Document Znq8VQr12xB4YOp5Gy5nmN9NZ

Proven Results. Attachment 2 -4 M ir t7 r tr j Analytical Report Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 10 Exygen Research Report No. L0001667 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 CZD f\5 OD o ~o zo m ~ o C';> V? o o ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 1 of 7 j K 305 8 Research Drive Sttaate College, PA 16801, USA J : 800.281.3219 0 0 4 5 ^ 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. Results are not reported for sample WWK-A-AMS2-E10 because of sampler malfunction. The samples were analyzed for Perfluorooctanoic Acid (C8 Acid) using liquid chromatography / mass spectrometry (LCMS). The method employed is entitled "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in OVS Airtubes by LCMS" (James Miller, Exygen Research, February 17, 2003). The OVS tubes were separated into three fractions for specific fluorochemical analysis. Fraction A consisted of the filter, backing material and plastic ring. Fraction B contained the first bed of XAD resin and the PUF backing. Fraction C contained the second bed of XAD resin and PUF backing. Fractions A and B were extracted with 1 mL of methanol. Fraction C was not analyzed but saved for possible future analysis. Perfluorodecanoic Acid (CIO Acid) was added as a surrogate spike to each fraction prior to extraction. Instrument operating conditions can be found at the beginning of each analytical run. Raw instrument data is given in Appendix A. Chain-of-custody information can be found in Appendix B . ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 2 of 7 00453 Results S u m m ary Request # WWK-A-AMS1-E10 A WWK-A-AMS1-E-10 B WWK-A-AMS1-E10 C WWK-A-AMS1-E10 (Total) Air Volume Sampled (L) 1447 1447 1447 C8 Acid (mg/m3) < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS3-E10 A WWK-A-AMS3-E10 B WWK-A-EMS3-E10 C WWK-A-EMS3-E10 (Total) 1413 1413 1413 0.0004 < 0.00007 NA 0.0004 WWK-A-AMS4-E10 A WWK-A-AMS4-E10B WWK-A-AMS4-E10 C WWK-A-AMS4-E10 (Total) 1410 1410 1410 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS5-E10 A WWK-A-AMS5-E10 B WWK-A-AMS5-E10 C WWK-A AMS5-E10 (Total) 1451 1451 1451 0.0003 < 0.00007 NA 0.0003 WWK-A-AMS6-E10 A WWK-A-AMS6-E10 B WWK-A-AMS6-E10C WWK-A AMS6-E10 (Total) 1456 1456 1456 < 0.00007 < 0.00007 NA <0.00014 NA - Not Analyzed. B fraction was below the quantitation limit, therefore the backup fraction does not require analysis. 1. "<" is defined as not detected at or above the reported level. 2. Sample results have not been corrected for blank results or control spike recoveries. 3. Please note the following descriptions of the OVS sample tube fractions: Fraction Fraction Description A Frit Extract B 1st set beads extract C 2nd set beads extract (not analyzed) ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 3 of 7 CO0454 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) 619 C8 Acid (percent recovery 124 Blanks Request # WWK-A-AMSFBLK-E10 A WWK-A-AMSFBLK-E10 B Voi. Of Air (L) 0 0 C8 Acid (ug/fraction) 0.74 <0.10 O ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH '71 71 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-E10 A WWK-A-AMSFBLK-E10 B WWK-A-AMS1-E10 A WWK-A-AMS1-E10B WWK-A-AMS3-E10 A WWK-A-AMS3-E10 B WWK-A-AMS4-E10 A WWK-A-AMS4-E10 B WWK-A-AMS5-E10 A WWK-A-AMS5-E10 B WWK-A-AMS6-E10 A WWK-A-AMS6-E10 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) 569 554 540 594 526 594 517 335 520 491 527 391 522 337 Percent Recovery (%) 114 111 108 119 105 119 103 67* 104 98 105 78 104 67* * Surrogate recovery outside of advisory range. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 000456 Calculations Request # WWK-A-AMSFBLK-E10 A WWK-A-AMSFBLK-E10 B WWK-A-AMS1-E10 A WWK-A-AMS1-E10 B WWK-A-AMS3-E10 A WWK-A-AMS3-E10 B WWK-A-AMS4-E10 A WWK-A-AMS4-E10 B WWK-A-AMS5-E10 A WWK-A-AMS5-E10 B WWK-A-AMS6-E10 A WWK-A-AMS6-E10 B Control Spike A Control Spike B Vol. Of Air (L) 0 0 1447 1447 1413 1413 1410 1410 1451 1451 1456 1456 0 0 C8 Acid (raw-ppb) 738 12 <10 <10 615 <10 <10 <10 396 <10 <10 <10 619 < 10 C8 Acid (ug/fraction) 0.74 <0.10 <0.10 <0.10 0.62 <0.10 <0.10 <0.10 0.40 <0.10 <0.10 <0.10 0.62 <0.10 C8 Acid (mg/m3) < 0.00007 < 0.00007 0.0004 < 0.00007 < 0.00007 < 0.00007 0.0003 < 0.00007 < 0.00007 < 0.00007 000457 AT T DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 7 Example Calculation For sample WWK-A-AMS5-E10 A C8 Acid, = [396 ng/ml of C8 Acid x (1 mL) x (1 ug / 1000 ng) x (1 mg /1 0 0 0 ug) ] / [(1451 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 COO458 ANALYTICAL DATA REVIEW SHEET LC/MS F tid e S Analyst 11f- J*/ fio F b - L e & > f Reviewed by Sig^(ture/Date -- F Z' ~C'/ Y 2 / / *} m L / Sinature/Date J v / ti Q8 000459 LC/MS SYSTEM AND OPERATING CONDITIONS Client: Dupont EXYGEN STUDY: L00Q1667 Instrument: Hewlett-Packard 1100 LC/MSD (LC/MS 3) API-ES Interface - Negative SIM mode Nitrogen: 10 L/min at 300C Fragmentor: Variable; Vcap: 3500V Computer: Hewlett-Packard Kayak workstation Software: Microsoft Windows NT 4.0 Agilent ChemStation Version A.08.03 HPLC Equipment: HP G1379A Solvent Degasser HP G1311A Quaternary Pump HP G1313A Autosampler HP G1316A Column Thermostat HP G1946A MSD HPLC Column: Column Temp.: Mobile Phase (A): Mobile Phase (B): Thermo Hypersil-Keystone Betasil 0 8 , 30 x 2.0 mm x 3pm 35 C 2mM Ammonium acetate in OmniSolv W ater HPLC grade Methanol Time %A 0.0 70 6.0 10 10.0 10 10.0 STOP Post Time = 4 min. Total run time = 14 min. Flow Rate: 0.3 mL/min Injected Volume: 5 pL %B 30 90 90 STOP U9 Page 1 of 2 COO460 Ions monitored: Analyte C8 Acid (PFOA) C10 Surrogate Ion (m /z ) 369 469 Extraction Date: January 21, 2004 Analyst: James R. Miller A ( H Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039, FAX: (814) 231-1580 uoio Page 2 of 2 COO4 6 1 Instrument : LCMS3 Wed Jan 07 09:11:11 2004 G194 6: API__ES Negative mode Page 1 of 3 C:\HPCHEM\1\1946TUNE\ATUNES.TUN Scan: 50.00 - 3000.00 Samples: 8 Thresh: 0 Step: 0.10 29501 peaks Base: 2233.85 Abundance: 1132032 F Raw,Gauss 0.3 100 -, 80 - 60 - 40 - 20 - 0 - U --- r- ,--- ,--- 1--- 1--- ,--- ,--- 1--- 1 U - i--- 11 500 1000 i1 i1 i 1500 , i~ 2000 2500 m/z gf Abund 112.99 80352 602.00 21400 1034.05 197568 1633.95 610624 2233.85 1132032 Rei Abund 100.00 26.63 245.88 759.94 1408.84 Iso m/z 113.98 602.99 1034.95 1634.95 2234.85 Iso Abund Iso Ratio 1768 2.20 3222 15.06 43112 21.82 217216 35.57 550720 48.65 U 1 Instrument : LCMS3 Wed Jan 07 09:11:11 2004 G1946: API_ES Negative mode C :\HPCHEM\ Mode: API -ES Polarity: NEG Fragment Skim2 Lensl Lens2 Iris Gain VAR WidthGain -128 6.0 WidthOffs VAR -4.0 MassGain- 36.30 18 MassOffs VAR 272 Energy 5.0 OpolPeak 300 OpolKnee 316 3.0 QuadDC 0.00 EMV VCap Status: CapCur ChamCur 2358 Samples 4000 Averages StepSize 8 1 0.10 55 DryingGas 6.0 0.82 Gas Temp 300 Quad Temp 99 Neb Pres 20 Page 2 of 3 r r-jf 0012 C004G3 Instrument : LCMS3 Wed Jan 07 09:11:11 2004 Gl946: API_ES Negative mode Page 3 of 3 C :\HPCHEM\1\194 6TUNE\ATONES.TUN v -,Mass Offset 2.00 Dynamic Parameter Ramp 1.00 0.00 - - 1.00 - - , , , 1 r-- ,-- ,-- 1-- 1-- m-- 1-- 1-- 1-- r-- 1-- 1-- 1-- 500 1000 1500 2000 Mass 112.99 1633.95 Setting 0.56 0.61 Mass 601.98 2233.91 Setting 0.62 0.56 Mass 1033.99 i |i i r '1 2500 3000 Setting 0.63 U013 C00464 Sequence : C:\HPCHEM\1\SEQUENCE\012104.S Sequence Table: Method and Injection Info Part: Line Location SampleName Method Inj SampleType InjVolume DataFile 1 Vial 1 STD 50 ppb 2 Vial 1 STD 50 ppb 3 Vial 2 STD 100 ppb 4 Vial 3 STD 250 ppb 5 Vial 4 STD 500 ppb 6 Vial 5 STD 750 ppb 7 Vial 6 STD 1000 ppb 8 Vial 7 STD 1500 ppb 9 Vial 92 solvent blank 10 Vial 11 L1667-22 11 Vial 12 L1667-23 12 Vial 13 LI 667-1 13 Vial 14 LI 667-2 14 Vial 15 L1667-4 15 Vial 16 LI 667-5 16 Vial 17 L1667-7 17 Vial 18 L1667-8 18 Vial 19 LI 667-10 19 Vial 20 L1667-11 20 Vial 4 STD 500 ppb 21 Vial 92 solvent blank 22 Vial 21 L1667-13 23 Vial 22 L1667-14 24 Vial 23 L1667-16 25 Vial 24 L1667-17 26 Vial 25 L1667-19 27 Vial 26 L1667-20 28 Vial 4 STD 500 ppb 29 Vial 92 solvent blank 30 Vial 1 STD 50 ppb 31 Vial 2 STD 100 ppb 32 Vial 3 STD 250 ppb 33 Vial 4 STD 500 ppb 34 Vial 5 STD 750 ppb 35 Vial 6 STD 1000 ppb 36 Vial 7 STD 1500 ppb FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 1 Sample 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Sample 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib 1 Calib Calibration Part: Line Location SampleName Method CalLev Update RF Update RT Interval 2 Vial 1 3 Vial 2 4 Vial 3 5 Vial 4 6 Vial 5 7 Vial 6 8 Vial 7 30 Vial 1 31 Vial 2 32 Vial 3 33 Vial 4 34 Vial 5 35 Vial 6 36 Vial 7 STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 1/21/04 5: 11 :03 PM jmiller / f . 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 0014 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 Cr 0rP;a0ge4G1 Sequence : C:\HPCHEM\1\SEQUENCE\012104.S CMS3 1/21/04 5:11:03 PM jmiller U0 i 5 Page 2 of 2 C004G6 Method C:\HPCHEM\1\METHODS\012104.M Calibration Table Calib. Data Modified Thursday, February 26, 2004 8:41:06 AM 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 11 | 7.256 1 1 50.00000 2.92183e4 2 100.00000 5.68997e4 3 250.00000 1 ,53989e5 4 500.00000 2.86689e5 5 750.00000 4.10786e5 6 1000.00000 5.27241e5 7 1500.00000 7.52 648e5 8.132 2 1 50.00000 7.91142e4 2 100.00000 1.53861e5 3 250.00000 3.99620e5 4 500.00000 7.28651e5 5 750.00000 1.02750e6 6 1000.00000 1.30010e6 7 1500.00000 1.80579e6 Amt/Area 11_ 1.71126e-3 1.7 5748e-3 1.62349e-3 1.74405e-3 1 ,82577e-3 1.89666e-3 1.99296e-3 6.31998e-4 6.49935e-4 6.25594e-4 6.86199e-4 7.29926e-4 7.69169e-4 8.30660e-4 Ref Grp Name 1 C8 Acid 1 CIO Surrogate More compound-specific settings: Compound: C8 Acid Time Window From 7.083 min To 8.084 min Compound: CIO Surrogate Time Window : From 7.936 min To 8.741 min Peak Sum Table ***No Entries in table*** 00414 2/26/04 9:07:13 AM jmi11er y u0 16 C 0 0 4 6 7 Pae 1 o 2 Method C :\HPCHEM\1\METHODS\012104.M Calibration Curves H C8 Acid at exp. RT: 7.256 MSD1 369, EIC=3 68.7:369.7 Correlation: 0.99836 Residual Std. Dev.: 16624.39920 Formula: y = mx + b m: 500.04793 b: 20324.66171 x: Amount[ppb] y : Area CIO Surrogate at exp. RT: 8.132 MSD1 469, EIC=468.7:469.7 Correlation: 0.99659 Residual Std. Dev.: 57325.18366 Formula : y = mx + b m: 1195.75543 b: 76037.28359 x: Amount[ppb] y : Area :00414 2/26/04 9:07:13 AM jmiller 0017 Page 2 of 2 C00468 Sample Name:STD 50 ppb Sample Info:Wann Up Injection Data file :C:\HPCHEM\1\DATA\Chemstor\12075253\A932864\FC000001.D 1 C8 Acid -CIO Surrogate 33510.20 90304.16 26.37 11.93 7.287 8.160 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 [ PC00414 Thu, 26. Feb. 2004 09:42 :51 am 0018 Page 1 of 1 C00469 Sample Name:STD 50 ppb Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\12064816\A929984\FC000002.D Injection Date Acq Operator Instrument Dilution 1/21/04 jmiller PC00414 1 5:29:55 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\012104,M 2/26/04 08:41:06 am 2 1 1 5 pi 1 Compound Name C8 Acid CIO Surrogate Area 32905.32 86693.89 Amount 25.16 8.91 Meas. Ret. T Signal Desc. 7.279 8.151 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 *** End of Report *** , i PC00414 Thu, 26. Feb. 2004 09:38:08 am 0019 Page 1 of 1 C00470 Sample Name:STD 100 ppb Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\12064886\A932032\FC000003.D 1 C8 Acid .CIO Surrogate 63015.27 167683.17 85.37 76.64 7.284 8.153 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:32:30 am 0020 Page 1 of 1 C00471 Sample Name:STD 250 ppb Sample Info: i Data file :C:\HPCHEM\l\DATA\Chemstor\12064964\A934144\FC000004.D Injection Date Acq Operator Instrument Dilution 1/21/04 jmiller PC00414 1 6:00:59 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method -- Last Changed FC8-10.M C :\HPCHEM\1\METHODS\012104 .M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 4 3 1 5 pi 1 C8 Acid CIO Surrogate 165912.75 427822.09 291.15 294.19 7.279 8.150 *** End of Report *** MSD1 369, EIC =368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:30:20 am U021 Page 1 of 1 CO0472 Sample Name:STD 500 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12075910\A941952\FC000005.D Injection Date Acq Operator Instrument Dilution 1/21/04 jmiller PC00414 1 6:16:32 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am 5 4 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\12075910\A941952\FC000005.D) 40000 : APl-ES, Neg, SIM, Frag: Var 7.260- C8 Acid 35000 30000 -i 25000 ^ 20000 ^ 15000 r 10000^ 5000 r 0 -_---------------------------------------------------------------------------------------------- 1 , I I I >------------------- 1--------- ---------- 1------------------- 1------------------- 1------------------- 1---------------- ______________________________ 2______________________ 4________________ *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\12075910\A941952\FC000005D) 6________________________ API-ES, Neg, SIM, Frag: Var T 8 8.130- C10 Surrogate 100000- \ 80000 - 1 i --r min 60000 - 40000 - 20000 - ,. Compound Name C8 Acid 4310 Surrogate ,j 2 Area 305549.25 770445.06 1 4 6 Amount Meas. Ret. T J..L . i' 1 8 Signal D e s c . min 570.39 580.73 7.260 8.130 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 09:29:33 am U022 Page 1 of 1 C00473 Sample Name:STD 750 ppb Sample Info: I Data file :C:\HPCHEM\l\DATA\Chemstor\12076078\A944064\FC000006.D Injection Date Acq Operator Instrument Dilution 1/21/04 jmiller PC00414 1 6:32:07 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : 6 5 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM2076078\A944064\FC000006.D) API-ES, Neg, SIM, Frag: Var 60000 - 7.254 - C8 Acid 1 50000 - 40000 - 30000 ^ 20000 -j 10000^ .. . ,/ ' , , , I -, r r - I ^ , , ] I I 1 1 r' I '-------------------- 2 4 6 8 min 1" *MSD1 469, EIC=468.7:469.7 (CHEMSTORV12076078\A944064\FC000006.D) API-ES, Neg, SIM, Frag: Var 8.129- C10 Surrogate 140000J 120000- J **** 100000: 80000 - 60000J p\ 40000 - 20000 - l 1 Compound Name 2 Area 46 Amount Meas. Ret. T J l___ n 8 1 Signal Desc. 1 1 r-------------------min C8 Acid ,C10 Surrogate 434924.00 1085061.12 829.12 843.84 7.254 8.129 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 09:29 :03 am U023 Page 1 of 1 COO474 Sample Name:STD 1000 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12076271\A946176\FCO00007.D 1 C8 Acid .CIO Surrogate 555513.00 1359380.87 1070.27 1073.25 7.261 8.133 *** End of Report *** MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7 :469.7 I PC00414 Thu, 26. F e b . 2004 09:28:13 am U24 Page 1 of 1 C 094*75 Sample Name:STD 1500 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12065231\A942528\FC000008.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/21/04 jmiller PC00414 1 7:03:18 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : FC8-10.M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 8 7 1 5 pi 1 C8 Acid ..CIO Surrogate 791063.56 1880773.88 1541.33 1509.29 7.266 8.138 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 I.. 1 PC00414 Thu, 26. Feb. 2004 09:27:30 am U025 Page 1 of 1 C00476 Sample Name:solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12076641\A950528\FC000009.D 1 C8 Acid ,,..CIO Surrogate ! 0.00 1913.89 0.00 0.00 0.000 8.143 *** End of Report *** MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:25:26 am U26 Page 1 of 1 CO0477 Sample Name:L1667-22 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\12071376\A870144\FC000010.D Injection Date Acq Operator Instrument ^ Dilution 1/21/04 jmiller PC00414 1 7:34:21 PM Seq Line Vial No. Inj. No . Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 10 11 1 5 pi 1 C8 Acid ,X10 Surrogate 329980.06 699878.50 619.25 521.71 7.253 8.124 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 08:43:11 am 0027 Page 1 of 1 C00478 Sample Name:LI667-23 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12071465\A872512\FC000Oil.D Injection Date Acq Operator Instrument Dilution 1/21/04 jmiller PC00414 1 7:49:54 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 11 12 1 5 pi 1 C8 Acid X 1 0 Surrogate 20182.10 479345.44 0.00 337.28 7.268 8.135 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 'CO 0414 Thu, 26. Feb. 2004 08:46:25 am U28 Page 1 of 1 00479 Sample Name:L1667-1 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12071604\A874560\FC000012.D Injection Date : 1/21/04 Acq Operator : jmiller Instrument : PC00414 ^ Dilution :1 8:05:33 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 12 13 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\12071604\A874560\FC000012.D) API-ES, Neg, SIM, Frag: Var 7.256- C8 Acid 50000 - 40000 30000 20000 r 10000- 1 *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\12071604\A874560\FC000012.D) 100000- API-ES, Neg, SIM, Frag: Var 8.129- C10 Surrogate 80000 60000 40000 20000 - Compound Name C8 Acid -- CIO Surrogate " ----1----------------------------------j 1---- !---- -,---- ---- ---- ---- ,---- ]--24 6 1 Area Amount Meas. Ret. T 8 Signal D e s c . mini 389183.53 756620.25 737.65 569.17 7.256 8.129 MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7_:_4_69.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 08:47:31 am 0029 Page 1 of 1 COO480 Sample Name:L1667-2 Sample Info: Data file :C :\HPCHEM\1\DATA\Chemstor\12071793\A876800\FC000013.D Injection Date Acq Operator Instrument Dilution 1/21/04 jmiller PC00414 1 8:21:10 PM Seq Line Vial N o . Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 13 14 1 5 pi 1 C8 Acid --- CIO Surrogate 26401.54 738775.06 12.15 554.24 7.264 8.134 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 08:48:23 am u G0 Page 1 of 1 000453. Sample Name:L1667-4 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12072032\A878976\FC000014.D Injection Date Acg Operator Instrument Dilution 1/21/04 jmiller PC00414 1 8:36:47 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq . Method Analysis Method Last Changed FC8-10.M C :\HPCHEMV1\METHODS\012104.M 2/26/04 08:41:06 am 14 15 1 5 pi 1 C8 Acid -CIO Surrogate 10446.42 722185.81 0.00 540.37 7.257 8.125 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC =468.7:469.7 PC 00414 Thu, 26. Feb. 2004 08:49:10 am U031 Page 1 of 1 000482 Sample Name:LI667-5 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12072196\A881216\FC000015.D 1 C8 Acid -- CIO Surrogate 6282.29 786418.44 0.00 594.09 7.261 8.135 *** End of Report MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 08:49:54 am 0 032 Page 1 of 1 00483 Sample Name:L1667-7 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12072360\A883328\FC000016.D 1 C8 Acid ^ CIO Surrogate 227296.11 701757.56 413.90 523.28 7.255 8.129 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 08:50:58 am UQ33 Page 1 of 1 C004.84 Sample Name:L1667-8 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12072574\A885568\FC000017.D 1 C8 Acid CIO Surrogate 6194.65 736877.69 0.00 552.66 7.261 8.130 *** End of Report *** MSDl 369, EIC =368.7 :369.7 MSDl 469, EIC=468.7 :469.7 PC00414 Thu, 26. Feb. 2004 08:53:52 am 0'64 Page 1 of 1 C 00431 Sample Name :L1667-10 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\12072788\A887744\FC000018.D Injection Date Acq Operator Instrument ... Dilution 1/21/04 jmiller PC00414 1 9:39:16 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : Acq. Method Analysis Method ~ Last Changed FC8-10.M C :\HPCHEMN1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 18 19 1 5 pi 1 C8 Acid - C I O Surrogate 327738.19 705300.25 614.77 526.25 7.256 8.129 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 08:56:36 am UU6 5 Page 1 of 1 c 00496 Sample Name:L1667-ll Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12072994\A889792\FC000019.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/21/04 jmiller PC00414 1 9:54:53 PM Seq Line Vial No. Inj.No. Inj. Vol. : : : : FC8-10.M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 19 20 1 5 pi 1 C8 Acid ..CIO Surrogate 21331.48 785976.25 2.01 593.72 7.254 8.123 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:00:40 am Q36 Page 1 of 1 50487 Sample Name:STD 500 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12073158\A891968\FC000020.D Injection Date Acq Operator Instrument ^ Dilution 1/21/04 jmiller PC00414 1 10:10:29 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method -- Last Changed FC8-10.M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 20 4 1 5 pi 1 C8 Acid ,C10 Surrogate 274769.03 700867.37 508.84 522.54 7.247 8.122 *** End of Report *** MSD1 369, EIC =368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:02:39 am U37 Page 1 of 1 C00 488 Sample Name:solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12073419\A894144\FC000021.D Injection Date Acq Operator Instrument Dilution 1/21/04 jmiller PC00414 1 10:25:58 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEMX1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 21 92 1 5 pi 1 C8 Acid .CIO Surrogate 0.00 0.00 0.00 0.00 0.000 0.000 *** End of Report *** MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 U0S8 09:03:46 am Page 1 of 1 CCO4 8 9 Sample Name:L1667-13 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12073506\A896256\FC000022.D Injection Date Acg Operator Instrument Dilution 1/21/04 jmiller PC00414 1 10:41:30 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : Acq. Method Analysis Method Last Changed F C 8 - 1 0 .M C : \HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 22 21 1 5 ul 1 C8 Acid iJCIO Surrogate 5073.57 694407.75 0.00 517.14 7.248 8.124 *** End of Report *** MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:04:41 am u059 Page 1 of 1 COO490 Sample Name:L1667-14 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12073595\A898368\FC000023.D Injection Date Acq Operator Instrument Dilution : 1/21/04 : jmiller : PC00414 :1 10:57:00 PM Seq Line Vial No. Inj . No. Inj . V o i . : : : : Acq. Method : FC8-10.M Analysis Method : C:\HPCHEM\1\METHODS\012104.M Last Changed : 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 23 22 1 5 pi 1 C8 Acid ,,..CIO Surrogate 2827.02 477008.69 0.00 335.33 7.252 8.122 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 1 PC00414 Thu, 26. Feb. 2004 09:05:29 am U40 Page 1 of 1 C0049 Sample Name:L1667-16 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12073684\A900416\FC000024.D Injection Date Acq Operator Instrument Dilution : 1/21/04 : jmiller : PC00414 :1 11:12:32 PM Seq Line Vial No. Inj . No. Inj . Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 24 23 1 5 pl 1 C8 Acid CIO Surrogate 218205.28 697914.50 395.72 520.07 7.254 8.131 *** End of Report *** MSDl 369, EIC =368.7 :369.7 MSDl 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:06:15 am u U41 Page 1 of 1 C09492 Sample Name :L1667-17 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12073773\A902464\FC000025.D Injection Date Acq Operator Instrument Dilution 1/21/04 jmiller PC00414 1 11:28:09 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 25 24 1 5 ul 1 C8 Acid . CIO Surrogate 4721.38 663417.75 0.00 491.22 7.261 8.132 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 Thu, 26. Feb. 2004 Q42 09:06:55 am Page 1 of 1 COO493 Sample Name :L1667-19 Sample Info : Data file :C :\HPCHEM\l\DATA\Chemstor\12073862\A904640\FC000026.D 1 C8 Acid -CIO Surrogate 5033.35 706496.94 0.00 527.25 7.244 8.122 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:10:31 am u 0 43 Page 1 of 1 to o 494 Sample Name:LI667-20 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\12073951\A907520\FC000027.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/21/04 jmiller PC00414 1 11:59:20 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : FC8-10 .M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 27 26 1 5 pi 1 C8 Acid -CIO Surrogate 3515.82 543472.75 0.00 390.91 7.245 8.118 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:20:44 am u044 Page 1 of 1 C00495 Sample Name:STD 500 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12074040\A913664\FC000028.D Injection Date Acq Operator Instrument r,. Dilution Acq. Method Analysis Method -. Last Changed 1/22/04 jmiller PC00414 1 12:14:56 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : FC8-10.M C :\HPCHEMX1\METHODS\012104.M 2/26/04 08:41:06 am 28 4 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 389, EIC=368.7:369.7 (CHEMSTOR\12074040\A913664\FC000028.D) API-ES, Neg, SIM, Frag: Var 7.263- C8 Acid 35000 - 30000 25000 j 20000 - 15000 - 10000- 5000 ^ 0- 24 *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\12074040\A913664\FC000028.D) 1 l '_ 11 68 API-ES, Neg, SIM, Frag: Var 8.139- C10 Surrogate 80000 - 1 min 60000- 4000020000 - Compound Name C8 Acid CIO Surrogate ! 2 Area 266125.50 686449.06 4 Amount 491.55 510.48 nI 6 1 Meas. Ret. T 1' I _______' _ 1 8 Signal D e s c . min 7.263 8.139 MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 *** End of Report *** I PC00414 Thu, 26. Feb. 2004 09:22:50 am 45 Page 1 of 1 00496 Sample Name :solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12074178\A917504\FC000029.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 1/22/04 jmiller PC00414 1 12:30:24 AM Seq Line Vial No. Inj. No. Inj. Vol. : : : : FC8-10.M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 29 92 1 5 pi 1 C8 Acid f CIO Surrogate 0.00 0.00 0.00 0.00 0.000 0.000 i _____________________________________ *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 t ! `" ! PC00414 Thu, 26. Feb. 2004 09 :23 :54 am uU46 Page 1 of 1 G0 0 4 9 7 Sample Name:STD 50 ppb Sample Info: Data file :C:\HPCHEM\1\DATA\Chemstor\12066508\A989120\FC000030.D 1 C8 Acid -- CIO Surrogate 25612.23 72586.63 10.57 0.00 7.256 8.135 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 i PC00414 Thu, 26. Feb. 2004 09:49:39 am u U4 / Page 1 of 1 G00498 Sample Name:STD 100 ppb c.- Sample Info : ! Data file :C :\HPCHEM\l\DATA\Chemstor\12066543\A991168\FC000031.D 1 C8 Acid 51526.66 62.40 7.257 MSD1 369, EIC =368.7:369.7 j-C10 Surrogate 142940.17 55.95 8.126 MSD1 469, EIC=468.7:469.7 j ------------------------------------------------------------------------------------------------ *** End of Report *** / PC00414 Thu, 26. Feb. 2004 u U48 09:48:21 am Page 1 of 1 c 00499 Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12066595\A993344\FC000032.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 1:17:00 AM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am 32 3 1 5 pi 1 Compound Name C8 Acid CIO Surrogate Area 142331.38 377106.56 Amount 243.99 251.78 Meas. Ret. T Signal Desc. 7.249 8.128 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 09:47:24 am U49 Page 1 of 1 C00500 Sample Name :STD 500 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12074750\A926656\FC000033.D Injection Date Acq Operator Instrument , Dilution 1/22/04 jmiller PC00414 1 1:32:35 AM Seq Line Vial N o . Inj. N o . Inj. Voi. : : : : 33 4 1 5 pi Acq. Method Analysis Method " Last Changed FC8-10.M C :\HPCHEM\1\METHODS\012104 .M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\12074750\A926656\FC000033.D) API-ES, Neg, SIM, Frag: 7ar 35000 ^ t I7.248- C8 Acid i I 30000 -j 25000 ^ 20000 -j 15000 -j 10000^ 5000 -j 0 1' ' 1' 2 1' ! 4 1r *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\12074750\A926656\FC000033.D) L 11 1 6 API-ES, Neg, SIM, Frag: Var i 8 8.129- C10 Surrogate r 80000 - ..... 60000 - 1 ___________ min 40000- 20000 - ,. Compound Name C8 Acid C I O Surrogate i |--------- i --------- ' 2 Area 267827.81 686857.69 AL_ i 1--------- 1--------- 1--------- 1--------- 1--------- 1--------- 1--------- 1--------- --------- '--------- r 4 6 8 min Amount Meas. Ret. T Signal Desc. 494.96 510.82 7.248 8.129 MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** 1 PC00414 Thu, 26. Feb. 2004 09:46:45 am U50 Page 1 of 1 to o 501 Sample Name:STD 750 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12074917\A928704\FC000034.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 1:48:10 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\012104.M 2/26/04 08:41:06 am 34 5 1 5 pi 1 Compound Name C8 Acid CIO Surrogate Area 386648.75 971416.81 Amount 732.58 748.80 Meas. Ret. T Signal Desc. 7.246 8.121 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 *** End of Report *** PC00414 Thu, 26. Feb. 2004 09:45:52 am UU1 Page 1 of 1 G00502 Sample Name:STD 1000 ppb Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\12075058\A930880\FC000035.D 1 C8 Acid -CIO Surrogate 498969.72 1240826.87 957.20 974.10 7.248 8.123 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 09:45 :07 am u U`2 Page 1 of 1 C00503 Sample Name:STD 1500 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\12071288\A867968\FC000036.D Injection Date Acq Operator Instrument Dilution 1/22/04 jmiller PC00414 1 2:19:21 AM Seq Line Vial No. Inj. No. Inj. Vol. : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEMX1\METHODS\01210 4 .M 2/26/04 08:41:06 am LC/MS analysis of perfluorooctanoic acid. 36 7 1 5 pi 1 C8 Acid CIO Surrogate 714769.62 1732664.00 1388.76 1385.42 7.258 8.134 *** End of Report *** MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 Thu, 26. Feb. 2004 08:42:42 am u053 Page 1 of 1 G00504 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 .ogin Login #: 1777................................ Project: P0000419 Project Storage: Company Name: DuPont de Nemours & Co, Inc. Submitted By: Michael D. Aucoin Login Type: Immediate Receipt of Samples Started: T Date Start: 01/19/2004 Due Date: 02/02/2004 Received Date: 01/17/2004 Received By: AM MERMAN, MARK Spread Sample: Label: Project Title/Type: Analysis of PFOA in OVS Tubes / ROUTINE Exygen SD/PI: MILLER, JAMES Login Notes: Conform Notes: ontorm ample: Conform COC: Conform Sample: Conform Request: l rue True True True Package PK0002255 Carton Packages / Containers Mail Date / C ondition S h ip p e r/ ID 1/17/2004 12:00:20PM Package & Contents Uncompromised FEDEX 8363912984560200 Temp. Control/Temp. None 23.3 D irection / Handled By RECEIVED AMMERMAN, MARK Container # C0026135 C0026136 C0026137 C0026138 C0026139 C0026140 C0026141 C0026142 C0026143 C0026144 C0026145 C0026146 C0026147 C0026148 C0026149 C0026150 C0026151 C0026152 C0026153 C0026154 C0026155 C0026156 C0026157 C0026158 G ross W eight 6.3 g 6.3 g 6.3 g 6.1 g 6.1 g 6.1 g 6.2 g 6.2 g 6.2 g 6.2 g 6.2 g 6.2 g 6.3 g 6.3 g 6.3 g 6.2 g 6.2 g 6.2 g 6.2 g 6.2 g 6.2 g 6.3 g 6.3 g 6.3 g pH M iscellaneous Item K ey None 1/19/2004 L o g in .rp t 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 P reservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE ICOC Description U54 Report Version: Dec 22 2003 10:44AM Page 1 of 4 Mfg. Lot Mfg. ID Instance: R0080901 R0080901 Login Sample ID L0001667-0001 L0001667-0002 L0001667-0003 L0001667-0004 L0001667-0005 L0001667-0006 L0001667-0007 L0001667-0008 L0001667-0009 L0001667-0010 L0001667-0011 L0001667-0012 L0001667-0013 L0001667-0014 L0001667-0015 L0001667-0016 L0001667-0017 L0001667-0018 L0001667-0019 L0001667-0020 L0001667-0021 L0001667-0022 L0001667-0023 L0001667-0024 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-E10 A WWK-A-AMS FBLK-E10 B WWK-A-AMSFBLK-E10 C WWK-A-AMS 1-E10 A WWK-A-AMS1-E10 B WWK-A-AMS 1-E10 C WWK-A-AMS2-E10 A WWK-A-AMS2-E10 B WWK-A-AMS2-E10 C WWK-A-AMS3-E10 A WWK-A-AMS3-E10 B WWK-A-AMS3-E10 C WWK-A-AMS4-E10 A WWK-A-AMS4-E10 B WWK-A-AMS4-E10 C WWK-A-AMS5-E10 A WWK-A-AMS5-E10 B WWK-A-AMS5-E10 C WWK-A-AMS6-E10 A WWK-A-AMS6-E10 B WWK-A-AMS6-E10 C Control 1 A Control 1 B Control 1 C Date Sampled Date Received 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/15/2004 01/17/2004 01/17/2004 01/17/2004 01/17/2004 Date Due 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 02/02/2004 1/19/2004 Login.rpt U55 Report Version: Dec 22 2003 10:44AM Page 2 of 4 Instance: 000506 R0080901 R0080901 h L0001667-0001 l Container C0026135/Other/NONE L0001667-0002 Container C0026136/Other/NONE L0001667-0003 Container C0026137/ Other /NONE L0001667-0004 Container C0026138/Other/NONE L0001667-0005 Container C0026139/Other/NONE ,L0001667-0006 Container C0026140/Other/NONE L0001667-0007 Container C0026141 / Other/NONE L0001667-0008 Container C0026142/Other/NONE -L0001667-0009 Container C0026143/Other/NONE L0001667-0010 Container C0026144 / Other / NONE L0001667-0011 Container C0026145 / Other / NONE -L0001667-0012 Container C0026146 / Other / NONE 1/19/2004 Bottles Method Method Method Method Method Method Method Method Method Method Method Method U056 Report Version: Dec 22 2003 10:44AM Instance: R0080901 R0080901 L0001667-0013 r . Container C0026147/ Other /NONE L0001667-0014 Container C0026148/Other/NONE ' L0001667-0015 i Container C0026149 / Other / NONE L0001667-0016 l , Container ! C0026150/Other/NONE ^ L0001667-0017 Container C0026151 / Other /NONE " L0001667-0018 Container C0026152 / Other / NONE L0001667-0019 Container C0026153/Other/NONE ,,L0001667-0020 Container C0026154/Other/NONE L0001667-0021 Container . ~ C0026155/Other/NONE L0001667-0022 Container C0026156/Other/NONE .L0001667-0023 Container C0026157/Other/NONE L0001667-0024 Container * C0026158 / Other / NONE 1/19/2004 Login.rpt Method Method Method Method Method Method Method Method Method Method Method Method u Ub7 Report Version: Dec 22 2003 10:44AM p age 4 of 4 Instance: R0080901 C 0 0 S 0 8 R0080901 Sam plers): AC, SO, RK DuPont Washington Works Air Sampling Program FedEx Airbill #: 836391298456 Event Number E ven t10 cO O' 669842 669908 669901 669890 669796 669865 Hours 0 1 2 3 4 Station # MS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes 0 60 120 180 240 W W K -A -A M S1-E10 W W K -A -A M S2-E10 WWK-A-AMS3-E10 WWK-A-AMS4-E10 WWK-A-AMS5-E10 WWK-A-AMS6-E10 Hours 5 6 7 8 9 1.022 0.997 1.001 1.014 1.006 1.009 Minutes 300 360 420 480 540 li 14-Jan 14-Jan 14-Jan 14-Jan 14-Jan 14-Jan Hours 10 11 12 13 14 S artT fm 0620 0630 0629 0635 0645 0652 Minutes 600 660 720 780 840 Date 15-Jan 0615 15-Jan 0622 15-Jan 0623 15-Jan 0630 15-Jan 0635 15-Jan 0645 Hours Minutes 15 900 16 960 17 1020 18 1080 19 1140 V ib r a tio n {post) Total Minate 0.995 1462 1.003 blank display 0.9703 1473 0.951 1479 1.023 1481 1.023 1483 Hours Minutes 20 1200 21 1260 22 1320 23 1380 24 1440 1447 liters 1413 Itters 1410 liters 1451 liters 1456 liters ao -O SAFER operational: yes yes or no Comments: Total minutes column is the reading from the monitor counter. Pump 2 had a blank display and was not running at sample collection time, due to the GFCI freezing. Replaced the GFCI before next test. 2/9/2004 Page 1 of 2 airdataeventIO 0 k'ijO o 3 Another Calculation #1V47A4L.U42E7t 1451.06246 1453 1175 1502.4745 1506.728 Os LO o o 2/9/2004 Page 2 of 2 airdataeventIO 00055 F RESEARCH PROJECT INFORMATION Client (name & address): CHAIN OF CUSTODY/ANALYSIS REQUEST FORM Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com j Page _ j ___of Project Manager (Name & E-mail Address): ANALYSES REQUESTED u U6 0 ________ \X>-Vqa-v va ksVt laaVoa \ abe YS c. i Phone: ( ~ Fax: Sampler: ^ j R. fi& vkd i_________ Project Name: r\ (Dir $^rAoYi(Y\ VP0ftC&wi RO. #: '/ \ U Quotation #: ^ Please fill out this form com pletely to ensure correct analysis and proper handling of your samples. C o m p osite Num ber of C o ntainers SAMPLE ANALYSIS ExyLIMS# Client Sample Identification Collection Collection Date T im e .<d Wu)^-fmFfcU^-tD WfcJvA-f-ftrnSya-KD lllsU 06lo y 1 MIS y. 0^3 % 63l3 % 630 u)u^-iA'4Vfv\;5-&n vuovL-ft-frons6"i ms I,V 0<p% /Tc-VW 1 LAB USE ONLY \ h rSpecify M atrix Comments \ __ 1____ \ \ \ \7 CHAIN OF CUSTODY Relinquished by Date Time 00/ f OTHER INFORMATION 1 16-$ 1 1 3 0 Ji 4 o / (u*N 3 )0 Cooler ID # --- Cooler Temp. (C) aJ Received by Date Time v //v M lab uiE Only _____.... - \1 L.U k M . U O --------------------------- {tc* * IX *% Ji r * PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: EH Sample results only EH Add case narrative I I Add quality control summary I I Add calibration summary EH Add raw data EH Other ____ G tS Li fut [L , orw.3-0?, J DuPont Washington Works Air Sampling Program Sam plers): AC, SO, RK FedEx Airbill #: 836391298456 Event Number Event 10 Pum p# 669842 669908 669901 669890 669796 669865 Hours 0 1 2 3 4 S ta tio n # AMS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes 0 60 120 180 240 Exygen ID W W k-A-AMS-ElO WWK-A-AMS2-E10 WWK-A-AMS3-E10 WWK-A-AMS4-E10 WWK-A-AMS5-E10 WWK-A-AMS6-E10 Hours 5 6 7 8 9 Calibration (pre) Date start u rne l i i i l S top Time Calibration (post) Total Minutes Total Volume 1.022 14-Jan 0620 15-Jan 0615 0.995 1462 0.997 14-Jan 0630 15-Jan 0622 1.003 blank display 1.001 14-Jan 0629 15-Jan 0623 0.9703 1473 1.014 14-Jan 0635 15-Jan 0630 0.951 1479 1.006 14-Jan 0645 15-Jan 0635 1.023 1481 1.009 14-Jan 0652 15-Jan 0645 1.023 1483 Minutes Hours Minutes Hours Minutes Hours Minutes 300 10 600 15 900 20 1200 360 11 660 16 960 21 1260 420 12 720 17 1020 22 1320 480 13 780 18 1080 23 1380 540 14 840 19 1140 24 1440 SAFER operational: yes yes or no Comments: Total minutes column is the reading from the monitor counter. Pump 2 had a blank display and was not running at sample collection time. 1/15/2004 Page 1 of 2 airdataevent10.xls RESEARCH Precise Research. Proven Results. Sample "Condition Upon Receipt" Form Protocol# Exy.Ren Study # Date & Time Received Condition o f Samples Temporary Storage Location initials & Date Waybill # Cj 6r i / - f i n f i o C>cao 2/ t / - '/ U f i a ,f / 'fic y 2 r*tf(p Comments: May 24, 2002/3 Q.'.WORD'.piocess-luszm'.SumpleConditiononReeeipt.doc u62 3 0 5 8 Research Drive State Colleoe, PA 16801 USA c o o rti T: 8 0 0 .2 8 1 .3 2 1 9 LF: 814.272.1019 ex\ "en.com USARM I Expjres^ \ \ 1 From \\ \ Dfts Q \ [ f Sender's * `A . - V * ** Name w * 1V l Company Address City i . y - \ \ P ^ T v > U 2 Your Internal B illing R e fe re n ti u i i ) ,, .pv/ , 3 To sr JcV/V'iV, 1 Company hi .c.i \ l ,i h ' r f o s f o ( \ t i D s p t/R o o r/S u ite /fto o m Address V\\^ T o " H O L D " a t F e d E x l o c a t io n , p n n t F e d E x a d d r B SSSs . Address rI.v -P \^ C W e ccaatn n o t d e l iv e r t o P . O . b o x e s o r P . 0 . 2 ) P c o d e s . Recipient's Copy 4a Express Package Service Packagesup to 150lbs. D e liv e ry c o m m itm e n t m a y b e la te r tn s o m e a re a s FedEx Priority Overnight * -- r x N e x t b u s in e s s m o rn in g i ] FedEx Standard Overnight L -- 1 N e x t b u s in e s s a fte rn o o n n FedEx First Overnight 1-- 1 E a r lie s t n e x t b u s in e s s t r o m in g d e liv e ry to s e le c t lo c a tio n s f l FedEx 2Day S e c o n d -b u s in e s s d a y , j | FedEx Express Saver T h ird b u sin e s s d ay i ---------------- F e d E x E n v e lo p e r a t e n o t a v a ila b le , M in i m u m c h a r g e : B n e - p o u o d r a t e ------------------- 4b Express Freight Service J- m FedEx t Day Freight** m j- 1 N ext busm ess day I 1 FedEx 20ay Freight *-- ' S e c o n d b u s in e s s d a y * C all f o r C o n firm a tio n ;. f Packaging x Envelope* FedEx Pak* In c lu d e s F e d E x S m a ll P a k, Fed E x la rg e P ak, a n d Fed E x S tu rd y P ak Packages over ISOlbs. D e liv e r/ c o m m itm e n t m a y b e la te r in s o m e a re a s. | j FedEx 3Dav Freight 1-- 1 T h ir d b u s in e s s d a y * D e c la re d v a lu e lim it $500 Other include FedEx address in Section 3. p . HOLD W eekday 1__ I at FedEx Location N o t a v a ila b le fo r Fed E x firs t O verm g tn o e s this shipment contain dangerous goods? Onebox must be checked. -------------- I-- i HOLD S aturday LJ at FedEx Location A v a ila b le o n ly fo r F e d E x P rio rity O v e rn ig h t a n d FedEx 2 0 a y to s e le c t lo c a tio n s 1 Yes i A s p e ra tia ...,. PLJI Yr-es S h ip p e r's D e c la ra tio n D a n g e ro u s G o o d s (in c lu d in g D ry te e l c a n n o t b s s h ip p e d in F e d E x p a c k a g in g . i j Dry Ice `-- 1 D ry Ic e , 9, I I Cargo A ircraft Only 7 Payment B ill to : ,, ~ Sb2inMRecip- vJ (-------"---------- Enter FedExA ccl No. or CreditCard No. b e lo w .--------------- 1 .A c c tN o . T y f Sender j [ Recipient | Third Party Q Credit Card I I Cash/Check 1 w iH b e b ille d . Total Packages T otalW eig h t Tola! D eclared V alue* 1 $ .00 *Qur liability is limited to $100 unless you declare a higher value. See back for details. SignCoauthorize deliverywithout obtainings ig n a t u r a . Total Charges By signing you authorize us to deliver this shipment without obtaining a signature and agree to indemnify and hold us harmless from any resulting claims. Q uestions? V isit our Web site at fedex.com o r c a ll 1 .8 0 0 .G o .F e d E x 6 0 0 .4 6 3 .3 3 3 3 . ,., Rev. D a te 1 Q /W *P a rt# l5 7 8 1 2 * 1 9 9 4 -? !X ri F e d Fx P filN TE O IN U .S A . W C S L Q 2 44b V *. i. c- t c o o D t