 3 4 AMS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes 0 60 120 180 240 WWK-A-AMS1 -E1 1 WWK-A-AMS2-E11 WWK-A-AMS3-E11 WWK-A-AMS4-E11 WWK-A-AMS5-E11 WWK-A-AMS6-E11 Hours 5 6 7 8 9 0.9970 1.0160 1.0200 1.0180 1.0210 1.0150 Minutes 300 360 420 480 540 Field Blank: yes WWK-K-AMSFBLK-E11 yes or no WB m m m m m w m m 15-Jan 0700 16-Jan 15-Jan 0625 16-Jan 15-Jan 0627 16-Jan 15-Jan 0632 16-Jan 15-Jan 0638 16-Jan 15-Jan 0647 16-Jan Hours Minutes Hours 10 600 15 11 660 16 12 720 17 13 780 18 14 840 19 0620 0635 0637 0658 0645 0722 Minutes 900 960 1020 1080 1140 0.9794 0.9739 1.0130 1.0140 0.9687 1.0330 Hours 20 21 22 23 24 Weather: 1/15 Cold, about 27 F, snow flurries, windy 1/16 Cold, cbout 18 F, clear, breezy Event 11 1398 1448 *931 1424 1402 1434 Minutes 1200 1260 1320 1380 1440 Total Volume 1383 liters 1443 liters *946 liters 1489 liters 1440 liters 1510 liters O vO CD CD SAFER operational yes yes or no Comments: Total minute;s column is the reading from the monitor counter, AMS-3 was still running when we collected the sample after about 1410 minutes, but the counter only read 931 minutes. 1/28/2004 Page 1 of 2 airdataeventl 1 RESEARCH ' Precise Research. Proven Results. Sample "Condition Upon Receipt" Form Protocol# Oac^a^/f? Exygen Study # oo /6-Cif Date & Time Received O/J *1/0*4 /Ic o Condition of Samples Temporary Storage Location Pciv Initials & Date /id(4 cs/r?/ff Waybill # r?6 i 9 /^ ____________________ Comments: A /C r /-/- cJy a`'Z /'7 /i* M ay 24, 2002/3 Q:'W ORD proeess-logm\SampleConditiononReceipt.doc 6 1 3053 Research Drive State College, PA 16801, USA T: 8 0 0 .2 8 1 .3 2 1 9 F: 814.272.1019 cyj5Bn.com UQ62 crcrr*6