Document 9oZE6LQK50m8z9ondXqEKaeR

AR226-3588 ANALYTICAL REPORT STLS E V E R N TRENT STL Denver 4955 Yarrow Street Arvada, CO 80002 Tel: 303 736 0 1 0 0 Fax: 303 431 7171 www.stl-inc.com - M J 90 E. I. DuPont Project: APFO Analysis (FAY) Fayetteville, NC Sampling 11/05 LBIO-65332 7035-504461-772000 Release STL 17459 Lot#: D5K230384 cn Michael Aucoin ADQM AP Services, CRG DuPont Barley Mill Plaza Bldg 27 Lancaster Pike & Route 141 Wilmington, DE 19805 Severn Trent Laboratories, Inc./STL Denver Project Manager November 30,2005 Revised Case Narrative January 26, 2006 Leaders in Environmental Testing UpgEV Severn Trent Laboratories, Inc. Tabl Of Contents p. 82 Standard Deliverables with Supporting Documentation R eport Contents Number o f Pages Standard Deliverables (The CoyerLetter and the Report Coverpage are considered intgrai parts o fthis StdfidardDelwerahfckkagfiTTKis'repcndWinmmptd''' unless allpages indicated in this Table o fContents are included.) Table of Contents Case Narrative Executive Summary - Detection Highlights Methods Summary Method/Analyst Summary Lot Sample Summary Analytical Results QC Data Association Summary Chain-of-Custody Supporting Documentation (Note: A one-page "Description o f Supporting Documentation" is provided at the beginning o fthis section.). Volatile GC/MS Check below when supporting documentation is present Semivolatile GC/MS Volatile GC Semivolatile GC LC/MS or HPLC Metals General Chemistry I Subcontracted Data STL D e n v e r L:\PMVPMs\Forais\toc_expanded.doc 1 D5K230384 p. 83 C ase N arrative D5K230384 The results included in this report have been reviewed for compliance with the Laboratory Quality Manual. All results have been found to meet all requirements of NELAC and any exceptions are noted below. This report shall not be reproduced except in full, without the written approval o f the laboratory or sponsor. Dilution factors and footnotes have been provided on each datasheet to assist in the interpretation of the results. Sample Arrival and Receipt The three aqueous samples and one field blank presented in this report were received at die STL Denver laboratory at a temperature o f 3.9C on November 23, 2005. Standards Analytical standards were prepared using the acid form of the compound perfluorooctanoic acid (PFOA). The concentrations are converted to express the concentration in round numbers as the ammonium salt ammonium perfluooctanoate (APFO) so that results can be reported as both PFOA and APFO. A di-carbon-13 labeled perfluorooctanoic acid, [l,2-di-'3C] was introduced at the extraction step and was used as an internal standard for quantitation of APFO and PFOA. Sample Extraction and Analysis The samples presented in this report were analyzed for the target analyte by STL Denver's SOP DENLC-0012A. The samples were tested unspiked only as insufficient sample volume was available to test the samples in duplicate and spiked with the target analyte. For water samples a 250 mL aliquot of each sample is acidified with 1 mL of 6N HC1 solution and it is extracted using solid phase extraction technique with methanol conditioned C l8 cartridges. Each sample is spiked with the internal standard, prior to extraction. After the sample is passed through the cartridge, the analytes are eluted with 4 mL of methanol. The final volume is brought to 5 mL using methanol and the extract is analyzed by LC/MS/MS. The target analyte is separated from other components on a high-performance liquid chromatography (HPLC) C18 column with a mobile phase mixture of water containing 0.1% formic acid and methanol. The mass spectrometer detector is operated in the electrospray (ESI) negative ion mode. The instrument is calibrated at 6 concentration levels (1, 2, 5,10,20, and 50 ug/L). The target analyte is detected as the perfluorooctanoate anion with the parent ion of 413 amu. The daughter ions used for analysis by LC/MS/MS are at 369 and 219 amu. The ratio of the peak areas to the two ions must be 20% of the ion ratios in the mid-point ICAL for qualitative identification. Sample results are quantitated using the internal standard method. Tuning and Calibration The instrument is tuned with a solution o f the target analyte such that mass assignments are within 0.5 amu of the daughter ions. The instrument is calibrated with six concentration levels from 1 ug/L to 50 ug/L. Linear regression (y=ax+b) was used with a correlation coefficient >0.990. STL D e n v e r 2 D5K230384 p. 84 Following initial calibration (ICAL), an initial calibration blank (ICB) is tested, which consists of methanol spiked with the surrogate. The result for the target analyte must be less than the limit of detection (LOD = 0.002 ug/L for waters) to proceed. Next an initial calibration verification (ICV) standard is tested. This is a mid-level concentration standard from a different vendor from the ICAL standard. The ICV must be within 80-120% of the true value. The quantitation limit verification standard (LOQ = 0.01 ug/L for waters) is a standard from the same source as the ICAL tested run at the LOQ level to determine accuracy near the detection limit. This recovery must be within 80-120%. Continuing calibration verification (CCV) standards are tested every 10 injections and are from the same source as the ICAL and are at mid-level concentration. The recovery of the CCVs must be 80-120% or recalibration is necessary. A closing calibration o f the six standards is also done to verify instrument drift and to verify the correlation coefficient. The recoveries of the 2, 10, and 50 ug/L standards must be 80-120%. Method OC Samples The Method Blank is processed reagent water spiked with internal standard and prepared with each batch of 20 samples o f the same matrix. All samples in the batch are processed at the same time and with the same reagents. The method blank must be less than the LOD or associated batch samples must be re extracted and reanalyzed. Each batch is prepared with a low- and a mid-level concentration spike Laboratory Control Samples (LCS). The recoveries o f these samples must be within 70-130% or associated batch samples must be re extracted and reanalyzed. If the recovery is biased high and samples are non-detect, results can be reported without re-extraction. Calculations 1. Sample Result Calculation For internal standard quantitation, APFO Response = area of APFO / area of APFO l,2-di13C Concentration in waters, ug/L = (C Vt)/(V0) Where: Cex = Concentration measured in sample extract from the target analyte response (ng/mL) Vt = Volume of total extract (mL) V0= Volume of water extracted (mL) If results are to be reported as ammonium perfluorooctanoate (APFO), in addition to PFOA, a multiplier of 1.0406 is applied to sample results to correct for the molecular weight differences between PFOA and APFO. This adjustment can also be made during the preparation of the standards used for calibration. STL D e n v e r 3 D5K230384 2. Percent Recovery Calculation Spike Recovery = (SSr-Sr)/(Sa)x100% Where: Ssr = Spike sample result Sr = Sample result SA= Spike added 3. Relative Percent Difference Calculation RPD = (S R - D r)/(1 /2 (S r-D r))x 100 Where: Sr = Sample result D r = Duplicate result PFOA/AfFO Analysis Anomalies No anomalies were noted. Revision . The report was revised 12/28/05 to report results to the LOD (recorded as the MDL in the report) and the LOQ (recorded as the RL in the report). The revision on 1/20/06 is to include the documentation on the LOD/LOQ determination, which follows the analytical report. The raw data is included in this submission. On 1/26/06 the case narrative was revised to remove references to APFN. STL D e n v e r p. 86 STL Denver STLS E V E K N TRUNT Executive Summary - Lot D5K230384 Sampling 11/05_________________________ Sample Number Clienti D 1 FAY-D-4328MLR Individual Results ug/L of APFO (a,b,c) 0.011 2 FAY-D-6999PED ND Final Result ug/L of APFO{d) 0.011 ND Reporting Detection Limit ug/L (e) Limit ug/L (f) 0.010 0.002 1 0.010 0.002 3 FAY-K-FBLK-1 ND ND 0.010 O.OQ'2 4 FAY-K-5319KAR NQ NQ 0.011 0.002 * (a) Method DEN-LC-0012 (b) DUP indicates a laboratory duplicate. (c) ND= Compound not detected at the detection limit (LOD) NQ= Compound detected at a level between the LOD and reporting limit (LOQ); result is not quantifiable Note: ND<LOD<NQ<LQQ . .. (d) If the sample and laboratory duplicate are both greater than 5X the L0 and the relative percent difference (f^PD) is less than 20, the average value is reported. If the RPD Is greater than 20, the higher of the sample and laboratory duplicate vajue is reported. If the sample/and or laboratory duplicate are less than 5X the LOQ, and the absolute difference is less than the L,OQ, the average value is reported, if the absolute difference is greater than the LOQ, the higher of the sample and laboratory duplicate value is reported. (e) Reporting Limit (RL) = LOQ adjusted for actual sample weight. See the case narrative concentration calculation. LOQ = Limit of Quantitation = 5 times LOD = 0.01 ug/L for waters. (f) Detection Limit (MDL) = LOD adjusted for actual sample weight. The LOD is the concentration of a method blnk that would correspond to three times the peak to peak amplitude of the baseline noise near the PFOA peak. - lh METHODS SUMMARY D5K230384 ANALYTICAL PARAMETER '______________________________________ __ METHOD______ LC/MS/MS, PFOA DEN -LC-0012 Rfrences: DEN Severn Trent Laboratores, Denver, Facility Standard Operating Procedure. PREPARATION METHOD STL D e n v e r p. 88 METHOD / ANALYST SUMMARY D5K230384 ANALYTICAL METHOD________________________ ANALYST_______________________ DEN -LC-0012 Steve Cowling References: " DEN Severn Trent Laboratores, Denver, Facility Standard Operating Procedure. ANALYST ID_____ 008738 STL D e n v e r 7 SAMPLE SUMMARY D5K230384 wo # SAMPLE# CLIENT SAMPLE ID HQW31 001 FAY-D-4328MLR HQW32 002 FAY-D-6999PED HQW34 003 FAY-K-FBLK-1 HQW3'? 004 FAY -D -5319iCAR NOTE(S): - The analytical results of the samples listed above are presented on the following pages. - All calculations are performed before rounding to avoid round-off errors in calculated results. - Results noted as "ND" were not detected at or above the stated limit. - This report must not be reproduced, except in full, without the written approval of the laboratory. - Results for the following parameters are never reported on a dry weight basis: color, corrosivity, density, flashpoint, ignitability, layers, odor, paint filter test, pH, porosity pressure, reactivity, redox potential, specific gravity, spot tests, solids, solubility, temperature, viscosity, and weight. SAMPLED SAMP DATE TIME 11/16/05 13:10 11/16/05 14:13 11/16/05 15:20 11/16/05 13:57 STL D e n v e r 8 p. 90 E.I. Dupont De Nemours and Co Client Sample ID: FAY-D-4328MLR HPLC Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #... Dilution Factor D5K230384-001 Work Order #...: HQW311AA 11/16/05 13:10 Date Received..: 11/23/05 11/28/05 Analysis Date..: 11/29/05 5329125 1 Analysis Time..: 18:43 Metfiodl........ : DEN -LC-0(112 Matrix PARAMETER_________________ PFQA Ammonium Perfluorooctanoate (APFO) RESULT 0.010 0.011 REPORTING LIMIT 0.010 0.010 UNITS ug/L ug/L MDL 0.0020 0.0020 SURROGATE 13C2 PERCENT RECOVERY RECOVERY_______ LIMITS 80 (50 - 200) WATER STL D e n v e r 9 E.X. Dupont De Nemours and Co Client Sample ID: FAY-D-6999PED HPLC Lot-Sample #... Date Sampled.;.. Prep Date..... Prep Batch #... Dilution Factor D5K230384-002 Work Order #... 11/16/05 14:13 Date Received.. 11/28/05 Analysis Date.. 5329125 Analysis Time.. 1 Method1:1....... HQW321AA 11/23/05 11/29/05 18:47 DEN" -EC- CTT2' Matrix PARAMETER PFOA . Ammonium Perfluorooctanoate (APFO) RESULT ND ND REPORTING LIMIT 0.010 0.010 UNITS ug/L ug/L MDL 0.0020 0.0020 SURROGATE 13C2 PERCENT RECOVERY 76 RECOVERY LIMITS (50 - 200) WATER STL D e n v e r E.I. Dupont De Nemours and Co Client Sample ID: FAY-K-FBLK-l HPLC Lot-Sample #... Date Sampled... Prep Date..... Prep Batch #... Dilution Factor D5K230384-003 Work Order #... 11/16/05 15:20 Date Received.. 11/28/05 Analysis Date.. 5329125 1 Analysis Time.. Method'/........ HQW341AA 11/23/05 11/29/05 18:52 DEW -ECT-01Z Matrix : WATER PARAMETER___________________ PFOA Ammonium Perfluorooctanoate (APFO) RESULT ND ND REPORTING LIMIT 0.010 0.010 UNITS ug/L ug/L MDL 0.0020 0.0020 SURROGATE 13C2 PERCENT RECOVERY 80 RECOVERY LIMITS (50 - 200) STL D e n v e r p. 93 E.I. Dupont De Nemours and Co Client Sample ID: FY-D-5319KAR HPIiC Lot-Sanple #... Date Sampled... Prep Date..... Prep Batch # __ Dilution Factor D5K230384-004 11/16/05 13:5 11/28/05 5329125 1 Work Order #...: HQW351AA Date Received..: 11/23/05 Analysis Date..: 11/29/05 Analysis Time..: 18:56 Method........ : DEN -LC-0012 Matrix P A R A M E T E R _______________________________ PFOA Ammonium Perfluorooctanoate (APPO) RESULT 0.0051 J 0.0053 J REPORTING LIMIT 0.011 0.011 UNITS_____ ug/L ug/L MDL 0.0020 0.0020 SURROGATE 13C2 PERCENT RECOVERY 89 RECOVERY LIMITS (50 - 200) N O T E (S ) :__________________ J Estimated result Result is less than RL. WATER STL D e n v e r 12 p. 94 QC DATA ASSOCIATION SUMMARY D5K230384 Sample Preparation and Analysis Control Numbers SAMPLE# MATRIX 001 WATER 002 . WATER 003 WATER 004 WATER ANALYTICAL METHOD DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 DEN -LC-0012 LEACH BATCH # PREP BATCH # 5329125 5329125 5329125 5329125 MS RUN# 5329070 5329070 5329070 5329070 STL D e n v e r 13 METHOD BLANK REPORT HPLC Client Lot # __ D5K230384 Work Order # __ : HQXPR1AA MB Lot-Sample # R5K250000-125 Prep Date..... : 11/28/05 Analysis Date.. 11/29/05 I Dilution Factor 1 Prep Batch. # __ : 5329125 M atrix................. : WATER Analysis Time..: 18:30 PARAMETER________________ PFOA Ammonium Perfluorooctanoate (APFO) REPORTING RESULT_________ LIMIT UNITS______ METHOD______ ND 0.010 ug/L DEN -LC-0012 ND 0.010 ug/L DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 80 RECOVERY LIMITS (50 - 200) N O T E (S ) :__________________________________________________ Calculations are performed before rounding to avoid round-off errors in calculated results. I STL D e n v e r 14 LABORATORY CONTROL SAMPLE DATA REPORT HPLC Client Lot #...: D5K230384 Work Order HQXPR1AC LCS Lot-Sample#: R5K250000-125 Prep Date..... : 11/28/05 Analysis Date..: 11/29/05 Prep Batch # -- : 5329125 Analysis Time..: 18:34 Dilution Factor: 1 Matrix PARAMETER Ammonium Perfluorooctanoate (APFO) SPIKE AMOUNT 0.208 MEASURED AMOUNT 0.211 UNITS ug/L PERCENT RECOVERY 101 METHOD DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 86 NOTE(S): ___________________________________ Calculations are performed before rounding to avoid round-off errors m calculated results. Bold print denotes control parameters RECOVERY LIMITS (50 - 200) STL D e n v e r 15 LABORATORY CONTROL SAMPLE DATA REPORT HPLC Client Lot #... LCS Lot-Sample# Prep Date..... Prep Batch #... Dilution Factor D5K230384 Work Order #... R5K250000-125 11/28/05 Analysis Date.. 5329125 Analysis Time.. 1 HQXPR1AD 11/29/05 18:39 Matrix........ : WATER PARAMETER_____________ __ Ammonium Perfluorooctanoate (APPO) SPIKE AMOUNT 0.0208 MEASURED AMOUNT 0.0212 PERCENT UNITS_____ RECOVERY METHOD______ ug/L 102 DEN -LC-0012 SURROGATE 13C2 PERCENT RECOVERY 79 NOTE(S):_____________________________________ Calculations are performed before rounding to avoid round-off errors in Bold print denotes control parameters results. RECOVERY LIMITS (50 - 200) STL D e n v e r 16 p. 98 Composite Number of Containers STL D enver PROJECT INFORMATION Client (name & address): - ........ / w - A / - ' / LC * i.l\ (Oje CHAIN O F CUSTODY/ANALYSIS REQUEST FORM Exygen Research Sample Receiving 3048 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com (x Page of , / AMAI V S P S D P m ICCTCr1 . : ... 1 n ^f Project Manager (Namey& E/-mail Address): Project Name: Fax:"6 ' Sampler: ----------------------------------------------- -- p F I T ------------ Quotation # : Please fill out this form co m p le tely to ensure correct analysis and proper handling of your samples. SA M PLE AN ALYSIS ExyLIMS# Client Sample Identification Collection Collection D ate Tim e - D - H I* /// ~ r /// F /I'J - D 'C s Ifa / P / / A ir ' ///; F / f a - - F / t Z - i ___________ //./6 r / n - V./fc.o/ r t n O 2 o Specify M atrix _5 f L t, 1_ Comments <79 J f / t 99 i 57 `n s r o ? 99z'fi r X s. o> \ V- \ s. 'vi Yy /X /y yy V H. Y TT `f n! oA-i7li 9it vci,, LAB USE ONLY CHAIN OF CUSTOD Relinquished by Date Time OTHER INFORMATION -- Cooler ID # Received by r13 Cooler Temp. (C )^ ^ Date Time ~ / / / ? Ar~ //U /y/T<--T&-/-g5-- LAB USE ONLY PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: [~l Sample results only I I Add case narrative Add quality control summary O A d d calibration summary I I Add raw data HU Other REV. 6-04 STL Denver Sample Receiving Checklist Lot #:_ l ^ K s ^ , ^ Company Name & Sampling Site: PM to Complete This Section: Yes Residual chlorine check required:Q Quote #: Special Instructions: Ni Yes Quarantined : No Time Zone: EDT/EST CDT/CST MDT/MST - PDT/PST OTHER Unpacking Checks: Cooler #(s): _ ! Temperatures (C): C3i 9 N/A Yes No X X 1. Cooler seals intact? (N/A i f hand delivered) I f no, document on CUR. 2. Chain o f custody present? I f no, document on CUR. Initiab _ X X 3. Bottles broken and/or are leaking? I f yes, document on CUR. 4. Multiphasic samples obvious? If yes, document on CUR. X 5. Proper container & preservatives used? (ref. Attachment D o f SOP# DEN-QA-0003) I f no, document on CUR. X 6. pH o f all samples checked and meet requirements? I f no, document on CUR. X 7. Sufficient volume provided for all analysis requested? (ref. Attachment D of SOP# DEN-Q A-0003) If no, document on CUR, and contact EM before proceeding. X 8. Did chain o f custody agree with labels ID and samples received? If no, document on CUR. X 9. Were VOA samples without headspace? If no, document on CUR. X 10. Were VOA vials preserved? Preservative dH C l 0 4 2 C QSodium Thiosulfate O Ascorbic Acid X 11. Did samples require preservation with sodium thiosulfate? X 12. If yes to #11, did the samples contain residual chlorine? I f yes, document on CUR. X 13. Sediment present in dissolved/filtered bottles? I f yes, document on CUR. x contact PM before proceeding. X 15. Receipt date(s) > 48 hours past the collection date(s)? X X S T l } Q '$ t T $ % 3*e Recs>vTMg\Saniple Receiving Checklist 12 13 04 revision 12/13/04 18 STL Denver Sample Receiving Checklist p. 100 Lot # M Login Checks: Initials N/A\ Yes No X ' 18. Sufficient volume provided for all analysis requested? (ref. Attachment D o f SOP# DEN-QA-0003) If no, document on CUR, and contact PM before proceeding. X 19. Is sufficient volume provided for client requested MS, MSD or matrix duplicates? If no, document on CUR, and contact PM before proceeding. 20. Did the chain o f custody includes "received by" and "relinquished" by signatures, dates, and times? J2T 21. Were special log in instructions read and followed? AO X 22 l Were AFCEE metals logged for refrigerated storage? 23. Were tests logged checked against the COC? Which samples were confirmed? X ' 24. Was a Rush form completed for quick TAT? A 25. Was a Short Hold form completed for any short holds? , /________ X 26. Is "Strict ICOC" required? X X 27. Were special archiving instructions indicated in the General Comments? If so, what were they? 28. Was the subcontract COC signed and sent with samples to bottle prep? 29. Were sample labels double-checked by a second person? -- Q 30. Were sample bottles and COC double checked for dissolved/filtered metals by a second person? O ''""'0 31. D id the sample ID, Date, and Time from label match what was logged? O O 32. Were stickers for special archiving instructions affixed to each b ox and to the ICOC? See #27 Q O 33. Were AFCEE metals stored refrigerated? O O Q 34. Were "Strict ICOC' copies given to satellite storage areas? Document any problems or discrepancies and the actions taken to resolve them on a Condition Upon Receipt Anomaly Report (CUR). \QA\Forms\Sample Receiving\Sample Receiving Checklist 12 13 04 revision STL Denver " 12/13/04 19 Lot Number: 2.3^3&,<4 u g am e w a ia jveview a e m p ia te p. 101 Client: XbuiDtPoT_________ Analytical Due Date: lS>- IS-CST____ Sample Numbers: I ~ H_________ PA/PM: Reviewed by/Date: d il- ^Q.oC" Method: -^ a . f ~P P oO _____________Batch #: 5 3 3 9 1 ^ 5 C alib ratio n Issues: YES (N O ) ICAL/ICV/CCV (NCM#04-________ ) Den-Std. /p B ' DCS CLP FormSrt^b / 6-8 AFCEE forms 1: H olding Time: _J^A U samples were prepped and analyzed within the method-specific holding time requirements. ______ Samples in this lot were extracted and/or analyzed beyond the required hold-time. (NCM#04-__________ ) 2: M ethod Blank S ' All criteria were met for the method blank. ______ Criteria for m ethod blank w ere not met. (NCM#04-__________) 3: LCS/LCSD i/^ All spike recoveries and RPD data met method QC criteria ______ Recoveries and/or RPDs failed method QC criteria. (NCM#04-__________ ) 4: MS/MSD ______ All spike recoveries and RPD data m et method QC criteria ______ Recoveries and/or RPDs failed method QC criteria. (NCM#04-__________ ) ______ Recoveries diluted out. S ' No MS/MSD. (NCM #04-_S58NV_) 5: Sample D ata ^ No issues w ith sample data. ______ The automated form ula printed on the quantitation report was checked and is accurate. ______ Sample(s)_______________________________ had surrogate failures. (NCM #04-__________) ______ Sample(s)_______________________________ had ISTD failures. (NCM#04-__________) ______ Sample(s)____________ :__________________ were analyzed at a dilution due to target compounds. ______ Sample(s)______________________________ were analyzed at a dilution due to final extract volume/ starting volume extracted. (NCM #04-_____________ ) ______ Sample(s)______________________________ were analyzed at a dilution due to non-target matrix. (NCM#04-__________ ) I 6: Based on review o f chromatograms for sam ple(s)___________________ , it is m y opinion that the evident interferences are potentially causing false positive/negative results. D a te ________A n aly st____________ 7: Comments STL D e n v e r p. 102 LOD/LOQ Detennination I STL D e n v e r 21 p. 103 STL D e n v e r 22 p. 104 STL D e n v e r 23 p. 105 3>0 Q o f \M c X e r ; LOO O. I j^ /l V ' l s y t ' ' - O.OOT~^L L061 0 , 0 0 % # S' 0'O l -- L O T > I o o .a s Y ' -gPO w *= __ - ttf ' / o cT' / U a , b '/V k3f r IDOL O S ' ^ $" r- U C^f !i | STL D e n v e r 24 p. 106 p. 107 L C /M S Supporting Documentation Sample Sequence, Chromatograms/Mass Spectra SEVERN TRENT Lot ID: Client: Method: Fc>A______ A ssociated Samples: ______ Batch #(s): I certify that, to the best o f my knowledge, the attached package represents a complete and accurate copy o f the original data. Sienature/Date: > - U. Z 0OS'" STL D e n v e r 26 p. 108 LC/MS SEMIVOLATILE ORGANIC EXTRACTION LOG SHEETS STL D e n v e r 27 p. 109 STL D enver RQC058 Severn Trent Laboratories, Inc. EXTRACTION BENCH WORKSHEET LEV LEV LEV LEV 12 '1 7~ ~ y Y Blank Y Y Weights/Volumes Y Y Check Y Y Spike & Surrogate Worksheet " m s /ms d Y Y Vial contains correct volume Y Y Labels, greenbars, worksheets computer batch: correct & all match Y Y Anomalies to Extraction Method Extractionist: 006091 Jon Laviolette Concentrationisf TJTT6091 Jon Laviolette ************************ ** * QC BATCH: 5329125 ** ************************ Run Date: 11/28/05 Time: 10:54:19 Expanded Deliverable COC Completed Bench Sheet Copied Package Submitted to AnalyticalGr Bench Sheet Copied per COC PREP DATE: 11/28/05 8:00 COMP DATE: 11/28/05 11:00 Reviewer/Date: LAVIOLJA / 11/28/05 EXTR EXPR ANL LOT#,MSRUN#/ TEST DUE WORK ORDER FLGS D5K230384-001 11/23/05 12/12/05 HQN31-1-AA D COMMENTS EXT MTH MATRIX B7 H5 WATER LC/MS/MS, PFOA SOLID PHASE EXTRACTION (NOMINAL) INIT/FIN PH"S SOLVENTS WT/VOL INIT ADJ1 ADJ2 EXTRACTION-VL EXCHANGE 251mL 7.0 2.0 NA MEOH 5.OOmL 4.0 SPIKE STANDARD/ VOL SURROGATE ID .0 1.0ML 919.47.3 11/16/ D5K230384-002 11/23/05 12/12/05 HQW32-1-AA D COMMENTS: B7 H5 WATER 250mL 5.OOmL 7.0 2.0 NA MEOH 4.0 .0 1.0ML 919.47.3 11/16/ D5K230384-003 11/23/05 12/12/05 HQM34-1-AA D COMMENTS: B7 H5 WATER 251mL 5.OOmL 7.0 2.0 NA MEOH 4.0 .0 1.0ML 919.47.3 11/16/ D5K230384-004 11/23/05 12/12/05 HQN35-1-AA D COMMENTS: B7 H5 WATER 233nL 5.OOmL 7.0 2.0 NA MEOH 4.0 .0 1.0ML 919.47.3 11/16/ R5K250000-125 11/23/05 0/00/00 HQXPR-l-AAB COMMENTS: B7 H5 WATER 250mL 7.0 2.0 NA MEOH 5.OOmL 4.0 .0 1.0ML 919.47.3 11/16/ R5K250000-125 11/23/05 0/00/00 HQXPR-l-ACC COMMENTS: B7 H5 WATER 250mL 7.0 2.0 NA MEOH 5.OOmL 4.0 .0 1.0ML 911.191.1 10/12 1.0ML 919.47.3 11/16/ R5K250000-125 11/23/05 0/00/00 HQXPR-l-ADC COMMENTS: LOW-LCS B7 H5 WATER 250mL 7.0 2.0 NA MEOH 5.OOmL 4.0 .0 0.1ML 911.191.1 10/12 1.0ML 919.47.3 11/16/ DEN-LC-0012 MEOH:B25B2Q 6N HCL:919.48.1 S/S:JL-A BAL:M9U2I2 H20:B28E53 CAKT ;5201-30,16648-4 W:JC R RUSH C = CLP E = EPA 600 D = EXP.DEL) NUMBER OF WORK ORDERS IN BATCH: ---7 C\J 00 p. 110 CLIENT REQ MS/MSD 1 STL D e n v e r 29 p. 111 LC/MS SEMIVOLATILE INSTRUMENT RUN LOG STL D e n v e r 30 Sample List Report MassLynx 4.0 SP4.525 Sample List: C:\MassLynx\PFOA.PRO\SampleDB\pf35k29(4).SPL Last Modified: Wednesday. November 30, 2005 7:39:38 AM Mountain Standard Time Printed: Wednesday, November 30, 2005 7:47:24 AM Mountain Standard Time p. 112 Page 1 of 2 Page Position (1,1) File Name Sample ID File Text Sample Type PFOA pg/L or kg APFO pg/L or kg Bottle 1 pf35k2972 919.59.1 Blank Blank 2 pf35k2973 919.59.2 0.2 pg/L Standard 3 pf35k2974 919.59.3 0.5 pg/L Standard 4 pf35k2975 919.59.4 1 pg/L Standard 5 pf35k2976 919.59.5 2 pg/L Standard 6 pf35k2977 919.59.6 5 pg/L Standard 7 pf35k2978 919.59.7 10 pg/L Standard 8 pf35k2979 919.59.8 20 pg/L Standard 9 pf35k2980 919.59.1 Blank Blank 10 pf35k2981 919.59.9 2 pg/L ICV QC 11 pf35k2982 919.59.2 0.2 pg/L QC 12 pf35k2983 HQXPR1AA R5K250000-125 MB Blank 13 pf35k2984 HQXPR1AC R5K250000-125 LCS QC 14 pf35k2985 HQXPR1AD R5K250000-125 LCS QC 15 pf35k2986 HQW311AA D5K230384-1 Analyte 16 pf35k2987 HQW321AA D5K230384-2 Analyte 17 pf35k2988 HQW341AA D5K230384-3 Analyte 18 pf35k2989 HQW351AA D5K230384-4 Analyte 19 pf35k2990 919.59.1 Blank Blank 20 pf35k2991 919.59.2 0.2 pg/L Standard 21 pf35k2992 919.59.3 0.5 pg/L Standard 22 pf35k2993 919.59.4 1 pg/L Standard 23 pf35k2994 919.59.5 2 pg/L Standard 24 pf35k2995 919.59.6 5 pg/L Standard 25 pf35k2996 919.59.7 10 pg/L Standard 26 pf35k2997 919.59.8 20 pg/L Standard 0 0.2 0.5 1 2 5 10 20 0 2 0.2 0 0.2 0.02 0 0 0 0 0 0.2 0.5 1 2 5 10 20 0 0.208 0.520 1.041 2.082 5.205 10.411 20.821 0 2.082 0.208 0 0.208 0.0208 0 0 0 0 0 0.208 0.520 1.041 2.082 5.205 10.411 20.821 1:1,A 1:1,B 1:1,C 1:1,D 1:1,E 1:1,F 1:2,A 1:2,B 1:1,A 1:2,C 1:1,B 2:1,A 2:1,B 2:1,C 2:1,D 2:1,E 2:1,F 2:2,A 1:1,A 1:1,B 1:1,C 1:1,D 1:1,E 1:1,F 1:2,A 1:2,B STL D e n v e r 31 Sample List Report MassLynx 4.0 SP4.525 Sample List: C:\MassLynx\PFOA.PRO\SampleDB\pf35k29(4).SPL Last Modified: Wednesday, November 30, 2005 7:39:38 AM Mountain Standard Time Printed: Wednesday, November 30, 2005 7:47:24 AM Mountain Standard Time Extract mL Sample mL or g Dilution Inject Volume MS Tune File Inlet File MS File 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 5.000000 5.000000 5.000000 5.000000 5.000000 5.000000 5.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 250.000000 250.000000 250.000000 251.000000 250.000000 251.000000 233.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 1.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 20.000000 PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOA2 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS STL D e n v e r p. 114 LC/MS SEMIVOLATILE STANDARD DATA STL D e n v e r 33 p. 115 STL Denver Quantify Calibration Raport PFQA Analysis Calibration: C:\NassLynx\PFQA.PRO\CurveDB\pa35k29d Last nodifiad: Mad Nov 30 07:13:38 2005 Printad: Had Nov 30 07:15:12 200$ U> p. 116 STL D enver Quantify Calibration Report PPQA Analysis Calibration: C: \MasLynx\PPOA. PRO\CurveDB\pe35)c29d Last Modified: Wed Nov 30 07:43:38 2005 Printed: Wed Nov 30 07:45:13 3005 Analyst: Steve Cowling OJ cn Page 2 p. 117 STL D enver Quantify Calibration Report proA Analysis Calibration: C:\MasaLynx\PPOA.PRO\CurveD8\pa35k29d Last modified: Wad Nor 30 07:43:38 2005 Printad: Wad Nov 30 07:45:12 2005 Compound 3 name: PFOA 13C2 Method File: pa35k29 Response Factor: 1130.98 R R F SD: 23.1531, % Relative SD: 2.04717 Response type: External Std, Area Curve type: RF Analyst: Steve Cowling OCTJi Page 3 p. 118 STL Denver Quantify Calibration Rsport PFOA Analysis Calibration: C: \MassLynx\PPOA.PRO\CurvaDB\pa3Sfc29d Last modi.fi4: Wed Nov 30 07:43:38 3005 Printad: Wad Nov 30 07:45:12 2005 Analyst: Stavs Cowling OJ <1 p. 119 STL Denver Quantify Sanple Report Pro* Analysis Sample List: C:\NaaSLynx\PrOA.PRO\8anpleDB\pf35k29(4) Last modified: Wed Nov 30 07:39:38 300S Method: C:\MassLynx\PFOA.PRO\MethDB\pa3Sk29b Last modified: Wed Nov 30 07:23:49 200S Job Code: Printed: wed Nov 30 07:45:13 2005 Name: pf35k2972 Text: Blank # Name 1 PPOA 2 APFO 3 PFOA 13C2 4 PPOS ID 919 59.1 919 59.1 919 59.1 919 59.1 Sample Text Blank Blank Blank Blank RT 2.009 2.009 1.981 Area Flags 256 bb 256 bb 12656 bb yg/L or kg<) KRec Mod-Coament 0.0401 0.0415 11.1904 111.90 Analyst: Steve Cowling OJ 00 p. 120 STL D enver Quantify Saiqple Report PFOA Analysis 8aaple List: C :\MASSLynx\PrOA.FRO\SanpleDB\pf35k29(4) Last modified: Wad Nov 30 07:39:38 2005 Msthod: C:\KsssLyax\PrOA.PRO\HethDB\pa3Sk29b Last modified: Wad Nov 30 07:23:49 2005 Job Coda: Prlntad: Wad Nov 30 07:45:13 2005 Pag 2 Nna: pf35k2973 Text: 0.2 pg/L 0.2 pg/L 919.59.2 pf35k2973 Sm (Mn, 1.98 57 ]\ 3: PFOA 13C2 29-Nov-2005 0.2 pg/L 29-Nov-2005 0.2 pg/L 29-Nov-2005 0.2 pg/L 29-NOV-2005 17:45:25 919.59.2 17:45:25 919.59.2 17:45:25 919.59.2 17:45:25 2x2)F1pf35k2973 Sm (Mn, 2x2) F1 pf35k2973 Sm (Mn, 2x2) F1 pf35k2973 Sm (Mn, 2x2)F1 412.8 >218.7 426 1.98 412.8 >218.7 5 7 1\ 426 1.98 414.8 >369.7 11361] 8.06e4 2.63 498.6 > 79.9 598 Area Area Area Area 1.00 2.00 3.00 1.00 2.00 3.00 pf35k2973 Sm (Mn, 2x2) F1 pf35k2973 Sm (Mn, 2x2) F1 1.99 412.8 >368.7 492 ]\ 3.09e3 1.99 412.8 >368.7 492 3.09e3 Area Area I PI f p l T l I f l M l j T l i *i | I ff'I \ l l IT^T T i T* T i m 1.00 2.00 3.00 3 1111 nifi'11<|ifTf| iiii |n11 Time 1.00 2.00 3.00 Naas 1 PFOA 2 APFO 3 PFOA 13C2 4 PFOS ID 919.59.2 919.59.2 919.59 2 919-59-2 8aapls Text 0.2 pg/L 0.2 pg/L 0.2 ug/L 0.2 ug/L AT 1.995 1.995 1.981 2.631 Area Flags 492 bb 492 bb 11361 bb 90 bb ug/L or kg() %R*c 0.2348 117.42 0.2442 117.41 10.0448 100.45 0 . 2 2 1 1 110.56 rpiii fTTHTj *!111 11irti |11 1 1 1 1 1 11 Time 1.00 2.00 3.00 Time 1.00 2.00 3.00 Analyst: Steve Cowling OJ KD p. 121 STL d (D Quantify Sauple Report PFOA Analyais 6m l List: C:\MessLyxuc\PFGA.PAQ\8esleDB\pf35K29(4) vD Le.t modified: wed Ncnr 30 07:39:38 2005 h Method: C :\MessLynx\PFOA.PR0\MathDB\pa3S*29b Lest modified: Wed Nov 30 07:23:49 2005 Job Code: Printed: Wed Nov 30 07:45:13 2005 Page 3 Name: pf35k2974 Text: 0.5 pg/L 3: PFOA 13C2 0.5 pg/L 29-Nov-2005 0 .5 1ig/L 29-Nov-2005 0.5 pg/L 29-Nov-2005 0.5 pg/L 29-Nov-2005 919.59.3 17:49:54 919.59.3 17:49:54 919.59.3 17:49:54 919.59.3 17:49:54 pf35k2974 Sm (Mn. 2x2) F1 1.99 412.8 >218.7 543 Area pf35k2974Sm (Mn, 2x2) F1 1.99 412.8 >218.7 79 ]\ 543 Area pf35k2974 Sm (Mn, 2x2) F1 1.98 414.8 > 369.7 11351] 8.15e4 Area pf35k2974 Sm (Mn, 2x2) F1 2.62 498.6 > 79.9 169 1.10e3 - Area 103 1.00 2.00 3.00 pf35k2974 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 7421\ 4.93e3 Area 10 j m Y f f i i n i n i .00 2.00 3.00 pf35k2974 Sm (Mn, 2x2) F1 1.98 412.8 > 368.7 742 4.93e3 Area Timein 111 M [in [T frif 1 1 m i 1.00 2.00 3.00 Iiytni;r111111lYpf111111111Hl Time 1.00 2.00 3.00 0s - n-n-rr Time 1.00 2.00 3.00 4 ' 1.00 2.00 3.00 Mene pfoa APPO PFOA 13C2 pros ID 919.593 919.59.3 919.59.3 919.59.3 Bewple Text 0.5 pg/L 0.5 pg/L 0.5 pg/L 0.5 pg/L RT 1.981 1.981 1.981 2.617 Aree Plegs 742 bb 742 bb 11351 bb 169 bb pg/L or kg() XRec 0 4204 84.08 0.4374 84.11 10.0365 100.37 0.4366 87.32 Analyst: Steve Cowling O p. 122 STL Denver Quantify S w v l e Raport PFOA Analyaia S u o la L i l t : C: \HlllLynx\PFOA .PRO\SmllDB\pf 35K29 (4 ) iwadifiad: Nad Nov 30 07:39:38 2005 Matbod: C:\MaaaLynx\PF0A.PR0\MathDB\pa35k29b Last modified: Nad Nov 30 07:23:49 2005 job Coda: Printad: Nad Nov 30 07:45:13 2005 Page 4 Nana: pf35k2975 Taxt: 1 pg/L 1: PFQA 1 pg/L 919.59.4 pf35k2975 Sm (Mn. 1.98 178 29-Nov-2005 17:54:22 2x2) F1 412.8 >218.7 1.32e3 Area 2: APPO 1 pg/L 29-Nov-2005 919.59.4 17:54:22 pf35k2975 Sm (Mn, 2x2) F1 1.98 412.8 >218.7 178 7\ 1.32e3 Area 3: PFQA 13C2 1 pg/L 29-NOV-2005 919.59.4 17:54:22 pf35k2975 Sm (Mn, 2x2) F1 1.98 414.8 >369.7 11377] 8.09e4 Area PFOS 1 pg/L 919.59.4 pf35k2975 Sm 29-Nov-2005 17:54:22 (Mn, 2x2)F1 2.63 498.6 > 79.9 388 2.49e3 Area 5 ~"rrsi'|Tin |T |n |1 n t 11M I"|rrr i f 1.00 2.00 3.00 pf35k2975 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 1574 1.07e4 Area 5 ~*lirrrrTTTfnI; ii* )>it 1.00 2.00 3.00 pf35k2975 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 1574 1.07e4 Area 1 V IM IN I "M M I 11" 1I " i r Time 1.00 2.00 3.00 T- Time11 1 1 1 1 1 1 | 11 | I | ri | i n 1.00 2.00 3.00 VrrrTT1T1TITTT Time 1.00 2.00 3.00 2 llirp| lTIT] IIn p IIqHHf|i ufi m I Time 1.00 2.00 3.00 _ # Nana 1 PFOA 2 APFO 3 PFOA 13C2 4 PFOS ID 919.59.4 919.59-4 919.59.4 919.59.4 Saavla Taxt 1 pg/L 1 pg/L 1 pg/L l pg/L RT 1.981 1.981 1.981 2.631 Araa Flag 1S74 bb 1574 bb 11377 bb 388 bb pg/L or kg<) %Rao Mod.C< 1.0354 103.54 1.0777 103.52 10.0596 100-60 1.0248 102.48 Analyst: stava cowling p. 123 STL D enver Quantify Sanple Report PFOA Analysis Sample List: C :\KaasLynx\PFQA. PRO\&aavleDB\pf 35k29 (4) Last modified: Mad Nov 30 07:39:38 3005 Method: C:\MassLynx\PrOA.PRO\MathOB\pa35k29b Last modified: Med Nov 30 07:23:49 3005 Job Code: Printed: wed Nov 30 07:45:13 2005 Name: pf3Sk2976 Text: 2 pg/L 2 |ig/L 919.59.5 2: APPO 29-Nov-2005 2 pg/L 17:58:49 919.59.5 29-Nov-2005 17:58:49 pf35k2976Sm (Mn, 2x2) F1 pf35k2976 Sm (Mn. 2x2) F1 1.99 412.8 >218.7 1.99 412.8 >218.7 332 H 2.37e3 332 2.37e3 Area Area 3 ~l|ilrfriiipm'rriili|ihiTii"T 1.00 2.00 3.00 3 '" m1111111m IMi'i11h IJH Ir|ITT 1.00 2.00 3.00 pf35k2976 Sm (Mn, 2x2) F 1 pf35k2976 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 1.98 412.8 >368.7 2800 1.97e4 2800 1.97e4 Area Area 1 i i ii i-r. iTT-p11 )iiJ.t.Vi 111 11 ;iti i Tim e 1.00 2.00 3.00 r p i r r p T i 111 ri )i n 1 1 1 n >11 r nr Time 1.00 2.00 3.00 Name 1 PFOA 2 APPO 3 PFOA 13C2 4 PFOS ID 919.59.S 919.59.5 919.59.5 919.59.5 flanple Text 2 pg/L 2 pg/L 2 ug/L 2 pg/L AT 1.981 1.981 1.981 2.631 Ares riege 2800 bb 2800 bb 11458 bb 757 bb pg/L or kg() XRec Mod. Consent 1.9283 96 41 2.0072 96 41 10.1311 101.31 2.0057 100 29 Analyst: Steve Cowling to Pag 5 ___ ___________________________ p. 124 STL D enver Quantity Sasv>la Raport pfoa Analysis 8 anpla List: C: \HaSSLynx\PFOA.PRO\SanplnDB\pi35k29<4) Last ModiClad: Mad Nov 30 07:39:3ft 2005 Matbod: C :\MassLyznc\PPOA.PRO\MathDB\pa35k29b Last modifiad: Mad Mov 30 07:23:49 2005 job coda: Priatad: Mad Mov 30 07:45:13 2005 Pag* 6 ________ ______ Nana: pf35k2977 Taxt: S pg/L 5 pg/L 29-Nov-2005 5 pg/L 919.59.6 18:03:17 919.59.6 pf35k2977 Sm (Mn, 2x2) F1 pf35k2977 Sm (Mn, 1.98 412.8 >218.7 1.98 765 5.53e3 765 Area 3: PFOA 1 3 C 2 __________________________. 4: PFOS _________________________ _______ 29-Nov-2005 5 pg/L 29-Nov-2005 5 pg/L 29-Nov-2005 18:03:17 919.59.6 18:03:17 919.59.6 18:03:17 2x2)F1pf35k2977 Sm (Mn, 2x2) F1 412.8 >218.7 1.98 414.8 >369.7 5.53e3 Area pf35k2977 Sm (Mn, 2x2) F1 2.63 498.6 >79.9 1859" 1.13e4 Area 1 li111 p r n 111111 1ii'|i> n |ttti 111 n 1 1 1 1 1 piti ip 1 1 1 1 1 1 n [i )n 1 1 1 1 1 1 1 1 n 1.00 2.00 3.00 1.00 2.00 3.00 pf35k2977 Sm (Mn, 2x2) F1 pf35k2977 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 1.98 412.8 >368.7 6829H 4.84e4 6829H 4.84e4 Area Area 0 i|" " l" IJl" l*i|i**'TI'i'TPIn Time 1.00 2.00 3.00 0 111111<<-f>iii Time 1.00 2.00 3.00 *>n i|tti i[ni 111 111 11 i1 in ^ r r Time 1.00 2.00 3.00 Nans 1 PFOA 2 APFO 3 PFOA 11C2 4 PFOS ZD 919.59.6 919.59.6 919.59.6 919.59.6 8 as>l* Taxt 5 pg/L 5 pg/L 5 pg/L 5 pg/L RT 1.981 1.961 1.981 2.631 Arsa Flags 6829 bb 6829 bb 11623 bb 1859 bb pg/L or kg() KRac 4.8178 96.36 5.0155 96.36 10.2767 102.77 4.8884 97.77 Analyst: Stava Cowling OJ p. 125 STL Denver Quantify 6 anpl* Raport pro* Analysis 8 mpl List: C :\MassLynx\PFQA .PRO\SaiuplOB\pf35K29 (4) Last Modified: Wad Nov 30 07:39:38 2005 Hatbod: c:SNsssLynx\Pro*.PRO\MathOB\pa35K29b Last Modified: Had Nov 30 07:23:49 200S Job Coda: Printed: Wad Nov 30 07:45:13 2005 Pago 7 __________________ Nana: pf35k2978 Text: 10 pg/L 3: PFOA 13C2 10 pg/L 919.59.7 29-Nov-2005 10 pg/L 18:07:46 919.59.7 29-NOV-2005 10 |igIL 18:07:46 919.59.7 29-Nov-2005 10 ug/L 18:07:46 919.59.7 29-Nov-2005 18:07:46 pf35k2978 Sm (Mn. 2x2) F1 1.99 412.8 >218.7 1516 1.10e4 Area pf35k2978 Sm (Mn. 2x2) F1 1.99 412.8 >218.7 1516]) 1.10e4 Area pf35k2978 Sm (Mn, 2x2) F1 1.98 414.8 >369.7 10986 8.04e4 Area pf35k2978 Sm (Mn. 2x2) F1 2.63 498.6 >79.9 36511 2.23e4 Area 1 11111111111111[11| in 1111111111> 1.00 2.00 3.00 pf35k2978 Sm (Mn. 2x2) F1 1.98 412.8 >368.7 13442 9.76e4 Area "1 *i n i {i ii 1111 r p i n 11Pi 11 m i| i m 1.00 2.00 3.00 pf35k2978 Sm (Mn. 2x2) F1 1.98 412.8 >368.7 13442 9.76e4 Area m1111 n 111' ifi ij1 1 1 1 1 1 Mi Time 1.00 2.00 3.00 i- Tim e11 r i-; 1 1 1 n 1 1 1 1 ................ ' n n " 1 1 "i't 'i t t 1.00 2.00 3.00 0 111111111>111<>|rT|'i 11 Time 1.00 2.00 3.00 Time 1.00 2.00 3.00 1 Name PPOA 2 APPO 3 PPOA 13C2 4 pros 10 919.59.7 919-59.7 919.59.7 919.59.7 Baivi Text 10 ug/L 10 ug/L 10 ug/L 10 ug/L RT 1.981 1.981 1 981 2.631 Area Piago 13442 bb 13442 bb 10986 bb 3651 bb ug/L or k f f { ) U i o Nod. Canont 10.1738 101.74 10.5915 101.73 9.7138 97.14 10.1922 10192 Analyst: Stave Cowling p. 126 STL Denver Quantify Saxpla Raport pro* Analysis 8 atipia List: C:\MaasLynx\PFOA.FRO\SaicplaDB\pi35k29 (4) Last nodifiad: Mad No t 30 07:39:38 2005 Matbod: C: \Nna*Lynx\PFQA.PRO\MathDB\pa35k29b Last nodifiad: Nad No t 30 07:23:49 2005 Job Coda: Printad: Nad Nor 30 07:45:13 2005 Pag* 8 ___ ____________ Nana; pf35k2979 Taxt: 20 ug/L 3: PFOA 13C2 20 pg/L 29-Nov-2005 20 yg/L 29-Nov-2005 20 pg/L 29-Nov-2005 20 pg/L 29-Nov-2005 919.59.8 18:12:13 919.59.8 18:12:13 919.59.8 18:12:13 919.59.8 18:12:13 pf35k2979 Sm (Mn. 2x2) F1 pf35k2979 Sm (Mn, 2x2) F1 pf35k2979 Sm (Mn, 2x2) 1.99 412.8 >218.7 1.99 412.8 >218.7 1.98 2939]! 2.20e4 2939]\ 2.20e4 11013" Area Area F1 pf35k2979 Sm (Mn, 2x2)F1 2.65 498.6 > 79.9 8.18e4 71331 4.45e4 Area Area 0 lrT""ll'l|" " TTT|l|" H TT*TrTT 1.00 2.00 3.00 pf35k2979 Sm (Mn. 2x2) F1 1.99 412.8 >368.7 26441]! 1.94e5 Area 0 ihi [ iii [ in 111n i | ifTqTTTvprrr 1.00 2.00 3.00 pf35k2979 Sm (Mn, 2x2) F1 1.99 412.8 >368.7 26441]) 1.94e5 Area 0 i i n |Tn1 1 1 1 1 1 11 n-r<|iSi 1 1 1 1 1 n11 it- Time 1.00 2.00 3.00 ' ^i if" ' ii Time1 1 1 1 11 11 11 11 1 1 1 11 1 1 1 1 1.00 2.00 3.00 - *rr11ri 11ii iii i 111n Imnri 11 ni" r Time 1.00 2.00 3.00 a? - 0 M M m i*p Time1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 11111 1 11 1.00 2.00 3.00 Nana 1 PFOA 2 APPO 3 PFOA 13C2 4 PFOS ZD 919.S9.8 919.59.8 919.59.8 919.59.8 Baxpla Taxt 20 ug/L 20 ug/L 20 pg/L 20 ug/L RT 1.99S 1.995 1.961 2.646 Araa Flags 26441 bb 26441 bb 11013 bb 7133 bb U9/D or kg() kftac 20.0894 100.45 20.9144 100.45 9.7375 97.38 19.9311 99.66 Analyst: Stava Cowling LT1 p. 127 STL D enver Quantify Sasv>le Report PFOA Analysis Saaple List: C :\MassLynx\PFOA.PRO\SaaplDB\pf35k29(4) Last Modified: Wed Nov 30 07:39:38 300S Method: C:\MassLynx\FFOA.PRO\MethDB\pa35k39b Last Modified: Wad Nov 30 07:33:49 3005 Job Coda: Printed: Wed Nov 30 07:45:13 3005 Pag 9 __ ____________________________________ Nana: pf35K3980 Text : Blank 3: PFOA 13C2 PFOA Blank 29-Nov-2005 Blank 29-Nov-2005 Blank 29-Nov-2005 Blank 29-Nov-2005 919.59.1 18:16:42 919.59.1 18:16:42 919.59.1 18:16:42 919.59.1 18:16:42 pf35k2980 Sm (Mn, 2x2) F1 2.04 412.8 >218.7 26 7l 221 pf35k2980 Sm (Mn, 2x2) F1 2.04 412.8 >218.7 2 6 1\ 221 pf35k2980 Sm (Mn, 2x2) F1 1.98 414.8 >369.7 12760] 9.10e4 pf35k2980 Sm (Mn, 2x2) F1 0.01 498.6 > 79.9 101 Area Area Area 1.00 2.00 3.00 1.00 2.00 3.00 pf35k2980 Sm (Mn. 2x2) F1 pf35k2980 Sm (Mn. 2x2) F1 1.99 412.8 > 368.7 1.99 412.8 >368.7 1.31e3 1.31e3 Area Area Time Time 1.00 1.00 2.00 3.00 11 '11 ]Ii-ri]11 il Iin 11 1 1 1 1 Time 1.00 2.00 3.00 # Nana 1 PFOA 2 APPO 3 PFOA 1302 4 PFOS ID 919 59-1 919 59.1 919 59.1 919 59.1 Sanple Text Blank Blank Blank Blank RT 1.995 1.995 1.981 Area Flags 212 bb 212 bb 12760 bb U0 /L or kg<) H M c Mod.Coment 0.0102 0.0104 11.2821 112.82 3.41 11' " 1111" 11'"'V r- Time 1.00 2.00 3.00 Analyst: Steve Cowling er p. 128 STL D enver Quaneify 5ang>l Raport PFOA Analysis Sanpl List: C :\MaasLynx\PrOA.PRO\6ai>laDR\pf35k29 (4 ) Last modlflad: N4 Mov 30 07:39:38 2005 Mathod: C:\MassLynx\PFOA.PAO\MsthDB\pa35K29b Last wdifid: Wad Mov 30 07:33:49 3005 Job Coda: Printd: Wad Mov 30 07:45:13 3005 Pag 10 ___ _______________ __________________ Hans: pf3Sfc3981 Txt: 3 ug/L ZCV 3: PFOA 13C2 1: PFOA 2 |jg/L ICV 29-Nov-2005 2 (jg/L ICV 29-Nov-2005 2 Jjg/L ICV 29-NOV-2005 2 \ig lL ICV 29-NOV-2005 919.59.9 18:21:09 919.59.9 18:21:09 919.59.9 18:21:09 919.59.9 18:21:09 pf35k2981 Sm (Mn. 2x2) F1 1.98 412.8 >218.7 308H 2.22e3 Area pf35k2981 Sm (Mn. 2x2) F1 1.98 412.8 >218.7 308 2.22e3 Area pf35k2981 Sm (Mn, 2x2) F1 1.98 414.8 >369.7 11436] 8.16e4 Area pf35k2981 Sm (Mn, 2x2)F1 2.63 498.6 > 79.9 800 4.87e3 Area 3 > n i pm 1 1 1 1 1 1 1 1 n | ifi 1 1 11 i'i| 1 111 1.00 2.00 3.00 pf35k2981 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 2643 1.86e4 Area 3 11 1ri 111 m 11 rrrjri h 11 fi < 'T 1.00 2.00 3.00 pf35k2981 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 2643 1.86e4 Area r Time11 i11 11 riTT'i 11 ri|iH-i |n H |" n 1.00 2.00 3.00 TTTTJT 1IIIIIIIIIII Time 1.00 2.00 3.00 0 " " i*rr| n Time11 1 1 1 1 1 1 1 1 1 1 1 h 11 1 1 1 11 11 1.00 2.00 3.00 1 ^T-rr]1 1 1 1 1 1 u1 1 1 ii i [ 1 1 1 u i ''i1 1 Time 1.00 2.00 3.00 Mans 2l PPOA APFO 3 PFOA 13C2 4 pros XD 919.59.9 919.59.9 919.59.9 919.59.9 Taxt 3 pg/L ICV 2 pg/L ICV 2 uff/L ICV 2 ug/L ICV RT 1.981 1.981 1.981 2.631 Araa Flags 2643 bb 2643 bb 11436 bb 800 bb pg/L or kg() U c Mod.CoMsant 1.8160 90.80 1.8903 90.79 10.1119 101.12 2.1259 106.30 Analyst: 8tvc Cowlino -0 p. 129 STL Denver Quantify Semple Report PFOA Analysis Semple List: C :\MassLynx\PFOA.PRO\SampleDB\pf35k29(4) Last modified: Wed NOV 30 07:39:38 3005 Method: C: \MessLynx\PFOA.PRO\MethDB\ps35U9b Last modified: Med Nov 30 07:23:49 2005 Job Code: Printed; wed Nov 30 07:45:13 2005 Pag 11 _______________ ____ pf35k2982 Text: 0.2 pg/L 3: PFOA 13C2 0.2 pg/L 919.59.2 29-Nov-2005 0.2 pg/L 18:25:38 919.59.2 29-Nov-2005 0.2 pg/L 18:25:38 919.59.2 29-Nov-2005 0.2 pg/L 18:25:38 919.59.2 29-Nov-2005 18:25:38 pf35k2982 Sm (Mn, 2x2) F1 pf35k2982 Sm (Mn, 2x2) F1 pf35k2982 Sm (Mn, 2x2) 1.98 412.8 >218.7 1.98 412.8 >218.7 1.98 342 342 ] - 11359] Area Area F 1 pf35k2982 Sm (Mn, 2x2) F1 2.65 498.6 > 79.9 8.13e4 93 608 Area Area ^ i1! r i p i m 11 i i f p T'iiJ iT i >i<7r?fTTfr 1.00 2.00 3.00 1.00 2.00 pf35k2982 Sm (Mn, 2x2) F1 pf35k2982 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 1.98 412.8 >368.7 446 2.92e3 446 2.92e3 Area Area '>Ti|.nn ii^hiitti " " r. Time 1.00 2.00 3.00 4 ~|tvi r^yi*rrj. iM111 i;i | i>n"| 1 1 11pi in Time 1.00 2.00 3.00 L111 rp til 111111 n n ......... Time 1.00 2.00 3.00 10-fcMM | lYl 1| 1l11| M 11| 1lPTrrrr^ y Time 1.00 2.00 3.00 # Name 1 PFOA 2 PFO 3 PFOA 13C2 4 PFOS ID 919.59.2 919.59.2 919.59.2 919.59.2 Sample Text 0.2 pg/L 0.2 pg/L 0.2 pg/L 0.2 pg/L RT 1.981 1.981 1.981 2.646 Aree Flags 446 bb 446 bb 11359 bb 93 bb pg/L or kg() KRec 0.2006 100.30 0.2086 100.27 10.0436 100.44 0.2295 114.74 Analyst: Steve Cowling 00 p. 130 STL D enver Quantify Saxple Report PFOA Analysis Modified:SSMple List: C: \HassLyiiK\PFOA.PRO\SaplD\pf35k29(4) Last Med Nov 30 07:39:36 300S Method: C:\MassLynx\PFOA.FRO\MethD8\pa35k29b Last modified: Wed Nov 30 07:33:49 2005 Job Code: Printed: Wed Nov 30 07:45:13 3005 Pag 19 Hama: pf35k2990 Text: Blank 3: PFOA 13C2 Blank 29-Nov-2005 Blank 29-Nov-2005 Blank 29-Nov-2005 Blank 29-Nov-2005 919.59.1 19:01:20 919.59.1 19:01:20 919.59.1 19:01:20 919.59.1 19:01:20 pf35k2990 Sm (Mn. 2x2) F1 1.99 412.8 >218.7 pf35k2990 Sm (Mn. 2x2) F 1 pf35k2990 Sm (Mn, 2x2) F1 1.99 412.8 >218.7 1.98 414.8 >369.7 pf35k2990 Sm (Mn, 2x2) F1 1.22 2 59 498.6 >79.9 28 1\ 208 28 ]\ 208 12831 9.10e4 ` '" 70.4 Area 25 " " i" " I" riffVTTjrnTpv; | Area 25 'l l l l l | i r i l | I M i p i l l T I I I I | H M | I I T1- Area /2.89 1.00 2.00 3.00 1.00 2.00 3.00 pf35k2990 Sm (Mn, 2x2) F1 pf35k2990 Sm (Mn, 2x2) F1 2.01 412.8 >368.7 2.01 412.8 >368.7 196]\ 1.21e3 196l\ 1.21e3 Area Area 8 i lrvii/pTrrrrr<^fTir^li^rwrfT'-m- Time 1.00 2.00 3.00 8 -*iti i/7^iVrTTri`ffr>fi| |i>ririTrfT-'rrr' Time 1.00 2.00 3.00 IIII'l II I1III1I1I1I1IrIiM11ImiVt |IMIIMI1|In111I1I Time 1.0 2.00 3.00 73 t ttt 1 fi Irym i |th i |iiii|iiiip~ni TIT16 1.00 2.00 3.00 Name 1 PFOA 2 APPO 3 PFOA 13C2 4 PPOS ZD 919 .59.1 919 59.1 919 59.1 919 59.1 Sanple Text Blank Blank Blank Blank RT 2.009 2.009 1.981 Area Flags 196 bb 196 bb 12631 bb tig / L or0o..0ok0oo0o()0o knee Nod. Consent 11.3449 113.45 Analyst : Steve Cowling p. 131 STL Denver Quantify Sanpla Raport PFOA Analysis Sanctis List: C :\NassLynx\PPOA.PRO\SamplsDB\pf3Sk29 <4) Last modified: Wad Mov 30 07:39:3 2005 Matbod: C:\MaasLynx\PFOA.PRO\HethDB\pa35k29b Last modified: Mad No t 30 07:23:49 2005 Job Coda: Printed: Mad Nov 30 07:45:13 2005 Pags 20 ______________________ Mans ; pf35k2991 Text: 0.2 pg/L 3: PPOA 13C2 4: PFOS 0.2 pg/L 29-Nov-2005 0.2 pg/L 29-Nov-2005 0.2 pg/L 29-Nov-2005 0.2 \ig lL 29-Nov-2005 919.59.2 19:05:47 919.59.2 19:05:47 919.59.2 19:05:47 919.59.2 19:05:47 pf35k2991 Sm (Mn. 2x2) F1 1.99 412.8 >218.7 383 Area pf35k2991 Sm (Mn, 2x2) F1 412.8 >218.7 383 Area pf35k2991 Sm (Mn, 2x2) F1 1.98 414.8 >369.7 11401] 8.09e4 Area pf35k2991 Sm (Mn, 2x2) F1 2.62 498.6 > 79.9 82 572 Area Ji Tl IIII.IIIIT| II.Ip-TTt 1.00 2.00 3.00 pf35k2991 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 428 2.83e3 Area 1.00 2.00 3.00 pf35k2991 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 428 2.83e3 Area 3 ^ rirfprirrf-rrr ri" r * ri iTiT|firr | ime 1 . 0 0 2.00 3.00 iirpiiw11 rr r;m ijTTrr | H T 1& 1 . 0 0 2.00 3.00 13C2 PFOS ZD 919.59.2 919.592 919.59.2 919-59.2 Sanale Text 0 . 2 pg/L 0.2 pg/L 0 . 2 ufl/L 0 . 2 ug/L RT 1.981 1.981 1.981 2.617 Area Flags 428 bb 428 bb 11401 bb 82 bb pg/L or kg() XRac 0.1864 93.20 0.1938 93.16 10.0805 100.81 0 . 2 0 0 0 99.96 -rTTT 11' r*i j 1 1 11 [I 111 1 1 11111' Time 1.00 2.00 3.00 Time J Analyst: Stava Cowling LH O p. 132 STL D enver Quantify Semple Report PPOA Analyaia Sample Liat: C: \MassLynx\prOA.PRO\8anpleDB\pf35k29(4) Laat modified: Wad Nov 30 07:39:36 2005 Mathod: C:\HaaaLyxix\prOA.FRO\MethDB\pa35k29b Laat Modified: wed Mot 30 07:23:49 2005 Job Code: Printed: Nod Nov 30 07:45:13 2005 Mama: pf3Sk2992 Text: 0.5 p/L 0.5 |jg/L 29-Nov-2005 0.5 pg/L 919.59.3 19:10:15 919.59.3 pf35k2992 Sm (Mn, 2x2) F1 pf35k2992 Sm (Mn. 1.98 412.8 >218.7 1.98 77 71 566 3 77 Area 3: PFOA 13C2 29-Nov-2005 0.5 |jg/L 29-NOV-2005 0.5 Iig/L 29-NOV-2005 19:10:15 919.59.3 19:10:15 919.59.3 19:10:15 2x2)F1pf35k2992 Sm (Mn, 2x2) F1 pf35k2992 Sm (Mn, 2x2) F1 412.8 >218.7 1.98 414.8 >369.7 2.65 498.6 > 79.9 566 11436" 8.15e4 172 1.08e3 Area Area Area i-frrrTT ?r?ij'iin* 1.00 2.00 3.00 pf35k2992 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 697 ]) 4.78e3 Area :iv7w>Myr>iri 11 i m T , M M I m 11n f i 1.00 2.00 3.00 pf35k2992 Sm (Mn, 2x2) F1 1.98 412.8 > 368.7 6971) 4.78e3 Area 3?- rTl" ITT' Time 1.00 2.00 3.00 1*1*111ipn 1111i*i11fTTyni i^i i i Time 1.00 2.00 3.00 m t p i M 11 h 11 u n . .......... ... Time 1.00 2.00 3.00 4 TimeV fi l|TTTT|n'Pl|(Ti frn~r^TTTTj~rF 1.00 2.00 3.00 1 PFOA 2 APPO 3 PFOA 13C2 4 PFOS ID 919.59.3 919.59.3 919.59.3 919.59.3 Sample Text 0.5 pg/L 0.5 pg/L 0.5 P0/L 0.5 pg/L RT 1 981 1.981 1.981 2.646 Area Flags 697 bb 697 bb 11436 bb 172 bb pg/L or kg() %Rec 0.3831 76 63 0 3986 76.65 10.1118 1 0 1 - 1 2 0.4407 88.13 Analyst: Steve Cowling ui H* p. 13 3 STL D enver Quantify Sample Report PFOA Analysis Sanple List: C :\MassLynx\PFQA. PRO\8anpleOB\pf35k29 (4) Last modified: Wed No t 30 07:39:38 3003 Method: C:\MassLynx\PPOA.PRO\MathDB\pa35k29b Last modified: Wed Nor 30 07:33:49 3005 Job Code: Printed: Wed No t 30 07:45:13 3005 Name: pf35k2993 Text: 1 ug/L 3: PFOA 13C2 1 |ig/L 29-Nov-2005 1 pg/L 29-Nov-2005 1 pg/L 29-Nov-2005 1 pg/L 29-Nov-2005 919.59.4 19:14:44 919.59.4 19:14:44 919.59.4 19:14:44 919.59.4 19:14:44 pf35k2993 Sm (Mn, 2x2) F1 pf35k2993 Sm (Mn, 2x2) F1 pf35k2993 Sm (Mn, 2x2) F1 pf35k2993 Sm (Mn, 2x2) F1 1.98 412.8 >218.7 1.98 412.8 >218.7 1.98 414.8 >369.7 2.63 498.6 > 79.9 174 1.31e3 174! 1.31e3 114601 377 2.30e3 Area Area Area Area 4 ' m ip ^ i'i 1 1 i t i 1 1 1 1 **i i p r i 1 1 1.00 2.00 3.00 pf35k2993 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 1493 1.05e4 Area 4 ~Nt i rpTi1 11 I*i*i|iTrt'irti Ipn i|T 1.00 2.00 3.00 pf35k2993 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 1493l\ 1.05e4 Area i ij i i n 11 ri ' i n r i | rf r i j ri r Time 1.00 2.00 3.00 1 ~tn rrp 1 !1 1 1111 !11 IiVi Time1 1 1 1 1 1 1 1 111 1.00 2.00 3.00 Time 1.00 2.00 3.00 i r p l T l T p ITT n r? |viri I'M Time 1.00 2.00 3.00 tf Mone 1 PFOA 2 APFO 3 PFOA 13C2 4 PFOS ZD 919.59.4 919.59.4 919.59.4 919.59.4 Sample Text 1 ug/L 1 ug/L 1 ug/L l ug/L RT 1.981 1.981 1.981 2.631 Area Flags 1493 bb 1493 bb 11460 bb 377 bb pg/L or kg() %Reo Mod. Consent 0.9674 96.74 1.0069 96.73 10.1330 101.33 0.9892 98.92 Analyst: SteTe Cowling U1 to p. 134 STL Denver Quantify Sampla Raport PTOA Analysis fianpla List: C :\MassLynx\prOA. PRO\ 8amplaDB\p 35*29 (4) Last wxUeisa: Wad Hov 30 07:39:38 2005 Mstbod: C :\KassLynx\prOA.PRO\MnthDB\pa35R29b Last modlfiad: Had Mov 30 07:23:49 2005 Job Coda: Printad: Wad Nov 30 07;4S:13 2005 Nana: pf35k2994 Taxt: 2 yg/L t Mama 1 PPOA 2 APFO 3 PFOA 13C2 4 PPOS ZD 919.59.5 919.59.5 919.59.5 919.59.5 Sarnpla Taxt 2 yg/L 2 yg/L 2 yg/L 2 yg/L RT 1.961 1.961 1.981 2.631 Araa Flags 2756 bb 2758 bb 11554 bb 796 bb yg/L or kg() kRac 1.8803 94.02 1.9573 9 4 0 1 10.2158 102.16 2.0932 104.66 Analyst: 6tava Cowling cUnJ p. 135 STL D enver Quantify Saxqpla Report proa Analysis Sanpla List : C: \M*ssLyn>\PrOA.PRO\San]plDB\pf35X29(4> Last modified: Wad Nov 30 07:39:36 2005 Mathod: C:\MaasLynx\PFOA.PRO\MathDB\pa3Sk29b Last modified: Nad Nov 30 07:23:49 2005 Job Coda: Printad: Wad Nov 30 07:45:13 2005 Pag 24 ___________________ Nana: p35k2995 Text: 5 pg/L 5 pg/L 29-Nov-2005 5 pg/L 5 pg/L 29-Nov>2005 29-Nov-2005 919.59.6 19:23:39 919.59.6 19:23:39 919.59.6 19:23:39 19:23:39 pf35k2995 Sm (Mn, 2x2) 1.98 412.8 763 F1 pf35k2995 Sm (Mn, 2x2) F1 >218.7 1.98 412.8 >218.7 5.58e3 7 6 3 5. 58e3 Area ? H ll Area pf35k2995 Sm (Mn, 2x2) F1 1.98 414.8 > 369.7 11592 8.33e4 Area pf35k2995 Sm (Mn, 2x2) F1 2.63 498.6 >79.9 1940l 1.17e4 Area *| ~*i iirpri 1 1 1 n 1 1 1 h i'i |ih i`n ri Ip r>t 1 111!" I" 111n*M 11*r'li 1.00 2.00 3.00 1.00 2.00 3.00 pf35k2995 Sm (Mn, 2x2) F1 pf35k2995 Sm (Mn, 2x2) F1 1.98 412.8 >368.7 1.98 412.8 >368.7 6792 4.89e4 6792 4.89e4 Area Area 11" " i1" 11" 111 1111Min-ri Time 1.00 2.00 3.00 111 [1 11 i-i II111 iviiVnI11 11111 Time 1.00 2.00 3.00 soP'* _ U 1.00 2.00 3.00 11I nr q^-TnT n11[111r-1fTi 1[ 1i n i111r1i i i] l ! <Ii l Time 1.00 2.00 3.00 ft Nana 1 PFOA 2 APPO 3 PFOA 13C2 4 PFOS ZD 919.59.6 919.59.6 919.59.6 919.59.6 Sanpla 5 ug/L 5 ug/L 5 ug/L 5 ug/L RT 1.961 1.981 1.981 2.631 Araa Flags 6792 bb 6792 bb 11592 bb 1940 bb pg/L or kg() Hltac 4.8044 96.09 5.0016 96 09 10.2492 102 49 5.1159 102.32 Analyst: Stava Cowling U1 p. 136 STL U fl) Quantify sanple Report J-J PPOA Analysis ^ sn*)le L is t: C: \MassLynx\PFOA.PRG\Sai^leDB\pf 35k29 (4) W Last Modified: Wed Wov 30 07:39:36 2005 h Matbod: C:\MassLyax\FroA.FRO\MethDB\pa3Sk29b Last nodifiad: Wad Mo t 30 07:23:49 2005 Job Coda: Printed: Wad Nov 30 07:45:13 2005 Paga 25 Nana: pf35k2996 Text: 10 pg/L 3 : PFOA 13C2 10 iig/L 29-Nov-2005 10 pg/L 29-Nov-2005 10 pg/L 29-Nov-2005 10 pg/L 29-Nov-2005 919.59.7 19:28:08 919.59.7 19:28:08 919.59.7 pf35k2996 Sm (Mn, 2x2) F1 pf35k2996 Sm (Mn, 2x2) F1 pf35k2996 Sm (Mn, 2x2) 1.99 412.8 >218.7 1.99 412.8 >218.7 1.98 1516 1.10e4 1516/ 1.10e4 11060 Area Area 19:28:08 919.59.7 19:28:08 F1 pf35k2996 Sm (Mn, 2x2) F1 2.65 498.6 > 79.9 37261 2.27e4 Area Area 0 `|Il 11' 111111II I'IHIiMI|1111111n 0 'h11n111111nnin 11 1.00 2.00 3.00 1.00 2.00 3.00 pf35k2996 Sm (Mn, 2x2) F 1 pf35k2996 Sm (Mn, 2x2) F1 1.99 412.8 >368.7 1.99 412.8 >368.7 13290 9.63e4 13290 9.63e4 Area Area |'fm ^ - Time11 1111 i i tu1 1 1 1 1 1 1 1 1 1 1 1 1 1.00 2.00 3.00 ~ | Timep it i itit1 1 1 1 1 1 1 1 1 1 1 1 1 111 11111 1.00 2.00 3.00 11m1111111111 Time 1.00 2.00 3.00 " " i i,Mi,i" ii"r,irirT(m V " 1 Time 1.00 2.00 3.00 * Mans 1 PPOA 2 APPO 3 PPOA 13C2 4 PPOS ID 919.59.7 919.59.7 919.59.7 919.59.7 Sanc* Text 10 pg/L 10 pg/L 10 pg/L 10 pg/L AT 1.995 1.995 1.981 2.646 Arsa Flags 13290 bb 13290 bb 11060 bb 3726 bb pg/L or kg() KRec Mod. Consent 9.9892 99 89 103993 99.89 9.7794 97.79 10.3326 103.33 Analyst: Stava Cowling uUil p. 137 STL D enver Quantity Sanple Report PFOA Analysis Single List: C: \MassLynx\PraA.PRO\8aj*>leDB\pf35k29<4) Last Modified: Wed Nov 30 07:39:38 2005 Method: C :\MassLynx\FPOA.PRO\MethDB\pe3Sfc29b Last modified: Wed Nov 30 07:23:49 2005 Job Code: Printed: Wed Nov 30 07:45:13 2005 Page 26 __________ __________________ Name: pf35k2997 Text: 20 U0/1* 2: APPO 20 iig/L 29-Nov-2005 20 iig/L 919.59.8 19:32:35 919.59.8 pf35k2997 Sm (Mn, 2x2) F1 pf35k2997 Sm (Mn. 1.99 412.8 >218.7 1.99 2966]) 2.24e4 2966]) Area s? A l 3: PFOA 13C2 4: PFOS 29-Nov-2005 20 gg/L 29-Nov-2005 20 pg/L 29-Nov-2005 19:32:35 919.59.8 19:32:35 919.59.8 19:32:35 2x2)F1pf35k2997 Sm (Mn, 2x2) F1 412.8 >218.7 1.99 414.8 > 369.7 2.24e4 109691 7.99e4 pf35k2997 Sm (Mn, 2x2)F1 2.65 498.6 >79.9 7336] 4.47e4 Area Area Area 0 V rrrp n 1111 u |n it{Fii)11 n {iirr 1.00 2.00 3.00 pf35k2997 Sm (Mn. 2x2) F1 1.99 412.8 >368.7 26699]) 1.96e5 Area 0 1 1 1 1 1 1 i 1 1 1 1 1 1 1 u i< 11 Fri 1 1 t i t [ 1.00 2.00 3.00 pf35k2997 Sm (Mn, 2x2) F1 1.99 412.8 >368.7 26699]) 1 ,96e5 Area '1 1 1 11 1 1 1 1 1 1 1 1h i i ' i ' 1 1 '''' Time 1.00 2.00 3.00 Time 1.00 2.00 3.00 111ili il i 1111 L Time!iTT|irrr|ittt 1.00 2.00 3.00 ' 111" 1r 11 11111,i/ii\fn ri Time 1.00 2.00 3.00 # Name 1 PFOA 2 APFO 3 PFOA 13C2 4 PFOS ZD 919.59 8 919.59.8 919.59.8 919.59.8 Sample Text 20 pg/L 20 pg/L 20 pg/L 20 pg/L RT 1.995 1.995 1.995 2.646 Area Flags 26699 bb 26699 bb 10969 bb 7336 bb pg/L or ko<) 20.3685 21.2050 9.6965 20.5823 Analyst: Steve Cowling LT1 CTi STL Denver Quantify Calibration Raport pro* Analysis Calibration: C: \MaaaL.ynx\Pro*. PRO\CurvDB\pa35k29a Last isodiflad: Wad Nov 30 07:47:0 2003 Prlntad: Wad Nov 30 07:47:14 2005 Analyst: Stava Cowling LD P*g 1 X p. 138 i < i . I '"'I r - p - r . J . . T - r - | 10.0 12.0 j ' 14.0 i ' ' ' 1i 1' 1' i 1 ' i 1' 11i Cone 16.0 18.0 20.0 STL D enver Quantity calibration Report PFOA Analysis Calibration: C:\MassLynx\PFOA.PRO\CurvaDB\pa35k29 Last iKMlitisd: Wd Nor 30 07:47:0 3005 Printed: Wad No t 30 07:47:14 2005 Analyst: Stavs Cowling LT1 00 Pag 2 i ' ' i ' 1' ' i 1' a 1111i 1111i 1111i 1' ' 1Cone 12.0 14.0 16.0 18.0 20.0 p. 139 p. 140 m -3 f a (D Quantify Calibration Haport p prOA JLnalyaia Calibration: C:\MaaiLynx\PFOA.PRO\CurvaDBVpa35k28 ID U s t nodiflad: Nad Nov 30 07:47:0 2005 h Printad: Nad Nov 30 07:47:14 2005 Compound 3 name: PFOA 13C2 Method File: pa35k29 Response Factor: 1135.31 R R F SD: 24.1972, % Relative SD: 2.13132 Response type: External Std, Area Curve type: RF 1.10e41.00e4-i 9.00e3-i 8.00e3-i 7.00e3 _Respo6n.s0e0e3-i 5.00e3^ Psgs 3 X Analyst: Stsv* Cowling i_n vd ' I ' ''-1 ' I 1' ' ' 1' 1''"1 ' 1' ' 1' ` 111 4.0 5.0 6.0 7.0 8.0 9.0 10.0 p. 141 cn *tr-3* Q cn o Pag 4 p. 142 LC/MS SEMIVOLATILE SAMPLE DATA STL Denver 61 STL Denver Quantify Caopouad Sunnary flport FPOA Analysis Sanpla List: C :\MaaaLynx\PF0A.PRO\SanplaDB\pf35K29(4) Last modified; Wd Nov 30 07:39:38 300S Metbod: C :\MassLynx\FPOA. PRO\MatbfiB\pa35K39b Last modified: Nad Nov 30 07:33:49 3005 Job Cod: Printed: Nod Nov 30 07:45:10 3005 Ccmpouad 1: PFOA Banpla List: pf35k29<4) Nathod P11: pa35k39b Cofficint of Dotamination: 0.999017 Calibration curva: 1.18743 x 0.154368 Raspons typ: Intimai 8 td ( Rat 3 ), Arsa ( 18 Cone. / 18 Ara ) Curvo typ: Linear, Origin: Exclude Nlghtisgi 1/x, Axis trans: Won # Hans 1 pf35R2972 2 pf35k2973 3 pf 35k2974 4 pf35k2975 S pf3Sk2976 6 pf35k2977 7 pf35k2978 8 pf35k2979 9 pf35k2980 10 pf35k2961 11 pf35k2982 12 pf3Sk2983 13 pf 3Sk2984 14 pf35k2985 iS pf35k2966 16 pf35k2987 17 pf 35k2988 18 pf35k2989 19 pf35k2990 20 pf3Sk2991 21 p35k2992 22 pf35k2993 23 pf35k2994 24 pf35k2995 25 pf35k2996 26 pf35k2997 ID 91959.1 919.59.2 919.59.3 919.59.4 919.S9.5 919.59.6 919.59.7 919.59.8 919.59.1 919.59.9 919.59.2 HQXPR1AA HQXPR1AC HQXPR1AD HQW311AA HQW321AA HQW341AA HQW351A 919.59.1 919.59.2 919.59.3 919.S9.4 919.59.5 919.59.6 919.597 919.59.8 Bangi Tene Blank 0.2 pg/L 0.5 pg/L 1 pg/L 2 pg/L 5 pg/L 10 pg/L 20 pg/L Blank 2 pg/L ICV 0.2 pg/L R5K250000-125 MB R5K250000-125 LCS R5K250000-125 LOS D5K230384-1 D5K230384-2 D5K230384-3 O5K230384-4 Blank 0.2 pg/L 0.5 pg/L 1 pg/L 2 pg/L 5 pg/L 10 pg/L 20 pg/L Typ Std Cone Blank Standard 0.20 Standard 0.50 Standard 1.00 Standard 2.00 Standard 5.00 Standard 1 0 . 0 0 Standard 2 0 . 0 0 Blank QC 2 . 0 0 QC 0 . 2 0 Blank QC 0 . 2 0 QC 0 . 0 2 Analyte Analyte Analyte Analyte Blank Standard 0.20 Standard 0.50 Standard 1.00 Standard 2.00 Standard 5.00 Standard 1 0 . 0 0 Standard 2 0 . 0 0 RT 2.01 2.00 1.98 1.98 1.98 1.98 1.98 2.00 2.00 1.98 1.98 2.07 1.94 1.94 1.81 2.01 2.05 2.01 2.01 1.98 1.98 1.98 1.98 1.98 2.00 2.00 A r u Plaga Ion Ratio 256 bb 7.966 492 bb 8.702 742 bb 9.416 1574 bb 8.854 2800 bb 8.434 6829 bb 8.923 13442 bb 8.869 26441 bb 8.995 2 1 2 bb 8.069 2643 bb 8.591 446 bb 10.475 185 bb 11884 bb 9.042 1215 bb 8.360 706 bb 7.284 151 bb 155 bb 442 bb 8.657 196 bb 7.019 428 bb 9.343 697 bb 9.062 1493 bb 8.589 2758 bb 8.463 6792 bb 8.902 13290 bb 8.765 26699 bb 9.000 Analyst : Stavo Cowling Pag 1 Raspona Cono pg/L or kg() XRac Extract al 6 ant>l* ML or g Dilution CalPile 3 0.202 0.0401 1.000 1.00 1 . 0 0 0 pa3Sk29d 3 0.433 0.2348 117.42 1.000 1.00 1 . 0 0 0 pa3Sk29d 3 0.653 0.4204 84.08 1.000 1.00 1 . 0 0 0 pa35k29d 3 1.384 1.0354 103.54 1.000 1.00 1 . 0 0 0 pa35k29d 3 2.444 1.9283 96.41 1.000 1.00 1 . 0 0 0 p35k29d 3 5.875 4.8178 96.36 1.000 1.00 1 . 0 0 0 p3Sk29d 3 12.235 10.1738 101.74 1.000 1.00 1 . 0 0 0 pa3Sk29d 3 24.009 20.0894 100.45 1.000 1.00 1 . 0 0 0 pa35k29d 3 0.166 0.0102 1.000 1.00 1 . 0 0 0 pa35k29d 3 2.311 1.8160 90.80 1.000 1.00 1 . 0 0 0 pa35k29d 3 0.392 0.2006 100.30 1.000 1.00 1 . 0 0 0 pa35k29d 3 0 204 0.0008 5.000 250.00 1 . 0 0 0 pa35k29d 3 12.185 0.2026 101.31 5.000 250.00 1 . 0 0 0 pa35k29d 3 1.364 0.0204 101.85 5.000 250.00 1 . 0 0 0 pa35k29d 3 0.770 0.0105 5.000 251.00 1 . 0 0 0 pa35k29d 3 0.176 0.0004 5.000 250.00 1 . 0 0 0 pa35k29d 3 0.172 0.0003 S.000 25100 1 . 0 0 0 pa3Sk29d 3 0.438 0.0051 5.000 233.00 1 . 0 0 0 pa35k29d 3 0 .1 S2 0.0000 1.000 1.00 1 . 0 0 0 pa35k29d 3 0.376 0.1864 93.20 1.000 1.00 1 . 0 0 0 pa3Sk29d 3 0.609 0.3831 76.63 1 .M 1.00 1 . 0 0 0 pa35k29d 3 1.303 0.9674 96.74 1.000 1.00 1 . 0 0 0 pa35k29d 3 2.387 1.6803 94.02 1.000 1.00 1 . 0 0 0 pa35k29d 3 5.859 4.8044 96.09 1.000 1.00 1 . 0 0 0 pa35k29d 3 12.016 9.9892 99.89 1.000 1.00 1 . 0 0 0 pa35k29d 3 24.340 20.3685 101.84 1.000 1.00 1 . 0 0 0 pa3Sk29d STL Denver Quantify Comouod Sunnary Report PPQA Analysis Sanple List: C :\MaasLynx\PPOA. PRO\8 a^>leOB\pf 35k29 (4) Last modified: Wed Nov 30 07:39:38 3005 Method: C: \MaaaLynx\PrGA.PRO\NethDB\pa35k29b Last modified: Wad Nov 30 07:23:49 2005 Job Cods: Printed: Wad N o t 30 07:45:10 2005 Compound 2: APPO Sample List: pf35k29(4) Natbod Pila: pa35k29b Coafficiant of Datarmination: 0.999020 Calibration curva: 1.14057 * x 0.154584 Response typa: Intanai Std ( Ref 3 ), Araa * ( IS Cone . / i s Arsa ) Curva typa: Linear, Origin: Exclude, Waigbting: 1/x, Axis trans: Nona Hi m 1 pf35k2972 2 pf351(2973 3 pf35k2974 4 pf35k2975 S pf35k2976 6 p35k2977 7 pf35k2978 8 pf35k2979 9 pf35k2980 10 pf35k2981 11 pf 35k2982 12 pf 35k2983 13 pf35k29B4 14 pf35k2985 15 pf35k2986 16 pf35k2987 17 pf35k2988 18 pf 35k2989 19 pf35k2990 20 pf35k2991 21 pf35k2992 22 pf35k2993 23 pf35k2994 24 pf35k2995 25 pf35k2996 26 pf35k2997 ID 919.59.1 919.59.2 919.59.3 919.59.4 919.59.5 919.59.6 919.59.7 919.59.8 919.59.1 919-59.9 919.59.2 KQXPR1AA HQXPR1AC HQXPR1AD HQW311AA HQW321AA HQW341AA HQW351AA 919.59.1 919.59.2 919.59.3 919.59.4 919.59.5 919.59.6 919.59.7 919.59.8 Sample Text Blank 0.2 pg/L 0.5 pg/L 1 pg/L 2 pg/L 5 pg/L 10 pg/L 20 pg/L Blank 2 pg/L ICV 0.2 pg/L RSK250000-125 MB RSK250000-125 LCS RSK250000-125 LCS D5K230384-1 D5K230384-2 05X230384*3 O5K230384-4 Blank 0.2 pg/L 0.5 pg/L 1 pg/L 2 pg/L 5 pg/L 10 pg/L 20 pg/L Typa Blank 8 td Cone Standard 0.21 Standard 0.52 Standard 1.04 Standard 2.08 Standard 5.21 Standard 10.41 Standard 20.82 Blank QC 2.08 QC 0 . 2 1 Blank QC 0 . 2 1 QC 0 . 0 2 Analyte Analyte Analyte Analyte Blank Standard 021 Standard 0.52 Standard 1.04 Standard 2.08 Standard 5.21 Standard 10.41 Standard 20.82 RT 2.01 2.00 1.98 1.98 1.98 1.98 1.98 2.00 2.00 1.98 1.96 2.07 1.94 1.94 1.81 2.01 205 2.01 2.01 1.98 1.98 1.98 1.98 1.98 2.00 2.00 Aram Plaga Ion Ratio 256 bb 7.966 492 bb 8.702 742 bb 9.416 1574 bb 8.654 2800 bb 8.434 6829 bb 8.923 13442 bb 6.869 26441 bb 8.995 2 1 2 bb 8.069 2643 bb 8.591 446 bb 10.475 185 bb 11884 bb 9.042 1215 bb 8.360 706 bb 7.284 151 bb 155 bb 442 bb 8.657 196 bb 7.019 428 bb 9.343 697 bb 9.062 1493 bb 8.589 2758 bb 8.463 6792 bb 8.902 13290 bb 8.765 26699 bb 9.000 Analyst: 8tava Cowling CT\ GJ Pag 2 I i r u ZS 12656 3 11361 3 11351 3 11377 3 11458 3 11623 3 10986 3 11013 3 12760 3 11436 3 11359 3 9089 3 9753 3 8911 3 9075 3 8581 3 9016 3 10078 3 12831 3 11401 3 11436 3 11460 3 11554 3 11592 3 11060 3 10969 3 Raaponaa 0.202 0.433 0.653 1.384 2.444 5.875 12.235 24.009 0.166 2.311 0.392 0.204 12.185 1.364 0-778 0.176 0.172 0.438 0.152 0.376 0 609 1.303 2.387 5.859 12.016 24.340 Conc ug/L or Kg() SStmc 0.0415 0.2442 117.41 0.4374 84.11 1.0777 103.52 2.0072 96.41 5.0155 96.36 10.5915 101.73 20.9144 100.45 0.0104 1.8903 90 79 0.2086 100.27 0.0009 0.2109 101.42 0 . 0 2 1 2 101.93 0.0109 0.0004 0 .0 0 0 3 0.0053 0.0000 0.1936 93.16 0.3986 76.65 1.0069 96.73 1.9573 94.01 5.0016 96.09 10.3993 99.89 21.2050 101.84 extract aL 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 5.000 5.000 5.000 5.000 5.000 5.000 5.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 Sanpl ni or g Dilution Caini 1.00 1 . 0 0 0 pa3Sk29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 p35k29d 1.00 1 . 0 0 0 p35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 p3Sk29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 p35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 250.00 1 . 0 0 0 pa3Sk29d 2 S0 . 0 0 1 . 0 0 0 pa35k29d 250.00 1 . 0 0 0 pa35k29d 251.00 1 . 0 0 0 p35k29d 250.00 1 . 0 0 0 pa35k29d 251.00 1 . 0 0 0 pa35k29d 233.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1 . 0 0 0 pa35k29d p. 144 Quantify Compound Sunnary Report pros Analysis Sanpls List: C: \MassLynx\pFOA.PRO\SanplaDB\pf351c29(4) Last nodifiad : Mad Nov 30 07:39:38 2005 Method: C :\MassLynx\PFOA.PRO\MathOB\pa35k29b Last nodifisd : Mad Nov 30 07:23:49 2005 Job Coda: Printed: Mad Nov 30 07:45:10 2005 Conpound 3: PFQA L3C2 Sanpls List: pf3Sk29(4) Response Factor: 1130.99 RAP SO: 23.1531# H Relativa 6 D: 2.04717 Response type: external 8 td, Area Curve typa: RF Mathod Pila: pa35k29b Nans 1 pf35k2972 2 pf35k2973 3 pf35k2974 4 pf35k297S 5 pf35k2976 6 pf35k2977 7 pf35k2978 8 pf35k2979 9 pf35k2980 10 pf3Sk2981 11 pf35k2962 12 pf35k2983 13 pf35k2984 14 pf35k2985 15 pf35k2986 16 pf35k2987 17 pf35k2968 18 pf35k2969 19 pf35k2990 20 pf35k2991 21 pf 3Sk2992 22 pf3Sk2993 23 pf35k2994 24 pf35k299S 25 pf35k2996 26 pf35k2997 ID 919.59.1 919.59.2 919.59.3 919.59.4 919.59.5 919.59.6 919.59.7 919.59.8 919.59.1 919.59.9 919.S9.2 HQXPR1AA HQXPR1AC HQXPR1AD HQW311A HQW321AA HQW341AA HQW351AA 919.59.1 919.59.2 919.59.3 919.59.4 919.59.5 919.59.6 919.59.7 919.59.8 Sanpls Text Blank 0.2 pg/L 0.5 ug/L 1 ug/L 2 ug/L 5 ug/L io ug/L 20 ug/L Blank 2 ug/L ICV 0.2 ug/L R5K250000-125 MB R5K250Q0Q-125 LCS R5K250000-125 LCS D5K230384-1 D5K230384-2 D5K230384-3 D5K230384-4 Blank 0 . 2 M9 /L .5 ug/L 1 ug/L 2 ug/L 5 ug/L io ug/L 20 ug/L Type Std Cono Blank Standard 1 0 . 0 0 Standard 1 0 . 0 0 Standard 1 0 . 0 0 Standard 1 0 . 0 0 Standard 1 0 . 0 0 Standard 1 0 . 0 0 Standard 1 0 . 0 0 Blank QC 1 0 . 0 0 QC 1 0 - 0 0 Blank oc 10.00 OC 1 0 . 0 0 Analyte Analyte Analyte Analyte Blank Standard 1 0 . 0 0 Standard 10.00 Standard 1 0 . 0 0 Standard 1 0 . 0 0 Standard 1 0 . 0 0 Standard 1 0 . 0 0 Standard 1 0 . 0 0 RT 1.98 1.98 1.98 1.98 1.98 1.98 1.98 1.98 1.98 1.98 1.98 1.90 1.94 1.94 1.81 1.80 1 87 2.00 1.98 1.98 1.98 1.98 1.98 1.98 1.98 2.00 Arsa Flags Ion 12656 bb 11361 bb 11351 bb 11377 bb 11458 bb 11623 bb 10966 bb 11013 bb 12760 bb 11436 bb 11359 bb 9069 bb 9753 bb 6911 bb 9075 bb 6581 bb 9018 bb 10078 bb 12831 bb 11401 bb 11436 bb 11460 bb 11554 bb 11592 bb 11060 bb 10969 bb Analyst : Stave Cowling Pag 3 28 Ara* I8 t Raspn 0 12656.092 0 11360.507 0 11351.100 0 11377.194 0 11458.034 0 11622.778 0 10986.110 0 11012.955 0 12759.809 0 11436.396 0 11359.144 0 9089228 0 9753.498 0 8911.388 0 9075.379 0 BS81.407 0 9018.342 0 10078-491 0 12830.908 0 11400.858 0 11436.228 0 11460.226 0 11553.841 0 11591.646 0 11060.273 0 10968.801 Cone pg/L or kg O %kac 11.1904 111.90 10.0448 100.45 10.0365 100.37 10.0596 100.60 10.1311 101.31 10.2767 102.77 9.7138 97.14 9.7375 97.38 11.2821 112.82 10.1119 1 0 1 . 1 2 10.0436 100.44 8.0366 80.37 8.6239 86.24 7.8793 78.79 8.0243 80.24 7.5876 75.88 7.9739 79.74 8.9113 89.11 11.3449 113.45 10.0805 100.81 10.1118 1 0 1 . 1 2 10.1330 101.33 10.2158 102.16 10.2492 102.49 9.7794 97.79 9.6985 96.98 extract mL 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 5.000 5.000 5.000 5.000 5.000 5.000 5.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 Saapla nL or g Dilution Cairila 1.00 1.000 p35k29d 1.00 1.000 pa35k29d 1.00 1 .0 0 0 p3Sk29d 1.00 1.000 pa35k29d 1.00 1 . 0 0 0 pa35k29d 1.00 1.000 pa35k29d 1.00 1.000 pa3Sk29d 1.00 1.000 pa3Sk29d 1.00 1.000 pa35k29d 1.00 1.000 pa35k29d 1.00 1.000 pa35k29d 250.00 1.000 pa35k29d 250.00 1.000 pa3Sk29d 250.00 1.000 pa35k29d 251.00 1.000 pa35k29d 250.00 1.000 pa3Sk29d 251.00 1.000 pa35k29d 233.00 1.000 pa3Sk29d 1.00 1.000 pa3Sk29d 1.00 1.000 pa35k29d 1.00 1.000 pa35k29d 1.00 1.000 pa35k29d 1.00 1.000 pa3Sk29d 1.00 1.000 pa3Sk29d 1.00 1.000 pa3Sk29d 1.00 1.000 pa35k29d p. 145 STL Denver Quantify Compound Summary Report PPOA Analysis Sample List: C:\MassLynx\prOA.PRO\8 anpleDB\pf3Sk29(4) Last modified: wed Nov 30 07:39:38 2009 Method: C:\MasaLynx\PPOA.PRO\MethDB\pe3Sk29b Last modified: Ned Mov 30 07:23:49 2005 Job Code: Printed: Ned Nov 30 07:45:10 2005 Compound 4: PROS Sample List: pf3Sk29(4) Method Pile: pa35k29b Coefficient of Determination: 0.999478 Calibration curve: -7.557890-5 x * 2 0.326145 * * 0.00682519 Response type: internal Std ( Ref 3 ), Area * ( IS Cone. / ZS Area ) Curve type: 2nd Order, Origin: exclude, Neighting: 1/x, Axis trans: None Na^ 1 p35k2972 2 pf35k2973 3 p35k2974 4 pf35k2975 S pf35k2976 6 pf3Sk2977 7 p35k2978 8 pf3Sk2979 9 pf35k2980 10 pf35k2981 U pf35k2982 12 pf 35k2983 13 pf35k2984 14 pf35k2985 15 pf35k2986 16 pf35k2987 17 pf35k2988 18 p35k2989 19 pf35k2990 20 pf35k2991 21 pf35k2992 22 pi35k2993 23 pf35k2994 24 pf35k2995 25 pf3Sk2996 26 pf35k2997 ID 919.59.1 919.59.2 919.59.3 919.59.4 919.59.5 919.59.6 919.59.7 919.59.8 919.59.1 919.59.9 919.592 HQXPRlAA HQXPR1AC HQXPR1AD HQW311AA HQW321AA HQW341AA HQW351AA 919.S9.1 919.59.2 919.59.3 919.59.4 919.595 919.59.6 919.59.7 919.59.8 Sampla Text Blank 0.2 yg/L 0.S ug/L 1 ug/L 2 ug/L 5 ug/L io ug/L 20 ug/L Blank 2 ug/L ICV 0.2 pg/L R5K250000-125 MB R5K250000-12S LCS R5K250000-125 LCS DSK230384-1 D5K2303842 OSK230384-3 D5K230384-4 Blank 0.2 ug/L 0.5 ug/L 1 ug/L 2 ug/L 5 ug/L io ug/L 20 ug/L Typ 8 td Cone Blank Standard 0.20 Standard 0.50 Standard 1.00 Standard 2.00 Standard 5.00 Standard 1 0 . 0 0 Standard 2 0 . 0 0 Blank QC 2 . 0 0 QC 0 . 2 0 Blank QC 0 . 2 0 QC 0 . 0 2 Analyte Analyte Analyte Analyte Blank Standard 0.20 Standard 0.50 Standard 1.00 Standard 2.00 Standard 5.00 Standard 1 0 . 0 0 Standard 2 0 . 0 0 RT 2.63 2.62 2.63 2.63 2.63 2.63 2.65 2.63 2.65 2.65 2.62 2.65 2.63 2.63 2.63 2.65 2.65 Area Plaga Ion Ratio 90 bb 169 bb 388 bb 757 bb 1859 bb 3651 bb 7133 bb 800 bb 93 bb 12 bb 82 bb 172 bb 37? bb 796 bb 1940 bb 3726 bb 7336 bb Analyst: Steve Cowling 03 tn PSQ 4 Hspoils Cone yg/L or ko() HRoe Extract mL Saxpla a L r g Dilution CalFila 3 1.000 1.00 1.000 pa3Sk29d 3 0.079 0 . 2 2 1 1 110.56 1.000 1.00 1.000 pa35k29d 3 0.149 0.4366 87.32 1.000 1.00 1.000 p35k29d 3 0.341 1.0248 102.48 1.000 1.00 1.000 pa35k29d 3 0.661 2.0057 100 29 1.000 1.00 1.000 pa35k29d 3 1.599 3 3.323 4.8884 97.77 10.1922 101.92 1.000 l.ooo 1.00 1.00 1.000 pa35k29d 1 . 0 0 0 pa35k29d 3 6.477 19.9311 99 66 1.000 1.00 1.000 pa35k29d 3 1.000 1.00 1.000 pa35k29d 3 0.700 2.1259 106.30 1.000 1.00 1.000 pa35k29d 3 0.082 0.2295 114.74 1.000 1.00 1.000 pa35k29d 3 5.000 250.00 1.000 pa3Sk29d 3 5.000 250.00 1 . 0 0 0 pa35k29d 3 5.000 250.00 1.000 pa35k29d 3 5.000 251.00 1.000 pa35k29d 3 5.000 250.00 1.000 pa35k29d 3 5.000 251.00 1.000 pa35k29d 3 0-011 0.0003 5.000 233.00 1.000 pa35k29d 3 1.000 1.00 1.000 pa35k29d 3 0.072 0 . 2 0 0 0 99.98 1.000 1.00 1.000 pa35k29d 3 0.151 0.4407 88.13 1.000 1.00 1.000 pa35k29d 3 0.329 0.9892 98.92 1.000 1.00 1.000 pa35k29d 3 0.689 2.0932 104.66 1.000 1.00 1.000 pa3Sk29d 3 1.673 5.1159 102.32 1.000 1.00 1 .0 0 0 pa35k29d 3 3.369 10.3326 103.33 1.000 1.00 1.000 pa3Sk29d 3 6.688 20.5823 102.91 1.000 1.00 1.000 p35k29d p. 147 STL Denver Quantify fiaopla Raport PFOA Analysis 8 anc>l List: C: \KassLynx\PrOA.PRO\Sa**>laDB\pf 35K29 (4) Last isodifiad: Mad Mov 30 07:39:38 2005 Matbod: C: \NassLynx\PPOA.PftO\MathDB\pa35k29b Last aodifiad: Mm 3 No v 30 07:23:49 2005 Job Coda: Printad: Mad Nov 30 07:45:13 2005 Nns: pf35k2983 Taxt: RSK250000-125 MB Faga 12 3: PFOA 13C2 29-Nov-2005 29-Nov-2005 HQXPR1AA 18:30:06 HQXPR1AA 18:30:06 pf35k2983 Sm (Mn, 2x2) F1 pf35k2983 Sm (Mn, 2x2) F1 1.90 414.8 >369.7 0.52 498.6 > 79.9 9089 i 3.69e4 90.8 1 Area v0Ps* f vi-- r 1 PPOA 2 APPO 3 PPOA 13C2 4 PROS ID HQXPRlAA HQXPRlAA HQXPRlAA HQXPRlAA Sanpla Taxt RSK2SOOOO-12S R5K250000-125 R5K250000-125 R5K2S0000-125 MB MB MB MB M 2.065 2 065 1896 n /in m Mui ime1 1 1 1 1 11 M - p 111 11 1 1 1 1 T. 1 1.00 2.00 3.00 Araa Flags 185 bb 185 bb 9089 bb yg/L or kg() VRac Mod.Coanint 0.0008 00009 8.0366 80.37 . 1.00 2.00 3.00 Analyst: fiteva Cowling Ch CTi p. 148 STL (J) Quantify saapls Raport 3 PPOA Analysis Sanpla List: C :\ H a s * L y n x \ P F G A . PRO\Ban>laDB\pf35k29 (4) Last modified: Nad Nov 30 07:39:36 2005 M Natbod: C:\MassLynx\PFOA.PRO\MathDB\pa3Sk29b Last nodifiad: Wad Nov 30 07:23:49 2005 Job Coda: Printad: Mad Nov 30 07:45:13 2005 F*9 * 13 Nam: pf35k2984 T*Kt: R5K250000-12S LC6 3: PFOA 13C2 29-Nov-2005 29-Nov>2005 29-Nov-2005 29-Nov-2005 HQXPR1AC 18:34:32 HQXPR1AC 18:34:32 HQXPR1AC 18:34:32 HQXPR1AC 18:34:32 pf35k2984 Sm (Mn, 2x2) F1 pf35k2984 Sm (Mn, 2x2) F1 pf35k2984 Sm (Mn, 2x2) 1.94 412.8 >218.7 1.94 412.8 >218.7 1.94 13147\ 6.46e3 1314]\ 6.46e3 9753 F1 pf35k2984 Sm (Mn, 2x2) F1 2.50^ 498.6 > 79.9 4.66e4 104 Area Area Area - 1.00 2.001 r r i | i n T] r n i | i h r 3.00 pf35k2984 Sm (Mn, 2x2) F1 1.94 412.8 >368.7 11884]\ 5.74e4 Area 1 I i ii p m ; m m 1 1 1 >11 h 1 1 1 1 1 1 1 1 rii 1.00 2.00 3.00 pf35k2984 Sm (Mn, 2x2) F1 1.94 412.8 >368.7 118847\ 5.74e4 Area x0Ps* ' i" " i" it Time 1.00 2.00 3.00 0 '111 ' 'i '1 11 1'' iI'fr1'i ' '' 1 1 H1Time 1.00 2.00 3.00 ipm111 Iii 11 Time 1.00 2.00 3.00 58 1.00 2.00 3.00 Nam 1 PPOA 2 APPO 3 PPOA 13C2 4 PPOS ID HQXPR1AC HQXPR1AC HQXPR1AC HQXPRLAC Saapla Taxt R5K250000-125 R5K250000-125 R5K250000-125 R5K250000-125 RT 1.938 1.938 1.938 Araa Plaga 11884 bb 11884 bb 9753 bb pg/L or kg() XRec Nod.Co-- isnt 0.2026 101.31 0.2109 101.42 8.6239 86.24 Analyst: Stava Cowling (T\ <1 p. 149 STL Denver Quantify Baapla Report PFOA Analysis Sample List : C :\NassLynx\PrQA.PRO\BanDleDB\pf 35R29 <4) Last aodifled: wad Nor 30 07:39:38 2005 Mathod: C:\MassLynx\PrQA.PRO\HetbOB\pa35R29b Last modified: Wad Mo t 30 07:23:49 2005 Job Coda: Printad: wad Mov 30 07:45:13 2005 Page 14 ____________________________________ ___________________ Naas: pf35R2985 Taxt: A5K250000-125 LCS 3: PFOA 13C2 29-Nov-2005 29-Nov-2005 29-Nov-2005 29-Nov-2005 HQXPR1AD 18:39:00 HQXPR1AD 18:39:00 HQXPR1AD pf35k2985 Sm (Mn, 2x2) F1 pf35k2985 Sm (Mn, 2x2) F1 pf35k2985 Sm (Mn, 2x2) 1.95 412.8 >218.7 145A 747 1.95 412.8 >218.7 145i 747 8911 Area S' - Area 18:39:00 HQXPR1AD 18:39:00 F1 pf35k2985 Sm (Mn, 2x2) F1 0.54 498.6 > 79.9 4.33e4 | 84.5 Area 2.25 3.03 8 -pA rpn n pn (iji?V| i?irp-in 8 -*! 11if if l rpn n I n 11 1 1V>I-| IT1 lurin' 1.00 2.00 3.00 1.00 2.00 3.00 pf35k2985 Sm (Mn, 2x2) F1 pf35k2985 Sm (Mn, 2x2) F1 1.94 412.8 >368.7 412.8 >368.7 12157\ 5.59e3 5.59e3 Area Area * i 3.34 nnp n r; 1 1 1 rjtMn in| 1 1 1 n Time 1.00 2.00 3.00 Time 1.00 2.00 3.00 i m ir Time" " 1" it m r r m 11 it1 1 1 1 1 1 1.00 2.00 3.00 69 tttttt- Time 1.00 2.00 3.00 Mana 1 PPOA 2 APFO 3 PFOA 13C2 4 PFOS ZD HQXPR1AD HQXPR1AD HQXPR1AD HQXPR1AD Banple Taxt RSK2SOOOO-125 .R5K250000-12S .. R5K250000-125 .. R5K250000-12S RT 1.938 1.938 1.936 Araa Flags 1215 bb 1215 bb 8911 bb Itg/L or kg( ) *Rac Nod.Constant 0.0204 101.8 S 0.0212 101.93 7.8793 78.79 Analyst: Steva cowling CTs 00 p. 150 STL Q ^ Quantify Sampl Raport ^ PFOA Analysis ^ Raspla List: C:\MasaLynx\PFQA.PRQ\SaMpla0B\pff35R29(4) (D Last axxlflad: Wad Nor 30 07:39:38 200S 1*1 Matbod: C:\MassLynx\PFOA.PftO\NathDB\pa3Sk29b Last odified: fad Nor 30 07:23:49 2005 Job Coda: Printad: ifad MOV 30 07:45:13 2005 Paga 15 ___ ____ ________________________________________ U m : pf35K2986 Taxt: DSK230384-1 3: PFOA 13C2 D5K230384-1 29-Nov-2005 D5K230384-1 29-Nov-2005 D5K230384-1 29-Nov-2005 D5K230384-1 29-Nov-2005 HQW311AA 18:43:28 HQW311AA 18:43:28 HQW311AA 18:43:28 HQW311AA 18:43:28 pf35k2986 Sm (Mn, 2x2) F1 1.82 412.8 >218.7 pf35k2986 Sm (Mn, 2x2) F1 1.82 412.8 >218.7 pf35k2986 Sm (Mn, 2x2) F 1 pf35k2986 Sm (Mn, 2x2) F1 1.81 414.8 > 369.7 0.58 498.6 > 79.9 97 n 303 97 T\ 303 9075 2.86e4 L o.76 161 Area Area Area ___11t 11111y1111111ii^ Tfi i p ii 111111 1.00 2.00 3.00 pf35k2986 Sm (Mn, 2x2) F1 1.81 412.8 >368.7 706 7 \ 2.24e3 Area n i'i" " i" " i" " i" " i 1.00 2.00 3.00 pf35k2986 Sm (Mn, 2x2) F1 1.81 412.8 > 368.7 706 7\ 2.24e3 Area ' mf| 1111|i111111111uTTpiniTiw Time 1.00 2.00 3.00 ' itwi 1 1 1 1 M1 1 1 1 1 1 111 i 11 i m Tin Time 1.00 2.00 3.00 0 ^i1 1 1 1 1 i'ii'i1 1 1 11 /i 1 1 1 1 m^*p ' iT'i'in r Time 1.00 2.00 3.00 V36 ii| iITTji " Time>1 |1 I I I M'T '1IT1T1 1 1 1 11 1 11 1 1 1 1 1 1.00 2.00 3.00 PFOA APFO PFOA 13C2 PFOS XD HQW3UAA HQW311AA HQW311AA HQW311AA Sanpla Taxe D5K230384-1 D5K230384-1 D5K230384-1 DSK230364-1 RT 1.811 1.811 1.811 Araa Flags 706 bb 706 bb 9075 bb pg/L or kg(> 0.0105 0.0109 6.0243 %*ac Mod.C< 80.24 Analyst: Stava Cowllng (T\ VO p. 151 STL D enver Quantify Sanpla Raport FPOA Analysis Sanvls List: C :\HassLynx\PPQA.PRQ\SanplsDB\pf35*29(4) Last modlfiad: Wad Now 30 07:39:3$ 3005 Matbod: C :\MassLynx\PFOA. PRO\MsthDB\pa35k29b Last aodifiad: Wad No t 30 07:33:49 3005 Job Coda: Prlntad: Wad Nov 30 07:45:13 3005 Pag 16 Nana: pf35*2987 Taxt: O5K330384-3 3: PFOA 13C2 D5K230384-2 29-Nov-2005 D5K230384-2 29-Nov-2005 D5K230384-2 29-Nov-2005 D5K230384-2 29-Nov-2005 HQW321AA 18:47:56 HQW321AA 18:47:56 HQW321AA 18:47:56 HQW321AA 18:47:56 pf35k2987 Sm (Mn, 2x2) F1 0.78 412.8 >218.7 181 3.34 pf35k2987 Sm (Mn, 2x2) F1 0.78 412.8 >218.7 181 3.34 pf35k2987 Sm (Mn, 2x2) F1 1.80 414.8 >369.7 8581 2.64e4 Area pf35k2987 Sm (Mn, 2x2) F1 n q o 1.53 498.6 > 79.9 88.4 | i i 1 1 [ i i n p -i !! 11 n 11 1 1 1 1 | i i r r 1.00 2.00 3.00 pf35k2987 Sm (Mn, 2x2) F1 2.01 412.8 > 368.7 151A 584 Area |IIII|IIIT)ITTTpri II|IIM 1.00 2.00 3.00 pf35k2987 Sm (Mn, 2x2) F1 2.01 412.8 > 368.7 151A 584 Area i\11'' ii" rri11111" iii111'in- Time 1.00 2.00 3.00 16 rin V |" " | T i" | " " r n " |i'iITTr r r r T i m e 1.00 2.00 3.00 limiiiirpmTf Time 1.00 2.00 3.00 3.44 Time 1.00 2.00 3.00 Nam 1 PFOA 2 APFO 3 PFOA 13C2 4 PFOS ZD HQW321AA HQW321AA HQW321AA HQW321AA flanpl* Taxt D5K230384-2 D5K230384-2 D5K230384-2 D5K230384 2 RT 2.009 2.009 1.797 Araa Flags 151 bb 151 bb 8581 bb yg/L or kg() 0.0004 0.0004 7.5876 \RSG Nod.Coewaant 75.88 Analyst: 8tava Cowling o p. 152 STL D enver Quantify Sanpla Raport PFOA Analysis fiaapla List: C: \MassLynx\FFOA.PRO\B*iaplaDB\pf351i29(4) Last aodifiad: wad Nov 30 07:39:38 3005 Matbod: c :\NassLynx\PPOA.FRO\MathDB\pa35k29b Last MOdifiad: Wad Nov 30 07:23:49 2005 Job Coda: Printad: Wad Nov 30 07:45:13 2005 Pag x7 Naas: pf35k2988 Tajct: 05X230384-3 3: PFOA 13C2 D5K230384-3 29-Nov-2005 D5K230384-3 29-Nov-2005 D5K230384-3 29-Nov-2005 D5K230384-3 29-Nov-2005 HQW341AA 18:52:24 HQW341AA 18:52:24 HQW341AA 18:52:24 HQW341AA 18:52:24 pf35k2988 Sm (Mn, 2x2) F1 pf35k2988 Sm (Mn, 2x2) F1 pf35k2988 Sm (Mn, 2x2) F1 pf35k2988 Sm (Mn, 2x2) F1 0.74 412.8 > 218.7 2.01 170 0.74 412.8 >218.7 2.01 170 1.87 9018 414.8 >369.7 3.44e4 0.52 498.6 > 79.9 82.5 ' 2.84 3.28 84 3.28 Area | I I'l'l I I I '| I l'I I J I I 1I |'l I I I |! i M f n i 1111 n p ' r i i j r M 11 t rr i ft 2.46 2.87 1.00 2.00 3.00 pf35k2988 Sm (Mn, 2x2) 1.00 2.00 3.00 F1 pf35k2988 Sm (Mn, 2x2) F1 3.42 2.05 412.8 >368.7 2.05 412.8 >368.7 155A 751 155A 751 Area Area f-mr, Mjr i~iy1 1 1 1 1 1 1 1 1 1 1 1 t1 1 1 1 Time 1.00 2.00 3.00 i|iiiT|Tn-i-riiii|iii.|niT Time 1.00 2.00 3.00 0 i>q Time^ttti^i r r rpTn p 1111l i t r i nM i1n11i1l1i11 1.00 2.00 3.00 TTTTj-,', ir , I I I I , I I I I | I l I I , l l 1I , l 1.00 2.00 3.00 Time * naia 1 PPOA 2 APPO 3 PFOA 13C2 4 PPOS ZD HQW341AA HQW341AA HQW341AA HQW341AA Sanpla Taxt DSK230384-3 D5K230384-3 DSK230384-3 D5K230384-3 RT 2.051 2 .0 51 1.867 Aram Flag* 1 SS bb ISS bb 9018 bb lg/L or kg() 0.0003 0.0003 7.9739 %Rac Mod.Comant 79.74 Analyst: Stava Cowling o p. 153 STL D enver Quantify Sample Report PPOA Analysis Sample List; C :\MaasLynx\PPQA.PAO\SanpleDB\pf35A29(4) Last modified: Wed Nov 10 07:39:31 2005 Method: C:\MassLynM\PPOA.PRO\MethDB\pa35A29b Last modified: Wed Ho t 30 07:23:49 2005 Job Code: Printed: Wed n o t 30 07:45:13 2005 Page 18 Name: pf35k2989 Text: DSK230384-4 3: PPOA 13C2 D5K230384-4 29-Nov-2005 D5K230384-4 29-Nov-2005 D5K230384-4 29-Nov-2005 D5K230384'4 29-Nov-2005 HQW351AA 18:56:52 HQW351AA 18:56:52 HQW351AA 18:56:52 HQW351AA 18:56:52 pf35k2989 Sm (Mn, 2x2) F1 pf35k2989 Sm (Mn, 2x2) F1 pf35k2989 Sm (Mn, 2x2) F1 pf35k2989 Sm (Mn, 2x2) F1 1.99 412.8 >218.7 1.99 412.8 >218.7 1.99 414.8 > 369.7 2.65 498.6 > 79.9 51 ]\ 369 369 10078 7.15e4 12 156 Area Area Area Area 1.00 2.00 3.00 1.00 2.00 3.00 pf35k2989 Sm (Mn, 2x2) F1 pf35k2989 Sm (Mn, 2x2) F1 2.01 412.8 >368.7 442 I 2.84e3 2.01 412.8 > 368.7 442]\ 2.84e3 Area Area i|piTqTTTT|'r.Ti 11 m1 1 1 111111 I Time 1.00 2.00 3.00 3 *rm`f>TTp Time 1.00 2.00 3.00 - nil 1 | r 1M j HM | 1 1H| ii>n' '' 'i 'ii Time 1.00 2.00 3.00 Name 1 PFOA 2 APPO 3 PPOA 13C2 4 PPOS ZO HQW351AA HQW351AA HQH3S1AA HQW351AA Sample Text D5K230364-4 D5K230384-4 D5K230384-4 D5K230384-4 RT 2.009 2.009 1.995 2.646 Area Flags 442 bb 442 bb 10078 bb 12 bb U9 /L or Ag() 0.0051 0.0053 8.9113 0.0003 %*ec Mod.Cement 89.11 M vw wuA/ V w 31 *'I'l r | 1 , 1 f'1 1 1 1 I'IT T T IT T I I j 1 1.00 2.00 3.00 Time Analyst: Steve Cowling