Document vyQxZbzNmb3RVVLO026bZ5B19

Attachment 2 Analytical Report Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 7 Exygen Research Report No. L0001444 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 &ias < CO t\> S p n `{ to c~:' O o o AT T. DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 1 of 7 A G002G8 305'8 Research Drive State College, PA 16801, USA T: 800.281.3219 F: 814.272.1019 exygen.com Summary Seven solid media samples were received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. The media represent samples of air collected on OVS tubes. Please see Table 1 for a completed listing of samples received and field air volumes collected. Sample WWK-A-AMS3-E7 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. Instmment operating conditions can be found at the beginning of each analytical run. Raw instrument data is given in Appendix A. Chain-of-custody information can be found in Appendix B. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 2 of 7 000269 Results Summary Request # WWK-A-AMS1-E7 A WWK-A-AMS1-E7 B WWK-A-AMS1-E7 C WWK-A-AMS1-E7 (Total) Air Volume Sampled (L) 1356 1356 1356 C8 Acid (mq/m3) 0.0003 < 0.00007 NA 0.0003 WWK-A-AMS2-E7 A WWK-A-AMS2-E7 B WWK-A-AMS2-E7 C WWK-A-AMS2-E7 (Total) 1490 1490 1490 0.0003 < 0.00007 NA 0.0003 WWK-A-AMS4-E7 A WWK-A-AMS4-E7 B WWK-A-EMS4-E7 C WWK-A-EMS4-E7 (Total) 1652 1652 1652 < 0.00006 < 0.00006 NA <0.00012 WWK-A-AMS5-E7 A WWK-A-AMS5-E7B WWK-A-AMS5-E7 C WWK-A-AMS5-E7 (Total) 1530 1530 1530 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS6-E7 A WWK-A-AMS6-E7 B WWK-A-AMS6-E7 C WWK-A AMS6-E7 (Total) 1539 1539 1539 < 0.00006 < 0.00006 NA <0.00012 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 OYS 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 000270 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) 397 C8 Acid (percent recovery 79 Blanks Request # WWK-A-AMSFBLK-E7 A WWK-A-AMSFBLK-E7 B Voi. Of Air (L) 0 0 C8 Acid (uq/fraction) <0.10 <0.10 000271 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-E7 A WWK-A-AMSFBLK-E7 B WWK-A-AMS1-E7 A WWK-A-AMS1-E7 B WWK-A-AMS2-E7 A WWK-A-AMS2-E7 B WWK-A-AMS4-E7 A WWK-A-AMS4-E7 B WWK-A-AMS5-E7 A WWK-A-AMS5-E7 B WWK-A-AMS6-E7 A WWK-A-AMS6-E7 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) 639 353 530 374 603 382 511 462 596 417 566 373 453 347 Percent Recovery (%) 128* 71* 106 75 121 76 102 92 119 83 113 75 91 69* * Surrogate recovery outside of advisory range. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 000272 Calculations Request # WWK-A-AMSFBLK-E7 A WWK-A-AMSFBLK-E7 B WWK-A-AMS1-E7 A WWK-A-AMS1-E7 B WWK-A-AMS2-E7 A WWK-A-AMS2-E7 B WWK-A-AMS4-E7 A WWK-A-AMS4-E7 B WWK-A-AMS5-E7 A WWK-A-AMS5-E7 B WWK-A-AMS6-E7 A WWK-A-AMS6-E7 B Control Spike A Control Spike B Vol. Of Air (L) 0 0 1356 1356 1490 1490 1652 1652 1530 1530 1539 1539 0 0 C8 Acid (raw-ppb) < 10 <10 429 < 10 426 <10 <10 <10 <10 <10 <10 <10 397 < 10 C8 Acid (ug/fraction) <0.10 <0.10 0.43 <0.10 0.43 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 0.40 <0.10 C8 Acid (mg/m3) 0.0003 < 0.00007 0.0003 < 0.00007 < 0.00006 < 0.00006 < 0.00007 < 0.00007 < 0.00006 < 0.00006 000273 AT T. DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 7 Example Calculation For sample WWK-A-AMS2-E7 A C8 Acid, = [426 ng/ml of C8 Acid x (1ml) x (1 ug / 1000 ng) x (1 mg / 1000 ug) ] / [(1490 L) x (1 m3 / 1000 L)] = 0.0003 mg / m3 Signatures Other Lab Members Contributing to Data James Miller Date Date ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 7 G00274 Table 1. Login Information / Field Data Sample ID Exygen Lab ID Date Received Description WWK-A-AMSFBLK-E7 A WWK-A-AMSFBLK-E7 B WWK-A-AMSFBLK-E7 C WWK-A-AMS1-E7 A WWK-A-AMS1-E7 B WWK-A-AMS1-E5 C WWK-A-AMS2-E7 A WWK-A-AMS2-E7B WWK-A-AMS2-E7 C WWK-A-AMS4-E7 A WWK-A-AMS4-E7 B WWK-A-AMS4-E7 C WWK-A-AMS5-E7 A WWK-A AMS5-E7 B WWK-A-AMS5-E7 C W W K-A-AMS6-E7 A WWK-A-AMS6-E7 B WWK-A AMS6-E7 C Control Spike A Control Spike B Control Spike C L0001444-1 L0001444-2 L0001444-3 L0001444-4 L0001444-5 L0001444-6 L0001444-7 L0001444-8 L0001444-9 L0001444-13 L0001444-14 L0001444-15 L0001444-16 L0001444-17 L0001444-18 L0001444-19 L0001444-20 L0001444-21 L0001444-22 L0001444-23 L0001444-24 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 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 1356 1356 1356 1490 1490 1490 1652 1652 1652 1530 1530 1530 1539 1539 1539 0 0 0 a o o N si Cl 000276 U0 09 Table 2. Chain of Custody Sample ID WWK-A-AMSFBLK-E7 A WWK-A-AMSFBLK-E7 B WWK-A-AMSFBLK-E7 C WWK-A-AMS1-E7 A WWK-A-AMS1-E7 B WWK-A-AMS1-E5 C WWK-A-AMS2-E7 A WWK-A-AMS2-E7B WWK-A-AMS2-E7 C WWK-A-AMS4-E7 A WWK-A-AMS4-E7 B WWK-A-AMS4-E7 C WWK-A-AMS5-E7 A WWK-A AMS5-E7 B WWK-A-AMS5-E7 C WWK-A-AMS6-E7 A WWK-A-AMS6-E7 B WWK-A AMS6-E7 C Control Spike A Control Spike B Control Spike C Date Collected 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 12/11/03 NA NA NA Date Received at Exygen 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 Date Extracted by Exygen 12/18/03 12/18/03 NA 12/18/03 12/18/03 NA 12/18/03 12/18/03 NA 12/18/03 12/18/03 NA 12/18/03 12/18/03 NA 12/18/03 12/18/03 NA 12/18/03 12/18/03 NA Date Analyzed by Exygen 12/18-12/19/03 12/18-12/19/03 NA 12/18-12/19/03 12/18-12/19/03 NA 12/18-12/19/03 12/18-12/19/03 NA 12/18-12/19/03 12/18-12/19/03 NA 12/18-12/19/03 12/18-12/19/03 NA 12/18-12/19/03 12/18-12/19/03 NA 12/18-12/19/03 12/18-12/19/03 NA ANALYTICAL DATA REVIEW SHEET LC/MS Analyst - /A 'H c r Signature/Date Join m Reviewed by ' j?J. /n ^Signature/Date 0010 000277 Sequence: C:\HPCHEM\1\SEQUENCE\121803.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 4 27 Vial 92 28 Vial 1 29 Vial 2 30 Vial 3 31 Vial 4 32 Vial 5 33 Vial 6 34 Vial 7 STD 50 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb solvent blank L0001444-22 L0001444-23 L0001444-1 L0001444-2 L0001444-4 L0001444-5 L0001444-7 L0001444-8 L0001444-13 L0001444-14 STD 500 ppb solvent blank L0001444-16 L0001444-17 L0001444-19 L0001444-20 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 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 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 28 Vial 1 29 Vial 2 30 Vial 3 31 Vial 4 32 Vial 5 33 Vial 6 34 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 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 jCMS5 12/18/03 4:36:36 PM jmiller i Page 1 of 1 000278 LC/MS SYSTEM AND OPERATING CONDITIONS Client: Dupont EXYGEN STUDY: L0001444 Instrument: Hewlett-Packard 1100 LC/MSD (LC/MS 5) 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 G1322A Solvent Degasser HP G1311A Quaternary Pump HP G1313A Autosampler HP G1316A Column Thermostat HP G1946AMSD 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 1 000279 Ions monitored: Analyte C8 Acid (PFOA) C10 Surrogate Ion (m/z) 369 469 Extraction Date: December 18, 2003 Analyst: James R. Miller '03 Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039, FAX: (814) 231-1580 Page 2 of 2 u0 !3 000280 Instrument : LCMS5 Tue Dec 16 12:15:46 2003 m/z 112.99 gfO.Ol Ab 262975 Pw 0.62 Gl946: API_ES Negative mode Page 1 of 3 C :\HPCHEM\1\19 46TUNE\ATUNES.TUN m/z 602.00 gf0.02 Ab 36351 Pw 0.59 m/z 1034 .05 max Ab 135231 Pw 0.66 J) -- i-- i-- |-- i ^1 -L-|---- 1-- ,---110 115 m/z 1634.05 max Ab 307839 Pw 0.64 J 600 11 1 605 m/z 2234 .15 max Ab 346109 Pw 0.66 , ,, ,, --r J,, , i . l- i 1030 1035 -1--1--!--1-^=L---1 I =P*-T 1630 1635 ,i 2230 J |11! 2235 Scan: 50.00 - 3000.00 Samples: 8 Thresh: 0 Step: 0.10 29501 peaks Base: 2234.15 Abundance: 335232 F Raw,Gauss 0.3 100 -, 80 - 60 - 40 - 20 - " 1-- 1 r 1-- r" r 1 500 1000 1500 11 2000 1r 2500 m/z gf 112.96 601.99 1034.05 1634.05 2234.15 Abund 243712 32600 147776 307520 335232 Rei Abund 100.00 13.38 60.64 126.18 137.55 Iso m/z 113.99 602.95 1035.05 1635.05 2235.15 Iso Abund Iso Ratio 4075 1.67 2771 8.50 32352 21.89 117312 38.15 156608 46.72 001 4 C00281 Instrument : LCMS5 Tue Dec 16 12:15:46 2003 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 1031 6.0 WidthOffs VAR -3.8 MassGain 93.65 14 MassOffs 0.516 -8 Energy 5.0 OpolPeak 300 OpolKnee. 315 2.0 QuadDC 0.00 EMV VCap Status: CapCur ChamCur 1788 Samples 8 4000 Averages 1 StepSize 0.10 39 DryinqGas 7.0 0.51 Gas Temp 300 Quad Temp 99 Neb Pres 15 Instrument : LCMS5 Tue Dee 16 12:15:46 2003 Gl946: API_ES Negative mode Page 3 of 3 C :\HPCHEM\1\194 6TUNE\ATUNES.TUN Width Offset 0- Dynamic Parameter Ramp -20 - -40 - -60 - -80 - -100 - -120 - -140 - -160 --------- 1-- 1 r--- , i i | , 500 1000 i 1500 ! | 1 1 1-- 1 r- 1 1-- r 1 1 2000 2500 3000 Mass 112.99 1633.95 Setting -159.00 -159.00 Mass 601.98 2233.91 Setting -159.00 -159.00 Mass 1033.99 Setting -159.00 y 0016 0Q02S3 Method C:\HPCHEM\1\METHODS\121803.M Calibration Table Calib. Data Modified Friday, December 19, 2003 1:56:55 PM Calculate Based on External Standard Peak Area Rel. Reference Window Abs. Reference Window Rel. Non-ref. Window Abs. Non-ref. Window Uncalibrated Peaks Partial Calibration Correct All Ret. Times 5.000 % 0.000 min 5.000 % 0.000 min not reported Yes, identified peaks are recalibrated No, only for identified peaks Curve Type Origin Weight Linear Ignored Equal Recalibration Settings: Average Response : Average Retention Time: Average all calibrations Floating Average New 75% Calibration Report Options : Printout of recalibrations within a sequence: Calibration Table after Recalibration Normal Report after Recalibration If the sequence is done with bracketing: Results of first cycle (ending previous bracket) Signal 1: MSD1 369, EIC=368.7 :369.7 Signal 2: MSD1 469, EIC=468.7 :469.7 RetTime Lvl Amount Area [min] Sig [ppb] I1 11 7.339 1 1 50.00000 ^1.91706e4 2 100.00000 3.74002e4 3 250.00000 9.89139e4 4 500.00000 1.89929e5 5 750.00000 2.73895e5 6 1000.00000 3.59012e5 7 1500.00000 5.28202e5 8.187 2 1 50.00000 2.24230e4 2 100.00000 4.55873e4 3 250.00000 1.19659e5 4 500.00000 2.31083e5 5 750.00000 3.33 034e5 6 1000.00000 4.39381e5 7 1500.00000 6.46494e5 Amt/Area Ref Grp Name ^2.60816e-3 2.67378e-3 2.52745e-3 2.63257e-3 2.73827e-3 2.78542e-3 2.83982e-3 2.22985e-3 2.19360e-3 2.0892 6e-3 2.16372e-3 2.25202e-3 2.27593e-3 2.32021e-3 1 1 C8 Acid CIO Surrogate Peak Slim Table ***No Entries in table*** C00414 12/19/03 1:58:12 PM jmiller 0 017 o 0 0 0 2 8 4 Page 1 of 2 Method C :\HPCHEM\1\METHODS\121803.M Calibration Curves C8 Acid at exp. RT: 7.339 MSD1 369, EIC=368.7:369.7 Correlation: 0.99960 Residual Std. Dev.: 5753.73977 Formula: y = mx + b m: 350.58149 b: 7372.79770 x: Amount[ppb] y : Area CIO Surrogate at exp. RT: 8.187 MSD1 469, EIC=468.7:469.7 Correlation: 0.99966 Residual Std. Dev.: 6500.97419 Formula: y = mx + b m: 429.63717 b: 7809.73846 x: Amount[ppb] y: Area l C00414 12/19/03 1:58:12 PM jmiller tz//n /. /03 U LI ! 8 0 0 0 2 8 5 age 2 of 2 initiate Date / Run# FCooo&o/ ~Jq Sample Name:STD 50 ppb Sample Info:Warm Up 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11665613\A439168\FC000001.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 4:46:08 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : i i i 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803 .M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11665613\A439168\FC000001.D) API- ES, Neg, SIM, Frag: Var 7.375 - C8 Acid 2000 - 1500- 1000- 500- _ . . . . . _____________ . 1i r 2 ^ r^ 4 1 i 6 1 *MS01 469, EIC=468.7:469.7 (CHEMSTORM 1665613\A439168\FC000001 .D) J1 _______ / \ / v ' 11 i 11i 8 min API-ES, Neg, SIM, Frag: Var 8.198- C10 Surrogate 2500- 2000 : 1500- 1000- 500- ', .Iri I| 24 Compound Amount (ng/mL) R.T. 18 Acid 31.12 10 Surrogat 31.07 7.375 8.198 r.I Area 18282 21159 LVi | 1^ 111r 6 8 min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 I PC00414 *** End of Report *** Fri, 19. Dec. 2003 U 0 19 02:04:37 pm Page 1 of 1 000286 Sample Name:STD 50 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11665743\A441600\FC000002.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method -.. Last Changed 12/18/03 jmiller PC00414 1 5:01:15 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : FC8-10 .M C :\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm 2 1 1 5 pi LC/MS analysis of perfluoro carboxylic acids. MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1665743\A441600\FC000002.D) API-ES, Neg, SIM, Frag: Var 2000- 7.342- C8 Acid 1750 1500-1 1250 1000- 750 J 500 250 H J_L 2250 8 MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1665743\A441600\FC000002.D) API-ES, Neg, SIM, Frag: Var 8.185 - C10 Surrogate min 2000 1750 1500 -jj 1250 1000 750 500 .. 1 250 --- !--- 1-- 1 2 1 -1--- --- 1--!--- ,--- ,--- 1--- 1--- '--- r---,--- r 4 6 8 min Compound Amount (ng/mL) R.T. Area Signal CT-8 Acid 32.67 10 Surrogat 32.63 7.342 8.185 18826 21827 MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 UQ2 02:05:11 pm Page 1 of 1 000287 Sample Name:STD 100 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11665844\A443840\FC000003.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 5:16:24 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 3 2 1 5 pi Acq. Method Analysis Method ,. Last Changed FC8-10.M C :\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *** *MS01 369, EIC=368.7:369.7 (CHEMSTORM1665844\A443840\FC000003.D) API-ES, Neg, SIM, Frag: Var 4000- 7.369 - C8 Acic -- 3500 - 3000 - ... 2500 j I 2000 - 1500- 1000 j ... 500 - .. ____________________________ 1 _L___ ,, _ 0- -r i I| r ' r [ ' ' 1 1 11 i -- . ---- r 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1665844\A443840\FC000003.D) API-ES, Neg, SIM, Frag: Var . r 4000- 8.201 - C10 Surrogata 3000- 2000- 1000- - 0- Compound ' -1 2 Amount (ng/mL) 7 4 R.T. C.8 Acid 86.58 10 Surrogat 88.74 7.369 8.201 J. 11 11 ' 1 -, | ' 11 1 r 6 8 min Area Signal 37725 45934 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:07:03 pm 0 021 Page 1 of 1 000288 r Sample Name:STD 250 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11665921\A446144\FC000004.D Injection Date Acq Operator Instrument ^, Dilution 12/18/03 jmiller PC00414 1 5:31:42 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : 4 3 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\121803 .M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11665921\A446144\FC000004.D) API-ES, Neg, SIM, Frag: Var 10000- 7.370 - C8 Acic 8000- 6000- 4000- 2000- 1 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1665921\A446144\FC000004.D) API-ES, Neg, SIM, Frag: Var 12000- 8.191 - C10 Surrogate, min 10000- 8000- 6000- 4000- 2000- Compound Amount (ng/mL) R.T. -8 Acid 262.43 10 Surrogat 264.26 7.370 8.191 - Area 99378 121344 min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** I PC00414 Fri, 19. Dec. 2003 02 2 02 :09 :01 pm Page 1 of 1 000289 Sample Name:STD 500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11665999\A448384\FC000005.D Injection Date Acq Operator Instrument .. Dilution Acq. Method Analysis Method -.* Last Changed 12/18/03 jmiller PC00414 1 5:46:50 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : FC8-10.M C:\HPCHEM\1\METHODS\121803 .M 12/19/03 01:56:57 pm 5 4 1 5 pi LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1665999\A448384\FC000005.D) API-ES, Neg, SIM, Frag: Var 7.356- C8 Acid 17500- 15000- 12500 -J 10000- 7500- 5000- 2500 H 0*MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1665999\A448384\FC000005.D) "-1 1 T 8 min API-ES, Neg, SIM, Frag: Var 8.182- C10 Surrogate: 20000 - 15000- 10000- 5000- Compound Amount (ng/mL) R.T. -38 Acid 512.44 10 Surrogat 513.11 7.356 8.182 Area 187025 228261 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 002.5 02:09:21 pm Page 1 of 1 C00290 Sample Name:STD 750 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11666074\A450688\FC000006 .D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 6:01:59 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 6 5 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODSU21803 .M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1666074\A450688\FC000006.D) API-ES, Neg, SIM, Frag: Var 7.354- C8 Acid 25000 - 20000 - 15000** 10000- 5000- I 0 , , . | ' 1 ' 1^ 1' | 1 246 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1666074\A450688\FC000006.D) i ' iii 8 API-ES, Neg, SIM, Frag: Var I min 8.182- C10 Surrogate 30000 - 25000 - 20000 -j 15000- 10000-^ 5000 J 1 1 1 ' I 1 1 1 i--- 1--- 1--- 1--- 1--- 1--- 1--- 1--- r 2__________________4__________________6__________________8________________ min Compound Amount (ng/mL) R.T. Area Signal 38 Acid 760.75 10 Surrogat 755.15 7.354 8.182 274076 332250 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 1 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:09:59 pm 0024 Page 1 of 1 000291 Sample Name:STD 1000 ppb r* Sample Info: i Data file :C:\HPCHEM\l\DATA\Chemstor\11666134\A452992\FC000007.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 6:17:10 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10.M C: \HPCHEM\1\METHODSU21803 .M 12/19/03 01:56:57 pm 7 6 1 5 pi LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11666134\A452992\FC000007.D) API-ES, Neg, SIM, Frag: Var 35000 -j 7.375- C8 Acid 30000 ^ 25000 - 20000 15000- 10000- 5000- 0- 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORYI1666134\A452992\FC000007.D) API-ES, Neg, SIM, Frag: Var 8.198- C10 Surrogata mm 40000 - 30000 - 20000 - 10000- --- , ,--- 1--- I- , i--- 1-- 24 LA -- 1--- 1 -- i--- --- 1--- 1--- 1--- 1--- r 6 8 min Compound Amount (ng/mL) R.T. Area Signal --8 Acid 1032.33 10 Surrogat 1037.58 7.375 8.198 369290 453592 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02 :10 :57 pm 0025 Page 1 of 1 000292 Sample Name:STD 1500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11666207\A455296\FC000008.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 6:32:20 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : 8 7 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11666207\A455296\FC000008.D) API-ES, Neg, SIM, Frag: Var 50000 - 7.352- C8 Aclc, 40000- 30000 - 20000 - 10000- II 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORYI1666207\A455296\FC000008.D) API-ES, Neg, SIM, Frag: Var 8.173- C10 Surrogata 60000 - min 50000 - 40000 -j 30000 - 20000 - 10000H o- -- !--- --- '--- '--- r ---- --- 1-- -, !--- 1 i--- 1--- r 2 4 6 8 min Compound Amount (ng/mL) R.T. Area Signal -''8 Acid 1496.55 10 Surrogat 1507.26 7.352 8.173 532034 655385 MSDl 369, EIC=3 68.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:11:24 pm UU2 Page 1 of 1 000293 Sample Name:solvent blank Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11666302\A457536\FC000009.D 1 ~8 Acid 0.00 10 Surrogat 0.00 7.366 0.000 327 0 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:12:01 pm 0 0 27 Page 1 of 1 000294 Sample NameL0001444-22 Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11666338\A460096\FC000010.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 7:02:35 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 10 11 1 5 pi Acq. Method Analysis Method -- Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11666338\A460096\FC000010.D) API- ES, Neg, SIM, Frag: Var 18000j 7.361 - C8 Acid 16000j 14000 -j 12000 10000^ 8000 j 6000 -7 4000 -7 2000 j o - I A_____ , , i i i i------- , i ' 1 1------- 1------- 1------- 1----- i ,------- ,------- ,------- r 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM1666338\A460096\FC000010.D) API-ES, Neg, 31M, Frag: Var 25000 - 8.192- C10 Surrogate 20000- 15000- 10000- 5000- 0 - ._ _ ' ' ' , . 1II 24 Compound Amount (ng/mL) R.T. -C8 Acid 397.35 .'IO Surrogat 453.57 7.361 8.192 . I Area 146677 202682 l I 1 1 i ,------- ,------- ,------- r 6 8 min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC 00414 *** End of Report *** Fri, 19. Dec. 2003 U28 02:12:28 pm Page 1 of 1 000295 ,iw*A Sample Sample Name:L0001444-23 Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11666444\A462400\FC000011.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 7:17:45 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 1 11 12 1 5 p.1 Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. MSD1 369, EIC=368.7:369.7 (CHEMSTORM1666444\A462400\FC000011.D) API-ES, Neg, SIM, Frag: Var 7.366- C8 Acid 1000 800- 600 400 200- 'MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1666444\A462400\FC000011.D) API-ES, Neg, SIM, Frag: Var 20000 H 8.190- ClOSurrogate 17500 15000- 12500- 10000 7500 -j 5000 2500 o-t Compound Amount (ng/mL) R.T. ''8 Acid 1.66 .`10 Surrogat 347.26 7.366 8.190 Area 7954 157006 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 0029 02:13:34 pm Page 1 of 1 000296 Sample Name :L0001444-1 Sample Info : Data file :C :\HPCHEM\1\DATA\Chemstor\11666499\A464640\FC000012.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmi H e r PC00414 1 7:32:54 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm 1 12 13 1 5 pi Compound Amount (ng/mL) R.T. '"8 Acid 0.00 :10 Surrogat 638.73 0.000 8.203 Area 0 282232 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:15:06 pm 0030 Page 1 of 1 c00297 Sample Name:L0001444-2 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11666575\A467008\FC000013 .D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 7:48:03 PM Seq Line Vial No. Inj. No. Inj. Voi. : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803 .M 12/19/03 01:56:57 pm 1 13 14 1 5 pi Compound Amount (ng/mL) R.T. --8 Acid 0.00 10 Surrogat 352.59 0.000 8.193 Area 0 159294 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:16:01 pm 03 ! Page 1 of 1 000298 Sample Name:L0001444-4 Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11666652\A469248\FC000014.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 8:03:13 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 14 15 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11666652\A469248\FC000014.D) API-ES, Neg, SIM, Frag: Var 18000 7.350- C8 Acid 16000 14000 12000 10000 8000 6000 4000 2000 0 MSD1 469, EIC=468.7:469.7 (CHEMSTORM1666652\A469248\FC000014.D) API-ES, Neg, SIM, Frag: Var 30000 8.182 - C10 Surrogate 25000 20000 - 15000- 10000- 5000- Compound Amount (ng/mL) R.T. "8 Acid 429.25 10 Surrogat 530.18 7.350 8.182 ~r 6 min Area Signal 157861 235597 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02 :16 :59 pm 0032 Page 1 of 1 000299 Sample Name :L0001444-5 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11666728\A471424\FC000015.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmi H e r PC00414 1 8:18:29 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm 1 15 16 1 5 pi Compound Amount (ng/mL) R.T. "'a8 Acid 0.00 10 Surrogat 374.36 7.389 8.203 Area 1267 168649 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:18:35 pm u036 Page 1 of 1 Sample Name:L0001444-7 Sample Info : 1 Data file :C:\HPCHEMN1\DATA\ChemstorM1666788\A473600\FC000016.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 8:33:39 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 16 17 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1666788\A473600\FC000016.D) API-ES, Neg, SIM, Frag: Var 7.365- C8 Acid 16000- 14000- 12000- 10000- 8000- 6000 H 4000- 2000- 0- _L *MSD1 469, EIC=468.7:469.7 (CHEMSTORVI1666788\A473600\FC000016.D) API-ES, Neg, SIM, Frag: Var 8.198 - C10 Surrogatei min 30000 25000 - 20000 -j 15000 10000- 5000 0 --- 1--- 1--- 1--- r---1--- 1--- r 24 Compound Amount (ng/mL) R.T. :8 Acid 425.78 :10 Surrogat 603.05 7.365 8.198 -[--- 1--- 1-- ~1--- 1--- 1--- 1--- 1 r 6 8 min Area Signal 156643 266904 MSDl 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 F' PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:21:12 pm 003 4 Page 1 of 1 000301 Sample N a m e :L0001444-8 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11666866\A475904\FC000017.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 8:48:49 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm 1 17 18 1 5 pi S8 Acid 0.00 10 Surrogat 382.30 7.358 8.183 1583 172062 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 j PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:22:11 pm Q 35 Page 1 of 1 00030 Sample Name :L0001444-13 Sample Info: Data file -.C:\HPCHEM\l\DATA\Chemstor\11666921\A478080\FC000018.D 1 f,8 Acid 0.00 10 Surrogat 510.68 7.347 8.185 5021 227217 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:23:06 pm 0036 Page 1 of 1 G Q 0303 Sample Name:L0001444-14 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11666976\A480128\FC000019.D 1 8 Acid 0.00 L0 Surrogat 462.39 0.000 8.209 0 206471 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 >000414 *** End of Report *** Fri, 19. Dec. 2003 02:24:30 pm 37 Page 1 of 1 000304 Sample Name:STD 500 ppb *i'- " Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11667053\A482368\FC000020.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 9:34:19 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 20 4 1 5 ]il Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. ` MSD1 369, EIC=368.7:369.7 (CHEMSTORM1667053\A482368\FC000020.D) API-ES, Neg, SIM, Frag: Var 7.361 - C8 Acid 20000 - 15000- I.. 10000- 5000- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1667053\A482368\FC000020.D) API-ES, Neg, SIM, Frag: Var 8.210- C10 Surrogate 25000 20000 15000- 10000- 5000- Compound Amount (ng/mL) R.T. 438 Acid 523.38 10 Surrogat 526.00 7.361 8.210 Area 190860 233800 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** CX Fri, 19. Dec. 2003 02:25:02 pm u U Page 1 of 1 000305 Sample Namesolvent blank Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11667132\A484608\FC000021.D 1 18 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 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:25:36 pm 0 39 Page 1 of 1 000306 Sample Name :L0001444-16 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11667167\A487104\FC000022.D 1 -8 Acid 0.00 :10 Surrogat 596.44 7.349 8.185 1127 264063 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 i ( PC00414 *** End of Report *** Fri, 19. Dec. 2003 U4U 02:29:26 pm Page 1 of 1 000307 Sample Name:L0001444-17 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\11667253\A489344\FC000023.D 1 ^8 Acid 0.00 10 Surrogat 416.90 t* 0.000 8.190 0 186925 MSDl 369, EIC=368.7 :369.7 MSDl 469, EIC=468.7:469.7 *** End of Report *** PC00414 Fri, 19. Dec. 2003 02 :29 :50 pm 00 4 ! Page 1 of 1 000308 Sample Name:L0001444-19 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11667330\A491712\FC000024.D 1 IZ8 Acid 0.00 10 Surrogat 565.53 7.347 8.187 1692 250781 MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:30:32 pm U Page 1 of 1 000309 Sample Name:L0001444-20 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11667385\A493760\FC000025.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmi H e r PC00414 1 10:50:07 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm 1 25 24 1 5 pi Compound Amount (ng/mL) R.T. G& Acid 0.00 10 Surrogat 372.65 0.000 8.183 Area 0 167914 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 02:31:06 pm 0043 Page 1 of 1 G00310 Sample Name:STD 500 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11667439\A495808\FC000026 .D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 11:05:14 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 26 4 1 5 g.1 Acq. Method Analysis Method ....... Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTORVI1667439\A495808\FC000026.D) API-ES, Neg, SIM, Frag: Var 7.347- C8 Adel 20000 15000 10000- 5000- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM1667439\A495808\FC000026.D) API-ES, Neg, SIM, Frag: Var 8.188- C10 Surrogate 25000 20000 15000- 10000- 5000- 0-- Compound Amount (ng/mL) R.T. C8 Acid 517.81 10 Surrogat 519.29 7.347 8.188 Area 188908 230918 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 ..... *** End of Report *** [ PC00414 Fri, 19. Dec. 2003 02:31:51 pm 0044 Page 1 of 1 G00311 Sample Name:solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11667493\A497984\FC000027.D Injection Date Acq Operator Instrument , Dilution 12/18/03 jmiller PC00414 1 11:20:23 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803 .M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. 1 27 92 1 5 pi 0.8 Acid 0.00 10 Surrogat 0.00 0.000 0.000 0 0 MSD1 369, EIC=3 68.7:3 69.7 MSDL 469, EIC=468.7:469.7 i *** End of Report *** PC00414 Fri, 19. Dec. 2003 U045 02:31:36 pm Page 1 of 1 000312 Sample Name:STD 50 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11667546\A500224\FC000028.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 11:35:37 PM Seq Line Vial No. Inj . N o . Inj. Voi. : : : : 28 1 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. MSD1 369, EIC=368.7:369.7 (CHEMSTORM1667546\A500224\FC000028.D) API-ES, Neg, SIM, Frag: Var 2000 7.337- C8 Acid, 1750 H 1500 1250 1000-j 750 500 250 _ L *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1667546\A500224\FC000028.D) API-ES, Neg, SIM, Frag: Var 2500- 8.174- C10 Surrogate, 2000- 1500- 1000- 500- .. 11 --- !--- 1-- 1 1 1 -1--- --- 1--- j--- ,--- 1--- --- 1--- >--- 1--- 1--- f 2 4 6 8 min Compound Amount (ng/mL) R.T. Area Signal G8 Acid 34.20 10 Surrogai 34.97 7.337 8.174 19364 22836 MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 i PC00414 *** End of Report *** Fri, 19. Dec. 2003 Q46 02:32:39 pm Page 1 of 1 COO313 Sample Name:STD 100 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11667644\A502400\FC000029.D Injection Date Acq Operator Instrument Dilution 12/18/03 jmiller PC00414 1 11:50:47 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : 29 2 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1667644\A502400\FC000029.D) API-ES, Neg, SIM, Frag: Var 7.336- C8 Acid. 3500- 3000- 2500- 2000- 1500H 1000- 500- 0- "--- 1--- r 4 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1667644\A502400\FC000029.D) API-ES, Neg, SIM, Frag: Var 8.178- C10 Surrogate min 4000- 3000- 2000 1000 Compound Amount (ng/mL) R.T. C8 Acid 84.49 10 Surrogat 88.11 7.336 8.178 Area 36993 45665 Signal MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 u (J4 1 02:33:03 pm Page 1 of 1 C00314 Sample Name:STD 250 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11667681\A504576\FC000030.D Injection Date Acq Operator Instrument Dilution 12/19/03 jmiller PC00414 1 12 :05 :55 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 30 3 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\1218 03 .M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. ` MSD1 369, EIC=368.7:369.7 (CHEMSTORM1667681\A504576\FC000030.D) API-ES, Neg, SIM, Frag: Var 10000- 7.354 - C8 Ad- 8000- 6000- 4000- 2000- _ ------------------------------------------------- ------------------------------------------------------------ ------- --- 1------------ . r i . --i r j i r | ' 246 1 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1667681 \A504576\FC000030.D) API-ES, Neg, SIM, Frag: Var r min 120001- 8.197- C10 Surrogate 10000 8000 6000- 4000- 2000-- ,------- ,------- . l i------- ,------- i------- 1------- 1------- 1------- i------- 1------- 1------- 1------- 1------- -------- 1------- 1------- 1------- 1------- r Compound Amount (ng/mL) R.T. C.8 Acid 259.73 L0 Surrogat 257.49 7.354 8.197 Area 98428 118436 Signal MSD1 369, EIC=3 68.7 :369.7 MSD1 469, EIC=468.7:469.7 3C00414 *** End of Report *** Fri, 19. Dec. 2003 48 02:33:31 pm Page 1 of 1 G00315 Sample Name :STD 500 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11667753\A506688\FC000031.D Injection Date Acq Operator Instrument Dilution 12/19/03 jmiller PC00414 1 12:21:11 AM Seq Line Vial No. Inj. N o . Inj. Voi. : : : : 31 4 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. 'MSD1 369, EIC=368.7:369.7 (CHEMSTORM1667753\A506688\FC000031 .D) API-ES, Neg, SIM, Frag: Var 20000 - 7.347 - C8 Acid, 17500 15000 12500 10000 7500 5000 2500 0-t A. *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1667753\A506688\FC000031.D) API-ES, Neg, SIM, Frag: Var 8.188- C10 Surrogate, min 20000 - 15000- 10000- 5000- 1 --,--- --- J--- 1------------1-- 1 ' 1 -, --- ,--- ,--- 1--- r 2 4 6 8 min Compound Amount (ng/mL) R.T. Area Signal C Acid 528.35 L0 Surrogat 527.34 7.347 8.188 192604 234376 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 >000414 *** End of Report *** Fri, 19. Dec. 2003 02:33:56 pm 0 0 49 Page 1 of 1 000316 Sample Name:STD 750 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11667808\A508928\FC000032.D Injection Date Acq Operator Instrument Dilution 12/19/03 jmiller PC00414 1 12:36:22 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 32 5 1 5 pi Acq. Method Analysis Method ,,,, Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1667808\A508928\FC000032.D) API-ES, Neg, SIM, Frag: Var 7.326- C8 Acid 25000 - 20000 - 15000- 10000- 5000- 0-- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1667808\A508928\FC000032.D) API-ES, Neg, SIM, Frag: Var 35000 - 8.171 - C10 Surrogate 30000 H 25000 - 20000 15000- 10000- 5000 H 0eL 4 Compound Amount (ng/mL) R.T. C8 Acid 760.03 10 Surrogat 760.01 7.326 8.171 Area 273825 334338 b o min Signal MSDl 369, EIC=3 68.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 19. Dec. 2003 5 C 02:34:26 pm Page 1 of 1 000317 Sample Name:STD 1000 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11667894\A511104\FC000033.D Injection Date Acq Operator Instrument Dilution : 12/19/03 : jmiller : PC00414 :1 12:51:29 AM Seq Line Vial N o . Inj . NO. Inj . Voi. : : : 33 6 1 5 y.1 Acq. Method : FC8-10.M Analysis Method : C:\HPCHEM\1\METHODS\121803.M Last Changed : 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1667894\A511104\FC000033.D) API-ES, Neg, SIM, Frag: Var 35000 - 7.335 - C8 Acic 30000 - 25000j 20000 - 15000- -- 10000- 5000 j ''r r^ 1r 1 ' I 1' 1r 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1667894\A511104\FC000033.D) API-ES, Neg, SIM, Frag: Var 1 40000 - 35000 - j 8.170- C10 Surrogate 30000 / 25000 - j 20000 / 15000 / 10000 -- 5000/ ,,.r 2 ^ 4 1 I ' 6 J, ' I ' 8 1r min Compound Amount (ng/mL) R.T. Area Signal CS Acid 976.71 L0 Surrogat 972.50 7.335 8.170 349789 425633 MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 >000414 *** End of Report *** Fri, 19. Dec. 2003 02:34:55 pm Ub i Page 1 of 1 000318 Sample Name:STD 1500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11667949\A513280\FC000034.D Injection Date | Acq Operator Instrument Dilution 12/19/03 jmiller PC00414 1 1:06:39 AM Seq Line Vial No. Inj. No. Inj . Voi. : : : 34 7 1 5 pi i Acq. Method Analysis Method r-- Last Changed FC8-10.M C:\HPCHEM\1\METHODS\121803.M 12/19/03 01:56:57 pm LC/MS analysis of perfluoro carboxylic acids. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1667949\A513280\FC000034.D) APl-ES, Neg, SIM, Frag: Var 60000 - 7.341 - C8 Acid, 50000 - 40000 - 30000 ^ 20000 ^ 10000- 0- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1667949\A513280\FC000034.D) APl-ES, Neg, SIM, Frag: Var 80000 8.192- C10 Surrogate! 70000 60000 50000 -I 40000 30000 -I 20000 10000 0 Compound Amount (ng/mL) R.T. 8 Acid 1475.40 10 Surrogat 1466.39 7.341 8.192 - Area 524621 637826 Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 *** End of Report *** PC00414 Fri, 19. Dec. 2003 01:57:52 pm u 52 Page 1 of 1 000319 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Loain Login #: 1554 Project: P0000419 Project Storage: Company Name: DuPont de Nemours & Co, Inc. Submitted By: Michael D. Aucoin -L o g in Type: Immediate Receipt of Samples Started: T Date Start: 12/12/2003 Due Date: 12/26/2003 Received Date: 12/12/2003 Received By: AMMERMAN, MARK Spread Sample: -L a b e l: 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 >ackaqe . X0002035 Carton Packages / Containers Mail Data/ Condition Shipper/ ID 12/12/2003 10:46:19PM Package & Contents Uncompromised FEDEX 8363913019600200 Temp. Control/Temp. None 23.3 Direction / Handled Bv RECEIVED AMMERMAN, MARK ontainer # C0021109 0021110 *""00021111 00021112 C0021113 .X0021114 00021115 00021116 C0021117 '"-'00021118 00021119 C0021120 0021121 " *00021122 00021123 C0021124 --C0021125 00021126 00021127 C0021128 - "00021129 00021130 C0021131 0021132 Gross Weight 72 g 7.2 g 7.2 g 7.0 g 7.0 g 7.0 g 72 g 7.2 g 72 g 7.1 g 7.1 g 7.1 g 7.2 g 7.2 g 72 g 7.2 g 72 g 7.2 g 7.0 g 7.0 g 7.0 g 7.0 g 7.0 g 7.0 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 Mfa. Lot Mfa. ID Miscellaneous , Item Key None Description ICOC i/23/2003 jgin.rpt Report Version: uu^ Page 1 of 4 Instance: G0Q320 Sample ID L0001444-0001 L0001444-0002 *" 10001444-0003 L0001444-0004 L0001444-0005 L0001444-0006 L0001444-0007 L0001444-0008 L0001444-0009 "1.0001444-0010 L0001444-0011 L0001444-0012 L0001444-0013 " '10001444-0014 L0001444-0015 L0001444-0016 ,,10001444-0017 _ L0001444-0018 <-0001444-0019 L0001444-0020 * 10001444-0021 .0001444-0022 L0001444-0023 L0001444-0024 Matrix GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS Fraction OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes Samples Sample WWK-A-AMSFBLK-E7 A WWK-A-AMSFBLK-E7 B WWK-A-AMSFBLK-E7 C VWVK-A-AMS1-E7 A VWVK-A-AMS1-E7 B WWK-A-AMS1-E7 C WWK-A-AMS2-E7 A WWK-A-AMS2-E7 B WWK-A-AMS2-E7 C WWK-A-AMS3-E7 A WWK-A-AMS3-E7 B WWK-A-AMS3-E7 C WWK-A-AMS4-E7 A WWK-A-AMS4-E7 B WWK-A-AMS4-E7 C WWK-A-AMS5-E7 A WWK-A-AMS5-E7 B WWK-A-AMS5-E7 C WWK-A-AMS6-E7 A WWK-A-AMS6-E7 B WWK-A-AMS6-E7 C Control 1 A Control 1 B Control 1 C Date SamDled Date Received 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/12/2003 12/12/2003 12/12/2003 12/12/2003 12/12/2003 12/12/2003 Date Due 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 12/26/2003 j i/23/2003 I- )gin.rpt Report Version: U0 5 4 Page 2 of 4 Instance: 0001444-0001 Container ^ C0021109/Other/NONE .-0001444-0002 -- Container C0021110/Other/NONE JL0001444-0003 Container C0021111 / Other/NONE 0001444-0004 Container -- C0021112/ Other / NONE L0001444-0005 Container C0021113/Other/NONE M)001444-0006 Container C0021114/Other / NONE 0001444-0007 Container ' * C0021115/Other/NONE L0001444-0008 Container C0021116/Other/NONE " 0001444-0009 Container C00211 1 7 /O th e r/N O N E -.3001444-0010 Container C00211 1 8 /O th e r/N O N E L0001444-0011 Container C00211 1 9 /O th e r/N O N E 3001444-0012 Container _ C0021120/ Other / NONE ...2/23/2003 ogin.rpt Login Bottles Method Method Method Method Method Method Method Method Method Method Method Method Report Version: Page 3 of 4 Ci (J *S* Instance: 0 0 0 3 *^ 2 0001444-0013 Container C0021121 / Other/NONE 1,0001444-0014 Container C00211 2 2 /O th e r/N O N E 0001444-0015 Container C0021123/Other/NONE L0001444-0016 Container C00211 2 4 /O th e r/N O N E 'D 0 0 1444-0017 Container C00211 2 5 /O th e r/N O N E 0001444-0018 Container C00211 2 6 /O th e r/N O N E L0001444-0019 Container C00211 2 7 /O th e r/N O N E D 0 0 1 444-0020 Container C00211 2 8 /O th e r/N O N E -0001444-0021 Container C0021129 /Other /NONE L0001444-0022 Container C00211 3 0 /O th e r/N O N E 0001444-0023 Container C0021131 / Other/NONE .0001444-0024 Container C00211 3 2 /O th e r/N O N E 2/23/2003 -ogin.rpt Login Method Method Method Method Method Method Method Method Method Method Method Method Report Version: Page 4 of 4 UU 5 6 Instance: Q Q Q 333 GOO RESEARCH PROJECT INFO RM A TIO N Client (nam e & address): 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 ]I Page [ o f ___ ANALYSES REQUESTED Project M a n a g er (Name^ E-mail Address): __________ i a V <w i 4- \ A )Tia V \ ~ (K&fcA (V P h o n e :___ L 3 Q 5 Q $ O Q _ \ ( C fe ______ P3.X" Sampler: 5 - D p p / A -------------- Project Nam e: rW Quotation # : P\ Please fill out this form com pletely to ensure correct analysis and proper handling of your samples. CO u/ Composite Number of Containers SAMPLE ANALYSIS -Q ExyLIMS# Client Sample Identification Collection Collection Date Time a ^aluk \f\\L- iV" PriwS \ - B Q - l/ll/l &ft(p l/it/lfi 7s idJ/i/SS fJit/p (M b 1 . aaV - t I V - PtOfA 5 ~ 6 ^ &n/&3 m c o l -fr -iv v .fc r e i Mita 0 7 /r / A Specify Matrix Comments _ l fVcT \ fVcc V re X ^ ' w ^ c ^ \ $cc KCC Comtl Pr^C \ (W \ LAB USE ONLY CHAIN OF CUSTODY Relinquished by Date Time 0 9 /S ' OTHER INFO RM ATIO N Cooler ID # /laccai^ Cooler Temp. (C) / I / / Received by Datei ' IJ / ,r h1biS/hl tv`v J/r/ i f ------------ -- -- ------------------- = -- =a" -- H-//.7 Time /cVC LAB USE ONLY a A "A A A PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: EH Sample results only ED Add case narrative EH Add quality control summary I l Add calibration summary EH Add raw data EH Other_____ i! ncv 3-qr J cn03?5 U058 USA A ir b ill FedEx fi3L3*l30:i,%0Express Tracking Number Recipient's Copy 1 From Date ( l l i 4a Express Package Service V/ P ackages up to m lb s Delivery commitment m8y be later in some areas. FedEx Priority Overnight ' -- - Next business morning l- ] FedEx Standard Overnight 1-- 1 Next business afternoon I I FedEx First Overnight 1-- Earliest next business morning deliveryto select locations Sender's Name Comcanv Address V V v A V Op...0 o .-V i l V' \1 *QKV, Phone . .5 ^ 55 ! !A . A !, \City ,J 2 Your Internal Billing Reference 3 To Recipients Name r~"\ n S ta te \/^ 'V ^ HP:! ^ Vi OZAJ'M Phone \j x v.\ J Address To "HOLD" et FedEx location, print FedEx address. \n FedEx 2Day Q FedEx Express Saver Second business day Third businessday FedEx Envelope rate not available. Minimum charge: One-pound rate ---------- 4b Express Freight Service P ackages w a r 150 lbs. Delivery commitment may be later in some areas. nvpQ\\t DeptTFIoor/Surte/Roorri ZIP QtUAl ^ >t oot:3 \' l r: C [ I FedExfeay Freight* 1-- I Next bdlfeess day Callfort^pfirm ation;___________ l FedEx2Day Freight ' Second business day I ! FedEx3Dav Freight I-- ' Third busines day - r i \ 5. Packaging * Declared value limitSSOO I I FedEx Envelope* FedEx Pak* Includes FedExSmall Psk,FedEx Large Pak, and FedEx Sturdy Pak ^ O th e r 6 Special Handling include FedExaddress in Section 3. p -, SATURDAYDeliveiy i___I NrateWeonNforFedfctPTtOfify Overnight and FedEx 2Day tosetectZIPcodes r--, HOLDWeekday I__I at FedExLocation Not available for FedEx First Overnight Does this shipment contain dangerous goods? ----- One box must be checked. ------------- i-- i HOLDSaturday i I at FedEx Location Available onlyfor FedEx Priority Overnight and FedEx2Dayto select locations No I ] Yes [-- i Yes I___I As per attached 1___ 1 f" I I Dry Ice I-- i Dryice, 9, Ut \\ v)f. We cannot deliver P.O. boxes or PO. ZIP codes. , - Dangerous Goods (including Dry Ice) cannot be shipped In FedEx packaging. I I Cargo Aircraft Only 1 Payment B ill to: s^.' / |--------:------- Enter FedExAcct No. or Credit Card No. below .------------- 1 Sender ^ I 1Recipient | [Third Party P i Credit Card AcctNo. | | Cash/Check Address Dept/Roor/Surt&Woom :,4 City Xy-' l\ ,3 113 State \ f t ^ ilbD \ U K r -V TotalPackages TotalWeight Teda! Declared Vahle* /$ .00 *Our liability is limited to $100 unless you declare a higher value. See back fo r details. Total Charges 8 Release Signature Signto authorize deitoerywithoutobtainingsignature. L Bysigninq you authorize us to deliver this sflpm ent w ithout obtaining a sign atu re...., and agree to indemnify and hold us harmlest.from any resulting claims. Questions? V isit our Web s iie a t fedex.com or call I.SOO.Go.FedEx 800.463.3339. ... Rev. Date 10/01 *Part#1576121994-?001 FedExPRINTED IN U SA. WCSL02 . . . 1 Samplers): SO, AC DuPont Washington Works Air Sampling Program FedEx Airbill #: 836391301960 Event Number P u tlf^ lll m m m # 669842 AMS-1 669908 AMS-2 669878 AMS-3 669809 AMS-4 669769 AMS-5 669848 AMS-6 Hours Minutes 00 1 60 2 120 3 180 4 240 WWK-A-AMS1-E7 WWK-A-AMS2-E7 WWK-A-AMS3-E7 WWK-A-AMS4-E7 WWK-A-AMS5-E7 WWK-A-AMS6-E7 Hours 5 6 7 8 9 1.006 1.005 1.003 1.011 1.007 1.015 Minutes 300 360 420 480 540 mmm 10-Dec 10-Dec 10-Dec 10-Dec 10-Dec 10-Dec Hours 10 11 12 13 14 0630 0635 0636 0643 0650 0701 Minutes 600 660 720 780 840 & A h 11-Dec 0616 11 -Dec 0625 11-Dec 0628 11 -Dec 0646 11-Dec 0700 11 -Dec 0715 Hours Minutes 15 900 16 960 17 1020 18 1080 19 1140 Field Blank: yes WWK-K-AMSFBLK-E7 yes or no Weather: 12/10 = Cloudy, mid 40's, rain expected. 12/11= Overcast 37 degrees, possible snow flurries. 0.8967 1.08 pump stopped 1.279 1.104 1.102 Hours 20 21 22 23 24 Event 7 1428 1434 987 1444 1448 1451 Minutes 1200 1260 1320 1380 1440 Total Volume 1356 liters 1490 liters 990* titers 1652 liters 1530 liters 1539 liters <0 Ci n o e o lO Z> D SAFER operational: yes yes or no Comments: Total minutes column is the reading from the monitor counter. 12/22/2003 Page 1 of 2 airdataevent7