Document vVv43qQZZ8q2kRoBDjGV0NydZ

RESEARCH Precise Research. Proven Results. HEC EiVK 0 n p p y I'p ;'" ZOOItKAY29 AH 8=59 Attachment 2 ~ /7 7 r > Analytical Report Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 4 Exygen Research Report No. L0001359 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 X 3058 Research Drive Staate College, PA 16801, USA 000144. A T1:F:880104.2.28712.3.1201199 exygen.com Summary Seven solid media samples were received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. The media represent samples of air collected on OVS tubes. Please see Table 1 for a completed listing of samples received and field air volumes collected. The samples were analyzed for Perfluorooctanoic Acid (C8 Acid) using liquid chromatography / mass spectrometry (LCMS). The method employed is entitled "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in OVS Airtubes by LCMS" (James Miller, Exygen Research, February 17, 2003). The OVS tubes were separated into three fractions for specific fluorochemical analysis. Fraction A consisted of the filter, backing material and plastic ring. Fraction B contained the first bed of XAD resin and the PUF backing. Fraction C contained the second bed of XAD resin and PUF backing. 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. Sample WWK-A-AMS6-E4 was not analyzed as per client request. Instrument operating conditions can be found at the beginning of each analytical run. Raw instrument data is given in Appendix A. Chain-of-custody information can be found in Appendix B. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 2 of 7 000145 Results Summary Request # WWK-A-AMS1-E4 A WWK-A-AMS1-E4 B WWK-A-AMS1-E4 C WWK-A-AMS1-E4 (Total) Air Volume Sampled (L) 1432 1432 1432 C8 Acid (mg/m3) < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS2-E4 A WWK-A-AMS2-E4 B WWK-A-AMS2-E4 C WWK-A-AMS2-E4 (Total) 1458 1458 1458 0.0002 < 0.00007 NA 0.0002 WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-EMS3-E4 C WWK-A-EMS3-E4 (Total) 1468 1468 1468 0.0002 < 0.00007 NA 0.0002 WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS4-E4 C WWK-A-AMS4-E4 (Total) 1421 1421 1421 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS5-E4 A WWK-A-AMS5-E4 B WWK-A-AMS5-E4 C WWK-A-AMS5-E24(Total) 1435 1435 1435 < 0.00007 < 0.00007 NA <0.00014 NA - Not Analyzed. Fraction B was below the quantitation limit, therefore the backup fraction does not require analysis. 1. "<" is defined as not detected at or above the reported level. 2. Sample results have not been corrected for blank results or control spike recoveries. 3. Please note the following descriptions of the OVS sample tube fractions: Fraction Fraction Description A Frit Extract B 1st set beads extract C 2nd set beads extract (not analyzed) ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 3 of 7 000146 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) 499 C8 Acid (percent recovery 100 Blanks Request # WWK-A-AMSFBLK-E4 A WWK-A-AMSFBLK-E4 B Voi. Of Air (L) 0 0 C8 Acid (uq/fraction) <0.10 <0.10 000147 ATT 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-E4 A WWK-A-AMSFBLK-E4 B WWK-A-AMS1-E4 A WWK-A-AMS1-E4 B WWK-A-AMS2-E4 A WWK-A-AMS2-E4 B WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS5-E4 A WWK-A-AMS5-E4 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) 931 443 946 465 802 498 797 474 794 471 804 424 889 412 Percent Recovery (%) 186* 89 189* 93 161* 100 159* 95 159* 94 161* 85 178* 82 * Surrogate recovery outside of advisory range. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 000148 Calculations Request # WWK-A-AMSFBLK-E4 A WWK-A-AMSFBLK-E4 B WWK-A-AMS1-E4 A WWK-A-AMS1-E4 B WWK-A-AMS2-E4 A WWK-A-AMS2-E4 B WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS5-E4 A WWK-A-AMS5-E4 B Control Spike A Control Spike B Vol. Of Air (L) 0 0 1432 1432 1458 1458 1468 1468 1421 1421 1435 1435 0 0 C8 Acid (raw-ppb) <10 < 10 <10 <10 311 <10 314 <10 <10 < 10 < 10 <10 499 < 10 C8 Acid (ug/fraction) <0.10 <0.10 <0.10 <0.10 0.31 <0.10 0.31 <0.10 <0.10 <0.10 <0.10 <0.10 0.50 <0.10 C8 Acid (mg/m3) < 0.00007 < 0.00007 0.0002 < 0.00007 0.0002 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 000149 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 7 Example Calculation For sample WWK-A-AMS2-E4 A C8 Acid, = [311 ng/ml of C8 Acid x (1 ml) x (1 u g / 1000 ng) x (1 m g/ 1000 ug) ] / [(1458 L) x (1 m3 / 1000 L)] = 0.0002 mg / m3 Signatures C AL Paul Connolly, LCMSTeam Leader l ft)fhd&jC hn M. Flaherty, Vice'f'resident 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 000150 TSTOOO pnnp Table 1. Login Information / Field Data Sample ID Exygen Lab ID Date Received Description W WK-A-AMSFBLK-E4 A WWK-A-AMSFBLK-E4 B WWK-A-AMSFBLK-E4 C WWK-A-AMS1-E4 A WWK-A-AMS1-E4B W W K -A -A M S 1-E 4C WWK-A-AMS2-E4 A WWK-A-AMS2-E4B WW K-A-AMS2-E4 C WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMS3-E4 C WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS4-E4 C WWK-A-AMS5-E4 A WWK-A AMS5-E4 B WWK-A-AMS5-E4 C Control Spike A Control Spike B Control Spike C L0001359-1 L0001359-2 L0001359-3 L0001359-4 L0001359-5 L0001359-6 L0001359-7 L0001359-8 L0001359-9 L0001359-10 L0001359-11 L0001359-12 L0001359-13 L0001359-14 L0001359-15 L0001359-16 L0001359-17 L0001359-18 L0001359-19 L0001359-20 L0001359-21 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 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 1432 1432 1432 1458 1458 1458 1468 1468 1468 1421 1421 1421 1435 1435 1435 0 0 0 f non Table 2. Chain of Custody Sample ID WWK-A-AMSFBLK-E4 A WWK-A-AMSFBLK-E4 B WWK-A-AMSFBLK-E4 C WWK-A-AMS1-E4 A WWK-A-AMS1-E4 B WWK-A-AMS1-E4 C WWK-A-AMS2-E4 A WWK-A-AMS2-E4B WWK-A-AMS2-E4 C WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMS3-E4 C WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS4-E4 C WWK-A-AMS5-E4 A WWK-A AMS5-E4 B WWK-A-AMS5-E4 C Control Spike A Control Spike B Control Spike C Date Collected 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 NA NA NA Date Received at Exygen 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 NA NA NA Date Extracted by Exygen 12/3/03 12/3/03 NA 12/3/03 12/3/03 NA 12/3/03 12/3/03 NA 12/3/03 12/3/03 NA 12/3/03 12/3/03 NA 12/3/03 12/3/03 NA 12/3/03 12/3/03 NA Date Analyzed by Exygen 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA 12/9 - 12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA ANALYTICAL DATA REVIEW SHEET LC/MS Analyst nature/Date C 0*1 J iU /-------------- L--------- f------- Reviewed by / / / % ^ / //f/rq--------------- f.--------------- xSignature/Date U , J 000153 Sequence : C :\HPCHEM\1\SEQUENCE\120 903.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 ppib STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb . STD 1000 ppb STD 1500 ppb Solvent'blank L0001359-19 L0001359-20 L0001359-1 L0001359-2 L0001359-4 L0001359-5 L0001359-7 L0001359-8 L0001359-10 L0001359-11 STD 500 ppb Solvent blank L0001359-13 L0001359-14 L0001359-16 L0001359-17 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 Sampl-eName Method CalLev Update RF Update RT Interval N )N )N )N )N )N )N )N )N )W N )N )N )N ) 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 1,500. ppb STD 50 ppb STD 100 ppb : STD 250 ppb STD 500 ppb STD 75.9. 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 2 Replace Average -2 3 Replace Average -2 4 Replace Average -2 5 Replace Average -2 6 Replace Average -2 7 Replace Average -2 1 Average Average -2 2 Average Average -2 3 Average Average -2 4 Average Average -2 5 Average Average -2 6 Average Average -2 7 Average Average -2 LCMS3 12/9/03 5:05:51 PM jmiller /2 03 U 01 1 0001S4 Page 1 of 1 Method C:\HPCHEM\1\METHODS\120903.M Calibration Table Calib. Data Modified Friday, January 09, 2004 2:13:25 PM Calculate Based on External Standard Peak Area Rel. Reference Window Abs. Reference Window Rel. Non-ref. Window Abs. Non-ref. Window Uncalibrated Peaks Partial Calibration Correct All Ret. Times 5.000 % 0.000 min 5.000 % 0.000 min not reported Yes, identified peaks are recalibrated No, only for identified peaks Curve Type Origin Weight Linear Ignored Equal Recalibration Settings Average Response Average Retention Time Average all calibrations Floating Average New 75% Calibration Report Options : Printout of recalibrations within a sequence: Calibration Table after Recalibration Normal Report after Recalibration If the sequence is done with bracketing: Results of first cycle (ending previous bracket) Signal 1: MSD1 369, EIC=368.7 :369.7 Signal 2: MSD1 469, EIC=468.7 :469.7 RetTime Lvl Amount Area [min] Sig [ppb] 11 1 7.463 1 1 50.00000 1.01066e4 2 100.00000 1.99451e4 3 250.00000 4.82344e4 4 500.00000 9.09422e4 5 750.00000 1.28865e5 6 1000.00000 1.58452e5 7 1500.00000 2.25877e5 8.336 2 1 50.00000 1.403 03e4 2 100.00000 2.74848e4 3 250.00000 6.62707e4 4 500.00000 1.26319e5 5 750.00000 1.79474e5 6 1000.00000 2.20810e5 7 1500.00000 3.12650e5 Amt/Area Ref Grp Name ^4.94728e-3 5.01377e-3 5.183 02e-3 5.497 99e-3 5.82003e-3 6.31106e-3 6.64079e-3 3.56372e-3 3.63837e-3 3.77241e-3 3.95823e-3 4.17888e-3 4.52879e-3 4 .79770e-3 1 1 C8 Acid CIO Surrogate More compound-specific settings: Compound: C8 Acid Time Window : From 7.291 min To 8.292 min Compound: CIO Surrogate Time Window : From 8.140 min To 8.945 min Peak Sum Table ***No Entries in table*** t C00414 1/9/04 2:21:08 PM jmiller U01 2 000155 Page 1 of 2 JJethod C :\HPCHEMV1\METHODS\12 0903 .M Calibration Curves C8 Acid at exp. RT: 7.463 MSDl 369, EIC=368.7:369.7 Correlation: 0.99698 Residual Std. Dev.: 6705.26193 Formula: y = mx + b m: 148.68546 b: 9339.65270 x: Amount[ppb] y : Area CIO Surrogate at exp. RT: 8.336 MSDl 469, EIC=468.7:469.7 Correlation: 0.99675 Residual Std. Dev.: 9660.28035 Formula: y = mx + b m: 206.36797 b: 12944.44413 x: Amount[ppb] y: Area | C00414 1/9/04 2:21:08 PM jmiller 0 0 1 3 000156 Page 2 of 2 LC/MS SYSTEM AND OPERATING CONDITIONS Client: Dupont EXYGEN STUDY: L0001359 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 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 (J 0 1 4 000157 Ions monitored: Analyte C8 Acid (PFOA) C10 Surrogate Ion (m/z) 369 469 Extraction Date: December 3, 2003 Analyst: James R. Miller Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039, FAX: (814) 231-1580 Page 2 of 2 0015 000158 Instrument : LCMS3 Tue Dec 02 09:17:46 2003 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: 2233.95 Abundance: 1314304 F Raw,Gauss 0.3 100 -, 60 40 20 - -- 1-- 1-- r--1-- ,-- 1 i-- 1-- r-- r 1 ` ' --1-- 1---1-- 1-- -- -1 | 500 1000 1500 2000 2500 m/z gf Abund 113.00 61000 601.99 21664 1033.97 210944 1633.95 695552 2233.95 1314304 Rei Abund 100.00 35.51 345.81 1140.25 2154.60 Iso m/z 114.02 602.99 1034.95 1634.95 2234.95 Iso Abund Iso Ratio 1982 3.25 4281 19.76 44120 20.92 256896 36.93 652160 4 9.62 01 000159 Instrument : LCMS3 Tue Dec 02 09:17:46 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 -128 6.0 WidthOffs VAR -4.0 MassGain- 36.25 19 MassOffs VAR 240 Energy 5.0 OpolPeak 300 OpolKnee 316 3.0 QuadDC 0.00 EMV VCap Status: CapCur ChamCur 2164 Samples 8 4000 Averages 1 StepSize 0.10 63 DryingGas 6.0 1.02 Gas Temp 300 Quad Temp 99 Neb Pres 20 Fragmentor Dynamic Parameter Ramp I I Mass 100.00 Setting 60.00 Mass 3000.00 Setting 250.00 Mass Setting U017 000160 Instrument : LCMS3 Tue Dec 02 09:17:46 2003 G1946: API_ES Negative mode Page 3 of 3 C:\HPCHEM\1\1946TUNE\ATUNES.TUN Mass Offset 2.00! 1.00 0.00 - - 1. 00- Dynamic Parameter Ramp " 2 .0 0 i l----------- 1----------- 1----------- 1----------- 1----------- t----------- i----------- 1----------- 1----------- 1----------- i----------- 1-----------1----------- 1----------- 1----------- 1--------" t----------- 1----------- j----------- 1----------- 1----------- 1----------- 1----------- 1----------- !-----------r 500 1000 1500 2000 2500 Mass 112.99 1633.95 Setting 0.56 0.63 Mass 601.98 2233.91 Setting 0.67 0.56 Mass 1033.99 Setting 0.64 3000 uQ ! a 000161 Run#_ F<~>oo001 __To_ FC-oO Q Q Si / 'A /a -j Date Initials Sample Name:STD 50 ppb Sample Info:Warm up 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11532797\A732352\FC000001.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 5:09:47 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 1 1 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. MSD1 369, EIC=368.7:369.7 (CHEMSTORM1532797\A732352\FC000001 .D) API-ES, Neg, SIM, Frag: Var 1800 7.474- C8 Acid 1600- 1400 1200 -3 1000 J 800 600 H 400 200 -T--- 1--- 1 r 4 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1532797\A732352\FC000001.D) API-ES, Neg, SIM, Frag: Var 2250- 8.350- C10 Surrogate 2000 -i 1750- 1500 d 1250- 1000- 750 "i 500 / 250- Compound Amount (ng/mL) R.T. 8 Acid 16.35 10 Surrogat 14.74 7.474 8.350 Area 11770 15986 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:19:20 pm UO'i 9 Page 1 of 1 000162 Sample Name:STD 50 ppb Sample Info : Data file :C :\HPCHEM\1\DATA\FC000002.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 5:25:19 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\120903 .M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. MSD1 369, EIC=368.7:369.7 (FC000002.D) API-ES, Neg, SIM, Frag: Var 1600 7.452- C8 Acic 1400 1200- 1000- 800 600 400 200 *MSD1 469, EIC=468.7:469.7 (FC000002.D) API-ES, Neg, SIM, Frag: Var 2250 8.331 - CIO Surrogate 2000 -j 1750 1500 1250 1000 750 500 2 5 0 -j 1 2 1 1 5 pi min Compound Amount (ng/mL) R.T. ' 18 Acid 10.44 .'10 Surrogat 10.39 7.452 8.331 Area 10892 15089 Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:12:23 pm U020 Page 1 of 1 000163 Sample Name:STD 100 ppb Sample Info : Data file :C :\HPCHEM\1\DATA\FC000003.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 5:40:50 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\12 0903 .M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000003.D) API-ES, Neg, SIM, Frag: Var 3000- 17.451 - C8 Ac! 2500 1 3 2 1 5 pi 2000 1500 1000- 500- i_L *MSD1 469, EIC=468.7:469.7 (FC000003.D) 4000- API-ES, Neg, SIM, Frag: Var 8 8.333- C10 Surrogate 3500- 3000 -j 2500- 2000- 1500 J 1000- 5000-- iLL min Compound Amount (ng/mL) R.T. 18 Acid 80.24 H O Surrogat 77.29 7.451 8.333 Area 21270 28894 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 i PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:13:08 pm U0 2 I Page 1 of 1 000164 Sample Name:STD 250 ppb Sample Info : Data file :C:\HPCHEM\1\DATA\FC000004 .D Injection Date Acq Operator Instrument Dilution 12/9/03 jmi H e r PC00414 1 5:56:25 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\120903 .M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000004.D) API-ES, Neg, SIM, Frag: Var 7000- 7.479 - C8 Acid 1 4 3 1 5 pi 6000 -j 5000 s 4000 s - - 3000 -j 2000 - 1000- 0' , . I ' 1^1 1' 11' 2 46 *MSD1 469, EIC=468.7:469.7 (FC000004.D) API-ES, Neg, SIM, Frag: Var L 1 1 I --, 8 10000- 8.350- C10 Surrogate I------- 1------- F min 8000- 6000-- 4000- 2000- - 0-, Compound Amount (ng/mL) R.T. *"`8 Acid 280.04 10 Surrogat 274.70 7.479 8.350 -C D "'t -C M Area 50977 69633 A ______ __ I ^ ------- 1 8 -r min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:13:53 pm 022 Page 1 of 1 000165 Sample Name:STD 500 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\FC000005.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 6:11:59 PM Seq Line Vial No. Inj . N o . Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METH0DS\12 09 03 .M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000005.D) API-ES, Neg, SIM, Frag: Var 7.487- C8 Acid 12000- 10000- 8000- 6000- 4000- 2000- 0- *MSD1 469, EIC=468.7:469.7 (FC000005.D) API-ES, Neg, SIM, Frag: Var 8 17500- 8.350- C10 Surrogati 15000- 12500- 10000- 7500 5000 2500 J 0- 1 5 4 1 5 pi Compound Amount (ng/mL) R.T. !8 Acid 583.46 '10 Surrogat 576.55 7.487 8.350 Area 96091 131926 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 j PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:14:31 pm 02 3 Page 1 of 1 000166 Sample Name:STD 750 ppb Sample Info : Data file :C:\HPCHEM\1\DATA\FC000006 .D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 6:27:34 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed F C 8 - 1 0 .M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000006.D) API-ES, Neg, SIM, Frag: Var 17500- 7.452- C8 Acid 15000- 12500- 10000J 750050002500- 0- _iLi . *MSD1 469, EIC=468.7:469.7 (FC000006.D) API-ES, Neg, SIM, Frag: Var 25000 - 8.325- C10 Surrogate 1 6 5 1 5 pi 20000 - 15000- 10000- 5000- 1---1 1 124 Compound Amount (ng/mL) R.T. Area "':8 Acid 849.14 .'10 Surrogat 846.39 7.452 8.325 135594 187613 1 --- 1--- 1--- '--- '--- r 6 8 min Signal MSDl 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 i PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:15:02 pm Q024 Page 1 of 1 000167 Sample Name:STD 1000 ppb | Sample Info : I Data file :C:\HPCHEM\1\DATA\FC000007.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 6:43:09 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000007.D) API-ES, Neg, SIM, Frag: Var 22500 / 7.445- C8 Acic 20000 - 17500/ 15000/ 12500/ 10000/ 7500/ 5000/ 2500/ A. . . . o- , ,,I 1 1 I 1 ' '1 1 1 i^ -- 2468 *MSD1 469, EIC=468.7:469.7 (FC000007.D) API-ES, Neg, SIM, Frag: Var -- 30000- 8.322 - C10 Surrogate 25000 ^ 1 7 6 1 5 pi . >r min 20000 ^ 15000 -j 10000^ - 5000 -J : 0 1' 11 2 r^ 11 4 Compound Amount (ng/mL) R.T. .8 Acid 1042.89 10 Surrogat 1037.25 7.445 8.322 ''' Area 164402 226999 Ji . | ' ' 11 'i . c 6 8 mi n Signal MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:15:25 pm u025 Page 1 of 1 000168 Sample Name:STD 1500 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\FC000008 .D Injection Date ! Acq Operator Instrument [*" Dilution 12/9/03 jmiller PC00414 1 6:58:44 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : ' Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\120903 .M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000008.D) API-ES, Neg, SIM, Frag: Var 30000 ^ 7.470- C8 Acid 1 8 7 1 5 pi 25000 ^ 20000 ^ 15000 ^ 10000- 5000 ^ ____ ____ 0 -j 1 1 1 1 ' 1 1 n ^ - r - r -f r 2 46 *MSD1 469, EIC=468.7:469.7 (FC000008.D) API-ES, Neg, SIM, Frag: Var _J r A ___________________________ ri f 1' i 8 min 1 45000 J 8.336 - C10 Surrogate i... 40000 -j ! 35000 - , , , 30000 ^ 25000 J 20000 15000 10000J 5000 r 0 ' 1 I ^^ 2 ^^^^ 4 r^ ^ 6 T f A r_____'_.______r_____( 8 min Compound Amount (ng/mL) R.T. Area Signal ' ''8 Acid 1541.14 :10 Surrogat 1525.55 7 470 8 336 238485 327769 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:16:00 pm 026 Page 1 of 1 ^0169 Sample Name:Solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11534243\A735360\FC000009.D 1 i `8 Acid 0.00 J10 Surrogat 0.00 0.000 0.000 0 0 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 [- i PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:23:04 pm 027 Page 1 of 1 000170 Sample Name:L0001359-19 Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11534393\A738368\FC000010.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 7:29:42 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\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1534393\A738368\FC000010.D) API-ES, Neg, SIM, Frag: Var 7.464- C8 Acid 10000 - 8000- 6000- 4000- 2000- J 0- ' ------ .------- ,------- I------- 1------- 1------- 1------- 1------- ]------- 1------- ------- '------- 1------- 1------- 1------- 1 i 1 1 1 i 2 4 6 8 min ` MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1534393\A738368\FC000010.D) API-ES, Neg, S M, Frag: Var 8.330- C10 Surrogate 25000- 20000 - 15000- 10000 - 5000- o - 'i ' ------ 1 :--- 1------- 1------- |------- 1 i 1 | i i 1 | 1 1 1 i 2468 min Compound Amount (ng/mL) R.T. Area Signal *8 Acid 499.30 '10 Surrogai 889.29 7.464 8.330 83579 196466 MSDl 369, EIC=368.7 :369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:23:35 pm U028 Page 1 of 1 000171 Sample Name:L0001359-20 Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11534545\A740928\FC000011.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 7:45:13 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 11 12 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02 :13 :25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1534545\A740928\FC000011.D) API-ES, Neg, SIM, Frag: Var 1400- 7.451 - C8 Acid 1200- 1000- 800- 600- 400- 2 0 0 -I LL 8 'MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1534545\A740928\FC000011.D) API-ES, Neg, SIM, Frag: Var 14000- 8.322- C10 Surrogate, min 12000 10000 8000 6000 H 4000 20000- --i--------- r~ Compound Amount (ng/mL) R.T. :8 Acid 2.54 J10 Surrogat 412.47 7.451 8.322 Area 9717 98065 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 1 PC00414 *** End of Report *** Pri, 9. Jan. 2004 02:24:06 pm 0029 Page 1 of 1 000172 Sample Name:L0001359-1 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11534697\A743616\FC000012.D 1 j ":8 Acid 0.00 j .'10 Surrogat 931.12 7.467 8.331 654 205098 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7 :469.7 PC 00414 *** End of Report *** Fri, 9. Jan. 2004 02:24:43 pm uOSG Page 1 of 1 000173 Sample Name :L0001359-2 Sample Info: Data file :C :\HPCHEM\1\DATA\Chemstor\11534847\A747072\FC000013.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 8:16:26 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02 :13:25 pm 1 13 14 1 5 pi Compound Amount (ng/mL) R.T. :8 Acid 0.00 110 Surrogat 442.77 0.000 8.344 Area 0 104318 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 t 1 .PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:25:08 pm 0 0 31 Page 1 of 1 000174 Sample N a m e :LOO01359-4 Sample Info: ' Data file :C :\HPCHEM\1\DATA\Chemstor\11534998\A749376\FC000014.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 8:32:00 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13 :25 pm LC/MS analysis of perfluorooctanoic acid. 1 14 15 1 5 pi Compound Amount (ng/mL) R.T. I :8 Acid 0.00 | CIO Surrogat 945.92 7.486 8.353 Area 4908 208153 Signal MSD1 369, EIC=368.7: 369.7 MSD1 469, EIC=468.7:469.7 |.. PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:25:49 pm u 03 i Page 1 of 1 000175 Sample Name-.L0001359-5 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11535129\A751616\FC000015.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 8:47:36 PM Seq Line Vial No. Inj . N o . Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. 1 15 16 1 5 pi .'8 Acid 0.00 210 Surrogat 464.61 7.463 8.323 265 108826 MSD1 369, EIC=3 68.7:3 69.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:26:34 pm U033 Page 1 of 1 000176 Sample Name :LOO01359-7 Sample Info: Data file :C :\HPCHEM\1\DATA\Chemstor\11535302\A754432\FC000016.D 1 Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 9:03:14 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\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORU1535302\A754432\FC000016.D) API-ES, Neg, SIM, Frag: Var 7.447- C8 Add 6000- 5000 4000 3000 2000 1000- 0- *MSD1 469, EIC=468.7:469.7 (CHEMSTORYI1535302\A754432\FC000016.D) _L 8 API-ES, Neg, SIM, Frag: Var 25000 H 8.317 - C10 Surrogate 20000 - 15000- 10000- 5000- o -- Compound Amount (ng/mL) R.T. :8 Acid 310.88 :10 Surrogat 802.05 7.447 8.317 Area 55563 178461 Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 ( ___________________________________________ *** End of Report ***' i L PC00414 Fri, 9 . Jan. 2004 02:27:30 pm 0 04 Page 1 of 1 G00177 Sample N a m e :LOO01359-8 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\11535463\A756736\FC000017.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 9:18:49 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. 1 17 18 1 5 pi 38 Acid 0.00 310 Surrogat 497.50 7.478 8.346 796 115613 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 l t; 1 PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:28:05 pm u 0 5 Page 1 of 1 000178 Sample Name:L0001359-10 Sample Info : 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11535624\A760064\FC000018:D Injection Date Acg Operator Instrument Dilution 12/9/03 jmiller PC00414 1 9:34:26 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : 18 19 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903 .M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11535624\A760064\FC000018.D) API-ES, Neg, SIM, Frag: Var 7.478- C8 Acid 6000 5000- 4000- 3000 2000 1000 0 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\11535624\A760064\FC000018.D) API-ES, Neg, SIM, Frag: Var 25000 - 8.351 - C10 Surrogate, 20000 - 15000- 10000- 5000- 0-- Compound Amount (ng/mL) R.T. :8 Acid 314.03 -10 Surrogat 797.47 7.478 8.351 Area 56031 177518 Signal MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7 :469.7 I PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:28:46 pm U36 Page 1 of 1 000179 Sample Name:L0001359-11 i Compound Amount (ng/mL) R.T. f;8 Acid 0.00 j :10 Surrogat 473.73 7.459 8.324 Area 803 110708 Signal MSDl 369, EIC =3 6 8 .7:369.7 MSDl 469, EIC=468.7:469.7 i ________________________________________________ *** End of Report *** i ! PC00414 Fri, 9. Jan. 2004 02:29:23 pm U0 6 7 Page 1 of 1 000180 Sample Name:STD 500 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11535837 \A767232\FC000020.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 10:05:37 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 20 4 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1535837\A767232\FC000020.D) API-ES, Neg, SIM, Frag: Var 12000- 7.447- C8 Aci 10000- 8000- 6000- 4000- 2000- 0 -" *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1535837\A767232\FC000020.D) API-ES, Neg, SIM, Frag: Var 16000- 8.318- C10 Surrogatei 14000- 12000- 10000- 8000- 6000- 4000- 2000-I 0- Compound Amount (ng/mL) R.T. 38 Acid 516.46 CIO Surrogat 526.59 7.447 8.318 Area 86130 121615 Signal MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 I PC00414 *** End of Report *** Fri, 9. Jan. 2004 02 :29 :49 pm 0 0 38 Page 1 of 1 000181 Sample Name :Solvent blank , Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11535971\A770944\FC000021.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 10:21:06 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm 1 21 92 1 5 pi Compound Amount (ng/mL) R.T. :8 Acid 0.00 ;10 Surrogat 0.00 0.000 0.000 Area 0 0 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:30:40 pm 0039 Page 1 of 1 000182 ,* Sample N a m e :L0001359-13 Sample Info: " - Data file :C :\HPCHEM\l\DATA\Chemstor\11536058\A774144\FC000022.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 10:36:38 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. 22 21 1 5 pi 1 Compound Amount (ng/mL) R.T. ':8 Acid 0.00 310 Surrogat 793.64 7.483 8.346 Area 330 176726 Signal MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 l L-. PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:31:19 pm 0 0 40 Page 1 of 1 000183 Sample Name:L0001359-14 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11536164\A776704\FC000023.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 10:52:11 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm 23 22 1 5 ul Compound Amount (ng/mL) R.T. , .'8 Acid 0.00 I :10 Surrogat 470.53 0.000 8.327 Area 0 110047 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:31:48 pm 004 ! Page 1 of 1 000184 ' Sample Name :L0001359-16 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11536541\A779904\FC000024.D 1 *ar--------- -------------------- ------ -------------------------------------- ------------ ------ ------ ----- ------ ------------ -- ----- ------ ------ ------ -- .'8 Acid 0.00 7.451 2365 MSD1 369, EIC=368.7 :369.7 J10 Surrogat 804.04 8.324 178872 MSDl 469, EIC=468.7:469.7 i PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:32:19 pm 0042 Page 1 of 1 000185 Sample Name:L0001359-17 Sample Info : .' '. ' Data file :C:\HPCHEM\l\DATA\Chemstor\11536801\A782592\FC000025.D Injection Date Acq Operator Instrument Dilution 12/9/03 jmiller PC00414 1 11:23:24 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm 25 24 1 5 pi Compound Amount (ng/mL) R.T. j .'8 Acid 0.00 ( J10 Surrogat 423.56 7.480 8.341 Area 246 100354 Signal MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 02:33:33 pm U043 Page 1 of 1 000186 --- Sample Name:STD 500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11536990\A785472\FC000026.D Injection Date Acq Operator Instrument Dilution : 12/9/03 : jmiller : PC00414 :1 11:38:58 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 26 4 1 5 pi Acq. Method : FC8-10.M Analysis Method : C:\HPCHEM\1\METHODSU20903.M Last Changed : 1/9/04 02 :13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1536990\A785472\FC000026.D) API-ES, Neg, SIM, Frag: Var 12000- 7.481 - C8 Acic 10000- 8000- 6000- 4000- 2000- _ 0- f-- 111! 2 1 ''1 ^ 4 1r r 6 r 1 , ! | 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1536990\A785472\FC000026.D) API-ES, Neg, SIM, Frag: Var ! 16000- 8.342- C10 Surrogate 14000 -j -- 12000 ^ 10000- 8000 s 6000 s 4000 s 2000 j I 0- _J 1 ------ ,------- ,------- ,------- j------- 1------- 1------- 1------- 1------- 1------- 1------- 1------- 1------- ------- 1------- ------- 1------- '------- 1------- 1------- r 2_________________ 4__________________6_________________ 8________________ min Compound Amount (ng/mL) R.T. Area Signal !8 Acid 529.14 :10 Surrogat 530.73 7.481 8.342 88015 122470 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 02 :34 :00 pm 0 44 Page 1 of 1 000187 Sample Name :Solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11537098\A787648\FC000027.D Injection Date Acq Operator Instrument ... D i l u t i o n 12/9/03 jmiller PC00414 1 11:54:26 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm 1 27 92 1 5 pi Compound Amount (n g /m L ) R.T. SUB Acid 0.00 10 Surrogat 0.00 0.000 0.000 A rea 0 0 S ig n a l MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 'C00414 *** End of Report *** Fri, 9. Jan. 2004 02:34:43 pm U0 45 Page 1 of 1 000188 Sample Name:STD 50 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\FC000028.D Injection Date Acq Operator Instrument Dilution 12/10/03 jmiller PC00414 1 12:09:58 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000028.D) API-ES, Neg, SIM, Frag: Var 1400- 7.455- C8 Acic 1 28 1 1 5 pi 1200- 1000- 800- 600- 400- 200- i ___ - ,- - 1- - 1- - 1- - - - '- - '- - 1- - ' 1 1 i 1 1 i 1 1 1 i 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (FC000028.D) API-ES, Neg, SIM, Frag: Var 2000 - 8.328- C10 Surrogate 1800 1600 ^1400 1200 1000^ 800- 600 400- 200- J 1 1 1 1 1 i 1 1 1 1 ' i------ 1------- 1------- 1------- ------- 1------- ------- ------- ------- ------- i'1 2 4 6 8 min Compound Amount (ng/mL) R.T. Area Signal :8 Acid 0.08 CIO Surrogat 0.27 7.455 8.328 9352 13001 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 r *** End of Report *** PC00414 Fri, 9. Jan. 2004 03:17:01 pm Q0 46 Page 1 of 1 000189 Sample Name:STD 100 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000029.D Injection Date Acq Operator Instrument Dilution 12/10/03 jmiller PC00414 1 12:25:30 AM Seq Line Vial No. Inj.No. Inj. Vol. : : : : Acq. Method Analysis Method *-- Las t Changed FC8-10.M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000029.D) API-ES, Neg, SIM, Frag: Var 7.474- C8 Add 2500- 2000 1500 1000 500- 1 29 2 1 5 pi *MSD1 469, EIC=468.7:469.7 (FC000029.D) API-ES, Neg, SIM, Frag: Var 3500 H 8.345- C10 Surrogatei 3000 2500- 2000- 1500- 1000- 500- 2ompound 1 1 --1--- --- 124 Amount (ng/mL) R.T. -]--- 1--- <---n--- 1--- 1--- 1--- 1--- r 6 8 min Area Signal ">3 Acid 62.42 10 Surrogat 63.94 7.474 8.345 18620 26139 MSDl 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 'C00414 *** End of Report *** Fri, 9. Jan. 2004 03:17:55 pm 0 0 47 Page 1 of 1 000190 Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\FC000030.D Injection Date Acq Operator Instrument Dilution 12/10/03 jmiller PC00414 1 12:41:03 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000030.D) API-ES, Neg, SIM, Frag: Var \I 7.476- C8 Acic 6000 - ; 5000 ^ 1 30 3 1 5 pi I " 400030001 20001 -- 1000^ _____L A ______ 0' 11111111' ' 1 1 r T 1- . j r-- 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (FC000030.D) API-ES, Neg, SIM, Frag: Var 9000 ~ 8.342- C10 Surrogate 8000- 7000 ^ -- 6000- 5000 4000- 3000 r 2000 / 1000-^ J ,______________ o - ------ ,------- ,------- 1-------~i1------- 11------- 11------- 11------- 11------- '------- 11------- '1------- 11------- 1------- 1 1'------- 11 1 1 1 r 2__________________ 4__________________6__________________8________________ min Compound Amount (ng/mL) R.T. Area Signal :8 Acid 243.39 110 Surrogat 242.11 7.476 8.342 45528 62908 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 r PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:18:13 pm u 48 Page 1 of 1 000191 Sample Name:STD 500 ppb Sample Info: Data file :C :\HPCHEMU\DATA\FC000031 .D Injection Date Acq Operator Instrument Dilution 12/10/03 jmiller PC00414 1 12:56:38 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. J *MSD1 369, EIC=368.7:369.7 (FC000031 .D) API-ES, Neg, SIM, Frag: Var 12000- 7.448- C8 Aclc 1 31 4 1 5 pi 10000- r 8000- 6000- 4000- 2000- - o- .. L 1 1 -------,------- 1 1 J ' ' [ 11111 ^ 1^ , -r , I -- 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (FC000031 .D) API-ES, Neg, SIM, Frag: Var 16000 -J 8.325 - C10 Surrogate 14000 -j 12000 ^ 10 0 0 0 7 8000- 6000 7 4000 -j 2000 -j 0- ------------- , ! j >1 '1 ... 24 Compound Amount (ng/mL) R.T. *'8 Acid 514.20 :10 Surrogat 522.21 7.448 8.325 ''1 Area 85794 120712 1' 6 J . 1__________ r i -r 8 . --m , min Signal MSDl 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 . i PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:18:39 pm 0049 Page 1 of 1 000192 Sample Name:STD 750 ppb Sample Info: Data file :C :\HPCHEMU\DATA\FC000032 .D Injection Date Acq Operator Instrument Dilution 12/10/03 jmiller PC00414 1 1:12:11 AM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODSU20903 .M 1/9/04 ,02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000032.D) API-ES, Neg, SIM, Frag: Var 16000- 7.466- C8 Acid, 14000- 12000- 10000H 800060004000 H 2000- 0- *MSD1 469, EIC=468.7:469.7 (FC000032.D) API-ES, Neg, SIM, Frag: Var 8.338 - C10 Surrogate 20000 - 1 32 5 1 5 ul min 15000- 10000- 5000- 0- Compound Amount (ng/mL) R.T. ~3 Acid 758.63 .0 Surrogat 767.52 7.466 8.338 Area 122137 171335 mm Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 'C00414 *** End of Report *** Fri, 9. Jan. 2004 03:19:08 pm 05 Page 1 of 1 000193 Sample Name:STD 1000 ppb Sample Info : Data file :C:\HPCHEM\1\DATA\FC000033.D Injection Date Acq Operator Instrument Dilution 12/10/03 jmiller PC00414 1 1:27:47 AM Seq Line Vial No. Inj . No.. Inj. Voi. : : : : Acq. Method Analysis Method *' Last Changed FC8-10.M C :\HPCHEM\1\METHODS\120903.M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000033.D) API-ES, Neg, SIM, Frag: Var 20000 - 7.473- C8 Acid 17500- 15000- 12500- 10000d 7500- 5000- 2500- 0--- '--- T 4 *MSD1 469, EIC=468.7:469.7 (FC000033.D) API-ES, Neg, SIM, Frag: Var 8 30000 - 8.345 - C10 Surrogate 25000 - 20000 - 15000- 10000 - 5000- 1 33 6 1 5 pi --- i--- 1- 1 2 1 4 Compound Amount (ng/mL) R.T. "8 Acid 962.85 10 Surrogat 977.27 7.473 8.345 Area 152502 214621 1 1111111 6 8 min Signal MSDl 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 V _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ ____________________________________________ ^ *** End of Report *** U0 5 I j PC00414 Fri, 9. Jan. 2004 03:19:44 pm Page 1 of 1 000194 ~ Sample Name:STD 1500 ppb Sample Info : Data file :C :\HPCHEM\1\DATA\FC000034.D Injection Date Acq Operator Instrument Dilution 12/10/03 jmiller PC00414 1 1:43:22 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEMX1\METHODS\12 0903 -M 1/9/04 02:13:25 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000034.D) API-ES, Neg, SIM, Frag: Var 7.460- C8 Acid 25000 - 1 34 7 1 5 p.1 ... 20000 - 15000- 10000- 5000- A 0- _ J 1____ 1' 1 1------- 1 1 ' 1 1 1 1 1^ 'i . 2468 *MSD1 469, EIC=468.7:469.7 (FC000034.D) API-ES, Neg, SIM, Frag: Var 40000 j 8.334- C10 Surrogate >, min 35000 j 30000 -j 25000 -j 20000 - 15000 j 10000 : 5000 j 0- A 1 1 1------- 1 '------- 1 1 1 24 11' 1' 6 ___ L 1 .. 1ni 1 1^ i 8 min Compound Amount (ng/mL) R.T. Area Signal 8 Acid 1371.55 10 Surrogat 1379.02 7.460 8.334 213269 297530 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Fri, 9. Jan. 2004 03:20:09 pm 0 52 Page 1 of 1 000195 January Projects Client Cecos DuPont DuPont DuPont 3M / Daikin Hercules BP Rutgers Organics SPI (fluoropolymer) Crompton Bayer Beazer Neolytica -N IH AMEC -SutbfivGaiii&tQia Lyondell Mise Environmental Calgon Carbon Lonza / TRS S& npfr& L, Phibro Phibro Cognis Aventis Pasteur Eyetech Pfizer Pfizer Pfizer Ft Dodge AH Ft Dodge AH Boston Scientific Vertex West Pharmaceutical -P tfv a Schering Plough Taxolog Par Pharmaceutical ALSO 3M Pfizer AH Ft Dodge Ft Dodge Ft Dodge Project Responsible Group Revenue quarterly monitoring water / blood / air samples reference standads DPX-MP062 ILV water and soil samples Rf-Teta paper analysis phytoremediation study routine environmental water / air / solids propargite ILV fipronil report craig farm monitoring 90 day stability fneed-prejeet)method development -perchefate' deicer characterization cyanide testing OP pesticides (low level) Kd Stud GCMS, Inorganics LCMS LC, GCMS, Inorganics, LCMS LCMS LCMS LCMS GCMS GCMS / Inorganics LCMS LCMS LCMS LCMS LC tC M S rLrGMS LCMS -tew sLCMS Inorganics GCMS (pending)E-Fate $80,000 W 9 9 5 0 ,0 0 0 $15,000 $ 1 3 ,0 0 0 $30,000 $10,000 $ 3 0 ,0 0 0 $6,000 $ 1 0 ,0 0 0 $13,000 $6,000 $5,000 $2,000 -sooroee$7,500 $3r0OO~$5,000 $15,000 $67666 ilo o o $8,000 stability and release salinomycin validation BAP in vitamin E method transfers (4) AN-TMD-1002 (samples) validation (Macugen mPEG) PEG sample analysis method development (6) Amitraz physical properties EU validation (initiation) MD + Samples stability and release cleaning validation dissolutiomratidaftoa "ane-io-cosmetics transfer stability and release rat plasma testing unknown ID LC, micro, Inorganics LCMS GCMS Inorganics LC LC (completion of analytical) LCMS GCMS (not yot awarded) GCMS, LC LC LC LC Inorganics tGMS-{peRcKfi) -ffwaffle&-(pgnding-) GCMS, LC LCMS (pending) LCMS $40,000 $18,000 $10,000 $ge,-OeO #|,oe > $25,000 $28,000 $6,000 $ 3 0 ,0 0 0 $27,500 $70,000 $ 2 0 ,0 0 0 $257060 30COO $3,000 $42^060<$67000' $10,000 $007060 K Z io o c ? $6,000 blood validation (prepaid) amoxycillin validation (prepaid) 5 batch (prepaid) MD report (prepaid) routine (waiting on Celsus) LCMS LCMS LC, GCMS Inorganics GCMS u055 000196 3058 Research Drive State College, PA 16801 RESEARCH Phone: 814-272-1039 Fax: 814-231-1580 Login #: L0001359> 1,469 Project: P0000419 Project Storage: Submitted By: Michael D. Aucoin Status: Unreceived Login Type: Immediate Receipt of Samples Started: Date Start: 11/25/2003 11:21:15AM Due Date: 12/09/2003 Received Date: 11/25/2003 Received By: AMMERMAN, MARK A+ Spread Sample: Label: Project Title/Type: Analysis of PFOA in OVS Tubes / ROUTINE Conform COC Sample: Conform COC: Conform Sample: Conform Request: frcvcs. True True True True Login Notes: Conform Notes: As per Mike Aucoin, sample WWK-A-AMS6-E4 is cancelled. MSA 11/25/03 Package PK0001939 Carton Packages / Containers Mail Date / Condition Shipper/ ID Temp. Control / Temperat 11/25/2003 10:50:59AM Package & Contents Uncompromised FEDEX 8363913019820200 RT Direction / Handled By . RECEIVED AMMERMAN, MARK Container # C0020181 C0020182 C0020183 C0020184 C0020185 C0020186 C0020187 C0020188 C0020189 C0020190 C0020191 C0020192 C0020193 C0020194 C0020195 C0020196 C0020197 C0020198 C0020199 C0020200 C0020201 Gross Weight 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.1 g 7.1 g 7.1 g 7.2 g 7.2 g 7.2 g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g RM Container Type Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Miscellaneous Item Key None Description Preservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE ICOC Mfg. Lot Mfg, ID U54 11/25/2003 Login.rpt Report Version: Nov 13 2003 4:51PM Page 1 of 4 Instance: R0074478 0 0 0 1 9 7 R0074478 Sample ID L0001359-0001 Matrix GAS L0001359-0002 GAS L0001359-0003----- -- GAS L0001359-0004 GAS L0001359-0005 GAS b0Q01359-0606'''' GAS L0001359-0007 GAS L0001359-0008 GAS L00013590000- GAS L0001359-0010 GAS L0001359-0011 GAS L00Q1350 0612- GAS L0001359-0013 GAS - L0001359-0014 GAS *0001350'0015 GAS L0001359-0016 GAS L0001359-0017 GAS " 1:0001359-00TO* GAS L0001359-0019 GAS L0001359-0020 GAS , ^ L0001359-0021 GAS Login Samples 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 Sample WWK-A-AMSFBLK-E4 A WWK-A-AMSFBLK-E4 B WWK=A-AM8FBLK'`E4"C ~ WWK-A-AMS1-E4 A WWK-A-AMS1-E4 B --WWK-A=AMai-C4 G WWK-A-AMS2-E4 A WWK-A-AMS2-E4 B -WWK-A AM62 E4 G WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMG3-E4 (3~ WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK A AMG4 E4 O WWK-A-AMS5-E4 A WWK-A-AMS5-E4 B -WWK A AMS5-E4 C Control 1 A Control 1 B -- Control 1-Q--' Date Sampled Date Received 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 Date Due 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 11/25/2003 Login.rpt u U55 Report Version: Nov 13 2003 4:51PM Page 2 of 4 Instance: R0074478 0 0 0 1 9 8 R0074478 L0001359-0001 i C o n ta in e r C0020181 / Other / NONE I L0001359-0002 Container C0020182/Other/NONE L0001359-0003 Container 00020183/ Other /NONE L0001359-0004 Container C0020184 / Other / NONE L0001359-0005 Container 00020185/Other / NONE ' L0001359-0006 Container C0020186 / Other / NONE L0001359-0007 Container 0 0 0 2 0 1 8 7 /O ther/N O N E L0001359-0008 Container C0020188/Other/NONE L0001359-0009 Container C0020189/Other/NONE L0001359-0010 C o n ta in e r C0020190/ Other/ NONE L0001359-0011 C o n ta in e r C0020191 /O ther/NO NE L0001359-0012 C o n ta in e r - 11/25/2003 Login.rpt Login Bottles Method Method Method Method Method Method Method Method Method Method Method M ethod u U56 Report Version: Nov 13 2003 4:51PM Page 3 of 4 Instance: 000199 R0074478 R0074478 C0020192/Other/NONE L0001359-0013 Container C0020193 / Other / NONE L0001359-0014 Container C0020194/Other/NONE ,,L0001359-0015 Container C0020195/ Other /NONE L0001359-0016 Container C0020196 / Other / NONE L0001359-0017 Container C0020197/Other/NONE L0001359-0018 Container . .. C0020198 / Other / NONE L0001359-0019 Container C0020199/Other/NONE - L 0 0 0 1 359-0020 Container C0020200/Other/NONE L0001359-0021 Container C0020201 / Other/NONE Method Method Method Method Method Method Method Method Method 11/25/2003 Login.rpt uOb? Report Version: Nov 13 2003 4:51PM Page 4 of 4 Instance: 000200 R0074478 R0074478 PROJECT INFORMATION Client (name & 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 Page__ |_ of I ANALYSES REQUESTED Project Manager (Name & E-mail Address): 000201 yruvj: Phone: ( ? > e s ^ Fax: Sampler: Project Name: RO # ^ Quotation #: r\ ____________ Please fill out this form com pletely to ensure correct analysis and proper handling of your samples. O o :.:d J SAMPLE ANALYSIS ExyUMS# Client Sample Identification v q m o K - ft ViOVY-y- ft - F v r n M - ^ nwOVs- Collection Collection Date Time IIM o -Qj oteV. * % euaa VMiife \a)v O V n- ft fr,-EHr 6-fc-V PUSH k0\ =5E dUM^ oo. _o fl Ec o =o u z u Specify Matrix He He aX. -C LAB USE ONLY Comments___________ "W - /U b i n*Iffti}f /lr*j CHAIN OF CUSTODY Relinquished by Date Time tl M o2> 9%2>0 (T Cooler ID # t/!0 ` ~l>-- Received b; Off Cooler Temp. (C) Time M ft? . 4 S /V~e OTHER INFORMATION LAB USE ONLY * 'S 2 PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: I I Sample results only Add case narrative 0 Add quality control summary Add calibration summary 1 I Add raw data Other : i. REV. 3 -0 2 \! 000202 Samplers): LK, REK DuPont Washington Works Air Sampling Program FedEx Airbill #: 836391301982 Event Number Event 4 669842 669908 669878 669901 669769 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-E4 WWK-A-AMS2-E4 WWK-A-AMS3-E4 WWK-A-AMS4-E4 WWK-A-AMS5-E4 WWK-A-AMS6-E4 Hours 5 6 7 8 9 1.018 1.029 1.028 1.021 1.015 1.014 Minutes 300 360 420 480 540 23-Nov 23-Nov 23-Nov 23-Nov 23-Nov 23-Nov Hours 10 11 12 13 14 6:35 6:30 6:30 6:44 6:09 6:56 Minutes 600 660 720 780 840 24-Nov 24-Nov 24-Nov 24-Nov 24-Nov 24-Nov Hours 15 16 17 18 19 6:12 6:22 6:22 6:34 6:01 6:45 Minutes 900 960 1020 1080 1140 Field Blank: yes WWK-K-AMSFBLK-E4 yes or no Weather. 11/23= 48 degrees and clear, expect temperature to go to upper 60's. 11/24= 45 degrees and clear, expect rain and drop in temperature to 30's. 1.003 1.008 1.022 0.9668 0.9892 * Hours 20 21 22 23 24 1428 1434 1433 1431 1434 880 Minutes 1200 1260 1320 1380 1440 SAFER operational: yes yes or no Comments: Total minutes column is the reading from the monitor counter. * The pump for AMS6 was not running when we collected the sample and the counter only read 880 minutes. We can not get the AMS6 pump to run for Post Calibration even plugged into building outlet. We will replace pump before next test. ON JTi ZD O 11/24/03 Page 1 of 2 airdataevent4 11/25/2003 000203 1442.994 146S825 1422 2709 1437,0114 1 m O vQ O 3 Page 2 of 2 airdataevent4 I uU6 I T 1 From Express Sate----- j | _ (')_ L) USA A irb ill FedEx fi3 L 3 `!1 3 Q n a 2Tracking Number 4a, Express Package Service r _ j r v p ; ^ n ,(a_ . U* i-- i 1- .r- Recipient's Copy elfverycommitmentmaybe laterin some areas, Sender's Name -- lfTV- i V-V. 2C 4X Phone "j . ] - 'j j :' A M - 'V , 4 V I \ ^ tU - D & s- delivery to select locations Company \) !; VJ Q -O V' ^ ~ T "N Address \ H \ K * . S; ^ ^ V o i \ ^\v S v >- ` Stats, ' ) Dept/Roor/Suite/Rqm " \1 V ^|p ' l l .1 Q \ 1>\ \ " 2 YourInternal Billing Reference 3 To \ Recipient's Name \ ..... ' ' \` 'T " ... . \ F \ X Y . y C ,-'\ 'S 1 1 ", t < (jv f -f' V . V,. . v \ j \ . ^ Phone 'N "f u . V 0 L: l U V A -w z : Company f \ \J v\ Address "} k \' L . !Yl . . To"HOLD' atFedExlocation,pmrt FedE*address. GftftSk "$<'i f , r ,5 : . i . .} "Jr ' W `'X-i . .i'i 1L 1 '$ r u^ Wecannd^m^.toP.O.boxesorP.O.ZIP codas. Address I Vt: y:^. % tF1,-, DeptyRoof/Surte/Room City ' . X . ; ----------------------------- rt------ FT V V 13 stare 32 ap \ f . \ ' Is M'- FedEx Envelope rale not availabte-Minimum chame; One-nound rale ______ i 4b,,Express Freight Service f. I FedEx 1Day Freight* f-- ' Next business clay .j Call for Confirmation;_______ . P I FedEx2DayFreight -- 1 Secondbusmessday Packages over 150lbs, itment maybe later in some areas. I l FedEx 3Dav Freight 1-- 1 Third business day 5 raKagmg FedEx Envelope' FedEx Pak* Includes FedEx Sma Pak, FedEx -- large Pak, and FedEx Sturdy Pak * Declared value limit S5Q Other SATURDAYDeBvay I_j AvailableonlyforFedExPriority Overnightand FedEx2Day s to selectZIP codes 7 ---- IncludeFedExaddressmSection3. p i ","i Weekday u tecation j-- j HOLDSaturday I-- 1 at FedEx Location Avaiable onlyfor FedEx Priority Overnight Does this shipm ent contain dangerous goo ds? and FedEx 20ayto ----------- One box must be checked. INo |--1Yes r~l Yes J ? 1___j1 As per attached , iU__ 1 SShhipippper's Declaration - I i D rvJce select locations Shipper's Declaration - not required I-- I Dry Ice, 9, UN 1845 _ Dangerous Goods (including Dry Ice) cannotbe shipped si FedEx packaging. j-- i '' > I__ I Cargo A ircraft Qnly 51 /Payment Biuta___ r , . V/ * ---------------- EnterFExte tt. No. w C rw a Cani No.bgk, j j Obtaffvfieci -- A c c t fife ... x P i u * : nter M nTMrdf^ ej,Yedit Card c$yCheck ' TotalPackages TotalWeiht htal DeclaredValue. l - * .00 r Our liability is limited to SIQ funi you declare a higher value. See back for details It Total Charges L 8 Release Signature't *yTM*deliverwnhout'obammggnm J By signing you a u th o n fe ffi& fo rth is shipment witftbutjifrtainina a a m end agree to inderanifeatjifhoP* harmless from anyresulting c la im & jF il Questions? V ls rt t Wb site a t fedex.com " or call I.B O O .G Q .ftd& tM Q p-333- '* '- U ?.' to.DatetO/01*f#T57^2y4' 2001 FedExPRINTED IN U S A WCS102 A JL -fe - - -i- 000204