Document 10m222kOpKGYbJ6v6RqwwmK5K

Attachment 2 * * 6 -/7 7 6 -e. Analytical Report Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 8 Exygen Research Report No. L0001448 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 eCfrTM> rv> vo 20* v*O* o o o ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 1 of 7 J & 3055;8 Research Drive J r State College, PA 16801, USA :7 V0 0 0 3 2 7 T: 800.281.3219 1 F: 814.272.1019 exygen.com Summary Seven solid media samples were received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. The media represent samples of air collected on OVS tubes. Please see Table 1 for a completed listing of samples received and field air volumes collected. Sample WWK-A-AMS6-E8 had sampler problems during collection. No results are reported for this sample. The samples were analyzed for Perfluorooctanoic Acid (C8 Acid) using liquid chromatography / mass spectrometry (LCMS). The method employed is entitled "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in OVS Airtubes by LCMS" (James Miller, Exygen Research, February 17, 2003). The OVS tubes were separated into three fractions for specific fluorochemical analysis. Fraction A consisted of the filter, backing material and plastic ring. Fraction B contained the first bed of XAD resin and the PUF backing. Fraction C contained the second bed of XAD resin and PUF backing. Fractions A and B were extracted with 1 mL of methanol. Fraction C was not analyzed but saved for possible future analysis. Perfluorodecanoic Acid (CIO Acid) was added as a surrogate spike to each fraction prior to extraction. Instrument operating conditions can be found at the beginning of each analytical run. Raw instrument data is given in Appendix A. Chain-of-custody information can be found in Appendix B. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 2 of 7 000338 Results Summary Request # Air Volume Sampled (L) C8 Acid (mq/m3) WWK-A-AMS1-E8 A WWK-A-AMS1-E8 B WWK-A-AMS1-E8 C WWK-A-AMS1-E8 (Total) 1666 1666 1666 < 0.00006 < 0.00006 NA <0.00012 WWK-A-AMS2-E8 A WWK-A-AMS2-E8 B WWK-A-AMS2-E8 C WWK-A-AMS2-E8 (Total) 1461 1461 1461 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS3-E8 A WWK-A-AMS3-E8 B WWK-A-EMS3-E8 C WWK-A-EMS3-E8 (Total) 1400 1400 1400 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS4-E8 A WWK-A-AMS4-E8B WWK-A-AMS4-E8 C WWK-A-AMS4-E8 (Total) 1521 1521 1521 < 0.00007 < 0.00007 NA <0.00014 WWK-A-AMS5-E8 A WWK-A-AMS5-E8 B WWK-A-AMS5-E8 C WWK-A AMS5-E8 (Total) 1431 1431 1431 < 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 CC0329 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) 435 C8 Acid (percent recovery 87 Blanks Request # WWK-A-AMSFBLK-E8 A WWK-A-AMSFBLK-E8 B Voi. Of Air (L) 0 0 C8 Acid (uq/fraction) <0.10 <0.10 COO330 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 4 of 7 Surrogates A surrogate spike (CIO Acid) was added to all OVS tubes to give a final concentration of 500 ppb in the extract. Surrogate spike recoveries are given in the following table. There are no set criteria for surrogate spike recoveries. Advisory ranges are 75-125%. Sample # WWK-A-AMSFBLK-E8 A WWK-A-AMSFBLK-E8 B WWK-A-AMS1-E8 A WWK-A-AMS 1-E8 B WWK-A-AMS2-E8 A WWK-A-AMS2-E8 B WWK-A-AMS3-E8 A WWK-A-AMS3-E8 B WWK-A-AMS4-E8 A WWK-A-AMS4-E8 B WWK-A-AMS5-E8 A WWK-A-AMS5-E8 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) 454 318 434 253 475 283 502 269 447 373 447 394 437 278 * Surrogate recovery outside of advisory range. Percent Recovery (%) 91 64* 87 51* 95 57* 100 54* 89 75 89 79 87 56* ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 000331 Calculations Request # WWK-A-AMSFBLK-E8 A WWK-A-AMSFBLK-E8 B WWK-A-AMS1-E8 A WWK-A-AMS1-E8 B WWK-A-AMS2-E8 A WWK-A-AMS2-E8 B WWK-A-AMS3-E8 A WWK-A-AMS3-E8 B WWK-A-AMS4-E8 A WWK-A-AMS4-E8 B WWK-A-AMS5-E8 A WWK-A-AMS5-E8 B Control Spike A Control Spike B Vol. Of Air (L) 0 0 1666 1666 1461 1461 1400 1400 1521 1521 1431 1431 0 0 C8 Acid (raw-ppb) < 10 <10 <10 <10 31 <10 27 <10 53 <10 71 <10 435 <10 C8 Acid (ug/fraction) <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 0.44 <0.10 C8 Acid (mg/m3) < 0.00006 < 0.00006 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 * 00033 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 7 Example Calculation For sample WWK-A-AMS2-E8 A C8 Acid, = [130100ngL/)m] l of C8 Acid x (1 ml) x (1 ug /1000 ng) x (1 mg /1000 ug) ] / [(1461 L) x (1 m3 / = < 0.00007 mg / m3 Signatures ^ 1 h <\ Date John M. Flaherty, Vice President Other Lab Members Contributing to Data James Miller Date ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 7 GC0333 000334 jUd Table 1. Login Information / Field Data Sample ID Exygen Lab ID Date Received Description WWK-A-AMSFBLK-E8 A WWK-A-AMSFBLK-E8 B WWK-A-AMSFBLK-E8 C WWK-A-AMS1-E8 A WWK-A-AMS1-E8B WWK-A-AMS1-E8 C WWK-A-AMS2-E8 A W WK-A-AMS2-E8B WWK--AMS2-E8 C WWK-A-AMS3-E8 A WWK-A-AMS3-E8 B WWK-A-AMS3-E8 C WWK-A-AMS4-E8 A WWK-A AMS4-E8 B WWK-A-AMS4-E8 C WWK-A-AMS5-E8 A WWK-A-AMS5-E8 B WWK-A AMS5-E8 C Control Spike A Control Spike B Control Spike C L0001448-1 L0001448-2 L0001448-3 L0001448-4 L0001448-5 L0001448-6 L0001448-7 L0001448-8 L0001448-9 L0001448-10 L0001448-11 L0001448-12 L0001448-13 L0001448-14 L0001448-15 L0001448-16 L0001448-17 L0001448-18 L0001448-19 L0001448-20 L0001448-21 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 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 1666 1666 1666 1461 1461 1461 1400 1400 1400 1521 1521 1521 1431 1431 1431 0 0 0 00335 Table 2. Chain of Custody Sample ID WWK-A-AMSFBLK-E8 A WWK-A-AMSFBLK-E8 B WWK-A-AMSFBLK-E8 C WWK-A-AMS1-E8 A WWK-A-AMS1-E8 B WWK-A-AMS1-E8C WWK-A-AMS2-E8 A WWK-A-AMS2-E8B WWK-A-AMS2-E8 C WWK-A-AMS3-E8 A WWK-A-AMS3-E8 B WWK-A-AMS3-E8 C WWK-A-AMS4-E8 A WWK-A AMS4-E8 B WWK-A-AMS4-E8 C WWK-A-AMS5-E8 A WWK-A-AMS5-E8 B WWK-A AMS5-E8 C C ontrol S pike A Control Spike B Control Spike C Date Collected 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 12/12/03 NA NA NA Date Received at Exygen 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 12/13/03 Date Extracted by Exygen 12/30/03 12/30/03 NA 12/30/03 12/30/03 NA 12/30/03 12/30/03 NA 12/30/03 12/30/03 NA 12/30/03 12/30/03 NA 12/30/03 12/30/03 NA 12/30/03 12/30/03 NA Date Analyzed by Exygen 12/30-12/31/03 12/30-12/31/03 NA 12/30 -12/31/03 12/30-12/31/03 NA 12/30-12/31/03 12/30-12/31/03 NA 12/30-12/31/03 12/30-12/31/03 NA 12/30-12/31/03 12/30-12/31/03 NA 12/30 -12/31/03 12/30-12/31/03 NA 12/30 -12/31/03 12/30 -12/31/03 NA ,, Sample Name:L0001448-19 Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11772125\A136704\FC000010.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 7:42:29 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 10 11 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1772125\A136704\FC000010.D) API-ES, Neg, SIM, Frag: Var 20000 7.264- C8 Acid, 17500 -j 15000 12500 -J 10000 7500- 5000 2500 0- 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1772125\A136704\FC000010.D) API-ES, Neg, SIM, Frag: Var 25000 - 8.073- C10 Surrogate! min 20000 - 15000- 10000- 5000- .1 1 -- 1--- 1--- 1-- 24 Compound Amount (ng/mL) R.T. Area 8 Acid 435.43 10 Surrogat 437.44 7.264 8.073 165161 205556 i--- !--- 1--- 1--- 1--- 1--- 1--- 1--- r 6 8 min Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 i na! d p nn 1 *** End of Report *** 0028 C onnyi no .1n .eo 000354 ANALYTICAL DATA REVIEW SHEET LC/MS Analyst 1^-. L^U\cr- Jo in m fU lc/ch/ Reviewed by Signature/Date ? / /n Signature/Date' U /rt U01U Sequence : C :\HPCHEM\1\SEQUENCE\123003.S Sequence Table: Method and Injection Info Part: Line Location SampleName Method Inj SampleType InjVolume DataFile 1 Vial 1 2 Vial 1 3 Vial 2 4 Vial 3 5 Vial 4 6 Vial 5 7 Vial 6 8 Vial 7 9 Vial 92 10 Vial 11 11 Vial 12 12 Vial 13 13 Vial 14 14 Vial 15 15 Vial 16 16 Vial 17 17 Vial 18 18 Vial 19 19 Vial 20 20 Vial 4 21 Vial 92 22 Vial 21 23 Vial 22 24 Vial 23 25 Vial 24 26 Vial 4 27 Vial 92 28 Vial 1 29 Vial 2 30 Vial 3 31 Vial 4 32 Vial 5 33 Vial 6 34 Vial 7 STD 50 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb solvent blank L0001448-19 L00014 48-20 L0001448-1 L0001448-2 L0001448-4 L0001448-5 L0001448-7 L0001448-8 L0001448-10 L0001448-11 STD 500 ppb solvent blank L0001448-13 L00014 48-14 L0001448-16 L0001448-17 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 SampleName Method CalLev Update RF Update RT Interval 2 Vial 1 3 Vial 2 4 Vial 3 5 Vial 4 6 Vial 5 7 Vial 6 8 Vial 7 28 Vial 1 29 Vial 2 30 Vial 3 31 Vial 4 32 Vial 5 33 Vial 6 34 Vial 7 STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 1500 ppb FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 FC8-10 1 Replace Average 2 Replace Average 3 Replace Average 4 Replace Average 5 Replace Average 6 Replace Average 7 Replace Average 1 Average Average 2 Average Average 3 Average Average 4 Average Average 5 Average Average 6 Average Average 7 Average Average -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 -2 XMS5 12/30/03 5:24:45 PM jmiller - w i i Page x of 000337 LC/MS SYSTEM AND OPERATING CONDITIONS Client: Dupont EXYGEN STUDY: LOOQ1448 Instrument: Hewlett-Packard 1100 LC/MSD (LC/MS 5) API-ES Interface - Negative SIM mode Nitrogen: 10 L/min at 300C Fragmentor: Variable; Vcap: 3500V Computer: Hewlett-Packard Kayak workstation Software: Microsoft Windows NT 4.0 Agilent ChemStation Version A.08.03 HPLC Equipment: HP G1322A Solvent Degasser HP G1311A Quaternary Pump HP G1313A Autosampler HP G1316A Column Thermostat HP G1946 MSD HPLC Column: Column Temp.: Mobile Phase (A): Mobile Phase (B): Thermo Hypersil-Keystone Betasil C18, 30 x 2.0 mm x 3pm 35 C 2mM Ammonium acetate in OmniSolv Water HPLC grade Methanol Time %A 0.0 70 6.0 10 10.0 10 10.0 STOP Post Time = 4 min. Total run time = 14 min. Flow Rate: 0.3 mL/min Injected Volume: 5 pL %B 30 90 90 STOP Page 1 of 2 0 01 2 000338 Ions monitored: Analyte C8 Acid (PFOA) C10 Surrogate Ion (m / z ) 369 469 Extraction Date: December 30, 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 0013 C00339 G1946: API_ES Negative mode Instrument : LCMS5 Page 1 of 3 Tue Dec 16 12:15:46 2003 . C :\HPCHSM\i\I94 6TUNE\ATUNES.TUN Scan: 50.00 - 3000.00 Samples: 8 Thresh: 0 Step: 0.10 29501 peaks Base: 2234.15 Abundance: 335232 F Raw,Gauss 0.3 100 n 80 - 60 - 40 - 20 - L----f l ~ 1-- r1--- ,-- r-L-rL 500 1000 1500 .r-^-- rL 2000 2500 m/z gf 112.96 601.99 1034.05 1634.05 2234.15 Abund 243712 32600 147776 307520 335232 Rel Abund 100.00 13.38 60.64 .126.18 137.55 Iso m/z 113.99 602.95 1035.05 1635.05 2235.15 Iso Abund Iso Ratio 4075 1.67 2771 8.50 32352 21.89 117312 38.15 156608 46.72 urn 4 COO340 Instrument : LCMS5 TTuiTT3c~T6~7r2Tr5T~6'~~2r(JO3 Gl946: API_ES Negative mode Page 2 of 3 C :\H?CHEM\1\1946TNE\ATUNES.TUN Mode: API--ES Polarity: NEG Fragment Skim2 Lensl Lens2 Iris Gain VAR WidthGain 1031 6.0 WidthOffs VAR -3.8 MassGain 93.65 14 MassOffs 0.516 -8 Energy 5.0 OpolPeak 300 OpolKnee 315 2.0 QuadDC 0.00 EMV VCap Status: CapCur ChamCur 1788 Samples 8 4000 Averages 1 StepSize 0.10 39 DryingGas 7.0 0.51 Gas Temp 300 Quad Temp 99 Neb Pres 15 Instrument LCMS5 Tue Dec 16 12:15:46 2003 Gl 946: API_ES Negative mode Page 3 of 3 C:\HPCHEM\1\1946TNE\ATNES.TUM Width Offset 0 Dynamic Parameter Ramp -20 - -40 - -60 -80 - -100 - -120 - -140 -160 I I-- 1-- 1-- r-- ---- 1---- ^-- r_ I-- 1 500 1000 1500 2000 2500 3000 Mass 112.99 1633.95 Setting -159.00 -159.00 Mass 601.98 2233.91 Setting -159.00 -159.00 Mass 1033.99 Setting -159.00 01 6 000342 Method C: \HPCHEM\1\METHODSU23003F.M Calibration Table Calib. Data Modified Monday, January 05, 2004 2:58:05 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 11 _ 7.253 1 1 [ppb] I1 50.00000 2.15119e4 2 100.00000 4.22031e4 3 250.00000 9.80112e4 4 500.00000 1.88180e5 5 750.00000 2.86941e5 6 1000.00000 3.79365e5 7 1500.00000 5.35063e5 8.078 2 1 50.00000 2.87544e4 2 100.00000 5.27461e4 3 250.00000 1.20893e5 4 500.00000 2.31809e5 5 750.00000 3.55658e5 6 1000.00000 4.67572e5 7 1500.00000 6.64232e5 Amt/Area 11 2.32430e-3 2.36949e-3 2.55073e-3 2.65702e-3 2.61377e-3 2.63598e-3 2.80341e-3 1.73886e-3 1.89587e-3 2.06795e-3 2.15695e-3 2.10877e-3 2.13871e-3 2 .25825e-3 Ref Grp Name 1 C8 Acid 1 CIO Surrogate More compound-specific settings: Compound: C8 Acid Time Window From 7.081 min To 8.081 min Compound: CIO Surrogate Time Window : From 7.882 min To 8.687 min Peak Sum Table ***No Entries in table*** C00414 1/5/04 3:10:02 PM jmiller 0 0 'I 7 0 0 0 3 4 3 Page 1 of 2 Method C:\HPCHEM\1\METHODS\123003F.M Calibration Curves C8 Acid at exp. RT: 7.253 MSD1 369, EIC=368.7:369.7 Correlation: 0.99908 Residual Std. Dev.: 8901.73779 Formula: y = mx + b m: 358.56812 b: 9031.31024 x: Amount[ppb] y: Area CIO Surrogate at exp. RT: 8.078 MSD1 469, EIC=468.7 :469.7 Correlation: 0.99927 Residual Std. Dev.: 9856.02722 Formula: y = mx + b m: 443.74955 b: 11443.44287 x: Amount[ppb] y : Area C00414 1/5/04 3:10:02 PM jmiller uQ'l 8 0 0 0 3 4 4 Page 2 of 2 Sample Name:STD 50 ppb Sample Info:Warm Up Data file :C:\HPCHEM\l\DATA\Chemstor\11775384\A158656\FC000001.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 5:27:24 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODSU23003F.M 1/5/04 02:58:26 pm 1 1 1 1 5 pi Compound Amount (ng/mL) R.T. '8 Acid 36.46 :10 Surrogat 30.12 7.289 8.081 Area 22103 24809 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 03:20:52 pm U01 9 Page 1 of 1 000345 Sample Name:STD 50 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11775962\A177280\FC000002.D Injection Date Acq Operator Instrument ,.. Dilution 12/30/03 jmiller PC00414 1 5:42:25 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 2 1 1 5 pi Acq. Method Analysis Method .- Last Changed FC8-10.M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1775962\A177280\FC000002.D) API-ES, Neg, SIM, Frag: Var 2500- 7.268 - C8 Acid, 2000 1500- 1000- 500- L U. *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1775962\A177280\FC000002.D) API-ES, Neg, SIM, Frag: Var 3000- 8.070- C10 Surrogate, min 2500- 2000- 1500- 1000- 500- 11111 24 Compound Amount (ng/mL) R.T. ra8 Acid 30.23 10 Surrogat 28.29 7.268 8.070 Area 19869 23998 1 i--- 1--- ,--- ,--- ,--- 6 8 min Signal MSDl 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 03 :32 :54 pm 0020 Page 1 of 1 000346 Sample Name:STD 100 ppb Sample Info : 1 Data file :C:\HPCHEMU\DATA\Chemstor\11776021\Al79072\FC000003.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 5:57:26 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 3 2 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\123003F .M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1776021W179072\FC000003.D) API-ES, Neg, SIM, Frag: Var 7.285 - C8 Acid 5000- 4000- 3000- 2000- -- 1000- 10 - . r . -j . r I" f ''! 246 l1 81 r 1 1 1 r min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1776021\A179072\FC000003.D) API-ES, Neg, SIM, Frag: Var 8.087- C10 Surrogate 6000 ^ 5000- 4000 ^ 3000 2000 71000 o- Compound *^r1 i 2 Amount (ng/mL) ''! 4 R.T. 8 Acid 94.45 10 Surrogat 92.39 7.285 8.087 ' 1 1 1 1 1 1 .1 . 1 1 1--- 1--- r 6 8 min Area Signal 42898 52442 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 03:33:36 pm 0 021 Page 1 of 1 000347 Sample Name:STD 250 ppb Sample Info: 1 Data file :C:\HPCHEM\1\DATA\Chemstor\11776080\A180928\FC000004.D Injection Date Acq Operator Instrument * Dilution Acq. Method Analysis Method - Last Changed 12/30/03 jmiller PC00414 1 6:12:28 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : FC8-10.M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm 4 3 1 5 pl LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1776080\A180928\FC000004.D) API-ES, Neg, SIM, Frag: Var 12000- 7.268- C8 Acid 10000- 8000- 6000- 4000- 2000- -- .. r, 'r i i I 2 46 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1776080\A180928\FC000004.D) i 11r I 1 > 8 API-ES, Neg, SIM, Frag: Var j min 1 8.078 - C10 Surrogatei 12000 6000 4000 l -1--------------, i i ] <---------------' '--------------- 1------------------------------1--------------- 1---------------1--------------- '--------------- --------------- '--------------- 1--------------- '-- -- --------------- '----------------r Compound Amount (ng/mL) R.T. **8 Acid 247.34 10 Surrogat 247.82 7 268 8 .078 Area 97718 121415 Signal MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 03:34:18 pm 022 Page 1 of 1 C00348 Sample Name:STD 500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11772709\A149440\FC000005.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 6:27:28 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 5 4 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1772709\A149440\FC000005.D) API-ES, Neg, SIM, Frag: Var 7.269- C8 Acid 20000 - 15000- 10000- 5000- 8 *MSD1 469, EIC=469.7:469.7 (CHEMSTORM 1772709\A149440\FC000005.D) API-ES, Neg, SIM, Frag: Var 30000 - 8.096- C10 Surrogate* min 25000 - 20000 - 15000- 10000- 5000- Compound Amount (ng/mL) R.T. ~'8 Acid 498.67 10 Surrogat 496.86 7.269 8.096 Area 187840 231927 Signal MSD1 369, EIC=3 68.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** 0023 Mon, 5. Jan. 2004 03:16:11 pm Page 1 of 1 000349 Sample Name:STD 750 ppb Sample Info : 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11776139\Al82720\FC000006.D Injection Date Acq Operator Instrument -- Dilution 12/30/03 jmiller PC00414 1 6:42:29 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEMN1\METHODSU23003F. M 1/5/04 02:58:26 pm 6 5 1 5 pi LC/MS analysis of perfluorooctanoic acid. -- *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1776139\A182720\FC000006.D) API-ES, Neg, SIM, Frag: Var 1 35000 - 7.263- C8 Add -- 30000 -j 25000 j 20000 15000 -j 10000j t- * socc .................................. _ _ J er , , | i - ' r 11i 1 24 6 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1776139\A182720\FC000006.D) l i r 11r 8 mi n API-ES, Neg, SIM, Frag: Var 45000 / 8.073- C10 Surrogate 40000 / 35000 - -- 30000 -I 25000 - 20000 i 15000- 10000- 5000 -j u ' ' ' i ' T 1X 24 1n 6 1 u `1 8 ' '' 1) min Compound Amount (ng/mL) R.T. Area Signal 8 Acid 761.96 10 Surrogat 763.35 7.263 8.073 282245 350179 MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 03:34:39 pm 24 Page 1 of 1 000350 Sample Name:STD 1000 ppb Sample Info : 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11772782\A151232\FC000007.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 6:57:31 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : 7 6 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. ` MSD1 369, EIC=368.7:369.7 (CHEMSTORY11772782\A151232\FC000007.D) API-ES, Neg, SIM, Frag: Var 2250 -; 7.274- C8 Add 2000 1750- }------- S S 3 wm 1500 _. JL 1250 BTXcJai** 1000^ 750/ K M Ihf#tfafs/ft*at#ei***. W * 500 / 250- 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM1772782\A151232\FC000007.D) API-ES, Neg, SIM, Frag: Var 8.083- C10 Surrogate 2500- 2000- 1500- 1000- 500- Compound Amount (ng/mL) R.T. '8 Acid 24.97 10 Surrogat 24.50 7.274 8.083 Area 17985 22315 o o min Signal MSD1 369, EIC=3 68.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 25 03:17:31 pm Page 1 of 1 00035 Sample Name:STD 1500 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11776198\A184576\FC000008.D Injection Date Acg Operator Instrument Dilution Acg. Method Analysis Method *~ Last Changed 12/30/03 jmiller PC00414 1 7:12:29 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : FC8-10.M C:\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm 8 7 1 5 pi LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1776198\A184576\FC000008.D) API-ES, Neg SIM, Frag: Var 7.286- C8 Add 60000 -j 50000 ^ r - 40000 -j 30000 ^ 20000 ^ 10000^ ' ____ . J I , , , , . r r I 1 24 1 1 1 1 1 r 1 1 1------------ r 6 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 177619B\A184576\FC000008.D) API-ES, Neg, SIM, Frag: Var 80000 j 8.099 - C10 Surrogate 70000 ~ 60000 50000 -j 40000 30000 r 20000 H 10000^ ' ' ' i^ 2 r 1 1 ' 1 1111 46 1) l r 1111 8 min Compound Amount (ng/mL) R.T. Area Signal "8 Acid 1492.19 '10 Surrogat 1506.15 7.286 8.099 544084 679798 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 u 026 03:35:23 pm Page 1 of 1 G00352 Sample Name :solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11772053\Al34976\FC000009.D 1 8 Acid 0.00 10 Surrogat 0.00 7.294 0.000 294 0 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 027 03 :10 :22 pm Page 1 of 1 000353 Sample Name:L0001448-20 Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11775443\A160512\FC000011.D Injection Date Acq Operator Instrument Dilution Acq. Method Analysis Method Last Changed 12/30/03 jmiller PC00414 1 7:57:28 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : FC8-10.M C:\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm 11 12 1 5 pi LC/MS analysis of perfluorooctanoic acid. MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1775443\A160512\FC000011.D) API-ES, Neg, SIM, Frag: Var 7.271 - C8 Acid 1000 800- 600 400- 200- MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1775443\A160512\FC000011,D) API-ES, Neg, SIM, Frag: Var 16000 8.077- C10 Surrogate* 14000 12000 10000 8000 6000 4000 2000 H 0 Compound Amount (ng/mL) R.T. "".8 Acid 0.00 .'10 Surrogat 277.89 7.271 8.077 Area 7815 134755 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 I PC00414 *** End of Report *** U02y Mon, 5. Jan. 2004 03:21:37 pm Page 1 of 1 C00355 Sample Name:L0001448-l Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11775502\A162368\FC000012.D 1 "*8 Acid 0.00 '10 Surrogat 454.27 7.292 8.099 869 213026 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 [ PC00414 *** End of Report *** Mon, 5. Jan. 2004 B 03:23:28 pm Page 1 of 1 000356 Sample N a m e :L0001448-2 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11775560\Al64224\FC000013.D 1 -8 Acid 0.00 10 Surrogat 318.28 0.000 8.098 0 152681 MSD1 369, EIC=368.7 :369.7 MSD1 469, EIC=468.7:469.7 i PC 00414 *** End of Report *** Mon, 5. Jan. 2004 o03 I 03:24:18 pm Page 1 of 1 000357 Sample Name:L0001448-4 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11772198\A138432\FC000014.D 1 8 Acid 0.00 10 Surrogat 434.27 7.271 8.080 3160 204150 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 U32 03:11:33 pm Page 1 of 1 C00358 Sample Name :LO001448-5 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11775617\A166080\FC000015.D Injection Date Acq Operator Instrument -- Dilution 12/30/03 jmiller PC00414 1 8:57:28 PM Seq Line Vial No. Inj . No. Inj. Voi. : : : : Acq. Method Analysis Method *' Last Changed FC8-10 .M C :\HPCHEMX1\METHODS\123003F. M 1/5/04 02:58:26 pm 1 15 16 1 5 pi Compound Amount (ng/mL) R.T. n8 Acid 0.00 0.000 10 Surrogat 252.71 8.076 Area 0 123582 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** 0033 Mon, 5. Jan. 2004 03:26:02 pm Page 1 of 1 000359 Sample Name:LO001448-7 Sample Info : 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11772271\Al40288\FC000016.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 9:12:25 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 16 17 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. MSD1 369, EIC=368.7:369.7 (CHEMSTORM1772271 \A140288\FC000016.D) API-ES, Neg, SIM, Frag: Var 2250 -] 2000 7.274- C8 Acic 1750 1500 -j 1250 1000 750 500 250 --i------------r-- 4 *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\11772271\A140288\FC000016.D) API-ES, Neg, SIM, Frag: Var 8.091 - C10 Surrogate. 25000 - 20000 - 15000- 10000- 5000- ---j--- ,--- .--- r 24 Compound Amount (ng/mL) R.T. Area "8 Acid 31.13 :10 Surrogat 475.46 7.274 8.091 20195 222430 i11 6 i--- 1 1 ' r 8 min Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 -- ..... PC00414 *** End of Report *** Mon, 5. Jan. 2004 03:12:15 pm 0034 Page 1 of 1 000360 Sample Name:L0001448-8 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11775675\A167936\FC000017.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmi H e r PC00414 1 9:27:24 PM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm 1 17 18 1 5 pi Compound Amount (ng/mL) R.T. *8 Acid 0.00 10 Surrogat 283.83 7.283 8.097 Area 284 137394 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 0035 03:27:27 pm Page 1 of 1 000363. Sample Name :L0001448-10 Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11772344\A142208\FC000018.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 9:42:25 PM Seq Line Vial No. Inj . N o . Inj. Voi. : : : : 18 19 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1772344\A142208\FC000018.D) API-ES, Neg, SIM, Frag: Var 2250 7.274- C8 Acid 2000 1750 1500 1250 1000 750 500250- *MSD1 469, EIC=468.7:469.7 (CHEMSTOR\11772344\A142208\FC000018.D) API-ES, Neg, SIM, Frag: Var 30000 8.088 - C10 Surrogate. 25000 - 20000 - 15000- 10000- 5000- Compound Amount (ng/mL) R.T. *8 Acid 26.57 10 Surrogat 502.38 7.274 8.088 Area 18559 234372 Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** 0036 Mon, 5. Jan. 2004 03:13:17 pm Page 1 of 1 C00362 Sample Name:L0001448-ll Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11775733\A169664\FC000019.D 1 -- 8 Acid 0.00 10 Surrogat 268.58 7.274 8.079 322 130625 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 P i PC00414 *** End of Report *** Mon, 5. Jan. 2004 u 03 7 03:28:21 pm Page 1 of 1 000363 Sample Name:STD 500 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11772417\Al43936\FC000020.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 10:12:24 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\123003F.M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\11772417\A143936\FC000020.D) API-ES, Neg, SIM, Frag: Var 7.271 - C8 Acic 20000 ... 15000- 10000- 5000- _ A__o - . .. J ' -CO -CM 1i 11i 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM1772417\A143936\FC000020.D) API-ES, Neg, SIM, Frag: Var 30000 ^ 8.095- C10 Surrogate 25000 - 20000 : 15000- 10000 ^ - , 5000 ^ o------ !------- ,------- 1------- | I ------- 1 > I -, 2 4 Compound Amount (ng/mL) R.T. *8 Acid 514.12 '10 Surrogat 510.73 7.271 8.095 ' ' Area 193378 238078 __J 1_______ ' I 1 '^ I , . i 6 8 min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 - , PC00414 *** End of Report *** Mon, 5. Jan. 2004 0038 03 :13 :52 pm Page 1 of 1 000364 Sample Name :solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\11775790\A171520\FC000021.D Injection Date Acg Operator Instrument Dilution 12/30/03 jmiller PC00414 1 10:27:27 PM Seg Line Vial No. Inj.No. Inj. Vol. : : : : Acg. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. 1 21 92 1 5 pi *8 Acid 0.00 HO Surrogat 0.00 0.000 0.000 0 0 MSD1 369, EIC=3 68.7:3 69.7 MSD1 469, EIC=468.7:469.7 I L PC00414 *** End of Report *** Mon, 5. Jan. 2004 0 Q3 9 03:30:14 pm Page 1 of 1 000365 Sample Name :L0001448-13 Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11772490\A145664\FC000022.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 10:42:25 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 22 21 1 5 pi Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1772490\A145664\FC000022.D) API-ES, Neg, SIM, Frag: Var 3000 7.269- C8 Acid 2500- 2000 1500 1000- 500- 8 MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1772490\A145664\FC000022.D) API-ES, Neg, SIM, Frag: Var 25000 - 8.090- C10 Surrogate, 20000 - 15000- 10000 5000- Compound Amount (ng/mL) R.T. *8 Acid 53.46 10 Surrogat 447.27 7.269 8.090 Area 28200 209917 min Signal MSD1 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. J a n . 2004 U40 03:14:42 pm Page 1 of 1 000366 Sample Name:L0001448-14 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11775847\Al73696\FC000023.D 1 I 3 Acid 0.00 L0 Surrogat 372.60 7.262 8.079 302 176786 MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 0041 03:31:16 pm Page 1 of 1 00367 ,,, Sample Name:L0001448-16 Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11772563\A147584\FC000024.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 11:12:23 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm 24 23 1 5 pi LC/MS analysis of perfluorooctanoic acid. MSD1 369, EIC=368.7:369.7 (CHEMSTORM1772563\A147584\FC000024.D) API-ES, Neg, SIM, Frag: Var 4000 7.263- C8 Acid, 3500- 3000 2500 2000-1 1500 1000 500 0 --I-------1~ 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1772563\A147584\FC000024.D) API-ES, Neg, SIM, Frag: Var 25000 - 8.089- C10 Surrogate, 20000 - 15000- 10000- 5000- Compound Amount (ng/mL) R.T. 8 Acid 70.76 10 Surrogat 446.79 7.263 8.089 Area 34404 209707 Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** 0042 Mon, 5. Jan. 2004 03:15:32 pm Page 1 of 1 000368 Sample Name:L0001448-17 Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11773039\Al56928\FC000025.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmiller PC00414 1 11:27:24 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : : 25 24 1 5 pi Acq. Method Analysis Method * Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\123003F.M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1773039\A156928\FC000025.D) API-ES, Neg, SIM, Frag: Var '------- 1------- 1 1------- 1 ' 1------- 1 1 1 1 1 1 1 r 246 8 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1773039\A156928\FC000025.D) API-ES, Neg, SIM, Frag: Var 18000 -7 8.101 - C10 Surrogate min 16000- 14000 j 12000 j 10000 j 8000 - 6000 -j 4000 2000 j 0- Aa, .. J ------ ,------- ------- ------- 1------- ------- 1------- 1------- 1------- ------- '------- 1 i------- 1-- ' ' I i i i I 2 4 6 8 min Compound Amount (ng/mL) R.T. Area Signal `*8 Acid 0.00 10 Surrogat 294.14 7.291 8.101 516 141968 MSD1 369, EIC=3 68.7 :369.7 MSDl 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 45 03:19:57 pm Page 1 of 1 000369 Sample Name:STD 500 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11772980\Al55072\FC000026.D Injection Date Acq Operator Instrument Dilution 12/30/03 jmil1er PC00414 1 11:42 :25 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 26 4 5 ]i1l Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1772980\A155072\FC000026.D) API-ES, Neg, SIM, Frag: Var 7.264 -C8 Acic 20000 - 15000- 10000- 5000- o- I iII1111 11 246 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1772980\A155072\FC000026.D) dA__ ' T r . if 8 min API-ES, Neg, SIM, Frag: Var 8.085 - C10 Surrogate 25000 : 20000 - 15000- 10000 - ** 5000^ . o- iiiii' 2 1 4 Compound Amount (ng/mL) R.T. Area "'8 Acid 507.95 10 Surrogat 507.21 7.264 8.085 191167 236518 1' 6 ____ u A . . . .'. . .... 'I'''I 8 min Signal MSDl 369, EIC= 368.7:369.7 MSD1 469 , EIC= 468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 u U4 4 03:18:50 pm Page 1 of 1 000370 Sample Name:solvent blank Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\11775905\A175424\FC000027.D Injection Date Acq Operator Instrument '* Dilution 12/30/03 jmiller PC00414 1 11:57:25 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C :\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. 1 27 92 1 5 pi 3 Acid 0.00 10 Surrogat 0.00 0.000 0.000 0 0 MSDl 369, EIC=368.7:369.7 MSDl 469, EIC=468.7:469.7 PC00414 *** End of Report *** U45 Mon, 5. Jan. 2004 03:31:55 pm Page 1 of 1 000371 Sample Name:STD 50 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11776257\A186432\FC000028 .D Injection Date Acq Operator Instrument Dilution 12/31/03 jmiller PC00414 1 12:12:25 AM Seq Line Vial No. Inj.No. Inj. Vol. : : : : 28 1 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C :\HPCHEMX1\METHODS\123003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1776257\A186432\FC000028.D) API-ES, Neg, SIM, Frag: Var 2500- 7.272 - C8 Acid 2000- 1500- 1000- 500- | ; - , , , | ' ' i i i ' 1 '------- 1------- 1------- 1-- , !------- ,------- 1------- ,------- f 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1776257\A186432\FC000028.D) API-ES, Neg, SIM, Frag: Var 8.092- C10 Surrogate 2500- 2000- 1500 1000^ 500- O-i-- 1 ---j--- 1--- -----,---------,---------,---------,------------------ 1---------!---------,---------,-------246 !--- ,--- ,--- ,--- r 8 min Compound Amount (ng/mL) R.T. Area Signal **3 Acid 31.85 L0 Surrogat 30.15 7.272 8.092 20450 24822 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 046 03 :36 :30 pm Page 1 of 1 000372 Sample Name:STD 100 ppb Sample Info: 1 Data file :C:\HPCHEM\1\DATA\Chemstor\11776316\A188352\FC000029.D Injection Date Acq Operator Instrument * Dilution 12/31/03 jmiller PC00414 1 12:27:22 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : 29 2 1 5 pi Acq. Method Analysis Method - Last Changed FC8-10.M C :\HPCHEM\1\METHODS\123003F,M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1776316\A188352\FC000029.D) API-ES, Neg, SIM, Frag: Var 5000- 7.273 - C8 Acid 4000- 3000- 2000- 1000- o-L --- 1--- r 6 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1776316\A188352\FC000029.D) LL API-ES, Neg, SIM, Frag: Var 6000- 8.091 - C10 Surrogate, 1 5000- 4000 3000 -j 2000- 1000- 0*. 1 1--- 1 1 1 i 24 Compound Amount (ng/mL) R.T. Area '"8 Acid 91.02 10 Surrogat 94.12 7.273 8.091 41669 53208 1 111111 6 8 min Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 03:37:18 pm 0047 Page 1 of 1 000373 Sample Name:STD 250 ppb Sample Info: 1 Data file :C :\HPCHEM\l\DATA\Chemstor\11776375\A190272\FC000030 .D Injection Date Acq Operator Instrument . Dilution 12/31/03 jmiller PC00414 1 12:42:24 AM Seq Line Vial No. Inj.No. Inj. Vol. : : : : 30 3 1 5 p.1 Acq. Method Analysis Method * Last Changed FC8-10.M C :\HPCHEM\ 1\METHODSU23003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM1776375NA190272\FC000030.D) API-ES, Neg, SIM, Frag: Var 12000- 7.258- C8 Acid 10000- 8000- 6000- 4000- 2000- 0- *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1776375\A190272\FC000030.D) API-ES, Neg, SIM, Frag: Var 8.083- C10 Surrogate 14000- 12000- 10000- 8000- 6000- 4000- 2000- 0- - 11 '1i 24 0ompound Amount (ng/mL) R.T. Area -8 Acid 248.97 L0 Surrogat 245.47 7.258 8.083 98304 120370 i i--- 1-- 6 !--- ,--- ,--- 1--- r 8 min Signal MSD1 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 3048 03:38:08 pm Page 1 of 1 000374 Sample Name:STD 500 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11776434\A192448\FC000031.D Injection Date Acq Operator Instrument Dilution 12/31/03 jmiller PC00414 1 12:57:22 AM Seq Line Vial No. Inj. No. Inj. Vol. : : : 31 4 1 5 pi Acq. Method Analysis Method *` Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 1776434\A192448\FC000031.D) API-ES, Neg, SIM, Frag: Var 7.254- C8 Acid 20000 - 15000- 10000 - 5000- 0- ji_L *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1776434\A192448\FC000031.D) API-ES, Neg, SIM, Frag: Var 8.076- C10 Surrogatei min 25000 - 20000 - 15000- 10000- 5000- 1 1 1 '--- 1-- 24 -- i--- --- 1---~, i 1 1--- 1--- r 6 8 min c ompound Amount (ng/mL) R.T. Area Signal "" " 3 Acid 500.57 L0 Surrogat 496.33 7.254 8.076 188521 231692 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 03:39:48 pm U49 Page 1 of 1 00037 Sample Name :STD 750 ppb Sample Info : 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11776493\A194240\FC000032.D Injection Date Acq Operator Instrument Dilution 12/31/03 jmiller PC00414 1 1:12:23 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : : 32 5 1 5 pi Acq. Method Analysis Method ~ Last Changed FC8-10.M C :\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (CHEMSTORU1776493\A194240\FC000032.D) API-ES, Neg, SIM, Frag: Var 35000 - 7.272 - C8 Acid 30000 -j 25000 - 20000 15000H 10000 5000 0 MSD1 469, EIC=468.7:469.7 (CHEMSTORM1776493\A194240\FC000032.D) API-ES, Neg, SIM, Frag: Var 45000 8.096- C10 Surrogate] 40000 -j 35000 30000 25000 20000 15000 -j 10000 5000- 0- 11 ' 1 ---- --- ,- 1 24 6 -,--- 1--- 1--- 1--- 1--- r 8 min c ompound Amount (ng/mL) R.T. Area Signal :"3 Acid 788.15 -0 Surrogat 788.04 7.272 8.096 291638 361138 MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 7C00414 *** End of Report *** Mon, 5. Jan. 2004 03:40:13 pm u II Page 1 of 1 000376 Sample Name:STD 1000 ppb Sample Info: 1 Data file :C:\HPCHEM\l\DATA\Chemstor\11772921\A153280\FC000033.D Injection Date Acq Operator Instrument Dilution 12/31/03 jmiller PC00414 1 1:27:21 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : : 33 6 1 5 pi Acq. Method Analysis Method Last Changed FC8-10.M C:\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:26 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, E!C=368.7:369.7 (CHEMSTORM1772921 \A153280\FC000033.D) API-ES, Neg, SIM, Frag: Var 7.269- C8 Acid 40000 - 30000 - 20000 - 10000- - 0 ' ' 1 1--------------- 1 ' 1 1' ^T 246 *MSD1 469, EIC=468.7:469.7 (CHEMSTORM 1772921 \A153280\FC000033.D) J1 T.T i 8 API-ES, Neg, SIM, Frag: Var f min . 8.088- C10 Surrogate 50000 - 40000 - 30000 - 20000 - 10000^ - 0 ' 11| ' ' rT 24 Compo\ind Amount (ng/mL) R.T. *3 Acid 1032.81 10 Surrogat 1027.90 7 269 8 088 1 1^ Area 379365 467572 JA _ ' i1 7 1^ rT 6 8 min Signal MSDl 369, EIC=368.7:369.7 MSD1 469, EIC=468.7:469.7 PC00414 ** End of Report *** Mon, 5. Jan. 2004 (J5 03:18:14 pm Page 1 of 1 000377 Sample Name:STD 1500 ppb Sample Info : Data file :C:\HPCHEM\1\DATA\FC000034.D Injection Date Acq Operator Instrument Dilution 12/31/03 jmiller PC00414 1 1:42:19 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed FC8-10 .M C:\HPCHEM\1\METHODS\123003F. M 1/5/04 02:58:06 pm LC/MS analysis of perfluorooctanoic acid. *MSD1 369, EIC=368.7:369.7 (FC000034.D) API-ES, Neg, SIM, Frag: Var 60000 - 7.248- C8 Acid 1 34 7 1 5 pi 50000 -j -- 40000 - 30000 -j 20000 - 10000^ t T t. .- __ ____ ._.._-.___ __ ______________________ L_ A ____ -r r , -| j ''|Ii1 1 iii| 2 4 6 8 min *MSD1 469, EIC=468.7:469.7 (FC000034.D) API-ES, Neg, SIM, Frag: Var 80000 J 8.074- C10 Surrogate 70000 7 60000 ^ 50000 -j 40000 -- 30000 20000 -i 10000 u J 1 l .. 'l , r 2 4 6 8 min ompound Amount (ng/mL) R.T. Area Signal ~~3 Acid 1441.88 10 Surrogai 1436.00 7.248 8.074 526043 648667 MSD1 369 EIC==368.7:369.7 MSD1 469, EIC=468.7 :469.7 PC00414 *** End of Report *** Mon, 5. Jan. 2004 02:58:30 pm uU52 Page 1 of 1 000378