Document YD0nBqzD6xa691edVEDNa01rn

S - 3 -T ^ if ATTACHMENT A bmittai tc 000004 Precise Research. Proven Results. ^ o e s N o T c ffM ro iix C B X Analytical Report Fluorochemical Monitoring Report CSR Inc Exygen Research Report No. L0002133 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester William Mizel CSR Inc. PO Box 201857 Arlington, TX 76006 Phone: (817)633-7236 000005 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 1 of 8 Research Orive >College, PA 16801, USA : 800.281.3219 f: 8-M ."72.1019 Summary Twenty-two solid media samples were received by Exygen Research from CSR, Inc. The media represent samples of air collected on OVS tubes and bulk solid materials. The samples were analyzed for perfluorooctanoic acid (PFOA) by solvent extraction followed by liquid choromatography / mass spectrometry (LCMS) analysis. The OVS tubes were separated into three fractions for 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 acetone. Fraction C was not analyzed but saved for possible future analysis. Bulk solid materials were extracted into methanol. The methanol extracts were diluted with water and subjected to solid phase extraction (SPE) to remove interferences and concentrate the extract. Chain-of-custody information can be found in Attachment A. Attachment B contains the raw data and analytical conditions for the OVS tube analysis. Attachment C contains the raw data for the bulk solids analysis. ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 2 of 8 000006 Results Summary Request # 1489 A 1489 B 1489 C 1489 (Total) 1490 A 1490 B 1490 C 1490 (Total) 1492 A 1492 B 1492 C 1492 (Total) 1493 A 1493 B 1493 C 1493 (Total) 1494 A 1494 B 1494 C 1494 (Total) 1495 A 1495 B 1495 C 1495 (Total) 1496 A 1496 B 1496 C 1496 (Total) Air Volume Sampled (L) 274 274 274 262 262 262 412 412 412 390 390 390 413 413 413 407 407 407 135 135 135 PFOA (ug/fraction) <0.10 <0.10 NA <0.20 1.2 <0.10 NA 1.2 <0.10 <0.10 NA <0.20 <0.10 0.20 NA 0.20 0.32 0.19 NA 0.51 0.16 <0.10 NA 0.16 <0.10 <0.10 NA <0.20 PFOA (mg/m3) < 0.0004 < 0.0004 NA < 0.0008 0.0046 < 0.0004 NA 0.0046 < 0.0002 < 0.0002 NA < 0.0004 < 0.0003 0.0005 NA 0.0005 0.0008 0.0005 NA 0.0013 0.0004 < 0.0002 NA 0.0004 < 0.0007 < 0.0007 NA <0.0014 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 3 of 8 000007 Request # 1497 A 1497 B 1497 C 1497 (Total) 1498 A 1498 B 1498 C 1498 (Total) 1499 A 1499 B 1499 C 1499 (Total) 1500 A 1500 B 1500 C 1500 (Total) 1501 A 1501 B 1501 C 1501 (Total) 1502 A 1502 B 1502 C 1502 (Total) 1503 A 1503 B 1503 C 1503 (Total) NA - Not Analyzed Air Volume Sampled (L) 134 134 134 89 89 89 327 327 327 320 320 320 320 320 320 327 327 327 327 327 327 PFOA (ug/fraction) <0.10 <0.10 NA <0.20 <0.10 <0.10 NA <0.20 <0.10 <0.10 NA <0.20 0.15 <0.10 NA 0.15 <0.10 <0.10 NA <0.20 <0.10 <0.10 NA <0.20 <0.10 <0.10 NA <0.20 PFOA (mg/m3) < 0.0007 < 0.0007 NA <0.0014 < 0.0011 < 0.0011 NA < 0.0022 < 0.0003 < 0.0003 NA < 0.0006 0.0005 < 0.0003 NA 0.0005 < 0.0003 < 0.0003 NA < 0.0006 < 0.0003 < 0.0003 NA < 0.0006 < 0.0003 < 0.0003 NA < 0.0006 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 4 of 8 000008 Notes: 1. "<" is defined as not detected at or above the reported level. 2. Sample results have not been corrected for blank results or matrix 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 5 of 8 000009 Summary of PFOA in Solids Sample ID Bulk-A *>loU> Bulk-B Fab-A Mem-A Wipe-A Wipe-B I***1 Fab-B PFOA (ng/g) (as received) 561 170 31.4 83.9 2560 834 155 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 8 0 0 0 0 10 OC Pata QVS Tubes) LCS A control sample was spiked with PFOA to give a final concentration of 500 ppb. The fractions were separated and analyzed. The acceptable range for control recovery is 75-125%. Sample Identification Control 1A Control 1B PFOA (raw-ppb) 624 499 PFOA (% recovery) 125 100 Blanks Sample Identification 1491 A 1491 B Vol. Of Air (L) 0 0 PFOA (raw-ppb) 14 14 PFOA (ug/fraction) <0.10 <0.10 PC Data (Bulk Material) Matrix Spike Recovery Sample Bulk-A was spiked with PFOA and analyzed to determine percent recovery. The acceptable range for matrix spike recovery is 70-130%. Concentrations represent the amount of material in the sample extract. PFOA Sample Identification Amount Spiked (ng/mL) Amount Found in Sample Amount Recovered (ng/mL) (ng/mL) Recovery (%) Bulk A 50.0 56.1 104 96 Laboratory Duplicate Samples Bulk-A was analyzed in duplicate. The maximum relative percent difference between duplicates is 30% for solid samples. Sample Identification Bulk A Sample Results (ng/g) 561 PFOA Sample Duplicate (ng/g) 564 RPD (%) 0.53 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 7 of 8 ooooii Signatures > V v\ V -L -X V^ Paul Connolly, LCMS Team Leader ydohn M. Flaherty, Vice President Other Lab Members Contributing to Data James Miller Karen Rysha Date Date ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 8 of 8 000012 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 .ogin Group: LQ002133 Login #: Project: 2244 P 0 0 0 0 7 18 Company Name: CSR, Inc Submitted By: William Mizel Login Type: Immediate Receipt of Samples Started: T Date Start: 03/23/2004 Due Date: 04/06/2004 Received Date: 03/19/2004 Received By: AMMERMAN, MARK Spread Sample: Label: Project Title/Type: Analysis of PFOA in Solids and OVS Tubes / ROUTINE Exygen SD/PI: RISHA, KAREN Login Notes: Conform Notes: Conform COC Sample: Conform COC: Conform Sample: Conform Request: True True True True Package PK0002767 Carton Packages / Containers Mail Date / Condition S h ip p e r/ ID 3/23/2004 9:59:50AM Package & Contents Uncompromised UPS 1Z75X4890340393715 Temp. Control/Tem p. Wet Ice 3.1 Direction / Handled By RECEIVED AMMERMAN, MARK Container # C0029398 C0029399 C0029400 C0029401 C0029402 C0029403 C0029404 C0029405 C0029406 C0029407 C0029408 C0029409 C0029410 C0029411 C0029412 C0029413 C0029414 C0029415 C0029416 C0029417 C0029418 C0029419 C0029420 C0029421 Gross Weight pH Container Type 245.0 g 315.3 g 156.7 g 85.9 g 60.9 g 58.8 g 100.5 g 6.4 g 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow Air tube 6.4 g Air tube 6.3 g Air tube 6.3 g Air tube 6.3 g Air tube 6.3 g Air tube 6.2 g Air tube 6.2 g Air tube 6.2 g Air tube 6.2 g Air tube 6.3 g Air tube 6.3 g Air tube 6.2 g Air tube 6.2 g Air tube 6.3 g Air tube 6.3 g Air tube 6.3 g Air tube Preservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE Mfg. Lot Mfg. ID 000013 3/23/2004 Login.rpt Report Version: Mar 11 2004 4:16PM Page 1 of 4 Instance: R0092139 R0092139 Login Group: L0002133 "lo g in #: Project: 2244 P0000718 Company Name: CSR, Inc Submitted By: William Mizel Login Type: Immediate Receipt of Samples Started: T Date Start: 03/23/2004 Due Date: 04/06/2004 Received Date: 03/19/2004 Received By: AMMERMAN, MARK Spread Sample: Label: Project Title/Type: Analysis of PFOA in Solids and OVS Tubes / ROUTINE Exygen SD/PI: RISHA, KAREN Login Notes: Conform Notes: Conform COC Sample: Conform COC: Conform Sample: Conform Request: True True True True Package PK0002767 Carton Packages / Containers Mail Date / C ondition S h ip p e r/ ID 3/23/2004 9:59:50AM Package & Contents Uncompromised UPS 1Z75X4890340393715 Temp. Control/Temp. Wet Ice 3.1 Direction / Handled By RECEIVED AMMERMAN, MARK Container # C0029422 C0029423 C0029424 C0029425 C0029426 C0029427 C0029428 C0029429 C0029430 C0029431 C0029432 C0029433 C0029434 C0029435 C0029436 Gross Weight 6.3 g 6.4 g 6.4 g 6.3 g 6.3 g 6.3 g 6.3 g 6.2 g 6.3 g 6.2 g 6.2 g 6.3 g 6.3 g 6.3 g 6.3 g pH Container Type Air tube Air tube Air tube Air tube Air tube Air tube Air tube Air tube Air tube Air tube Air tube Air tube Air tube Air tube Air tube Preservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE Mfg._Lot Mfg. ID 3/23/2004 Login.rpt Report Version: Mar 11 2004 4:16PM Page 2 of 4 000014 Instance: R0092139 ogin Sample ID L0002133-0001 Container C0029398 L0002133-0002 C0029399 L0002133-0003 C0029400 L0002133-0004 C0029401 L0002133-0005 C0029402 L0002133-0006 C0029403 L0002133-0007 C0029404 L0002133-0008 C0029405 L0002133-0009 C0029406 L0002133-0010 C0029407 L0002133-0011 C0029408 L0002133-0012 C0029409 L0002133-0013 C0029410 L0002133-0014 C0029411 L0002133-0015 C0029412 L0002133-0016 C0029413 L0002133-0017 C0029414 L0002133-0018 C0029415 L0002133-0019 C0029416 L0002133-0020 C0029417 Matrix SOLID Fraction Solids Samples Sample Bulk-A SOLID Solids Bulk-B SOLID Solids Fab-A SOLID Solids Mem-A SOLID Solids Wipe-A SOLID Solids Wipe-B SOLID Solids Fab-B GAS OVS Tubes 1489 A GAS OVS Tubes 1489 B GAS OVS Tubes 1490 A GAS OVS Tubes 1490 B GAS OVS Tubes 1492 A GAS OVS Tubes 1492 B GAS OVS Tubes 1493 A GAS OVS Tubes 1493 B GAS OVS Tubes 1494 A GAS OVS Tubes 1494 B GAS OVS Tubes 1495 A GAS OVS Tubes 1495 B GAS OVS Tubes 1496 A 3/23/2004 Login.rpt Report Version: Mar 11 2004 4:16PM Page 3 of 4 Date Sampled Date Received Date Pi 03/11/2004 03/19/2004 04/06/20 03/11/2004 03/19/2004 04/06/20 03/11/2004 03/19/2004 04/06/20 03/11/2004 03/19/2004 04/06/20I 03/12/2004 03/19/2004 04/06/20I 03/12/2004 03/19/2004 04/06/201 03/12/2004 03/19/2004 04/06/20C 03/19/2004 04/06/20C 03/19/2004 04/06/20C 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200. 03/19/2004 04/06/200- 03/19/2004 04/06/200. 03/19/2004 04/06/200. 03/19/2004 04/06/200. 03/19/2004 04/06/200. 000015 Instance: R0092139 R0092139 L0002133-0021 C0029418 L0002133-0022 C0029419 L0002133-0023 C0029420 L0002133-0024 C0029421 L0002133-0025 C0029422 L0002133-0026 C0029423 L0002133-0027 C0029424 L0002133-0028 C0029425 L0002133-0029 C0029426 L0002133-0030 C0029427 L0002133-0031 C0029428 L0002133-0032 C0029429 L0002133-0033 C0029430 L0002133-0034 C0029431 L0002133-0035 C0029432 L0002133-0036 C0029433 L0002133-0037 C0029434 L0002133-0038 C0029435 L0002133-0039 C0029436 GAS OVS Tubes 1496 B GAS OVS Tubes 1497 A GAS OVS Tubes 1497 B GAS OVS Tubes 1498 A GAS OVS Tubes 1498 B GAS OVS Tubes 1499 A GAS OVS Tubes 1499 B GAS OVS Tubes 1500 A GAS OVS Tubes 1500 B GAS OVS Tubes 1501 A GAS OVS Tubes 1501 B GAS OVS Tubes 1502 A GAS OVS Tubes 1502 B GAS OVS Tubes 1503 A GAS OVS Tubes 1503 B GAS OVS Tubes 1491 A Blank GAS OVS Tubes 1491 B Blank GAS OVS Tubes Control 1 A GAS OVS Tubes Control 1 B 3/23/2004 Login.rpt Report Version: Mar 11 2004 4:16PM Page 4 of 4 03/19/2004 04/06/20 03/19/2004 04/06/20' 03/19/2004 04/06/20I 03/19/2004 04/06/20( 03/19/2004 04/06/20C 03/19/2004 04/06/20C 03/19/2004 04/06/20C 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200 03/19/2004 04/06/200- 03/19/2004 04/06/200- 03/19/2004 04/06/200- 03/19/2004 04/06/200- 03/19/2004 04/06/200- 03/19/2004 04/06/2004 000016 Instance: R0092139 R0092139 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 SAM PLE C O N D ITIO N UPON RECEIPT FORM Protocol # fj.i Exvcjen Studv # X Date & Time Received Condition of Samples C j ^ //t 'y /a Za / 4 / /rr-*c Temporary Storaqe Location Initials & Date M w f/ / 9 /c ir Waybill # _____________/ . g J Z l X . V8J c 3 V o l l f 7 /< ~ ___________ LIBRARY ID: 70001402 v i LABORATORY FORM 000017 !> V * 7 - " H IS /S a n EXiACT re ^ O n / lN A L S g 42016801 1Z75X4890340393715 000018 r / Industrlktjygiene Laboratory 9742 S killm R^tallas, Texas 75234 *214/343-2025 1-800 937jg35SQutside 214 Area) Analytical Request Form Fax 244i 343-9757s^--- FEE ACCOUNTS Send Report To Company Name: , C , :> V - Aririre- VO T* Attn- \ \ - A *'*-' vT 'tt 'W\~ Phone: <fe 1~? > ( A * , - b O _ l FAX: Send Invoice To Comoanv Name: __________^ AHHrnss- ^ ~7boou \ P.O. #: Taxable Non Taxable (Texas Clients Only) LAB USE ONLY Rept. #: _____________________________________________ Date Received:----- ----------- ---- ------------- INTERNAL ACCOUNTS Client Name:_________________________________________ Street Address:----------------------------------------------------------------City, state, Z ip :----------------------------------------------------------------- Billing Info Cost Center: _ _ _ _ _ _ Risk C ode:_______ CIN Service Provider:______________________________________ Office Address:_______________________ _______________ Telephone No.: i_____ 1__________ Fax No.: {______ l_____ ITEM # IHL# (Lab Only) SAMPLE ID# SAMPLE MEDIA SAMPLE AIR VOL. ANALYSIS REQUESTED (One Analyte perline) \ V -Y.A-'O L ? 9oA \ c\ t o Vv 'X V i l_ \ i L W 3. 1- * Vv 4 u fp u o 5 io 7 * \o \\ \0_ \M ^ 5 \H ^H \o ASO V VV *\ Vv ^V w L \V '\ \\ H \? > u Ho =n_ 1V7>H L u 1 ,^ 0 9 po A p f O4 P F oa P F o a F F OA 9 P o /) F o4 9 F 0 /5 9 PO VV P F u o '5 \M ^ u fyy AnVc Comments: Page Of. CTEK -1367-E CHAIN OF CUSTODY Relinquished By:_______________________________ Date: ______________ (Signature) Priority Routine Q Rush (3 Day) [ j Urgent (Next Day) Same Day Accepted By: -- Sample Condition: (When received by Lab) _ (Signature) ---------- Date: -- - C fm d l - U fa- L - e / ffr z/i*<1 (TOO x r t s Printed in U.S.A. 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 * Page X o f _______ ANALYSES REQUESTED Project Manager (Name & E-mail Address): Avv^ovi r w ~7 k o ^ ' o Phone: ttiV b V *- Fax: tfO-b^>b Sampler: i c - W . '"Vvvb.eA Project Name: RO. # : Q u o ta tio n #: Please fill out this form com pletely to ensure correct analysis and proper handling of your samples. Grab Composite Number of Containers " ' ii':ii\1*c H j Vif'\i?-*\Uj...VJ' C/fK-.? Collection Collection ExyLIMS# Client Sample Identification Date Time Vlt"4 -Q V-A*- A 'VAS.w'S - A w *0 4?. - A w-O-e F*b - "VW '>'> 'Viv--i LAB USE ONLY Specify Matrix j l \ \ A_ V \ Comments Co-vta-v.-- M"7-A3i b HT- * MA Vt >5g Hl^No H? U \ l Relinquished by Date Time OTHER INFORMATION dr o Uo JL X >< JL. >< V X PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: j^LSample results only I^ A d d case narrative 2 Add quality control summary Add calibration summary Add raw data Other_________________ 000020 RFV 0? Sequence: C:\HPCHEM\1\SEQUENCE\033004F.S Sequence Table: Method and Injection Info Part: Line Location SampleHame Method Inj SampleType InjVolume DataFile 1 Vial 1 STD 10 ppb 2 Vial 1 STD 10 ppb 3 Vial 2 STD 50 ppb 4 Vial 3 STD 100 ppb 5 Vial 4 STD 250 ppb 6 Vial 5 STD 500 ppb 7 Vial 6 STD 750 ppb 8 Vial 7 STD 1000 ppb 9 Vial 92 solvent blank 10 Vial 11 Surrogate 11 Vial 12 L2133-38 12 Vial 13 L2133-39 13 Vial 14 L2133-36 14 Vial 15 L2133-37 15 Vial 16 L2133-8 16 Vial 17 L2133-9 17 Vial 18 L2133-10 18 Vial 19 L2133-11 19 Vial 20 L2133-12 20 Vial 4 STD 250 ppb 21 Vial 92 solvent blank 22 Vial 21 L2133-13 23 Vial 22 L2133-14 24 Vial 23 L2133-15 25 Vial 24 L2133-16 26 Vial 25 L2133-17 27 Vial 26 L2133-18 28 Vial 27 L2133-19 29 Vial 28 L2133-20 30 Vial 29 L2133-21 31 Vial 30 L2133-22 32 Vial 4 STD 250 ppb 33 Vial 92 solvent blank 34 Vial 31 L2133-23 35 Vial 32 L2133-24 36 Vial 33 L2133-25 37 Vial 34 L2133-26 38 Vial 35 L2133-27 39 Vial 36 L2133-28 40 Vial 37 L2133-29 41 Vial 38 L2133-30 42 Vial 39 L2133-31 43 Vial 40 L2133-32 44 Vial 4 STD 250 ppb 45 Vial 92 solvent blank 46 Vial 41 L2133-33 47 Vial 42 L2133-34 48 Vial 43 L2133-35 49 Vial 4 STD 250 ppb 50 Vial 92 solvent blank 51 Vial 1 STD 10 ppb 52 Vial 2 STD 50 ppb 53 Vial 3 STD 100 ppb 54 Vial 4 STD 250 ppb 55 Vial 5 STD 500 ppb 56 Vial 6 STD 750 ppb 57 Vial 7 STD 1000 ppb POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Sample Calib Calib Calib Calib Calib Calib Calib Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Sample Calib Calib Calib Calib Calib Calib Calib LCMS3 3/30/04 4::50 :40 PM jmiller A 000021 Page 1 of 2 Sequence: C:\HPCHEM\1\SEQUENCE\033004F.S Calibration Part: Line Location SampleName Method CalLev Update RF Update 2 Vial 1 3 Vial 2 4 Vial 3 5 Vial 4 6 Vial 5 7 Vial 6 8 Vial 7 51 Vial 1 52 Vial 2 53 Vial 3 54 Vial 4 55 Vial 5 56 Vial 6 57 Vial 7 STD 10 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 10 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR 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 LCMS3 3/30/04 4:50:40 PM jmiller A? 000022 Page 2 of 2 LC/MS SYSTEM AND OPERATING CONDITIONS Client: CSR Inc. EXYGEN STUDY: L0002133 Instrument: Hewlett-Packard 1100 LC/MSD (LCMS 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 2.1 mm x 3pm 30 C 2mM Ammonium acetate in OmniSolv Water HPLC grade Methanol Time %A 0.0 90 5.0 10 9.0 10 9.0 STOP Post Time = 5 min. Total run time = 14 min. Flow Rate: 0.3 mL/min Injected Volume: 5 pL %B 10 90 90 STOP 000023 Ions monitored: Analyte TH-PFOS (I.S.) PFOA (POAA) Surrogate Ion (m /z) 427 369 513 Extraction Date: March 30, 2004 Analyst: James R. Miller A & l Exygen ResearCn 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 000024 Method C:\HPCHEM\l\METHODS\033004F.M Calibration Table Calib. Data Modified Wednesday, March 31, 2004 9:04:59 AM Calculate Based on Internal Standard Peak Area Rel. Reference Window A b s . 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 Quadratic (some peaks differ, see below) Included (some peaks differ, see below) Equal (some peaks differ, see below) 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) Default Sample ISTD Information (if not set in sample table): ISTD ISTD Amount Name # [ppb] 1 500.00000 TH-PFOS Signal 1: MSD1 427, EIC= 426.7:427.7 Signal 2 : MSD1 369, EIC= 368.7 :369.7 Signal 3 : MSD1 513, EIC= 512.7:513.7 RetTime Lvl Amount Area Amt/Area Ref Grp Name [min] Sig [ppb] ___ 11 1S--1.1 11_ ________ I1__ ____ 7.273 1 1 500.00000 3.06333e5 1.63221e-3 TH-PFOS 2 500.00000 2.87995e5 1.73614e-3 3 500.00000 2.82575e5 1.76944e-3 4 500.00000 2.66974e5 1.87284e-3 5 500.00000 2.56077e5 1.95254e-3 6 500.00000 2.32126e5 2.15400e-3 7 500.00000 2.46664e5 2.02705e-3 7.281 2 1 10.00000 7944.07910 1.25880e-3 PFOA 2 50.00000 2.6997 8e4 1.85200e-3 3 100.00000 5.28759e4 1.89122e-3 4 250.00000 1.29464e5 1.93104e-3 5 500.00000 2.52757e5 1.97818e-3 6 750.00000 3.56357e5 2.10463e-3 7 1000.00000 4.51134e5 2 .21664e-3 7.747 3 1 10.00000 1760.20929 5.68114e-3 SURROGATE 2 50.00000 4853.52673 1.03018e-2 3 100.00000 8862.66040 1.12833e-2 4 250.00000 1.9667 6e4 1 -27113e-2 5 500.00000 3.71388e4 1.3463 0e-2 6 750.00000 4.98274e4 1.50520e-2 7 1000.00000 6.49905e4 1.53869e-2 7C00414 3/31/04 9:05:54 AM jmiller ^ T \ Y 7iM 000025 Page 1 of 3 Method C:\HPCHEM\1\METHODS\033004F.M More compound-specific settings: Compound: TH-PFOS Time Window From 5.653 min To 8.073 min Curve Type Linear Origin Forced Calibration Level Weights / Level 1 1 Level 2 1 Level 3 1 Level 4 1 Level 5 1 Level 6 1 Level 7 1 Compound: PFOA Time Window : From 5.652 min To 8.100 min Compound: SURROGATE Time Window : From 7.227 min To 8.578 min Peak Sum Table ** *No Entries in table*** Calibration Curves Area Ratio 0.80.6 : 0.4 : 0 .2 - C / ii x ii|iii 0.5 Amount Ratio / TH-PFOS at exp. R T : 7.273 MSD1 427, EIC=426.7 :427.7 Correlation: 1.00000 Residual Std. Dev.: 0.00000 Formula: y = mx m: 1.00000 x: Amount Ratio' y: Area Ratio Calibration Level Weights: Level 1 :1 Level 2 : 1 i| 1 Level Level Level 3 4 5 :1 :1 :1 Level 6 : 1 Level 7 : 1 PFOA at exp. RT: 7.281 MSD1 369, EIC=368.7 :369.7 Correlation: 0.99868 Residual Std. Dev.: 0.04011 Formula: y = axJ + bx + c a: -8.86528e-2 b: 1.11680 c: -1.61426e-2 x: Amount Ratio y: Area Ratio ?C00414 3/31/04 9:05:54 AM jmiller 000026 Page 2 of 3 Method C :\HPCHEM\l\METHODS\033004F.M SURROGATE at exp. RT: 7.747 MSD1 513, El0=512.7:513.7 Correlation: 0.99966 Residual Std. Dev.: 0.00287 Formula: y = ax2 + bx + c a: -1.34309e-2 b: 1.59540e-l c: 4.31606e-4 X : Amount Ratio y: Area Ratio ?C00414 3/31/04 9:05:54 AM jmiller 000027 Page 3 of 3 Sample Name:STD 10 ppb Sample Info:Warm up 1 Data file .-C:\HPCHEM\l\DATA\Chemstor\13030415\A199168\FC000001.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 5:09:40 PM Seq Line vial No. Inj. No. Inj. Voi. : : i i i 5 fil Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09 :05 :00 am Initials Date V>/CH Run# F C o b o o a i To,, 1F c - o o o o MSD1 427. EIC=426.7:427.7 (CHEMSTORV13030415\A199168\FC000001 .D) API-ES, Neg, SIM, Frag: Var 35000 4 30000 25000 20000 15000 100005000 7.196- TH-PFOS, o4 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13030415\A199168\FC000001.D) API-ES, Neg, SIM, Frag: Var 1600 7.217- PFOA. 1400 1200 ~ 1000^ 800 i 600 i 400 - 200 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13030415\A199168\FC000001.D) API-ES, Neg. SIM, Frag: Var 700/ 7.696- SURROGATE, 600 500 400 300 200 Compound Name Area Amount Meas. Ret. T Signal Desc. mir mid TH-PFOS PFOA SURROGATE 381058.06 14793.73 4655.52 500.00 24.71 37.17 7.196 7.217 7.696 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7 :369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:31:55 am Page 1 of 1 000028 Sample Name:STD 10 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13030525\A201216\FC000002.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 5:25:17 PM Seq Line Vial N o . Inj. No. Inj. Voi. : : : A c q . Method Analysis Method Last Changed POAASUR.M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 2 1 1 5 ill 1 'MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13030525\A201216\FC000002.D) API-ES, Neg, SIM, Frag: Var 35000 7.294- TH-PFOSt 30000 -g 25000 20000 -j 15000 10000-3 5000 0 ---- ,---------- .-----------'-----------1---- ri |> 24 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13030525\A201216\FC000002.D) 6 API-ES, Neg, SIM, Frag: Var 1200- 7,305- PFOA 1 8 1000 800- r1 i 600 / i\ 400 / // 200 / __ 11' I ' ' ' ] 24 *MSD1 513, EIC=512.7:513.7(CHEMSTOR\13030525\A201216\FC000002.D) ' 11 6 API-ES, Neg, SIM, Frag: Var l 8 450/ 400/ 7.735- SURROGATE. 1< ii 350/ 300 / 250/ 2 0 0 - / .......................................... . I 1I | 2 Compound Name i Area i i 1i 46 Amount Meas. Ret. T / ''a'.' vi-- " 1---------8 Signal Desc. mi mir min TH-PFOS PFOA SURROGATE 351174.81 8939.94 2169.02 500.00 18.68 18.06 7.294 7.305 7.735 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:33:19 am Page 1 of 1 000029 Sample Name:STD 50 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13030612\A2 032 00\FC0 00 003.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 5:40:50 PM Seq Line vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09 :05 :00 am 3 2 1 5 1 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTORM3030612\A203200\FC000003.D) API-ES, Neg, SIM, Frag: Var 30000 - 7.280 - TH-PFOS, 25000 20000 15000- j! ii .i ii 100005000- i: I; u. , , | | , ' 1| ' ' !------------------ 1 '------------------ '------------------ >------------------ 1------------------------------------ 2 4 6 8m -MSD1 369, EIC=368.7:369.7 (CHEMSTORM3030612\A203200\FC000003.D) API-ES, Neg, SIM, Frag: Var 3000 2500 - 7.287 - PFO/y. I !I 2000 i 1500 i 1000 il i i 500 i ______ i / - ^ 111111' I ' 24 1' 11 6 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13030612\A203200\FC000003.D) API-ES, Neg. SIM, Frag: Var ' 1 1 r " .... 8 800700 i 7.720- SURROGATB i 600 -I 500 i 400 i 300- 200 i '' 'I ' 'I _____ / W "~r ' ' I T r 1 1------------------ 1-------- ' mi Compound Name Area Amount Meas. Ret. T Signal Dse. TH-PFOS PFOA SURROGATE 315424.91 29009.79 6317.18 500.00 48.78 62.06 7.280 7.287 7.720 MSD1 427, EIC=426.7:427.7 M S D 1 369, E I C = 3 6 8 .7 :369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:34:31 am Page 1 of 1 000030 Sample Name:STD 100 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13030748\A205440\FC000004.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 5:56:25 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004 F .M 3/31/04 09 :05 :00 am 4 3 1 5 1 1 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13030748\A205440\FC000004.D) API-ES, Neg, SIM, Frag: Var 30000 25000 - 7.287 - TH-PFOS, !^ 1 j 20000 15000- 1 i. i ii 10000- 5000- , ' | 2 1' i ' 4 "MSD1 369, EIC=368.7:369.7(CHEMSTOR\13030748\A205440\FC000004.D) 6000 / 6 API-ES, Neg, SIM, Frag: Var 7.294- PFOA 8 mi 5000 4000 - 3000 / ; 2000- 1000/ 0- 1 ' ' 1 2 i i I i "* 1 i 1 46 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13030748\A205440\FC000004.D) API-ES, Neg. SIM, Frag: Var ;/ 1---------- 1---------- 1--------- 8 1200 / 7.731 - SURROGATE, mir 1000^ ;; 800- 600 / 400 Z 200 / I JI j I i Ii y \jy' '..... r" ..-- 1111' 1 2 4 6 8 min Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 301721.16 56373.87 10383.05 500.00 92.23 108.48 7.287 7.294 7.731 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=3 68.7:369.7 MSD1 513, EIC=512.7:513.7 II II II II II II II II it II II II II II II II II II II II II II II II i! II II II II II II II II II II * End of Report *** ===== PC00414 Wed, 31. Mar. 2004 09:35:33 am Page l of 1 000031 Sample Name:STD 250 ppb Sample Info: Data file :C :\HPCHEM\1\DATA\Chemstor\13030810\A2 07360\FC000005.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 6:11:58 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 5 4 1 5 /il 1 MSD1 427, EIC=426.7:427.7 (CHEMSTORU3030810\A207360\FC000005.D) API-ES, Neg, SIM, Frag: Var 35000 7.295 - TH-PFOS 30000 25000 20000 15000 -j 10000 -I 5000 / 0i *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13030810\A207360\FC000005.D) API-ES, Neg, SIM, Frag: Var 17500 1 7.302- PFOA, 15000 12500-1 10000 7500 5000^ 2500 04 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13030810\A207360\FC000005.D) API-ES, Neg, SIM, Frag: Var 3000 7.729- SURROGATE, 2500 20001 15001 10001 500 mi Compound Name TH-PFOS PFOA SURROGATE Area 286496.72 139903.34 21990.65 Amount 500.00 234.59 249.70 Meas. Ret. T Signal Desc. min 7.295 7.302 7.729 MSD1 427, EIC=426.7:427.7 M S D 1 369, E I C = 3 6 8 . 7 :3 6 9 . 7 M S D 1 513, E I C = 5 1 2 .7 :5 1 3 . 7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:36:39 am Page 1 of 1 000032 Sample Name:STD 500 ppb "* Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13030945\A209408\FC000006.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 6:27:35 PM Seq Line vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 6 5 1 5 i 1 1 MSD1 427, EIC=426,7:427.7 (CHEMSTOR\13030945\A209408\FC000006.D) API-ES, Neg, SIM, Frag: Var 35000 -i 7.279 - TH-PFOS 30000 4 25000 4 20000 -j 15000 -j 10000^ 5000 -j 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13030945\A209408\FC000006.D) API-ES, Neg, SIM, Frag: Var 35000 7.286 - PFOA 30000 25000 20000 -t 15000 -, 10000/ 5000 -j o4 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13030945\A209408\FC000006.D) 5000 API-ES, Neg, SIM, Frag: Var 7.730- SURROGATE, mi mir 4000 3000 2000 1000- 0- Compound Name Area Amount Meas. R e t , T Signal Desc. TH-PFOS PFOA SURROGATE 273931.84 270093.41 41181.93 500.00 486.19 514.35 7.279 7.286 7.730 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:37:51 am Page 1 of 1 000033 Sample Name:STD 750 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13031032\A92288\FC000007 .D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 6:43:10 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 03:59:57 pm 7 6 1 5 /il 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13031032\A92288\FC000007.D) 30000 - API-ES, Neg. SIM, Frag: Var 7.276- TH-PFOS, 25000 - rj 20000 15000- 1' ;i ! 10000- 5000- 0. ----------------- , 1 ------------------ 1 -r r 1 24 *MSD1 369, EIC=368.7:369.7 (CHEMSTORU 3031032\A92288\FC000007.D) 11 . r 6 API-ES, Neg, SIM, Frag: Var 1\ ,; \ 7.283- PFOA 1 I 8 40000 / 30000 / 20000 10000/ 1 1! 1 i1 I 11 !j 1i i 0---------- ,----------- 1------------------ 1----------- j----------- '----------- ' ' i 1 24 ` MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031032\A92288\FC000007.D) 7000 -j 6000 -j 5000 -j 4000 -j 3000 / 2000 -j 1000/ J 6 API-ES, Neg, SIM, Frag: Var 7.710- SURROGATE^ 1 1. 8 ,i I Ii Ij ' -------- ,o 4 ------------------ ,------------------ 1------------------ [------------------ 1------------------ ' 2 Compound Name Area 1 11 46 Amount Meas. Ret. T 1 8 Signal Desc. ' mi mi mi TH-PFOS PFOA SURROGATE 244656.30 371633.72 54317.40 500.00 785.17 803.02 7.276 7.283 7.710 MSD1 427, EIC=426.7:427.7 MSD1 369, E I C = 3 6 8 . 7:369.7 MSD1 513, E I C = 5 1 2 .7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:01:22 pm Page 1 of 1 000034 Sample Name:STD 1000 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13031168\A94208\FC000008 .D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 6:58:48 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03:59:57 pm 8 7 1 5 a*1 1 30000 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13031168\A94208\FC000008.D) API-ES, Neg, SIM, Frag: Var 7.284 - TH-PFOS^ 25000 20000 - 15000 i 10000 5000 i Oi *MSD1 369. EIC=368.7:369.7 (CHEMSTOR\13031168\A94208\FC000008.D) API-ES, Neg, SIM, Frag: Var 60000 7.293- PFOA, 50000 40000 30000 i 20000 / 10000 0 mi *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031168\A94208\FC000008.D) 9000 E 8000 -j 7000 4 6000 5000 4000 3000 2000 i 1000-= 0 API-ES, Neg, SIM, Frag: Var 7.737- SURROGATE Compound Name Area Amount Meas. R e t . T Signal Desc. TH-PFOS PFOA SURROGATE 256301.19 469969.84 70507.30 500.00 980.93 1044.48 7.284 7.293 7.737 MSD1 427, EIC=426.7 :427.7 MSD1 369, EIC=368.7:369.7 MSD1 513 , EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:02:36 pm Page 1 of 1 000035 Sample Name:solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13031375\A96192\FC00 0009.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 7:14:19 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 9 92 1 5 /il 1 'MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13031375\A96192\FC000009.D) API-ES, Neg. SIM, Frag: Var 35000 7.287 - TH-PFOS. 30000 -3 25000 20000 -E 15000 - 10000 5000 ~3 0 6 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13031375\A96192\FC000009.D) API-ES, Neg, SIM, Frag: Var 500 450 400 7.339- PFOA 350 300 250 -i 200 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031375\A96192\FC000009.D) API-ES, Neg, SIM, Frag: Var 350 -E 325 300 275-3 250 225 200 -3 175 V Compound Name TH-PFOS PFOA SURROGATE N_. Area 294378.31 949.01 705.08 7.743- SURROGATE Amount 500.00 8.68 6.16 Meas. Ret. T Signal Desc. mu 7.287 7.339 7.743 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 M S D 1 513, E I C = 5 1 2 .7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:03:43 pm Page 1 of 1 000036 Sample Name :Surrogate Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13031485\A217408\FC000010.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 7:29:52 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 10 11 1 5 /il 1 'MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13031485\A217408\FC000010.D) 35000 -= 30000 25000 j 20000 i 15000 - 10000 5000 0 -r API-ES, Neg, SIM, Frag: Var 7.294 - TH-PFOS, *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13031485\A217408\FC000010.D) API-ES, Neg, SIM, Frag: Var 800- 7.305- PFOA 700 ~ 600 500 : 400 300 t 200 ^ ,,-V 'T~ *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031485\A217408\FC000010.D) API-ES, Neg. SIM, Frag: Var 5000 7.739- SURROGATE 4000 3000- 2000 / 1000- mi Compound Name TH-PFOS PFOA SURROGATE Area 297779.28 4568.15 38976.33 Amount 500.00 14.13 441.71 Meas. Ret. T Signal Desc. 7.294 7.305 7.739 M S D 1 427, E I C = 4 2 6 .7 :427.7 M S D 1 369, EI.C=368.7 :369.7 M S D 1 513, E I C = 5 12.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:07:09 am Page 1 of 1 000037 Sample Name:L2133-38 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\130 31597\A219328\FC0 00011.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 7:45:26 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05 :00 am 11 12 1 5 fi 1 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13031597\A219328\FC000011.D) 35000 i 30000 25000 j 20000 -j 15000 i 10000 5000 0 API-ES, Neg, SIM, Frag: Var 7.286- TH-PFOS, !| MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13031597\A219328\FC000011,D) API-ES, Neg, SIM, Frag: Var 7.294- PFOA 40000 30000 I mu 20000 -j 10000 0 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031597\A219328\FC000011.D) API-ES, Neg, SIM, Frag: Var 5000 7.724 - SURROGATE, 4000 3000-d 2000 1000 0 Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 290741.16 360322.87 38528.03 500.00 623.87 447.70 7.286 7.294 7.724 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:08:57 am Page 1 of 1 000038 Sample Name :L213 3-39 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13 0317 92\A22144 0\FC0 0O012.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 8:01:02 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\l\METHODS\033004F. M 3/31/04 09 :05 :00 am 12 13 1 5 il 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13031792\A221440\FC000012.D) API-ES, Neg, SIM, Frag: Var 35000 j 7.301 - TH-PFOSj. 30000 -j 25000 4 20000 -j 15000j 10000 -j 5 0 0 0 -I oi MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13031792\A221440\FC000012.D) 35000 30000 -j 25000 4 20000 -j 15000 -j 10000-i 5000 -I o-i API-ES, Neg, SIM, Frag: Var 7.308- PFOA mu 'MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031792\A221440\FC000012,D) API-ES, Neg. SIM, Frag: Var 5000 7.752- SURROGATE, 4000- 3000 2000 1000H 0i Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 290724.38 293724.41 38285.21 500.00 499.10 444.65 7.301 7.308 7.752 MSD1 427, EIC=426.7 :427.7 MSD1 369, EIC=368.7 :369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:10:18 am Page 1 of 1 000039 Sample Name:L2133-36 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13031853\A223360\FC000013.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 8:16:39 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 13 14 1 5 fll 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13031853\A223360\FC000013.D) 40000 j 35000 j 30000 i 25000 20000 -j 15000 i 10000j 5000 -j 0-i- API-ES, Neg, SIM, Frag: Var 7.284- TH-PFOS 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13031853\A223360\FC000013.D) API-ES, Neg, SIM, Frag: Var 800 - 7.296- PFOA, 700 -j 600- 500 -3 400- 300- 200 i j *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031853\A223360\FC000013.D) API-ES, Neg, SIM, Frag: Var 5000 7.753 - SURROGATE 4000 3000- 2000 1000- mi Compound Name TH-PFOS PFOA SURROGATE Area 317239.12 4890.69 37853.95 Amount 500.00 14.16 399.48 Meas. Ret. T Signal Desc. 7.284 7.296 7.753 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=3 68.7 :369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:11:26 am Page 1 of 1 000040 Sample Name:L2133-37 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13 031914\A225344\FC000014.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 8:32:16 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F.M 3/31/04 09:05:00 am 14 15 1 5 111 i *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13031914\A225344\FC000014.D) 40000 35000 30000 25000 20000 15000 10000 5000 0-4 API-ES, Neg, SIM, Frag: Var 7.270- TH-PFOS}, *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13031914\A225344\FC000014.D) API-ES, Neg, SIM, Frag: Var 800 i 7.279- PFOA 700 600 4 500 400 300 200 -3 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031914\A225344\FC000014.D) API-ES, Neg. SIM, Frag: Var 5000- 7.731 - s u r r o g a t e ; mi 4000 3000 -J 2000 1000 0 Compound Name TH-PFOS PFOA SURROGATE Area 301105.63 4725.47 37147.81 Amount 500.00 14.29 414.18 Meas. Ret. T Signal Desc. 7.270 7.279 7.731 MSD1 427 , EIC=426.7:427,7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:12:34 am Page 1 of l 000041 Sample Name:L2133-8 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13031976\A98112\FC000015.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 8:47:53 PM Seq Line Vial No. Inj.No. Inj. Voi. : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 15 16 1 5 ill 1 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13031976\A98112\FC000015.D) API-ES, Neg, SIM, Frag: Var 40000 7.283- TH-PFO^ 35000 30000 25000 20000 15000 10000^ 5000 0 "MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13031976\A98112\FC000015.D) API-ES, Neg, SIM, Frag: Var 2500 7.286- PFOA, 2 0 0 0 -I 1500 ii 1000H 500 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13031976\A98112\FC000015.D) API-ES, Neg, SIM, Frag: Var 4500 4000 -E 3500 3000 2500 ^ 2000 1500 1000-E 500 0 7.722 - SURROGATE, Compound Name Area Amount Meas. Ret. T Signal Desc. mi mu TH-PFOS PFOA SURROGATE 313245.38 18395.42 33291.57 500.00 33.70 352.67 7.283 7.286 7.722 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:05:49 pm Page 1 of 1 000042 Sample Name:L2133-9 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13032176\A100096\FC000016.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 9:03:30 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\ H P C H E M \ 1 \ M E T H O D S \ 0 3 3 0 0 4 F . M 3/31/04 03 :59 :57 p m 16 17 1 5 /il i 'MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13032176\A100096\FC000016.D) API-ES, Neg, SIM, Frag: Var 40000 7.276- TH-PFOS, 35000 30000 25000 20000 H 15000 4 100004 5000 4 0 TI *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13032176\A100096\FC000016.D) 1000 900-4 800 700 -4 600 500 400 i 300 4 200 API-ES, Neg, SIM, Frag: Var 7.286- PFOA MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032176\A100096\FC000016.D) API-ES, Neg. SIM, Frag: Var 5000- 7.761 - SURROGATE 4000 3000 2000- 1000 4 mir Compound Name TH-PFOS PFOA SURROGATE Area 323992.78 6460.67 39744.98 Amount 500.00 16.20 411.63 Meas. Ret. T Signal Desc. 7.276 7.286 7.761 MSD1 427, EIC=426.7:427.7 M S D 1 369, E I C - 3 6 8 .7 :3 6 9 . 7 M S D 1 513, E I C = 5 1 2 . 7 :5 1 3 . 7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:08:02 pm Page 1 of 1 000043 Sample Name:L2133-10 Sample Info: Data file .-C:\HPCHBM\l\DATA\Chemstor\13032237\A230976\FC000017 .D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 9:19:09 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05 :00 am 17 18 1 5 fll 1 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13032237\A230976\FC000017.D) API-ES, Neg, SIM, Frag: Var 7.289- TH-PFOS 30000 25000 20000 15000 10000 5000 0 1 I ..... I" --i----------------- r~ 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13032237\A230976\FC000017.D) API-ES, Neg, SIM, Frag: Var 70000 7.297- PFOA, 60000 50000 40000 30000 - 20000 10000- 0- MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032237\A230976\FC000017.D) API-ES, Neg. SIM, Frag: Var 5000 7.770- SURROGATE, 4000 3000 2000 1000 Compound Name TH-PFOS PFOA SURROGATE Area 272033.38 597702.44 36879.13 Amount 500.00 1231.81 458.99 Meas. Ret. T Signal Desc. 7.289 7.297 7.770 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=3 68.7:369.7 MSD1 513 , EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:13:16 am Page 1 of 1 000044 Sample Name:L2133-11 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13032323\A102144\FC000018.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 9:34:52 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 03:59:57 pm 18 19 1 5 /I 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13032323\A102144\FC000018.D) API-ES, Neg, SIM, Frag: Var 40000 i 7.277 - TH-PFOS 35000 / 30000 j 25000 -j 20000 -j i 15000 -i 10000 -i 5000 / 0- *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13032323\A102144\FC000018.D) API-ES, Neg, SIM, Frag: Var 1800 -3 7.283- PFOAfi 1600 1400 1200 1000 800 600 -t 400 200 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032323\A102144\FC000018.D) API-ES, Neg, SIM, Frag: Var 5000-] 7.727- SURROGATE 4000 3000 2000 1000-1 0 -C Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PPOA SURROGATE 303139.19 12458.16 39190.64 500.00 25.73 435.80 7.277 7.283 7.727 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:09:35 pm Page 1 of 1 000045 Sample Name:L2133-12 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13032360\A104 064\FC0 00 019.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 9:50:34 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 19 20 1 5 fil 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTORM 3032360\A104064\FC000019.D) 40000 -i 35000 4 30000 25000 4 20000 4 15000 4 10000 4 5000 J API-ES, Neg, SIM, Frag: Var 7.270- TH-PFOS. ________ __________________2__________________________4___________ ____________ 6__________ "MSD1 369, EIC=368.7:369.7 (CHEMSTORM 3032360\A104064\FC000019.D) API-ES, Neg, SIM, Frag: Var mu 2000 1750 4 1500 4 7.277- PFOA, I' 1250- 10004 ! 750 -: 500 250 4 4 .......... .................... ......... ,,..._.......... .... ........../ \ ___ ________ ________ __ ________ - .....- ..- ----------"1------------------ 1------------------ 1------------------ 1------------------ '----------------- '-- 1-- ------------------ 1------------ -- 1--------------- '----------------- '-------------------- i------------------ 1----------- ____________________ 2____________________ 4__________________________6__________ *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032360\A104064\FC000019.D) API-ES, Neg, SIM, Frag: Var I i p8___________ mir 4500 i 4000 4 3500 4 3000 4 2500 4 2000 4 1500 4 1000 4 500 4 0J- Compound Name 1----- --- 1 2______ __ Area 7.737 - SURROGATE 4 Amount ----- 1---------1---------r _________________ 6 Meas. Ret. T _________________ 8 Signal Desc. min TH-PFOS PFOA SURROGATE 319936.38 13914.09 33598.00 500.00 26.81 348.18 7.270 7.277 7.737 MSD1 427, EIC=42 6.7 :42 7.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:12:14 pm Page 1 of 1 000046 Sample Name:STD 250 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\130324 51\A2 3673 6\FC0 00020.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 10:06:07 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\l\METHODS\033004F. M 3/31/04 09:05:00 am 20 4 1 5 /il X 'MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13032451\A236736\FC000020.D) API-ES, Neg, SIM, Frag: Var 30000 -i 7.279- TH-PFOS 25000 20000 15000 10000 5000 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13032451\A236736\FC000020.D) API-ES, Neg, SIM, Frag: Var 16000-1 7.286- PFOA 14000 120001 10000 8000 6000 4000 2000 0-3 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032451\A236736\FC000020.D) API-ES, Neg, SIM, Frag: Var 2250 j 7.753- SURROGATE, 2 0 0 0 -j 1750 -j 1500 i 1250 j 1000/ 750-I 500 i 250 3. Compound Name Area Amount Meas. Ret. T Signal Desc. mir mir TH-PFOS PFOA SURROGATE 251367.09 120153.27 16885.06 500.00 229.60 217.10 7.279 7.286 7.753 MSD1 427, EIC =4 2 6 .7 :427.7 MSD1 369, EIC=368.7 :369.7 MSD1 513 , EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:17:18 am Page 1 of 1 000047 Sample Name:solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13032488\A106048\FC000021.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 10:21:39 PM Seq Line vial NO. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F .M 3/31/04 03:59:57 pm 21 92 1 5 /zl 1 fMSD1 427. EIC=426.7:427.7 (CHEMSTOR\13032488\A106048\FC000021.D) API-ES, Neg, SIM, Frag: Var 35000 7.278- TH-PFOS 30000 -I 25000 4 20000 4 150004 10000j 5000 4 o4- *MSD1 369, EIC=368.7:369.7 (CHEMSTORU 3032488\A106048VFC000021 .D) API-ES, Neg, SIM, Frag: Var 450 400 350 300 H 250 200 -4 7.340- PFOA ___ x *MSD1 513, EIC=512.7:513.7 (CHEMSTORM3032488VA106048\FC000021.D) API-ES, Neg, SIM, Frag: Var 320 300 4 280 260 -; 240 4 220 200 180 -i----------- r~ Compound Name Area TH-PFOS PFOA SURROGATE 278424.84 530.74 467.79 7.728- SURROGATE Amount 500.00 8.09 3.92 Meas. Ret. T --i------------------ r - Signal Desc. min 7.278 7.340 7.728 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:45:01 pm Page 1 of 1 000048 Sample Name:L2133~13 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13032573\A108032\FC000022.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 10:37:15 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1'\METHODS\033 004 F .M 3/31/04 03 :59 :57 pm 22 21 1 5 n1 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13032573\A108032\FC000022.D) API-ES, Neg, SIM, Frag: Var 40000 7.276 - TH-PFOS, 35000 -j 30000 / 25000 20000 -j 15000 10000-^ 5000 0 1000 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13032573\A108032\FC000022.D) API-ES, Neg, SIM, Frag: Var 7.286- PFOA 800 600- 400- 200 6 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032573\A108032\FC000022.D) API-ES, Neg, SIM. Frag: Var 5000 7.729- SURROGATE, 4000- 3000 / 2000 1000 H mi Compound Name TH-PFOS PFOA SURROGATE Area 309027.56 6937.89 38306.29 Amount 500.00 17.33 416.31 Meas. Ret. T Signal Desc. mil 7.276 7.286 7.729 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:45:55 pm Page 1 of 1 J 00049 Sample Name:L2133-14 Sample Info: Data file :C :\HPCHEM\1\DATA\Chemstor\13032740\Al10016\FC000023.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 10:52:50 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 23 22 1 5 /il 1 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13032740\A110016\FC000023.D) API-ES, Neg, SIM, Frag: Var 40000 7.279 - TH-PFOS 35000 30000 -3 25000 20000 1 15000 / 100001 5000 1 0 MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13032740\A110016\FC000023,D) 7000 " 6000 1 50001 4000 3000 2000 10001 API-ES, Neg, SIM, Frag: Var 7.286 - PFOA *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032740\A110016\FC000023.D) API-ES, Neg, SIM, Frag: Var 4500 J 7.764- SURROGATE^, 4000350030002500- 2000 -j 1500 1000- 500 Compound Name TH-PFOS PFOA SURROGATE Area 306091.31 57381.82 33845.78 Amount 500.00 92.52 367.99 Meas. Ret. T Signal Desc. 7.279 7.286 7.764 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:48:12 pm Page l of 1 000050 Sample Name:L2133-15 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13032825\A111936\FC000024.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 11:08:24 PM Seq Line vial NO. Inj.No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03:59:57 pm 24 23 1 5 fil 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13032825\A111936\FC000024.D) 35000 30000 25000 20000 -j 15000 10000 - 5000 -! 0 API-ES, Neg, SIM, Frag: Var 7.284 - TH-PFOSj, *MSD1 369, EIC=368.7:369.7 <CHEMSTOR\13032825\A111936\FC000024.D) 16000i 14000 12000 10000i 8000 - 6000 4000 i 2000 -i Oi API-ES, Neg, SIM, Frag: Var 7.292- PFO/V mi *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032825\A111936\FC000024.D) API-ES, Neg. SIM, Frag Var 5000 7.746 - SURROGATE-. 4000 3000 2000 -J 1000 0-1 Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 296662.34 125197.53 37054.03 500.00 202.69 419.76 7.284 7.292 7.746 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:50:09 pm Page 1 of 1 000051 Sample Name:L2133-16 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13032862\A246528\FC000025.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 11:23:57 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 25 24 1 5 il 1 'MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13032862\A246528\FC000025.D) 35000 30000 25000 20000 15000 10000- 5000 0- API-ES, Neg, SIM, Frag: Var 7.267 - TH-PFOS, *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13032862\A246528\FC000025.D) API-ES, Neg, SIM, Frag: Var 25000 7.273- PFOA 20000 15000 10000 5000 0 mi MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13032862\A246528\FC000025.D) API-ES, Neg, SIM, Frag: Var 7.727- SURROGATE 4000- 3000 2000- 1000/ i i 0 -- Compound Name 2 Area 4 Amount T 6 Meas. Ret. T ""T -- ------- |---- I- t~ 8 min Signal Desc. TH-PFOS PFOA SURROGATE 290834.09 190187.05 34084.31 500.00 315.84 391.78 7.267 7.273 7.727 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:18:23 am Page 1 of 1 000052 Sample Name:L2133-17 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13033092\A113920\FC000026.D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 11:39:34 PM Seq Line Vial No. Inj.No. Inj. Voi. ; : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 26 25 1 5 /il 1 *MSD1 427. EIC=426.7:427.7 (CHEMST0R\13033092\A113920\FC000026.D) 35000 30000 - 25000 20000 -j 15000 / 10000 / 5000 0 API-ES, Neg, SIM, Frag: Var 7.261 - TH-PFOS MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033092\A113920\FC000026.D) API-ES. Neg, SIM, Frag: Var 14000 7.269- PFOA, 12000 10000 8000 6000 4000 2000-3 0 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033092\A113920\FC000026.D) API-ES, Neg. SIM, Frag: Var 7.749- SURROGATE, 4000- r 3000 / 2000 1000 0-1 Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 294437.66 115131.87 36761.68 500.00 187.90 419.58 7.261 7.269 7.749 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04 :51 :20 pm Page 1 of 1 000053 Sample Name:L2133-18 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13 03312 9\A115 904\FC0 0002 7 .D Injection Date Acq Operator Instrument Dilution 3/30/04 jmiller PC00414 1 11:55:13 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F .M 3/31/04 03 :59 :57 pm 27 26 1 5 11 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTORM3033129\A115904\FC000027.D) API-ES, Neg, SIM, Frag: Var 35000 30000 25000 20000 1500010000- 7.283 - TH-PFOS, 'i I I! j iI .i i 5000- 0 , , , | ' ' 1I ' ' ' I ' 246 *MSD1 369, EIC=368.7:369.7 (CHEMSTORM 3033129\A115904\FC000027.D) API-ES, Neg, SIM, Frag: Var ' ' 12000/ 10000/ 8000/ 60004000/ 7.288- PFO/V| M !I ji !i fi ji :i 2000- ii I 8 0 - 1 ' " ....' 1 1 '... 1 ..... 1 1 1 1 ' ! ....... 246 *MSD1 513, EIC=512.7:513.7 (CHEMSTORM3033129\A115904\FC000027.D) API-ES, Neg, SIM, Frag: Var 1 8 4000/ 3500/ 3000/ 2500/ 2000/ 7,748- SURROGATE, fi ! ji i 1500/ 1000/ 500/ 0s , , Compound Name I; , | 11' 1' ' ' 1` 1' , 246 8 Area Amount Meas. Ret. T Signal Desc. '' mi 1 mil mif TH-PFOS PFOA SURROGATE 299029.22 99718.22 34284.52 500.00 160.62 382.62 7.283 7.288 7.748 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:51:56 pm Page 1 of 1 000054 Sample Name :L2133 -19 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13033217\A117888\FC000028.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 12:10:51 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 28 27 1 5 fxl 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13033217\A117888\FC000028.D) 40000 35000 30000 25000 20000 15000 10000 5000 -i 0 API-ES, Neg, SIM, Frag: Var 7.277- TH-PFOS, 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033217\A117888\FC000028.D) 1000 900 800 -j 700 600 500 400 -j 300 200 API-ES, Neg, SIM, Frag: Var 7.285- PFOA *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033217\A117888\FC000028.D) API-ES, Neg. SIM. Frag: Var 7.754- SURROGATE mil mir 4000 3000 2000- 1000 I Compound Name -- ,-----(-----1-----1-- --- ,-----j-----r 1 246 Area Amount Meas. Ret. T ----------- u 1 1! 8 Signal Desc. 1 min TH-PFOS PFOA SURROGATE 307450.34 6871.85 35730.28 500.00 17.28 388.25 7.277 7.285 7.754 MSD1 427, EIC=426.7:427.7 MSD1 369, E1C=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04 :52 :54 pm Page 1 of 1 000055 Sample Name:L2133-20 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\1303 3279\A119872\FC0 00029.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 12:26:31 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\ 033004F .M 3/31/04 03 :59 :57 pm 29 28 1 5 nl l MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13033279\A119872\FC000029.D) 35000 4 30000 4 25000 20000 15000 -i 10000-i 5000 0 API-ES, Neg, SIM, Frag: Var 7.263 - TH-PFOS, MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033279\A119872\FC000029.D) API-ES, Neg, SIM, Frag: Var 7.272- PFOA 900 800-1 700 600 500 i !I 400300 200 'MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033279\A119872\FC000029.D) API-ES, Neg. SIM, Frag: Var 4000 -i 7.722- SURROGATE, 3500 3000 2500 -j 2000 1500 1000 500 0- Compound Name Area Amount Meas. Ret. T 8 Signal Desc. mir TH-PFOS PFOA SURROGATE 299260.06 6391.48 31405.99 500.00 16.83 347.93 7.263 7.272 7.722 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04 :53 :55 pm Page 1 of 1 000056 Sample Name:L2133-21 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13033475\A121856\FC000030.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 12:42:09 AM Seq Line Vial No. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 30 29 1 5 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13033475\A121856\FC000030.D) API-ES, Neg, SIM, Frag: Var 35000 7.261 - TH-PFOS, 30000 25000 20000 15000- 10000- 5000- 0- 6 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033475\A121856\FC000030.D) API-ES, Neg, SIM, Frag: Var 900 -i) 7.273- PFOA 800 700 600- 500- 400- 300- 200- *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033475\A121856\FC000030.D) API-ES, Neg, SIM, Frag: Var 7.725- SURROGATE 4000- 3000 2000 1000- i - , , -- , Compound Name |. 2 Area TH-PFOS PFOA SURROGATE 293701.81 5472.77 35186.57 r- '-----1 4 Amount 500.00 15.61 401.22 1----6 -- n-----1---- ->----- r 8 min Meas. Ret. T Signal Desc. 7.261 7.273 7.725 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513 , EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:54:24 pm Page 1 of 1 000057 Sample Name :L2133-22 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13033536\A123712\FC0 00 031.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 12:57:51 AM Seq Line Vial NO. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 31 30 1 5 il 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13033536\A123712\FC000031.D) 40000 35000 j 30000i 25000 - 20000 -i 15000 10000 5000 -3 0 API-ES, Neg, SIM, Frag: Var 7.278- TH-PFOS, *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033536\A123712\FC000031.D) API-ES, Neg, SIM, Frag: Var 7.289- PFOA,, 800 700 600 500 400 -3 300 200-3 "1 111 ! *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033536\A123712\FC000031 .D) 4500 4000 j 3500 4 3000 2500 i 2000 -i 1500 1000 500 0 API-ES, Neg, SIM, Frag: Var 7.752- SURROGATE, Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 305413.34 4772.74 32984.04 500.00 14.26 358.79 7.278 7.289 7.752 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7 :369.7 MSD1 513, EIC =5 1 2 .7 :513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:55:13 pm 000058 Page 1 of 1 Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13033597\A260352\FC000032.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 1:13:24 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 32 4 1 5 fj.1 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13033597\A260352\FC000032.D) API-ES, Neg, SIM. Frag: Var 30000 7.272 - TH-PFOS 25000 20000 15000 10000 - 5000 0 --I------------------ T " *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033597\A260352\FC000032.D) API-ES, Neg, SIM, Frag; Var 16000 7.278- PFOA^ 14000 12000 10000 8000- 6000 -ij 4000- 2000- o-1.. ...... *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033597\A260352\FC000032.D) 2250 2000 1750 1500 j 1250 j 1000 4 750 500250 A API-ES, Neg. SIM, Frag- Var 7.741 - SURROGATE, -.iJ Compound Name Area Amount Meas. Ret. T Signal Desc. mu TH-PFOS PFOA SURROGATE 244879.00 118710.01 16083.03 500.00 232.87 212.05 7.272 7.278 7.741 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513 , EIC=512.7 :513.7 II li li H II II II 1! il il II il il li II II Il 1 ii 1 II 1 II il il II il ii II li il ii II ** End of Report ** ==^= PC00414 Wed, 31. Mar. 2004 09:19:07 am Page 1 of 1 000059 Sample Name:solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13 033659\A12 5760\FC000 03 3 .D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 1:28:53 AM Seq Line vial NO. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 33 92 1 5 p ii 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTORV13033659\A125760\FC000033.D) API-ES, Neg, SIM, Frag: Var 35000 - 30000- 25000 - 20000 - 15000- 10000- 5000 - Oi . - ' I r ' ' I 24 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033659\A125760\FC000033.D) 7.267- TH-PFOS, M ,Ii i ;I !I | ! 1i , Tf ' 6 API-ES, Neg, SIM, Frag: Var j1 \ ' 450/ ' I 8 400/ \ 350/ 7.325- PFOA 300/ 250; /I 2 0 0 / '' i\ ; ' ....... ........." ' ......... ......................... ..,|' -- --..... .. `... 11| 1 24 *MSD1 513, EIC=512.7:513.7 (CHEMSTORV13033659\A125760\FC000033.D) 6 API-ES, Neg, SIM, Frag: Var /' V. / :\ \S 1 8 350/ 325/ 300/ 275/ 250/ 225/ 200 / 175 / \_ / '- \ y"'1' '' Compound Name ...-- - - - ___............../ I 2 Area ^-- I 4 Amount ., 6 Meas. Ret. T ,\ ! !I ii /A / \ .A 'v / ' '---------- 1---------8 Signal Desc. mi / mir mir TH-PFOS PFOA SURROGATE 270813.50 647.58 0.00 500.00 8.31 0.00 7.267 7.325 0.000 MSD1 427, EIC=426.7 :427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:55:06 pm 000060 Page 1 of 1 Sample Name:L2133-23 Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\13033831\A127872\FC000034.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 1:44:28 AM Seq Line Vial NO. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\l\METHODS\033004 F .M 3/31/04 03:59:57 pm 34 31 1 5 ill 1 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13033831\A127872\FC000034.D) 35000 30000 25000 20000 15000 10000^ 5000 0 API-ES, Neg, SIM, Frag: Var 7.280 - TH-PFOS *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033831\A127872\FC000034.D) API-ES, Neg, SIM, Frag: Var 7.290- PFOAi 700 600/ 500 / 400 300 200 MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033831\A127872\FC000034.D) 4500 i 4000 i 3500 i 3000 i 2500 2000 i 1500 -j 1000 500 i 0 -/ API-ES, Neg, SIM, Frag: Var 7.748- SURROGATE, Compound Name Area Amount Meas. R e t . T Signal Desc. mi TH-PFOS PFOA SURROGATE 299113.31 4805.65 34079.96 500.00 14.45 380.04 7.280 7.290 7.748 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:56:41 pm 000061 Page 1 of 1 Sample Name:L2133-24 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13033916\A12972 8\FC0 00 035.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 2:00:05 AM Seq Line Vial NO. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 03:59:57 pm 35 32 1 5 fil 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13033916\A129728\FC000035.D) 40000i 35000-| 30000 j 25000 4_ 200004 150004 10000 -! 5000 4 o4- API-ES, Neg, SIM, Frag: Var 7.274 - TH-PFOS *MSD1 369, EIC=368.7:369.7 (CHEMSTORM3033916\A129728\FC000035.D) API-ES, Neg, SIM, Frag: Var 1000 i 900 4 800 i 700 j 600 i 500-! 400 4 300 4 200 4. 7.281 - PFOA /\ i\ *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033916\A129728\FC000035.D) API-ES, Neg, SIM, Frag: Var 7.754- SURROGATE 4000 H 3000 iI mi mu 2000 - 1000- 0 Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 306321.38 7006.48 35915.12 500.00 17.52 391.97 7.274 7.281 7.754 MSD1 427, EIC=426.7 :427.7 MSD1 369, E I 0 3 6 8 .7 :369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04 :57 :33 pm Page 1 of 1 000062 Sample Name:L2133-25 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13033978\A131712\FC000036.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 2:15:41 AM Seq Line vial NO. Inj.No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F .M 3/31/04 03:59:57 pm 36 33 1 5 ill 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13033978\A131712\FC000036.D) API-ES, Neg, SIM, Frag: Var 35000 -j 7.265- TH-PFOS, 30000 -j 25000 - 20000 -i 15000-1 10000-^ 5000 j o-i MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13033978\A131712\FC000036.D) API-ES. Neg, SIM, Frag: Var 7.276- PFOA, 800 700 ii i! 600 500 400 - 300 200 T *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13033978\A131712\FC000036.D) API-ES, Neg, SIM, Frag: Var 5000 -J 7.729- SURROGATE, mu mir 4000- 3000 2000- 1000- 0 Compound Name Area Amount Meas. Ret. Signal Desc. min TH-PFOS PFOA SURROGATE 294770.19 5014.12 37270.63 500.00 14.88 425.38 7.265 7.276 7.729 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:58:10 pm Page 1 of 1 000063 Sample Name :L2133-26 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13034172\A133632\FC000037.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 2:31:21 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\ 033004F .M 3/31/04 03 :59 :57 pm 37 34 1 5 l *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13034172\A133632\FC000037.D) 35000 30000 25000 j 20000 4 15000 4 10000-4 5000 4 o 4} API-ES, Neg, SIM, Frag: Var 7.268 - TH-PFOS, *MSD1 369, EIC=368.7;369.7 (CHEMSTOR\13034172\A133632\FC000037.D) API-ES, Neg, SIM, Frag: Vai 7.274- PFOA 2500 4 2000 1500 1000 500-4 .... y ..... r........ *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13034172\A133632\FC000037.D) 4000- 3500 4 3000 4 2500 4 2000 4 1500 4 1000 4 500 4 0-4-- API-ES, Neg, SIM, Frag: Var 7.734- SURROGATE^ Compound Name Area Amount Meas. Ret. T Signal Desc. mi mi mi TH-PFOS PFOA SURROGATE 300039.00 21172.05 33212.82 500.00 39.06 368.42 7.268 7.274 7.734 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:59:17 pm Page 1 of 1 000064 Sample Name:L2133-27 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\130342 33\A135616\FC000038.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 2:47:00 AM Seq Line vial NO. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03:59:57 pm 38 35 1 5 I1 1 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13034233\A135616\FC000038.D) 40000 35000 30000 25000 20000 15000 10000 -E 5000 0 API-ES, Neg, SIM, Frag: Var 7.268- TH-PFOS *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13034233\A135616\FC000038.D) API-ES, Neg, SIM, Frag: Var 5000 7.275- PFOA 4000 3000 2000- 1000- *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13034233\A135616\FC000038.D) API-ES, Neg, SIM, Frag: Var 5000 7.747- SURROGATE, mir 4000 3000 2000 1000- 0 -i Compound Name Area Amount Meas. Ret. T Signal D e s c . mir TH-PFOS PFOA SURROGATE 309396.13 37705.35 38518.58 500.00 62.41 418.28 7.268 7.275 7.747 MSD1 427, EIC =4 2 6 .7 :42 7.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 04:59:43 pm Page 1 of 1 000065 Sample Name:L2133-28 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13034294\A1374 08\FC000039.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 3:02:38 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 3/31/04 03 :59 :57 pm 39 36 1 5 fjil 1 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13034294\A137408\FC000039.D) API-ES, Neg, SIM, Frag: Var 35000 -j 7.279- TH-PFOE^ 30000 4 25000 il 20000 15000-3 10000 5000 0 6 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13034294\A137408\FC000039.D) API-ES, Neg, SIM, Frag: Var 12000 7.285- PFO/y 10000 8000-J 6000 4000 2000 0 mu *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13034294\A137408\FC000039.D) 4500 i 4000 3 3500 3000 2500-3 2000 1500 1000 500 -3 API-ES, Neg, SIM, Frag: Var 7.752- SURROGATE Compound Name TH-PFOS PFOA SURROGATE Area 301672.38 94443.52 33247.03 Amount 500.00 151.01 366.68 Meas. Ret. T Signal Desc. min 7.279 7.285 7.752 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 05:00:17 pm Page 1 of 1 000066 Sample Name :L2133-2 9 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13075255\A464640\FC000040 .D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 3:18:16 AM Seq Line vial NO. Inj . N o . Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :12 :43 am 40 37 1 5 Ml 1 'MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13075255\A464640\FC000040.D) API-ES, Neg, SIM, Frag: Var 35000 7.264 - TH-PFOS, 30000 25000 20000 15000-1 10000 5000 0 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13075255\A464640\FC000040.D) API-ES, Neg, SIM, Frag: Var 1000 900 800 700-1 600 500 400 300 200 7.272- PFOA mu *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13075255\A464640\FC000040.D) API-ES, Neg, SIM, Frag: Var 4500 4000 3500 3000 2500 2000 i 15001 1000 500-1 0 7.743- SURROGATE, Compound Name Area Amount Meas. R e t . T Signal Desc. mm min TH-PFOS PFOA SURROGATE 303869.59 6630.79 34009.48 500.00 17.04 372.81 7.264 7.272 7.743 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** 000067 Sample Name :L213 3-3 0 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13075455\A467264\FC000041.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 3:33:57 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :1 2 :43 am 41 38 1 5 fil 1 'MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13075455VA467264\FC000041 .D) API-ES, Neg, SIM, Frag: Var 40000 7.258 - TH-PFOS 35000 30000 25000 20000 i 15000 A 10000 5000 04 MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13075455\A467264\FC000041.D) API-ES, Neg, SIM, Frag: Var 3500 i 7.264- PFOA, 3000 2500 2000 1500 1000 500 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13075455\A467264\FC000041 .D) API-ES, Neg. SIM, Frag: Var 4000 3500 i 3000 - 2500 2000 -lj 1500 1000^ 500 0 7.721 - SURROGATE, min Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 309346.59 26716.35 32683.64 500.00 46.23 350.45 7.258 7.264 7.721 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** 000068 Sample Name:L2133-31 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13075628\A469568\FC000042.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 3 :4 9 :35 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :12 :43 am 42 39 1 5 Ml 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13Q75628\A469568\FC000042.D) API-ES, Neg, SIM, Frag: Var 40000 -i 7.279 - TH-PFOSi 35000 30000 25000 - i i' i ;i 20000- ! 15000- 10000/ 5000/ ii 0/ ' .........................'........ ' " I .............................' ........................... ' 2 I .....' ........... " 4 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13075628\A469568\FC000042.D) 1 ' ...............!.........................1 ` 6 API-ES, Neg, SIM, Frag: Var -------------------------- 1 8 8001 7.290- PFOA, 700/ 600- j1 i' 500 400 i 300 4 A ' ' / 200 / ---- 1-----1-----<-----1-----1 1 1 i 24 *MSD1 513, EIC-512.7:513.7 (CHEMSTOR\13075628\A469568\FC000042.D) 'i 1 6 API-ES, Neg, SIM, Frag: Var ' i 8 4000/ 3500/ 3000/ 2500/ 2000/ 1500/ 1000/ 500/ 0J ....... -........................ ........................ 1 Compound Name 1" 1 ............." r 2 Area 7.764- SURROGAT^, i: ii ' 1 ' ......... ' 4 11 6 Amount Meas. Ret. T 1 " '' '' 1 8 Signal Desc. mi ^^ 1----- r_ mir ' -r- mir TH-PFOS PFOA SURROGATE 303647.50 5664.11 33678.26 500.00 15.62 369.20 7.279 7.290 7.764 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Thu, 1. Apr. 2004 10:18:49 am Page 1 of 1 000069 Sample Name:L2133-32 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13075764\A472256\FC000043.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 4:05:16 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 4/1/04 10:12:43 am 43 40 1 5 /il 1 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13075764\A472256\FC000043.D) API-ES, Neg, SIM, Frag: Var 7.269- TH-PFOS, 35000 30000 j 25000 20000 15000 10000 5000-3 0 ...V v-- *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13075764\A472256\FC000043.D) 1800 i 1600 -j 1400 -j 1200 -j 1000 J 800 -j 600 -j 400 -j 200- /t API-ES, Neg, SIM, Frag: Var 7.277- PFOA *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13075764\A472256\FC000043.D) 4000 i 3500 3000 2500 2000 E 1500 1000 j 500 - 0 API-ES, Neg, SIM, Frag: Var 7.731 - SURROGATE mu Compound Name Area Amount Meas. R e t . T Signal Desc. TH-PFOS PFOA SURROGATE 304940.03 12592.52 30228.34 500.00 25.82 327.36 7.269 7.277 7.731 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Thu, 1. Apr. 2004 10:19:43 am Page 1 of 1 000070 Sample Name:STD 250 ppb Sample Info; Data file :C :\HPCHEM\l\DATA\Chemstor\13 03487 0\A284032\FC000044.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 4:20:50 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 44 4 1 5 /il 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13034870\A284032\FCC00044.D) API-ES, Neg, SIM, Frag: Var 30000 / 7.262- TH-PFOS.i! 25000 - 20000 / 15000 10000/ 5000 / r ---------------- T - ------- --------- 1-------------------1----------- _________ 6_______ 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13034870\A284032\FC000044.D) APtES, Neg, SIM, Frag: Var 14000 7.270- PFOA, ii 12000- 10000/ 8000- 6000 / 4000 - 2000- oi *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13034870\A284032\FC000044.D) API-ES, Neg, SIM, Frag: Var 7.731 - SURROGATE 2000 5 1750 -j 1500 \ 1250 -j 1000/ 750 / 500-: 250 5 .. 8________ m 8 ___ mi. Compound Name 2 Area 46 Amount M e a s . Ret. T 8 Signal Desc. mil TH-PFOS PFOA SURROGATE 238043.88 114189.80 15935.87 500.00 230.42 216.33 7.262 7.270 7.731 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7 :369.7 MSD1 513 , EIC=512.7 :513.7 11 II II li II II li II II II 11 II II II II il II II II II II End of Report *** ==== = = = = = = = = = = = = = = PC00414 Wed, 31. Mar. 2004 09:20:13 am Page 1 of 1 000071 Sample Name :solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13075865\A474560\FC000045.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 4:36:19 AM Seq Line vial NO. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :12 :43 am 45 92 1 5 jul 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13075865\A474560\FC000045.D) API-ES, Neg, SIM, Frag: Var 35000 7.270- TH-PFOS, 30000-3 25000 20000 -3 15000 10000 5000 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13075865\A474560\FC000045.D) API-ES, Neg, SIM, Frag: Var 400350 300 250 200 7.344- PFOA mt *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13075865\A474560\FC000045.D) API-ES, Neg, SIM, Frag: Var 340 320 300 -3 280 260 240 220 -I 200 -j 180 mtr Compound Name Area Amount Meas. Ret. T Signal Desc. min TH-PFOS PFOA SURROGATE 269087.53 795.73 0.00 500.00 8.56 0.00 7.270 7.344 0.000 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=3 68.7:369.7 MSD1 513 , EIC=512.7:513.7 *** End of Report *** PC00414 Thu, 1. Apr. 2004 10:21:07 am Page 1 of 1 000072 Sample Name:L2133-33 Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13075 965\A4 77184\FC0 0004 6 .D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 4:51:58 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 4/1/04 10:12:43 am 46 41 1 5 i 1 1 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13075965\A477184\FC000046.D) API-ES, Neg, SIM, Frag: Var 7.276 - TH-PFOSj 35000 30000 25000 -3 20000 15000 10000 5000 -t| 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13075965\A477184\FC000046.D) API-ES, Neg, SIM, Frag: Var 2000 7.283- PFOA 1750 1500 1250 1000^ 750 500 250 mi *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13075965\A477184\FC000046.D) API-ES, Neg, SIM, Frag: Var 4500 4000 3500 3000 i 2500 - 2000 1500 rj 1000 500 7.757- SURROGATE 0 Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 301122.06 14898.15 33244.16 500.00 29.52 367.37 7.276 7.283 7.757 MSD1 427, EIC=426.7 :427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 1 il li il li II II II II II il II II il II II II * End of Report ======== ==== II IIII ii II II II H II II II H II 1! II II PC00414 Thu, 1. Apr. 2004 10:22:04 am Page 1 of 1 000073 Sample Name:L2133-34 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13076098\A479616\FC000047.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 5:07:34 AM Seq Line vial NO. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 4/1/04 10:12:43 am 47 42 1 5 ill 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13076098\A479616\FC000047.D) API-ES, Neg, SIM, Frag: Var 40000 7.273 - TH-PFOS, 35000 4 30000 25000 20000 4 15000 10000 4 5000 04 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13076098\A479616\FC000047.D) API-ES, Neg, SIM, Frag: Var 1600 7.280- PFOA 1400 1200 1000 :I iI 800 600 400 200- MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13076098\A479616\FC000047,D) API-ES, Neg, SIM, Frag: Var 4000 3500 3000 2500 2000 7.740- SURROGATE, 1500 4 1000 500 4 Compound Name J 11 2 1 ^-----1-----1---4 1 1 1-----1-----1-----r 68 Area Amount Meas. R e t . T , Signal Desc. mir TH-PFOS PFOA SURROGATE ================*= 303977.50 11583.06 32820.80 500.00 24.38 358.69 7.273 7.280 7.740 ** End of Report MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=3 6 8.7:369.7 MSD1 513, EIC=512.7:513.7 ======== = = = = == =:= == = == == PC00414 Thu, 1. Apr. 2004 10:23:15 am Page 1 of 1 000074 Sample NameL2133-35 Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13076185\A482304\FC000048.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 5:23:11 AM Seq Line vial No. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\l\METHODS\033004F. M 4/1/04 10:12:43 am 48 43 1 5 M1 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13076185\A482304\FC000048.D) API-ES, Neg, SIM, Frag: Var 35000 7.269- TH-PFOS, 30000 25000 20000 15000 10000 5000 0- MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13076185\A482304\FC000048.D) 2250 2000 1750 1500 1250 1000750 500 250- /\ API-ES, Neg, SIM, Frag: Var 7.277- PFOA mi *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13076185\A482304\FC000048.D) API-ES, Neg, SIM, Frag: Var 4000 -j 3500 7.747- SURROGATE- I 3000 -j 2500 -j 2000 -j 1500 4 1000 500 Compound Name --- ,-----1--------- -----,-----1 24 Area Amount 1 6 Meas. Ret. T 1-----'-----1-----18 Signal Desc. TH-PFOS PFOA SURROGATE 302776.56 16011.21 31464.02 500.00 31.06 344.29 7.269 7.277 7.747 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 li tl li II II li il il II li li il li II il il II tl II Il 1 || l II II II II II II II it II II II II II II II II II II II II k* End of Report * PC00414 Thu, 1. Apr. 2004 10:24:25 am Page 1 of 1 000075 Sample Name:STD 250 ppb Sample Info : Data file :C:\HPCHEM\l\DATA\Chemstor\13035313\A293888\FC000049.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 5:38:47 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 49 4 1 5 11 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTORU 3035313\A293888\FC000049.D) API-ES, Neg, SIM, Frag: Var 30000 - 7.273 - TH-PFOS, 25000 - 20000 - 15000- 100005000- i1 0- ' [ ' 1 ' 1 246 8 *MSD1 369, EIC=368.7:369.7 (CHEMSTORV13035313\A293888\FC000049.D) API-ES, Neg, SIM, Frag: Var mi 14000 12000 / 7.280- PFOA) : 10000- 8000 / 6000/ ;j 4000/ 2000/ o- , , , | i i i | ' ' 1 11 246 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13035313\A293888\FC000049.D) API-ES, Neg, SIM, Frag: Var 111 8 min 2000 / 7.760- SURROGATE, 1750/ 1500/ 1250/ 1000/ 750/ :i 500/ 2 5 0 /: Compound Name 2 Area 4 Amount `I 6 Meas. Ret. T '---1./. .. t_ __ ___ 11 8 Signal Dse. min TH-PFOS PFOA SURROGATE 241887.81 114801.61 15566.03 500.00 227.96 207.58 7.273 7.280 7.760 MSD1 427 , EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513 , EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:21:17 am Page 1 of 1 000076 Sample Name:solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13076277\A484608\FC000050.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 5:54:19 AM Seq Line Vial No. Inj. No. Inj. Voi. Acq. Method Analysis Method Last Changed POAASUR.M C:\HPCHEM\1\METHODS\033004F.M 4/1/04 10:12:43 am 50 92 1 5 l 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13076277\A484608\FC000050.D) API-ES, Neg, SIM, Frag: Var 35000 t 7.276 - TH-PFOS, 30000 4 25000 4 20000 4 15000 ^ 100004 5000 4 i i o l --- ^ .;-- | ---- ;--- | | ... ;--- ________________________________ 2__________________________4___________ __________ 6_______ *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13076277\A484608\FC000050.D) API-ES, Neg, SIM, Frag: Var T 8 mil 400 -j 350 300 250 200 - i 7.345- PFOA 4 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13076277\A484608\FC000050.D) API-ES, Neg, SIM, Frag: Var 340 -E 320 4 300 4 280 t 260 4 240 4 220 J 200 t 180 t , 'X' 160 ^ Compound Name X. 2__________________________ 4__________________________ 6 Area Amount Meas. Ret. T T _______ 8 Signal Desc. mir TH-PFOS PFOA SURROGATE 270083.06 863.55 0.00 500.00 8.67 0.00 7.276 7.345 0.000 MSDl 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSDl 513, EIC=512.7 :513.7 *** End of Report *** PCO 0414 Thu, 1. Apr. 2004 10:25:15 am Page 1 of 1 000077 Sample Name:STD 10 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\1303 5435\A2 97 792\FC0 00 051.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 6:09:52 AM Seq Line vial NO. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F. M 3/31/04 09:05:00 am 51 1 1 5 pi 1 25000 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13035435\A297792\FC000051.D) API-ES, Neg, SIM, Frag: Var 7.278- TH-PFOS, 20000 15000 10000-j 5000 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTORU3035435\A297792\FC000051 .D) API-ES, Neg, SIM, Frag: Var 900 -j 7.290- PFOA-, 800 -j 700 -j 600 4 500 400 300 200 6 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13035435\A297792\FC000051.D) API-ES, Neg, SIM, Frag: Var 340 320 -i 300 4 280 4 260 4 240 -j 220 4 200 4 180 7.764- SURROGATE-, mi mir Compound Name Area Amount Meas. Ret. T Signal Desc. min TH-PFOS PFOA SURROGATE 263472.88 6735.55 1258.45 500.00 18.73 13.65 7.278 7.290 7.764 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Wed, 31. Mar. 2004 09:28:35 am 000078 Page 1 of 1 Sample Name:STD 50 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13076373\A487424\FC000052.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 6:25:25 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\033004F .M 4/1/04 10 :12 :43 am 52 2 1 5 /il 1 30000 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13076373\A487424\FC000052.D) API-ES, Neg, SIM, Frag: Var 7.264 - TH-PFOS 25000 -i 20000 -i 15000 10000 * 5000 0 6 MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13076373\A487424\FC000052.D) API-ES, Neg, SIM, Frag. Var 7.272- PFOA 3000 2500 1 2000 1500 1000 500 " MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13076373\A487424\FC000052.D) API-ES, Neg. SIM, Frag: Var 700- 7.725- SURROGATE* 600-i 500 400 -j 300 200 mir Compound Name Area Amount Meas. Ret. T Signal Desc. mm TH-PFOS PFOA SURROGATE 261640.47 24845.60 3856.23 500.00 50.14 45.18 7.264 7.272 7.725 MSD1 427, EIC=426.7 :427.7 MSD1 369, EIC =3 6 8 .7 :369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Thu, 1. Apr. 2004 10:26:18 am Page 1 of 1 000079 Sample NamerSTD 100 ppb " Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\1307 6461\A489984\FC000053.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 6:41:01 AM Seq Line vial N o . Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :12 :43 am 53 3 1 5 /il 1 *MSD1 427, IC=426.7:427.7 (CHEMSTOR\13076461\A489984\FC000053.D) API-S, Neg, SIM, Frag- Var 7.274 - TH-PFOS 30000 i 25000 i 20000 15000 10000 5000 -3 0 ` MSDI 369 EIC=368.7:369.7 (CHEMSTOR\13076461\A489984\FC000053.D) 6000 i API-ES, Neg, SIM, Frag: Var 7.280 PFOA 5000 4000 t 3000 2000- 1000- 0 *MSD1 513, EIC=512.7:513.7 <CHEMSTOR\13076461 \A489984'FC000053.D) 1000 API-ES, Neg, SIM, Frag: Var 7.748 - SURROGATS 800- 600 400 200-I Compound Name TH-PFOS PFOA SURROGATE Area 264437.66 49178.01 7253.66 Amount 500.00 91.83 85.86 Meas. Ret. T Signal Base. 7.274 7.280 7.748 MSDI 427, EIC=426.7:427.7 MSDI 369, EIO-3 6 8 .7:369.7 MSDI 513, EIC=512.7:511.7 *** End of Report *** PC00414 Thu, 1. Apr. 2004 10:26:59 am Page 1 of 1 0008o Sample Name:STD 250 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13076550\A492352\FC000054.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 6:56:35 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :12 :43 am 54 4 1 5 pi 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13076550\A492352\FC000054.D) API-ES, Neg, SIM, Frag: Var 30000 ^ 7.272- TH-PFOS, 25000 ^ 20000 -E 15000- 10000 -E 5000 0 MSD1 369, EIC=368.7:369.7 (CHEMSTORV13076550\A492352\FC000054.D) API-ES, Neg, SIM, Frag: Var 16000 7.279- PFOA 14000 12000 M 10000 8000 6000 -E 4000 -E 2000 0 mi *MSD1 513, EIC=512.7:513,7 (CHEMSTOR\13076550\A492352\FC000054.D) API-ES, Neg, SIM, Frag: Var 2000 i 7.759- SURROGATE 1750 i 1500 -i 1250 1000 1 750 500 250 Compound Name Area Amount Meas. Re t . T Signal Desc. mir TH-PFOS PFOA SURROGATE 247451. 16 119024. 13 15913.5 0 500.00 231.05 207.44 7.272 7.279 7.759 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513,7 *** End of Report *** PC00414 Thu, 1. Apr. 2004 10:29:06 am Page 1 of 1 0f)0 81 Sample Name:STD 500 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13076612\A494656\FC000055 .D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 7:12:13 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed POAASUR.M C :\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :12 :43 am 55 5 1 5 (Jil 1 MSD1 427, EIC=426.7:427 7 (CHEMSTORM3076612\A494656\FC000055.D) API-ES, Neg, SIM, Frag: Var 30000 7.268 - TH-PFOSi 25000 20000 15000 4 10000- 5000 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTORM3076612\A494656\FC000055.D) API-ES, Neg, SIM, Frag: Var 30000 4 7.276- PFOA 25000 4 20000 15000 10000 5000 -3 0 MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13076612\A494656\FC000055.D) 4000 3500 3000 4 2500 2000 1500 -j iooo 4 500 0 API-ES, Neg, SIM, Frag: Var 7.737- SURROGATE^. Compound Name Area Amount Meas. Ret. T Signal Desc. rrur min TH-PFOS PFOA SURROGATE 238222.09 235420.88 31545.33 500.00 487.38 447.35 7.268 7.276 7.737 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 IIIIIIII IIIt IIIIIIIfIIII IIII u II >1 I|I| 11 |j|| 1 It 1l I|I| If 111IIII111IIII It IIII II II1II! II II * End of Report it ie ir = = === PC00414 Thu, 1. Apr. 2004 10:29:53 am Page l of 1 000082 Sample Name:STD 750 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13076674\A497152\FC000056.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 7:27:50 AM Seq Line Vial No. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :12 :43 am 56 6 1 5 fll 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13076674\A497152\FC000056.D) 25000 20000 - API-ES, Neg, SIM, Frag: Var 7.270- TH-PFO& 'i j 15000 10000- 5000- i j| I !( I '. 0- L -- ,-- , , , ..........r . i..................-.......... | - ............-< i 2 46 -MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13076674VA497152\FC000056.D) API-ES, Neg, SIM, Frag: Var ' -- r" .............. r................ ^ 8 mi 45000 i 40000 4 35000 4 30000 4 25000 i 20000 i 15000 4 10000i 5000 4 04 ---------- , i i ] < i <-- - ] i 24 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13076674\A497152\FC000056 D) 7.278 - i ^y T 6 API-ES, Neg, SIM, Frag: Var PFOAj, I !i fi jl I\ r1 1 r 8 mil 50004000 4 3000/ 7.744- SURROGATE, 1j ;1 i' 1| I| 2000 4 10004 0- Compound Name i1 / 1-----1-----1-----'-----1-----1-----1-----r-- --- 1----- 1-----1-----r----- 1-- -- 1----- r 2___________________________ 4___________________________ 6____________________________ 8 ___ mil Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 219595.55 341079.84 45337.44 500.00 805.66 737.19 7.270 7.278 7.744 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Thu, 1. Apr. 2004 10 :30 :21 am Page 1 of 1 000083 Sample Name:STD 1000 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13076736\A499648\FC000057.D Injection Date Acq Operator Instrument Dilution 3/31/04 jmiller PC00414 1 7:43:29 AM Seq Line vial NO. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\033004F. M 4/1/04 10 :12 :43 am 57 7 1 5 x1 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13076736\A499648\FC000057.D) API-ES, Neg, SIM, Frag: Var 30000 7 7.274- TH-PFOS 25000 / 20000 15000 10000 5000 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13076736\A499648\FC000057.D) API-ES, Neg, SIM, Frag: Var 1 50000 1 7.281 - PFOA 40000 30000 20000 / 10000/ 0 'MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13076736\A499648\FC000057.D) API-ES, Neg, SIM, Frag: Var ........ ... 7000 7.748- SURROGATE, 6000-3 5000 4000 3000 -j 2000 4 1000 0 Compound Name TH-PFOS PFOA SURROGATE Area 237026.95 432297.72 59473.75 Amount 500.00 974.55 930.94 Meas. Ret. T Signal Desc. 7.274 7.281 7.748 MSD1 427, EIC--.-426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC-512.7:513.7 *** End of Report *** PC00414 Thu, 1. Apr. 2004 10:31:18 am Page 1 of 1 000084 Sequence: C:\HPCHEM\1\SEQUENCE\040104.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 51 11 Vial 4 12 Vial 92 13 Vial 1 14 Vial 2 15 Vial 3 16 Vial 4 17 Vial 5 18 Vial 6 19 Vial 7 STD 10 ppb STD 10 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb solvent blank L2133-10 2X STD 250 ppb solvent blank STD 10 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb POAASUR 1 Sample POAASUR 1 Calib POAASUR 1 Calib POAASUR 1 Calib POAASUR 1 Calib POAASUR 1 Calib POAASUR lv Calib POAASUR 1 Calib POAASUR 1 Sample POAASUR 1 Sample POAASUR 1 Sample POAASUR 1 Sample POAASUR 1 Calib POAASUR 1 Calib POAASUR 1 Calib POAASUR 1. Calib POAASUR 1 Calib POAASUR 1 Calib POAASUR 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 13 Vial 1 14 Vial 2 15 Vial 3 16 Vial 4 17 Vial 5 18 Vial 6 19 Vial 7 STD 10 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb STD 10 ppb STD 50 ppb STD 100 ppb STD 250 ppb STD 500 ppb STD 750 ppb STD 1000 ppb POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR POAASUR 1 Replace Average 2 Replace Average 3 Replace Average 4 Replace Average 5 Replace Average 6 Replace Average 7 Replace Average T X 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 O -2 -2 -2 -2 -2 -2 -2 LCMS3 4/1/04 10:50:45 AM jmiller Of 000085 Page I of 1 Method C:\HPCHEM\1\METHODS\040104F.M Calibration Table Calib. Data Modified Friday, April 02, 2004 8:47:24 AM Calculate Based on Internal Standard Peak Area Rel . Reference Window A b s . 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 We ight: Quadratic (some peaks differ, see below) Included (some peaks differ,, see below) Equal (some peaks differ, see below) 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) Default Sample ISTD Information (if not set in sample table): ISTD ISTD Amount Name # [ppb] 500.00000 TH-PFOS Signal 1 : MSD1 427, EIC= 426.7:427.7 Signal 2 : MSD1 369, EIC= 368.7:369.7 Signal 3 ; MSD1 513, EIC= 512.7 :513.7 RetTime Lvl Amount Area Amt/Area Ref Grp Name [min] Sig [ppb] 11__ I1 _ I1. II__________ 7.366 1 1 500.00000 3.56778e5 ^1.40143e-3 ""i" i II TH-PFOS 2 500.00000 3.50146e5 1.42797e-3 3 500.00000 3.542 04e5 1.41162e-3 4 500.00000 3.08978e5 1.61824e-3 5 500.00000 3.05992e5 1.63403e-3 6 500.00000 2.78856e5 1.79304e-3 7 500.00000 2.95806e5 1.69030e-3 7.375 2 1 10.00000 7730.66968 1.29355e-3 1 PFOA 2 50.00000 2.83580e4 1.76317e-3 3 100.00000 6.83229e4 1 .46364e-3 4 250.00000 1.23253e5 2.02835e-3 5 500.00000 2.71475e5 1.84179e-3 6 750.00000 3.89000e5 1.92802e-3 7 1000.00000 4.58630e5 2.18041e-3 7.794 3 1 10.00000 1211.51978 8.25410e-3 1 SURROGATE 2 50.00000 4570.3.6548 1.094 0Oe-2 3 100.00000 8758.15869 1.14179e-2 4 250.00000 1.72 815e4 1.44663e-2 5 500.00000 3.49914e4 1.42892e-2 6 750.00000 5.04186e4 1.4 8755e-2 7 1000.00000 6.30135e4 1.58696e-2 >000414 4/2/04 8:50:55 AM jmiller V 000086 Page 1 of 3 Method C:\HPCHEM\1\METHODS\040104F.M More compound-specific settings: Compound: T H -PFOS Time Window From 5.746 min To 8.166 min Curve Type Linear Origin Forced Calibration Level Weights / Level 1 1 Level 2 1 Level 3 1 Level 4 1 Level 5 1 Level 6 1 Level 7 1 Compound : PFOA Time Window From 5.746 min To 8.194 min Compound: SURROGATE Time Window From 7.274 min To 8.625 m i n : Peak Sum Table ***No Entries in table*** Area Ratio - 0.80.60.40.2- o-f0 Calibration Curves / -i-- I-- I-- I-- I-- I-- r 0.5 1 Amount Ratio TH-PFOS at exp. RT: 7.366 MSD1 427, EIC=426.7;427.7 Correlation: 1.00000 Residual Std. Dev.: 0.00000 Formula: y = mx m: 1.00000 x: Amount Ratio y: Area Ratio Calibration Level Weights: Level 1 :1 Level 2 :1 Level 3 :1 Level 4 :1 Level 5 :1 Level 6 :1 Level 7 :1 PFOA at exp. RT: 7.375 MSD1 369, EIC=368.7:369.7 Correlation: 0.99608 Residual Std. Dev.: 0.06020 Formula: y = a x ' + bx + c a: -1.22587e-l b: 1.05531 C: -2.02004e-2 x: Amount Ratio y: Area Ratio PC00414 4/2/04 8:50:55 AM jmiller V 000087 Page 2 of 3 Method C:\HPCHEM\1\METHODS\040104F.M SURROGATE at exp. RT: 7.794 MSD1 513, EIC=512.7:513.7 Correlation; 0.99821 Residual Std. Dev.: 0.00543 Formula: y = ax J + bx + c a: -1.00284e-2 b: 1.2 9210e -1 c: -7.987 98e-4 X: Amount Ratio y: Area Ratio 3C00414 4/2/04 8:50:55 AM jmiller / & * ? 000088 Page 3 of 3 Sample Name:STD 10 ppb Sample Info:Warm up l Data file :C:\HPCHEM\l\DATA\Chemstor\13087308\A913408\FC000001.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 11:37:41 AM Seq Line Vial N o . Inj. No. Inj. Voi. : : : 1 1 1 5 /il Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\040104F.M 4/2/04 08:47:26 am Initials Date ... __ _____V V o v Run#_F<Lc^oooo i 1 q F c go c o t i MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13087308\A913408\FC000001.D) API-ES, Neg, SIM, Frag: Var 7.384- TH-PFOS 40000 30000 20000 10000-j 0 MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13087308\A913408\FC000001.D) API-ES, Neg, SIM, Frag: Var 1600 7.402- PFO/V 1400 1200 -z 1000 800 600 400 200 --1------------------ r~ *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13087308\A913408\FC000001.D) 6 API-ES, Neg. SIM, Frag: Var 1800 1600 1400 1200 -3 1000 800 -3 600 400-3 200 7.797- SURROGATE m Compound Name TH-PFOS PFOA SURROGATE Area 356990.38 11158.69 1354.99 Amount 500.00 24.52 17.83 Meas. Ret. T Signal Desc. 7.384 7.402 7.797 MSD1 427, EIC=426.7:427.7 MSD1 369, El0=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 08:53 :25 am Page 1 of 1 000089 Sample Name:STD 10 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13 0873 94\A915392\FC000002.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 11:53:13 AM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 2 1 1 5 il 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13087394\A915392\FC000002.D) API-ES, Neg, SIM, Frag: Var 35000 7.376 - TH-PFOS 30000 25000 -3 20000 15000 10000 5000 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13087394\A915392\FC000002.D) API-ES, Neg, SIM, Frag: Var 1000900800- 700 J 600- 500 - j 400 - j 300 4 200 / -------- .............................-- - --- --------- --- -- -- ------------------------- --- ....-------------------- ------- - --...... i 24 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13087394\A915392\FC000002.D) 7.382- PFOA f* i5 ; i! /i ________ 11i 6 API-ES, Neg, SIM, Frag: Var i/ ... / '\ 1 8 350/ 7.799- SURROGATE-, 325/ 300/ 275-; 250/ 225 / 200/ .... 175 / ....................X . ,, Compound Name ^ \ ,| 2 Area ........ ............................................................. 1' I 4 Amount / " " ..... 6 Meas. Ret. T j f\ i ! .'~ y ' \ .l' 'V ' ' " i 8 Signal Desc. /. mi s '" mir min TH-PFOS PFOA SURROGATE 354735.72 7660.40 969.38 500.00 19.89 13.69 7.376 7.382 7.799 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 08:54:17 am Page 1 of 1 000090 Sample Name:STD 50 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13 0374 55\A917504\FC0 000 03.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 12:08:49 PM Seq Line vial NO. Inj. No. Inj. Vol. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\040104F. M 4/2/04 08 :47:26 am 3 2 1 5 /I 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13087455\A917504\FC000003.D) API-ES, Neg, SIM, Frag: Var 35000 7.366 - TH-PFOSj; 30000 25000 1 20000 -j 15000 -j 100001 5000 04 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13087455\A917504\FC000003.D) API-ES, Neg, SIM, Frag: Var 30001 7.372- PFOA 25001 20001 1500 1000 500 mi *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13087455\A917504\FC000003.D) API-ES, Neg. SIM, Frag: Var 700 7.789- SURROGATE, 600 500 400 300 200- mir Compound Name Area Amount Meas. R e t . T Signal Desc. min TH-PFOS PFOA SURROGATE 352644.63 28374.35 4789.71 500.00 48.23 56.14 7.366 7.372 7.789 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 08:56:29 am Page 1 of 1 000091 Sample Name-.STD 100 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13087564\A919424\FC000004.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 12:24:24 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\l\METHODS\040104F. M 4/2/04 08:47:26 am 4 3 1 5 (il MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13087564\A919424\FC000004.D) API-ES, Neg. SIM, Frag: Var 35000 7.368 - TH-PFOS, 30000 25000 20000 15000 10000 3 5000 0 "1 6 MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13087564\A919424\FC000004.D) API-ES, Neg, SIM, Frag: Var 7000-3 7.374- PFOA 6000 5000 4000 3000 2000 1000-3 1000 MSD1 513. EIC=512.7:513.7 (CHEMSTOR\13087564\A919424\FC000004.D) API-ES, Neg, SIM, Frag: Var 7.794- SURROGATE, 800 1 mi m 200 -. 1 1 -- ,-----|-----r---- 12 Compound Name Area TH-PFOS PFOA SURROGATE 351885.25 66469.05 8635.50 '1 4 Amount 500.00 101.46 99.60 -- [-----r ' ' 1 68 Meas. Ret. T Signal Desc. min 7.368 7.374 7.794 MSD1 427, EIC=426.7 :427.7 MSD1 369, EIC=368.7 :369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 08:57:27 am 000092 Page 1 of 1 Sample Name:STD 250 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13087601\A921408\FCOOO005.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 12:40:00 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\04010 4F .M 4/2/04 08:47:26 am 5 4 1 5 (il 1 *MSD1 427. E10=426.7:427.7 (CHEMSTOR\13087601\A921408\FC000005.D) 35000 30000 25000 5 20000 15000 10000 5000 0 API-ES, Neg, SIM, Frag: Var 7.367 - TH-PFOS *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13087601\A921408\FC000005.D) API-ES,'Neg, SIM, Frag: Var 16000 14000 7.374- PPOA 12000 10000 8000 6000 4000 2000 0 T" 4 *MSD1 513, EIC=512.7:513 7 (CHEMSTOR\13087601\A921408\FC000005.D) r " -- r-- API-ES, Neg, SIM, Frag: Var 7.792- SURROGATE, 2000 1500 -j 1000 500- mi mu II 1 II 1 II 1 II 1 II It II II li II II II II II II II II II It II II Compound Name TH-PFOS PFOA SURROGATE Area 308243.25 124214.29 17317.49 Amount 500.00 210.82 228.61 Meas. Ret. T Signal Desc. 7.367 7.374 7.792 MSD1 427, EIC=426.7:427.7 MSD1 369, ElC=3 68.7:369.7 MSD1 513, EIC =5 1 2 .7 :513.7 ** End of Report ==== ================ PC00414 Fri, 2. Apr. 2004 08:58:48 am Page 1 of 1 000093 Sample Name:STD 500 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13087844\A923264\FC000006.D Injection Date Acg Operator Instrument Dilution 4/1/04 jmiller PC00414 1 12:55:35 PM Seq Line Vial No. Inj . N o . Inj. Vol. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 6 5 1 5 Ml 1 MSD1 427, EIC=426.7:427 7 (CHEMSTOR\13087844\A923264\FC000006.D) API-ES, Neg, SIM, Frag: Var 30000 7.371 - TH-PFO& 25000 20000 15000-3 10000 5000 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13087844\A923264\FC000006.D) 25000 API-ES, Neg, SIM, Frag: Var 7.378- PFOA 20000 15000 10000 5000 0- *MSD1 513, EIC=512.7:513.7 <CHEMSTC>R\13087844\A923264\FC000006.D) API-ES, Neg, SIM, Frag: Var mir 3500 i 7.792- SURROGATE 3000 4 2500 -! 2000 -j 1500 / 1000 500 - 0J---- r---- "I----- r------1-----' --- i-----'-----1 :-- 1-- --'-----'-----1-----' 1------ --1-----1-----1-----r ________ ______________________2 _________________________ 4__________________________6______________ .___________ 8________ min Compound Name Area Amount Meas. Ret. T Signal Desc. T H -PFOS PFOA SURROGATE 307319.81 270138.06 34356.35 500.00 479.44 469.98 7.371 7.378 7.792 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513 , EIC=512.7:513.7 II it II II II 1! II II II II II II II II II II II II It II II II II II II II II If II II II II II II 1 II 1 II 1 II *** End of Report == = = = PC00414 Fri, 2. Apr. 2004 09:00:14 am Page 1 of 1 000094 Sample Name:STD 750 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13088724\A925312\FC000007.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 1:11:12 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 7 6 1 5 fil 1 ! *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13088724\A925312\FC000007.D) API-ES. Neg, SIM, Frag: Var 25000 - 7.365 - TH-PFO, 20000 15000- 11 jI :1 10000- 5000- 0^ r 7I T 11l 246 *MSD1 369. EIC=368.7:369.7 (GHEMSTOR\13088724\A925312\FC000007.D) API-ES, Neg, SIM, Frag: Var !\ / 1 I 8 mil 40000 -j 7.373- PFOA 35000 / 30000 / 25000 j ;1 20000 - 15000 / 10000j 5000 / O/ ' ' 111` 11 24 ' ' 1' 6 *MSD1 513, EIC=512.7:513.7(CHEMSTORV13088724\A925312\FC000007.D) API-ES, Neg, SIM, Frag: Var 1 ! 8 1 min 5000 - 7.791 - SURROGATE 4000 3000/ 2000/ iI : 1000/ 0- 1 1 1 I 1 I 2 Compound Name Area I JI 46 Amount Meas. Ret. T 1 "1-- 8 Signal Desc. >-- min TH-PFOS PFOA SURROGATE 277681.97 385419.88 48821.63 500.00 825.51 777.22 .7.365 7.373 7.791 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC =512.7 :513.7 *** End of Report *** PC00414 Pri, 2. Apr. 2004 09:01:17 am Page 1 of 1 000095 Sample Name:STD 1000 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13089884\A927296\FC000008.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 1:26:48 PM Seq Line Vial No. Inj. No. Inj . V o i . : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\040104F.M 4/2/04 08:47:26 am 8 7 1 5 PlI 1 25000 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13089884\A927296\FC000008.D) API-ES, Neg, SIM, Frag: Var 7.364- TH-PFOSf; 20000 15000 10000-j 5000 0 'MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13089884\A927296\FC000008.D) API-ES, Neg, SIM, Frag: Var 7.373- PFOA* 40000 mi 30000 20000 - 10000- 0- MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13089884\A927296\FC000008.D) API-ES, Neg. SIM, Frag: Var 6000 7.795- SURROGATE. 5000-3 4000 3000 2000 1000 0^1 mu Compound Name Area Amount Meas. Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 294882.97 458266.38 63190.88 500.00 959.97 982.02 7.364 7.373 7.795 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7 :369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:01:49 am Page 1 of 1 000096 Sample Name:solvent blank Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13090445\A929408\FC000009.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 1:42:18 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\040104F.M 4/2/04 08:47:26 am 9 92 1 5 (il 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13090445\A929408\FC000009.D) API-ES, Neg, SIM, Frag: Var 40000 35000 30000 25000 i 20000 4 15000 10000^ 5000 0 7.371 - TH-PFOS, 'MSD1 369. EIC=368.7:369.7 (CHEMSTOR\13090445\A929408\FC000009.D) API-ES. Neg, SIM, Frag: Var 375 - 350 325 300 ^ 275 250 225 200 -X. 175 mu *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13090445\A929408\FC000009.D) API-ES, Neg. SIM, Frag: Var 320 300^ 2 8 0 - 260 240 " 220 200 180 \ /\/ ' Compound Name Area Amount Meas. R e t . T Signal Desc. min TH-PFOS PFOA SURROGATE 346065.75 0.00 0.00 500.00 0.00 0.00 7.371 0.000 0.000 MSD1 427 , EIC=426.7 :427.7 MSD1 369, EIC=3 68.7:369.7 MSD1 513 , EIC=512.7 :513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:02:28 am Page 1 of 1 000097 Sample Name:L2133-10 2X Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13090 966\A931392\FC000 010.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 1:57:55 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\l\METHODS\04 0104 F .M 4/2/04 08:47:26 am 10 51 1 5 fil 1 'MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13090966\A931392\FC000010.D) API-ES, Neg, SIM, Frag: Var 30000 7.366 - TH-PFOS, 25000 20000 15000 -3 10000 5000 0 MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13090966\A931392\FC000010.D) API-ES, Neg, SIM, Frag: Var 30000 ^ 7.372- PFOA 25000 20000 -3 15000 10000 5000 -i] 0 -T ------------------ T " *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13090966\A931392\FC000010.D) API-ES, Neg, SIM, Frag: Var 2250 j 2000 4 1750 -j 1500 4 1250 4 1000 4 750 4 500 4 250 4 7.785 - SURROGATE, mu Compound Name TH-PFOS PFOA SURROGATE Area 247135.17 254884.70 15840.49 Amount 500.00 575.04 261.76 Meas. Ret. T Signal Desc. 7.366 7.372 7.785 MSD1 427, EIC=426.7 :427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 ;513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:03:32 am Page 1 of 1 000098 Sample Name:STD 250 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\1309163 2\A93 3312\FC0 00011.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 2:13:29 PM Seq Line Vial No. Inj. N o . Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\l\METHODS\040104F. M 4/2/04 08:47:26 am 11 4 1 5 1 1 MSD1 427. EIC=426.7:427.7 (CHEMSTORU3091632\A933312\FC000011.D) API-ES, Neg, SIM, Frag: Var 35000 7.364- TH-PFO^ 30000 25000 20000 15000 10000 5000- 0- MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13091632\A933312\FC000011.D) API-ES, Neg, SIM, Frag: Var mi 16000 14000 12000 10000 8000 6000 4000- 2000 0- ..... ................................................-.................................................................. *i r f r i' 24 *MSD1 513, EIC=512.7:513.7 (CHEMSTORU 3091632\A933312\FC00001 .D) 7.371 - PI- CA, - ........... ..... |y - ' 111 1 6 API-ES, Neg, SIM, Frag: Var I......... ........ . ..... *.... 1 8 mir 2500 7.790- SURROGATE! 2000 1500 1000 500- Compound Name TH-PFOS PFOA SURROGATE Area 309885.84 122156.09 17604.30 Amount 500.00 206.22 231.22 Meas. Ret. T Signal Desc. 7.364 7.371 7.790 MSD1 427, ETC=426.7:427.7 MSD1 369, ElC=368.7:369.7 MSD1 513 , EIC=512,7:513.7 *** End of Report * * * PC00414 Fri, 2. Apr. 2004 09:05:13 am Page 1 of 1 000099 Sample Name:solvent blank Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13091812\A935360\FC000012.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 2:28:58 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 12 92 1 5 /il 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13091812\A935360\FC000012.D) 40000 35000 30000 25000 20000 15000 10000- 5000 0- API-ES. Neg. SIM, Frag: Var 7.371 - TH-PFOS, *MSD1 369, EIC=368:7:369.7 (CHEMSTOR\13091812\A935360\FC000012.D) API-ES, Neg, SIM, Frag: Var 350 325 300 275 250225 200175 V. *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13091812\A935360\FC000012.D) API-ES, Neg, SIM, Frag: Var mi 280 260 240 220 -j 200 180 160 Compound Name TH-PFOS PFOA SURROGATE Area 346328.72 0.00 0.00 \_y Amount 500.00 0.00 0.00 Meas. Ret. T Signal Desc. mn 7.371 0.000 0.000 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:08:15 am Page 1 of 1 000100 Sample Name:STD 10 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13 092264\A937344\FC000013.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 2:44:30 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed POAASUR.M C:\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 13 1 1 5 il *MSD1 427, E!C=426.7:427.7 (CHEMSTORM 3092264\A937344\FC000013.D) API-ES, Neg, SIM, Frag: Var 35000 7.373- TH-PFO& 30000 25000 20000 15000-3 10000 5000 0 *MSD I 369, EIC=368.7:369.7 (CHEMSTOR\13092264\A937344\FC000013.D) API-ES, Neg, SIM, Frag: Var . 1000 7.379- PFOA 900 3 800 700^ 600 500 400 -j 300 200 MSD1 513, EIC=512.7:513.7 (CHEMSTORM 3092264\A937344\FC000013.D) API-ES, Neg, SIM, Frag: Var 375 E 350 325 300 275 250 225 200 175 7.799- SURROGATE Compound Name TH-PFOS PFOA SURROGATE Area 356246.53 7658.50 1416.25 Amount 500.00 19.85 18.53 Meas. Ret. T Signal Desc. 7.373 7.379 7.799 MSD1 427, EIC=426.7:427.7 . MSD1 369, EIC=3 68.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:09:57 am Page 1 of 1 000101 Sample Name:STD 50 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13092531\A939392\FC000014.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 3:00:08 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 14 2 1 5 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13092531\A939392\FC000014.D) API-ES, Neg, SIM, Frag: Var 35000 - 7.372 - TH-PFOS 30000 - 25000 i 20000 4 15000 10000-3 5000 Otz 3000 MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13092531\A939392\FC000014.D) API-ES, Neg, SIM, Frag: Var 7.379 - PFOA 2500 2000 1500 1000^ 500 mi 6 'MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13092531\A939392\FC000014.D) API-ES, Neg. SIM, Frag: Var 700 7,795- SURROGATE^ 600 500 400 300- 200 L. Compound Name Area Amount Meas. R e t . T Signal Desc. min TH-PFOS PFOA SURROGATE 348357.78 28341.27 4376.44 500.00 48.67 52.13 7.372 7.379 7.795 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:11:43 am Page 1 of 1 000102 Sample Name:STD 100 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13092616\A941376\FC000015.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 3:15:44 PM Seq Line vial No. Inj. No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 15 3 1 5 /il 1 MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13092616\A941376\FC000015.D) API-ES, Neg. SIM, Frag: Var 35000 7.367- TH-PFOS. 30000 25000 20000 15000 i: !i 100004 5000 4 Oi MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13092616\A941376\FC000015.D) API-ES, Neg, SIM, Frag: Var 7000 7.372- PFOA 6000 5000 4000 -3 3000 2000 1000 0 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13092616\A941376\FC000015.D) API-ES, Neg, SIM, Frag: Var 7.790- SURROGAT^ 1000 800 600 H 400 200- Compound Name TH-PFOS PFOA SURROGATE Area 357273.00 70043.46 9109.27 Amount 500.00 105.02 103.41 Meas. Ret. T Signal Dse. 7.367 7.372 7.790 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PCO 0414 Fri, 2. Apr. 2004 09:13:04 am Page 1 of 1 000103 Sample Name:STD 250 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13092750\A943296\FC000016.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 3:31:20 PM Seq Line Vial No. Inj.No. Inj. Voi. : : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 16 4 1 5 fil 1 *MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13092750\A943296\FC000016.D) API-ES, Neg, SIM, Frag: Var 35000 7,370- TH-PFOS, 30000 -3 25000 20000 -3 15000 10000-r 5000 3 0 *MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13092750\A943296\FC000016.D) API-ES, Neg, SIM, Frag: Var 16000 7.377- PFOA 14000 12000 10000 8000 6000 4000 2000 0-3 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13092750\A943296\FC000016.D) API-ES, Neg, SIM, Frag: Var 2500- 7.797 - SURROGATE mu 2000 J 1500 1000 500 Compound Name TH-PFOS PFOA SURROGATE Area 309713.47 122291.34 17154.91 Amount 500.00 206.56 225.31 Meas. Ret. T - 1----------- r* Signal Desc. mir 7.370 7.377 7.797 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=368.7 :369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:13:51 am Page 1 of 1 000104 Sample Name:STD 500 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13093592\A945472\FC000017.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 3:46:56 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : : A c q . Method Analysis Method Last Changed P 0 A A S U R .M C :\HPCHEM\1\METH0DS\040104F.M 4/2/04 08:47:26 am 17 5 1 5 fj.1 1 *MSD1 427. EIC=426.7:427.7 (CHEMSTOR\13093592\A945472\FC000017.D) API-ES, Neg, SIM, Frag: Var 30000-: 7.374 - TH-PFOSj, 25000 20000 1500010000- ' !i i l! i| 5000 - 0- i i i I i i i I i 2 46 *MSD1 369, EIC=368.7:369.7 (CHEMSTORM3093592\A945472\FC000017.D) API-ES, Neg, SIM, Frag: Var \ j\ 25000 / 7.381 - PFOA, \ -- |--------8 20000 / 15000- i1 11 10000/ 5000/ ; j1 0 -- 1 ... | .ij i ii i 2 46 8 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13093592\A945472\FC000017.D) API-ES, Neg. SIM, Frag: Var 3500 - 7.800- SURROGATE-r, i\ 3000 -j 2500 / 2000 / i 1500 / 1000- 1 ii 500 -z 0" ' ' ' I ' ` 1 I 24 ''1 6 Compound Name Area Amount Meas. Ret. T j i 8 Signal Desc. mi mir min TH-PFOS PFOA SURROGATE 304949.88 272757.56 34619.75 500.00 488.87 477.84 7.374 7.381 7.800 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=3 68.7:369.7 MSD1 513, EIC=512.7 :513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:17:12 am Page 1 of 1 000105 Sample Name:STD 750 ppb Sample Info: Data file :C :\HPCHEM\l\DATA\Chemstor\13 093 72 6\A947648\FC000018.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 4:02:33 PM Seq Line vial No. Inj. No. Inj. Vol. : : : : A c q . Method Analysis Method Last Changed P O A A S U R .M C:\HPCHEM\1\METHODS\040104F. M 4/2/04 08:47:26 am 18 6 1 5 pi 1 25000 MSD1 427, EIC=426.7:427.7 (CHEMSTOR\13093726\A947648\FC000018.D) API-ES, Neg, SIM, Frag: Var 7.373 - TH-PFOS. 20000 15000- 10000 5000- 0 T MSD1 369, EIC=368.7:369.7 (CHEMSTOR\13093726\A947648\FC000018.D) API-ES, Neg, SIM, Frag: Var 40000 -4 35000 30000 25000 20000 15000 10000 5000- 0- 7.380- PFOA. 5000 MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13093726\A947648\FC000018.D) API-ES, Neg, SIM, Frag: Var 7.798 - SURROGATE, 4000 3000 -4 2000 - 1000 / Ii ; o i --- ,-----1-----1-----r---- 1----------'-----1-----1-----1-----'-----1-----1-----1----- 1-----1-----'--- -- _________________________________2__________________________4__________________________6__________________________ 8________ min Compound Name Area Amount M e a s . Ret. T Signal Desc. TH-PFOS PFOA SURROGATE 280172.09 392147.00 49627.12 500.00 834.52 783.92 7.373 7.380 7.798 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=3 68.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:17:49 am Page 1 of 1 000106 Sample Name:STD 1000 ppb Sample Info: Data file :C:\HPCHEM\l\DATA\Chemstor\13093875\A949440\FC000019.D Injection Date Acq Operator Instrument Dilution 4/1/04 jmiller PC00414 1 4:18:09 PM Seq Line Vial No. Inj. No. Inj. Voi. : : : Acq. Method Analysis Method Last Changed P O A A S U R .M C :\HPCHEM\1\METHODS\04 010 4F .M 4/2/04 08 :4 7 :26 am 19 7 1 5 /il 1 *MSD1 427, EIC=426 7:427.7 (CHEMSTORV13093875\A949440\FC000019.D) API-ES, Neg, SIM, Frag: Var 35000 - 7.365- TH-PFOS, 30000 25000 H 20000 15000 10000-3 5000 0 *MSD1 369, E!C~368 7:369.7 (CHEMSTOR\13093875\A949440\FC000019.D) API-ES, Neg, SIM Frag: Var 60000 7.374- PFOA, 50000 40000 30000 !I 20000 10000 0 *MSD1 513, EIC=512.7:513.7 (CHEMSTOR\13093875\A949440\FC0000'l9.D) API-ES. Neg, SIM, Frag: Var 8000 7000 6000 5000 4000 3000 -3 7.793- SURROGATE 2000 1000-3 0 Compound Name Area Amount Meas. Ret. T 8 Signal Desc. mir TH-PFOS PFOA SURROGATE 296890.44 459125.56 62778.01 500.00 953.48 966.27 7.365 7.374 7.793 MSD1 427, EIC=426.7:427.7 MSD1 369, EIC=3 68.7:369.7 MSD1 513, EIC=512.7:513.7 *** End of Report *** PC00414 Fri, 2. Apr. 2004 09:18:31 am Page 1 of 1 000107 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L2133 PFOA 413 -> 369 NA RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: 0.2 ng/mL (2 ng/g) 15 pL Solids 1g 10 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 032604AR Amy Sheehan LC/MS/MS Unit 8 7 03/26-29/04 04/01/04 Exygen ID C032604-6 C032604-5 C032604-4 L2133-5" C032604-3 C032604-2 C032604-1 Sponsor ID - Wipe-A - - - Sample Code CS CS CS s CS CS CS Run No. 032604AR-201 032604AR-202 032604AR-203 032604AR-204 032604AR-205 032604AR-206 032604AR-207 PFOA Found (ng/mL) = (peak area - intercept) / slope x DF Recovery (% )= [PFOA found (ng/mL)-PFOA found in control (ng/mL)] amount PFOA added (ng/niL) Std. Cone. (ng/mL) 0.2 0.5 1 2 5 10 x 100 Dilution Factor - - 100 - - PFOA Found (ng/g) = PFOA found (ng/mL) x Ext. Volume (mL) / Sample Weight (g) Peak Area 4041 8434 16736 23296 36520 89915 186372 PFOA Found (ng/mL) - - 128 - - * PFOA Foun4 (ng/g) - - Amount PFOA Added (ng/mL) - - Recovery (%) . - 2560 - - - . . . - -- Standard Curve : Linear (1/x weighted) Intercept =-152.256 Slope = 18338.6 Coef. Of Det. * 0.999392 CS = Calibration standard C = Control sample S * Sample LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike **Due to the butkiness of the sample 20 mL of methanol was used for the extraction. CK = Check Standard ND = Not detected * Response between 0 and LOD NQ ~ Not quantifiable = Response between LOD and LOQ Spreadsheet prepared by: 000108 LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L2133 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Binary Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID:MA13296) (JONESCHROMATOGRAPHY: Part No. FK5962EJ) Mobile Phase (A) : 2 mM Ammonium Acetate in Water Mobile Phase (B) : Methanol Analyst: Amy Sheehan Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by:_______ C~_____ 000109 Masslynx Sample List S am ple List: C :\M A S S L Y N X \F lu o ro c h e m s .P R O \S a m p le D B \0 3 2 6 0 4 A R C S R S olids.SP L Printed: W e d M a r 31 13:59:07 2004 Exygen study n o . Page 1 Page Position: ( 1 , 1 ) Vial File Name LIMS ID Client ID Sample Description Matrix Sample Type Cone (ng/mL) Cone B Cone C Test ID DF MS Method 1 61 032604AR-201 -- 2 62 032604AR-202 -- 3 63 032604AR-203 -4 68 032604AR-204 -- 5 64 032604AR-205 -- 6 65 032604AR-206 -- 7 66 032604AR-207 -- __ -- -- -- -- -- -- C032604-6, 0.2 ng/mL standard C032604-5, 0.5 ng/mL standard C032604-4,1.0 ng/mL standard L2133-5, DF=100 C032604-3, 2.0 ng/mL standard C032604-2,5.0 ng/mL standard C032604-1, 10.0 ng/mL standard __ -- -- -- -- -- -- Standard Standard Standard Analyte Standard Standard Standard 0.2 0.5 1.0 -- 2.0 5.0 10.0 __ 0 --- 0 --0 ----0 --0 --0 --0 1 008 PFOA 1 008 PFOA 1 008 PFOA 100 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 000110 Masslynx - Sample List S a m p le List: C :\M A S S L Y N X \F lu o ro c h e m s .P R O \S a m p le D B \0 3 2 6 0 4 A R C S R S olids.SP L Printed: W ed M ar 31 13:59:07 2004 ^W\<2> O S \S l\o *-l HPLC Method MS Tune File In] Volume (pL) 1 w ater Fluorochems 15 2 w ater Fluorochems 15 3 w ater Fluorochems 15 4 w ater Fluorochems 15 5 w ater Fluorochems 15 6 w ater Fluorochems 15 7 w ater Fluorochems 15 000111 Exygenstudy NO. Page 2 Page Position: (2,1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L2133 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Binary Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID:MA13296) (JONESCHROMATOGRAPHY: Part No. FK5962EJ) Mobile Phase (A) : 2 mM Ammonium Acetate in Water Mobile Phase (B) : Methanol Analyst: Amy Sheehan Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by:______ ______ 000112 Scanning Method Report Method: C :\MASSLYNX\FLUOROCHEMS. PRO\ACQUDB\008 PFOA Last Modified: Thu Oct 02 13:56:38 2003 Printed: Wed Mar 31 13:59:18 2004 ^ ^ ^ Solvent Delay ( mins ) : 0.00 Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 413.00 369.00 0.20 10 10 Page 1 000113 Method Report Method File: Last Modified: Printed HP1100 LC Pump Initial Conditions c :\masslynx\fluorochems.pro\acqudb\water Wednesday, March 31, 2004 13:52:32 Wednesday, March 31, 2004 13:59:25 __________________ Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 60.0 40.0 0.0 0.0 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are Time 0 .00 0 .40 1 .00 7 .00 7 .50 9 ,.00 9 .50 13 .50 14 .00 15 ,.00 A% 60 .0 60. 0 10 .0 10 .0 0 .0 0 .0 60 .0 60 .0 60 .0 60 .0 B% 40 .0 40 .0 90. 0 90 .0 100. 0 100 .0 40 .0 40. 0 40 .0 40 .0 c% 0- 0 0. 0 0. 0 0 .0 0. 0 0 .0 0 .0 0. 0 0 .0 0. 0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Contactl Off Off Off On Off Off Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/1/min) Draw Position (mm) Stop Time (mins) Injection Volume(/l) Vial Number 200.0 200 0.10 15.00 15.0 71 Page 1 Pressure 400 400 400 400 400 400 400 400 400 400 000114 Tuning Method Report Method: C :\MAS SLYNX\ FLUOROCHEMS .PRO\ACQUDB\FLUOROCHEMS Printed: Wed Mar 31 13:59:36 2004 A w i6 p3|3i]oy 80.00_________________________ I Page 1 I----- 1-----T---- r ----1"': I .""I -- 1 -- I---- T"" J .5___ 76 77 78 79 80 81 82 83 84 Dau 299.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 30 0.0 0.0 0.0 100 300 -2.93 -10 101 300 Pressures Analyser Vacuum Gas Cell Rdbk OFF 2.9e- 3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 30 2 14.0 14.0 2.0 700 8 9 11 -695 Rdbk 87.8 697.1 000115 Quantify Calibration Report StudyNo:L2133,SetNo:032604AR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Page 1 Calibration: P :\Data\LCMSMS7\Masslynx\Fluorochems .PRO\CurveDB\032604AR CSR Solids Last modified: Thu Apr 01 13:41:03 2004 Printed: Thu Apr 01 13:42:47 2004 ^ OMfl , Exygen Research, 3058 Research Drive, State College, PA 16801 000H 6 Quantify Sample Report StudyNo:L2133,SetNo:032604AR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P :\Data\LCMSMS7\Masslynx\Fluorochems .PRO\SampleDB\032604AR CSR Solids Thu Apr 01 13:35:12 2004 P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 040104 Thu Apr 01 13:40:08 2004 Initials _ Thu Apr 01 13:42:48 2004 Date J M M Q j Run#/ )32fr)Vfl g-Zo/ T ...... -- . o7 Name: 032604AR-201 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000117 Quantify Sample Report StudyNo:L2133,SetNo:032604AR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Page 2 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604AR CSR Solids Last modified: Thu Apr 01 13:35:12 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 040104 Last modified: Thu Apr 01 13:40:08 2004 Job Code: Printed: Thu Apr 01 13:42:48 2004 Marne: 032604AR-202 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 00118 Quantify Sample Report StudyNo:L2133,SetNo:032604AR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Page 4 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604AR CSR Solids Last modified: Thu Apr 01 13:35:12 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 040104 Last modified: Thu Apr 01 13:40:08 2004 Job Code: Printed: Thu Apr 01 13:42:48 2004 Name: 032604AR-204 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000119 Quantify Sample Report StudyNo:L2133,SetNo:032604AR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Page 5 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604AR CSR Solids Last modified: Thu Apr 01 13:35:12 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 040104 Last modified: Thu Apr 01 13:40:08 2004 Job Code: Printed: Thu Apr 01 13:42:48 2004 Name: 032604AR-205 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000120 Quantify Sample Report StudyNo:L2133,SetNo:032604AR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Page 6 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604AR CSR Solids Last modified: Thu Apr 01 13:35:12 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 040104 Last modified: Thu Apr 01 13:40:08 2004 Job Code: Printed: Thu Apr 01 13:42:48 2004 Name: 032604AR-206 Text: PFOA C032604-2, 5.0 ng/mL standard 032604AR-206 Sm (Mn, 2x2) %- 5.04 8991^ 01-Apr-2004 10:57:21 LCMSMS #7 MRM of 1 Channel ES413 >369 5.91e5 Area 0 T-T-, Time -oo 2.00 3.00 4.00 ' 5.00 6.0 7.00 ' 8.0 Exygen Research, 3058 Research Drive, State College, PA 16801 000121 Quantify Sample Report StudyNo:L2133,SetNo:032604AR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Page 7 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604AR CSR Solids Last modified: Thu Apr 01 13:35:12 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 040104 Last modified: Thu Apr 01 13:40:08 2004 Job Code: Printed: Thu Apr 01 13:42:48 2004 Name: 032604AR-207 Text: 1 : PFOA________________________________________________________________________________ C032604-1,1 0 .0 ng/mL standard 01-Apr-2004 11:14:12 LCMSMS #7 032604AR-207 Sm (Mn, 2x2) r ru MRM of 1 Channel ESs -IRQ Exygen Research, 3058 Research Drive, State College, PA 16801 000122 Quantify Sample Report StudyNo:L2133,SetNo:032604AR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Page 3 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604AR CSR Solids Last modified: Thu Apr 01 13:35:12 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 040104 Last modified: Thu Apr 01 13:40:08 2004 Job Code: Printed: Thu Apr 01 13:42:48 2004 Name: 032604AR-203 Text: 1 : PFOA C 0 3 2 6 0 4 -4 ,1.0 ng/mL standard 032604AR-203 Sm (Mn, 2x2) 100- 5.05 16736 k oo CO oo :c\i oq %o A- ..................................................................................................... J ... -- 4.00 5.00 01-Apr-2004 10:07:10 LCMSMS #7 MRM of 1 Channel ES- 413 >369 1.09e5 Area! j 6.00 7.00 8.00 IiI Exygen Research, 3058 Research Drive, State College, PA 16801 000123 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L2133 PFOA 413 ->369 NA RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample WeightFinal Volume: 0.2 ng/mL (2 ng/g) 15 pL Solids 1g 10 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 032604A Amy Sheehan LC/MS/MS Unit# 7 03/26-29/04 03/31/04 Exygen ID C032604-6 C032604-5 C0326O4-4 C032604-3 C032604-2 C032604-1 Methanol wash Reagent Blank Reagent Spk A Reagent Spk B L2I33-1 Spk C L2133-1 Spk C C032604-6 L 2 133-1 L2133-1 Rep L2133-2 L2133-3 C032604-5 L2133-4 L2133-5** L 2 133-6** L2133-7 C032604-4 L2133-1 L2133-1 Rep L2133-2 L 2 133-3 C032604-3 L2133-4 L2133-5 L2133-6 L2133-7 C032604-2 C032604-1 Sponsor ID - - - - - - Bulk-A Bulk-A Bulk-A Bulk-A Bulk-B Fab-A - Mem-A Wipe-A Wipe-B Fab-B - Bulk-A Bulk-A Bulk-B Fab-A Mem-A Wipe-A Wipe-B Fab-B - - Sample Code CS CS CS CS CS CS c c LCS LCS LF LF CS S s s s CS s s s s CS s s s s CS S s s s CS CS Run No. 032604A-101 032604A-102 032604A-103 032604A-104 032604A-105 032604A-106 032604A-107 032604A-108 032604A-109 032604A-110 032604A-111 032604A-112 032604A -113 032604A-114 032604A - l15 0 32604A -116 032604A-117 032604A-118 032604A - l19 032604A-120 032604A-121 032604A-122 032604A-123 032604A-124 032604A-125 032604A-126 032604A-127 032604A-128 032604A-129 032604A-130 032604A-I31 032604A-132 032604A-133 032604A-134 PFOA Found (ng/mL) = (peak area - intercept) / slope x DF Recovery (%) = fPFOA found (ng/mL)-PFOA found in control (ng/mL)l amount PFOA added (ng/mL) Std. Cone. (ng/mL) 0.2 0.5 1 2 5 10 - - - 0.2 . 0.5 - 1 - - - 2 - 5 10 x 100 Dilution Factor - - 1 1 1 100 10 - 10 10 10 10 - 10 10 10 10 - 1 1 1 1 1 1 1 1 - - Peak Area 4334 9435 18127 36646 89299 187621 0 0 7656 31984 19268 190450 4247 101805 102476 31177 7160 9048 15557 229092 75752 28423 16775 963512 943166 256353 57136 36761 142643 2126942 732340 281935 88895 179913 PFOA Found (ng/g) = PFOA found (ng/mL) x Ext. Volume (mL) / Sample Weight (g) PFOA Found (ng/mL) - - - - 0.402 1.75 104 105 - 56.1 56.4 17.0 * - 8.39 41.7 15.5 * * * 3.14 * * * * - - PFOA Found (ng/g) . - - Amount PFOA Added (ng/mL) - - - Recovery (%) . . . . . - 4.02 17.5 1040 1050 - 0.5 2.0 50 50 - 80 87 96 * . 561 564 170 - -- -. 83.9 . -- - - . _ . 834 . 155 - -- ---31.4 . ------- %. . _ . . . _ . . . _ _ - Standard Curve : Linear (1/x weighted) Intercept = 388.036 Slope = 18086.8 Coef. Of Det. = 0.998929 CS = Calibration standard C = Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS * Laboratory Control Spike **Due to the bulkiness of the sample 20 mL of methanol was used for the extraction. Sample was analyzed at several dilution levels in this set. The appropriate results are reported. ASample requires dilution. For reanalysis see data set 032604AR CK * Check Standard ND = Not detected * Response between 0 and LOD NQ = Not quantifiable * Response between LOD and LOQ Spreadsheet prepared by: 000124 Ew g en 3058 Research Drive State College, PA 16801 c: h Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L2133 Matrix: Solids Sponsor Study/Protocol No: NA The samples listed below were removed from storage cabinet No. Time J m s i Date _____ Initials f E C L IE N T SA M PLE ID EXYGEN ID NUMBER I W EIG H T (g) 1 FO R T IFIC A T IO N (ng) - Bulk-A Bulk-A Bulk-A Bulk-B Fab-A Mem-A W ipe-A Wipe-B Fab-B - - - - - - - Reagent Blank - - Reagent Spk A - 5.0 Reagent Spk B - 20.0 L2133-1 Spk C 1.0 500.0 L2133-1 1.0 - L 2 133-1 Rep 1.0 - L 2133-2 1.0 - L 2 133-3 1.0 - L 2133-4 1.0 - L 2 133-5 1.0 - L 2133-6 1.0 - L2133-7 1.0 - - -- - -- - -- - -- - -- - -- - -- - -- Reagent Spk A Reagent Spk B L2133-1 Spk C Spiking Solution Used F030804-5 (10 ng/mL) F030804-4 (100 ng/mL) F030804-2 (10000 ng/mL) -- -- -- -- All samples were weighed on balance no. 2-0______: Time /W5~________ Date C & jzufQ 'j____ j_After weighing samples were returned to storage cabinet N o ._ O ij ZLt jo ^Time__ W 3 0 _______ Date Comments: Volume Used for Spiking 500 pL (200 pL micropipette) 200 pL (200 pL micropipette) 50 pL (100 pL micropipette) - - - - Initia1/Date U% - 0 3 K & 't lZ /o'- - - Initials CEE Initials CEE Analysis Summary: Data Set: Data Set: Data Set: Q 32(gC X j^ r)M fSet extraction/analysis data verified by: & 000125 Date: July 26, 2001/6 3058 Research Drive <;h State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L2133 MATRIX: Solids METHOD: Modified 03M-001-035S ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID Bulk-A Bulk-A Bulk-A Bulk-B Fab-A Mem-A Wipe-A Wipe-B Fab-B - Exygen ID Reagent Blank Reagent Spk A Reagent Spk B L2133-1 SpkC L2133-1 L2133-1 Rep L 2 133-2 L2133-3 L2133-4 L2133-5 L2133-6 L2133-7 - STEP 1 $ r - STEP 2 Dilutions (mL/mL) - STEP 3 Dilutions (mL/mL) - - T 7n/oV.o\ 0.A,y<op - * - J L 'V/al ..oP OA/\i..o0 ' / . 0A/\ .0 -- - 'V i. ' '1 < -- - - -- - -- - - '- - -- - - -- - -- - - -- - -- - - -- - -- - - -- - -- - - -- - -- - - -- - -- - - -- - -- - *Initials/Date - -- - oCshfzu.M o&liteEtfi> iW AD3\20|OH .r i STEP 1: Add 10 mL Methanol and Shake on a wrist action shaker overnight. STEP 2: Centrifuge and filter through a glass acrodisc filter, collect elute. STEP 3: LC/MS/MS analysis s a m e VJ& STEP 4: LC/MS/MS reanalysis. STEP 4 ' - V - - - - - - OSfello*/ Reagents/ Materials Methanol - - Initials/Date . . Lot # , - /ie r ofafeH - . - - - - HPLC - - - Methanol Ammonium Acetate Water - iVfsiqlfiolS - Initials/Date 03\3i oV 101 W A PBUvjsinIKlWTb to* *Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Peril uorooctanoic Acid in Soil by LC/MS/MS. COMMENTS: Final extracts stored in refrigerator $ Sxnplt Vdfcv? p lacej en shaJttf on Oijzb and -taken o ff on O ifa . /*> iff -I * L & LInitials: Date: July 19, 2001/4 000126 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochems.PRO\SampleDB\032604A CSR Solids.SPL Printed: Tue Mar 30 10:57:31 2004 Q 5 ^ | Q<-f______________________________ Vial File Name LIMS ID Client ID Sample Description Mai 1 61 032604A-101 2 62 032604A-102 -- 3 63 032604A-103 -- 4 64 032604A-104 5 65 032604A-105 -- 6 66 032604A-106 -- 7 92 032604A-107 -- 8 41 032604A-108 -- 9 42 032604A-109 -- 10 43 032604A-110 -- 11 44 032604A-111 -- 12 45 032604A-112 -- 13 61 032604A-113 -- 14 46 032604A-114 -- 15 47 032604A-115 -- 16 48 032604A-116 -- 17 49 032604A-117 -- 18 62 032604A-118 -- 19 50 032604A-119 -- 20 51 032604A-120 -- 21 52 032604A-121 -- 22 53 032604A-122 -- 23 63 032604A-123 -- 24 54 032604A-124 -- 25 55 032604A-125 -- 26 56 032604A-126 -- 27 57 032604A-127 -- 28 64 032604A-128 -- 29 58 032604A-129 -- 30 59 032604A-130 -- 31 60 032604A-131 -- 32 67 032604A-132 -- 33 65 032604A-133 -- 34 66 032604A-134 -- ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- C032604-6, 0.2 ng/mL standard C032604-5, 0.5 ng/mL standard C032604-4,1.0 ng/mL standard C032604-3, 2.0 ng/mL standard C032604-2, 5.0 ng/mL standard C032604-1,10.0 ng/mL standard -- Methanol Wash Reagent Blank -- Reagent Spk A, 0.5 ng/mL Reagent Spk B, 2.0 ng/mL L2133-1 Spk C, 50 ng/mL, DF=100 -- L2133-1 Spk C, 50 ng/mL, DF=10 -- C032604-6, 0.2 ng/mL standard -- L2133-1, DF=10 L2133-1 Rep, DF=10 L2133-2, DF=10 L2133-3, DF=10 C032604-5, 0.5 ng/mL standard -- L2133-4, DF=10 L2133-5, DF=10 -- L2133-6, DF=10 L2133-7, DF=10 C032604-4,1.0 ng/mL standard L2133-1 L2133-1 Rep L2133-2 L2133-3 C032604-3, 2.0 ng/mL standard L2133-4 L2133-5 L2133-6 L2133-7 C032604-2, 5.0 ng/mL standard C032604-1,10.0 ng/mL standard -- Exygen STUDY NO. Z /3 3 Page 1 p` a` Posilion: a1 ) Sample Type Cone (ng/mL) Cone B Cone C Test ID DF MS Method Standard Standard Standard Standard Standard Standard Blank Blank QC QC QC QC Standard Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Standard Standard 0.2 0.5 1.0 2.0 5.0 10.0 -- -- 0.5 2.0 50 50 0.2 -- -- -- -- 0.5 -- -- -- -- 1.0 -- -- -- -- 2.0 -- -- -- -- 5.0 10.0 0____ ____ 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- 0------- 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 100 008 PFOA -- -- 0 10 008 PFOA --- -- 0 1 008 PFOA -- -- 0 10 008 PFOA -- -- 0 10 008 PFOA -- -- 0 10 008 PFOA -- -- 0 10 008 PFOA -- -- 0 1 008 PFOA -- -- 0 10 008 PFOA -- -- 0 10 008 PFOA -- -- 0 10 008 PFOA -- -- 0 10 008 PFOA -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- -- 0 1 008 PFOA -- 0 1 008 PFOA -- -- 0 1 008 PFOA 000127 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochems.PRO\SampleDB\032604A C SR Solids.SPL Printed: Tue Mar 30 10:57:31 2004 03^ _____________________________ HPLC Method MS Tune File Inj Volume (pL) 1 water Fluorochems 15 2 water Fluorochems 15 3 water Fluorochems 15 4 water Fluorochems 15 5 water Fluorochems 15 6 water Fluorochems 15 7 water Fluorochems 15 8 water Fluorochems 15 9 water Fluorochems 15 10 water Fluorochems 15 11 water Fluorochems 15 12 water Fluorochems 15 13 water Fluorochems 15 14 water Fluorochems 15 15 water Fluorochems 15 16 water Fluorochems 15 17 water Fluorochems 15 18 water Fluorochems 15 19 water Fluorochems 15 20 water Fluorochems 15 21 water Fluorochems 15 22 water Fluorochems 15 23 water Fluorochems 15 24 water Fluorochems 15 25 water Fluorochems 15 26 water Fluorochems 15 27 water Fluorochems 15 28 water Fluorochems 15 29 water Fluorochems 15 30 water Fluorochems 15 31 water Fluorochems 15 32 water Fluorochems 15 33 water Fluorochems 15 34 water Fluorochems 15 Exygen study n o . L V 2 > Page 2 Page Position: (2, 1) 000128 LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L2133 Instrument: Computer: Software: Micromass Quattro Ultima (LC/M S/M S Unit #7) COMPAQ Professional Workstation AP200 M icrosoft Windows NT: Version 4 Build 1381 : Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Binary Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID:M A 13296) (JONESCHROMATOGRAPHY: Part N o. FK5962EJ) M obile Phase (A) : M obile Phase (B) : Analyst: 2 mM Ammonium Acetate in Water Methanol Amy Sheehan f # 4 * ^ Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814)272-1039 FAX: (814)231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by: 03)3/ jo*-/ 000129 Scanning Method Report Method: C :\MASSLYNX\FLUOROCHEMS .PRO\ACQUDB\008 PFOA Last Modified: Thu Oct 02 13:56:38 2003 Printed: Tue Mar 30 10:55:42 2004 0 3 ] s p )oY Solvent Delay ( mins ) : 0.00 Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay Span ( Daltons ) : Start Time ( Mins ) End Time ( Mins ) : Repeats : Channel Parent Secs ) : Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 413.00 369.00 0.20 10 10 Page 1 000130 Method Report Method File: Last Modified: Printed: c :\masslynx\fluorochems.pro\acqudbWater Tuesday, March 30, 2004 10:39:54 Tuesday, March 30, 2004 10:55:54 favfe P 32p )p V Page 1 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are : Time 0 .00 0 .40 1..00 7 ,.00 7 .50 9..00 9 ..50 13 ..50 14 .00 15 .. 00 A% 60 .0 60 .0 10 .0 10 .0 0. 0 0. 0 60 .0 60 .0 60 .0 60 . 0 B% 40 .0 40 .0 90 .0 90 .0 100. 0 100 . 0 40 .0 40. 0 40. 0 40 . 0 C% 0 .0 0 .0 0. 0 0.0 0. 0 0. 0 0. 0 0. 0 0. 0 0. 0 D% 0. 0 0. 0 0. 0 0. 0 0. 0 0. 0 0. 0 0. 0 0. 0 0. 0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 Pressure 400 400 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contactl Off On Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (^tl/min) Draw Position (mm) Stop Time (mins) Injection Volume (/xl) Vial Number 200.0 200 0.10 15.00 15.0 34 000131 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMS .PRO\ACQUDB\FLUOROCHEMS Printed: Tue Mar 30 10:56:06 2004 D $ \3 o }o H 80.00 j xGU Page 1 r--- T -----1---- r-- t '"-- 'i-- ~ ~ v " i i 5 76 77 78 79 80 81 82 Dau 299.00 i-------- 1-- " i 83 84 E SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 30 0.0 0.0 0.0 100 300 -2. 93 -10 102 300 Pressures Analyser Vacuum Gas Cell Rdbk OFF 2.8e- 3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 30 2 14.0 14.0 2.0 700 8 9 11 -695 Rdbk 87.8 697.1 000132 Quantify Calibration Report Page 1 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Calibration: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\CurveDB\032604A CSR Solids Last modified: Wed Mar 31 11:52:14 2004 Printed: Wed Mar 31 12:00:53 2004 a ii ___________________________ P3foW_________________________ Exygen Research, 3058 Research Drive, State College, PA 16801 000133 Quantify Sample Report Page 1 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A C SR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Initials a im ib Printed: Wed Mar 31 12:00:54 2004 Data . . _ L _ _ f l3 j 3 l M Run#P32-(gCxjfi-|&l To 0 A - 13^ Name: 032604A-101 Text: 1 : PFOA C032604-6, 0.2 ng/mL standard 032604A-101 Sm (Mn, 2x2) 100n % 31-Mar-2004 02:01:08 LCMSMS #7 MRM of 1 Channel ES- 4.89 413 >369 3.06e4 Area tv-'. ' V - H w " v ... . _ 0 r r^.,, , Time ! 2.00 3.00 4.............. 5.00 6.00 7.00 8.00 ! Exygen Research, 3058 Research Drive, State College, PA 16801 000334 Quantify Sample Report Page 2 StudyNo:L 2 1 3 3,SetNo:032604A CSR Solids, ExtDate:03/26-29/04 , Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-102 Text: 1 : PFOA C032604-5, 0.5 ng/mL standard 31 -Mai^2004 02:17:56 LCMSMS #7 032604A-102 Sm (Mn, 2x2) MRM of 1 Channel ES- 100. 4.89 J 413 >369 6.60e4 Area %- 0 1.0 ' 2.0 " ' 3.00 ' 4.00 5.0 60 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000135 Quantify Sample Report Page 3 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04 , Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-103 Text : 1 : PFOA C032604-4, 1.0 ng/mL standard 032604A-103 Sm (Mn, 2x2) 100- % o 1 1.00 2.00 3.00 4.89 18127"! 4.00 J 5.0 31-Mar-2004 02:34:40 LCMSMS #7 MRM of 1 Channel ES413 >369 1.25e5j Areal 6.00 7.0 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000136 Quantify Sample Report Page 4 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-104 Text: 1 : PFOA C032604-3, 2.0 ng/mL standard 0326(J4A-104 Sm (Mn, 2x2) 100- %0A 1.0 2.0 3.00 4.89 366^^ 4.00 5.0 6.00 31 -M ar-2004 02 :51:34 LCMSMS #7 MRM of 1 Channel ES413 >369 2.72e5! AreafI ! ii i...... i t""'..i.i inie 1 7.00 8.00 i Exygen Research, 3058 Research Drive, State College, PA 16801 000137 Quantify Sample Report Page 5 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-105 Text: PFOA C032604-2, 5.0 ng/mL standard 032604A-105 Sm (Mn, 2x2) 100- % 4.89 89299 31-Mar-2004 03:08:18 LCMSMS #7 MRM of 1 Channel ES413 >369 6.62e5 Area 0 Time 1.00 2.00 3.00 4.00 5.00 6.00 7.0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000138 Quantify Sample Report Page 6 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-106 Text: 1 : PFOA C 032604-1,10.0 ng/mL standard 032604A-106 Sm (Mn, 2x2) 41nUnU - %- n ! 1.00 " ' " 2.00 3.00 4.88 187621"! J 4.00 5.00 31-Mar-2004 03:25:09 LCMSMS #7 MRM of 1 Channel ES413 >369 1.34e6 Area 6.00 7.00 ' 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000139 Quantify Sample Report Page 7 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004*1 Name: 032604A-107 Text: 1 : PFOA Methanol Wash 032604A-107 Sm (Mn, 2x2) 100- -12 % 0.61 0.77 1.20 0 1.00 1.97 2.00 2.64 3 43 3.70 31-Mar-2004 03:41:52 LCMSMS #7 MRM of 1 Channel ES- 413 > 369 I 5.605-79 6.056.51 8.62e3 4 88 5.48 4.65 A \r/ 6.82 , 7.17 7-71 7.97 V^A/Vi 3.00 4.0 5.00 6.0 7.00 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000140 Quantify Sample Report Page 8 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0Anon t. rstract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-108 Text: 1 : PFOA Reagent Blank 032604A-108 Sm (Mn, 2x2) 100^ 0.11 : - % -l o -65 0 9 8 1.551.61 2.30 2.84 1 1.00 1 2.00 3.00 31-M ar4 004 03:58:30 LCMSMS #7 MRM o* i Channel ES- 413 >369 1.48e4 j 5 6 2 5'87_6.p8 6.36 4 TM4.88 4.42 Jxi'\ ,,j f n\ , 6.67 7 :1"'MlVMU.W\,vA-.. 13 . - A * . - ' . 4.00 ' 5.00 1 6 .bo 7.00 7.93 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000141 Quantify Sample Report Page 9 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: W e d Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004*1 Name: 032604A-109 Text: 1 : PFOA Reagent Spk A, 0.5 ng/mL 032604A-109 Sm (Mn, 2x2) 100- % 4.88 31-Mar-2004 04:15:09 LCMSMS #7 MRM of 1 Channel ES413 > 369 5.98e4 Area 1.0 2.00 3.00 4.00 5.00 6.00 7.0 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000142 Quantify Sample Report Page 10 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: W e d Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-110 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000143 Quantify Sample Report Page 11 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-111 Text: 1 : PFOA L2133-1 Spk C, 50 ng/mL, DF=100 0 32 604A -111 Sm (Mn, 2x2) 100- % 0- 1.00 ' 2.00 3.00 4.89 192681 J 31-Mar-2004 04:48:43 LCMSMS #7 MRM of 1 Channel ES413 >369 1.31e5 Area 4.00 1 5.00 ' 6.00 7.00 ' 8 .0 0 imC Exygen Research, 3058 Research Drive, State College, PA 16801 000144 Quantify Sample Report Page 12 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: W e d Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-112 Text: 1 : PFOA L2133-1 Spk C, 50 ng/mL, DF=10 032604A-112 Sm (Mn, 2x2) 100 %- o ' 1.00 2.0 3.00 4.86 1904501 A[ 4.00 1 5.00 31-Mar-2004 05:05:22 LCMSMS #7 MRM of 1 Channel ES413 >369 1.31e6 Area i 1; t 1i ' 1 6.00 i j .............. "i''.!! i | Tim 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000145 Quantify Sample Report Page 13 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-113 Text: 1 : PFOA C032604-6, 0.2 ng/mL standard 31-Mar-2004 05:22:08 LCMSMS #7 032604A-113 Sm (Mn, 2x2) MRM of 1 Channel ES- 100, 4.86 413 > 3 6 9 2.86e4 Area 1.00 2.00 3.00 4.00 ' 5.00 1 6.00 7.0 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000146 Quantify Sample Report Page 14 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: W e d Mar 31 12:00:54 2004 Name: 032604A-114 Text: 1 : PFOA L2133-1, DF=10 032604A -114 Sm (Mn, 2x2) ! 100 % 4.88 101 31-Mar-2004 05:39:02 LCMSMS #7 MRM of 1 Channel ES413 > 369! 6.82e5! Areaj 0 L. T.0 2.0 3.00 ' 4.00 5.00 - T - T - r : I .!-- l - r - r - l Tihie 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000147 Quantify Sample Report Page 15 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-115 Text: 1 : PFOA L2133-1 Rep, DF=10 032604A -115 Sm (Mn, 2x2) 100- %- o 2.00 co r 3.00 4.88 1024761 4.00 i 5.00 " 31-Mar-2004 05:55:45 LCMSMS #7 MRM of 1 Channel ES- 413 >369 6.55e5 Area 6.0 V.bo j ----- ---i--i Tim e i 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000148 Quantify Sample Report Page 16 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-116 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000149 Quantify Sample Report Page 17 StudyNo:L 2 133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032S Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-117 Text: 1 : PFOA L2133-3, DF=10 032604A-117 Sm (Mn, 2x2) 100n 4.88 7160 31-Mar-2004 06:29*12 LCMSMS #7 MRM of 1 Channel ES- 413 >369| 4.48e4 Area' 1.00 2.0 3:00 4.00 5.00 6.00 7.0 r-- Time 8.0 Exygen Research, 3058 Research Drive, State College, PA 16801 000150 Quantify Sample Report Page 18 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-118 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000151 Quantify Sample Report Page 19 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A C.'SR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: W e d Mar 31 12:00:54 2004 Name: 032604A-119 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000152 Quantify Sample Report Page 20 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-120 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000153 Quantify Sample Report Page 21 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-121 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 0001S4 Quantify Sample Report Page 22 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-122 Text: 1: PFOA L2133-7, DF=10 032604A-122 Sm (Mn, 2x2) 100-, ! 31-M ar-2004 07:53:051 LCMSMS #7 MRM of 1 Channel ES- 4.88 413 >369 1.77e5 Area 0 - `- f "1l I- I ' l~ T r T - p V T - T - T - T - '- f'- l 1.00 2.0 3.00 4.00 ' 5.00 r r - r - r r , - f - r r - r - . Ti me 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000155 Quantify Sample Report Page 23 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-123 Text: 1 : PFOA C032604-4, 1.0 ng/mL standard 032604A-123 Sm (Mn, 2x2) 100 % o A-,--.., 1.00 2.00 ... 3.00 4.89 167751 j 4.00 ' 1 5.00 31-Mar-2004 08:09:49 LCMSMS #7 MRM of 1 Channel ES413 >369 1.15e5 Area . 6.00 7.00 r , Time ! 8.00 ! Exygen Research, 3058 Research Drive, State College, PA 16801 000156 Quantify Sample Report Page 24 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: W e d Mar 31 12:00:54 2004 Name: 032604A-124 Text: 1 : PFOA L2133-1 032604A-124 Sm (Mn, 2x2) 100-, %- 31-Mar-2004 08:26:43 LCMSMS #7 MRM of 1 Channel ES- 4.90 413 >369 5.88e6 Area 1.00 2.00 3.00 4.00 5.0 6.00 7.00 -- 1 Time i 8.0 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000157 Quantify Sample Report Page 25 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A C SR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: W e d Mar 31 12:00:54 2004 Name: 032604A-125 Text: 1 : PFOA L2133-1 Rep 032604A-125 Sm (Mn, 2x2) 100-, %- I j o 'U -- 1.0 2.0 4.89 3.00 1 4.00 ` 5.00 31-Mar-2004 08:43:34 LCMSMS #7 MRM of 1 Channel ES413 >369 5.98e6 Area 6.00 ' 7.00 Time ^bo Exygen Research, 3058 Research Drive, State College, PA 16801 000158 Quantify Sample Report Page 26 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-126 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000159 Quantify Sample Report Page 27 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-127 Text: 1: PFOA L2133-3 032604A -127 Sm (Mn, 2x2) %- 11 1.00 .................. 2.00 3.00 4.89 A571361 4.00 5.00 31 -M ar-2004 09:17:03' LCMSMS #7 MRM of 1 Channel ES 413 >369 3.94e5 Area 1' ' 1j ' i ! | 6.00 7/30 eTbToime Exygen Research, 3058 Research Drive, State College, PA 16801 000160 Quantify Sample Report Page 28 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-128 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000161 Quantify Sample Report Page 29 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 06:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-129 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000162 Quantify Sample Report Page 30 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P: \Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-130 Text: 1: PFOA L2133-5 032604A-130 Sm (Mn, 2x2) 100- %- 4.90 2126942" 31-Mar-2004 10:07:21 LC M S M S #7 MRM of 1 Channel ES413 > 369 1 .46e7 Area 1.0 2.00 3.00 4.00 5.00 6.0 7.00 --n-n Time i 8.00 ! Exygen Research, 3058 Research Drive, State College, PA 16801 000163 Quantify Sample Report Page 31 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-131 Text: 1 : PFOA L2133-6 032604A-131 Sm (Mn, 2x2) %- 31-Mar-2004 10:24:07 LC M S M S #7 MRM of 1 Channel ES- 4.90 413 >369 5.25e6 Area ' 1.00 2.00 3.0 -r-- . , , , v. , , . .", i i 1i 4.00 5.00 6.00 Time | 7.00 ' 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000164 Quantify Sample Report Page 32 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-132 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000165 Quantify Sample Report Page 33 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-133 Text: 1 : PFOA C032604-2, 5.0 ng/mL standard 31-Mar-2004 10:57:53 LC M S M S #7 032604A-133 Sm (Mn, 2x2) MRM of 1 Channel ES- 100 4.90 413 >369 5.85e5 Area %- 0 'III. Time 1.00 2.0 3 .bo 4 .0 0 ' 5.0 6.00 7.bo ' 8.00 Exygen Research 3058 Research Drive State College, PA 16801 000166 Quantify Sample Report Page 34 StudyNo:L2133,SetNo:032604A CSR Solids, ExtDate:03/26-29/04, Analyst A. Sheehan Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\032604A CSR Solids Last modified: Wed Mar 31 11:45:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA non extract 032904 Last modified: Tue Mar 30 08:18:31 2004 Job Code: Printed: Wed Mar 31 12:00:54 2004 Name: 032604A-134 Text : 1: PFOA_______________________ C032604-1,10.0 ng/mL standard 032604A-134 Sm (Mn, 2x2) 100^ I^ % 4.90 179913 31-Mar-2004 11:14:48 LC M S M S #7 MRM of 1 Channel ES413 >369 1.21e6 Area 1.0 " ' " 2.00 3.0 1 4.0 1 5.00 6.00 7.0 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000167