Document jmb3NvKzqEm484gd6M25Xd5xp

EVe( riR E S E A R C H X / m Precise Research. Proven Results. Enclosure 5 AR << _ 701 Analytical Report Fluorochemical Characterization of Water and Sediment Samples Decatur Bakers Creek #2 - July 2003 (E03-0561) Exygen Research Laboratory Report No. L34910 Revision 1 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Jess Eldridge 3M Environmental Technology and Safety Services 935 Bush Avenue Building 0002-03-E-09 PO Box 33331 ST. Paul, MN 55133-3331 po cr^> TP* 'O Zj ~Xj VO 'j n i ro `O o --\ r'T'i 9? trno o o o o io ^3058 Research Drive l!State College, PA 16801, USA P A G E W ^ f. 800.281.3219 kF: 814.272.1019 exygen.com 1 Introduction Results are reported for the analysis of surface water and sediment samples received by Exygen Research (Exygen) from Pace Analytical. The Exygen study num ber assigned to the project is L34910. Specific fluorochem ical characterization by liquid chromatography / tandem mass spectrom etry (LC/MS/MS) was requested for all samples. A total of 26 samples were received for analysis. The samples were prepared and analyzed by LC/MS/MS fo r the following list of fluorochem icals: Table 1: Target Analysis Compound Name Perfluorohexanesulfonate Perfluorooctanesulfonate Perfluorooctanoic Acid Perfluorooctanesulfonvlam ide Acronvm C6 Sulfonate fPFHSI C8 Sulfonate iPFOS) C8 Acid (PFOA1 FOSA The analytical methods used were originally developed for groundwater sam ples and were validated by Exygen. The validation protocol and results are on file with Exygen. Only the C8 Sulfonate, FOSA, and C8 Acid were included in the original method validation. It should be noted that the quality control elements included in this analysis dem onstrate the applicability of the method to the additional analytes. 2 Sample Receipt The samples were subm itted in plastic containers. All samples were cooled to 4C from tim e of collection to receipt at Exygen Research. Samples were stored at 4C from receipt at Exygen Research until analysis. Samples were collected on 7/21/03 and 7/23/03. Chain-of-custody information is presented in Attachm ent C. 3 Holding Times Field and laboratory spikes of these fluorochem icals have shown stability for periods greater than 90 days. Samples were analyzed within 30 days of receipt. PAGE2 OFS uOOOll 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis W ater samples were initially treated with 200 uL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-m illiliter portion of sample was used for analysis. The samples were transferred to a C ,8 SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatm ent resulted in an eight-fold concentration of the diluted samples prior to analysis. Sediment samples were first extracted into methanol (5 grams of sediment to 5 mL of m ethanol). The methanol extract was diluted to forty-m illiliters and treated in the same manner as the water samples, using SPE. 4.1.2 Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract Is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochem icals are observed and quantitated against standards. A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples extractions and analyses were performed between 7/31/03 and 8/13/03. Exact dates for extraction and analysis of each sample batch are given in the raw data. Raw analytical data is provided in Attachments D and E. 5 Analysis 5.1 Calibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/MS/MS analysis. The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. A calibration curve is acceptable if r >0.985 (r2 > 0.970). Calibration standards are prepared using the same SPE procedure used for samples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained If the standard analyte concentrations are within +/-20% of the actual value. All calibration criteria were met for this analysis. PAGE 3 OF5 000012 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant. Instrum ent blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical methods. 5.4 Matrix Spikes Field m atrix spikes were prepared at low and high levels for each sample for all compounds of interest. Single laboratory m atrix spikes were also performed for each sample. Laboratory control spikes (see section 5.6) consisting of laboratory water spiked at the tim e of extraction were performed with each analytical set. Matrix spike recoveries are given in Attachm ent B. For sediment samples, recovery is calculated from the amount present in the sample extract. Please see Section 5.7 for additional discussion of m atrix spike recoveries. 5.5 Duplicates Field and laboratory duplicates were performed for each sample. The duplicate results are included with the sample results in Attachment A. 5.6 Laboratory Control Samples For LC/MS/MS analyses, Milliq water was spiked with all compounds with each extraction set. All recoveries for all compounds were between 70-130% in each LCS. Results are given along with the raw data in Attachment D. 5.7 Statement of Accuracy Based on results of field spikes, laboratory spikes, field blank spikes, and laboratory control spikes, the analytical accuracy for all compounds Is 30%. Exceptions for the water samples are as follows: BC2 SW-04 high spike (PFOA - 57%, PFOS - 62%, FOSA - 58% ), BC2 SW05 high spike (PFOA - 66%, FOSA - 40%), BC2 SW-06 high spike (FOSA - 60%), Outfall to River SW-25 (FOSA - 58%). Also, several low spike samples showed unacceptable recoveries in cases where the spiking concentration was comparable or below the inherent sample concentration. However, all laboratory control spikes, laboratory m atrix spikes, and all other field spikes showed recoveries between 70% and 130% for all compounds. The accuracy for the sedim ent samples is based upon laboratory spike recoveries, all of which were between 70% and 130% for all compounds. 6 Data Summary Please see Attachm ent A for a detailed listing of the analytical results. Results are reported in parts per billion (ppb) (ng/mL) for the water samples. Sediment samples are also reported in units of parts per billion (ppb) (ng/g). Sediment results are reported on both an as-received and dry-weight basis. PAGE 4 OF5 000013 7 Data/Sample Retention Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders m aintained by Exygen. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachm ent C: Chain of Custody 8.4 Attachm ent D: Raw Analytical Data (Surface W ater Samples) 8.5 Attachm ent E: Raw Analytical Data (Sediment Samples) 9 Signatures Other Lab Members Contributing to Data Karen Risha Date Date PAGES OF5 000014 SECTION A 000015 Repiort 1 Proven Results. Summary of PFOA, PFHS, PFOS and FOSA in Water Samples S am ple ID BC2SW-04 BC2 SW-04* BC2 SW-04 Dup BC2 SW-05 BC2 SW-05* BC2 SW-05 Dup BC2-SW-06 BC2-SW-G6* BC2-SW-06 Dup Outfall to River SW-25 Outfall to River SW-25* Outfall to River SW-25 Dup Equipment Blank-Pump Equipment Blank-Dredge Field Control/Travel Blank A n a lyte F ound (ng /m L) C8 A cid PFOA C6 S u lfo n a te PFHS Perfluorooctanolc Acid Perfluorohexanesulfonate 4.21 0.896 4.21 0.882 2.54 0.571 0.591 0.155 0.616 0.152 1.56 0 .3 7 7 12.1 6.06 12.3 6.30 11.6 5 .8 7 15.8 7.66 16.0 14.4 7 .1 0 6.77 ND ND ND ND ' ND ND S am ple ID BC2 SW-04 BC2 SW-04* BC2 SW-04 Dup BC2 SW-05 BC2 SW-05* BC2 SW-05 Dup BC2-SW-06 BC2-SW-06* BC2-SW-06 Dup Outfall to River SW-25 Outfall to River SW-25* Outfall to River SW-25 Dup Equipment Biank-Pump Equipment Blank-Dredge Field Control/Travel Blank A n a lyte F ound (ng /m L) C8 S u lfo n a te PFOS FOSA Perfluorooctanesulfonate Perfluorooctanesulfonylamide 11.5 11.5 8.25 1.67 1.54 4.33 26.1, 26.7 25.1 31.2 31.5 30.8 ND ND ND , 1.39 1.37 0.790 0.146 0.150 0.389 2 .4 3 2.30 2.57 3.26 3.18 3.28 ND ND ND ND=Not Detected=Response between 0 and 0.025 ng/mL NQ=Not Quantifiable=Response between 0.025 ng/mL and LOQ (0.05 ng/mL) Laboratory Duplicate 000016 X .3058 Research Drive State College, PA 16801, USA V,T: 814.272.1039 F: 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDENTIALITY-- Exygen Research ( Exygen," "us." or "w e") maintains the strictest confidentiality in all of our client interactions. If a signed confidentiality agreement is required, we will provide one. If a regulatory or legal body subpoenas inioimatron, the clienl will be notified promptly. The client agrees not to use Exygen's name and/or data in any manner that might cause harm to Exygen's reputation or business. Approval must be obtained, in writing, before Exygen's name ain.be published in any way CONTRACTS--M contracts are subject to review' and approval by Exygen's legal council and must be signed by a corporate officer. PAYMENT TERMS--Unless otherwise set forth in this Purchase Order, terms of payment are "Met 30 Days." The time allowable for payment shall begin after b o llr (a) client's receipt of Exygen's invoice; and (b.l the satisfactory performance of the services contemplated hereunder. A 1,5.. monthly service charge shall be added to all past due balances Notwithstanding any payment terms to the contrary set forth in this Purchase Order, Exygen, in its sole discretion, reserves the right to request payment in advance tram client In the event ot default in payment for services rendered, Exygen shall be entitled to reasonable costs of collection, including, but not limited to, attorneys' fees. BILLING--All fees and charges are billed directly to the client requesting services. Exygen will not bill a third party without prior notification irr writing, via a signed statement acknowledging and accepting responsibility for payment. Exygen will assume that the paperwork submitted with a sample describes the desired testing protocol. Any changes to the piotocol must be submitted in writing Please fax changes to Exygen marked, "URGENT" to your assigned representative. If changes are made after the originally requested lusting has been initiated or completed, the client accepts responsibility for payment. Exygen will not Be responsible for hold times that are missed due to such changes RUSH SERVICE--Exygen routinely offers expedited turnaround times on critical analyses. Rush analysis services are contingent upon availability and prearrangement with an authorized Exygen representative. A surcharge is usually added to the list fee if rush analysis is requested M IN IM U M FEE--The minimum fee for commeicial services is one hundred dollars <S100). SAMPLE COLLECTION/SUBMISSION--!:. 11ent shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law anc good commercial practice. Title and risk of loss with respect to submitted samples shall at all times remain with client prior to acceptance by an Exygen sample custodian. Exygen will initiate a chain-of-custody upon sample receipt unless the client includes one with the sample(s). By request, Exygen will provide chuin-of-custoriy forms for client's use All samples submitted must be accompanied by: purchase order, oi signed quotation; sample description, including sample type, source, time and date of collection; specific analyses requested, estimated concentration levels; requested report date; current billing address; and other relevant Information Upon request. Exygen will provide and ship appropiiale sample containers to clients. These containers will include the appropriate preservative if particular analyses require one. It Is the responsibility of the clienl to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced tor freight Exygen reserves the right to charge a fee for sample containers SAMPLE DISPOSAL--Exygen retains samples for one month after reporting results, then disposes of or returns the sample. Unless the client requests that the sampleisi be teUirned. or prior airangemenfs have been made for long-tenn storage, Exygen shall dispose of the samplers). Exygen shall charge a monthly tee for long-term storage. Samples found or suspected to contain hazardous waste, according to definitions m state ar -'or federal guidelines, will be relumed to the client upon completion ot tb ^ analysis The cost of returning the samplers) will be invoiced lo the client, Exygen reserves the right to charge a disposal lee for the disposal of any and all samples unless returned by Exygen to client. Exygen shall, unless the nature arid diameter of the sample dictates otherwise, store all samples under locked, temperature-controlled conditions. An internal charn-ofcustody is maintained for each lot of samples received. HAZARD COMMUNICATION-- The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics ot the sample, and to provide information on hazard prevention and personal protection as necessary oi otherwise leq jiie d by applicable law. QUALITY ASSURANCE-- Exygen will perform services consistent with its Quality Assurance Standard Operating Procedures (SOPs), the terms of which are expressly incorporated herein by reference: pioviden, however :t shall be the exclusive responsibility or the client to confirm that Exygen's standard practices will meet the client's needs prior to placing an older for woik. In the event client desires an alternative to these SOPs. such requests must be made in writing prior to sample submission arid acceptance by Exygen, ETHICS POLICY-- Exygen Research strives to provide its clients with the highest, quality data in the fastest realistic turnaround time. We balance the high standards oi this goal by insisting that each employee also perform within the guidelines ol the highest possible professional ethics Each Exygen employee is required to sign a statement of personal and professional integrity. SPECIAL REPORTS--Additional charges may be necessary for custom report formats LITIGATION--All costs associated with compliance to any subpoena for documents, for testimony in a court of law. or for any other purpose ^ relating to work performed by Exygen Research shall he invoiced by Exygen and paid by client These costs shall include, but are not limited to, hourly charges foi the persons involved, travel, mileage, and accommoda tions, and tor any and all other expenses associated with said litigation. INDEMNIFICATION, LIABILITY, A N D INSURANCE-- Exygen agrees to indemnify, defend, and save the ciient. its oificeis. directors, employees, agents, and representatives harmless from all losses, expenses, demands, and claims made against the client, its officers, directors employees,.agents and representatives because of any personal injuries, death, or property damage to the extent caused by the negligence or willful misconduct of Exygen Its employees, agents, or representatives in connection with the perfoimance of services undet this agreement, except to tne extent such losses, expenses, demands, or claims, occur as a result of the negligent or willful acts or omissions of the client, its otticors, directors, employees, agents, and representatives; however, such indemnification and damages shall, in the aggregate, be limited to the amount equal to the lesser of (a) damages suffered by the client as the direct result thereof, or (b) the total amount paid to Exygen for the work herein covered. Exygen will, it requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage, WARRANTY AN D LIMITS OF LIABILITY-- In accepting analytical work. Exygen guarantees the accuracy of the test results for the sample as submitted within the tolerances set forth in the SOPs We disclaim any other warranties expressed or implied by law. Exygen does not accept any legal responsibility for the purposes for which client uses the lest results Exygen will not accept any purchase order or any other order for work that Includes conditions that vary from these Standard Conditions ACCEPTANCE OF PURCHASE ORDER-- This Purchase Order becomes a ^ binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement ol work. 000017 Analytical ^ Report 1 Proven Results. SuluvV* Summary of PFOA, PFHS, PFOS and FOSA In $dil Samples Sample ID BC2 SED-04 BC2 SED-04* BC2SED-05 BC2 SED-05* BC2-SED-06 BC2-SED-06' Outfall to River SED-25 Outfall to River SED-25* Outfall to River SED-25 Dup Analyte Found (ng/g, as received) Kr* C8 Add PFOA C6 Sulfonate PFHS Perfluorooctanolc Acid Perfluorohexanesulfonate 3.02 0.566 2.14 5.14 4.41 0.413 1.45 1.75 14.2 13.6 10.7 2.46 2.61 3.19 7.59 2.26 17.7 4.98 Sample ID BC2 SED-04 BC2 SED-04* BC2 SED-05 BC2 SED-05* BC2-SED-06 BC2-SED-06* Outfall to River SED-25 Outfall to River SED-25* Outfall to River SED-25 Dup Analyte Found (ng/g, as received) C8 Sulfonate PFOS FOSA Perfluorooctanesulfonate Perfluorooctanesulfonylamlde 14.6 11.9 22.8 7.15 7.84 7.86 25.0 12.1 . 880 71.4 992 83.2 \ 107 28.0 72.1 23.5 140 35.7 ND=Not Detected=Response between 0 and 0.2 ng/g NQ=Not Quantifiable=Response between 0.2 ng/g and LOQ (0.4 ng/g) Laboratory Duplicate O O O O IS J & 3 .03055(8 Research Drive / U Stlate College, PA 16801, USA YJ : 814.272.1039 F: 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDENTIALITY-- Exygen Research (' Exygen,' ` us." or "w e ") maintains the strictest confidentiality in all of our client interactions If a signed confidentiality agreement is required, we will provide one. If a regulatory or legal body subpoenas information, lire client, will .be notified promptly. The client agrees not to use Exygen's name and/or data in any manner that might cause harm to Exygen's reputation or business. Approval must be obtained, in writing before Exygen's name can be published in any way CONTRACTS-- All contracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer. PAYMENT TERMS--Unless otherwise set forth in this Pinchase Orden terms o payment are " Net 30 Days " The lime allowable for payment shall begin alter both: (a) client's receipt of Exygen's invoice: and (b) the satisfactory performance of the services contemplated hereunder, A 1.5% monthly service charge shall be added to all past due balances. Notwithstanding any payment terms to the contrary set forth in this Purchase Order, Exygen, in its sole discretion, reserves the right to request payment in advance from client In the event of default in payment for services rendered. Exygen shall be entitled to reasonable costs of collection, including, but not limited to, attorneys' fees. BILLING--All fees and charges aie billed directly to the client requesting services. Exygen will not bill a third party without prior notification m 'writing, via a signed statement acknowledging and accepting responsibility for payment. Exygen will assume ihat the paperwork submitted with a sample describes the desired testing protocol. Any changes to the protocol must be submitted in writing. Please fax changes to Exygen marked, "URGENT'' to your assigned representative. If changes are made after the originally requested testing has been initiated or completed, the client accepts responsibility tor payment.. Exygen will not be responsible tor hold times that are missed due to such changes. RUSH SERVICE-- -Exygen routinely offers expedited turnaround times on critical analyses. Rush analysis services are contingent upon availability and prearrangement with an authorized Exygen representative. A surcharge is usually added to the list lee if rush analysis is requested. M IN IM U M FEE-- The minimum fee for commercial services is one hundred doilars ($100). SAMPLE COLLECTION/SUBM/SSION--CJient shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law and good commercial practice. Title and risk o loss with respect to submitted samples shall at all times remain with client prior to acceptance by fin Exygen sample custodian. Exygen will initiate a chain-of-custody upon sample receipt unless the client includes one with the sample(s). By request. Exygen will provide chain-of-custody forms for client's use All samples submitted must be accompanied by: purchase order, or signed quotation; sample description, including sample type, source, time and date of collection; specific analyses requested; estimated concentration levels, requested report date current billing address: and othei relevant information Upon request, Exygen will provide and ship appropriate sample containers to clients. These containers will include the appropriate preservative if particular analyses require one. It is the responsibility of the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers'. SAMPLE DISPOSAL-- Exygen retains samples for one month after reporting results, then disposes of or returns the sample. Unless the client requests that the sample) be returned, or prior airangemems have been made for long-term storage. Exygen shall dispose of the sampie(s), Exygen shall chaige a monthly lee loi long-term storage. Samples found or suspected to contain hazardous waste, according to definitions m slate or /or federal guideline!, will be relumed lo the client upon completion ul l i t * analysis. The cost of returning the samplets) will be invoiced to the client. Exygen reserves the right to charge a disposal fee for the disposal of any and all samples unless relumed by Exygen to client. Exygen shall, unless the nature and character of the sample dctales otherwise, store all samples under locked, temperature-contiailed conditions. An internal chain-ofoustody Is maintained for each lot cit samples received HAZARD COMMUNICATION--The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law QUALITY ASSURANCE-- Exygen will perfoim services consistent with it? Quality Assurance Standard Operating Procedures (SOPs). the terms ot which are expressly incorporated herein by reference: provided however, it shall be the exclusive responsibility of the client to conhrin that Exygen's standard practices will meet the client's needs prior lo placing an order for work, in the event client desires an alternative to these SOPs, such requests must be made in writing pnor to sample submission and acceptance by Exygen. ETHICS POLICY-- Exygen Research strives In provide its clients with the highest quality data in the fastest realistic tumaiound time. We balance the high standards of this goal by insisting that each employee also perform within the guidelines ot the highest possible professional ethics. Each Exygen employee is required to sign a sintemen! of personal and professional integriry. SPECIAL REPORTS--Additional charges may be necessary' for custom report formats. LITIGATION--All costs associated with compliance !o any subpoena tor documents, for testimony in a court of law. or tor any other purpose relating to work perfoimed by Exygen Research shall be invoiced by Exygen and paid by client. These costs shall include, but are not limited to. hourly charges for the persons involved, travel, mileage, and accommoda tions, and for any and all other expenses associated with said litigation. INDEMNIFICATION, LIABILITY. AND INSURANCE-- Exygen agrees to indemnify, defend, arid save the client, its officers, directors, employees, agents, and representatives harmless from all losses, expenses, demands, and claims made against the client, its officers, directors, ernployees^agents and representatives because of any personal injuries, death, or property damage to the extent caused by the negligence or willful misconduct of Exygen, its employees, agents, or representatives in connection with the performance of services undet this agreement, except to the extent such losses, expenses, demands, or claims, occur as a result or the negligent or willful acts or omissions of the client, its officers, directors, employees, agents, and representatives; however, such indemnification and damages shall, in the aggregate, he limited to the amount equal to the les.se of (a) damages suffered by the client as the direct result thereof, or (L>) the total amount paid to Exygen for the work herein covered. Exygen will if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage. WARRANTY AN D LIMITS OP LIABILITY-- In accepting analytical woik. Exygen guarantees the accuracy of the test results for die sample as .submitted within the tolerances set forth in the SOPs We disclaim any other warranties, expressed or implied by law. Exygen does not accept any legal responsibility for the purposes for which client uses the test results. Exygen will not accept any purchase order or any other order for work that Includes conditions that vary from these Standard Conditions ACCEPTANCE OF PURCHASE ORDER-- This Purchase Order becomes a ^ binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement ot work. 000019 Analytical ^ Report Proven Results. Summary of PFOA, PFHS, PFOS and FOSA in J>til Samples Sample ID BC2 SED-04 BC2 SED-04* BC2SED-05 BC2 ED-05* BC2-SED-06 BC2-SED-Q6* Outfall to River SED-25 Outfall to River SED-25* Outfall to River SED-25 Dup Analyte Found (ng/g, dry weight) C8 Acid PFOA C6 Sulfonate PFHS Perfluorooctanolc Acid Perfluorohexanesulfonate 4.31 0.809 3.06 0.591 7.39 2.09 6.34 2.51 23.6 4.08 22.5 4.33 16.9 5.05 12.0 3.57 26.2 7.39 Sample ID BC2 SED-04 BC2 SED-04* BC2 SED-05 BC2 SED-05* BC2-SED-06 BC2-SED-06* Outfall to River SED-25 Outfall to River SED-25* Outfall to River SED-25 Dup Analyte Found (ng/g, dry weight) C8 Sulfonate PFOS FOSA Perfluorooctanesulfonate Perfluorooctanesulfonylamlde 20.9 10.2 17.0 11.2 32.8 11.3 36.0 \ 1460 17.4 118 1640 169 114 208 138 44.3 37.2 52.9 ND=Not Detected=Response between 0 and 0.2 ng/g NQ=Not Quantifiable=Response between 0.2 ng/g and LOQ (0.4 ng/g) Laboratory Duplicate 000020 J ^ 3 03055f8 Research Drive 4 P d is St atalte College, PA 16801, USA \ J : 814.272.1039 F: 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDENTIALITY-- Exygen Research ( 'Exygen,'1 "us," or "we") maintains the strictest confidentiality in all of cm client interactions. If a signed confidentiality agreement is required, we will provide one. If a regulatory 01 legal body subpoenas information, the client will be notified promptly. The client agrees not to use Exygen's name and/or data In any manner that might cause harm to Exygen s reputation or business. Approval must be obtained, in writing, before Exygen's name can be published in any way. CONTRACTS--- All contracts are subject to review and approval by Exygen's iegal council and must be signed by a corporate officer. PAYMENT 7CT/KS-- Unless otherwise set forth m this Purchase Older, terms of payment are "Net 30 Days " The lime allowable for payment shall begin after both' (a) client's receipt of Exygen's invoice; and (b) the satisfactory performance of the services contemplated hereunder. A 1.5% monthly service charge shall be added to all past due balances. Notwithstanding any payment terms to the contrary set forth in this Purchase Order, Exygen. in its sole discretion, reserves the right to request payment in advance from client. In the event of default in payment for services rendered, Exygen shall be entitled io reasonable costs ot collection, including, but not limited to, attorneys' fees. BILLING-- All fees arid charges are billed directly to the- client requesting services. Exygen will not bill a third patty without prior notification in writing, via a signed statement acknowledging and accepting responsibility for payment. Exygen will assume that the paperwork submitted with a sample describes the desired testing protocol. Any changes to the protocol must be submitted in writing. Please fax changes to Exygen marked, "URGENT1 to your assigned representative. If changes are made after the originally requested testing has been initiated or completed, the client accepts responsibility for payment. Exygen will not be responsible lor hold times that are missed due to such changes. RUSH SERVICE--Exygen routinely otters expedited turnaround times on critical analyses. Rush analysis services are contingent upon availability and prearrangement with an authorized Exygen representative. A surcharge is usually added to the list fee if rush analysis is requested. M IN IM U M FEE--The minimum fee for commercial services is one hundred dollars ($100). SAMPLE COLLECTION/SUBM/SSION-Oient shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law and good commercial practice. Title and risk of loss with respect to submitted samples shall at all times remain with client prior to acceptance by an Exygen sample custodian Exygen will Initiate a chain-of-custody upon sample receipt unless the client includes one with the sample(s). By request. Exygen will provide chain-of-custody forms for client's use. Ali samples submitted must be accompanied by; purchase order, or signed quotation, sample description, including sample type, source, time and date of collection; specific analyses requested, estimated concentration levels; requested report date; current billing address; and other relevant information Upon request, Exygen will provide and ship appropriate sample containers to clients. These containers will include the appropriate preservative if particular analyses require one. It is the responsibility of the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SAMPLE DISPOSAL-- Exygen retains samples for one month after reporting results, then disposes of or returns the sample. Unless the client requests that the sample(s) be returned, or prior mrangements have been made tor long-term storage. Exygen shall dispose of the sample(s) Exygen shall charge a monthly fee fo- long-term storage Samples found or suspected to contain hazardous waste, according to definitions in state ;ir /o r federal guideline, will be renam'd to the client upon completion of tlx * analysis. The cost of returning tire samplers) will be invoiced to the client. Exygen reserves the right to charge a disposal tee for the disposal of any and all samples unless returned by Exygen to client. Exygen shall, unless the nature, and character of the sample dictates otherwise, store all samples under locked, temperature-controlled condition?. An inlcrnal chain-ofcustody Is maintained tor each lot of samples it-ceivc-d HAZARD COMMUNICATION-- The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and la provide information on hazard prevenlion and personal protection as necessary oi otherwise required by applicable law. QUALITY ASSURANCE--ixygen will perfoim services consistent with its Quality Assurance Standard Operating Procedures (SOPs). the ten ns of which are expiessly incorporated herein by re'eience; provided however, it shaft Ire tiie exclusive responsibility of die client to confirm that Exygen's standard practices will meet the client's needs prior to placing an order for work. In the event client desucs an alternative to these SOI-'s, such requests must be nude in writing poor to sample submission and acceptance by Exygen. ETHICS POLICY-- Exygen Research strives to piovide its clients with the highest quality data in the fastest realistic turnaround time We balance the high standards of this goal by insisting that each employee also perform within the guidelines of the highest possible professional ethics. Each Exygen employee- is required to sign a stateroom of personal arid professional integrity SPECIAL REPORTS -Additional charges may be necessary fnr custom report formats LITIGATION--All costs associated with compliance to any subpoena for documents, for testimony in a court of law. or for any other purpose ''' relating to work performed by Exygen Research shall be invoiced by Exygen and paid by client. These costs shah include, but are not limited to. hourly charges for the persons involved, travel, mileage, and accommoda tions, arid for any and all other expenses associated with said litigation. INDEMNIFICATION, LIABILITY, AND INSURANCE- Exygen agrees to indemnify, defend, and save the client, its officers, directors, employees, agents, and representatives harmless from all losses, expenses, demands, and claims made against the client, its officers, directors, einpioyees.jisents and representatives because of any persona! injuries, death, or property damage to the extent caused by the negligence or willful misconduct of Exygen. its employees, agents, or represent;)fives in connection with the performance of services under this agreement, except to the extent such losses, expenses, demands, or claims, occur as a result of the negligent or willful acts or omissions of the client, its officers, directors, employees, agents, and representatives; however, such indemnification and damages shall, in hie aggregate, he limited to the amount equal to the lesser of (a) damages suffered by the client as the direct result thereof or (b) the total amount paid to Exygen for the work herein covered. Exygen will, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage. WARRANTY AN D LIMITS OF LIABILITY-- in accepting analytical work, Exygen guarantees the accuracy of the test results for the sample as submitted within the tolerances set forth in the SOFs. We disclaim any other warranties, expressed or implied by law Exygen does not accept any legal responsibility for the purposes for which client uses the test results. Exygen will not accept any purchase order or any other order for work that includes conditions that vary from these Standard Conditions. ACCEPTANCE OF PURCHASE ORDER-- This Purchase Order becomes a binding, agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement of work. 000021 SECTION B 000022 Recovery Summary lor PFOA, PFHS, PFOS and FOSA In Water Sample Description Amount Spiked (nq/m ll C8 Acid PFOA_________________________ C6 Sulfonate PFHS Amt Found Amount Amount Amt Found Amount In Sample Recovered Recovery Spiked in Sample Recovered (n g /m l) (ng/mL) (%> (ng/mL) (ng/mL) (ng/mL) Recovery (%) BQ2 5W-04 Lab Spike 5 4.21 8.14 79 5 0.896 5.52 92 BC2 SW-04 Low Soke 0.1 4.21 2.76 -1450- 0.1 0.896 0.647 -249' BC2 SW-04 High Splka 10 4.21 9.92 57 10 0.696 9.73 88 BC2 SW-05 Lab Spike BC2 SW-05 Low Spika 5 0.591 0.1 0.591 4.98 87 5 2.17 1579' 0.1 0.155 0.155 5.00 0.607 97 452 BC2 SW-05 High Spike 10 0.591 7.21 66 10 0.155 9.58 94 BC2 SW-06 Lab Spike . 5 12.1 17.8 114 5 6.06 11.8 115 BC2 SW-06 Low Spike . 0.1 12.1 13.9 1800' 0.1 6.06 7.11 1050' BC2 SW-06 High Spike 10 12.1 24.2 121 10 6.06 17.4 113 Outfall to River SW-25 Lab Spike - 5 15.8 22.1 126 5 7.66 12.2 91 Outfall to River SW-25 Low Spike OutfaM to River SW-25 High Spike 0.1 10 15.8 15.8 15.0 26.2 -800' 104 0.1 10 7.66 7.66 6.64 -1020* 18.1 104 Held Control/Travel Blank Low Spike 0.1 ' ND 0.114 114 0.1 ND 0.119 119 Field Control/Travel Blank High Spike 10 ND 11.9 119 10 ND 10.8 108 Sample Description Amount Spiked {ngftnU C8 Sulfonate PFOS Am t Found Amount in Sample Recovered (n g /m l) (ng/mL) Recovery <%) Amount Spiked (ng/mL) FOSA Amt Found Amount in Sample Recovered (ng/mL) (ng/mL) Recovery <%> BC2 SW-04 Lab Spike 5 11.5 17.1 112 5 1.39 5.58 84 BC2 SW-04 Low Spike BC2 SW-04 High Spike 0.1 11.5 10 11.5 6.89 -4610' 0.1 1.39 0.672 -718' 17/7 62 10 1.39 7.18 58 BC2 SW-05 Lab Spike 5 1.67 5.94 \ 85 5 0.146 4.86 94 BC2 SW-05 Low Spike 0.1 1.67 5.37 . 3700" 0.1 0.146 0.498 352 BC2 SW-OS High Spike 10 1.67 12.8 111 10 0.146 4.14 40 BC2 SW-06 Lab Spike 25 26.1 49.8 95 5 2.43 7.18 95 8C2 SW-06 Low Spike 0.1 26.1 32.1 6000* 0.1 2.43 2.55 120' BC2 SW-06 High Spike 10 26.1 43.9 178 . 10 2.43 8.44 60 OutfaU to River SW-25 Lab Spike 50 31.2 80.9 99 5 3.26 7.97 94 Outfall to River SW-25 Low Spike 0.1 31.2 29.4 1800' 0.1 3.26 2.66 -600* Outfall to RJver SW-25 High Spike 10 31.2 41.2 100 10 3.26 9.02 56 Field Contrat/Travei Blank Low Spike 0.1 ND 0.109 109 0.1 ' .ND 0.0898 90 Field Control/Travel Blank High Spike 10 ND 11.4 114 10 NO 11.9 119 NDNot Datactad-Responaa between 0 and 0.025 ng/mL NONot QuantiliablR*sponae between 0.025 ng/mL and LOO (0.0S ng/mL) Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. 000023 J ^ 3 03055i8 Research Drive E m s tSatal te College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com Recovery Summary for PFOA, PFHS, PFOS and FOSA in Soil Sample D e scrip tio n BC2 SED-04 Lab Spike, BC2 SED-05 Lab Spike BC2 SED-06 Lab Spike Outfall to River SED-25 Lab Spike C8 Acid PFOA C6 Sulfonate PFHS Amount Amt Found Amount Amount Amt Found Amount Spiked in Sample Recovered Recovery Spiked In Sample Recovered Recovery (ng/g) (ng/g) (ng/g) (%) (ng/g) (ng/g) (ng/g) (*/.) 40 3.02 41.5 96 40 0.566 42.2 104 40 5.13 43.7 96 40 1.46 44.2 107 40 14.2 49.4 88 40 2.46 44.5 105 40 10.7 47.1 91 40 3.19 44.5 103 Sample D escription BC2 SED-04 Lab Spike BC2 SED-05 Lab Spike BC2 SW-06 Lab Spike Outfall to River SW-25 Lab Spike C8 Sulfonate PFOS FOSA Amount Amt Found Amount Amount Amt Found Amount Spiked in Sample Recovered Recovery Spiked in Sample Recovered Recovery (ng/g) (ng/g) (ng/g) (%) (ng/g) (ng/g) (ng/g) (%) 40 14.6 51.8 93 40 7.15 46.5 98 40 22.8 61.0 95 40 7.86 48.1 101 800 88 1720 105 800 71.4 650 72 40 107 153 114 40 28.0 59.0 77 Results reported on an as-received basis 000024 J & 3 035058 Research Drive < # W S St atalte College, PA 16801, USA YT: 800.2813219 F: 814.272.1019 exygen.com SECTION C 000025 / zraceAnalyticar ww.yaeelabs.tom R e q u ire d Citent Information: Company' 3m *t gr i Address Section A s$ P( K l ) ? ? - S 2 3 3 CHAIN-OF-CUSTODY / Analytical Request Document The Chain-of-Custody Is a LEGAL DOCUMENT. A ll relevant fields must be completed accurately. R _e q_u_ir_e d_C_lt_en_l _In_fo_rm_a_tio_n ____ Section B Rteopport To: ti M r, J& S. g / d rrJ q Copy To: Page: j o f ^ Invoke To: Client Inlorroalion (Check quote/cootracl): Requested Due Date: ` TAT: 715679 To Ba Completed by P ace Analytical and Client Section C Quoto Reference: Project Manager P.O. jC T S l -- ----- Hr M rr^lBfJuoibor Turn around times toss than 14 days subject to laboratory and contractual obligations and may result in a C w t # 2. Rush Turnaround Surcharge. t / vd d h r- S- Sect itami {* Turn Around Time {TAT) in calendar days. Pro fk Profile#: L k 1> Requested Analyst t iu - v W T 0 3 '-c S (a l T e in "C R eo iv e d on Ice , y 1 N S d ftd Cooler Samples Intact ty!N Additional C ' 'Menta: SAMPLE NOTES : S P hP cr*^ Q) c . rr < 9 *0 0/2 I d p *m ^ c h l riv u i / ( f{($ ri+ jt' ) SAMPLER NAME AND SIGNATURE PRINT Nai mm ie o t S A U P g t R : (L v W SIGNATURE ,. . /lW i - t D A T E Sign*g; {MM / DO /Y Y ) 03 /^ jic e Analytical" i ' www.MCelita.CDm i ftw q u lred Client Information: Section A R e q u ire d Client Information: Refrn To: - tfUr. 'fcss $ CHAIN-OF-CUSTODY /Analytical Request Document The Chaln-of-Cuslody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. S e ctio n B ,t Eldrt't/f _ -----------------------------Page: 3 o f 3 . 639392 To Ba Completed by Pace Analytical and Client Section C T el in C Rejgved on Ice Y/N Seaid Cooler Y/N Samples Intact Y/N Additional Qr 3NATUREAMPLER: f 7/21/2003 Project: E03-0561 3M ENVIRONMENTAL LABORATORY PreHminary/Unauthorized Report 1 of 3 Requester Schnobrich, Dana M (223-1N-08) Department: 530711 Project Number 0022674449 Date Received: 6/26/2003 Project Description: Decatur Bakers Creek #2 Surface Water and Sediment Comments: Completion Date: Project Lead: Jess S. Eldridge Phone Number 651-778-5233 Email Address: jseldridge@mmm.com W lflK * NETS 4 T * * ' A ll fa * yd -f-jot p V J r tf P roject R esults/A ct!vitv Pace Field Sampling Event O s ^d riiio -y 3M Sample Number ' Sampled Date E03-0561-49786 7/22/2003 LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49787 7/22/2003 1M EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49788 7/22/2003 LM EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN PFHS FOSA EXYGEN PFOA E 03-O 561-- 4 9 7 8 9 7/22/2003 LAB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E 03-0561-49790 7/22/2003 LAS EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49791 7/22/2003 LM EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA Sample Description BC2 SW-04 Component PFOS PFHS FOSA PFOA BC2 SW-04 DUP ComcomnH PFOS PFHS FOSA PFOA BC2 SED-04 , CpniDQnent PFOS PFHS FOSA PFOA BC2 SW -05 Component PFOS PFHS FOSA PFOA BC2 SW-05 DUP Component PFOS PFHS FOSA PFOA BC2 SED-05 Component PFOS PFHS FOSA Ksiuli Remit Result Remit Result Result BL Oualifler BL Qualifier BL Qualifier BL Qualifier BL Qualifier BL Oualifler 000028 7/21/2003 3M ENVIRONMENTAL LABORATORY Prelim inary/Unauthorized Report Project: E03-0561 (cont.) 3M Sample Number______ Sampled Date_______ Sam ple Description E03-0561-49791 (cont.) 7/22/2003 BC2 SED-05 LAB EXYGEN Analytical Method PFOA E03-0561-49792 7/22/2003 LM EXYGEN Analytical Method PFOS by ESMS EXYGEN PFHS EXYGEN EXYGEN FOSA PFOA E03-0561-49793 7/22/2003 LAB EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49794 7/22/2003 LM EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49795 7/22/2003 LAS EXYGEN Analytical Method PFOS by ESMS EXYGEN PFHS EXYGEN FOSA EXYGEN PFOA E03-0561-49796 7/22/2003 LAS EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49797 7/22/2003 LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49813 7/22/2003 LAS EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA Components PFOA BC2 SW-06 Camaanfata PFOS PFHS FOSA PFOA BC2 SW-06 DUP CPHiatwcnt! PFOS PFHS FOSA PFOA BC2 SED-06 Components PFOS PFHS FOSA PFOA Outfall to River SW-25 Components PFOS PFHS FOSA PFOA Outfall to River SW-25 DUP Components PFOS PFHS FOSA PFOA Outfall To River SED-25 Components PFOS PFHS FOSA PFOA Outfall to River SED-25 DUP Components PFOS PFHS FOSA PFOA Result Result Result RUM Result Result Remit Remit 2 of 3 EL Qualifier RL Oualifier EL Qualifier EL Qualifier EL Qualifier EL Oualifier RL Qualifier EL Qualifier 000029 7/21/2003 3M ENVIRONMENTAL LABORATORY Prettm inary/Unauthoiized Report Project: E03-0561 (coot.) 3M Sample Number______ Sampled Date_______ Sample Description E03-0561-59479 Field Control/Travel Blank LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOSby ESMS PFHS FOSA PFOA E03-0561-59480 Component PFOS PFHS FOSA PFOA Equipment Blank - Pump LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561 -59481 CgfllBQn?nt2 PFOS PFHS FOSA PFOA Equipment Blank - Dredge LM EXYGEN EXYGEN EXYGEN EXYGEN Aaalytital Method PFOS by ESMS PFHS FOSA PFOA Component PFOS PFHS FOSA PFOA Remit Result Result 3 of 3 RL Qualifier EL OwnlifUr EL Q m ltftei 000030 3058 Research Drive State College, PA 16801 ' * >. / Laboratory Sample Log-in Sheet (Environmental Complete upon sample receipt: Phone: 800-281-3219 Fax: 814-272-1019 Client and/or Project Name Method of Delivery Q Walk-in Tracking #: Pick-up O UPS I f Y i f J & 7 & ^ `i f 0 .EfFedEx. Air Borne i; Other (explain) Chain of Custody Temperature Preservation Custody Seals: presgotrirO intact / broken (explain) LTetSsent Thermometer ID: Cooler ID: <? Cooler ID: Cooler ID: Cooler ID: 2- P i vo Cooler temo: Cooler temD: Cooler temp: Cooler temo: Chain of Custody Record: ^ "p re s e n t l absent . Samples Received: L f *C ^E T on ice C In Ice melt "C r with ice pack "C none Explanation Completed by . Slanature: L // Data (Timet: ^ 7 / 2 H e ? Complete durinct sample log-in: . 1 j. *- LIMS Log-in # " L J Y * ) '* Physical Condition Samples Intact? ^ y f e s No (explain) Chain of Custody Samples received agree with COC record? -T?es No (explain) Analysis Request Analysis request clear? 'lU Y e s O No (explain) Preservation Sample containers appropriate? Chemical preservation appropriate? Yes Yes No (explain) No (explain) Samples received within holding time? Yes No (explain) Sample volume/mass adequate? Yes No (explain) ^ Explanation Completed by Slanature: / ^ Complete follow ing resolution of any nonconformances: Client Contacted Yes Client: No Resolution ~ D ti! ^/ -- c ~? 1 f^ -3 f Data fTimel: ' Completed by Slanature: Lab Sx Log-in Sheet -Ex Date:  f r r * r r 4* __^__e__CE^xpress' USAAirbiU 1 From Bfi*a-- 4 h ^I0 $-- Sendar's ^r - 4/ j jJ 4 4 ***+ fl 1)1551,3621,30 Phone f e y C .------ y t t o C> Eiix-------- ~A /^r 7^VC \ j J l - ? ____State j y r ^ YourInternal BillingReference ZIP ,^/j. {/ / f m wiXAuiMm Q^ AQO i--4 vk>\-- __ a Company \ . ^ <* . . Address___ ________ H*HQU)*MNdL<te*to*,MN<MMrm -- ^ 4 '" 4/y i ^ ---------3 0 -S~ 8 ________t V n / e rjy/- * 33`t f can* itkm P.O.km* orf JLHfa 4a ExpressPackageServica j < *\ ' fPMAMrarryytcoannNMnnPUunt'iMMdjumMwgyMkutuoiHMprrtieianlSoNwBmt Ilmit /7 \V Priority Ovarnight uf~*fl.Afa.dWflxh(SWtManrdtt(anrdoaOvernight D1-- 1lMaMrviiEatna*vMMftiftrteascttsthnOcMvaieaMrDnMMiwghigt 1~1 Sf*dnErfxbw2t0natsy<tov *----- P I SFewddEkxuvEwxnpdrfeyss Saver MirwdMrfliHaunJae ------ 4b Express Freight Service1 r*--~ '| MFeadXEixotImDaulynfrreight* *[--~1I SFedMEdxk2<0H*My 4Fir|eight ft* MRMPMaUtnkapttgontotmMtarteUnMNarhia. 5 Packaging 'eKlvarfMiualmutQQO ( 1 Fadb Envelope* ] FedEx Pk* kKUFNlt>SlMlfAFMCi Urgi P* tudF^O.aSb<4P*k l^j/Othe fi Special Handling ' r n n*OAYDefcy L J AMliMarlrhiMiMeray J----- -----------utantaiwctniwJuFadinExatAnJaimiiclawSioacXttM1 --------- .e [--j HMDWMki.y LJ e*MFMedUBXtillao.cation UE,fn!W*< i--iJMHil Saturday ^ LI iAtvFileUdMEaxanleoiDcraBon . " t --* tlip w * connitoyam a I0.1 ----. - OitakcatauMldtatkad . S S S itm !'" `t o n ^ s p ] Yes SfttppaE'iDad'raMn UpGwsfrWkalanpryleaf>>rfoapadatFaiCa n DryIce * ----------- a----------- d l Cargo Aircraft Only 7 Payment fliSio; - { [Obtainitedp I----- tK erfed 6a*cctlMa.*C<idilC#dti#.fc#<0W . -------------------j '----'A cC tN o. Recipient J iT hird Party ( Q Credit Card QCasVCheck 000032 & ^ ri h i t a ( o I f , tr ' L <*> AMIS SbBfl 2430 ^Owrbbfeyh imkfi tori^iWaxrjwudallan t hither ttx Sm bwt to H i I Release Sign$bjrf,dfji$f /fdWymrmdAs--ewyayuna^. Byegningyoutittarirt tpffAVisiih^Hntflrwwemtohtinhg agMuro in l( r H 3>IpSemeav nrfJHl m h a rrio u from *ny muitiofi tliim a.' Q u a id o n i? V U t A y Web It* a t Fedex.com orc*a tboo.ga f i.*W9^6j x i i 0 ,v MML] ) iie ^ rMikpn .7e:g AvX^-A<tS5iiidlb^vj /.vva>,'.v...,. 'T`' y*/'/Tf*>yft LOGIN CHAIN OF CUSTODY REPORT (InOl) Jul 28 2003, 07:54 am Login Number: L34910 Account: 2046 3M ENVIRONMENTAL LABORATORY Laboratory Sample Number client = Collect Receive ; Due L34910-1 : 3C2 SW-04 SAMPLES KEPT IN D0000539. .. . 21-JUL-03 25-JUL- ...... ......... L34910-2 BC2 SW-04. LOW SPK (0.1 PPB.) 21-JUL-03: 25-JUL-C3 1: L3s4r910-:3 .:- v 3C2 SW-04 HIGH SPK :<T0. PPB) 21-JUL-03::25-JUL-C3 : L34910-4 , /; 3C2 SW-04 DDP ;:vu;: L34910-5 ;V 302 SEDr 04 SOIL S PERC SOLID Hold:01-AUG-03 d0000539 ?::L: : ' V r>:; L3491G-6 :V- BC2 SW-05 21-JUL-03 25-JUL-03 ;, L3491C-7 : BC2 SW-05 LOW SPK (0,1 PPB} 21-JUL-03 25-JUL-03 L34910-8 < 3C2 SW-05 HIGH SPK (10 PPB) 21-JUL-03 25-JUL-03 . L34910-9 : BC2 SW-05 DUP 1 T l: L34910-10 3C2 SED-05 21 -JUL-03 25-JUL-03 SOIL S PERC SOLID Hold:01-AUG-03 d0000539 .. L34 910-11 :. ; 3C2 SED-06 23-JUL-03 25-JUL-03 SOIL S PERC SOLID Hold:01-AUG-03 d0000539 : .. - L34910-12 . BC2 sw-06 L34910-13 : i; 3C2 SW-06 LOW SPK (0.1 PPB) 23-JUL-03 25-JUL-03 L34910 -14 , BC2 SW-06 HIGH SPK (10 PPB) 23-JUL-03 25-JUL-03 L3491Q-15 . BC2 SW-06 DUP 23-JUL-03 25-JUL-03. :: ... i .;.) ; L34910-16 : , OUTFALL. TO..RIVER SW-25 23-JUL-03 .25-JUL-03 .. . . L34910-17 : OUTFALL TO RIVER. SW-25. 23-JUL-03 25-JUL-03 COMPLETE ID READS OUTFALL TO RIVER SW-25 LOW SPK (0.1 PPB). : L3 4910-18 1 : OUTFALL TO RIVER SW-25 23-JUL-03 25-JUL-03 COMPLETE ID READS OUTFALL TO RIVER SW-25 HIGH SPK (10 PPB). L3 4910-19 OUTFALL TO RIVER SW-25 DUP 23-JUL-03 25-JUL-03.: ;;: Page 1 000033 LOGIN CHAIN OF CUSTODY REPORT (InOl) Jul 28 2003, 07:54 am Login Number: L34910 Account: 2046 3M ENVIRONMENTAL LABORATORY Laboratory Sample Number illlllililllil; Sample Number; Collect Receive Due Pate Date , PR Date: L34910-20 OUTFALL TO RIVER SED-25 23-JUL-03 25-JUL-03 SOIL S PERC SOLID Hold:01-AUG-03 d0000539 L34310-21 v OUTFALL TO RIVER SSD-25 DUP 23-JUL-03 25-JUL-03 SOIL S PERC SOLID Hold:01-AUG-03 d0000539............. L 34910-22 : . - FIELD CONTROL/TRAVEL BLANK ^.3'^ -.= L34910-23 , , FIELD CONTROL/TRAVEL BLANK LOW 23-JUL-03 25-JUL-03 COMPLETE ID READS FIELD CONTROL/TRAVEL BLANK LOW SPIKE (0.1 PPB) ...... L34910-24 FIELD,CONTROL/TRAVEL;BLANK 23-JUL-03 ,25-JUL-03 : COMPLETE ID READS FIELD CONTROL/TRAVEL BLANK HIGH SPIKE (10 PPB). L34 910-2 5 , , EQUIPMENT BLANK-PUMP 21-JUL-03 25-JUL-03 ; L34 91:0-26 ;,<: : EQUIPMENT BLANK-DREDGE 23-JUL-03 25-JUL-03 : ' Page 2 Signature: :S c,, 000034 SECTION D 000035 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 D ate: 0 8 /2 6 /0 3 Exygen S tudy# L34910 NOTE TO FILE NOTE: T h ro u g h o u t th e ra w d a ta g e n e ra te d fo r s tu d y L 3 4 91 0 th e 4 98 > 7 8 m o n ito re d tra n s itio n (p e rflu o ro o c ta n e s u lfo n y la m id e ) w a s a s s ig n e d th e a cro n ym P F O S A in s te a d o f F O S A . A n y re fe re n c e to P F O S A in th e ra w d a ta is e q u iv a le n t to F O S A . In itia ls : p lL 0 & l2 b ) W 000036 Sponsor Study No: Exygen Study No: .Analyte: Ions Monitored: Site: NA L34910 PFOA 413->369 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ppt 15 pL Water 40.0 mL 5,0 mL Set No: Analyse Instrument Type: Extraction Date: Analyzed oq: 073103A Karen Risha LC/MS/MS Unit # 6 07/31/03 08/01-02/03 Exygen ID XC072503-0 XC072503-1 XCQ72503-2 XC072503-3 XCO72503-4 XC072503-5 XCQ725Q3-S Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spk B L349L0-1 Spk C L34910-6 Spk D L34910-12 Spk E L349I0-I6 Spk F XC072503-1 L34910-1 L34910-1 Rep U4910-4 L34910-2 L34910-3 XC072503-2 L34910-6 L34910-6 Rep L34910-9 L34910-7 L34910-8 XC072503-3 U4910-12 L349L0-12 Rep L349KM5 L34910-13 L34910-14 XCO72503-4 L349IO-16 L349HM6Rep L34910-19 U 49I0-17 L34910-18 XC072503-5 L34910-25 L34910-26 L34910-22 L34910-23 L34910-24 XC071003-6 Sponsor ID BC2 SW-04 BC2 SW-05 BC2SW-06 Outfill to River SW-25 ' BC2 SW-04 BC2 SW-04 BC2 SW-04 Dup BC2 SW-04 Low Spk BC2 SW-04 High Spk - BC2 SW-05 BC2 SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk BC2 SW-06 BC2 SW-06 B O SW-06 Dup BC2 SW-06 Low Spk BC2 SW-06 High Spk Outfall to River SW-25 OutfcOI to River SW-25 Outfall bo River SW-25 Dup Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk . Equipment Blank-Pump Equipment Blank-Dredge Field Control/Travei Blank Field Control/Travei Blank Low Spk Field Control/Travei Blank High Spk - Sample Code cs cs cs cs cs cs cs c c LCS LCS LF LF LF LF CS s s s FF FF CS s s s FF FF CS s s s FF FF CS S s s FF FF CS s s s FF FF CS Run No. 073103A-1001 073103A-1002 073103A-1003 073103A-1004 073103A-ID05 073103A -1006 073I03A-1007 073103A-1008 073103A-1009 073103A-1010 073103A-1Q11 073103A-1012 0731Q3A-1013 07303A-1014 073103A-1015 073103A-1016 073103A-1017 073103A-1018 073I03A-I019 073103A-1020 073103A-I021 073103A-I022 073103A-1023 073103A-1024 073103A-1025 073I3A-1026 073103A-1027 073103A-1028 073103A-1029 073I03A-1030 073103A-I03I 07313A-I032 073I03A-1033 073103A-1034 073103A-1035 073103A-1036 073103A-1037 0 7 3 103A-1038 073103A-1039 073103A-1040 073I03A-1041 073103A-1042 073103A-1043 0731Q3A-1044 073103A-1045 0731Q3A-I046 Analyte Found (ppt) * (peak area - intercept) l slope x DP Recovery ( 96 ) * [analyte found (ppt)-analyie found in control (ppt)} x 100 amount added (ppt) Std. Cone. (ppo 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Peak Factor Area 550 - 8614 - 16102 - 29438 - 66169 - 142891 - 264459 - 267 1 659 I 14411 1 132909 10 239247 10 145872 10 418651 10 ' 515606 - 6931 1 849301 1 826648 1 575640 1 605630 100 29529 13780 1 173871 1 181075 1 355190 1 521363 100 21596 - 31758 1 2471389 l 2425189 2527002 2849870 100 71294 ; 75537 3072978 3276529 275829^ 3102823 100 77205 156964 652 940 808 34004 100 35258 - 322068 Analyte Found (ppo Amount Added (ppo Recovery (%> ND 47.6 452 8140 4960 * * * * 9920 . . . . . . . 50 500 5000 5000 5000 5000 . - 100 10000 - 95 90 79a 87 - * 57A 591 616 * 7210 * * 24200 * 26200 . . 100 10000 100 10000 . . 100 10000 - 66 - 121A - - 104 ND ND ND 114 11900 . . - 100 10000 - 114 119 -- - Standard Curve : Linear (1/x weighted) Intercept * 445.037 Slope * 293 -343 Coef. O f D el * 0.986042 GS Calibration standard LF * Lab fortified sample C * Control sample FF Field fortified sample S * Sample LCS * Laboratory Control Spike CK Check Standard NO = Not detected a Response between 0 and 25 ppt NQ Not quantifiable * Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by: ASample was corrected using the data found in set 073103AR. 'Sample requires hither dilution. See data set 073103AR 000037 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA U4910 PFHS 399 -> 80 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume; Final Volume: SO ppt 15 nL Water 40.0 mL 5.0 mL Set No: Analyst Instrument Type: Extraction Date: Analyzed on: 073103A Karen Risha LC/MS/MS Unit # 6 07731/03 08 1*02/03 Exygen ID XC07250M XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spit B L349IQ-I SpicC L34910-6 Spk D L34910-12 SpIcE L349lO-16SpkF XC072503-1 L34910-1 L349KM Rep L34910-4 L34910-2 L34910-3 XC072503-2 L349104S L3491Q-6 Rep L349I0-9 L34910-7 L34910-8 XC072503-3 L34910-12 U4910.12Rep L34910-13 L349IO-13 L34910-14 XCO72503-4 U4910-16 04910-16 Rep L34910-19 L34910-U U4910-18 XCO72503-5 L34910-25 L349IO-26 L34910-22 L34910-23 L34910-24 XCD71003-6 Sponsor CD BC2 SW-04 BC2 SW-05 BC2 SW-06 Outfall to River SW-25 BC2 SW-04 BC2 SW-04 BC2 SW-04 Dup BC2 SW-04 Low Spk BC2 SW-04 High Spk BC2 SW-05 BC2 SW-Q5 BC2 SW-Q5 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk BC2 SW-06 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk BC2 SW-06 High Spk Outfall to River SW-23 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk Outfall 10 River SW-2 3 High Spk Equipment Blank-Pump Equipment Blank-Dredge Field Cantroi/Travel Blank Field Control/Travel Blank Low Spk Field Control/Travel Blank High Spk Sample Code CS CS CS CS CS CS CS c c LCS LCS LF LF LF LF CS s s s FF FF CS s s s FF FF CS S s s FF FF CS s s s FF FF CS s' s $ FF FF CS Run No. 073103A-1001 073103A-1002 073103A-1003 073103A-1004 0731Q3A-10Q5 073103A-1006 073103A-1007 073103A-100J 073103A -1009 073103A-1010 073103A-1011 073103A-1012 073103A-1013 073103A-1014 Q731Q3A-1015 073103A-I01 073103A-1017 073103A-1018 073103A-1019 073103A-I020 073103A-1021 073103A-1022 073103A-1023 073103A-1024 073103A-1025 073103A-1026 073103A -1027 073103A -1028 073103A-I029 073103A-1030 073103A-I031 073103A-1032 073103A-1033 073103A-1034 073103A -1035 073103A-1036 073103A-1037 073103A-1038 073103A-1039 073103A -1040 073103A-104I 073103A -1042 0731Q3A-1043 073103A-1044 073103A-1045 073103A-1046 Analyte Found (ppt) = (peak area * intercept) t slope x DF Recovery (%) * {analyte found (noO-analyte found in control (ppttf x 100 amount added (pp<) Std. Cene. (PPI) 0 25 50 100 250 500 10OG 25 50 100 250 500 1000 Dilution Factor 10 10 10 10 100 100 1 1 1 100 1 1 1 100 1 1 l l 100 - Peak Area a 1401 2842 5604 13137 26976 51345 Q 0 2759 26598 30859 27946 55454 60284 1444 50162 49342 31968 36223 5426 2420 8666 8505 21096 33965 5342 5959 259042 237649 245687 275858 9718 14198 283517 302530 276429 278698 10133 29038 0 0 0 6648 6002 60941 Analyte Found (PPO Amount Added (ppt) . ,, _ Recovery (%) . ND 49.7 475 5520 5000 . 896 882 571 647 9730 - 155 152 377 607 9580 * 17400 . . . 50 500 5000 5000 5000 5000 - . 100 10000 . . . 100 10000 . . - 100 10000 . 99 95 92 97 -249+ 88 . . . . 452 94 113* 18100 . 100 10000 104* ND ND ND 119 10800 - - 100 10000 - 119 108 - Standard Curve : Linear (1/x weighted) Intercept - -23.5660 Slope 55.9970 Coef. Of Dct - 0.989093 CS * Calibration standard LF * Lab fortified sample C Control sample FF - Field fortified sample S = Sample LGS * Laboratory Control Spike CK Check Standard ND a Not detected Response between 0 and 25 ppt NQ Not quantifiable * Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by: ^Sample was corrected using the data found in set 073103Ait. Sample requires futher dilution. See data set 073103AR. Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L34910 PFOS 499 *> 99 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume; Matrix: Sample Volume: Final Volume: 50 ppt 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: Q73103A Karen Ridia LGMS/MS Unii 07/31/03 QMH-Q2/03 Exygen ID XCQ72503-0 XC0725G3-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC0725Q3-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 SpkB L34910-1 SpkC L34910-6 Spk D L34910-12SpkE L34910-16 Spk F XC071S03-1 L34910-I L34910-I Rep U49HM L34910-2 L34910-3 XC072503-2 L349I0-6 L34910-6 Rep L34910*9 L34910-7 L3491Q-8 XC0725O3-3 L34910-12 L34910-I2 Rep L34910-15 L34910-13 U49I0-14 XC072503-4 L349UM6 L34910-16 Rep L34910-19 U4910-17 L34910-18 XC072503-5 U4910-23 L34910-26 L34910-22 L34910-23 L349IO-24 XC071003-6 Recover/ {%) Sponsor ID - .. BC2 SW-04 BC2 SW-05 BC2 SW-06 Outfall to River SW-2S -' BC2 SW-04 BC2 SW-04 BC2 SW-04 Dup BC2 SW-04 Low Spk BC2 SW-04 High Spk BC2 SW-OJ BC2 SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk BC2 SW-06 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk BC2 SW-06 High Spk ' OutfalUo River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk Equipment Blank-Pump Equipment Blank-Dredge Field Control/Travel Blank Field Control/Travel Blank Low Spk Field Control/Travel Blank High Spk Sample Code cs cs cs cs cs cs cs c c LCS LCS LF IF LF IF CS S S S FF FF CS S S s FF FF CS s s s FF FF es s s s PF FF es s S s FF FF CS Rua No. 073HBA-1001 073103A-1002 073103A-103 073103A -1004 073I03A-1005 073103A-1006 073103A-1007 073103A-1008 073I03A-1009 73103A-1010 073103A-1I1 073103A-1012 73103A-1013 073103A-1014 073I03A-1015 073103A-1016 073103A-I017 073I03A-1018 073103A-1019 073103A-1020 073103A-1021 073I03A-1022 073103A-1023 073103A-1024 073103A-1025 073103A -1026 073103A-1027 073103A-1028 073103A-1029 073103A-IQ30 073103A-1031 073103A-1032 073103A-133 0731Q3A-1034 073103A-I035 073103A -1036 073103A-1037 073103A-103S 073103A-1039 073103A-1040 073103A-1041 073103A-1042 073103A-1043 073103A-1044 073103A-1044 073103A-1046 (analyte found (ntx)-analyte found in control (pool x 100 amount added (ppt) Std. CODC. (ppo 0 23 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Peak Factor Area 0 971 1963 3040 7518 17228 32298 0 -0 1673 15199 10 50011 10 20296 10 96734 10 120697 954 280183 274170 211725 19(631 100 6016 1656 44922 46036 112926 149088 100 4333 3500 558236 571211 560118 667186 100 14981 8521 691166 1 707270 1 636333 1 683659 too 14072 19341 316 [0 10 3691 100 3853 - 35665 Analyte Found (ppO Amount Added (ppt) Recovery (%) .. . ' ND 50.4 445 * 5940 * * m * 17700 - * 12800 . 43900 - * 41200 50 500 5000 3000 5000 5000 . . - 100 10000 . . . 100 10000 - . 100 10000 . . . . too 10000 . 101 89 85* . . . . 62** . . . - Ill* . - . . . 178** . - . 100* ND ND ND 109 11400 . - 100 10000 - - 109 114 -- Standard : Linear (l/x weighted) Intercept * .56.2500 Slope - 34.2805 C oef.O fD et.* 0.992844 CS Calibration standard LF * Lab fortified sample C * Contrai sample FF * Field fortified sample S Sample . LCS - Laboratory Control Spike CK Check Standard ND - Not detected - Response between 0 and 23 ppt NQ - Not quantifiable Response between 25 ppt and LOQ (SO ppt) & ribhlo?) Soreadaheet oreoared bv: F f f U l / ^ *Sample was corrected using the data found in set 073103AR. **Sample was corrected using the data found in set 080603A. Sample requires futher dilution. See data m i 073103AR. Sponsor Study Nor Exygcn Study No: Analyte: ions Monitored: Site: NA L34910 FOSA 498 -> 78 Decatur Baker's Creek RAW DATA REPORT Limit o f Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume; 50 ppt 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on; 0 7 3 103A Karen Risha LC/MS/MS Unit # 6 07/31/03 08/01-02/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 SpkB L34910-1 Spk C L349I0-6 Spk D L34910-12 Spk H L349I0-16 Spk F XC072503-1 L34910-1 L349I0-1 Rep L34910-4 L34910-2 L34910-3 XC072503-2 L349I0-6 L34910-6 Rep L349I0-9 L34910-7 L34910-8 XC072503-3 L3491Q-12 L34910-12 Rep L34910-I5 L349IO-I3 L34910-14 XC072503-4 L349IO-16 L34910-16 Rep L34910-19 L34910-17 U4910-18 XC072503-5 U 4 9 10-25 L34910-26 L349I0-22 L34910-23 L34910-24 XCQ71003-6 Sponsor ID - BC2 SW-04 BC2 SW-05 BC2 SW-06 Outfall to River SW-25 BC2 SW-04 BC2 SW-04 BC2 SW-04 Dup BC2 SW-04 Low Spk BC2 SW-04 High Spk B a SW-05 BC2 SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk BC2 SW-06 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk BC2 SW-06 High Spk Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk Equipment Blank-Pump Equipment Blank-DTedge Field Control/Travel Blank Field Control/Travel Blank Low Spk Field Control/Travel Blank High Spk Sample Code CS CS CS CS CS CS CS c c LCS LCS LF LF LF LF CS S s s FF FF CS s s s FF FF CS s s s FF FF cs s S S FF FF CS s S S FF FF CS Run No. 0 7 3 103A-1001 0731D3A-1D02 0 7 3 103A-1003 073103A-I004 0 7 3 103A-1005 073103A-1006 073103A-1007 073103A-1008 073103A -1009 073103A-101Q 073103A-1011 0731D3A-1Q12 0 7 3 103A-013 073103A-1014 073103A-10J5 073103A-1016 073103A-1017 073103A-1018 073103 A-1019 0 7 3 103A-I020 073103 A-1021 073103A-1022 073103A-3 023 073103A-1024 073103A -1025 073103A-1026 073103A-1027 073103A-1028 073103A-1029 0 7 3 103A-1030 073103A-103I 073103 A-1032 073103A-1033 073103A-1034 073103A-1035 073103A-1036 073I03A-1037 0 7 3 103A-1038 073103A-1039 073103A-1040 073 03 A-1041 073I03A-1042 073103A-1043 073103A-1044 073103A -1045 073103A-1046 Analyte Found (ppt) (peak area - intercept) / slope x DF Recovery (%) * fanalyte found (ppt)-ana]yte found in control (ppt)l x 100 amount added (ppt) Std. Conc. (ppO 0 25 50 100 250 500 1000 25 50 100 . 250 500 . 1000 Dilution Factor 10 10 10 10 100 1 1 1 100 l 1 ] 1 100 1 1 1 1 100 - 1 l 1 1 100 - Peak Area 0 3440 6725 13321 31340 65687 127765 0 Q 6872 62898 74954 65330 96556 107094 3545 148109 143575 106161 90364 9716 6634 19717 20175 52363 67031 5639 13989 269867 263411 276134 284082 11410 33866 358032 358872 369645 311246 12191 72430 0 814 0 12140 16047 139302 Analyte Found (ppo . Amount Added (ppo Recovery (%) . . . . ND 50.6 468 5580 4860 7180 7970 * 790 672 7180 146 150 389 498 4140 * * 8440 * * * * 9020 . ND ND ND 89.8 11900 50 500 5000 5000 5000 5000 . _ . 100 10000 . . . _ 100 10000 . . . 100 10000 . . . . 100 10000 . . . . 100 10000 101 94 84A 94 95A 94A . . . . -718A+ 58A . . . 352 40 60* 58A 90 119 - - S f r n d r ilf lir v t : Linear (1/x weighted) Intercept = 78.1882 Slope * 134.313 Coef. O f DeL 0.995963 CS Calibration standard LF * Lab fortified sample C Control sample FF - Field fortified sample S = Sample LCS = Laboratory Control Spike CK Check Standard ND Not detected Response between 0 and 25 ppt NQ - Not quantifiable - Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by;. d2> 'Sample was corrected using the data found in set 073103AR Sample requires father dilution. See data set 073103AR. +Sample residue significantly exceeds the spiking level; therefore, in accurate recovery cannot be calculated. 000040 eV8; e n 3058 Research Drive Phone: 814-272-1039 w RESEARCH State College, PA 16801 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number: Exygen Sample # -E349 40-2- L34910-3-fc34910-4 -L34940 ; - L34910- 49KTr -4)34910 8 L34 91Q-9 1 349 lX U lflL319K H --L31946H2 L349K H 0 NA Sponsor Sample # BC2 SW-04 BC2 SW-04 Lout Spit BC2 SW-04 High Spk BC2 SW-04 Pup BC2 SED-04 BC2 SW-05 BC2 SW-05 Low Spk BC2 SW-05 HighSpk BC2 SW-OS Pup BC2 SED-05 BC2 SED-06 BC2 SW-06 BC2 SW-06 Low Spk Karen Risha 7/31/03 0800 Requested By (Printed Name/Date/Time) Exygen Study Number: L34910 Exygen Sample # L34940 14. L3494^4$ L340 4O-47L31910 U . L9494 0 -19- y m 0=20J-34Q1CL21. `L-34 9 10-2&-7 4910 -231.34910-24W4S4CL25. L3 494 0 -24 . Sponsor Sample # BC2 SW-06 High Spk BC2 SW-06 Pup Outfall to River SW-25 Outfall tp River SW-25 Low Spk Outfall to River SW-25 High Spk Outfall to River SW-25 Pup Outfall to River SW-25 SED Outfall to River SW-25 SED DUP Field Control/Travel Blank Field Control Low Spk Field Control High Spk Equipment Blank Pump Equipment Blank-Dredge Samples removed from: Box# Samples removed from: -- Box# Shelf# Shelf# Samples transferred to the custody o f. J!m >9<s q Sample Custodian Initials/Date/Time Samples received from custodian; Samples moved to R fcf 3*2- j^ 6 ~ z l3 lk>2 Laboratory Personnel Initials/Date/Time Samples removed from . g Samples returned to h C / C Q 3 ^ 7 Comments: A ll S W lf i f u i K /ih s Sample Custodian Initials/Date/Time December 19, 2002/6 000041 3058 Research Drive State C ollege, PA 16801 Phone: 814-272-1039 Fax:814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34910 Matrix Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator N o.. OX . , Time r f i t f ) ________ Date A l l - I n 5 CLIENT SAMPLE ED na na na BC2 SW-04 BC2 SW-05 BC2 SW-06 Outfall to River SW-25 BC2 SW-04 BC2 SW-04 BC2 SW-04 Dup BC2 SW-04 Low Spk BC2 SW-04 High Spk BC2 SW-05 BC2 SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk BC2 SW-06 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk BC2 SW-06 High Spk EXYGEN ID NUMBER ' 0106020 Control 0106020 Spk A 0106020 Spk B L34910-1 Spk C L34910-6 Spk D L34910-12 Spk E L34910-16 Spk F L34910-1 L34910-1 Rep L34910-4 L34910-2 L34910-3 L34910-6 L34910-6 Rep L34910-9 L34910-7 L34910-8 L34910-12 L34910-12 Rep L34910-15 L34910-13 L34910-14 VOLUME (mL) 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 FORTIFICATION (ng) - 2.0 20.0 200.0 200.0 200.0 200.0 - - - - 0106020 Spk A 0106020 Spk B L34910-1 Spk C L34910-6 Spk D L34910-12 Spk E L34910-16 Spk F - Spiking Solution Used F061103-2 {10 ng/mL) F061103-1 (100 ng/mL) F060203-2 ( 1000 ng/mL) F060203-2 (1000 ng/mL) F060203-2 (1000 ng/mL) F060203-2 (1000 ng/mL) - Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 2 0 0 pJL (2 0 0 jiL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - Initial/Date p iJ jr tfr ty . /613I a / I 2l ><nb / 6713.1 U t, / 7)5|l W W f a l> F- 1 All samples were measured: Time ! O l O ________ Date anij/aai/aS After measuring samples were returned to refrigerator No. 3 3 ~ Time .llQQ_________ Date Q1P/ &fIoO A Initials J 1 8 L . Initials Comments: 200 pL Of 230 m g/m L sodium thiosulfate was added to all samples before spiking. Initials/Date: l Analysis Summary: Data Set:. DataSet: j D i a j a A L Data Set: CPC&0^>/\ Initials/Date: Initials/Date: Initials/Date: Set extraction/analysis data verified by: July 26, 2001/6 000042 ( RESEARCH 3058 Research Drive State C ollege, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 O O 000043 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34910 MATRIX: Water METHOD: " ANALYTES: PFHS. PFOS. PFOA and PPOSA PROTOCOL NUMBER: NA Client ID na na na BC2 SW-04 BC2 SW-05 BC2SW-06 Outfall to River SW-25 BC2 SW-04 BC2 SW-04 BC2 SW-04 Dup BC2 SW-04 Low Spk BC2 SW-04 High Spk BC2 SW-05 BC2 SW-05 Exygen1D 0106020 Control 0106020 Spk A 0106020 Spk B L34910-1 Spk C L34910-6 Spk D L34910-12 Spk E L34910-16 Spk F L34910-1 L34910-1 Rep L34910-4 L34910-2 L3491-3 L34910-6 L34910-6 Rep STEP 1 STEP 2 Dilutions (mL/mL) - 'V | ,o D-V ,.o O '/..0 'V i . o .-- _ -- STEP 3 1 Dilutions (mL/mL) . -- W M .o - STEP 4 l *Vi .0 >- '/|.D () -- O -V t.o \ f-- - Reagents/ Materials Methanol CIS SPE Type Water ,, Initials/D ate Lot# NA CEE cnl*i,/r*> BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk BC2 SW-06 BC2 SW-06 BC2SW-06 Dup BC2 SW-06 Low Spk BC2 SW-06 High Spk L34910-9 L34910-7 L34910-8 L34910-12 L34910-I2 Rep L34910-15 L34910-13 L34910-14 4f -- O-'/l.O - \j V\Q HPL c - 0 tO/.O Methanol *4 3 0 8 T 3 i - 0 '5/ l . 0 Ammonium Acetate V j^ L iC ;6! - ili% 0 7 t> Type I water \/ V \0 r -----\l -- s NA *Initials/D aSe .- -, - - , 1- c m itV -- f c -- o i s ilo s P h cek S fe A Initials/D ate * r* ** " IV M U u p ^ U U l i U l U ^ w iV n a j l l f STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reaoalysis. Initials and date under each step indicates the personnel that performed this step. b'OJTsW pStiXifiL. l i l W s Tfe\COSb( tsUUTEbSA^Al.FtL.M,f=lCD. .. 3 ()SAM?lWFS FKSHiX blUOTh m {o-'/iD MUmO W 'V ____6_i_M_M*enFAc us%^ U0 W^ A, SET 0>A. $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water j^ o jo tj S COMMENTS: Final extracts stored in r e f r i g e r a t o r I n i t i a l s : /r 7 z Date: July 19, 2001/4 en RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34910 Matrix: Water Sponsor Study/Prolocol No: NA The samples listed below were removed from refrigerator No.. ? 2 - , . Time MID Date n~! 31 05 Initials. Ce M CLIENT SAMPLE ED Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk Field Control/Travel Blank Field Control/Travel Blank Low Spk Field Control/Travel Blank High Spk Equipment Blank-Pump Equipment Blank-Dredge EXYGEN ID NUMBER L34910-16 L3491Q-16 Rep L34910-19 L34910-17 L34910-18 L34910-22 L34910-23 L34910-24 L34910-25 L34910-26 VOLUME (mL) 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 FORTIFICATION (ng) . _ . _ . - - - -. - - -_ - -- - - -. - - -_ - - -- - w- -- -- - - -. -- . - -- - - -- - . . . - Spiking Solution Used - - - Volume Used for Spiking . . . . - Initial/Date . . . - All samples were measured: Time 1020. Date _ c atJis3lt/cm After measuring samples were returned to refrigerator No. 3 2 Time M W ________ Date 0j3lJd3 Initials CEE? cm.Initials Comments: 200 pL o f 250 rag/mL sodium thiosulfate was added to all samples before spiking. loitials/Date: Analysis Summary: Data Set: 6 7 3 |O A ' Data Set: i S S f f i E Data Set: rPirA Iniittiiaallss//DDaatete::, Initials/Date:. Initials/Date:. Set extraction/analysis data verified by:. Date: /03 fly 26, 2001/6 000044 <( ( RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34910 MATRIX: Water METHOD:" ANALYTES: PFHS. PFOS. PFOA and PFOSA PROTOCOL NUMBER: N Client ID Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk Field Control/Travel Blank FieldCowrol/TravdBlank LowSpk Field CnatroVTravel Blank High Spk Equipment Blank-Pump Equipment Blank-Dredge - *lnitials/Date Exygen ID L34910-16 L34910-16Rep L34910-19 L34910-17 L34910-18 L34910-22 L34910-23 L34910-24 L34910-25 L34910-26 - - STEP 1 Nt * - CSf, ifeb STEP 2 Dilutions (raL/mL) _ _ - oVA 0 - a-V,o - Nt - .- --- - ,- - -. --- -._ -- &f , C& i mm I s m STEP Dilutions STEP 3 (mL/mL) 4 <D Ho (0 \/ Reagents/ Materials Methanol C18 SPE Type Water . Lot# f a 114*11A NA _ - * -- , .. . . . \i -- a-- -_ _ -V . -_ -- Inittals/Date Ercnl*iic& ._ .. .. . -- -. . . . _ -._ -_ . HPLC _ - _- Methanol M 50873A - _ _ Ammonium Acctalc - _ . Type I water NA __ J- w&te Initials/Date l/' STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reanalysis. 100^ W tC .w O ) ^ o |6 3 6 3 Initials and date under each step indicates the personnel that performed this Step. $$ Method of Analysis for the Determination of Periluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctauoate (POAA) in Water COMMENTS: Final extracts stored in refrigerator 3 ^ - Initials: $ 3 3 Date: July 19, 2001/4 000045 c( Masslynx - Sample List Sample List: C:VMASSLYNX\Fluoroch :cals.PRO\SampieDB\073103A Decatur BC.SPL Printed: Fri Aug 01 08:36:23 2003 Vial File Name LIMS ID Client ID Sample Description Mat 1 41 073103A-1001 ___ 2 42 073103A-1002 -- 3 43 073103A-1003 -- 4 44 073103A-104 ___ 5 45 073103A-1005 -- 6 46 073103A-1006 -- 7 47 073103A-1007 -- 8 92 Q73103A-1Q08 -- 9 51 073103A-1009 -- 10 52 Q73103A-1010 .___ 11 53 073103A-1011 -- 12 54 0731Q3A-1012 -- 13 55 073103A-1013 -- 14 56 073103A-1014 -- 15 57 073103A-1015 -- 16 42 073103A-1016 -- 17 58 073103A-1017 -- 18 59 073103A-1018 ___ 19 60 073103A-1019 -- 20 61 073103A-1020 -- 21 62 073103A-1021 -- 22 43 073103A-1022 -- 23 63 073103A-1023 -- 24 64 073103A-1024 -- 25 65 073103A-1025 -- 26 66 073103A-1026 -- 27 67 073103A-1027 -- 28 44 073103A-1028 -- 29 68 073103A-1029 -- 30 69 073103A-1030 -- 31 70 073103A-1031 -- 32 71 073103A-1032 -- 33 72 073103A-1033 -- 34 45 073103A-1034 -- 35 73 073103A-1035 -- 36 74 073103A-1036 -- 37 75 073103A-1037 -- 38 76 073103A-1038 -- 39 77 073103A-1039 -- 40 46 073103A-1040 -- 41 78 073103A-1041 -- 42 79 073103A-1042 -- 43 80 073103A-1043 -- 44 81 073103A-1044 -- ___ -- -----___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- TM -- -- -- ... -- -- -- -- -- XC072503-0, 0 ng/L Standard XC072503-1, 25 ng/L Standard XC072503-2, 50 ng/L Standard XC072503-3,100 ng/L Standard -- XCO72503-4, 250 ng/L Standard XC072503-5, 500 ng/L Standard XC072503-6,1000 ng/L Standard Methanol Wash -- 0106020 Control -- 0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/L -- L34910-1 Spk C, 5000 ng/L, DF=10 -- L34910-6 Spk D, 5000 ng/L, DF=10 -- L34910-12 Spk E, 5000 ng/L, DF=10 -- L34910-16 Spk F, 5000 ng/L, DF=10 -- XCQ72503-1, 25 ng/L Standard L34910-1 L34910-1 Rep L34910-4 L34910-2 L34910-3, DF=100 XC072503-2, 50 ng/L Standard L34910-6 L34910-6 Rep -- L34910-9 L34910-7 -- L34910-8, DF=100 XC072503-3,100 ng/L Standard L34910-12 L34910-12 Rep L34910-15 -- L34910-13 L34910-14, DF=100 XC072503-4, 250 ng/L Standard -- L34910-16 L34910-16 Rep L34910-19 L34910-17 L34910-18, DF=100 XC072503-5, 500 ng/L Standard L34910-25 L34910-26 L34910-22 L34910-23 000046 Iw g e n STUDY NO. L S t i m Page 1 Page Position: (1,1) nx Sample Type Cone (ng/L) Cone B Cone C Test ID DF Standard Standard Standard Standard Standard Standard Standard Blank Blank QC QC QC QC QC QC Standard Analyte Analyte Analyte QC QC Standard Analyte Analyte Analyte QC QC Standard Analyte Analyte Analyte QC QC Standard Analyte Analyte Analyte QC QC Standard Analyte Analyte Analyte QC 0 25 50 100 250 500 1000 -- -- 100 500 5000 5000 5000 5000 25 -- -- -- 100 10000 50 -- -- -- 100 10000 100 -- -- -- 100 10000 250 -- -- 100 10000 500 -- -- -- 100 0___ ___ 0-- -- 0-- ___ 0-- ___ 0-- ___ 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- --0 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- ... -- 0 0-- -- 0-- -- 0-- -- 0-- . . . --0 0-- - - 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 0-- -- 1 1 1 1 1 1 1 1 1 1 1 10 10 10 10 1 1 1 1 1 100 1 1 1 1 1 100 1 1 1 1 1 100 1 1 1 1 1 100 1 1 1 1 1 (( Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorocl imicals.PRO\SampleDB\073103A Decatur BC.SPL Printed: Fri Aug 01 08:36:23 2003 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 o 43 44 I* MS Method HPLC Method MS Tune File Inj.Volume C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACtO PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 CB SULF CB ACID PFOSA C6 CB SULF CB ACID PFOSA C6 C8 SULF CB ACID PFOSA C6 C8 SULF CB ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 CB SULF CB ACID PFOSA C6 CB SULF C8 ACID PFOSA CB C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 CB SULF CB ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 CB SULF C8 ACID PFOSA C6 CB SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 CB SULF C8 ACID PFOSA C6 CB SULF CB ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA C6 CB SULF CB ACID PFOSA C6 CB SULF C8 ACID PFOSA C6 CB SULF CB ACID PFOSA C6 CB SULF CB ACID PFOSA C6 CB SULF C8 ACID PFOSA C6 C8 SULF C8 ACID PFOSA pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 Exygen study n o . j f f i f / p ( Page 2 Page Position: (2, 1) C( Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorocl imicals.PRO\SampleDB1D73103A Decatur BC.SPL Printed: Fri Aug 01 08:36:23 2003 J jo i 53______________ Exygen study n o . ( Page 3 Page Position: (1,2) Vial File Name LIMS ID Client ID Sample Description 45 82 073103A-1045 -- 46 47 073103A-1046 -- -- -- L34910-24, DF=100 XCO72503-6.1000 n g /l Standard Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF - QC 10000 -- -- 0 100 -- Standard 1000 ---- 01 00004S t Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroche Printed: Fri Aug 01 08:36:23 2003 Is. PRO\Samp|eDB\073103A Decatur BC.SPL cft|p||o3____________ MS Method HPLC Method MS Tune File Inj.Volume 45 C6 C8 SULF C8 ACID PFOSA 46 C6 C8 SULF C8 ACID PFOSA pfbs water pfbs water Fluorochems 15 Fluorochems 15 000049 Exygerrsnipy no^LtOTp * K Page 4 P age Position: (2,2) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exygen Study No: L34910 Instrument: Computer: Software: Micromass Quattro Ultima (LC/MS/MS Unit #6) COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: HPLC Column: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven Genesis C-8, 5 cm x 2 .1 mm i.d. x 4 p (Exygen ID: 74A ) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 W 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 000050 Scanning Method Report Page 1 Method: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 C8 SULF C8 ACID PFOSA Last Modified: Thu Jul 31 16:23:50 2003 Printed: Fri Aug 01 08:36:30 2003 .16 oi ( > Solvent Delay { mins ) : 0.00 Analog Channel 4 : Unused Function : 1 MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Secs ) : Span { Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 1 2 .00 1 Dwell (Secs) Coll Energy (eV) 1 399.00 80.00 0.20 2 413.00 369.00 0.20 3 498.00 78.00 0.20 4 499.00 99.00 0.20 35 10 30 40 Cone ( V ) 50 10 50 30 000051 Method Report Method File: Last Modified: Printed: c :\masslynx\fluorochemicals.pro\acqudb\pfbs water Friday, August 01, 2003 08:27:00 Friday, August 01, 2003 08:36:39 Paga X HP1100 LC Pump Initial Conditions Solvents A% B% c% D% 90.0 10.0 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 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time 0.00 2.00 5.00 9.00 9.50 14.00 14.50 20.00 A% 90.0 90.0 10.0 10.0 0.0 0.0 90.0 90.0 B% ' 10.0 10.0 90.0 90.0 100.0 100.0 10.0 10.0 C% 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 Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contactl Off On Off Off Off Off Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/il/min) Draw Position (mm) Stop Time (mins) Injection Volume(^1) Vial Number 200.0 200 0.50 20.00 15.0 69 w 0000S 2 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS Printed: Fri Aug 01 08:37:00 2003 Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -21 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.4e- 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 15 2 14.0 14.0 2.0 550 12 14 16 -548 Rdbk 131.4 754.2 000053 Quantify Calibration Report %/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaba Page 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103A Decatur BC Last modified: Sun Aug 03 07:12:46 2003 ,1 . . | Printed: Sun Aug 03 07:19:26 2003 I- 'J Exygen Research, 3058 Research Drive, State College, FA 16801 0000S4 Quantify Calibration Report \m 0 Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 2 Calibration: P:\Data\LCMSMS6\Mas8lynx\Fluorocheraicals.PR0\CurveDB\073103A Decatur BC Last modified: Sun Aug 03 07:12:46 2003 Printed: Sun Aug 03 07:19:26 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000055 Quantify Calibration Report '</ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 3 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103A Decatur BC Last modified: Sun Aug 03 07:12:46 2003 Printed: Sun Aug 03 07:19:26 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000056 Quantify Calibration Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Faga 4 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\CurveDB\073103A Decatur BC Last modified: Sun Aug 03 07:12:46 2003 Printed: Sun Aug 03 07:19:26 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000057 Quantify Sample Report H/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 1 Saiqple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0SSarapleDB\073103A Decatur BC tSun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethUDJXB3\\ JDecatur BC 080103 Sun Aug 03 07:11:59 2003 Initials. Printed: Sun Aug 03 07:19:29 2003 Run# Name: 073103A-1001 Text: 1: C8 Acid (PFOA) Exygen Research, 3058 Research Drive, State College, PA 16801 000058 Quantify Sample Report %ml0 Study No.:L34910, Set No. :073103A, East.Date:07/31/03, Analyst:K.Risha Paga 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1001 Text : 4: PFOSA w Exygen Research 3058 Research Drive, State College, PA 16801 000059 Quantify Sample Report Sm? Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 030103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1002 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000060 Quantify Sample Report V Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Rsha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1002 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000061 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicala.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1003 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000062 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, AnalystsK.Risha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochomicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1003 Text: 4: PFOSA w Exygen Research, 3058 Research Drive, State College, PA 16801 000063 Quantify Sample Report \ ^ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Harne: 073103A-1004 Text: 1: C8 Acid (PFOA) XC072503-3,100 ng/L Standard 073103A-1004 Sm (Mn, 2x3) 1 0 0 -] %: 9.15 29438 01-Aug-2003 10:29:31 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.81e5 Area 0 't I 1 1" T " ^ 1" ' I 1 ' 1 I I I 1 I 1 2.00 4.00 2: C6 Sulfonate (PFHS) 6.00 1 I ' ">' r ' ~ 8.00 I r l' io 7 o o r-r-i Time 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000064 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 8 Sample List: P:\Data\LCMSMS6\Masslynx\Kluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1004 Text : 4: PFOSA XC072503-3,100 ng/L Standard, 073103A-1004 Sm (Mn, 2x3) 1 0 0 -, %- 0 2.00 01-Aug-2003 10:29:31 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 13321 498 > 78 7.20e4 Area 1 T T"T-"|"-I 1 I Time 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000065 Quantify Sample Report \ S t u d y No-:L34910, Set Nb.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Marne: 073103A-1005 Text: 1: C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 073103A-1005 Sm (Mn, 2x3) ' 100"] %: 01-Aug-2003 10:51:16 LC/MS/MS #6 9.15 MRM of 4 Channels ES413 >369 4.06e5 Area 2.00 4.00 6L00 8.00 ..... I I I ' I Tim e 10.00 12.00 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103A-1005 Sm (Mn, 2x3) 100n %- 01-Aug-2003 10:51:16 LC/MS/MS #6 [18.99 131371 MRM of 4 Channels ES399 > 80 8.10e4 Area 0 - " r ' ' 1_T .......... | --'- ' I l I <r --I-- ! I i-- r- 1- r - r i 1, t -t- 'i- T......... T .... ............ 2.00 4.00 6.00 8.00 3: C8 Sulfonate (PFOS) 1 ' 1 1 - f ' * ' ri Tim 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000066 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 10 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCHSMS6\Masslyzuc\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1005 Text: 4 : PFOSA XC072503-4, 250 ng/L Standard 073103A -1005 Sm (Mn, 2x3) 100-1 %: 01-Aug-2003 10:51:16 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1.69e5 Area 0 11 1i 1111i 1111i 11' ' i 1 2.00 4.00 'T-- r "r 6.00 8.00 10.00 ' r Ti me 12. Bxygen Research, 3058 Research Drive, State College, PA 16801 000067 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1006 Text: 1: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 073103A-1006 Sm (Mn, 2x3) 10CH 9.13 142891 01-Aug-2003 11:12:56 LC/MS/MS #6 MRM of 4 Channels ES413 >369 8.51 e5 Area 2.00 2: C6 Sulfonate (PFHS) 4.00 6.00 8.00 10.00 T im e 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000068 Quantify Sample Report \ ^ f Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSHS6\Masslyiuc\7luorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1006 Text: 4: PFOSA w Exygen Research, 3058 Research Drive, State College, PA 16801 000069 Quantify Sample Report Hi/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1007 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 073103A-1007 Sm (Mn, 2x3) 100-1 8.97 51345 01-Aug-2003 11:34:42 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 3.14e5 Area 2.00 3: C8 Sulfonate (PFOS) 4.00 6.00 8.00 10.00 T im e 12.00 %0 Exygen Research, 3058 Research Drive, State College, PA 16801 000070 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst :K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1007 Text: 4: PFOSA w Exygen Research, 3058 Research Drive, State College, PA 16801 000071 Quantify Sample Report 1/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, AnalystK.Risha Faga 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1008 Text: 2: C6 Sulfonate (PFHS) Exygen Research, 3058 Research Drive, State College, PA 16801 000072 Quantify Sample Report V^ 0 Study No . :1.34910, Set No.:073103A, Ext.Date:07/31/03, AnalystsK.Risha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PKO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1008 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000073 Quantify Sample Report X trif Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 17 Sample List: P:\Data\IjCMSMS6\Masslynac\Pluorocheiiiicals.PR0\SanpleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1009 Text: 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000074 Quantify Sample Report W 1 Study No.:L34910, Set No .j073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1009 Text: w Exygen Research, 3058 Research Drive, State College, PA 16801 000075 Quantify Sample Report ' W Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Rlaha Paffe 19 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 ama: 073103A-1010 Text: 1: C8 Acid (PFOA) Exygen Research, 3058 Research Drive, State College, PA 16801 000076 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1010 Text : 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000077 Quantify Sample Report W Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Paga 21 Sample List: P:\Data\LCMSMS6\Masslynx\71uorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1011 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) 0106020 Spk B, 500 ng/L 073103A-1011 Sm (Mn, 2x3) 100^ %: 0 1T I r I T- l ' r I . T I I I I I I I I , 2.00 4.00 IT I I I 6.00 01-Aug-2003 13:01:43 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 8.83e4 Area --r T" i ' i t-|.........-- r | Tim e 10.00 12.00 Exygen Research, 3058 Research Drive, State College, FA 16801 000078 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha paga 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Mama: 073103A-1011 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 00007 Quantify Sample Report Study No.:L34910, Set N o .:073103A, Ext.Date:07/31/03, AnalystjK.Risba Page 23 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemical8.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSHS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Hama: 073103A-1012 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000080 Quantify Sample Report W Study No.: 1.34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMSS\Masslynx\Fluorochemicals.PRO\MethDB\Dacatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1012 Text : 4 : PFOSA L34910-1 S pkC , 5000 ng/L, DF=10 073103A-1012 Sm (Mn, 2x3) 100i %: 01-Aug-2003 13:23:31 LC/MS/MS #6 MRM of 4 Channels ES- 9.92 498 > 78 4.01 e5 Area 0 I ........ I I r I I I 1 1 1 1 r ' 2.00 4.00 6.00 8.00 I H .. ' 10.00 -r-i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000081 Quantify Sample Report Study N o . :1.34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS6\Masslynx\71uorocheinicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1013 Text: 1: C8 Acid (PFOA) L34910-6 Spk D, 5000 ng/L, DF=10 073103A-1013 Sm (Mn, 2x3) 10Q- %- 9.13 1458721 01-Aug-2003 13:45:17 LC/MS/MS #6 MRM of 4 Channels ES413 >369 8.79e5 Area Ch r V 1 'T ~ i-.-I-'I r-' ' 1 ' I ' ' ' - ' I '1' ' ' I-' ' I 1T"*r | i 1i r 1v y r r - T T - ^ ^ `r "`i 1 ) ' 1 i i i ' I Time __________________ 2 X 0 ___________ 4X10___________ 6 X 0 ___________ 8 X 0 ___________ 1 0X 0 __________ 12X 0 W 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0000S2 Quantify Sample Report Study No.:L34910, Set No.;Q731Q3A, Ext.Date;07/31/03, Analyst:K.Risha Page 26 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1013 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000083 Quantify Sample Report i*/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 27 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1014 Text: 1: C8 Acid (PFOA) L34910-12 Spk E, 5000 ng/L, DF=10 073103A-1014 Sm (Mn, 2x3) 1 0 0 -, 9.14 418651 01-Aug-2003 14:07:06 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.49e6 Area r 111I 2.00 2: C6 Sulfonate (PFHS) 4.00 6.00 Time 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-12 Spk E, 5000 ng/L, DF=10 073103A-1014 Sm (Mn, 2x3) 10(h %- 0 -^ -T ~r'T ''' 1' 2.00 - T -I"" '.. 4.00 - j -- r - r -T*"T " [ ""T " 6.00 9.24 96754 01-Aug-2003 14:07:06 LC/MS/MS #6 MRM o f 4 Channels ES499 > 99 5.61e5 Area -T -p -r- 8.00 T r-fT r 10.00 Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000084 Quantify Sample Report / Study N o .:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst :K.Risha Page 28 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LOISMS6\Masslynx\Fluorocheniicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1014 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000085 Quantify Sample Report ^11*/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 29 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Marne: 073103A-1015 Text: 1: C8 Acid (PFOA) C6 Sulfonate {PFHS) L34910-16 Spk F, 5000 ng/L, DF=10 073103A-1015 Sm (Mn, 2x3) 10CH %- 0 i i i I 1 I 1 ' I 2.00 4.00 6.00 3: C8 Sulfonate (PF0S L34910-16 Spk F, 5000 ng/L, DF=10 073103A-1015 Sm (Mn, 2x3) 100-] %: --i--i--i--p i--i--I--i--;--I--I--r--i--I--i--I--i--I--I--`--r-1--I--I--i--i--I--t--i--r--i--r 2.00 4.00 6.00 01-Aug-2003 14:28: LC/MS/MS #6 8.98 MRM of 4 Channels ES399 > 80 3.61 e5 Area 'T 8.00 '~i 1 1 ' ......... * ' r ) Tim e 10.00 12.00 9.25 120697 01-Aug-2003 14:28:57 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 6.80e5 Area T 8.00 --'"t ** i--' I T~r-t t 1 1; Time 10.00 12.00 Ei^ygen Research, 3058 Research Drive, State College, PA 16801 000086 Quantify Sample Report Study No.:L34910, Set N o . :073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 30 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1015 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000087 Quantify Sample Report f Study No.:L34910, Set No.:073103A, Kxt.Date;07/31/03, Analyst:K.Risha Page 31 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1016 Text: 1: C8 Acid (PFOA) ^nb/ 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000088 Quantify Sample Report X S Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 32 Sample List: P:\Data\LCMSMS6\Ma8slyinc\Fluorocheniicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1016 Text : 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000089 Quantify Sample Report Study No.:L34910, Set No.-.073103A, Ext .Date:07/31/03, Analyst:K.Risha Page 33 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1017 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) L34910-1 073103A-1017 Sm (Mn, 2x3) 100n %: 01-Aug-2003 15:12:28 LC/MS/MS #6 . MRM of 4 Channels ES- 8.99 399 > 80 501621 3.04e5 Area i o1 ' ' 1 ' 1 ' 1 1 1 i ' 1 ' 1 1 1 ' ' ' 1 ' -- ............ ... ' i 1-- t --i I r-i i i | i i i i Tim 2.00___________ 4.00 6.00___________ a o o ___________ 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-1 073103A-1017 Sm (Mn, 2x3) 10^ 01-Aug-2003 15:12:28 LC/MS/MS #6 1I9.25 2801831 MRM of 4 Channels ES499 > 99 1.61e6 Area 0 - ' i r~1 1-111 1 1 1 i ...... T"'i 1 1 i ' 1 -, ,--, ", ~T-- T--1--, , . . ' i1 2.00__________ 4^00__________ & 00__________ L00_______ 10.00 t ' ' 1 ' i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000090 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date-.07/31/Q3, Analyst-.K.Risha Paga 34 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SaiapleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Mama: 073103A-1017 Text: 4 : PFOSA L34910-1 073103A-1017 Sm (Mn, 2x3) 100- %- 01-Aug-2003 15:12:28 LC/MS/MS #6 MRM of 4 Channels ES- 9-90 498 > 78 1481091 7.51e5 1 Area 0- .... i 1 1 1i 2.00 i 11 i 1 1<-' i '-1" 1' T ' . -i--i ! i--r-i r-p-i i -r i | i i i i ' i i i i ! i Time 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000091 Quantify Sample Report Study No. .-L34910, Set No.:073103A, Ext .Date: 07/31/03, Analyst sK.Risha Page 35 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSHS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1018 Text: L34910-1 Rep 073103A-1018 Sm (Mn, 2x3) 100n %: 0 - ' ' I ' ' ' 1 I 1 1 1 1 I 1 1 1 " I 1 1 1 r T 1 1 1 ,~ r ~r 4.00 6.00 w 9.26 274170 01 -Aug -2003 15:34:18 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.56e6 Area 8.00 -I T r I ! r I I I I T I Tim e 10.00 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 000092 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 36 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1018 Text: 4 : PFOSA L.34910-1 Rep 073103A-1018 Sm (Mn, 2x3) 100] %- 01-Aug-2003 15:34:18 LC/MS/MS #6 MRM of 4 Channels ES- 9-90 498 >78 143575 1 7.30e5 Area 0 1 1I 111' ! ' ' ' I ' ' 11I 1 2.00 4.00 6.00 8.00 10.00 T im e 12.00 Zxygen Research, 3058 Research Drive, State College, PA 16801 000093 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 37 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1Q19 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000094 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 38 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1019 Text : 4 : PFOSA L34910-4 073103A-1019 Sm (Mn, 2x3) lo o n %- 01-Aug-2003 15:56:09 LC/MS/MS #6 MRM of 4 Channels ES498 > 78 5.46e5 Area 0 ............... ................i 1 1 '" ' " i " I 1 1 i 1 1 2.00 4.00 6^00 8.00 10.00 -T-i Tim e 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000095 Quantify Sanqple Report ^ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 39 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SarapleDB\Q73103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sim Aug 03 07:19:29 2003 Name: 073103A-1020 Text: 1: C8 Acid (PFOA) L34910-2 073103A-1020 Sm (Mn, 2x3) 100] %: 9.13 6056301 1 01-Aug-2003 16:17:55 LC/MS/MS #6 MRM of 4 Channels ES413 > 3 6 9 3.49e6 Area Ch 1 1 1 1 i *" 1 1 1 i * t~1 1 i 1 1 1 1 i 1 1 1 ' 1i .... ' 1 i ' ' ' ................ ... ` 1 ' 1 *r ~i 1 i 1 1 i ' ' ' ' I T im e ___________________ZOO___________ 41)0___________ 6X10___________ Z 0 0 ___________ 10.00__________ 12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-2 073103A-1020 Sm (Mn, 2x3) 100- %- 0- 1 ' ' | 1-- <-- -- r -| i ' i | 2.00 I' -T" r-|..... . 4.00 6.00 9.27 1916311 1 1 01-Aug-2003 16:17:55 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.08e6 Area 8.00 ' [' ....... 1 I ......... ... T im e 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000096 Quantify Sample Report Study No.SL34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 40 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1020 Text : 4 : PFOSA L34910-2 073103A-1020 Sm (Mn, 2x3) 100] %- . 01 -Aug-2003 16:17:55 LC/MS/MS #6 MRM of 4 Channels ES498 > 78 4.67e5 Area 0 ' ................ > i i | 2.00 III|II|i 4.00 6.00 8.00 10.00 -T-i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000097 Quantify Sample Report Study No.:L34910, Sat No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 41 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1021 Text : 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000098 Quantify Sempia Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Pape 42 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1021 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000099 Quantify Sample Report \ ^ 0 Study No.:L34910, Set No.:073103A, Ext.Data:07/31/03, Analyst:K.Risha Page 43 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Mama: 073103A-1022 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000100 Quantify Sample Report Study No.:L34910, Set No.s073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 44 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1022 Text: 4: PFOSA Exygen Research 3058 Research Drive, State College, PA 16801 OOOlOl Quantify Sample Report Study No.:L34910, Sat No. :073103A, Ext.Date:07/31/03, AnalystsK.Risha Paga IS Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1023 Text: 1: C8 Acid (PFOA) L34910-6 073103A-1023 Sm (Mn, 2x3) inn-, %- 9.14 1738711 1 01 -Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 Channels ES- 413 >369 1.01e6 Area <h 1 1 1 1 r p^ - ' 1-| v11-r--l " 1 ' r-! ! 1-1 1 r i i ' ' ' F 1 1 ' ' 1 1 1 1 > TM *r ' 1 1 i 1 i|i"' i 1 1 1 1 i Tim e __________________ ZOO___________ 4 j00___________ 6,00___________ 8JOO___________ 10.00__________ 12.00 V tS 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) %0 Exyyen Research, 3058 Research Drive, State College, PA 16801 000102 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 46 Sample List: P:\Data\LCMSMS6\Masslynx\Kluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 . Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1023 Text : 4 : PFOSA L34910-6 073103A-1023 Sm (Mn, 2x3) 100~i %- 01-Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 Channels ES- 9.88 19711 498 > 78 1.01e5 Area 0 -i-i Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000103 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 47 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1024 Text: 1: C8 Acid (PFOA) L34S 10-6 Rep 0731 33A -1024 Sm (Mn, 2x3) 10(h] %: 0 0 CO 01-Aug-2003 17:45:07 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.07e6 Area A - 1 . . 1 , T 1 . . , 1 1 1 j 1 * 1 - i TM1 1 1 r 1 2.00 4.00 6.00 1 8.00 "r ' ' 1 1" 1 I ' 1 1 1 Tim e ' 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-6 Rep 073103A-1024 Sm (Mn, 2x3) 100n %: 0 `-T'l-!"I--] , I I I I I I ' I""I I ! r-l- 2.00 4.00 6.00 01-Aug-2003 17:45:07 LC/MS/MS #6 9.25 MRM of 4 Channels ES499 > 99 2.62e5 Area '..v - p r i - r - r 8.00 ' F 1' 10.00 I ...... ' I Tim e 12.00 Sxygen Research, 3058 Research Drive, State College, PA 16801 000104 Quantify Sample Report Study No.SL34910, Set N o .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 48 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sim Aug 03 07:19:29 2003 Name: 073103A-1024 Text: 4: PFOSA L34910-6 Rep 073103A-1024 Sm (Mn, 2x3) 100n %: 01-Aug-2003 17:45:07 LC/MS/MS #6 MRM of Channels ES- 9.90 498 > 78 1.01e5 Area 0 1 n 1 ri I I . 1 ! ! I-I-1 ! I I"it "I I--r 1 : n " 2.00 4.00 6.00 V 8.00 10.00 T T -n Time 12.00 Bxygen Research, 3058 Research Drive, State College, PA 16801 000105 Quantify Sample Report Study No.SL34910, Set No.:073103A, Ext.Data:Q7/31/03, AnalystsX.Riaha Page 49 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\MaBSlynx\Fluorocheniicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1025 Text: 1: C8 Acid (PFOA) L34910-9 073103A-1025 Sm {Mn, 2x3) 10Ch %-J 9.13 355190 01-Aug-2003 18:06:53 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.13e6 . Area 1 "I ' 1 I 1 io!oo2.00 4.00 6.00 8.00 i Time 12.00 2 : C6 Sulfonate (PFHS) L34910-9 073103A-1025 Sm (Mn, 2x3) 100n %: 01-Aug-2003 18:06:53 LC/MS/MS #6 MRM of 4 Channels ES8.99 399 > 80 1.26e5 Area o T 1 I 'T I I I ,-r 2.00 3: C8 Sulfonate (PFOS) 4.00 T -r-r 6.00 8.00 - '- - I - ' 1-'-.... 10.00 -r '- 'i I Time 12.00 Bxygen Research, 3058 Research Drive, State College, PA 16801 000106 Quantify Sample Report Study No.:L34910, Sat No.:073103A, Ext.Date:07/31/03, Analyst:1C.Risha Page 50 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1025 Text: 4: PFOSA ^0 Exygen Research, 3058 Research Drive, State College, PA 16801 000107 Quantify Sample Report Study N o .:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 51 Sample List: P :\Data\LCMSMS6\Masslynx\S'luorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P :\Data\LCMSMS6\Masslynx\Fluorochemicals,PRO\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1026 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L 3 4 9 1 0 -7 073103A-1026 Sm (Mn, 2x3) 100- %- 9.26 1490881 01-A u g -2 0 0 3 18:28:44 LC /M S /M S #6 MRM of 4 Channels ES- 499 > 99 8.38e5 Area 0: . >, r r --T-- . i " . k - i i - r- r - r - r ~i T im e i i r T " r " | " i i i...t- t t ; ...................... i "i i i |- t--t i i..| r - r r -- r T ^ ^ ii ti 2.00___________ 4/30___________ 6,00___________ i00___________ 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000108 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Oate:07/31/03, Analyst:K.Risha Page 52 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1026 Text: 4 : PFOSA L34910-7 073103A-1026 Sm (Mn, 2x3) 10 0 --i 01-Aug-2003 18:28:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.92 498 > 78 670311 3.44e5 Area 2.00 4.00 i '' 1 ' ''' i 1' 6.00 8.00 10.00 ~i r -i Tim e 12.00 E^ygen Research, 3058 Research Drive, State College, PA 16801 000109 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 53 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRQ\SajnpleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslyme\Fluorochemicals.FRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1027 Text: 1: C8 Acid (PFOA) L34910-8, DF=100 073103A-1027 Sm (Mn, 2x3) 100-1 %: 9-13 215961 1 01-Aug-2003 18:50:30 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.32e5 Area Ch-T -, . . " p > -T " ` 1 f I ' - ' i " ' 1~i ~ r 1" 1--'1 T 1 1 1 T 1 1 1 i r | - | i - ' i . ' 1 ' . . P ' 1 h 1 1 i t i - I T im e 2.00__________40__________ 6,00__________8.00 10.00 12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 18801 000110 Quantify Sample Report 1^ / Study No.:L34910, Set N o .:073103A, Ext.Date:07/31/Q3, Analyst:K.Risha Page 54 Sample List: P:\Data\LCMSMS6\Masslynjc\Fluorochemicals.PR0\SamgpleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslyrue\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1027 Text: 4 : PFOSA w Exygen Research, 3058 Research Drive, State College, PA 16801 000111 Quantify Sample Report 'll Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 55 Sample List: P:\Data\LCMSMS6\Masslymc\Fluoroclieniicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslyiuc\Fluorochemicals.PRQ\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1028 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000112 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Fags 56 Sample List: F:\Data\LCMSMS6\Masslynx\7luorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\71uorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1028 Text: 4 : PFOSA XC072503-3,100 ng/L Standard 073103A-1028 Sm (Mn, 2x3) 100i %- 01-Aug-2003 19:12:20 LC/MS/MS #6 MRM of 4 Channels ES- 9-90 _ 498 > 78 139891 7.45e4 Area T ' "1 ' ~ > m I"r " 2.00 4.00 -r r i I l i I 'I ' 1 1 6.00 8.00 T*110.00 Time 12.00 w Exygen Research/ 3058 Research Drive, State College, FA 16801 000113 Quantify Sample Report '* Study No.:L34910, Set No.;G73103A, Ext.Dates07/31/03/ Analyst:K.Risha Page 57 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslyiut\Pluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1029 Text: 1: C8 Acid (PFOA) L34910-12 073103A-1029 Sm (Mn, 2x3) 100-1 %- 9.14 2471389 01-Aug-2003 19:34:03 LC/MS/MS #6 MRM of 4 Channels ES413 > 3 69 1.47e7 Area 0 1 1 1 I 1 1 ' ' I ' -'""1.. . 1 '"I ' 111 ' r'I " 2.00 4.00 6.00 2: C6 Sulfonate (PFHS) 8.00 -1" I 1 ' t I ' ' ' I Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000114 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, AnalystsK.Risha Page 58 Sample List: P:\Data\LCMSMS6\Masslyux\Fluorochanicals.PR0\SamplaDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1029 Text: 4 : PFOSA W Exygen Research, 3058 Research Drive, State Collage, PA 1S801 000115 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:X.Risha Page 59 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1030 Text: 1: C8 Acid (PFOA) L34910-12 Rep 073103A-1030 Sm (Mn, 2x3) 100-] %: 01-Aug-2003 19:55:50 LC/MS/MS #6 119.11 24251891 MRM of 4 Channels ES413 >369 1.43e7 Area (y ' 1 I { t t -i 1 1 1 1 r-r 1-- 1 .' T ' 1 ' 1 1 ' 1 1 1 1 1 1 1^ `T' 1 1 1 ................ Tim e __________________ 2 X 0 ___________ 4X10___________ 6 X 0 ___________ 8 X 0 ___________ 1 0X 0 __________ 12X 0 2: C6 Sulfonate (PFHS)_________________________________________________ L34910-12 Rep 01-Aug-2003 19:55:50 LC/MS/MS #6 073103A-1030 Sm (Mn, 2x3) 100^ 8.98 2376491 I MRM of 4 Channels ES399 > 80 1.45e6 Area %- [ o1 ......... ............. I |,">l 1 1T f 2X0 4X0 r" ", t ' "1"' 1" 6X0 ' ! i '` - I ' M ' 8X0 10X0 ................ 1 Tim e 12X0 3: C8 Sulfonate (PFOS) L34910-12 Rep 073103A-1030 Sm (Mn, 2x3) 100n %: 9.24 571211 01 -Aug -2003 19:55:50 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.17e6 Area O -t-T I - 1 - 1 [ T - I - ! - I- ' T " I T - I -- I I I I I I I 1 I " 2X0 4X0 I 1 -I-- I 6X0 8X0 I .......... I ' ' ' ' [ Tim e 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000116 Quantify Sample Report '*/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 60 Sample List: P:\Data\LCMSMS6\Hasslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1030 Text : 4 : PFOSA L34910-12 Rep 073103A-1030 Sm (Mn, 2x3) 100-1 %- 01-Aug-2003 19:55:50 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 263411 1.32e6 Area 0- -, T~r -r- r , | Time 2.00 4.00 6.00 8.00 10.00 12.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 000117 Quantify Sample Report '*/ Study No.:L34910, Sat No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 61 Sample Lists P:\Data\LCMSMS6\Masslyiut\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LaMSMS6\Masslynx\yiuorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Sun Aug 03 07:19:29 2003 Mama: 073103A-1031 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, FA 16801 000118 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, AnalystsK.Risha Page 62 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1031 Text: 4: PFOSA L34910-15 0 73 1 03A -1031 Sm (M n, 2x3) 100: %: A- ' i ' ' ' ' i ' i ! I 1 1 1 1 1 1 2.00 4.00 01-Aug-2003 20:17:38 LC/MS/MS #6 MRM of 4 Channels ES- 9 90 498 > 78 27613 4 l 1 39e0 1 Area ' r 1 '' ' 1 i--i rT ,| , i 1 i i ...! i i i i i i i i i i TTim e 6.00 8.00 10.00 12.00 Bxygen Research, 3058 Research Drive, State College, PA 16801 000119 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 63 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\71uorochamicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1032 Text: 1: C8 Acid (PFQA.) L34910-13 073103A-1032 Sm (Mn, 2x3) -inn-, %- 9.11 28498701 l 1 01-Aug-2003 20:39:25 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.69e7 Area 0- 'r "1 ' T 'l 1 1 1 1 1 '..I'"1 ' I ' | i ' r- i | i-i r-1' T-|' l-T-1 l"|' 1 'T " i i ' 1 i 1 1 1~i" i 1 1--1-- 1 i Time __________________ 2/30___________ 4,00___________ 6 ^ 0 ___________ L00___________ 10.00__________ 12.00 ' W 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-13 073103A-1032 Sm (Mn, 2x3) 100-, %- 0*^ i "I ' ' i ' ' ' ' i ' I W 2.00 i1 4.00 T-J-T6.00 9.24 667186 01-Aug-2003 20:39:25 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.69e6 Area 8.00 .i-r t "t -,..... . i I -| Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000120 Quantify Sample Report Study No.:L34910, Set No.073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 64 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC Q80103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1032 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000121 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Pago 65 Sanale List: P:\Data\LCHSHS6\Hasslynx\Pluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1033 Text : 1: C8 Acid (PFOA) L34910-14, DF=100 073103A-1033 Sm (Mn, 2x3) 100n %- 01-A u g -2 0 0 3 21:00:58 L C /M S /M S #6 |19.12 712941 MRM of 4 Channels ES413 >369 4.14e5 Area 0- ^ 1 1 1T*1. 1 f r 1 1 1 1 i 11 r 1 1 i '-- '-- t--1 1 1 1 ' ' I 1 |M1 1 l 1 1 ' 1 ^ ' i ' ' i 1' ................ Tim e ___________________2,00___________ 4 j00___________ a 0 0 ___________ 8J00___________ 10.00 ________ 12.00 W 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34S 10-14, DF=100 0731 D3A-1033 Sm (Mn, 2x3) 100-; %- 9.24 149811 01-Aug-2003 21:00:58 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 8.40e4 Area ^ 1 1 1................... 2.00 1 ' 1 1 ' ' 1 1 1 ' 1 1 1".. . 1"H 4.00 6.00 1i i i i i i 8.00 I i i | i I I i I < 1 ] l Kilt; 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000122 Quantify Sample Report Study No.:L3491Q, Set No.:073103a , Ext.Date;07/31/Q3, Analyst:K.Risha Page 66 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluarochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1033 Text : 4: PFOSA w Exygen Research 3058 Research Drive, State College, PA 18801 000123 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst-.K.Risha Page 67 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\Q73103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masalynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1034 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103A-1034 Sm (Mn, 2x3) 100n %H 0 2.00 3: C8 Sulfonate (PFOS) 4.00 6.00 8.98 14198 01-Aug-2003 21:22:34 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 8.49e4 Area 8.00 10.00 -"-i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000124 Quantify Sample Report Study No.:L3491Q, Set No.:073103A, Ext.Data:07/31/03, Analyst:K.Hisha Page 68 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheinicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1034 Text : 4: PF0SA w Exygen Research, 3058 Research Drive, State College, PA 16801 000125 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:X.Risha Page 69 Sample List: P:\Data\LC3MSMS6\Masslynx\Pluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1035 Text: 1: C8 Acid (PFOA) W 2: C6 Sulfonate (PFHS) L34910-16 073103A-1035 Sm (Mn, 2x3) 100n %- 0 i 1 1 1 i i-1 111 ' i ' 2.00 4.00 3: C8 Sulfonate (PFOS) L34910-16 0 7 3 103A-1035 Sm (Mn, 2x3) 1 0 0 -] %- 0 2.00 4.00 6.00 6J00 8.98 283517 01-Aug-2003 21:44: LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.74e6 Area 8.00 1 1 1 ' '"i 1 ! 1 i Time 10.00 12.00 9.24 691166 01-Aug-2003 21:44:25 LC/MS/WIS #6 MRM of 4 Channels ES499 > 99 3.86e6 Area 8.00 ~f" r * '' T 1 ' ' i Tim e 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000126 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 7O Sample List: P:\Data\LCHSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1035 Text: 4: PFOSA Exygen Research 3058 Research Drive, State College, PA 16801 000127 Quantify Sample Report X m j Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 71 Sample List: F:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1036 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) L34910-16 Rep 073103A-1036 Sm (Mn, 2x3) nr\_ %- 02.00 3: C8 Sulfonate (PFOS) L34910-16 Rep 073103A-1036 Sm (Mn, 2x3) lOCh %- 4.00 8.98 |3025301 I 01-Aug-2003 22:06:04 LC/MS/MS #6 MRM of 4 Channels ES- 399 > 80 1.79e6 Area 1 ' r''" ' ' r i 1 ^ ' f 1 1 i 1 1 i ' '-i Time 6.00___________ 8^00___________ 10.00__________ 12.00 9-25 7072701 I 01-Aug-2003 22:06:04 LC/MS/MS #6 MRM of 4 Channels ES499 >99 3.94e6 Area 0- 1-1" 1' ' i 1 1 1 1 i 1 1 r"' i 1 1 1 1 i 1^ ' 1"t 11r ' ' i - i "'-1 i i i i i i i i-- i-- r-- 2.00 4.00 6.00 8.00 1 ' i ' i1 i i 1- - '" 1 r~i Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000128 Quantify Sample Report Ve/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 72 Sample List: P:\Data\LCMSMS6\Masslynx\Fluoracheinicals.PRO\SainplaDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicais.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 dob Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1036 Text: 4: PF0SA %0 Exygen Research 3058 Research Drive, State College, PA 16801 000129 Quantify Sample Report 'le^ Study NO. 1.34910, Set No.:073103A, Ext .Date: 07/31/03, Analyst sK.Risha Page 73 Sample List; P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1037 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000130 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 74 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SarapleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1037 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 00131 Quantify Sample Report Study No.: 1,34910, Set N o .:073103A, Ext.Date:07/31/03, AnalystsK.Risha Page 75 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1038 Text: 1: C8 Acid (PFOA) L34910-17 073103A-1038 Sm (Mn, 2x3) 100-, %- 9.12 3102823 01-Aug-2003 22:49:40 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.85e7 Area 2.00 V e / 2: C6 Sulfonate (PFHS) t I T" 1 t4.00 6.00 8.00 10.00 T im e 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000132 Quantify Sample Report W Study No.:L34910, Set N o .:073103A, Ext.Date:07/31/03, AnalystsK.Risha Page 76 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MetUDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1038 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000133 Quantify Sample Report V Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 77 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1039 Text : 1: C8 Acid (PFOA) 2 : C6 Sulfonate (PFHS) L34910-18, DF=100 073103A-1039 Sm (Mn, 2x3) 100n %- 0 ^ ... I 1~r"ri ,f~1 1 r 111 '11 I ' 2.00 4.00 3: C8 Sulfonate (PFOS) L34910-18, DF=100 073103A-1039 Sm (Mn, 2x3) 100^ %- o- 2.00 4.00 ' I 11 6.00 6.00 01-Aug-2003 23:11:32 LC/MS/MS #6 8.96 MRM of 4 Channels ES399 > 80 6.07e4 Area 8.00 T ' ' ' I ........ I Time 10.00 12.00 9.26 140721 I 01-Aug-2003 23:11:32 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 8.21 e4 Area 1 8.00 s i , i 1 1 t '| 1 T -i-T 'i Tim e 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000134 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Dates 07/31/03, AnalystsX.Risha Page 78 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1039 Text: 4: PFOSA L34910-18, DF=100 073103A-1039 Sm (Mn, 2x3) 100-1 01-Aug-2003 23:11:32 LC/MS/MS #6 MRM of 4 Channels ES- 9-90 498 > 78 12191 i 6.51 e4 Area 2.00 i I r I t I i-- r r - T - T - r 4.00 6.00 8.00 10.00 Time 12.00 W %*0 Exygen Research, 3058 Research Drive, State College, PA 16801 000135 Quantify Sample Report 11**/ Study No. :L34910, Set N o .:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 79 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1040 Text: 1: C8 Acid (PFOA) H*/ 2: C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 073103A-1040 Sm (Mn, 2x3) 100n %- 0 i 1 1 i i 1 1 | - ' ..' i i | ' ' i i | i 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) 01-Aug-2003 23:33: LC/MS/MS #6 8.98 MRM of 4 Channels ES399 > 80 1.78e5 Area 8.00 1 I ' ' 1 1 I 1 1 1 ` I Time 10.00 12. Exygen Research, 3058 Research Drive, State College, PA 16801 000136 Quantify Sample Report \^0 Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page BO Sample List: P:\Data\LCMSHS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1040 Text : 4: PFOSA XC072503-5, 500 ng/L Standard 073103A-1040 Sm (Mn, 2x3) 100-] %- 01-Aug-2003 23:33:24 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 72430 3.86e5 Area 0W 11I1111I1 2.00 4.00 6.00 8.00 10.00 Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000137 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, AnalystjK.Risha Rage 81 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1041 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) Exygen Research, 3058 Research Drive, State College, PA 16801 000138 Quantify Sample Report x ^ / Study No.:L34910, Set No.:073103A, Ext.Date:07/31/Q3, Analyst:K.Risha Page 82 Sample List: P:\Data\LCMSMS6\Masslynx\Kluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1041 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000139 Quantify Sample Report ^ 0 Study No.:L34910, Set No.:073103A, Ext.Date:07/31/Q3, Analyst:K.Risha Page 83 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1042 Text: 1: C8 Acid (PFOA) W r 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000140 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 84 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1042 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000141 Quantify Sample Report w Study No. .-L34910, Set N o .:073103A, Ext .Date :07/31/03, Analyst :K.Risha Page 85 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code : Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1043 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000142 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst .'K.Risha Page 86 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1043 Text: Exygsn Research, 3058 Research Drive, State College, PA 16801 000143 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 87 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1044 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate {PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000144 Quantify Sample Report \m0 Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 88 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SainpleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1044 Text : 4: PFOSA L34910-23 073103A -1044 Sm (Mn, 2x3) 10CH %- 02-Aug-2003 01:00:38 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 1214C 6.45e4 Area 6.00 I I { T 'T ' I "T 8.00 10.00 T im e 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000145 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Dato:Q7/31/03, Analyst:K.Riaha Page 89 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslymc\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1045 Text: 1: C8 Acid (PFOA) 2: CG Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000146 Quantify Sample Report Study No.:L34910, Set No.:073103A, East.Dates 07/31/03, Analyst:K.Risha Page 90 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SarapleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1045 Text: 4 : PFOSA L34910-24, DF=100 073103A-1045 Sm (Mn, 2x3) 100] %: A2.00 02-Aug-2003 01:22:10 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 160471 8.50e4 I1 Area 4.00 ............ ............... -1 11 1 1-y 1 1 1 1 1 1 1^ 6.00 8.00 10.00 i ' ' 1 1 1 I ime 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000147 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 91 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SamplaDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1046 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 073103A-1046 Sm (Mn, 2x3) 100-1 %- 2.00 3: C8 Sulfonate (PFOS) 4.00 6.00 8.98 60941 02-Aug-2003 01:43:42 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 3.71 e5 Area T im e 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000148 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 92 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorachemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1046 Text: 4 : PFOSA XC072503-6,1000 ng/L Standard 073103A-1046 Sm (Mn, 2x3) 100-1 ' %- 02-Aug -2003 01:43:42 LC/MS/MS #6 MRM of 4 Channels ES9.89 498 > 78 7.38e5 Area a y*0 T Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000149 Sponsor Study No; Exygen Study No: Analyte: loos Monitored: Site: NA U4910 PFOA 413 -> 369 Decatur Baker's Creek R A W DATA REPORT Limit o f Quantitation; Injection Volume: Matrix: Sample Volume: Final Volume: 50pp( 15 ml Water 40.0 mL 3.0 mL Set No: Analyst* Instrument Type: Extraction Date: Analyzed on: 073103AR Karen Riikn LC/MS/MS Unit # 6 07/31/03 08/03-04/03 Std. Analyte Amount Exygen Sponsor Sample Run Cone. Dilution Peak Found Added Recovery ID XC072503-0 ID Code No. (PPO Factor Area (PPO (ppd <%> - CS 073103AR-101 0 794 XC072503-1 - CS 073103AR-102 25 14221 - XC072503-2 XC072503-3 - CS 073103AX-103 50 27994 - . CS 073I03AR-104 100 34680 XC072503-4 CS 073103AR-105 230 128556 - XC072503-5 CS 073103AR-I06 500 264862 - XC072503-6 - CS 073103AR-107 1000 516215 - L34910-1 Spk C BC2SW-04 LF 0731Q3AR-I08 100 50564 * 5000 L349l0-l2SpkE B a SW-06 LF 073103AR-109 100 92540 17800 5000 114 L34910-l6SpkF Outfall to River SW-25 LF 073103AR-110 100 l 14710 22100 5000 126 XC072503-1 L34910-1 BC2 SW-04 CS 073103AR-111 23 s 73103AR-112 14631 10 216041 4210 - L34910-] Rep L34910-4 BC2SW-04 BC2 SW-04 Dup S 073103AR-113 s 73103AR-114 10 216268 4210 10 131415 2540 - - U4910-2 BC2 SW-04 Low Spk FF 073I03AR-115 10 142555 2760 10 0 -1450+ XC072503-2 L34910-6 BC2 SW-05 CS 073103AR-U6 50 s 073103AR-117 29284 10 40498 * - - L34910-6 Rep B a sw -05 s 073103AR-118 10 39782 * w U4910-9 BC2 SW-05 Dup s 073103AR-119 10 81652 1560 - L34910-7 B a S W - 0 5 Low Spk FF 073103AR-120 10 112700 2170 1 0 0 1579*+ XC072503-3 L34910-12 L34910-12 Rep L34910-15 L34910-13 - B a SW-06 Basw-o B a SW-06 Dup B a SW-06 Low Spk CS 073103AR-121 100 s 073103AR-122 s 073103AR-123 s 073103AR-124 FF 073103AR-125 55667 20 308911 12100 20 315651 12300 20 297735 11600 20 354730 13900 100 1800+ XC072503-4 - CS 0731Q3AR-126 250 127797 - L34910-16 Outfall to River SW-23 s 073103AR-I27 100 82315 15800 - L34910-16 Rep Outfall to River SW-25 s 073103AR-128 100 83658 16000 - L34910-19 Outfall to River SW-23 Dup s 073103AR-129 100 75424 14400 . L34910-17 Outfall to River SW-25 Low Spk FF 073103AR-130 - 100 78536 15000 100 -800+ XC072503-5 L34910-16 L34910-16 Rep U4910-19 L34910-I7 Outfall to River SW-23 Outfall to River SW-23 Outfall to River SW-23 Dup Outfall to River SW-23 Low Spk CS s s s FF 073103AR-131 073103AR-132 073103AK-133 073103AR-134 07 3 1 0 3 A R -135 300 - 271906 20 380900 20 391789 20 364595 2 0 362898 V* * ** 100 - - - X C 0 7 1003-6 - CS 073103AR-136 1000 - 477931 - - - Analyte Found (ppt) * (peak area - intercept) / slope x DF Recovery (9b) = fanalyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Standard Pttrv* : Linear (1/x weighted) Intercept * 220117 Slope 208.394 Coef. Of DeL a 0.99621! CS s Calibration standard LF * Lab fortified sample C Control sample KF s* Field fortified sample S * Sample LCS =*Laboratory Control Spike CK * Check Standard ND * Not detected * Response between 0 and 22 ppt NQ s Not quantifiable * Response between 22 ppt and LOQ (50 ppt) Spreadsheet prepared by: Sample was analyzed with several dilution factors in order to accommodate all compounds. The appropriate results are reported. ASample was corrected using the data found in set 073103A. -Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. 000150 Sponsor Study No: Exygea Study No: Analyte: Ions Monitored: Site: NA L3491Q PFHS 399 *>80 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ppt 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 073103AR Karen RJsha LC/MS/MS Unit # 6 07/31/03 08/03-04/03 Exygen Sponsor Sample Run ID ID Code No. XC072J03-0 CS 073103AR-101 XC072503-1 c s 073103AR-102 XC072S03-2 CS 073103AR-103 XC072503-3 c s Q73103AR-104 XC07253-4 c s 073103AR-105 XC072503-5 c s 073103AR-106 XC072503-6 c s 073103AR-107 L34910-1 SpItC BC2 SW-04 LF Q73103AR-1O8 L34910-12 Spk E BC2 SW-06 LF 073103AR-109 L3491Q-16 Spk F Outfall to River SW-25 LF 073103AR-l 10 XC072503-1 - c s 073103AR-U1 [-34910-1 BC2 SW-04 s 073103AR-112 L34910-1 Rep L34910-4 BC2 SW-04 BC2 SW-04 Dup s 073103AR-U3 s 073103AR-l 14 L34910-2 XC072503-2 L34910-6 L34910-6 Rep L349I0-9 BC2 SW-04 Low Spk - BC2 SW-03 BC2 SW-05 BC2 SW-05 Dup FF 073103AR-115 cs 073103AR-116 s 073103AR-117 s 073103AR-118 s 073103AR-l 19 L34910-7 XC072503-3 L34910-12 L34910-12 Rep BC2 SW-05 Low Spk - BC2 SW-06 BC2 SW-06 FF 073103AR-120 cs 073103AR-121 s 073103AR-122 s 073103AR-123 L34910-15 BC2 SW-06 Dup s 073103AR-124 L349UM3 XC072503-4 BC2 SW-06 Low Spk - FF 073103AR-125 cs 073103AR-126 L34910-I6 Outfall to River SW-25 S 073103AR-I27 L34910-16 Rep L 3 4910-19 Outfall to River SW-25 OutfaU to River SW-25 Dup S 073103AR-128 s 073103AR-129 L34910-17 Outfall to River SW -25 Low Spk FF 073103AR-130 XC072503-5 - CS 073103AR-131 134910-16 Outfall to River SW-25 s 073103AR-132 L34910-16 Rep L34910-19 Outfall to River SW-25 Outfall to River SW -2J Dup s 073103AR-133 s 073103AR-134 L34910-17 Outfall to River SW-25 Low Spk FF 073103AR-135 XC071003-6 - CS 073103AR-136 Analyte Found (ppt) * (peak area - intercept) / slope x DF Recovery (%) * fanalyte found (ppt)-analyte found in control (ppc)j x 100 amount added (ppt) Std. Cone. (ppo 0 25 30 100 250 500 1000 25 50 - . 100 250 500 1000 Dilution Factor 100 100 100 10 10 10 10 10 10 10 10 20 20 20 20 100 100 100 100 20 20 20 20 Peak Area 0 2074 4718 9231 21488 43819 87115 5566 10314 10701 2324 9381 10152 6122 7036 4266 1526 1565 3729 6025 9486 26169 27209 25364 30673 21551 6872 6261 6156 6030 45496 33004 30633 29219 28660 80818 Analyte Found (pp Amount Added (ppo . - Recovery (%) . - - -- - -* *. 11800 12200 - ** a mm mm ** * 6060 6300 5870 7110 ** * -- 7660 7100 6770 6640 - - 5000 5000 5000 - - - - 100 - 100 - 100 - - 100 100 * - 115 91 - - 1050+ -1020+ - Standard Curve : Linear ( l fx weighted) Intercept * 218.845 Slope s 85.6521 Coef. O f DeL = 0.99656G CS * Calibration standard LF s Lab fortified sample C * Control sample FF * Field fortified sample S = Sample LCS Laboratory Control Spike CK a Check Standard ND a Not detected a Response between 0 and 25 ppt NQ a Not quantifiable a Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by: 3 Sample was analyzed with several dilution factors in order to accommodate all compounds. The appropriate results are reported. Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. 000151 Sponsor Study No; Gxygen Study No: Analyte: Ions Monitored: Site: NA L34910 PFOS 499 >99 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ppt 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 073103AR Karen Risha LC/MS/MS Unit # 6 07/31/03 08/03-04/03 Exygea ID XC072303-0 XC072503-I XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 L3490-1 Spk C L34910-l2SpkE L34910-16 Spk F XC072503-1 L34910-1 L34910-1 Rep L34910-4 L34910-2 XC072503-2 L34910-6 L34910-6 Rep L34910-9 L34910-7 XC072503-3 L34910-12 L3491-12 Rep L34910-15 L34910-13 XC072503-4 L34910-16 L34910-16 Rep L34910-19 L34910-17 XC072503-5 L34910-16 L34910-16 Rep L34910-I9 134910-17 XC071003-6 Sponsor ID BC2SW-04 BC2 SW-06 Outfall to River SW-25 BC2 SW-04 BC2 SW-04 BC2 SW-04 Dup BC2 SW-04 Low Spk BC2SW-05 BC2 SW-03 BC2 SW-05 Dup BC2 SW-03 Low Spk BC2 SW-06 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk - Sample Code CS CS CS CS CS CS CS LF LF LF CS s s s FF CS s s s FF CS s s s FF CS s s s FF CS S 5 S FF CS Run No. 073103AR-101 073103AR-102 073103AR-103 073103AR-104 073103AR-105 073103AR-106 073103AR-107 073103AR-108 073103AR-109 073103AR-I10 073103A R -1 11 073103AR-112 073103 AR-U3 Q73103AR-114 073103AR-115 073103AR-l 16 073103AR-U7 0 7 3 103AR-118 073103AR-119 073103AR-120 073103AR-121 073103AR-122 073L03AR-I23 073103AR-124 07313AR-12S 073103AR-126 073103AR-127 073103AR-128 073103AR-129 073103AR-130 073103AR-13I 073103AR-I32 073103AR-133 073103 AR-134 073103 AR-13S 073103AR-136 Analyte Found (ppt) = (peak area intercept) / slope x DF Recovery ( % ) a (analyte found (ppt)-anolyte fouod in control (ppt)] x 100 amount added (ppt) Std. Cone. (ppo 0 25 50 100 250 500 1000 - - 25 - - 50 - - 100 . 230 - 500 1000 Dilution Factor 100 100 100 10 10 10 10 10 10 10 10 20 20 20 20 100 100 100 100 20 20 20 20 - Peak Area 0 1481 2986 3100 13285 28978 53617 9428 17124 22403 1473 61501 59888 44921 37560 2882 9224 8484 23649 29284 6004 64499 64047 64656 77839 13289 17094 17264 16861 16123 28469 81862 64263 82201 7969* 53157 Analyte Found (pp . - Amount Added (PPO Recovery <%> . . -. . -. . - - 17100 AA AA - . 5000 5000 5000 . 112* - - * 8250 6890 - 100 -4610*+ - 1670 - 1540 - 4330 - 5370 100 3700+ -- *- *- - * 100 - - 31200 - 31500 - 30*00 - 29400 100 -1800+ ** * ** 100 - Standard Curve : Linear (l/x weighted) Intercept = 152.345 Slope * 34.2582 Coef. Of Det 0.998217 CS * Calibration standard LF * Lab fortified sample C a Control sample FF Field fortified sample S 3 Sample LCS * Laboratory Control Spike CK a Check Standard NO Not detected = Response between 0 and 23 ppt NQ s Not quantifiable a Response between 25 ppt and LOQ (50 ppc) ^oeltnlflgSpreadsheet prepared by: Sample was analyzed with several dilution factors in order to accommodate all compounds. The appropriate results are reported. ASample was corrected using the data found in set 080603A Sample requires hither dilution. See data set 080603A ^S am p le requires a higher spiking level. See data set 080603A. Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. 000152 Sponsor Study No: Ex ygen Study No: Analyte: Ions Monitored: Site: NA L34910 FOSA 498 -> 78 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ppt 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 073103AR Karen Risha LC/MS/MS Unit # 6 07/31/03 08/03-04/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC07250J-6 U49IO-1 SpkC L34910-12 SpkE L34910-16 Spk F XC072503-1 L34910-1 L34910-1 Rep L34910-4 L34910-2 XC072503-2 L34910-6 L349I0-6 Rep L34910-9 L34910-7 XC072503-3 L34910-12 L349I0-12 Rep L34910-15 L34910-13 XC072S03-4 L34910-16 L34910-16 Rep L349I0-19 L34910-17 XC072503-5 L34910-16 L349I0-16 Rep L34910-19 L34910-17 XC071003-6 Sponsor ID - BC2 SW-04 BC2 SW-06 Outfall to River SW-25 BC2 SW-04 BC2 SW-04 BC2 SW-04 Dup BC2 SW-04 Low Spk - BC2 SW-05 BC2 SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk - BC2 SW-06 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk - Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup Outfall to River SW-25 Low Spk - Sample Code CS CS CS CS CS CS CS LF LF LF CS s s s FF CS s s s FF CS s s s FF CS S S s FF CS s s s FF CS Run No. 073103AR-101 073103AR-102 073103AR-103 73103AR-14 073103AR-105 0 7 3 103AR-I06 0731O3AR-1O7 073103AR-I08 073 103R-109 73103AR-UO 0 7 3 103AR-111 073103AR-112 07M03AR-U3 073103AR-114 073103 AR-115 0731Q3AR-116 073103AR-117 073103AR-l 18 073103 AR-119 073103AR-I20 0 7 3 103AR-121 0731Q3AR-122 073103AR-I23 073103AR-124 0 7 3 103AR-125 0 7 3 103AR-126 0 7 3 103AR-127 073103A R -128 073103AR-129 073103 AR-130 073103 AR-131 073103AR-132 073103AR-133 073103AR-134 073103AR-135 073103AR-136 Analyte Found (p p t)3 (peak area - intercept) ! slope x DF Recovery ( % ) 3 fanalyte found (ppt)-analyte found in control (ppt)l x 100 amount added (ppt) Std. Cone. (ppt) 0 25 50 100 250 500 1000 25 50 100 - 250 - 500 . . - 1000 Dilution Factor - 100 100 100 10 10 10 10 - 10 10 10 10 - 20 20 20 20 - 100 10Q 100 100 20 20 20 20 Peak Area 0 5175 10303 20719 48632 104085 196920 13039 16006 18398 5382 27920 27505 20497 16630 10890 3460 3402 8876 11595 21221 24495 23261 25908 25736 49195 6718 6206 6506 5831 102292 32659 31916 32869 26767 190680 Analyte Found (ppo . . - * 44 Amount Added (ppt) _ . Recovery (%) . . 5000 5000 5000 1390 1370 * * ** ** 100 100 2430 2300 2570 2550 ** 4* 4* 4 100 100 120 3260 3180 3280 2660 100 -600+ -- - Standard Curve : Linear (l/x weighted) Intercept 3 611.080 Slope s 196.925 C o e f.O fD e u - Q.998392 CS = Calibration standard LF 3 Lab fortified sample C * Control sample FF * Field fortified sample S = Sample LCS 3 Laboratory Control Spike CK = Check Standard ND - Not detected Response between 0 and 25 ppt NQ 3 Not quantifiable = Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by: *'Sample was analyzed with several dilution factors in order to accommodate all compounds. The appropriate results are reported. ^Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated- 000153 lK Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochen jicals.PRO\SampleDB\073103AR Decatur BC.SPL Printed: Sun Aug 03 08:19:25 2003 |ta|o3 ____________ ,,_____ .. Vial File ame LIMS ID Client ID Sample Description Ma 1 41 073103AR-101 _ 2 42 073103AR-102 -- 3 43 073103AR-103 -- 4 44 073103AR-104 -- 5 45 073103AR-105 -- 6 46 073103AR-106 -- 7 47 073103AR-107 -- 8 51 073103AR-108 -- 9 52 073103AR-109 -- 10 53 073103AR-110 -- 11 42 073103AR-111 -- 12 54 073103AR-112 -- 13 55 073103AR-113 -- 14 56 073103AR-114 -- 15 57 073103AR-115 -- 16 43 073103AR-116 -- 17 58 073103AR-117 -- 18 59 073103AR-118 -- 19 60 073103AR-119 -- 20 61 073103AR-120 -- 21 44 073103AR-121 -- 22 62 073103AR-122 -- 23 63 073103AR-123 -- 24 64 073103AR-124 -- 25 65 073103AR-125 -- 26 45 073103AR-126 -- 27 66 073103AR-127 -- 28 67 073103AR-128 -- 29 68 073103AR-129 -- 30 69 073103AR-130 -- 31 46 073103AR-131 -- 32 70 073103AR-132 -- 33 71 073103AR-133 34 72 073103AR-134 -- 35 73 073103AR-135 -- 36 47 073103AR-136 -- ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC072503-0, 0 ng/L Standard XC072503-1, 25 ng/L Standard XC072503-2, 50 ng/L Standard XC072503-3.100 ng/L Standard XC072503-4. 250 ng/L Standard XC072503-5, 500 ng/L Standard XC072503-6,1000 ng/L Standard L34910-1 Spk C, 5000 ng/L, DF=100 L3410-12 Spk E. 5000 ng/L, DF=100 L34910-16 Spk F, 5000 ng/L, DF=100 XC072503-1,2 5 ng/L Standard L34910-1, DF=10 L34910-1 Rep, DF-10 L34910-4, DF=10 L34910-2, DF=10 XC072503-2, 50 ng/L Standard L34910-6, DF=1Q L34910-6 Rep, DF=1Q L34910-9, DF=10 L34910-7, DF=10 XC072503-3,100 ng/L Standard L34910-12, DF=20 L34910-12 Rep, DF=20 L34910-15, DF=20 L34910-13, DF=20 XC07253-4, 250 ng/L Standard L34910-16, DF=100 L34910-16 Rep, DF=100 L34910-19, DF=100 L34910-17, DF=100 XC072503-5, 500 ng/L Standard L34910-16, DF=20 L34910-16 Rep, DF=20 L34910-19, DF=20 L34910-17, DF=20 XC072503-6,1000 ng/L Standard -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- 000154 Exygen study NO. I Page 1 Page Position: (1,1) Sample Type Cone (ng/L) Cone B Cone C Test ID DF Standard Standard Standard Standard Standard Standard Standard QC QC QC Standard Analyte Analyte Analyte QC Standard Analyte Analyte Analyte QC Standard Analyte Analyte Analyte QC Standard Analyte Analyte Analyte QC Standard Analyte Analyte Analyte QC Standard 0 25 50 100 250 500 1000 5000 5000 5000 25 -- -- -- 100 50 -- -- -- 100 100 -- -- -- 100 250 -- -- -- 100 500 ... -- -- 100 1000 0___ ___ ----0 ----0 ----0 ----0 ----0 ----0 ----0 ---- ---- 0 0 ----0 ----0 ----0 ---- ---- 0 0 ---- 0 ----0 ---- 0 ----0 ----0 ---- --. . . 0 0 ----0 -- 0. . . ---- 0 ---- 0 -- 0. . . -- 0. . . ----0 -- --0 ----0 ----0 ----0 -- --0 ---- 0 ----0 1 1 1 1 1 1 1 100 100 100 1 10 10 10 10 1 10 10 10 10 1 20 20 20 20 1 100 100 100 100 1 20 20 20 20 1 <( Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochei |cals.PRO\SampleDB\073103AR Decatur BC.SPL Printed: Sun Aug 03 08:19:25 2003 Q3 l o3________________________ MS Method HPLC Method MS Tune File Inj.Volume 1 C6 C8 SULF C8 ACID PFOSA pfbs water 2 C6 C8 SULF C8 ACID PFOSA pfbs water 3 C6 C8 SULF C8 ACID PFOSA pfbs water 4 C6 C8 SULF C8 ACID PFOSA pfbs water 5 C6 C8 SULF C8 ACID PFOSA pfbs water 6 C6 C8 SULF C8 ACID PFOSA pfbs water 7 C6 C8 SULF C8 ACID PFOSA pfbs water 8 C6 C8 SULF C8 ACID PFOSA pfbs water 9 C6 C8 SULF C8 ACID PFOSA pfbs water 10 C6 C8 SULF C8 ACID PFOSA pfbs water 11 C6 C8 SULF C8 ACID PFOSA pfbs water 12 C6 C8 SULF C8 ACID PFOSA pfbs water 13 C6 C8 SULF C8 ACID PFOSA pfbs water 14 C6 C8 SULF C8 ACID PFOSA pfbs water 15 C6 C8 SULF C8 ACID PFOSA pfbs water 16 C6 C8 SULF C8 ACID PFOSA pfbs water 17 C6 C8 SULF C8 ACID PFOSA pfbs water 18 C6 C8 SULF C8 ACID PFOSA pfbs water 19 C6 C8 SULF C8 ACID PFOSA pfbs water 20 C6 C8 SULF C8 ACID PFOSA pfbs water 21 C6 C8 SULF C8 ACID PFOSA pfbs water 22 C6 C8 SULF C8 ACID PFOSA pfbs water 23 C6 C8 SULF C8 ACID PFOSA pfbs water 24 C6 C8 SULF C8 ACID PFOSA pfbs water 25 C6 C8 SULF C8 ACID PFOSA pfbs water 26 C6 C8 SULF C8 ACID PFOSA pfbs water 27 C6 C8 SULF C8 ACID PFOSA pfbs water 28 C6 C8 SULF C8 ACID PFOSA pfbs water 29 C6 C8 SULF C8 ACID PFOSA pfbs water 30 C6 C8 SULF C8 ACID PFOSA pfbs water 31 C6 C8 SULF C8 ACID PFOSA pfbs water 32 C6 C8 SULF C8 ACID PFOSA pfbs water 33 C6 C8 SULF C8 ACID PFOSA pfbs water 34 C6 C8 SULF C8 ACID PFOSA pfbs water 35 C6 C8 SULF C8 ACID PFOSA pfbs water 36 C6 C8 SULF C8 ACID PFOSA pfbs water Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 0 0 0 15 5 Exygen STUDY N O . i Page 2 Page Position: (2,1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exveen Study No: L34910 Instrument: Micromass Quattro Ultima (LC/M S/M S Unit #6) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: M assLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin 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: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol V Analyst: Karen Risha 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. A ll H andwritten P eak ED's by: C3 W 000156 Scanning Method Report Page 1 Method: C:\MASSLTOX\FLU0R0CHEMICALS.PR0\ACQUDB\C6 C8 SULF C8 ACID PFOSA Last Modified: Thu Jul 31 16:23:50 2003 Printed: Sun Aug 03 08:20:40 2003 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay ([ Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone 1 399.00 80.00 0.20 2 413.00 369.00 0.20 3 498.00 78.00 0.20 4 499.00 99.00 0.20 35 10 30 40 50 10 50 30 w 000157 Method Report Method File: Last Modified: w Printed: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs water Sunday, August 03, 2003 08:06:07 Sunday, August 03, 2003 08:20:45 Page X KPX100 LC Pump initial Conditions Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(Cj Oven Temperature Right(C) 0.300 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time 0.00 2.00 5.00 9.00 9.50 14.00 14.50 20.00 A% 90.0 90.0 10.0 10.0 0.0 0.0 90.0 90.0 B% 10.0 10.0 90.0 90.0 100.0 100.0 10.0 10.0 C% 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 Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off. Off Contactl Off On Off Off Off Off Contact2 Off Off Off On Off Off Contacts Off Off Off Off On Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (fil/min) Draw Position (mm) Stop Time (mins) Injection Volume(/xl) Vial Number 200.0 200 0.50 20.00 15.0 27 000158 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\FLUOROCHEMS Printed: Sun Aug 03 08:20:54 2003 Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -15 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 4.2e- 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 15 2 14.0 14.0 2.0 650 8 9 11 -647 Rdbk 135.1 767.4 000159 Quantify Calibration Report Study No.:L34910, Set No.:0731Q3AR, Ext.Date:07/31/03, AnalystsK.Risha Pagre 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103AR Decatur BC Last modified: Tue Aug 05 07:03:45 2003 Printed: Wed Aug 06 11:03:59 2003 W Exygen Research, 3058 Research Drive, State College, PA 16801 000160 Quantify Calibration Report Study No.-.1,34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst :K.Risha Page 2 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103AR Decatur BC Last modified: Tue Aug 05 07:03:45 2003 Printed: Wed Aug 06 11:03:59 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000161 Quantify Calibration Report \ mif Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 3 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorocharaicals.PRO\CurveDB\Q73103AR Decatur BC Last modified: Tue Aug 05 07:03:45 2003 Printed: Wed Aug 06 11:03:59 2003 w Exygen Research, 3058 Research Drive, State College, PA 16801 000162 Quantify Calibration Report \m * Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, AnalystsK.Risha Page 4 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103AR Decatur BC Last modified: Tue Aug 05 07:03:45 2003 Printed: Wed Aug 06 11:03:59 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000163 Quantify Sample Report Study No.:L34910, Set N o . :073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: F:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Initiais Date. Run# lQ Llb Q T ?lb^g.-\?^ Name: 073103AR-101 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) Exygen Research, 3058 Research Drive, State College, PA 16801 000164 Quantify Sample Report W Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 2 Sample List: P: \Data\LCMSMS6VMasslynx\Fluorochemical*.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamical3.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-101 Text: w Exygen Research, 3058 Research Drive, State College, PA 16801 000165 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 3 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-102 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0001G6 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Dates07/31/03, Analyst:K.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 030103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-102 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000167 Quantify Sample Report Vwt* Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, AnalystsK.Risha Page 5 Sample List: P:\Data\LCMSMS6\Hasslynx\Fluorochemicals.PR0\SamplaDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-103 Text: 1: C8 Acid (PFOA) XC072503-2, 50 ng/L Standard 073103AR-103 Sm (Mn, 2x3) 10Ch %- nu--1_____ A ____________________ ,,,,,,,,, o -O 'V - Oo eg 6.00 Xm* 2: C6 Sulfonate (PFHS) 9.13 279941 I 1 03-Aug-2Q03 19:54:17 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.66e5 Area 8.00 ~i T T "r-r ........ I1 1 1 Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000168 Quantify Sample Report S + * Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tua Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sim Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-103 Text: 4: PFOSA XC072503-2, 50 ng/L Standard 073103AR-103 Sm (Mn, 2x3) 100] %: 03-Aug-2003 19:54:17 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 10303^ 5.55e4 Area 0 1 I r - l I "[ |T 'T f [T 'l T I "I" I I I I I'T I T r I I I 11 I I 2.00 4.00 6.00 8.00 T-r- 10.00 T im e 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 000169 Quantify Sample Report Study N o .:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FR0\MetbDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug Q6 11:04:02 2003 Name: 073103AR-104 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) XC072503-3,100 ng/L Standard 073103AR-104 Sm (Mn, 2x3) 10Oi 0 n 1i i i |'~f 1i } i i p i i i r i r iTi 2.00 4.00 9.25 5100 03-Aug-2003 20:16:01 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.99e4 Area i) i i- i p . i i r i 6.00 8.00 10.00 Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000170 Quantify Sample Report Study No.:L34910, Set N o . :073103AR, Ext.Date:07/31/03, Analyst:K.Risha Paga 8 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AH-104 Text : 4: PFOSA XC072503-3,100 ng/L Standard 073103AR-104 Sm (Mn, 2x3) 10Ch 03-Aug-2003 20:16:01 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 2071 1.07e5 Area a V 'T 1' 1' I T 2.00 4.00 6.00 8.00 1 ]~t I I I I Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000171 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, AnalysttK.Risha Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tu b Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-105 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103AR-105 Sm (Mn, 2x3) 100n %- 0 1 1 1 1 i ' '~r '"i 11111'~1' i11 ' r~,i 1 2.00 4.00 3: C8 Sulfonate (PFOS) 6.00 8.98 21488 03-Aug-2003 20:37:5q LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1,29e5 Area -i Time 8.00 io!oo 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000172 Quantify Sandle Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, AnalystsK.Riaha Page 10 Sample List: P:\Data\LCMSMS6\Maeslynx\Fluorocheaiicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-105 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000173 Quantify Sample Report Study No.:L34910, Set N o . :073103AR, Ext.Date:07/31/03, Analyst .-K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name : 073103AR-106 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 073103AR-106 Sm (Mn, 2x3) m ru %- 8.98 438191 1 1 03-Aug-2003 20:59:39 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.54e5 Area <y ' 1'' ' - 1 1 ' 1 1 1 r" r ~r~' '! ' 2.00 1 ( 1 ' 1 1 1 ' ' ' ....... 1 i ' 1T ' 1 - TM 1 i 1 ' i Time 4.00 6.00 _____&QQ___________ 10.00__________ 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000174 Quantify Sample Report X J Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst;K.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 ' Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wad Aug 06 11:04:02 2003 Name: 073103AR-106 Text: 4: PFOSA XC072503-5, 500 ng/L Standard 073103AR-106 Sm (Mn, 2x3) 100-] %: Q3-Aug-2003 20:59:39 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 5.47e5 Area 0 --I-- r--I-- I-- |-- I"t I-- I--|--i-- I-- I-- i-- [--t-- r~i-- I-- I-- I-- I-- i-- I--^--I-- i-- I-- i-- I-- r- 2.00 4.00 6.00 8.00 10.00 1 1 1 I Time 12.00 Zxygen Research 3058 Research Drive, State College, PA 16801 000175 Quantify Sample Report %^ Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst-.K.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-107 Text: 1: C8 Acid (PFOA) XC072503-6,1000 ng/L Standard 073103AR-107 Sm (Mn, 2x3) an n _ %: 9.15 5162151 1 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.96e6 Area c ' ' ' 1 1 r - i- r - i i . , 'T--I ; .... i i i ' I 1 ' T" ' ' '' 1 1 1 ' 1 1 1. 1-^1-- lr - T~T-n'-i~ '-i i i Time ___________________Z 0 0 ___________ 40___________ 6X50___________ ZOO___________ 10.00__________ 12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) XC072503-6,1000 ng/L Standard 073103AR-107 Sm (Mn, 2x3) 100-i %- I '1i1 2.00 T-'4.00 1T~i~ 6.00 9.27 53617 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.12e5 Area 8.00 10.00 T im e 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000176 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-107 Text: 4: PFOSA XC072503-6,1000 ng/L Standard 073103AR-107 Sm (Mn, 2x3) 10CH %- 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 >78 196920 1 1.01e6 Area 0-^' > ' ' I 1 1 ' 1 I 1 ' 1'1" I 111 I 2.00 4.00 1 I1 6.00 8.00 10.00 T im e 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000177 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-108 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State Collage, PA 16801 000178 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, AnalystsK.Riaha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-108 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000179 Quantify Sample Report Study No.:L34910, Set N o . :073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 17 Sample List; P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Hed Aug 06 11:04:02 2003 Name: 073103AR-109 Text: 1: C8 Acid (PFOA) L349 10-12 Spk E, 5000 ng/L, DF=100 0731 33AR-109 Sm (Mn, 2x3) 10O] %- 9.13 925401 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 5.53e5 Area 0 - ' ' ' ' T 1 1 ' 1 ! 1 1 1 ' 1 1 ' 1 1 1 ' ' ' 1 [ 1 ' 1"! 1 1 1l|ll1 1 1 r 1 , , , . 2.00 4.00 6.00 8.00 ^ i 1 1 1 ' T 1 r" i 1 1 Jme 10.00 12.00 %m? 2: C6 Sulfonate (PFHS) L349 10-12 Spk E, 5000 ng/L, DF=100 0731 33AR-109 Sm (Mn, 2x3) 100n %- 8.98 103141 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 6.00e4 Area 0" ............. 1""'................ 1 1 1 1 1 1 1 I 1 1 * 1 I 1,1,11 ..1 ` ' ` I1 ' , ! 1 1 1 1 1 1 1 1 1 1 1 1 1 j 1in 1C 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-12 Spk E, 5000 ng/L, DF=100 073103AR-109 Sm (Mn, 2x3} 100-1 9.25 17124 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1 .03e5 Area 2.00 f r I |" i 1I r 4.00 .. I 6.00 8.00 10.00 T im e 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000180 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 18 Sample List; P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-109 Text: 4: PFOSA L34910-12 Spk E, 5000 ng/L, DF=100 073103AR-109 Sm (Mn, 2x3) 10CH %- 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 160061 8.15e4 Area TT 2.00 r-|"I't11I1r11"iI I I I I 4.00 6.00 r t i " |" i I i 8.00 10.00 T im e 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000181 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 19 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SarapleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 0BQ103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-110 Text: 1: C8 Acid (PFOA) L34910-16 Spk F, 5000 ng/L, DF=100 073103AR-110 Sm (Mn, 2x3) 100-1 9.13 114710 03-Aug-2003 22:26:40 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 6.50e5 Area 2.00 4.00 2 : C6 Sulfonate (PFHS L349 10-16 Spk F, 5000 ng/L, DF=100 6731 D3AR-110 Sm (Mn, 2x3) 100-3 6.00 8.00 8.96 107011 %: o-`n 1 I1 1 I I 1 I 1 I 1-- 1T i"'T 1 1 1 1 1 1 1-- 1 i "V ' ' 1 r 1 ' 1 1 i-i-- 1 ] > 1 1 2.00 4.00 6.00 8.00 rTT'T-,' 10.00 Time 12.00 03-Aug-2003 22:26:40 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 6.13e4 Area 10.00 12.00 %0 Exygen Research, 3058 Research Drive, State College, PA 16801 000182 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Faga 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\Q73103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-110 Text: 4 : PFOSA w Exygen Research, 3058 Research Drive, State College, PA 16801 000183 Quantify Sample Report \ ^ 0 Study N o.:1*34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K .Riaha Paga 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-111 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000184 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-111 Text: 4: PFOSA %0 Exygen Research, 3058 Research Drive, State College, PA 16801 000185 Quantify Sample Report Study No.:L34910, Set No.;073103AR, Ext.Date:07/31/03, AnalystsK.Risha Page 23 Sample List: P:\Data\LCMSMS6\Masslynx\Pluorocheaiicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-112 Text: 1: C8 Acid (PFOA) L34910-1, DF=10 073103A R -112 Sm (Mn, 2x3) 10Ch %: 03-Aug-2003 23:10:02 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.26e6 Area 0 ' i f' 1 i i i i--' i i i 2.00 4.00 im* 2: C6 Sulfonate (PFHS) 6.00 ~i ' 1 1 1 i 1 1 1 1 i Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-1, DF=10 073103AR-112 Sm (Mn, 2x3) 100-1 %- ' 11T n r 2.00 i- 1-iTM i*iT-r 4.00 6.00 9.24 61501 03-Aug-2003 23:10:02 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.57e5 Area priT 8.00 - n '- r 10.00 i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000186 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tu b Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-112 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000187 Quantify Sample Report 'h*/ Study No.:L34910, Set No.:073103AR, Ext.Dates07/31/03, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-113 Text: 1: CB Acid (PFOA) L34910-1 Rep, DF=10 073103A R -113 Sm (Mn, 2x3) 100n %- 9.13 216268 03-Aug-2003 23:31:52 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.26e6 Area 0 i * | P*1 I 7 --p 'r t I .......... i1 'I [* y *'i I T " [ 11) I I i I I I1 r - T -] T T T f | i 2.00 4.00 6.00 8.00 10.00 T im e 12.00 3: C8 Sulfonate (PFOS) L34910-1 Rep, DF=10 073103AR-113 Sm (Mn, 2x3) 10Ch %H ot 2.00 1 1 r* 4.00 6.00 9.25 59888 03-Aug-2003 23:31:52 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.52e5 Area 8.00 '' 11111111 10.00 r-i-i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000188 Quantify Sample Report \]i^0 Study No.:L34910, Set No. :073103AR, Ext .Date:07/31/03, AnalystsK.Risha Page 26 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-113 Text: 4 : PFOSA W Exygen Research, 3053 Research Drive, State College, PA 16801 000189 Quantify Sample Report W Study Ho.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 27 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-114 Text: 1: C8 Acid (PFOA) L34910-4, DF=10 073103A R -114 Sm (Mn, 2x3) 100TM %- 9.13 1314151 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES413 >369 7.74e5 Area 0: 1 ' I * 1 1 1 1 r" 1 1 ~ 1 I ! I - I 1 1 -- r ' - I - I 1 r i 1 T T - r 1 1 1 1 1 1 ^ ^ ....................... I1 : T im e ___________________ZOO___________ 4/30___________ 6J30___________ a o o ___________ 10.00__________ 12.00 W 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-4, DF=10 073103A R-114 Sm (Mn, 2x3) 100^ %1 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 I4492l l I 2.59e5 Area 0 - ' 1 ' r ....... I1 "1 I' i t i 1 T-i1 , 1*i*'ti*11 i - i " n - n r r ' | T T T T - l t- ' I I ' ' r-i ITMI I-.' 1 Tim e 2.00 4.00 6.00 8.00 10.00 12.00 w Exygen Research, 3058 Research Drive, State College, PA 16801 000190 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 28 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 0731Q3AR-114 Text : 4: PFOSA L34910-4, DF=10 073103AR-114 Sm {Mn, 2x3) 100-1 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9-90 498 > 78 20497 I 1 ,05e5 Area 2.00 T " 1 1- T I < 4.00 T '1 1 r " T" l 6.00 1" 8.00 10.00 Time 12.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 000191 Quantify Sample Report Study No.:L34910, Set No. .-073103AR, Ext.Date:07/31/03, Analyst:X.Risha Page 29 Sample List: P:\Data\LCMSMS6\Masslynx\Pluorooliemicals.PRO\SainpleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-115 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000192 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 30 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-115 Text : 4: PFOSA %0 Exygen Research 3058 Research Drive, State College, PA 16801 000193 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 31 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-116 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000194 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 32 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: . Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-116 Text: 4: PFOSA XC072503-2, 50 ng/L Standard 073103AR -116 Sm (Mn. 2x3) 100-] 04-Aug-2003 00:37:19 LC/MS/MS #6 MRM of 4 Channels ES- 9-90 498 > 78 108901 5.94e4 Area -i Time 2.00 4.00 6.00 8.00 10.00 12.00 w %0 Exygen Research 3058 Research Drive, State College, PA 16801 000195 Quantify Sample Report Study Mo.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 33 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SamplaDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-117 Text : 1: C8 Acid (PFOA) Vs/ 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 305S Research Drive, State College, PA 16801 000196 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 34 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AH Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSHS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-117 Text : 4 : PFOSA Exygen Research 3058 Research Drive, State College, PA 16801 000197 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 35 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslymc\Fluorochemicals.PRO\MetbDB\Decatur BC 0S0103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-118 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) Exygen Research, 3058 Research Drive, State College, PA 16801 000198 Quantify Sample Report '*/ Study N o .:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 36 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 . Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-118 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000199 Quantify Sample Report W Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst :K.Risha Page 37 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SarapleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-119 Text: 1: C8 Acid CPFOA) L34910-9, DF=10 073103AR-119 Sm (Mn, 2x3) 100-1 9.13 81652 04-Aug-2003 01:42:36 LC/MS/MS #6 MRM of 4 Channels ES413 >369 4.77e5 Area I ` T`-'I I I ' 2.00 2: C6 Sulfonate (PFHS) 4.00 6.00 Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000200 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 38 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-119 Text : 4: PFOSA L34910-9, DF=10 073103AR-119 Sm (Mn, 2x3) 10CH %- 04-Aug-2003 01:42:36 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 8876 4.44e4 Area 0 I |- T"T 4.00 I' I I I j I I I I 6.00 8.00 I 10.00 - n Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000201 Quantify Sample Report <l)-r/ Study No.:L34910, Set N o .:073103AR, Ext.Date: 07/31/03, Analyst sK.Risha Page 39 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-120 Text: 1: C8 Acid (PFOA) L34910-7, DF=10 073103AR-120 Sm (Mn, 2x3) 10CHj %: 04-Aug-2003 02:04:23 LC/MS/MS #6 MRM of 4 Channels ES413 >369 6.62e5 Area 0 I--I-- r - r - j -- r --i-- i-- i-- p - r -- r --i-- r-- p - i -- i-- r - i -- p - i -- i i i | -T - 2.00 4.00 6.00 2: C6 Sulfonate (PFHS) L349 10-7, DF=10 0731 D3AR-120 Sm (Mn, 2x3) 100: %- T-p-i" 1 I "i- p'i ' Time 10.00 12.00 8.97 6025^ 04-Aug-2003 02:04:23 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 3.66e4 Area U~ ' 1'1 ' 1 '' r 1 1 1 1 1 1 1 T--T-1--I--r-T--T-T-l , . , , , 1 , , , 1 1 1 1 1 1 1 1 . 1 1 ...... "1 ' 1 - ' j 1 Time 2.0 0 4.00 6.0 0 8.0 0 1 0 .0 0 12 .00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000202 Quantify Sample Report Study N o .:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 40 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-120 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000203 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 41 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC hast modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-121 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000204 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 42 Sample List: P:\Data\LCMSMS6\Masslymt\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-121 Text: 4: PFOSA XC072503-3,100 ng/L Standard 073103AR-121 Sm (Mn, 2x3) 10Ch %- 04>Aug-2003 02:26:03 LC/MS/MS #6 MRM of 4 Channels ES9-90 498 > 78 212211 "1.1265 Area 0 1 tI -I-- I I I- I " I I ; I I 'I 1 - p - i - ' l l - r 1 ; I I I I I I -I ) I I r - T 2.00 4.00 6.00 8.00 10.00 Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000205 Quantify Sample Report Study No. :L34910, Set No.-.073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 43 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Harne: 073103AR-122 Text: 1: C8 Acid (PFOA) L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) 10O, 9.13 308911 04-Aug-2003 02:47:47 LC/MS/MS #6 MRM of 4 Channels ES413> 369 1.81e6 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 2: C6 Sulfonate (PFHS) L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) 100- %: 8.98 261691 1 [ 04-Aug-2003 02:47:47 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.54e5 Area 0 -I , , , r, tI--r--r-.j 1 I I I I 1 * 1 [ 1 1 * * r'"'1"~T 1 1 T.r.T'l 1 1 1 1 1 1 1 1 ^*1 t ' ' r 1"'"1"1- 1--'t 1 ! I- 1 Time 2.00 4.00 ________ &00__________8^00_________ 10.00_________ 12.00 L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) 100-1 %- 04-Aug -2003 02:47:47 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.81 e5 Area 2.00 4.00 6.00 ' [ 1 ' < 1 I ' 1 ' ' I Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000206 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 44 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SainpleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-122 Text: 4: PFOSA L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) 10CH %- 04-Aug-2003 02:47:47 LC/MS/MS #6 MRM of 4 Channels ES- 9-88 4 9 8 > 78 24495 I 1 ,25e5 Area 0 ' 1-- 1 1t " f 'I'" T- T" r - f r T " r....r | i i 1 1r i | 1 r 1 2.00 4.00 6.00 irII 8.00 10.00 Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 wu 0J207 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, AnalystsK.Risha Page 45 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-123 Text: 1: C8 Acid (PFOA) L34910-12 Rep, DF=20 073103AR-123 Sm (Mn, 2x3) 100^ %- 0 - 1 1 1 'T ^ 1 r"l 1 2.00 1111' 111' 111 4.00 6.00 9.13 |3156511 i 04-Aug-2003 03:09:25 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.84e6 Area TT" 1 r i 1 1 ' ' 1 TM 1 1 I ' ' 1 > ; i-r-r i Time ____ 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-12 Rep, DF=20 073103AR-123 Sm (Mn, 2x3) 10Ch %- 0 1 ' r 1 I 1"T 1 r 1 1 I 1 2.00 4.00 6.00 04-Aug-2003 03:09:25 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.75e5 Area t~ I' 10.00 I r-i ..... I Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000208 Quantify Sample Report IU| Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 46 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-123 Text : 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000209 Quantify Sample Report . j Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 47 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tua Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-124 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) L349 10-15, DF=20 0731 03AR-124 Sm (Mn, 2x3) 100: %- U 2 .0 0 3: C8 Sulfonate (PFOS) L34910-15, DF=20 ' 1 1 I 1111I 1 1 1 1 1 1 4.00 6 .0 0 073103AR-124 Sm (Mn, 2x3) 100] %: 0 '''1!1''1I1'1'I1111I1 2.00 4.00 6.00 8.98 253641 04-Aug-2003 03:31:09 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.46e5 Area 8 .0 0 . 1. 1 0 .0 0 12 .00 04-Aug -2003 03:31:09 LC/MS/MS #6 MRM of 4 Channels ES- 9.27 499 > 99 3.74e5 Area 8.00 I 1 1 nr--I--..I I 1 1 Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000210 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 48 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-124 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000211 Quantify Sample Report Study No.:L34910, Set No.s073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 49 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-125 Text: 1: C8 Acid (PF0A) L34910-13, DF=20 073103AR-125 Sm (Mn, 2x3) 10O] %: 9.13 354730 04-Aug-2003 03:52:55 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.09e6 Area 2.00 4.00 6.00 8.00 --r 1 1 1 1.i1 1 1 1 i Time 10.00 12.00 *** 2: C6 Sulfonate (PFHS) L34910-13, DF=20 073103AR-125 Sm (Mn, 2x3) 10Ch %- 04-Aug-2003 03:52:55 LC/MS/MS #6 118.98 306731 MRM of 4 Channels ES- 399 > 80 1.82e5 Area 0 - 1 1 i 1 ' 1 i 1 ' i ........... ................... ''T 1 r -r"T_1"' i * i 1 ' 1 i 1 1 1 1 i Time 2.00__________4^00__________6^00__________8.00 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-13, DF=20 073103AR-125 Sm (Mn, 2x3) 100-1 %- 04-Aug-2003 03:52:55 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.48e5 Area Q - L - r I --I " f ' ) r T ' "'T "T... T....T-- T " I I I I I I I I I 2.00 4.00 6.00 -i T "'.i"1 1...........r "T""' "i Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000212 Quantify Sample Report Study No.:L34910, Set No.;073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 50 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-125 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000213 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 51 Sample List: P:\Data\LCMSMS6\Mas3lynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 0S0103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-125 Text : 1: C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) 100-1 9.13 127797 04-Aug-2003 04:14:42 LC/MS/MS #6 MRM of 4 Channels ES413> 369 7.35e5 Area (y-r T -- T -- I---- 1 T T -- I 2.00 'rT 1 ' 4.00 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) 100n %- 2.00 4.00 3: C8 Sulfonate (PFOS) XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) 100-| 6.00 6.00 8.00 8.96 21551 10.00 Time 12.00 04-Aug-2003 04:14:42 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.28e5 Area 8.00 10.00 Time 12.00 9.27 13289 04-Aug-2003 04:14:42 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 7.65e4 Area 0 Li - I r I I ",rT 11 I 2.00 II|III 4.00 6.00 8.00 1 1 f r '-* Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000254 Quantify Sample Report Study No.:L34910, Set N o . :073103AR, Ext.Date:07/31/03, Analyst:K.Risha Rage 52 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-126 Text : 4: PFOSA XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) 10CH %: 04-Aug-2003 04:14:42 LC/MS/MS #6 MRM of Channels ES9.92 498 > 78 2.56e5 Area 0 L -1" I , I - - I- I I - I ' I I T---| " I I I I 2.00 4.00 1 1"11r 6.00 'I' 8.00 10.00 r 1 .I Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000215 Quantify Sample Report %luf Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, AnalystsK.Risha Page 53 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-127 Text: 1: C8 Acid (PFOA) V 2 : C6 Sulfonate (PFHS) 3 : C8 Sulfonate (PFOS) L34910-16, DF=100 073103AR-127 Sm (Mn, 2x3) 100- %: 02.00 4.00 9.27 17094 j 1 04-Aug-2003 04:36:30 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.90e4 Area ' i i 1 ' i '1 i ... i t ' v i-i-- 6.00 8.00 1 i "i ' 1 1 i 1 1 1 1 1 Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000216 Quantify Sample Report 'W Study No.:L34910, Set No. :073103AR, Ext.Date:07/31/03, AnalystsK.Risha Paga 54 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-127 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000217 Quantify Sample Report '/ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 55 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SainplaDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-128 Text: 1: C8 Acid (PFOA) 3 : C8 Sulfonate (PFOS) L34910-16 Rep, DF=100 073103AR-128 Sm (Mn, 2x3) 100- 9.27 172641 04-Aug-2003 04:58:16 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.56e4 Area < y r "! i r p i -- i ) y--'i"" i t " T '* f r--T'" i i-- . ,1. 2.00 4.00 ,.. [-[f v t - i i I i I "i t t 1 ! i r j I ' T i 6.00 8.00 Lr-r-j-r-i r r i T i T r ) Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000218 Quantify Sample Report . Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Paga 56 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-128 Text: 4: PFOSA w % *0 Exygen Research, 3058 Research Drive, State College, PA 16801 000219 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 57 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochsraicals.PRO\SainpleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheroicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-129 Text: 1: C8 Acid (PFOA) Sm* 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-19, DF=100 073103AR-129 Sm (Mn, 2x3) 100^ %- 04-Aug-2003 05:20:01 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 ]168611 1 9.96e4 Area 0 - *T ' J ' ' T ' ' \ ' ' 1 "1 ' T* ' f ' 1 " ! ' * 1 1 I 1^ ^r-' I ..... r ' ' ...... Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000220 Quantify Sample Report Study N o .:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 58 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tua Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-129 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000221 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 59 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-130 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-17, DF=100 073103AR-130 Sm (Mn, 2x3) 100-1 9.25 16123 04-Aug-2003 05:41:49 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.43e4 Area iwr 0 > i-- i-- i-- i i i i-- i-- i--i-- i--P2.00 4.00 6.00 8.00 10.00 T T- Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000222 Quantify Sample Report <w / Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 60 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluarochemicals.PRO\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-130 Text: 4: PFOSA w Exygen Research, 3058 Research Drive, State College, PA 16801 000223 Quantify Sample Report X ^ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 61 Sample List: P:\Data\LGMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-131 Text: 1: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 073103AR-131 Sm (Mn, 2x3) miv, %- 9.15 2719061 1 1 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.53e6 Area 0 - ................ T l ~ r - r - 1 | 1- 1--I--r--|--r- 1 r | , ,.., r-i-r r i t- , , r - i - ]i r -i-- i-- i i i i ^ t - - ' 1 r -Ti '' 11T" 1 ' 1 < i Time 2.00 4.00 6.00 _______ a o o _________10.00________ 12.00 W 2: C6 Sulfonate (PFHS) XC072503-5,500 ng/L Standard 073103AR-131 Sm (Mn, 2x3) ino_ %: 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 1454961 1 2.61 e5 Area 0 - ' 1"' I ' 'I ' 2.00 11 1 1 1.....1 1 1 y -r-r-v r- r ' Ir r - i -- ,.. . ' i 1 1 ' ' i 1 1 1 1 iTime 4.00 6,00__________ aoo__________10.00_________ 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000224 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Dates07/31/03, Analyst:K.Risha Page 62 Sample List: P:\Data\LCMSMS6\Masslyxnc\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MetbDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-131 Text : 4: PFOSA XC072503-5, 500 ng/L Standard 073103AR-131 Sm (Mn, 2x3) 10Ch %- 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 102292 5.22e5 Area 0w T -r-i Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000225 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 63 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080X03 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wad Aug 06 11:04:02 2003 Name: 073103AR-132 Text : 1: C8 Acid (PFOA) L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) 100^ %- o: ' ' ' ' r r r-r- 11'1 1 1 I"1 ' r- 1 I 1 1 1 ' I 1 '' 1r T ' 2.00 4.00 6.00 2 : C6 Sulfonate (PFHS) L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) 100n %: 9.13 3809001 1 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2 .2 0 e6 Area 1 1 1.......... . , . . 8.00 f- ' 1 ' -r ' * ........... .. Time 10.00 12.00 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES8.96 399 > 80 1.86e5 Area Q l - , - , . , r*""j' , r - r - r- T- i ' r ................................... . - t - r ' | > i i i |- 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) 10O-i 8.00 ~ |111 ' 10.00 -t--r- r-r I Time 12.00 9.26 81862 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.68e5 Area -- I 1--1 I 1 11 ' I ' '' 'T I T J ... I I - r t r ! I Time 2.00 4.00 6.00 8.00 100(7 12.00 w Exygen Research, 3058 Research Drive, State College, PA 16801 000226 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, AnalystrX.Risha Faga 64 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-132 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000227 Quantify Sample Report % f Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst :K.Risha Faga 65 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: F:\Data\LCHSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-133 Text : 1: C8 Acid (PFOA) L34910-16 Rep, DF=20 073103AR-133 Sm (Mn, 2x3) 100- %- 9.12 3917891 I 04-Aug-2003 06:47:22 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.26e6 Area 0 : ' ' ' ' T 1' 1 1 . 1 1 1 T 1 1 T.1 T -r' ''"r_' 1 ' ' ' .............. ^ T~i' 1 i 1 1 |" 1 i 1 1 1 1 i Time 2.00 4.00 6.00 8.00 10.00 12.00 2: C6 Sulfonate (PFHS) L34910-16 Rep, DF=20 073103AR-133 Sm (Mn, 2x3) 100n %: 04-Aug-2003 06:47:22 LC/MS/MS #6 MRM of 4 Channels ES- 8.97 399 > 80 1.81e5 Area 0 L 1 1 i 1 1 1 i 1 1 r 1~r~r11 T' 2.00 4.00 3: C8 Sulfonate (PFOS) 6J30 ' T 1 1 ' r ......... - i Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000228 Quantify Sample Report % ^ > Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 66 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaapleDB\Q73103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochexaicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-133 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000229 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 67 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-134 Text: 1: C8 Acid (PFOA) \m * 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-19, DF=20 073103AR-134 Sm (Mn, 2x3) 100-, 2.00 4.00 9.25 82201 04-Aug-2003 07:09:05 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.64e5 Area 6.00 T--r" 181.0..0... 10.00 T im e 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000230 Quantify Sample Report fc|LJ# Study N o .:L34910, Set No.;073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 68 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-134 Text: 4: PFOSA X* Exygen Research, 3058 Research Drive, State College, PA 16801 000231 Quantify Sample Report Yj* Study No.:L34910, Set No.s073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 69 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleD8\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AH-135 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) L34910-17, DF=20 073103AR-135 Sm (Mn, 2x3) 10CH %: 0 2.00 3: C8 Sulfonate (PFOS) 4.00 6.00 8.96 28660 04-Aug-2003 07:30:42 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.69e5 Area Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000232 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 70 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-135 Text: 4: PFOSA W *0 Exygen Research, 3058 Research Drive, State College, PA 16801 000233 Quantify Sample Report Study N o.11.34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:R.Risha Page 71 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sim Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-136 Text: 1: C8 Acid (PFOA) XC072503-6,1000 ng/L Standard 073103AR-136 Sm (Mn, 2x3) 100n %: 9.12 477931 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES413> 369 2.78e6 Area o-w 2.00 4.00 w 2: C6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 073103AR-136 Sm (Mn, 2x3) 10Ch %: 6.00 8.00 8.96 1"i ' ' 1'~i.I 10.00 T im e 12.00 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 4.81 e5 Area 0 ' ' ' I ' ' I 1 1--1 1 1 1 ''T"1 ' I ' ' i ' 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) 8.00 ' t........... I 1 1 1 1 I Tim e 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000234 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, AnalystsK.Risha Page 72 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Last modified: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-136 Text: 4: PFOSA XC072503-6,1000 ng/L Standard 073103AR-136 Sm (Mn, 2x3) lOCh %- Ch 1' ' ' ............ 1 , 2.00 w 4.00 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES- 9-90 _. 498 >78 1906801 9.76e5 II Area 6.00 r 1 1 r--1 I 1 1 1 1 1 1 1 1 1.1 1 ' 1 1 r-i 1 1 Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000235 Sponsor Study No: Exygen Study No: Analyte: loos Monitored: Site: NA L34910 PFOS 499 -> 99 Decatur Baker's Creek R A W DATA REPORT Limit o f Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ppt 13 (iL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 080603A Karen Risha LC/MS/MS Unit # 6 07/31/03 & 08/06/03 08/06/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 0106020 Control 0106020 Spk A 0106020 Spk B L3491Q-12 Spk E L34910-16 Spk F L349I0-16 Spk F XCQ72503-I XC072503-2 XC072503-3 L34910-I L34910-1 Rep L3491-12 L34910-12 Rep L34910-15 L34910-13 XC072503-4 XC072503-3 XC071003-6 Sponsor CD BC2 SW-06 Outfall to River SW-25 Outfall to River SW-25 BC2 sw-oa BC2 SW-W BC2 SW-06 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk - Sample Code CS CS CS CS CS CS CS c LCS LGS LF LF LF CS CS CS s s s s s FF CS CS CS Run No. 080603A-1001 08603A-1002 080603A-1003 080603A-1004 080603A-1005 080603A-1006 080603A-1007 80603A-1008 080603A-I009 080603A-1010 080603A-1011 080603A-1012 080603A-1013 080603A-1014 080603A-1015 080603A-1016 080603A-1017 080603A-1018 080603A-1019 80603A-1020 080603A-1021 080603A-1022 080603A-1023 080603A-1024 080603A -1025 Analyte Found (ppt) : (peak area * intercept) / slope x DF Recovery (%) = (analyte found (ppt)-analytc found in control (ppt)] x 100 amount added (ppt) Std. Cone. (ppo 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Factor 1 1 100 200 100 . 100 100 100 100 100 100 .. - Peak Area 0 1238 2570 4455 10551 22336 43039 0 2436 21693 22031 18543 35655 1229 2338 4928 5243 5235 11612 11877 11205 14257 10803 23323 44271 Analyte Found (ppo Amount Added (p p o Recovery (ft) ND 51.3 490 49800 * 80900 . . . 11500 11500 26100 26700 25100 32100 . . 50 500 25000 50000 50000 . _ . . . . . 100 . . 103 98 95 . 99 6000+ . - -- Standard Curve : Linear (1/x weighted) Intercept = 184.312 Slope = 43.8624 Cocf. Of Dec. * 0.998804 CS = Calibration standard LF Lab fortified sample C Control sample FF * Field fortified sample S = Sample LGS = Laboratory Control Spike CK = Check Standard ND = Not detected a Response between 0 and 25 ppt NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by: Sample was analyzed with several dilution factors. The appropriate result is reported. ^Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. w 000236 Eve n RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34910 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. Time IQ 3 0 ______ Date 0>(0bl0'?> Initials. CLIENT SAMPLE ID na na na BC2 SW-06 Outfall to River SW-25 - - - EXYGEN ID NUMBER 0106020 Control 0106020 Spk A 0106020 Spk B L34910-12 Spk E L34910-16 Spk F VOLUME (mL) 40.0 40.0 40.0 40.0 40.0 FORTIFICATION (ng) _ 2.0 20.0 1000.0 2000.0 -_ -_ -- -- - . -. - ._ -- - w- _ -_ - ._ - -_ - .. -_ 0106020 Spk A 0106020 Spk B L34910-12 Spk E L34910-16 Spk F - - - Spiking Solution Used F061103-2 (10 ng/mL) F06I103-1 (100 ng/mL) F060203-1 (10000 ng/mL) F060203-I (10000 ag/mL) - - All samples were measured: Time | 2 . 4 0 ______ Date. After measuring samples were returned to refrigerator No. 3 2 Time. \ 5 C S ______ Date Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 uL micropipet) 100 pL (200 pL micropipet) 200 pL (200 pL micropipet) Initlal/Date W VL - / 081/h*%/( / or fejo /HR Obli I&- /o& ofeIl*o- yj - - 4Initials. - Initials. Comments: 200 pL o f 250 mg/mL sodium thiosulfate was added to all samples before spiking. lnicials/Dace:. Q 6 )o fc)o 3 Analysis Summary: Data Set: Data Set: Data Set:________ Initials/Date: 1IMn.itimaIlms//TDA AabtMe:. Initials/Date: B ^ - / Pfilobfo3! //_ -/ Set extraction/analysis data verified by: s *- Date: % / M y 26, 2001/6 000237 i (t 3058 Research Drive Phone: 814-272-1039 RESEARCH State College, PA 16801 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34910 MATRIX: Water METHOD: " ANALYTES: PFHS. PFOS. PFOA and PFOSA PROTOCOL NUMBER: NA Client ID aa Da na BC2SW-06 Outfall to River SW-25 -' - - - - - - ExygeuID 0106020 Control 0106020 Spk A 0106020 Spk B L3491Q-12 Spk E L34910-16 Spk F - - '- - - -' - - - STEP 1 >/ . - - . - STEP 2 Vi/ - - . .. - j/. *Initials/Date - STEP 1: SPE column clean-up (omitting 40% wash) STEP 2: Final volume lo 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reanalysis. Dilutions (mUmL) - - -- *Vvo rP . . . . . - 1" STEP 3 1 . _ _ - 1f Dilutions (mL/rnl.) - ~~~ -- r- STEP 4 - r- -- -- -- __ -- -- -- -- ._ __ -- -. _- -. -- -- . ._ -- '- - -- - - LF s 160 -t 2 60. pcO&)ot|0?) v Reagents/ Materials Methanol C18 SPE Type IWater . Lot# 4 3 (1 ^ 1 8 U J3 1 |2 E > I NA _ _ -. . _. __ - Initials/Date jilwlcb/o?: rD . _ - . . . . ItPLC Metbaaol AmmoniumAcetate Type I water 4-3087314 V 36^ NA . . ill" Initials/Date o8|oi}c0> 'Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA). and Perfluorooctanoate (POAA) in Water COMMENTS: 00 Final extracts stored in refrigerator. 3 k Initials; Date: te > U |o 3 > M y 19, 2001/4 00023 t S hK Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroche iicals.PRO\SampleDB\080603A Decatur BC.SPL Printed: Wed Aug 06 13:15:20 2003 t o __________________________ Vial File Name UNIS ID Client ID Sample Description 1 41 080603A-1001 _ 2 42 080603A-102 -- 3 43 080603A-1003 -- 4 44 080603A-1004 -- 5 45 080603A-1005 -- , 6 46 80603A-1006 -- 7 47 080603A-107 -- 8 51 08O63A-18 -- 9 52 080603A-1009 ~ 10 53 08O6Q3A-101Q -- 11 54 080603A-1011 -- 12 55 080603A-1012 -- 13 56 080603A-1013 -- 14 42 080603A-1014 -- 15 43 Q80603A-115 -- 16 44 080603A-1016 -- 17 57 080603A-1017 _ _ 18 58 080603A-1018 -- 19 59 080603A-1019 -- 20 60 080603A-120 -- 21 61 080603A-1021 -- 22 62 080603A-1022 -- 23 45 080603A-1023 -- 24 46 080603A-1024 -- 25 47 080603A-1025 _ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- ----- -- -- -- -- -- -- -- XC072503-0, 0 ng/L Standard XC072503-1, 25 ng/L Standard XC072503-2, 50 ng/L Standard XC072503-3, 100 ng/L Standard XC072503-4, 250 ng/L Standard XC072503-5, 500 ng/L Standard XC072503-6,1000 ng/L Standard 0106020 Control 0106020 Spk A, 50 ng/L 0106020 SpkB, 500 og/L L34910-12 Spk E. 25000 ng/L, DF=100 L34910-16 Spk F, 50000 ng/L, DF=200 L34910-16 Spk F, 50000 ng/L, DF=100 XC072503-1,25 ng/L Standard XC072503-2, 50 ng/L Standard XC072503-3,100 ng/L Standard L34910-1, DF=100 L34910-1 Rep, DF=100 L34910-12, DF=100 L34910-12 Rep, DF=100 L34910-15, DF=100 L34910-13, DF=100 XC072503-4,250 ng/L Standard XC072503-5, 500 ng/L Standard XC072503-6,1000 ng/L Standard C2000 C5 Exygen STUDY NO. i W l o M K Page 1 Page Position: (1,1) 5 Matrix Sample Type Cone (ng/rat!) Cone B Cone C Test ID DF -- Standard 0 -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 -- Blank -- -- QC 100 -- QC 500 -- QC 25000 -- QC 50000 -- QC 50000 -- Standard 25 -- Standard 50 -- Standard 100 -- Analyte -- Analyte -- Analyte -- -- -- Analyte -- -- Analyte -- -- QC 100 -- Standard 250 -- Standard 500 -- Standard 1000 _ __ 0 ----0 ----0 ----0 -- --0 0. -- -- 0___ ___ 0-- ___ ----0 ----0 -- --0 -- --0 ----0 ----0 --0 ----0 ----0 -- --0 ----0 ----0 0-- --- -- --0 --V -- 0 -- --0 ----0 1 1 1 1 1 1 1 1 1 1 100 200 100 1 1 1 100 100 100 100 100 100 1 1 1 K Masslynx - Sample List Sample List: C:\MASSLYNX\fluorochemicals.PRO\SampleDB\080603A Decatur BC.SPL Printed: Wed Aug 06 13:15:20 2003 |A j) ^ ^ ___________ ______________ MS Method HPLC Method MS Tune File Inj.Volume 1 C6 C8 SULF C8 ACID PFOSA 2 C6 C8 SULF C8 ACID PFOSA 3 C6C8 SULF C8 ACID PFOSA 4 C6 C8 SULF C8 ACID PFOSA 5 C6 C8 SULF C8 ACID PFOSA 6 C6 C8 SULF C8 ACID PFOSA 7 C6 C8 SULF C8 ACID PFOSA 6 C6 C8 SULF C8 ACID PFOSA 9 C6 C8 SULF C8 ACID PFOSA 10 C6 C8 SULF C8 ACID PFOSA 11 C6 C8 SULF C8 ACID PFOSA 12 C6C8 SULF C8 ACID PFOSA 13 C6 C8 SULF C8 ACID PFOSA 14 C6 C8 SULF C8 ACID PFOSA 15 C6 C8 SULF C8 ACID PFOSA 16 C6 C8 SULF C8 ACID PFOSA 17 C6 C8 SULF C8 ACID PFOSA 18 C6 C8 SULF C8 ACID PFOSA 19 C6 C8 SULF C8 ACID PFOSA 20 C6 C8 SULF C8 ACID PFOSA 21 C6 C8 SULF C8 ACID PFOSA 22 C6 C8 SULF C8 ACID PFOSA 23 C6 C8 SULF C8 ACID PFOSA 24 C6 C8 SULF C8 ACID PFOSA 25 C6 C8 SULF C8 ACID PFOSA pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 000240 Exygen STUDY NO. ( 3 ^ 10 Page 2 Page Position: (2,1 ) LC/MS/MS SYSTEM AND OPERATING CONDITIONS it Sponsor Protocol No: N A . Exygen Study No: L3491Q Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: Software: COMPAQ Professional Workstation AP200 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 Bin 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: 74A) (JONESCHROMATOGRAPHY: Part N o. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are com puter generated printouts from the m asslynx software program . The pages contain the instrum ent settings used for the analysis of this data set. A ll Handwritten Peak ID 's by: 0-b W 000241 'W Scanning Method Report Page 1 Method: C:\MASSLYNX\FLU0R0CHEMICALS.PR0\ACQUDB\C6 C8 SULF C8 ACID PFOSA Last Modified: Thu Jul 31 16:23:50 2003 Printed: Wed Aug 06 13:15:53 2003 flit# Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 M R M of 4 Mass Pairs 1; ESP- ;) Inter Channel Delay I; Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V 1 399.00 80.00 0.20 2 413.00 369.00 0.20 3 498.00 78.00 0.20 4 499.00 99.00 0.20 35 10 30 40 50 10 50 ' 30 w 000242 Method Report Page 1 Method File: Last Modified: C :\MAS SLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs water Wednesday, August 06, 2003 13:15:26 Printed: Wednesday, August 06, 2003 13:16:00 HP1100 LC Pump Initial Conditions 2& > Solvents A% B% C% D% 90.0 10.0 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 20.0 Q 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time A% B% C% D% Flow Pressure 0.00 90.0 10.0 0.0 0.0 0.300 400 2.00 90.0 10.0 0.0 0.0 0.300 400 5.00 10.0 90.0 0.0 0.0 0.300 400 9 .00 10.0 90.0 0.0 0.0 0.300 400 9.50 0.0 100.0 0.0 0.0 0.300 400 14.00 0.0 100.0 0.0 0.0 0.300 400 14.50 90.0 10.0 0.0 0.0 0.300 400 20.00 90.0 10.0 0.0 0.0 0.300 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contactl Off On Off Off Off Off Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/xl/min) Draw Position (mm) Stop Time (mins) Injection Volume(^l) Vial Number 200.0 200 0.50 20.00 15.0 82 000243 Tuning Method Report Method: Printed: C :\MASSLYNX\FLUOROCHEMICALS. PRO\ACQUDB\FLUOROCHEMS Wed Aug 06 13:19:13 2003 Cfo]o6|o3 Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -43 99 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 4 .Oe- 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 15 2 14.0 14.0 2.0 650 24 29 27 -646 Rdbk 132.1 770.3 000244 Quantify Calibration Report studir No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Faga 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochejnicals.PR0\CurveDB\080603A Decatur BC Last Modified: Thu Aug 07 12:27:57 2003 Printed: Thu Aug 07 12:49:55 2003 Exygen Research, 3058 Research Drive, State College, FA 16801 000245 Quantify Sample Report Study No.:L34910, Set No.:080603a , Ext.Date:07/31 & 08/06/03, Analyst:K.Risba Page 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 J b C deS Initial. Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1001 Text: 1: C8 Sulfonate (PFOS) %0 Exygen Research 3058 Research Drive, State College, PA 16801 000246 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SainpleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1002 Text: 1: C8 Sulfonate (PFOS) W Exygen Research 3058 Research Drive, State College, PA 16801 000247 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRCASampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\P70S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Coda: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1003 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000248 Quantify Sample Report Study Mo.:L34910, Set No.:080603A, Bxt.Date:07/31 & 08/06/03, Analyst:K.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:43:56 2003 Name: 080603A-1004 Text : 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000249 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Dates 07/31 & 08/06/03, AnalystsK.Risha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SajnpleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1005 Text : 1: C8 Sulfonate (PFOS) XC072503-4,250 ng/L Standard 080603A-1005 Sm (Mn, 2x3) 100- /c r 9-35 105511 1 06-Aug-2003 16:24:39 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.71 e4 Area 0- 1 ' 1 r ' ' ' | ''7 --I-I- 1... 1 r r-'i '1 1 1 1 1 I ~'i- t" i i ' t t i .~r i - n - r - | - ^ r p i T r m - i t t Time _______________ loo_________ 400_________ aoo_________ aoo_________io.oo w w Exygen Research, 3058 Research Drive, State College, PA 16801 000250 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 6 Sample Lists P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1006 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000251 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, AnalystsK.Risha Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1007 Text: 1: C8 Sulfonate (PFOS) XC072503-6,1000 ng/L Standard 080603A-1007 Sm (Mn, 2x3) 10Ch %- 9.33 43039 06-Aug-2003 17:08:00 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.83e5 Area r i I I.I'T"" 2.00 4.00 6.00 8.00 T-p-r-r 10.00 T im e W Exygen Research, 3058 Research Drive, State College, PA 16801 000252 Quantify Sample Report \ ^ / Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur ,BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicala.PR0\MethDB\PF0S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1008 Text : 1: C8 Sulfonate (PFOS) w Exygen Research, 3058 Research Drive, State College, PA 16801 000253 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SamplBDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1009 Text: 1: C8 Sulfonate (PFOS) %0 Exygen Research, 3058 Research Drive, State College, PA 16801 000254 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 10 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1010 Text: 1: C8 Sulfonate (PFOS) 0106020 Spk B, 500 ng/L 080603A-1010 Sm (Mn, 2x3) 100h %- 9-31 216931 1 06-Aug-2003 18:13:04 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.58e4 Area 0- --L"i !--r--I--I I'T' 1 r--p \ 1 r \ 1| - r n , , i i i--!--i--|-- i--i--r 1 1 1 1 1 - ............. 1 11 T 1 1 1 1 1 I 1 1 1 . Time ___________________Z 0 0 ___________ 4XX)___________ 60___________ a o o ___________ 10 .0 0 w w Exygen Research, 3058 Research Drive, State College, PA 16801 000255 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, AnalystsK.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1011 Text: 1: C8 Sulfonate (PFOS) L34910-12 Spk E, 25000 ng/L, DF=100 080603A -1011 Sm (Mn, 2x3) 100^ %: 9-33 220311 ft 06-Aug-2003 18:34:45 LC/MS/MS #6 MRM of 4 Channels ES49g > 99 9.36e4 Area 0- ................'' 1 1 - i - i I' T-- ..... ...... ... .... 1 1 l-r-T-i > 1 1 ' '-I1 I 1 ~T" 1 1 r~i..r 1 2.00 4.00 6.00 8.00 1 ~T""r 1 10.00 T im e V lie# Eacygen Research 3058 Research Drive, State College, PA 16801 000256 Quantify Sample Report ' W studY No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1012 Text : 1: C8 Sulfonate (PFOS) L34910-16 Spk F, 50000 ng/L, DF=200 080603A-1012 Sm (Mn, 2x3) 100n %: 9-32 185431 1 06-Aug-2003 18:56:25 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 7.99e4 Area o- 1 1 ` 1 1 1 1 1 1 ' 1 1 1 1 1 11 1' 1 1 ' 1 1 1 1 1 T - l --- f " l '!' 1 ' " i 1 ' " i " | l " 1" 1 2.00___________ 4,00___________ 6 M ___________ 8.00 1 1 ' i 1 1 ' Time 10.00 w Exygen Research, 3058 Research Drive, State College, FA 16801 000257 Quantify Sample Report I' Study No .:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Tbu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Nome: 080603A-1013 Text: 1: C8 Sulfonate (PFOS) W Exygen Research, 3058 Research Drive, State College, PA 16801 000258 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 6 08/06/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1014 Text: 1 : C8 S u lf o n a t e (PFOS) w Exygen Research, 3058 Research Drive, State College, PA 16801 000259 Quantify Sample Report Study No.:L34910, Set No.:080603A, Bxt.Date:07/31 6 08/06/03, AnalystsK.Risha Page 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemical3.PR0\MethDB\PF0S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1015 Text: 1 : C8 S u l f o n a t e (PFOS) % t* Exygen Research 3058 Research Drive, State College, PA 16801 000260 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 08Q603A-1016 Text: 1 : C8 S u lf o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000261 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\Q80603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1017 Text: 1 : C8 S u lf o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0002G2 Quantify sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SamplaDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\DataSLCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1018 Text : Exygen Research, 3058 Research Drive, State College, PA 16801 000263 Quantify Sample Report 1l-- / Study No.:L34910, Set No.:080603A, Ext.Date: 07/31 & 08/06/03, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1019 Text: 1 : C8 S u lf o n a t e (PFOS) W Exygen Research 3058 Research Drive, State College, PA 16801 000264 Quantify Sample Report Page 20 Study No.:L34910, Sat No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha W Sample List: P:\Data\LCMSMS6\Masalynx\Fluorochemicals.PR0\SaunpleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1020 Text: 1 : C8 S u lf o n a t e (PFOS) W Exygen Research, 3058 Research Drive, State College, PA 16801 0002G5 Quantify Sample Report Page 21 i Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FR0\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1021 Text: 1 : C8 S u lf o n a t e (PFOS) Exygen Research 3058 Research Drive, State College, PA 16801 000266 Quantify Sample Report Page 22 > Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1022 Text: 1 : C8 S u lf o n a t e (PFOS) L.34910-13, DF=100 080603A-1022 Sm (Mn, 2x3) 100-] %- 9-36 142571 1 06-Aug-2003 22:33:46 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 6.13e4 Area o : ' 1 1 ....................................i T"> i - r i i i 1 i i r i , r " - r - r ,,T- _T"i r - '" ' i 11 ' t-- i T 2.00 4.00 6.00 8.00 w ii i i - i r i i i i i T im e 10.00 w Exygen Research, 3058 Research Drive, State College, PA 16801 000267 Quantify Sample Report iu < Study N o .:L34910, Set No.:080603A, Ext-Date:07/31 & 08/06/03, Analyst:K.Risha Page 23 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1023 Text : 1 : C8 S u lf o n a t e (PFOS) XC072503-4, 250 ng/L Standard 080603A-1023 Sm (Mn, 2x3) 10CH %- 9.34 10803 06-Aug-2003 22:55:27 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.85e4 Area 0 W I 1 ..........I 1 1 1 2.00 IT f I I I 4.00 6.00 8.00 10.00 T im e Exygen Research, 3058 Research Drive, State College, PA 16801 000268 Quantify Sample Report Study No.:L34910, Set No.:080603a , Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1Q24 Text: 1 : C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0002G9 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SampleDB\080603A Decatur BC Last modified: Thu Aug 07 08:12:08 2003 Method: P :\Data\LCMSMS6'iMasslynx\Fluarochemicals.PRO\MethDB\PFOS only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1025 Text: 1 : C8 S u l f o n a t e (PFOS) XC072503-6,1000 ng/L Standard 080603A-1025 Sm (Mn, 2x3) 100- /o: 06-Aug-2003 23:38:52 LC/MS/MS #6 MRM of 4 Channels ES- 9.31 1442711 1 499 > 99 -1.9-feS Area o: 1 i i i I - r - r i i 1 i i i V-- , , , .. r - i - ................ , < - 1 1 1 i 1 ' 1 1 i ...............r " T ' i 2.00 4.00 6.00 8.00 Time. i ! i r-- i i 10.00 W Sxygen Research, 3058 Research Drive, State College, PA 16801 000270 SECTION E 000271 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L34910 PFOA 413 > 369 Decatur Baker's Creek R A W DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: JO ppt 15 pL Soil 5.0 g 3.0 mL Set No: Analyse Instrument Type: Extraction Date: Analyzed on: 080I03A Karen Risiu ICMSMS #6 08/01/03 08/0203 Std. Analyte Amount Analyte Total Exygen Sponsor Sample Run Cone. Dilution Peak Found Added Recovery Found Solids ID XC0725O3-O ID Code No. (ppt) Factor Area (ppo (ppt> <%) (ppt>) (%) CS 080103A-2001 0 333 XC072503-1 CS 080103A-2002 25 9882 - XC072503-2 CS 08013A-2003 30 17917 - XCD72503-3 XC072503-4 CS 080103A-204 100 CS 080103A-2005 250 34827 78794 - XC0725O3-5 XC072503-6 Methanol Wash Reagent Blank Reagent Spk A CS 08Q1Q3A-2006 500 171634 - CS 080103A-2007 tooo 315768 - c 080103A-2008 325 - na c 080103A-2009 i 518 ND - oa LCS 08103A-2010 18939 55.3 50 Ml - Reagent Spk B na LCS 080103A-2011 163063 536 500 107 - XC072503-1 CS 080103A-20I2 25 9820 - L34910-5 Spk C U 4910-10SpkD BC2 SED-04 BC2SED-05 LF 08Q103A-2013 LF OROI03A-20U 10 157971 5190 10 166134 5460 3000 5000 96 96 - L349I0-U Spk E BC2 SED-06 LF 080103A-2015 10 187666 6180 5000 88* - U 4 9 10-20 Spk F Outfall to River SED'25 UP 08Q103A-016 10 179090 5890 5000 91* - w XC072503-2 - CS 080103A-2017 50 18190 - L34910-5 BC2 SED-04 s 080103A-2018 115451 377 3.02 69.96 L34910-5 Rep BC2 SED-04 s 080103A-20I9 82762 268 2.14 69.96 L34910-10 BC2SED-05 s 080103A-2020 195055 642 5.14 69.54 L34910-10 Rep BC2SED-05 s 080103A-2021 167826 551 4.41 69.54 XC072503-3 . CS 080I03A-2022 100 33920 - XC072303-4 L34910-U U 4 9 1 0 .ll Rep L349I0-20 U 4 9 10-20 Rep L349I0-21 BC2 SED-06 B O SED-06 Outfall to River SED^25 Outfall to River SED-25 Outfall to River SED-25 Dup CS 080103A-2023 250 s 0801Q3A-2024 s 080103A-2025 s 0B0103A-2026 s 0801Q3A-2027 s 080103A-2028 79282 473416 463017 404209 301201 532619 t * - 60.41 * 60.41 - 63.27 - 63.27 - 67.43 XC072503-5 CS 080103A-2029 500 140009 -- XC072503-6 - CS 080103A-2030 1000 - 273386 - Analyte Found (ppt) * (peak area - intercept) / slope x DF Recovery (%) = (analyte found (ppQ-analyte found io control (ppt)) x 100 amount added (ppt) Stand* f-IITV* : Linear (1/x weighted) Intercept * 2344.75 Slope 300.076 Coef. Of Del. * 0.988097 Analyte Found (ppb) * (analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight analyte found (ppb) x (100% / total solid* (%)) CS * Calibration standard C = Control sample S Sample LF wLab fortified sample FF a> Field fortified sample LCS * Laboratory Control Spike CK Check Standard ND * Not detected * Response between 0 and 25 ppt NQ mNot quantifiable Response between 25 ppt and LOQ (50 ppt) Analyte Found (ppb) Dry Weight . 431 3.06 7.39 6.34 Sam ple requires dilution. See data set 080103AR. ^Sample was corrected using the data found in set 080103AR. Spreadsheet prepared by:. c& 000272 Sponsor Study No: Exygcn Study No: Analyte: Ions Monitored: Site: NA L34910 PFHS 399 -> 80 Decatur Baker's Creek R A W DATA REPORT lim it of Quantitation: Injection Volume: Matrix; Sample Weight: Final Volume: 50 ppt 15*iL Soil 5.0 g 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on; 080103A Karen Risha LCMSMS #6 08V01/03 082/03 Exygea ID XC0725Q3-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072303-5 XC072503-6 Methanol Wash Reagent Blank ReagentSpkA Reagent Spk B XC072503-I L34910-5 Spk C L34910-10 Spk D L34910-I1 SpkE L34910-20 Spk F XC072503-2 L349I0-5 L34910-5 Rep L34910-10 L34910-lORep XC072503-3 XC072503-4 L34910-11 L34910-U Rep L34910-20 L34910-20 Rep L34910-21 XC072503-5 XC072503-6 Spoasor ID -' na na na - BC2SED-04 BC2SED-05 BC2 SED-06 Outfall to River SED-25 BC2 SED-04 BC2 SED-04 BC2 SED-05 BC2SED-05 BC2 SED-06 BC2 SED-06 Outfall to River SED-25 Outfall to River SED-25 Outfall to River SED-25 Dup Sample Code CS CS CS CS CS CS CS C C LCS LCS CS LF LF LF LF CS s s s s CS CS s s s s s CS CS Run No. 0801Q3A-2QI 080I03A-2002 080103A-2003 080103A-2004 08013A-2005 080103A-2006 080103A-2007 80103A-2008 080103A-2009 080103A-2010 080103A-2011 080103A-2012 080103A-2013 OS0103A-2014 080103A-2015 080I03A-2016 080103A-2017 080103A-201B 080103A-2019 08013A-2020 080103A-202I 080I03A-2022 080103A-2023 080103A-2024 080I03A-2025 080103A-2026 080103A-2027 0B0LQ3A-2028 080103A-2029 080103-2030 Analyte Found (ppt) (peak area - intercept) / slope x DF Recovery (%) * [analyte found (pptVanalytc found in control (pm)) x 100 amount added (ppt) Std. CoQC. (ppt) Q 25 50 100 250 300 1000 25 50 100 250 500 1000 Dilution Factor 1 1 1 10 10 10 10 1 1 1 1 1 t 1 1 l Peak Area Q 1572 3699 6481 15770 31281 58308 0 0 3457 31000 1765 30746 32192 32334 32343 3449 4534 3439 10896 12999 6560 14801 18133 19203 23354 16649 36172 28497 54198 Analyte Found (ppb) = [analyte found (ppt) x volume extracted (Q.04 L)| / sample weight (S g) Analyte Found (ppb) dry weight * analyte (bund (ppb) x (100% / total solids (%)) Analyte Found (pp<) Amount Added (ppt) Recovery (%) Analyte Found (ppb) . . . . - ND 52.0 50 533 500 104 107 - 3280 5530 5560 5560 5000 5000 5000 5000 104 107 105 103 70.8 0.57 31.7 0.41 182 1,45 218 1.75 - 308 327 399 282 623 - 2.46 161 3.19 2.26 4.98 -- - -- Standard Cnrv e ; Linear (\jx weighted) Intercept 476.906 Slope - 573138 Coef. O f B e t * 0.995587 Total Solids (SO .. . _ _ . . ,, . . . . 69.96 69.96 69.54 69.54 . . 60.41 60.41 63.27 63.27 67.43 _ - CS = Calibration standard C * Control sample S 3 Sample LF Lab fortified sample FF n Field fortified sample LCS Laboratory Control Spike CK * Check Standard ND * Not detected * Response between 0 and 25 ppt NQ Not quantifiable * Response between 23 ppt and LOQ (50 ppt) Analyte Found (ppb) .Dry Weight . . _ . 0.809 0.591 2.09 2.51 . . 4.08 4.33 5.05 3.57 7.39 . - Spreadsheet prepared by: 000273 Sponsor Study No: Exygen Study No: Analyte: loos Monitored: Site: NA L34910 PFOS 499 -> 99 Decatur Baker's Creek RAW DATA REPORT lim it of Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: SOppt 15 pL Soil 5.0 g 5.0 mL Set No: Analyse Instrument Type: Extraction Date: Analyzed on: 080I03A Karen Risha LCMSMS #6 08/01/03 08/02/03 Exygen ID XCQ72503-0 XC0725O3-1 XCQ72503-2 XCO72503-3 XC072503-4 XC072503-5 XC072503-6 Methanol Wash Reagent Blank Reagent Spk A Reagent SpkB XC072503-1 L34910-5 Spk C L349tO-tOSpkD L34910-11 Spk E L3491O-20SpkF XCO72503-2 U4910-5 L34910-5 Rep L34910-10 L34910-10 Rep XCO72503-3 XC072503-4 U49I0-11 L34910-11 Rep L34910-20 L34910-20 Rep L34910-21 XCO72503-5 XC072503-6 Sponsor ID - ' ' _ na oa aa BC2 SED-04 BC2 SED-05 BC2 SED-06 Outfall to River 5ED-25 BC2 SED-04 BC2 SED-04 BC2 SED-05 BC2 SED-05 BC2 SED-06 BC2 SED-06 Outfall to River SED-25 Outfall to River SED-25 Outfall to River SED-25 Dup - Sample Code CS CS CS CS CS CS CS c c LCS LCS CS LF LF LF LF CS S s s s CS CS s s s s s CS CS Sid. Run Cone. No. 080103A-2001 (pw) 0 080103A-2002 25 080103A-2003 5<l` 080103A-2004 100 080103A-2005 250 080L03A-2006 500 080103A-2007 0S0103A-2008 1000 080103A-2009 080103A-2010 080103A-2011 080103A-2012 23 08Q103A-2013 080103A-2M4 080103A-2015 080J03A-2016 080103A-2017 50 080103 A-2018 080103A-2019 080103A-2020 080103A-202I 080103A-2022 100 080103A-2Q23 080103A-2024 250 080I03A-2025 080103A-2026 080103A-2027 080103A-2023 080103A-2029 500 080103A-2030 1000 Analyte Found (ppt) (peak area - intercept)/ slope x OF Recovery (%) * (analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Dilution Factor .v 1 1 1 10 to to 10 1 1 1 1 I 1 1 l 1 Peak Area 0 1018 2072 3701 9370 19171 37079 0 0 2011 17583 938 22878 26935 336383 72248 2233 60613 51074 93844 106350 3634 8965 2354673 1794353 418516 287933 409821 17108 32192 Analyte Found (ppo Amount Added (ppo Recovery <%) Analyte Found (PPB) . ND 51.4 496 6470 7620 50 500 . 5000 5000 5000 5000 103 99 93A 95* * * - - Standard Curve ; Linear (1/x weighted) Intercept 208.543 Slope * 35.0593 Coef. O f Dec. * 0.990916 Total Solids (%) . . . . - - - 69.96 69.96 6954 69.54 60.41 60.41 63.27 63.27 67.43 - Analyte Found (ppb) [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight* analyte found (ppb) x (100% / total solids (%)) CS Calibration standard C Control sample S * Sample LF * Lab fortified sample FF * Field fortified sample LCS Laboratory Control Spike CK - Check Standard ND * Not detected Response between 0 and 25 ppt NQ * Not quantifiable * Response between 25 ppt and LOQ (50 ppt) Analyte Found (ppb) Dry Weight . . . . . - . . - . - - - S am ple requires dilution. See data set 080103AJR. "'Sample was corrected using the data found in set 080103AR. Spreadsheet prepared by:. 000274 Sponsor Study No: Exygeo Study No: Analyte: Ions Monitored: Site; NA L34910 FOSA 498 -> 78 Decatur Baker's Creek R A W DATA REPORT Limit o f Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 15 /xL Soil 5.0 g 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 080103A Karen Risha LCMSMS #6 08/01/03 08/02/03 Exygen ID XC072503-0 XC072503-I XC072503-2 XCQ725Q3-3 XC072503-4 XC072503-5 XC072503-6 Methanol Wash Reagent Blank Reagent Spk A Reagent Spk B XC072S03-1 L34910-5 Spk C L34910-10 Spk D L34910-11 Spk E L34910-20 Spk F f XC072503-2 L3491Q-5 L34910-5 Rep L34910-10 L34910-10 Rep XC072503-3 XC072503- L34910-1I L34910-U Rep L34910-20 L34910-20 Rep U 4 9 10-21 XC072503-5 XC072503-6 Sponsor ID - - - - na na na BC2 SED-04 BC2 SED-05 BC2 SED-06 Outfall to River SED-25 BC2 SED-04 BCJ SED-04 BC2 SED-05 BC2 SED-05 - - BC2 SED-06 BC2 SED-06 Outfall to River SED-25 Outfall to River SED-25 Outfall to River SED-25 Dup - Sample Code CS CS CS CS CS CS CS c c LCS LCS CS LF LF LF LF CS S s s s CS CS s s s s s CS CS Run NoQ8O1O3A-2Q0I 080I03A-202 O8O1O3A-2O03 080103A-2004 080103A-2005 08013A-2006 080103A-2007 080103A-2008 080103A-2009 08103A-2010 080103A-2011 080103A-2012 080103A-2013 080103A-2014 Q8Q103A-2Q15 080103A-2016 080103A-2017 080103A-2018 080103A-2019 080103A-2020 080103A-2021 080103A-2022 080103A-2023 080103A-2024 080103A-2025 080103A-2026 080103A-2027 080103A-2028 080103A-2029 80103A-2030 Analyte Found (ppt) * (peak area - intercept) / slope x DF Recovery (%) * [analyte found (ppt)-analyic found in control (ppt)) x 100 amount added (ppt) Std. Cone. (p p o 0 25 50 100 250 500 1000 25 50 100 250 - - . 500 1000 Dilution Factor 10 10 10 10 1 1 1 . 1 1 I 1 1 . - Peak Area 0 3995 7728 15082 36693 72894 137821 0 0 6750 65424 3817 79517 82212 155090 100640 7957 121382 133583 133763 191201 14698 34282 1215533 929771 412369 346384 357273 67231 129118 Analyte Found (ppti Amount Added (ppo Recovery <%) Analyte Found (ppb) ND 43.6 so 477 500 .- 87 95 . 5810 6010 * 7370 - 5000 5000 5000 5000 98 101 77A . 894 7.15 981 - 7.84 982 . 7.86 . . . *. . . . -- Standard Curve : Linear (1/x weighted) Intercept 849,062 Slope - 135.358 Cocf. O f Det. = 0.996863 Total Solids <%) ,, . . . _ . . . . . * . 69.96 69.96 69.54 69.54 . 60.41 60.41 63.27 63.27 67.43 . - Analyte Found (ppb) = [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight = analyte found (ppb) x ( 100% / total solids (%)) CS " Calibration standard C = Control sample S Sample LF * Lab fortified sample FF - Field fortified sample LCS = Laboratory Control Spike CK - Check Standard NO Not detected = Response between 0 and 25 ppt NQ = Not quantifiable * Response between 25 ppt and LOQ (50 ppt) Analyte Found (ppb) . . _ ._ _ . . .. . 10.2 11.2 11.3 _. . . . . . . . - Sam ple requires dilution. See data set 080103AR. ^Sam ple was corrected using the data found in set 030103AR. Spreadsheet prepared by:. .03 000275 Analyst: \ W ork Group'*VG46121 Analysis: S o lid ! Title: Send Date Prepared: 29-.V '003 ^ ID Result Product Matrix DF MDLxDF CRDLxDF Flags Time Collect L34905-21 100 PERC SOLID SOUD 1 0.01 0 08-Jul-03 00:00 L34905-22 100 PERC SOLID, SOLID 1 0.01 0 08-Jul-03 00:00 L34905-23 100 PERC SOLID SOUD 1 0.01 0 0B-Jul-03 00:00 L34905-24 100 PERC SOLID SOLID 1 0.01 0 0B-Jul-03 00:00 L34905-25 100 PERC SOLID SOLID 1 0.01 0 OB-Jul-03 00:00 L34905-26 100 PERC SOLID SOUD 1 0.01 0 06-JUI-03 00:00 L34905-27 100 PERC SOUD SOUD 1 0.01 0 8-JUI-03 00:00 L34905-28 100 PERC SOLID SOLID 1 0.01 0 O8-Jul-03 00:00 L34905-29 100 PERC SOLID SOUD 1 0.01 0 OB-Jul-03 00:00 L34905-30 100 PERC SOLID SOUD 1 0.01 0 08-Jul-03 00:00 L34910-5 69.96 PERC SOLID SOUD 1 0.01 0 23-JUI-03 14:50 L34910-10 69.54 PERC SOUD SOUD 1 0.01 0 21-JUI-03 14:15 L34910-11 60.41 PERC SOLID SOL1D 1 0.01 0 23-JUI-03 15:25 L34910-20 63.27 PERC SOLID SOLID 1 0.01 0 23-Jul-03 16:15 L34910-21 67.43 PERC SOLID SOLID 1 0.01 0 23-Jul-03 16:15 L34921-1 81.19 PERC SOLID SOLID 1 0.01 0 23-Jul-03 14:00 Time Run 29-Jul-03 15:34 29-Jul-03 15:34 29-Jul-0315:34 29-Jul-03 15:34 29-Jul-0315:34 29-Jul-03 15:34 29-Ju)-03 15:34 29-Jul-03 15:34 29-Jul-03 15:34 29-Jul-03 15:34 29-Jul-03 15:34 29-Jul-03 15:34 29-JUI-03 15:34 29-Jul-03 15:34 29-Jul-03 15:34 29-Jul-03 15:34 Client ID 200874 X33238-32-21 200875 X33238-32-22 200876 X33238-32-23 200877 X33238-32-24 200878 X33238-32-25 200879X33238-32-26 200880 X33238-32-27 200881 X33238-32-28 200882 X33238-32-29 200883 X33238-32-30 BC2 SED-04 BC2 SED-05 BC2 SED-06 OUTFALL TO RIVER SED-25 OUTFALL TO RIVER SED-25 DUP BASR7-23 000276 Print Date: 30-Jui-03 Page 1 of 1 Analyst: AJ i Work Group:^ 46121 Analysis: Solids^ Title: Data 4* Date Prepared: 2 9 -J ^ >03 Analyst Initials Date and Time Data Aquired (ctrl+t) AJH 29-Jul-03 15:34 AJH 29-Jul-03 1S:06 AJH 30-Jul-03 08:34 CAL ID CLIENT ID MATRIX PAN ID PAN W EIGHT (a) S A M P LE +PAN |g) DRIED SAMPLE IGNITED SAM PLE + PAN (g) +PAN (g) % Solids o r % TVS or % Ash WG4612M WG46121-2 L34905-21 L34Q5-22 L34905-23 L34905-24 L34905-25 L34905-26 L34905-27 L 34905-28 L34905-29 L34905-30 L34910-5 L3491-1 L34910-11 L3490-20 L 34910-21 L34921-1 MB PERC SOLID | SOLO UP: L34910- PERC SOLID | SOUD 74 X33238-3 : PERC SOLID 1SOLID 75 X33238-3 ! PERC SOLID | SOUQ 76 X33238-3 : PERC SOLID I SOLID 77 X33236-3 ! PERC SOUD JSOUD 78 X33238-3 : PERC SOLID ( SOUD 79 X3323S-3 ; PERC SOLID | SOUD 80 X33238-3 ! PERC SOLID | SOLID 81 X3323B-3 P E R C SO UD (SO LID 82 X33238-3 'P E R C SOUD (SOLID 83 X33236'3 !PER C SOUD (SOLID BC2 SED-04 PERC SOUD ( SOUD BC2 SED-05 PERC SOLID ( SOLID BC2 SED-06 PERC SOLID JSOLID L TO RIVER PERC SOLID IS O L O TO RIVER Si PERC SOLID IS O L O BASR7-23 PERC SOLID 1SOLID 1 2 3 4 5 6 7 B 9 10 11 12 13 14 15 16 17 18 1.2578 1 2521 1 1 1 1 1 1 1 1 1 1.2512 1.2517 1.2578 1 2574 1.2638 1.2556 1.2S7B 43.5159 2 2 2 2 2 2 2 2 2 2 39.8338 28 6584 34.2073 23.9616 200233 4.2022 1.257B 31.9212 2 2. 2 2 2 2 2 2 2 2 28245 20.3121 21.1653 . 15.6246 13.9150 36481 0 72.56 100 100 1 100 100 100 100 100 100 100 69.96 69.54 60.41 63.27 67.43 81.19 000277 Print Date: 06-Aug-03 Page 1 of 1 Exygen RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34910 Sponsor Study/Protocol No: NA Matrix: M l The samples listed below were removed from refrigerator No. eaja ja s Time f)8 S O Date DA Ini in ^ ___ Initia CLIENT SAMPLE ID na EXYGEN ID NUMBER Reagent Blank W EIGHT (g) I FORTIFICATION (ng) _ na na BC2 SED-04 BC2 SED-05 Reagent Spk A Reagent Spk B L34910-5 Spk C L34910-10 SpkD 5.0 5.0 2.0 20.0 200.0 200.0 BC2 SED-06 Outfall to River SED-25 BC2 SED-04 BC2 SED-04 L34910-1I Spk E L34910-20 Spk F L34910-5 L34910-5 Rep 5.0 5.0 5.0 5.0 200.0 200.0 . . BC2 SED-05 L 34910-10 5.0 BC2 SED-05 L34910-10 Rep 5.0 BC2 SED-06 BC2 SED-06 L34910-11 L34910-1! Rep 5.0 5.0 . W Outfall to River SED-25 134910-20 Outfall to River SED-25 L 34910-20 Rep 5.0 5.0 . Outfall to River SED-25 Dup - 134910-21 _ 5.0 _ . .- ,, - - -- Reagent Spk A Reagent Spk B L34910-5 SpkC ' L34910-10 Spk D L34910-11Spk E L34910-20 Spk F - Spiking Solution Used F061103-2 (10 ng/mL) F06U03-1 (100 ng/mL) F060203-2 (1000 ng/mL) F060203-2 (1000 ng/mL) F060203-2 (1000 ng/mL) F060203-2 (1000 ng/mL) - All samples were weighed on balance No. 2 0 Time S '_______ Date f L j H Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - Initial/Date & L /06oij3 " *ltTtT--- /oYfioiiS- v L /o&)tub /Mb fa /0 Oik WL B jo li u. Initials. After weighing samples were returned to refrigerator No. 3 2 - Thn - 3 2 2 _________ Date . 8 M Q 3 Initials /fc iK Com m ents: 200 pL of 230 mg/mL sodium thiosulfate was added to ail samples before spiking. Initials/Date: I nfjjni^nK Analysis Summary: Data Set: Data Set: C '& h \O i & - Data Set: _______ Initials/Date: Initials/Date:. Initials/Date:. fe y " / flft/l] J & _/__ - Set extraction/analysis data verified b y :, Date: <?/ July 26, 2001/A n n o - ? O {K L 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34910 MATRIX: Sfiil METHOD: ExM-023-014 " PROTOCOL NUMBER: NA ANALYTES: PFHS. PEPS. PFOA and PFOSA Client ID na na na BC2 SED-04 BC2 SED-05 BC2 SED-06 Outfall to River SED-25 BC2 SED-04 BC2 SED-04 BC2 SED-05 BC2 SED-05 BC2 SED-06 BC2 SED-06 Outfall to River SED-25 Outfall to River SED-25 Outfall to River SED-25 Dun Exygen ID Reagent Blank Reagent Spk A Reagent Spk B L34910-5 SpkC L34910-10 Spk D L34910-11 Spk E L34910-20 Spk F L34910-5 L34910-5 Rep L34910-10 L34910-10Rep L34910-11 L34910-11 Rep L34910-20 L34910-20 Rep L34910-21 _ STEP 1 STEP 2 STEP 3 STEP 4 STEP 5 1 STEP 6 >V A1/ A \y N .. - . - _- _ - - _ _- _- - - . - -- - - -- - CE d /cfo /jE a^o/jos COSdf/,M STEP l: Add 5mL of methanol and shake by hand for ~1 minute STEP 2: Bring up to 40 mL with hypercarb filtered type 1 water STEP 3: Centrifuge for 10 minutes at -3000 rpm STEP 4: Filter through glass acrodisc STEP 5: SPE column clean up (omitting 40% wash) STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 7: LC/MS/MS analysis STEP 8: LC/MS/MS reanalysis. Dilutions (mL/mL) -- -- V l.o V |.0 l/ | . o e -'/i.o -- -- -- -- -- -- -- -- - - - - - ceja lob STEP Dilutions STEP 7 (mL/mL) 8 -- --- ---- -* - rS-MbcM.o y .o > - - - r S jl cVu0 . ... - & <s>___ - - 4-- L_ - - vl-- cejfif? Reagents/ Materials Lot# Methanol W 3 & ____ C18SPE U3I1ZBI TypeI Water Glass acrodisc NA M W 3A (inl -- -- -- -- - Initials/Date - - C&z celoilab i - -- -- HPLC Methanol 4V>frI5l4 AmmoniumAcetate Type I water NA - ------ -ly ------------ Initials/Date ioccwvMOo SHdAh >M.O,0V..O hp' io Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctanesulfonate (PFOS) and Pentadecafluorooctanoic Acid (PFOA) in Soil COMMENTS: Final extracts stored in refrigerator Initials: US T Date: July 19, 2001/4 000279 << Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorocheiimjicalis.PHRt O\SampleDB\080103A Decatur BC.SPL Printed: Fri Aug 01 15:28:30 2003 l^lIid iIoS Vial File Name LIMS ID Client ID Sample Description Matrix 1 41 080103A-2001 2 3 42 43 080103A-2002 080103A-2003 -- __ 4 5 44 45 080103A-2004 080103A-2005 -- __ 6 46 080103A-2006 -- 7 47 080103A-207 -- 8 92 080103A-2008 -- 9 1 080103A-2009 -- 10 2 0801Q3A-2010 -- 11 3 080103A-2011 -- 12 42 08103A-2012 -- 13 4 080103A-2013 -- 14 5 080103A-2014 -- 15 6 080103A-2015 -- 16 7 080103A-2016 -- 17 43 080103A-2017 -- 18 8 080103A-2018 -- 19 9 80103A-2019 -- 20 10 080103A-2020 -- 21 11 080103A-2021 -- 22 44 080103A-2022 -- 23 45 080103A-2023 -- 24 12 080103A-2024 -- 25 13 080103A-2025 -- 26 14 080103A-2026 -- 27 15 080103A-2027 -- 28 16 080103A-2028 -- 29 46 080103A-2029 -- 30 47 080103A-2030 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC072503-0,0 ng/L Standard XCO72503-1, 25 ng/L Standard XC072503-2, 50 ng/L Standard XC072503-3,100 ng/L Standard -- XC072503-4, 250 ng/L Standard -- XC072503-5, 500 ng/L Standard -- XC072503-6,1000 ng/L Standard Methanol Wash -- Reagent Blank -- Reagent Spk A, 50 ng/L ~ Reagent Spk B, 500 ng/L -- XC072503-1, 25 ng/L Standard L34910-5 Spk C, 5000 ng/L, DF=10 ~ L34910-10 Spk D, 5000 ng/L, DF=10 -- L34910-11 Spk E, 5000 ng/L, DF=10 -- L34910-20 Spk F, 5000 ng/L, DF=10 -- XC072503-2, 50 ng/L Standard -- L34910-5 -- L34910-5 Rep L34910-10 -- L34910-10 Rep -- XC072503-3, 100 ng/L Standard XC072503-4,250 ng/L Standard -- L3491-11. L34910-11 Rep -- L34910-20 -- L34910-20 Rep -- L34910-21 -- XC072503-5, 500 ng/L Standard -- XC072503-6,1000 ng/L Standard 000280 1 Exygen study n o . ( Page 1 Page Position: (1,1) Sample Type Cone (ng/L) Cone B Cone C Test ID DF Standard Standard Standard Standard Standard Standard Standard Blank Blank QC QC Standard QC QC QC QC Standard Analyte Analyte Analyte Analyte Standard Standard Analyte Analyte Analyte Analyte Analyte Standard Standard 0 25 50 100 250 500 1000 100 500 25 5000 5000 5000 5000 50 100 250 500 1000 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 0 10 -- 0 10 -- 0 10 -- 0 10 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 -- 01 i( Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemicals.PRO\SampleDB\080103A Decatur BC.SPL Printed: Fri Aug 01 15:28:30 2003 JA/) ________ MS Method HPLC Method MS Tune File Inj.Volume 1 C6 C8 SULF C8 ACID PFOSA 2 C6 C8 SULF CB ACID PFOSA 3 C6 C8 SULF C8 ACID PFOSA 4 C6 C8 SULF C8 ACID PFOSA 5 C6 C8 SULF CB ACID PFOSA 6 C6 C8 SULF C8 ACID PFOSA 7 C6 C8 SULF C8 ACID PFOSA 8 C6 C8 SULF C8 ACID PFOSA 9 C6 C8 SULF C8 ACID PFOSA 10 C6 C8 SULF C8 ACID PFOSA 11 C6 C8 SULF C8 ACID PFOSA 12 C6 C8 SULF C8 ACID PFOSA 13 C6 C8 SULF C8 ACID PFOSA 14 C6 C8 SULF C8 ACID PFOSA 15 C6 C8 SULF C8 ACID PFOSA 16 C6 C8 SULF C8 ACID PFOSA 17 C6 C8 SULF C8 ACID PFOSA 18 C6 C8 SULF C8 ACID PFOSA 19 C6 C8 SULF C8 ACID PFOSA 20 C6 C8 SULF CB ACID PFOSA 21 C6 C8 SULF C8 ACID PFOSA 22 C6 C8 SULF C8 ACID PFOSA 23 C6 C8 SULF C8 ACID PFOSA 24 C6 C8 SULF C8 ACID PFOSA 25 C6 C8 SULF C8 ACID PFOSA 26 C6 C8 SULF CB ACID PFOSA 27 C6 C8 SULF C8 ACID PFOSA 28 C6 C8 SULF C8 ACID PFOSA 29 C6 C8 SULF C8 ACID PFOSA 30 C6 CB SULF C8 ACID PFOSA pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs wafer pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 000281 1 Exygen study n o . Page 2 Page Position: {2,1 ) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exveen Study No: L34910 Instrument: Computer: Micromass Quattro Ultima (LC/MS/MS Unit #6) 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 Bin 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: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are com puter generated printouts from the m asslynx software program . The pages contain the instrum ent settings used for the analysis o f this data set. All Handwritten Peak ID's by: 000282 Scanning Method Report Page 1 Method: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 C8 SULF C8 ACID PFOSA Last Modified: Thu Jul 31 16:23:50 2003 Printed: Fri Aug 01 15:29:10 2003 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 MRM of 4 Mass Pairs { ESP- ) Inter Channel Delay i( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone I 399.00 80.00 0.20 2 413.00 369.00 0.20 3 498.00 78.00 0.20 4 499.00 99.00 0.20 35 10 30 40 50 10 50 30 000283 Method Report Method File: Last Modified: Printed: c :\masslynx\fluorochemicals.pro\acqudb\pfbs water Friday, August 01, 2003 15:20:36 Friday, August 01, 2003 15:29:16 Page 1 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 10.0 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 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time 0.00 2.00 5.00 9.00 9.50 14.00 14.50 20.00 A% 90.0 90.0 10.0 10.0 0 .0 0.0 90.0 90.0 B% 10.0 10.0 90.0 90.0 100.0 1 0 0 .0 10.0 10.0 C% 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 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contactl Off On Off Off Off Off Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300 Contact4 Off Off Off Off Off Off Pressure 400 400 400 400 400 400 400 400 HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (il/min) Draw Position (mm) Stop Time (mins) Injection Volume (il) Vial Number 200.0 200 0.50 20.00 15.0 69 000284 .jp Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS Printed: Fri Aug 01 15:29:30 2003 Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block. Temp. Desolvation Temp. Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -33 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.3e-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 Rdl 14.0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650 36 19 40 -6' Rdbk 131.8 751.3 000285 Quantify Calibration Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 1 Calibration: P :\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\CurveDB\080103A Decatur BC Last modified: Sun Aug 03 07:26:03 2003 Printed: Sun Aug 03 07:32:22 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000286 Quantify Calibration Report Study No.:L34910, Set No.:080103A, 2xt.Date:08/01/03, Analyst:K.Risha Page 2 Calibration: P:\Data\LGHSMS6\Hasslynx\Fluorochemicals.PR0\CurveDB\080103A Decatur BC Last modified: Sun Aug 03 07:26:03 2003 Printed: Sun Aug 03 07:32:22 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 0002S7 Quantify Calibration Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, AnalystsK.Rieha Page 3 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\0801Q3A Decatur BC Last modified: Sun Aug 03 07:26:03 2003 Printed: Sun Aug 03 07:32:22 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000288 Quantify Calibration Report Study No.:L34910, Set No.s080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 4 Calibration: P:\Data\LCMSMS6\Masslyxuc\Fluorochemicals.PRO\CurveDB\080103A Decatur BC Last modified: Sim Aug 03 07:26:03 2003 Printed: Sun Aug 03 07:32:22 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000289 Quantify Sample Report Study No.:L34910, Set N o . :080103A, Ext.Date:08/01/03, Analyst:K.Riaha Paga 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Sun Aug 03 07:32:25 2003 Initial*_ _ _ _ _ Date ce io ilo ? > % =- Run# c60lc*A-2O 0\ To o S o i o3A - zasO Name: 080103A-2001 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000290 Quantify Sample Report Study No.SL34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Eata\LCMSMS6\Mas3lynx\Fluorochemicals.PRQ\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2001 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000291 Quantify Sample Report Study No-:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SamplaDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2002 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000292 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst :K.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheinicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2002 Text: 4: PFOSA Exygen Research 3058 Research Drive, State College, PA 16801 000293 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluoxochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Hasslynx\Fluoxochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2003 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000294 Quantify Sample Report \ ^ f Study No.;L34910, Set No. 080103*., Ext.Date:08/Ql/03, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\08Q103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Dacatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2003 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16,801 000295 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, AnalystjK.Rlsha Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2004 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000296 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:Q8/01/03, Analyst:K.Risha Page 8 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2004 Text: 4: PFOSA XC072503-3,100 ng/L Standard 080103A-2004 Sm (Mn, 2x3) 100-1 %- 02-Aug-2003 03:32:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 15082 7.93e4 Area 0 1I 111 r-i ' I Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000297 Quantify Sample Report Study No.:L34910, Set No.:080103Af Ext.Date:08/01/03, Analyst:K.Risha w Page 9 Sample List: Last modified; Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\Q80103A Decatur BC Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2005 Text: 1: C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 080103A-2005 Sm (Mn, 2x3) 100i %- 9.13 78794 02-Aug-2003 03:54:13 LC/MS/MS #6 MRM of 4 Channels ES413 >369 4.78e5 Area 2.00 4.00 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 080103A-2005 Sm (Mn, 2x3) 1 0 0 -1 %- 6.00 " ' 'I ' 8.00 I"1 10.00 Time 12.00 8.98 15770 02-Aug-2003 03:54:13 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 9.57e4 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000298 Quantify Sample Report Study No.:1*34910, Set No.:080103A, Ext.Date:08/01/03, Analyst-.K.Risha Page 10 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2005 Text: 4: PFOSA w w Exygen Research, 3058 Research Drive, State College, PA 16801 000299 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2006 Text: 1: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 080103A-2006 Sm (Mn, 2x3) 100n %- 9.12 1716341 1 1 02-Aug-2003 04:15:54 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1 .0 1 e6 Area Ch "r * T-i i Time....................... , 1 , i 'i II 1i 1| --T' " '11 Ii--" 1i" "" 1| r 1 i1 'rI '- 'I ' I1 n' " I 1 1i -T " ' 1 7 "" ' r' ~ r' r' "TT 1 r1 " T' 11 I -1 *' 1.........................iI I1 1 -rr--i r 'II--rr---ri i ii- i| II II 2.00_________ 4.00 6.00 8.00 10.00 12.00 ,2: C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 080103A-2006 Sm (Mn, 2x3) 100- %- 8.98 312811 1 1 02-Aug-2003 04:15:54 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.90e5 Area CH ................. 1 1 ' 1 I ' ' 2.00 i" [' T " i r'-'i I i --r "i 4.00 , r ........... I ' " ' T " T 1 6.00 1" '""I 1 ' ' 8.00 '............. i ' 10.00 I ' ' -|-- 1 Time 12.00 3: C8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 080103A-2006 Sm (Mn, 2x3) inn- %: o 2.00 4.00 02-Aug-2003 04:15:54 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 11I191711 1.11e5 Area -------------------------------- ^ i r '1 'I- .............. Time 6.00 8.00 10.00 _______ 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 000300 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Dacatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2006 Text : 4 : PFOSA XC072503-5, 500 ng/L Standard 080103A-2006 Sm (Mn, 2x3) 10Ch %- 02-Aug-2003 04:15:54 LC/MS/MS #6 MRM of 4 Channels ES- 9.92 498 > 78 72894 3.82e5 Area T Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 000301 Quantify Sample Report Study No.:L34910, Set N o .:080103A, Ext.Date:08/01/03, Analyst:K.Riaha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2007 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) XC072503-6,1000 ng/L Standard 080103A-2007 Sm (Mn, 2x3) 100n %- %0 Q -l. r .,.r -- i-- r - | . . f - p , , t-- 'i ' r r " i i | - r - r " i r " T t " p v r - i i p r 2.00 4.00 6.00 02-Aug-2003 04:37:34 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.12e5 Area i'T '> i i 10.00 i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000302 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, AnalystsK.Riaha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMSG\Masslynx\Fluorochamicals.PROVMethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2007 Text: 4: PFOSA XC072503-6,1000 ng/L Standard 080103A-2007 Sm (Mn, 2x3) 10Ch 02-Aug-2003 04:37:34 LC/MS/MS #6 MRM of 4 Channels ES- 9.92 498 > 78 137821 7.22e5 Area 0- T 2.00 4.00 T 6430 8.00 * 10.00 i ....... Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000303 Quantify Sample Report ^ t Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P :\Data\LCMSMS6\Masslynx\Fluorocheraicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sim Aug 03 07:32:25 2003 Name: 080103A-2008 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) %0 Exygen Research, 3058 Research Drive, State College, PA 18801 000304 Quantify Sample Report Study No.:L34910, Sat No.:080103A, Ext.Date:08/01/03, Analyst:K.Riaha Page 16 Sample List: P:\Data\LCMSUS6\Hasslyruc\Fluorochemicals.PR0\SanvlaDB\080103A Decatur BC Laat modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2008 Text: Zxygen Research, 3058 Research Drive, State College, PA 16801 000305 Quantify Sample Report Study No.:L34910, Set N6.:080103A, Ext.Date:08/01/03, AnalystsK.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslyux\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2009 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 1S801 Quantify Sample Report Study No.:L34910, Set No.:080103A, Bxt.Date:08/01/03, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2009 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000307 Quantify Sample Report Study No.:L34910, Set No.;080103A, Ext.Date:08/01/03, Analyst:K.Risha Page ]_ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheniicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Marne: 080103A-2010 Text: 1: C8 Acid (PFOA) Reagent Spk A, 50 ng/L 08Q103A-2010 Sm (Mn, 2x3) 100n %- A- / \ 2 .0 0 'r i i I"' 1 1 1 4.00 6 .0 0 02-Aug-2003 05:42:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 >369 1I189391 I 1.1265 Area 1 ' * 1 pi.-!-T-r=*pT=p"T" l-,i 1-1 1 1 i 1 "'"p-r-i rime 8 .0 0 1 0 .0 0 1 2 .0 0 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000308 Quantify Sample Report L^y Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sanj>leDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2010 Text: 4 : PFOSA %0 Exygen Research, 3058 Research Drive, State College, PA 16801 000309 Quantify Sample Report V Study No.:L34910, Set No.:080103A, Ext.Data:08/01/03, Analyst:K.Risha Page 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRa\SaxnplaDB\0B01Q3A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorbchemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2011 Text: 1: C8 Acid (PFOA) Reagent Spk B, 500 ng/L 080103A-2011 Sm (Mn, 2x3) 1 0 O- %- 9.15 1630631 1 1 02-Aug-2003 06:04:23 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 9.90e5 Area 0 : t i "pi i r" r I 1 r-r i-i | - i \ m\ i l \ ryrr" 2.00__________ 4JD0__________ 6,00__________8.00 '"i* - 1 1 ' - ' i " ' 1 1 Time 10.00 12.00 w 2: C6 Sulfonate (PFHS) Reagent Spk B, 500 ng/L 080103A-2011 Sm (Mn, 2x3) 10Ch /< r 02-Aug-2003 06:04: LC/MS/MS #6 MRM of 4 Channels ES8.99 399 > 80 1.83e5 Area 0 - L'^'' '-- 1 i....... i 1 r"i .... .... 1 1 1 1 |-'-r- '~r i T ' 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) 8.00 10.00 - n Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000310 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2011 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000311 Quantify Sample Report Study N o . 1.34910, Set No.:080103A, Ext.Date:08/01/03, AnalystsK.Risha Page 23 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2012 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 06312 Quantify Sample Report Study No.:L34910, Sat No.:080103A, Ext.Date:Q8/01/03, AnalystsK.Risha Page 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2012 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000.313 I, Quantify Sample Report <1 Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2013 Text: 1: C8 Acid (PFOA) L34910-5 Spk C, 5000 ng/L, DF=10 080103A-2013 Sm (Mn, 2x3) 10<H %- 9.13 157971 02-Aug-2003 06:47:56 LC/MS/MS #6 MRM of 4 Channels ES413 >369 9.32e5 Area C H -t 1I1 2.00 1 I 1 ' 1 1 I 1 1 ....... I ' 4.00 6.00 ' i 1 1 1 T ' 1 1 1 i Time 8.00 10.00 12.00 2: c6 Su1fonate (PFHS) L34910-5 Spk C, 5000 ng/L, DF=10 080103A-2013 Sm (Mn, 2x3) 10CH %i 8.98 307461 I [ 02-Aug-2003 06:47:56 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.76e5 Area o- I ' ' II 1 11 1 '1 r1 '1"' 1 ' 1 I I1 I1-r" I' I' ;1 I' I1 r - i' 1) , .' . I 1 1 1 1I - -'" . . I I - 11---` I[ ' .' ''---r '---J -1-- ,...........I |Ti| mli e 2.00 4.00 6.00 8.00__________10.00_________ 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000314 Quantify Sample Report . ^ Study No.:L34910, Set No.:0B0103A, Ext.Date:08/01/03, Analyst:K.Risha Pag 26 Saitla List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Ma8Slynx\Fluorochemicals.PR0\MetbDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2013 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 00031.5 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date;08/01/03, Analyst:K.Risha Page 27 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 0S0103A-2014 Text: 1: C8 Acid (PFOA) L34910-10 Spk D, 5000 ng/L, DF=10 080103A-2014 Sm (Mn, 2x3) 100- %- 9.13 1661341 1 02-Aug-2003 07:09:35 LC/MS/MS #6 MRM of 4 Channels ES413 >369 9.88e5 Area 0 - 11 11 1 1 1 1 1 1 1 1 1 1 1 1 1 i 1 1 1 Time' ' ' T > r " 1' 1' II 'i'' 1 1 1 [ T " '1 '' '1 I '1 1 ' '1 ' I 1 '1 '1 1 !1 '1 11 '' l - i 1; 1! 1r 11 1i I1 11 *, '1 1, ^I 1 1 1 1 Ii ' 1 " 1 1 I 1 " T - 1| I II 2.00__________ 4X10__________ 6X0__________ 8 X 0 _________ 10X0 12.00 3: CB Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 316 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 28 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2014 Text : 4: PFOSA %0 Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 317 Quantify Sample Report Study No.:L34910, Sat N o .:080103A, Ext.Date:08/01/03, Analyst:X.Risha Page 29 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2015 Text: 1: C8 Acid (PFOA) L3491Q-11 Spk E, 5000 ng/L, DF=10 080103A-2015 Sm (Mn, 2x3) 100- %- 02-Aug-2003 07:31:17 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 >369 11876661 1 1.11 e6 Area Ch 1 ,1 > -T f1 1 '"i 1 r 11 i"1' 111 \ 1 1 1 i 1 1 ' 1 i 1 r"' r' l' ' r r '< I i-- 'T~r >t ' i ' ' i Time ____________ ZOO_______ 400_______ 6T)0_______ aoo_______ loop_______12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) w Exygen Research, 3058 Research Drive, State College, PA 16801 0Ool8 Quantify Sample Report . ^ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Pag 30 Sample List: P:\Data\LCMSMS6\Hasslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2015 Text : 4: PFOSA L34910-11 Spk E, 5000 ng/L, DF=10 080103A-2015 Sm (Mn, 2x3) 100-1 %- 02-Aug-2003 07:31:17 LC/MS/MS #6 MRM of 4 Channels ES- 9.88 498 > 78 15509 7.93e5 Area O W T 2.00 4.00 T T T' 6.00 TT 8.00 10.00 ->-i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 319 Quantify Sample Report V*/ Study No.:L34910, Sat N o .:080103A, Ext.Date:08/01/03, Analyst:K.Riaha Page 31 Sample List: P:\DataNLCMSMS6\Masslynx\Fruorochamicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2016 Text: 1: C8 Acid (PFOA) L34910-20 Spk F, 5000 ng/L, DF=10 02-Aug-2003 07:52:54 LC/MS/MS #6 080103A-2016 Sm (Mn. 2x3) MRM of 4 Channels ES- 100: 9.13 1790901 413 >369 1.02e6 1 Area 1%- n 1 ' 1 i 1 i 1 ' i i "> 1 1 i 1 ` 1 1 ' ' > 1 1 ` , -P-l- | ! 1 `r~i 1 i' ' 111' i 1 * * i Time 2.00 4.00 6.00 8.00 10.00 12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-20 Spk F, 5000 ng/L, DF=10 080103A-2016 Sm (Mn, 2x3) 100] %- 0 ` ' 1 I ' ' 1 I 1 ' 1 r "l T~ r ~ l ' |-- I""' - T - l -- I ! I I T '*I I 2.00 4.00 6.00 02-Aug-2003 07:52:54 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.13e5 Area 10.00 i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000320 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Rage 32 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemical8.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2016 Text: 4 : PFOSA L34910-20 Spk F, 5000 ng/L, DF=10 080103A-2016 Sm (Mn, 2x3) 100-1 %: 02-Aug-2003 07:52:54 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 >78 100640 1 5.19e5 Area 0 1 I 1 1 I 1 1 1-1 I11 1 1 1 I ... . I"r~'~i'' I ' t - i Time 2.00 4.00 6.00 8.00 10.00 12.00 'i Exygen Research, 3058 Research Drive, State College, PA 16801 &Q0321 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 33 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2017 Text: 1: C8 Acid (PFOA) w Exygen Research, 3058 Research Drive, State College, FA 16801 000322 Quantify Sample Report Study No.;L34910, Set No.:080103A, Ext.Date:08/01/03, AnalystsK.Risha paffe 34 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sar^)leDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2017 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 0003^3 Quantify Sample Report Study No.:L34910, Set No.;080103A, Ext.Date:08/01/03, Analyst:K.Risha page 35 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2018 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-5 080103A-2018 Sm (Mn, 2x3) 100-1 %- O-1- '1 i' i) i 2.00 T -I-T 4.00 6.00 02-Aug-2003 08:36:27 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.58e5 Area 1 i 1 1-- 1 1 i 111 1 1 i Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000324 Quantify Sample Report Study No. .-L34910, Set N o . :080103A, Ext.Date: 08/01/03, Analyst :K.Risha Page 36 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemioals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\MasslyHx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2018 Text: 4 : PFOSA L34910-5 080103A-2018 Sm (Mn, 2x3) 100; %- 02-Aug-2003 08:36:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1218821 6.28e5 I Area 0- 1 1 ' 1 1 1 ' ' 1 2 .0 0 111 4.00 i i , > ] i 'l 1 i 6 .0 0 i ' ' ' 8 .0 0 i r i ' 1? 1 0 .0 0 t ' ' ' i Time 1 2 .0 0 V Exygen Research, 3058 Research Drive, State College, PA 16801 000325 Quantify Sample Report Study No.:L34910, Set N o . :080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SanpleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2019 Text : 1 : C8 Acid (PFOA) 2: C 6 Sulfonate (PFHS) 3: C 8 Sulfonate (PFOS) L34910-5 Rep 080103A-2019 Sm (Mn, 2x3) 100: %- 02-Aug-2003 08:58:12 LC/MS/MS #6 1I9.25 510741 MRM of 4 Channels ES499 > 99 3.06e5 Area 0 - r-t" i T"] r i i r,,j' i "p f"r*-r"r-vr i | i i r i |,i"r" i "t 1 i 1 1 1 ' "T ' 2.00 4.00 6.00 ................. ^ i r-r-r--r-T-T in Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000326 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 38 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2019 Text : 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000327 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Riaha Page 39 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaiHpleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2020 Text: 1: C 8 Acid (PFOA) L34910-10 080103A-2020 Sm (Mn, 2x3) 100n %- 9.13 1950551 1 1 02-Aug-2003 09:19:59 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.13e6 Area 0- ..................................... "r 1 1 1 ' 1"1 1 ' 1 1 1 ' ' 1 1 TM '-'-'-i..... . 1 ' ' ' 1 Time 2.00__________ 40__________ 6,00__________ a00_______ 10.00 12.00 V 2: C 6 Sulfonate (PFHS) L34910-10 080103A-2020 Sm (Mn, 2x3) 10O] %: 02-Aug-2003 09:19:59 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 6.71e4 Area 0 ' 1 ' I ' I ' 1 1 I ' I .... ` T ' ' I '' 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) L34910-10 080103A-2020 Sm (Mn, 2x3) 100n 10.00 --i Time 12.00 9.25 93844 02-Aug-2003 09:19:59 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 5.38e5 Area 2.00 ~r ~r i ~ ' " ' 1 I" 4.00 6.00 T -1- T --r* 8 00 10.00 r-r-i Time 12.00 %0 Exygen Research, 3058 Research Drive, State Collage, PA 16801 000328 Quantify Sajnple Report ^ Study No.:L34910, Set No.:Q80103A, Ext.Date:08/01/Q3, Analyst:K.Risha Page 40 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2020 Text : 4: PFOSA L34910-10 080103A-2020 Sm (Mn, 2x3) 100~i 02-Aug-2003 09:19:59 LC/MS/MS #6 MRM of 4 Channels ES- 9-91 _ 498 > 78 1337631 6.89e5 Area T I ' ' I'I'I" 2.00 T-rrrrr 4.00 6.00 8.00 10.00 '-pi Time 12.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 000329 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 41 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\0801Q3A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2021 Text: 1: C8 Acid (PFOA) W 2: C 6 Sulfonate (PFHS) L34910-10 Rep 080103A-2021 Sm (Mn, 2x3) 100] %- 02-Aug-2003 09:41:47 LC/MS/MS #6 MRM of 4 Channels ES8.98 399 > 80 7.94e4 Area Q " ,~i 1 1 i ..... . I I I *-r-` I 2.00 4.00 3: C 8 Sulfonate (PFOS) L34910-10 Rep 080103A-2021 Sm (Mn, 2x3) 100^ %- 0- %0 2.00 4.00 "t~r--r 6.00 6.00 f-n Time 8.00 10.00 12.00 02-Aug-2003 09:41:47 LC/MS/MS #6 19.24 1063501 MRM of 4 Channels ES499 > 99 6.22e5 Area [ 8.00 ^ 1 I 1 1 1 1T 1 ' i|" 1 1 Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000330 Quantify Sample Report Study No.SL34910, Set No.s080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 42 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2021 Text: 4: PFOSA L34910-10 Rep 080103A-2021 Sm (Mn, 2x3) 100- %- AV- 1 1 * i ' i ` 1 ' i 2.00 4.00 02-Aug-2003 09:41:47 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 1912011 9.92e5 11 Area i-'"' i >' ' 1 1 r~~' i 1 1 1 i 1 1 1...P 1 1 i-1""' ' ' i Time 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000331 Quantify Sample Report Study No.:L34910, Sat N o .:080103A, Ext.Date:08/01/03, Analyst:K .Riaha Page 43 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2022 Text : 1: C 8 Acid (PFOA) 2: C 6 Sulfonate (PFHS) 3: C 8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000332 Quantify Sample Report / Study No.:L34910, Set No.:080103A, Ext.Dates08/01/03, AnalystsK.Riaha Page 44 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2022 Text: 4: PFOSA XC072503-3,100 ng/L Standard 080103A-2022 Sm (Mn, 2x3) 100- %- A_ Ir ' ] 11 . 2.00 1 1 1 1 1 T T -T 1 4.00 02-Aug-2003 10:03:27 LC/MS/MS #6 MRM of 4 Channels ES- 9-9 146981 498 > 78 7.86e4 1I Area 1 1 r 111 ' 1 ......... .. 1 1 ' ........... ................ 1 ........ .1 Time 6.00 8.00 10.00 12.00 w Exygen Research, 3058 Research Drive, State College, PA 16801 000333 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 45 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SamipleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MetbDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2023 Text: 2: C 6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 080103A-2023 Sm (Mn, 2x3) 10CH %: 0 1 ' l'- ....... I 1 ' 2.00 r"r"'' '..<-[ -I- 1--r-T.f- l--II ..T-T-T- 4.00 6.00 3: C8 Sulfonate (PFOS) 02-Aug-2003 10:25:10 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 9.02e4 Area ' "I"............ 10.00 1 Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000334 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 46 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2023 Text: 4: PFOSA M0 Exygen Research, 3058 Research Drive, State College, PA 16801 000335 Quantify Sample Report \ ^ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 47 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2024 Text: 1: C 8 Acid {PFOA) L34910-11 080103A-2024 Sm (Mn, 2x3) 100-1 %- 02-Aug-2003 10:47: LC/MS/MS #6 MRM of 4 Channels ES9.12 413> 369 2.88e6 Area 0T '"I 111 1~i~i ' ' ' 1 Time 2.00 400 (LOO 8.00 10.00 12.00 2: C 6 Sulfonate (PFHS) L34910-11 080103A-2024 Sm (Mn, 2x3) 100- %: 02-Aug-2003 10:47:05 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 1181331 1 1.03e5 Area o- L~r ' ' '' 1 ........... 1 1' 1.........-'-I .... I"1 1 r ......... r 1 1~1" 1 1 1 1 1 .............. I ' ' i i Time 2.00__________ 400__________ 6X10__________ 8.00__________10.00_________ 12.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 000336 Quantify Sample Report Study No.:L34910, Set No.:0S0103A, Ext.Dates08/01/03, AnalystsK.Risha Page 48 Sample List: P:\Data\LCMSMS6\Masalynx\Fluorocheaiicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2024 Text: 4 : PFOSA L34910-11 080103A-2024 Sm (Mn, 2x3) 10CH %- O- 1'1 ' 1 1 ' ` ' "I > I 111 i i1"' 1 ' 1 1'IT" 1 2.00 4.00 6.00 02-Aug-2003 10:47:05 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 12155331 6.18e6 II Area 1 1 11 ' 1 1 ...... 1 1 1 ' ' T ' ' T ~r~i ' ' 1 1 i Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000337 Quantify Sample Report . Study No.-.L34910, Set No.:080103A, Ext .Dates 08/01/03, Analyst -.K.Risha Page 49 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheiaicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2025 Text: 1: C 8 Acid (PFOA) L34910-11 Rep 080103A-2025 Sm (Mn, 2x3) 100i %- 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of 4 Channels ES9.12 413 >369 2.77e6 Area 0j~r"1 .T -T "i 1 1"1 1 I 1 1 1 1 I Time 2.00 Zoo Zoo 8.00 10.00 12.00 w 2: C 6 Sulfonate (PFHS) L34910-11 Rep 080103A-2025 Sm (Mn, 2x3) 10CH 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of 4 Channels ES8.96 399 > 80 1.09e5 Area %- . 0 ' 1 * 1 I ' 1 1 I-1 1 '~r I 1-f"1 I I 1 ' I I I I ' ' I I 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) L34910-11 Rep 080103A-2025 Sm (Mn, 2x3) 100- %- o- --1-- 1"1 1 1 1 1 1 1 r >[--T11i "T.i",r ,r,T i~r~' 2.00 4.00 6.00 1 8.00 T 1 1 1~'"i 1 1 1 I Time 10.00 12.00 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.26 499 > 99 117943531 I 1.00e7 Area ` 1 ' ' 1^ W", i~! I I r-| 1 -I--111 '1 Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000338 Quantify Sample Report Study Mo. s1.34910, Set No.:080103A, Ext.Date:08/01/03, AnalystsK.Risha Page 50 Sample List: P:\Data\LCMSMS6\Masslynx\FlUorochemicals.PR0\SainplaDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicala.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2025 Text: 4: PFOSA L34910-11 Rep 080103A-2025 Sm (Mn, 2x3) 10CH %- 0- 1 ' 1 ' 1 ' 1 ' ' 1 1 ' ' 1 2.00 4.00 --'----'--1--i--'--'--'--'--i 6.00 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.87 498 > 78 9297711 4.73e6 i Area ........... .. 1 ~i" i 1 ' > .i Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College PA 16801 000339 Quantify Sample Report ,<i^, Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Riaha Page 51 Sample List: P:\Data\LCMSMS6\Masslynx\Kluorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Dscatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2026 Text: 1: C 8 Acid (PFOA) L34910-20 080103A-2026 Sm (Mn, 2x3) 100- %- 9.12 4042091 I 1 02-Aug-2003 11:30:26 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.37e6 Area 0- ' 1 1 1 I 1 1 1 ' I 1 1 1 1 r 1 * '- t- ' i 1 1 1 1 1"1 1- r ,-- T" ' ' ,'" 'r T ' 1 ' ' ' ' " T~i' 1 1 1 1 1 ' 1 I Time ________________ Z 00__________4^00__________6JD0__________aoo_________ 10,00_________ 12,00 \<m/ 2: C 6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-20 080103A-2026 Sm (Mn, 2x3) 10Ch %- a I"'" 1 ' ' ' I 1 1 ' ' - T'1" '-"1" '1T~ ' ~ 2.00 4.00 6.00 02-Aug-2003 11:30:26 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.35e6 Area 10.00 t-' Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000340 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst.`K.Risha Page 52 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\08Q103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Mame: 080103A-2026 Text: 4: PFOSA L34910-20 080103A-2026 Sm (Mn, 2x3) 100-1 02-Aug-2003 11:30:26 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 >78 412369 I 2.10e6 Area O-L-t 'i~r ' 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 W W Exygen Research 3058 Research Drive, State College, PA 16801 000341 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 53 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochsmicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2027 Text: 1: C 8 Acid (PFOA) L34910-20 Rep 080103A-2027 Sm (Mn, 2x3) 100i 9.13 301201 02-Aug-2003 11:52:11 LC/MS/MS #6 MRM of 4 Channels ES 413 >369 1.76e6 Area 2.00 2: C 6 Sulfonate (PFHS) L34910-20 Rep 080103A-2027 Sm (Mn, 2x3) 100n 1 I'' 4.00 6.00 1 11 I '.1 8.00 10.00 Time 12.00 8.97 16649 02-Aug-2003 11:52:11 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 9.68e4 Area i 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000342 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 54 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRQ\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2027 Text : 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 $00343 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Paffe 55 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Auff 03 07:25:44 2003 Method: P:\Data\LCMSHS6\Hasslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Auff 03 07:11:59 2003 Job Code: Printed: Sun Auff 03 07:32:25 2003 Name: 080103A-2028 Text: 1: C 8 Acid (PFOA) 2: C6 Sulfonate (PFHS) L34910-21 080103A-2028 Sm (Mn. 2x3) 100n %: 02-Aug-2003 12:13: LC/MS/MS #6 MRM of 4 Channels ES8.98 399 > 80 2.11eS Area 0 1 1 I 1 I 11 1 1 I 1 1 1 '"I 1 1 1 I 1 * 1 1 i * 2.00 4.00 6.00 3 : C 8 Sulfonate (PFOS) L34910-21 080103A-2028 Sm (Mn, 2x3) 10Ch %- cy T-I |~l ' ' I '.'~T- ' 2.00 1 ' T"1 ' T ...... i" t t"r ii"ri 4.00 6.00 ............... .. r i-i Time 8.00 10.00 12.00 02-Aug-2003 12:13:52 LC/MS/MS #6 |19.25 4098211 MRM of 4 Channels ES499 > 99 2.39e6 Area r-n1"i "Tmi 1 8.00 r--;-i t "i -! . . i . Tim6 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000344 Quantify Sample Report tie/ Study No.:L34910, Set No.s080103A, Ext.Dates 08/01/03, AnalystsK.Risha Page 56 Sample List: P:\Data\LCMSMS6\Maaslynx\Fluorochemieals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MetbDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2028. Text: 4 : PFOSA Exygen Research, 3053 Research Drive, State College, PA 16801 000345 Quantify Sample Report Study No.:L34910, Set No.:0B0103A, Ext.Date:08/01/03, Analyst:X.Risha Rage 57 Sample List: P :\Data\LCMSMS6\Masslynx\71uorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2029 Text: 1: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 080103A-2029 Sm (Mn, 2x3) 100- %- 9.13 1400091 1 1 02-Aug-2003 12:35:39 LC/MS/MS #6 MRM of 4 Channels ES413 >369 8.49e5 Area ---------- ------ I1 1 1 1 11 1 1 1 1 1 1 1 1 1(y I ' ' '' I ' ' I1 . , . |-T ~ 1 , . , -- f-- 1 T ~ | -- r ~ l 7-- 1 |- . "! I ' ' I1 | T l - l I I' IT 1 r''' I 1 'T-'' 1 Ir - r 1il - l iI 'r I| '1 ', ', 'r l1TIIIime 2.00__________ 4,00__________ 6XX)__________ 8X30_________ 10.00 12.00 2: C 6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 080103A-2029 Sm (Mn, 2x3) 100- %- 02-Aug-2003 12:35:39 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 1284971 | 1.72e5 Area 0- 1 ' ' r i 1 ' ' "i 1 1 T 1 1"1 1 | 1-i "I" 1 ,' 1 ' 1 i 1 1 i 1 2.00__________ 4X30__________ 6,00__________ 8.00 3: C 8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 080103A-2029 Sm (Mn, 2x3) 10Ch %: ' 1 ' i 1T" 1 '-"i ' ' ' I Time 10.00 12.00 02-Aug-2003 12:35:39 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.02e5 Area 0 -T 1 1 ' ~| 1 ' 1 ` | 1 ' 1 r- 1'T 'i-l . T""r 2.00 4.00 *0 i' 6.00 '"'I I I r , I , I r'i Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000346 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst .-K.Risha Page 58 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sim Aug 03 07:32:25 2003 Name: 080103A-2029 Text : 4: PFOSA XC072503-5, 500 ng/L Standard 080103A-2029 Sm (Mn, 2x3) 10CH %- 02-Aug-2003 12:35:39 LC/MS/MS #6 MRM of 4 Channels ES- 9.88 498 > 78 67231 3.54e5 Area 0 ^T`1 '"1 1 ' ' 1 I'' 2.00 T 1" -- '- 1' I "T' 4.00 6.00 Time 8.00 10.00 12.00 E^ygen Research, 3058 Research Drive, State College, PA 16801 000347 Quantify Sample Report 't*/ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 59 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SasqpleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2030 Text: 1: C 8 Acid (PFOA) 2: C 6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 080103A-2030 Sm (Mn, 2x3) 1 00~i I ' ' ' ' I ' ' 1 ' I ' ' 1~"' I ' 2.00 4.00 3: C 8 Sulfonate (PFOS) 6.00 8.98 54198 02-Aug-2003 12:57:26 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 3.29e5 Area Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000348 Quantify Sample Report Study No.:L34910, Set N o .:080103A, Ext.Date:08/01/03, Analyst:K.Riaha page go Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code; Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2030 Text: w w Exygen Research, 3058 Research Drive, State College, PA 16801 000349 Sponsor Study No: Exygen Study No: Analyte: loos Monitored: Site: NA L3490 PFOA 413 ->369 Decatur Baker's Creek R A W DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 1 5 mL Soil 5.0 g 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 080103AR Karen Risha LCMSMS #6 08/01/03 08/04/03 Exygen LD XC072503-0 XC072503-1 XC0725Q3-2 XC072503-3 XC072503-4 XCQ72503-5 XC072503-6 L34910-II SplcE L349I0-11 Spk E L34910*20 S pkF L34910-5 L34910-5 Rep L34910-10 L34910-10 Rep XC0T2503-1 XC072503-2 L34910-11 L349I0-11 Rep L34910-11 L3491-U Rep L34910-20 L34910-20 Rep XC072503-3 XC072503-4 L34910-20 L349I0-2Q Rep L349IO-21 L 3 4 9 10-21 XC0725Q3-5 XC072503-6 Sponsor ID B C l SED-0 BC2 SED-06 Outfall to River SED-25 BC2 SED-04 BC2 SED-04 BC2 SED-05 BC2 SED-05 - BC2 SED-06 BC2SED-06 BC2 SED-06 BC2 SED-06 Outfall to River SED-25 Outfall to River SED-25 - Outfall to River SED-25 Outfall to River SED-25 O utfall to R iver SED-25 Dup Outfall to River SED-25 Dup Sample Code CS CS CS CS CS CS CS LF LF LF S s s s CS CS s s s s s s CS CS s s s s CS CS Run No. D80103AR-301 080103AR-302 080103AR-303 080103AR-304 080103AR-305 080103AR-306 08Q103AR-307 080103AR-308 080103AR-309 080I03AR-310 080103AR-3U 080103AR-312 080103AR-313 080103AR-314 080103AR-315 080103AR-316 08013AR-317 080103AR-318 080L03AR-319 Q80103AR-32Q 080103AR-321 080103AR-322 080103AR-323 080I03AR-324 080103AR-325 80I03AR-326 080103AR-327 080103AK-328 080103AR-329 080103AR-330 Analyte Found (ppt) * (peak area *intercept) / slope x DF Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)) x 100 amount added (ppt) Std. Cone. (p p O 0 25 50 100 250 500 1000 25 50 too 250 500 1000 Dilution Factor 1000 100 100 10 10 10 10 100 100 10 10 100 100 10 10 too 10 Peak Area 672 13717 29040 51582 113798 242355 469994 3691 29373 28261 18223 14512 32394 31062 12807 25414 9410 9587 80473 76840 7081 5379 41160 96206 61092 44037 10169 99240 215048 406254 Analyte Found (ppo * ** * * ** * * 1780 1700 *0 ** 1340 949 * 2210 Amount Added (ppo Recovery (%) 3000 5000 5000 . Analyte Found (ppb) . . . . . - 14.24 13.60 - 10.72 7J9 - 17.68 - Standard Curve : Linear (1/x weighted) Intercept a 2443.00 Slope 438.457 Coef. O f D e l* 0.990236 Total Solids (%) . - . - 69.96 69.96 69.34 69.54 - 60.41 60.41 60.41 60.41 63.27 63.27 - 63.27 63.27 67.43 67.43 - Analyte Found (ppb)* [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight * analyte found (ppb) x (100% / total solids (%)) CS * Calibration standard C Control sample S * Sample LF * Lab fortified sample FF " Field fortified sample LCS Laboratory Control Spike CK * Check Standard NO * Not detected * Response between 0 and 25 ppt NQ Not quantifiable * Response between 25 ppt sod LOQ (50 ppt) AnaJyte Found (ppb) Dry Weight . . . . . - . . - 23.6 22.5 . . 16.9 12.0 - 26.2 - Spreadsheet prepared by: S am ple was analyzed with several dilution factors in order to accommodate all compounds. The appropriate results are reported. 000350 Sponsor Study No: Exygen Study No: Analyte: loos Monitored: Site: NA L34910 PFOS 499 -> 99 Decatur Baker's Creek R A W DATA REPORT Limit of Quantitation. Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 15pL Soil 5.0 g 5.0 mL Set No; Analyst: Instrument Type: Extraction Date: Analyzed on: 080103 AR Karen Risba LCMSMS #6 08/01/03 08/04/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC0725Q3-5 XC072303-6 L34910-11 SpkE L34910-U SpltE L34910-20SpkF L34910-5 L349L0-5 Rep L34910-10 L34910-10 Rep XC072503-1 XC072503-2 L34910-11 L349I0-U Rep L34910-11 L34910-U Rep L 3 4 9 10-20 U 4910-20 Rep XC072503-3 XC0725Q3-4 134910-20 134910-20 Rep 134910-21 L34910-21 XC072503-5 XC072503-6 Sponsor ID BC2 SED-06 BC2 SED-06 Outfall to River SED-25 BC2 SED-04 BC2 SED-04 BC2SED-05 BC2 SED-05 BC2 SED-06 BC2 SED-06 C2 SED-06 BC2 SED-06 Outfall to River SED-25 Outfall to River SEC-23 Outfall to River SED-25 Outfall to River SED-25 Outfall to River SED-25 Dup O utfall to River SED -25 Dup * ' Sample Code CS CS CS CS CS CS CS LF LF LF S s s s CS CS s s s s s s CS CS s s s s CS CS Run No. 080103AR-30L 080103AR-302 080103AR-3G3 080103AR-304 080103AR-305 0801Q3AR-3Q6 080103AR-307 080103AR-308 080103AR-3Q9 080103A-310 080103AR-3I1 Q8QIQ3AR-312 080103AR-313 080103AR-314 080103AR-315 080103AR-316 080103AR-317 Q80103AR-318 080103AR-319 080103AR-320 080103AR321 080103AR-322 080103AR-323 0&0103AR-324 080103AR-325 080103AR-326 080103AR-327 080103AR-328 080103AR-329 Q80103AR-330 Analyte Found (ppt) * (peak area - intercept) / slope * DF Recovery (%) a [analyte found (ppfl-analyte found ia control (ppt)) x 100 amount added (ppt) Std. Cone. w 0 25 50 100 250 500 1000 - . - 25 50 too 250 500 1000 Dilution Factor 1000 100 100 10 IQ 10 10 100 100 10 10 too 100 10 10 100 10 Peak Area 0 1442 3003 5613 11976 25896 51730 5387 51842 9506 9121 7449 14012 15401 noi 2860 66379 48518 525238 390663 6714 4609 4445 11649 65108 45122 8701 80003 24473 44784 Analyte Found (ppo Amount Added <ppt) Recovery w Analyte Found (ppb) AA *3* 19100 1830 1490 2850 3130 AA AA ** 13400 9010 5000 5000 5000 - (14 14.64 11.92 22.80 25.04 - - 107.20 72.08 * * 175QO 140.00 - Standard Curve: Linear (l/x weighted) Intercept 254.789 Slope a 48.3413 Coef. Of D ei.* 0.991571 Total Solids m . . . . . 69.96 69.96 69.54 69.54 - 60.41 60.41 60.41 60.4] 63.27 63.27 63.27 63.27 67.43 67.43 - Analyte Found (ppb) = [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight analyte found (ppb) x (100% / total solids (%)) CS Calibration standard C Control sample S * Sample LF Lab fortified sample FF * Fteld fortified sample LCS = Laboratory Control Spike CK a Check Standard ND * Not detected 3 Response between 0 and 25 ppt NQ Not quantifiable * Response between 25 ppt and LOQ (50 ppt) Analyte Found (ppb) Dry Weight _ . _ . . . 20.9 17.0 32.8 36.0 . . . . 169 114 . 208 - Spreadsheet prepared by:. S am p le was analyzed with several dilution factors in order to accom m odate ail compounds. The appropriate results are reported. ^S am ple requires reextractioQ. See data set 080603B. m3 000351 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L34910 FOSA 498 -> 78 Decatur Baker's Creek R A W DATA REPORT Limit o f Quantitation. Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 15 fiL Soil 5.0 g 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 080103AR Karen Risha LCMSMS #6 08/01/03 08/04/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC0725M-4 XC072503-5 XC072503-6 U 4910-U Spk E L349I0-11 Spk L34910-2D Spk F L34910-5 L34910-5 Rep L3491Q-IO L349IO-10 Rep XC072503-I XC072503-2 f L34910-11 L34910-II Rep L34910-11 L34910-11 Rep L349I0-20 L34910-20 Rep XC072503-3 XC072503-4 L34910-20 L34910-20 Rep L 3 4 9 10-21 L34910-21 X C 072i03-i XC072503-6 Sponsor ED - - - - BC2 SED-06 BC2 SED-06 Outfall to River SED-25 BC2 SED-04 BC2 SED-04 BC2 SED-05 BC2 SED-05 - - BC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 SED-06 Outfall to River SED-25 Outfall to River SED-25 Outfall to River SED-25 Outfall to River SED-25 Outfall to River SED-25 Dup Outfall to River SED-25 Dup - - Sample Code CS CS CS CS CS CS CS LF LF LF S S S S CS CS s s s s S s CS CS s s s S CS CS Run No. 080103AR-301 080103AR-302 080103AR-303 080103AR-304 080103AR-305 080I03AR-306 080103AR-307 080103AR-308 080103 AR-309 080103AR-310 080103 AR-311 080103 AR-312 OSOIQ3AR-313 080103AR-314 080103AR-315 08013AR-316 080103AR-317 080103AR-318 080103AR-319 080103AR-320 080103AR-321 080103AR-322 080103AR-323 080103 AR-324 080103 AR-325 080103AR-326 080103AR-327 080103AR-328 080I03AR-329 080103AR-330 Analyte Found (ppt) * (peak area * intercept) / slope x DF Recovery (%) * [analyte found (ppt)-analytc found in control (ppt)] x 100 amount added (ppt) Std. Cone. (pp<> 0 25 50 100 250 500 1000 25 50 100 230 . 500 1000 Dilution Factor 1000 100 to o 10 10 10 10 100 100 10 10 100 100 10 10 100 10 Peak Area 0 5040 10269 19684 45565 93155 179184 2308 21870 13524 16680 18189 19503 26862 4380 8991 21988 16805 200293 150384 6516 5371 17628 40103 61447 51717 9119 78207 86063 167421 Analyte Found (ppo Amount Added (p p O Recovery (%) . . . Analyte Found (ppb) ** AA ** 1510 . 5000 5000 5000 12.08 . AA AA . ** a . a* . . -. . 3500 2940 a 4460 . . 28.00 23.52 . . 35.68 _ - -- Standard Curve : Linear (I/x weighted) Intercept = 610.451 Slope * 174.067 Coef. O f Dct. 0.996985 Total Solids w) . . _ . . ,, . . 69.96 69.96 69.54 69.54 60.41 60.41 60.41 60.41 63.27 63.27 63.27 63.27 67.43 67.43 - Analyte Found (ppb) * [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight ~ analyte found (ppb) x (100% / total solids (V*)) CS ~ Calibration standard C * Control sample S " Sample LF = Lab fortified sample FF " Field fortified sample LCS Laboratory Control Spike CK Check Standard ND = Not detected * Response between 0 and 25 ppt NQ * Not quantifiable Response between 25 ppt and LOQ (50 ppt) Analyte Found(ppb) Drv Weicht . _ . ,, . . . . . 17.4 . _ . . . . . . . 44.3 37.2 . 52.9 . - Spreadsheet prepared by: *"Sam ple was analyzed with several dilution factors in order to accom m odate all com pounds. The appropriate results are reported. ^S am p le requires reextraction. See data set 080603B. mu* 000352 <( Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorocheimiicals.PROU\iSampleDB\080103AR Decatur BC SPL Printed: Mon Aug 04 07:47:05 2003 I03,_________________________ Vial File Name LIMS ID Client ID Sample Description Ma 1 41 080103AR-301 2 42 080103AR-302 -- 3 43 080103AR-3Q3 -- 4 44 080103AR-304 -- 5 45 080103AR-305 -- 6 46 080103AR-306 -- 7 47 080103AR-307 -- 8 1 080103AR-308 -- 9 2 0B0103AR-309 -- 10 3 080103AR-310 -- 11 4 080103AR-311 -- 12 5 0801Q3AR-312 -- 13 6 080103AR-313 -- 14 7 080103AR-314 -- 15 42 080103AR-315 -- 16 43 0801Q3AR-316 -- 17 8 080103AR-317 -- 18 9 080103AR-318 -- 19 10 080103AR-319 -- 20 11 080103AR-320 -- 21 12 080103AR-321 -- 22 13 080103AR-322 -- 23 44 080103AR-323 -- 24 45 080103AR-324 -- 25 14 080103AR-325 -- 26 15 080103AR-326 -- 27 16 08013AR-327 -- 28 17 08013AR-328 -- 29 46 080103AR-329 -- 30 47 080103AR-330 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC072503-0, 0 ng/L Standard XC072503-1. 25 ng/L Standard XC072503-2, 50 ng/L Standard XC072503-3, 100 ng/L Standard XC072503-4, 250 ng/L Standard XC072503-5, 500 ng/L Standard XC072503-6. 1000 ng/L Standard L34910-11 SpK E, 5000 ng/L, DF=1000 -- L34910-11 Spk E, 5000 ng/L, DF=100 -- L3491Q-20 Spk F, 5000 ng/L, DF=100 -- L34910-5, DF=10 -- L34910-5 Rep, DF=10 -- L3491O-10, DF=10 -- L34910-10 Rep, DF=10 -- XC072503-1. 25 ng/L Standard -- XC072503-2, 50 ng/L Standard -- L34910-11, DF=100 -- L34910-11 Rep, DF=100 -- L34910-11, DF^IO -- L34910-11 Rep, DF=10 -- L34910-20, DF=100 L3491O-20 Rep, DF=100 XC072503-3, 100 ng/L Standard XC072503-4. 250 ng/L Standard L34910-20, DF=10 L3491O-20 Rep, DF=10 L34910-21. DF=100 L34910-21, DF=10 XC0725Q3-5, 500 ng/L Standard XC07253-6, 1000 ng/L Standard esBooo Exygen study n o . L ^ l O Page 1 Page Position: (1,1) trix Sample Type Cone (ng/L) Cone B Cone C Test ID DF Standard Standard Standard Standard Standard Standard Standard QC QC QC Analyte Analyte Analyte Analyte Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Standard Standard Analyte Analyte Analyte Analyte Standard Standard 0 25 50 too 250 500 1000 5000 5000 5000 -- -- -- -- 25 50 -- -- -- -- -- -- 100 250 -- -- -- -- 500 1000 _ 01 ---- 01 ---- 01 -- -- 01 -- -- 01 ---- 01 -- -- 01 -- -- 0 1000 ---- 0 100 -- -- 0 100 ---- 0 10 ---- 0 10 ---- 0 10 ---- 0 10 ---- 01 ---- 01 -- 0- - - 100 ---- 0 100 -- -- 0 10 -- -- 0 10 ---- 0 100 -- -- 0 100 -- -- 01 ---- 01 -- -- 0 10 -- -- 0 10 -- -- 0 100 -- -- 0 10 ---- 01 ---- 01 <C Masslynx - Sample List Sample List'. CAMASSLYNX\Fluorochemica!s.PRO\SampteDB\080103AR Decatur BC.SPL Printed: Mon Aug 04 07:47:05 2003 MS Method HPLC Method MS Tune File Inj.Volume 1 C6 C8 SULF C8 ACID PFOSA 2 C6 C8 SULF C8 ACID PFOSA 3 C6 C8 SULF C8 ACID PFOSA 4 C6 C8 SULF C8 ACID PFOSA 5 C6 CB SULF C8 ACID PFOSA 6 C6 C8 SULF C8 ACID PFOSA 7 C6 C8 SULF C8 ACID PFOSA 8 C6 C8 SULF C8 ACID PFOSA 9 C6 C8 SULF CB ACID PFOSA 10 C6 C8 SULF C8 ACID PFOSA 11 C6 C8 SULF C8 ACID PFOSA 12 C6 C8 SULF C8 ACID PFOSA 13 C6 C8 SULF C8 ACID PFOSA 14 C6 C8 SULF C8 ACIO PFOSA 15 C6 C8 SULF C8 ACID PFOSA 16 C6 C8 SULF C8 ACID PFOSA 17 C6 C8 SULF C8 ACID PFOSA 18 C6 C8 SULF C8 ACID PFOSA 19 C6 C8 SULF C8 ACID PFOSA 20 C6 C8 SULF C8 ACID PFOSA 21 C6 C8 SULF C8 ACID PFOSA 22 C6 C8 SULF C8 ACIO PFOSA 23 C6 C8 SULF CB ACID PFOSA 24 C6 C8 SULF C8 ACID PFOSA 25 C6 C8 SULF C8 ACID PFOSA 26 C6 C8 SULF C8 ACID PFOSA 27 C6 C8 SULF C8 ACID PFOSA 28 C6 C8 SULF C8 ACID PFOSA 29 C6 C8 SULF C8 ACIO PFOSA 30 C6 C8 SULF C8 ACID PFOSA pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water pfbs water Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 000354 Exygen study n o . 1 3 ^ io Page 2 Page Position: (2,1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exvgen Study No: L34910 Instrument: Computer: Software: Micromass Quattro Ultima (LC/MS/MS Unit #6) COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: HPLC Column: Mobile Phase (A) : Mobile Phase (B) : Analyst: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) 2 mM Ammonium Acetate in Type I Water Methanol Karen Risha 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 m asslynx software program . The pages contain the instrum ent settings used for the analysis of this data set. All Handwritten Peak ID 's by:. 109 0003 Scanning Method Report W Page 1 Method: C:\MASSLXllX\FLUOROCHEMICALS.PRO\ACQUDB\C6 C8 SULF C8 ACID PFOSA Last Modified: Thu Jul 31 16:23:50 2003 Printed: Mon Aug 04 07:47:13 2003 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Secs ) : Span { Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 399.00 80.00 0.20 2 413.00 369.00 0.20 3 498.00 78.00 0.20 4 499.00 99.00 0.20 35 10 30 40 50 10 50 30 W *% 0 000356 Method Report Method File: Last Modified: , m Printed: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs water Monday, August 04, 2003 07:38:50 Monday, August 04, 2003 07:47:18 Page 1 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 10.0 0 .0 0.0 Flow (ml/min) 0.300 Stop Time (mins) 20.0 Min Pressure (bar) 0 Max Pressure (bar) 400 Oven Temperature Left(C) , 35.0 Oven Temperature Right(C) 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time 0.00 2.00 5.00 9.00 9.50 14.00 14.50 20.00 A% 90.0 90.0 10.0 10.0 0.0 0.0 90.0 90.0 B% 10.0 10.0 90.0 90.0 100.0 100.0 10.0 10.0 C% 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 Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contactl Off On Off Off Off Off Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HP11Q0 Autosampler Initial Conditions Draw Speed Eject Speed (/1/min) Draw Position (mm) Stop Time (mins) Injection Volume(/il) Vial Number 200.0 200 0.50 20.00 15.0 27 w 000357 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS. PRO\ACQUDB\FLUOROCHEMS Printed: Mon Aug 04 07:47:28 2003 0) Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -16 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.6e- 3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Plows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 15 2 14.0 14 .0 2.0 650 11 21 14 -647 Rdbk 134.7 765.9 000358 Quantify Calibration Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Rage 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\080103AR Decatur BC Last modified: Tue Aug 05 07:30:00 2003 Printed: Tue Aug 05 07:31:58 2003 bica m ( - w Exygen Research, 3058 Research Drive, State College, PA 16801 000359 Quantify Calibration Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha w Page 2 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\CurveDB\080103AR Decatur BC Last modified: Tue Aug 05 07:30:00 2003 Printed: Tue Aug 05 07:31:58 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000360 Quantify Calibration Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 3 Calibration.: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\080103AR Decatur BC Last modified: Tue Aug 05 07:30:00 2003 Printed: Tue Aug 05 07:31:58 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000361 Quantify Calibration Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Rage 4 Calibration: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\080103AR Decatur BC Last modified: Tue Aug 05 07:30:00 2003 Printed: Tue Aug 05 07:31:58 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000362 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Coda: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Tua Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Tue Aug 05 07:32:01 2003 Initials. D a te . JBjfttelffia Run# 3 f t L 1b C flo tQ J A t- 3 3 .0 Name: 080103AR-301 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) W Exygen Research, 3058 Research Drive, State College, PA 16801 000363 Quantify Sample Report Study No.:L34910, Set N o . :080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-301 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000364 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-302 Text: 1: C 8 Acid (PFOA) 2: C 6 Sulfonate (PFHS) 3: C 8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000365 Quantify Sample Report Study No.:L34910, Sat No.:Q8Q1Q3AR, Ext.Date:08/01/03, Analyst:K.Rista Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-302 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State Collage, PA 16801 000366 Quantify Sample Report x^j Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Riaha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-303 Text : 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0003B7 Quantify Sample Report %m/ Study No.:L34910, Set No.:080103R, Ext .Date:08/01/03, Analyst .-K.Risha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-303 Text : 4: PFOSA XC072503-2, 50 ng/L Standard 04-Aug-2003 09:19:12 LC/MS/MS #6 080103AR-303 Sm (Mn, 2x3) 100i MRM of 4 Channels ES- 9.90 498 > 78 10269 5.34e4 Area %- la T Time 2.00 4.00 6.00 8.00 10.00 w w Exygen Research 3058 Research Drive, State College, PA 16801 000368 Quantify Sample Report W * Study No.:L34910, Set N o .;080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 7 Sample Lists P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified; Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-304 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000369 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 8 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-304 Text: 4: PFOSA____________________________________________________________________________________________ XC072503-3,100 ng/L Standard 04-Aug-2003 09:41:00 LC/MS/MS #6 080103AR-304 Sm (Mn, 2x3) 100^ MRM of 4 Channels ES- 9.92 498 > 78 196841 1,03e5 Area %- n- 1 I T i l l - 1 1 , , . 1 1 1 1 1 r T 1' 1 1 1 1 1 1 ' 1 1 1 ' ' Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000370 Quantify Sample Report Study N o .:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SamspleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-305 Text: 1: C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 080103AR-305 Sm (Mn, 2x3) 10Ch %: 04-Aug-2003 10:02:40 LC/MS/MS #6 9.15 MRM of 4 Channels ES413 >369 6.66e5 Area O '1 - ' - i 1 ' 1 I I ' I t I I I I I r I -r-r-i i |- i ' i i i"T'i 2.00 4.00 6.00 8.00 r1 1 I I I -I I t t-t t Time 10.00 %0i 2: C 6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 080103AR-305 Sm (Mn, 2x3) 1i nv j/sv-_r %\ 8.98 209471 I [ 04-Aug-2003 10:02:40 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1,20e5 Area 0^ ' 1 1 ' 1 1 I 1 1 1 1 1 ........... ! , i i , 1. ...1 t -t-1' r i i i-i 1 1 1 i't Time 2.00 4.00 6,00___________ 8 ^ 0 ___________ 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000371 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 10 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-305 Text : 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000372 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug OS 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-306 Text: 1: C 8 Acid (PFOA) 2 : C 6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 080103AR-306 Sm (Mn, 2x3) 10Ch %: o iI`.I.I<I> 2.00 4.00 6.00 04-Aug-2003 10:24:22 LC/MS/MS #6 8.97 MRM of 4 Channels ES399 > 80 2.48e5 Area 8.00 r-T -r -t-- -r-T t 't-~i r I Time 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000373 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-306 Text: 4: PFOSA Exygen Research 3058 Research Drive, State College, PA 16801 0 0 0 -374 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-307 Text : 1: C8 Acid (PFOA) XC072503-6,1000 ng/L Standard 080103AR-307 Sm (Mn, 2x3) 100-, 9.13 469994 04-Aug-2003 10:46:08 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.69e6 Area 2.00 4.00 2: C 6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 6.00 r- 8.00 0 80103A R -307 Sm (M n ,'2x3) 10Ch %- 8.96 815101 1 [ Ch 1 ............ I ' 1 ' 1 ........................... 1 I . I . I . . . I | 1 I 1 2.00___________ 4,00___________ 6.00 8.00 ' 3: C8 Sulfonate (PFOS) XC072503-6,1000 ng/L Standard 080103AR-307 Sm (Mn, 2x3) 100-1 9.25 51730 10.00 Time 04-Aug-2003 10:46:08 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 4.74e5 Area .i .......... ................Time 10.00 04-Aug-2003 10:46:08 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.90e5 Area "t i 1" i r r- 2.00 ~r~' T" 1 4.00 6.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 10.00 T im e 000375 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date;08/01/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080l03AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslymc\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-307 Text: 4 : PFOSA XC072503-6,1000 ng/L Standard 080103AR-307 Sm (Mn, 2x3) 100-1 %- 04-Aug-2003 10:46:08 LC/MS/MS #6 MRM of 4 Channels ES9.91 498 > 78 9.27e5 Area 0J f ' T I.r - T r -T.J-T 2.00 4.00 6.00 8.00 10.00 ' Time Exygen Research, 3058 Research Drive, State College, PA 16801 000376 Quantify Sample Report Study No. :L34910, Set N o .:080103AR, Ext.Date.-08/01/03, Analyst K.Riaha Page 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SamplaDB\080103AR Decatur BC Last modified: Tua Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS5\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 08Q103AR-308 Text: 1: C8 Acid (PFOA) 2: C 6 Sulfonate (PFHS) Exygen Research, 3058 Research Drive, State College,.PA 16801 000377 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Riaha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheinicals.PRO\Sa3npleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslyxui\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-308 Text: 4 : PFOSA L349 10-11 Spk E, 5000 ng/L, DF=1000 0801 33AR-308 Sm (Mn, 2x3) 10CH %J 04-Aug-2003 11:07:51 LC/MS/MS #6 MRM of 4 Channels ES- 9-90-, 498 > 78 23081 1 .. " 1.26e4 Area U~ " T t 'I t i l - : - , , T " . 2.00 . . , .r I - T - T r - y - i - T - , -T-J r- 1 1 1r1 4.00 6.00 8.00 1 r" 1 ........... . 1 1 . ' ' Tim e 10.00 Exygen Research 3058 Research Drive, State College, PA 16801 000378 Quantify Sample Report Study No.:L34910, Set No.080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-309 Text: 1: C8 Acid (PFOA) L34910-11 Spk E, 5000 ng/L, DF=100 080103AR-309 Sm (Mn, 2x3) 100-] %: 04-Aug-2003 11:29:36 LC/MS/MS #6 9.13 MRM of 4 Channels ES413 >369 1.82e5 Area 0 I-- --i-- I-- I--I--r I I )--r--i--I r~ 'j i-- i-- i--i-- | r i r p 2.00 4.00 6.00 2: C6 Sulfonate (PFHS) I 1 1 ... ' " 8.00 ^n - ^ - r.T T 'T 10.00 Time 3: C8 Sulfonate (PFOS) L34910-11 Spk E, 5000 ng/L, DF=100 080103AR-309 Sm (Mn, 2x3) 100] %- 0 ' ' ' ' ! 1 ' '" '" I T-t'T , ! . I . i T T i n - r - j .... 2.00 4.00 6.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 04-Aug-2003 11:29:36 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.13e5 Area "' I ' ' ' I"' '.Time 10.00 000379 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Hethod: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-309 Text: 4: PFOSA L34910-11 Spk E, 5000 ng/L, DF=100 080103AR-309 Sm (Mn, 2x3) 100] - %- 04-Aug -2003 11:29:36 LC/MS/MS #6 MRM of 4 Channels ES498 > 78 1.12e5 Area 0 T -- I ' r - T ' i I -r-i I T ~ r-- I i-i-i" I' r- I " , -, i I ' I1 "I I [ " r 2.00 4.00 6.00 W '1 I1 8.00 T im e Exygen Research 3058 Research Drive, State College, PA 16801 000380 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date :08/01/03, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-310 Text : 1: C8 Acid (PFOA) L34S10-20 Spk F, 5000 ng/L, DF=100 0801 03AR-310 Sm (Mn, 2x3) 10O %: 04-Aug-2003 11:51:14 LC/MS/MS #6 9.13 MRM of 4 Channels ES413 >369 1.66e5 Area (V 2.00 4.00 2: C 6 Sulfonate (PFHS) L349 10-20 Spk F, 5000 ng/L, DF=100 0801 33AR-310 Sm (Mn, 2x3) 100n %: 1 ! 1 | 1 1 1 1 ' ' 1 ! 1 ' ' I ~ 1 1 i - ' ' ' i '.' ' 6.00 8.00 10.00 Time 8.96 4336^ 04-Aug-2Q03 11:51:14 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.50e4 Area n- ' ' ' ' 1 ' ' 1 1 1 1 ' ' 1 ! ' ' ' ' 1 1 1 1 1 1 2.00 4.00 6.00 8.00 n " - - j-. -, , - , I-, i Time 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000381 Quantify Sample Report 'S Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Riaha Page 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-310 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000382 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-311 Text: 1: C8 Acid (PF0A) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L349 10-5, DF=10 08011D3AR-311 Sm (Mn, 2x3) 100 %- Lr- t- t"r |--r 2 .0 0 4.00 9.25 91211 04-Aug-2003 12:12:52 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 5.30e4 Area " 11P 111 1 ...............TM Ln i rr 1 1 , 11 i 1 1 , 1 ' ti ,im, el 6 .0 0 8 .0 0 1 0 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 000383 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:X.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochsniicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-311 Text : 4: PFOSA L34910-5, DF=10 080103AR-311 Sm (Mn, 2x3) 100 %- ir 2 .0 0 04-Aug-2003 12:12:52 LC/MS/MS #6 MRM of 4 Channels ES9.90 498 > 78 8.67e4 Area 1I I I I I I I ! --'--^----'--I--'--'--'----I I I I I I I I I 1 1 ' ' ..1 1 1 1 1 1--r-r-r-r--Time 4.00 6 .0 0 8 .0 0 1 0 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 000384 Quantify Sample Report Study No.:L34910, Sat N o . :080103AR, Ext.Date:08/01/03, Analyst:K.Hisha w Rage 23 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-312 Text: 1: C8 Acid (PFOA) L34910-5 Rep, DF=10 04-Aug-2003 12:34:39 080103AR-312 Sm (Mn, 2x3) 100: 9.12 145121 LC/MS/MS #6 MRM of 4 Channels ES413 >369 8.59e4 %- -0 l r P M I 1 'i1 I [ t i " | - | | ) " n y -- j > i ' i n | ' | H ' 1 ' 1 ' 1 1 ' ' `--T.-T-T-T-t-pr- 2.00__________ 4,00__________ 6 XM_______ 8.00 10.00 it V i . Area Time 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) % m*l> Exygen Research, 3058 Research Drive, State College, PA 16801 000385 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Riaha Page 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-312 Text: 4: PFOSA L34910-5 Rep, DF=10 080103AR-312 Sm (Mn, 2x3) 100- %- 04-Aug-2003 12:34:39 LC/MS/MS #6 MRM of 4 Channels ES- 9-87 498 > 78 18189 1 9.40e4 1 Area ru w 2 .0 0 4.00 1' 11I ' ' '' 6 .0 0 8 .0 0 11111 -f -rI i i l r....r - r 1 0 .0 0 J|m e Exygen Research 3058 Research Drive, State College, PA 16801 000386 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:;K.Riasha w Page 25 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified! Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-313 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) V Exygen Research, 3058 Research Drive, State College, PA 16801 000387 Quantify Sample Report Page 26 Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha w Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslyxuc\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-313 Text: 4: PFOSA L34910-10, DF=10 080103AR-313 Sm (Mn, 2x3) 10Ch %: 04-Aug-2003 12:56:21 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 195031 1.01e5 Area Q - t- ,-- r--,-- I-- j--I-- I-- I-- i-- ]-- I-- r--T-- I--]-- I-- I-- r--i-- |-- r 2.00 4.00 6.00 8.00 10.00 Time Exygen Research 3058 Research Drive, State College, PA 16801 000388 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha v Page 27 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslymc\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-314 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) W 3: C8 Sulfonate (PFOS) L34910-10 Rep, DF=10 080103AR-314 Sm (Mn, 2x3) 100-1 %- 9.25 15401 04-Aug-2003 13:18:10 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.18e4 Area 1 i" 1 1 ' 2.00 4.00 6.00 8.00 10.00 Time V Exygen Research, 3058 Research Drive, State College, PA 16801 000389 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 28 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-314 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000390 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 29 Sample List: P:\Data\LCMSMS6\Masslymt\Pluorochenvicals.PRO\SaanpleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-315 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000391 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 30 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-315 Text: 4: PFOSA XC072503-1, 25 ng/L Standard 080103AR-315 Sm (Mn, 2x3) 100] %- 04-Aug-2003 13:39:58 LC/MS/MS #6 MRM of 4 Channels ES- 9-89 498 > 78 43801 2.30e4 1 Area 0^'~T~n..r T " 1' ' '"'"I 1..1 ' '"1 1 ... I11 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 ' ' ' Time 2.00 4.00 6.00 8.00 10.00 Exygen Research/ 3058 Research Drive, State College, PA 16801 000392 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:Q8/01/03, Analyst:K.Risha Rage 31 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-316 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFQS) Exygen Research, 3058 Research Drive, State College, PA 15801 000393 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 32 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-316 Text: 4: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000394 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 33 Sample List: Last modified: Method: Last modified: Job Code: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MetbDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Name : 080103AR-317 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3 : C8 Sulfonate_(PFOS) L34910-11, DF=100 080103AR-317 Sm (Mn, 2x3) AO A _ %: 9.24 663791 I 04-Aug-2003 14:23:27 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.85e5 Area 2.00 4.00 ' i 1 1 ' i 1 1 ................. .. ^ 6.00__________ aoo__________10.00 % m0 Exygen Research, 3058 Research Drive, State College, PA 16801 i-r- '' i Time 000395 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 34 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-317 Text: 4: PFOSA L34910-11, DF=100 080103AR-317 Sm (Mn, 2x3) 10CH %: 04-Aug-2003 14:23:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.39 498 > 78 21988 * 1.09e5 Area 10 " 1 1 1 - 1-- 1-- 1 ' 1 1 ' "'l 1 ' 1 ' V 1 l~ r" 1 ~ |" T - r - ' v- r ,- T - T - I ! r - v 2.00 4.00 6.00 W T -p-r- 8.00 r -'10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 000396 Quantify Sample Report Study No.:L34910, Set No.:080103AK, Ext.Date:08/01/03, Analyst:K.Risha Page 35 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-318 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000397 Quantify Sample Report Study No.:L34910, Set No.s080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 36 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SamplaDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslymc\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-318 Text : 4: PFOSA L34910-11 Rep, DF=100 08Q103AR-318 Sm (Mn, 2x3) 100-, %- 04-Aug-2003 14:45:17 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 1680; 8.63e4 Area a 2.00 4.00 ' ' I' 8.00 10.00 Time V Exygen Research, 3058 Research Drive, State College, PA 16801 000398 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 37 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-319 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) w 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000399 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 38 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocliemicals.PR0\SajrpleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-319 Text : 4 : PFOSA L34910-11, DF=10 080103AR-319 Sm (Mn, 2x3) 100] %- 04-Aug-2003 15:07:04 LC/MS/MS #6 MRM of 4 Channels ES- 9-87 498 > 78 2002931 10.00e5 Area 0 I ' I ' T ' ' ' '"I ' 1 ' ' I ' 1 ' 1 I I 2.00 4.00 6.00 8.00 10.00 Time W Exygen Research, 3058 Research Drive, State College, PA 16801 000400 Quantify Sample Report Study No.:L34910/ Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 39 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-320 Text : 1: C3 Acid (PFOA) L34910-11 Rep, DF=10 080103AR-320 Sm (Mn, 2x3) 100n 9.13 76840 04-Aug-2003 15:28:46 LC/MS/MS #6 MRM of 4 Channels ES413 >369 4.58e5 Area T I r ' " "1 2.00 r~ ^ ' r ' r-r"v 1 r'i 1 r'1 1 r 1 4.00 6.00 2: C6 Sulfonate (PFHS) 1I 1 1 1 1 I 8.00 ~1"'1T "' ' 10.00 Time 3 : C8 Sulfonate (PFOS) L34910-11 Rep, DF=10 080103AR-320 Sm (Mn, 2x3) 100- %- 9.25 390663 1 I 04-Aug-2003 15:28:46 LC/MS/WIS #6 MRM of 4 Channels ES499 >99 2.30e6 Area O r " 1 1 T"1 1 1 1 1 1 ' ' ~ n 2.00 ' 1 '--I--r -T--i i 1 i i n - | - r - r i i [ i i i i [ t t t t t W . . 1 ....... . 1 1 1 1 1 Time 4.00 6.00 8.00 10.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 000401 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 40 Sample List: Last modified: Method: Last modified: Job Code: P :\Data\LCMSMS6\Mas3lynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-320 Text: 4: PFOSA_________________________________________________________________________ _ L34910-11 Rep, DF=10 04-Aug-2003 15:28:46 LC/MS/MS #6 080103AR-320 Sm (Mn, 2x3) 100: %- rLvr I . . . . I 1 1 1 1 r r 1' 1 1 1 1 -- - 1 t ' ' T*"' 2 .0 0 4.00 6 .0 0 MRM of 4 Channels ES- 9.87 1503841 498 > 78 7.59e5 1 Area 8 .0 0 ' 1 1 ' ' ^ T 1 T ' 1 1 ' ' ' ' Time 1 0 .0 0 W Exygen Research, 3058 Research Drive, State College, PA 16801 000402 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risba Page 41 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-321 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) w Exygen Research, 3058 Research Drive, State College, PA 16801 000403 Quantify Sample Report Study No. -.L34910, Set No. :080103AR, Ext.Date:08/01/03, Analyst-.K.Risha W* Page 42 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Deeatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-321 Text: 4: PFOSA w Exygen Research, 3058 Research Drive, State College, FA 16801 000404 Quantify Sample Report Study No.:L34910, Set No.:Q80103AR, Ext.Dates08/01/03, AnalystsK.Risha Page 43 Sample List: P:\Data\LCMSMS6\Masslymc\Fluorochemicals.PR0\SainplaDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-322 Text: 1: C8 Acid (PFOA) Exygen Research, 3058 Research Drive, State Collage, PA 16801 000405 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Riaba Page 44 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MetbDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AK-322 Text : 4 : PFOSA w Exygen Research, 3058 Research Drive, State College, PA 16801 000406 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha W Page 45 Sample Lists P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-323 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) Exygen Research, 3058 Research Drive, State College, PA 16801 000407 Quantify Sample Report Study Ho.sL34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha \'^ 0 r Page 46 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-323 Text: 4 : PFOSA XC072503-3,100 ng/L Standard 080103AR-323 Sm (Mn, 2x3) 10CH %\ 04-Aug-2003 16:33:50 LC/MS/MS #6 MRM of 4 Channels ES- 9-89 _ 17628 i 498 > 78 9.31 e4 Area O -1- 1! i i r - 1 --i i i i | --i --r r r | - r i T i | i - 'i i > | i 2.00 4.00 i i| i 6.00 t --1 I r- 8.00 10.00 Time W Exygen Research, 3058 Research Drive, State College, PA 16801 000408 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Riaha Page 47 Sample List: P:\Data\LCMSHS6\Masslynx\71uorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Tue Aug 05 07:32:01 2003 Marne: 080103AR-324 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 080103AR-324 Sm (Mn, 2x3) 100n %: 0 - J -i r i i - y i I i i ( I I I -i ! 1 1 r- 1 . [ , 2.00 4.00 3: C8 Sulfonate (PFOS) 6.00 04-Aug-2003 16:55:35 LC/MS/MS #6 MRM of 4 Channels ES8.96 399 > 80 1.05e5 Area n ' ' ' ....... Time 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000409 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 48 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemieals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-324 Text: 4: PFOSA XC072503-4, 250 ng/L Standard 080103AR-324 Sm (Mn, 2x3) 1 0 0 -] %: 04-Aug-2003 16:55:35 LC/MS/MS #6 MRM of Channels ES9.89 498 > 78 2.14e5 Area O ' 1 1 '~i 1 1 i~r"i |~T~1 1 I" 1 1 1' [ 1 1 1 I n 1 1111 I ' ' ' ' Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000410 Quantify Sample Report Study No.:L34910, Set N o . :Q80103AR, Ext.Date:08/01/03, Analyst:X.Risha Page 49 Sample List; P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-325 Text: 1: C8 Acid (PFOA) L34910-20, DF=10 080103AR-325 Sm (Mn, 2x3) 100- %- 9.11 610921 1 04-Aug-2003 17:17:20 LC/MS/MS #6 MRM of 4 Channels ES413 >369 3.65e5 Area 0J I -r--i . . , r r -I" I T- r T-- i i " 1t-- i -- i -- ) | . ....... - .....r ,r '.r"'....... . i 2.00__________ 4X30__________ 6.00__________ 8.00 2: C6 Sulfonate (PFHS) w " '1--" i ' n ' ' Time 10.00 3: C8 Sulfonate (PFOS) L34910-20, DF=10 080103AR-325 Sm (Mn, 2x3) 1 0 0 -| 9.24 65108 04-Aug-2003 17:17:20 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.76e5 Area -j-r-r Time 2.00 4.00 6.00 8.00 10.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 000411 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 50 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslyznc\Fluorochemicals.PR0\MetbDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-325 Text : 4 : PFOSA L34910-20, DF=10 080103AR-325 Sm (Mn, 2x3) 100-1 %- 04-Aug-2003 17:17:20 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 61447 3.12e5 Area a W 2.00 n 11r 4.00 6.00 T T- Time 8.00 10.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 000412 Quantify Sample Report Study No.:L3491Q, Set No.:080103AR, Ext.Datei08/01/03, Analyst:K.Risha Page 51 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorocheiuicals.PRO\SampleDB\080103AR Decatur BC Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorocfaemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-326 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) w L34S 10-20 Rep, DF=10 0801 D3AR-326 Sm (Mn, 2x3) 10Ch %: 1 1 1 1 1 1 1 | ........i ' ' r " " ' <... r ' i . 1f " r - v - r - ..... 2.00 4.00 6.00 3: C8 Sulfonate (PFOS) ' 8.96 21691 04-Aug-2003 17:39:07 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.35e4 Area 8.00 i i i | i i i i [ i i i i J JIY1G ' 1 0 .0 0 W Exygen Research, 3058 Research Drive, State College, PA 16801 000413 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K .Riaha Page 52 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-326 Text : 4: PFOSA L34910-20 Rep, DF=10 080103AR-326 Sm (Mn, 2x3) 100-] %- U --r--r-i r-| v i - r - i r i i t- i- | ---'------I------1----1 1 1 1 ' 1 1 1 T' 1 1 1 1 1 1 1 '' 2.00 4.00 6.00 8.00 04-Aug-2003 17:39:07 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 517171 2.62e5 Area 1 ............. ............... --1--1--1 Tim e 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0 00 4 14 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Riflha Page 53 Sample List: P:\Data\LCMSMS6\Masslyruc\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: ' Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-327 Text: 1: C8 Acid (PFOA) L34910-21, DF=100 080103AR-327 Sm (Mn, 2x3) 100n %- 9.13 101691 1 Q4-Aug-2003 18:00:47 LC/MS/MS #6 MRM of 4 Channels ES413 >369 6.21 e4 Area o- ...' I ' ' ' I"' T~1' '~T ' ~r' ' ,l" ~I--1 T - I -- T-- 1-|~' ..... I 'VTV'-iT 11' 1I i -- 'T- 1-- T--|- 7-' i ' ''-'i-i-i ' ^ Time 2 .0 0 ___________ 4 . 0 0 6.00 8.00 10.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 4 15 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Rape 54 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MetbDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-327 Text: 4: PFOSA W Exygen Research, 3058 Research Drive, State College, PA 16801 000416 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Data:08/01/03, Analyst:K.Riaha Rage 55 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PR0\SampleDB\080103AJR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-328 Text: 1: C8 Acid {PFOA) L34910-21, DF=10 080103AR-328 Sm (Mn, 2x3) 1 0O -i 9.16 99240 04-Aug-2003 18:22:28 LC/MS/MS #6 MRM of 4 Channels ES413> 369 5.73e5 Area 2.00 " i-- i-- i-- r --T" 4.00 6.00 II II 8.00 10.00 T im e W 3: C8 Sulfonate (PFOS) L34910-21, DF=10 080103AR-328 Sm (Mn, 2x3) 100i 9.28 80003 04-Aug-2003 18:22:28 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.68e5 Area 2.00 t " 1" : 1 4.00 f r1i1r r i*"i f r i ft'"`i--r-r-y-r*t-t i" 6.00 8.00 ................................i i i i i T i m e 10.00 Zxygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 4 17 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date-.08/01/03, Analyst-.K.Risha Page 56 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\08Q103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-328 Text: 4: PFOSA L34910-21, DF=10 080103AR-328 Sm (Mn, 2x3) 100i %- 04-Aug-2003 18:22:28 LC/MS/MS #6 MRM of 4 Channels ES- 9.87 498 > 78 78207 3.95e5 Area 0w T z o o 4.00 6.00 8.00 10.00 Time w Bxygen Research, 3058 Research Drive, State College, PA 16801 000418 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 57 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-329 Text: 1: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 080103AR-329 Sm (Mn, 2x3) 100^ %: 9.15 2150481 I 04-Aug-2003 18:44:11 LC/MS/MS #6 MRM of 4 Channels ES413 > 3 69 1.26e6 Area o1L-| I ....... 1 1--1-..... 2.00 1 1 1 1 1 1 11 11..T1-H --r 1--1-- 1-- 1-- 1y..r ' T 1 f 1 1t t -- 4.00 6.00 8.00 T-'i I I I I--T'-| r-r-i - T im e 10.00 2: C6 Sulfonate (PFHS) XCOirasoS-S, 500 ng/L Standard 0801 D3AR-329 Sm (Mn, 2x3) 100 %- 04-Aug-2003 18:44:11 LC/MS/MS #6 8.99 MRM of 4 Channels ES399 > 80 2.23e5 Area ' ' '^ 1..' ' T 1 1 ' ' 1 ' ` 1 ' 1 1 1 1 1 1 1 1 ' 1 1 1 ' 1 ' 1 1 1 1 ' ' 1 1i_r_' r f 1 ' 1 ' " " Tim 2.00 4.00 6.00 8.00 10.00 3: C8 Sulfonate (PFOS) ____________________________________________________________ XC072503-5, 500 ng/L Standard 04-Aug-2003 18:44:11 LC/MS/MS #6 080103AR-329 Sm (Mn, 2x3) MRM of 4 Channels ES " " 499 > 99 1.4105 Area T-i r ' > r ' -r Time ___________________2T00___________ 4.00___________ a o o ___________ 8,00___________ 10.00__________________ Exygen Research, 3058 Research Drive, State College, PA 16801 000419 Quantify Sample Report Study No. :L34910 , Set N o .:080103AR, Ext.Date:08/01/03, Analyst-.K.Risha Page 58 Sample List: P:\Data\LCMSMS5\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AK-329 Text : 4 : PFOSA XC072503-5, 500 ng/L Standard 080103AR-329 Sm (Mn, 2x3) 1 0 0 -1 %4 04-Aug-2003 18:44:11 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 86062 4.48e5 Area a 2.00 4.00 6.00 8.00 Time Exygen Research/ 3058 Research Drive, State College, PA 16801 000420 Quantify Sample Report Study N o .:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 59 Sample List: P:\Data\LCMSMSS\Masslynx\Fluorocharaicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMSS\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-330 Text: 1: C8 Acid (PFOA) XC072503-6,1000 ng/L Standard 080103AR-330 Sm (Mn, 2x3) 100i %- 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.39e6 Area 0a "' 1 " i r " 1 i " " i 1 " 1 i 1 2.00 4.00 2: C6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 'I''' 6.00 080103AR-330 Sm (Mn, 2x3) 100-1 %- 8.99 715211 1 1 0- ' 1 ' ` ................... | , , . , | ,-- 1-- r-- 1-- . i r j r", T-r~, . . , 2.00___________ 4,00__________ 6.00 8.00 3: C8 Sulfonate (PFOS) XC072503-6,1000 ng/L Standard 080103AR-330 Sm (Mn, 2x3) 1 0 0 -, %: 10.00 T im e 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 4 .1 9e5 Area i ....... 10.00 ' ' ' Tim e 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.57e5 Area 0 ' ' I - V , ' "I T I "f I 2.00 W t| r t' i r ]' ! i T"'r | "r 4.00 6.00 - t i ' ' r-i"' - i- t- Tim e 10.00 Exygen Research, 3058 Research Drive, State College, PA 18801 000421 Quantify Sample Report jr Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 60 Sample List: P:\Data\LCMSMSi5\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 0S0103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-330 Text : 4 ; PFOSA_________________________________________________________________________________________________________ XC072503-6,1000 ng/L Standard 04-Aug-2003 19:05:53 LC/MS/MS #6 080103AR-330 Sm (Mn, 2x3) 10 0 ] MRM of 4 Channels ES- 9.89 498 > 78 1674211 8.67e5 Area %: 1 rv_ b~TTMr~rTMnTM n i-- 1 2.00 1 ' 1 1 ' ' ' 1 1 1 1 1 1 i ........... 4.00 6.00 8.00 11 k1 ......,..........:t -v '-- 1 ime 10.00 W Exygen Research, 3058 Research Drive, State College, PA 16801 00042 w Sponsor Study No: Exygen Study No: Analyte: loos Monitored: Site: NA L34910 pros 499 -> 99 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: 50 ppt Injection Volume: 15 pL Matrix: Soil Sample Weight 5.0 g ' Final Volume: 5.0 [nL Set No: Analyst Instrument Type: Extraction Date: Analyzed on: 081203A Karen Risha LCMSMS #6 08/12/03 08/13/03 V Exygen . ID XC081103-0 XC08II03-1 X C 0 8 1103*2 XC081103-3 XC081103-4 XC081103-5 XC081103-6 Methanol Wash Reagent Blank Reagent Spk A Reagent Spk B L34910-1I Spk L34910-11 Spk E XC081103-1 XC081103-2 XC081103-3 L34910-U U 49I0-11 Rep L34910-U L349L0-1I Rep XC081103-4 X C 0 8 1103-5 XC081103-6 Sponsor ID - na na na BC2SED-06 BC2 SED-06 BC2 SED-06 B Q SED-06 BC2 SED-06 BC2 SED-06 Sample Code CS cs CS cs cs cs cs c c LCS LCS LF LF cs cs cs s s s s cs cs cs Run No. 08123A-3001 081203A-3002 081203A-3003 081203A-3004 081203A-3005 081203A-3Q06 081203A-3007 0S1203A-3008 081203A-3009 01203A-3010 081203A-3011 081203A-3OI2 08123A-3013 0&1203A-3014 081203A-3015 081203A-3016 081203A-3017 081203A-30I8 081203A-3019 081203A-3020 081203A-3021 081203A-3022 081203A-323 Analyte Found (ppt) (peak area intercept) / slope x DF Recovery (%) [analyte found (ppQ-analyte found in control (ppt)) x 100 amount added (ppt) Std. Cone. (ppo 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Factor 1 1 1000 too - 1000 1000 too 100 - . Peak Area 0 909 1896 3803 9700 19165 39020 0 0 1963 21166 8541 91234 954 2208 4213 4378 4935 42296 48356 11039 20668 39291 Analyte Found (ppd Amount Added (ppo Recovery (%) Analyte Found (ppb) ND 49.2 533 215000 - 50 500 100000 100000 98 107 105 110000 124000 - 880.00 99200 - - - . Standard Curve : Linear (l/x weighted) Intercept * 10-4732 Slope 39.6727 Coef. O f DeL 0.998540 Total Solids {%) Analyte Found(ppb) ' Dry Weight 60.41 60.41 60.41 60.41 . . 1460 1640 . . . Analyte Found (ppb) * [analyte found (ppt) x volume extracted (0.04 L)J / sample weight (5 g) Analyte Found (ppb) dry weight * analyte found (ppb) x (100% / total solids (%)) CS a Calibration standard C * Control sample S Sample LF * Lab fortified sample FF Field fortified sample LGS Laljoratory Control Spike CK Check Standard ND * Not detected * Response between 0 and 25 ppt NQ Not quantifiable Response between 25 ppt and LOQ (SO ppt) D ilution was for PFOSA. Spreadsheet prepared by: 000423 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L34910 FOSA 498 -> 78 Decatur Baker's Creek RAW DATA REPORT Limit o f Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 15 pL Soil 5.0 g 5.0 mL Set No: Analyst Instrument Type: Extraction Date: Analyzed on: 081203A Karen Risha LCMSMS m 08/12/03 08/13/03 Exygen ID X C 0 8 1103-0 X C 0 8 1103-1 XC081103-2 XC08U03-3 XC081103-4 XCQ81103*5 X C 0 8 1103-6 Methanol Wash Reagent Blank Reagent Spk A Reagent Spk B L34910-11 Spk E - L349L0-11 Spk E ~ XC081103-1 X C 0 8 1103-2 XC081IO3-3 L 349IG .il L34910-11 Rep L34910-11 L34910-11 Rep X C 0 8 1 103-4 X C 0 8 1103-5 XC0S1103-6 Sponsor ID - - - - - - - - a* na na BC2 SED-06 BC2 SED-06 - BC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 SED-06 Sample Code CS CS CS CS CS CS CS C c LCS LCS LF LF CS CS CS s s s s CS CS CS Run No. 081203A-300I 081203A-3002 081203A-3003 08I203A-3004 081203A-3005 081203A-3006 081203A-3007 081203A-3008 081203A-3009 08I203A-3010 08I203A-3011 081203A-3012 081203A-3013 081203A-3014 081203A-3015 081203A-30I6 081203A-30I7 081203A-30I8 081203A-3019 081203A-3020 08I203A-3021 081203A-3022 081203A-3023 Analyte Found (ppO - (peak area intercept) / lope x DF Recovery (%) * (analyte found (ppt)analytc found in control (ppt)| x 100 amount added (ppt) Std. Conc. (p p O 0 25 50 100 250 500 1000 25 30 100 250 500 1000 Dilution Factor I 1 1 1000 100 . 1000 1000 100 100 - - Peak Area 0 3547 7692 15522 39080 73905 14S023 0 0 7255 72614 11415 122331 4230 8197 16248 1446 1737 13834 16015 41122 78848 149443 Analyle Found (p p o Amount Added (p p o Recovery w Analyte Found (ppb) ND 45.5 481 81200 50 500 tooooo 100000 91 96 72 8930 10400 71.44 83.20 - -- Standard Curve ; Linear (1/x weighted) intercept 4 3 4 .4 S 5 Slope = 150.03 7 Coef. O f Det. * 0.998129 Total Solids (%) 60.41 60.41 60.41 60.41 - Analyte Found (jppb) (analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight * analyte found (ppb) x (100% / total solids (%)) CS * Calibration standard C - Control sample S - Sample LF * Ufa fortified sample FF - Field fortified sample LCS * Laboratory Control Spike CK Check Standard ND " Not detected Response between 0 and 25 ppt NQ =*Not quantifiable 8 Response between 25 ppt and LOQ (50 ppt) Analyte Found(ppb) Dry Weicht . . - - . - - - - - - . 118 138 - D ilution was for PFOS Spreadsheet prepared by: 000424 Ev enRESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 W Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34910 Matrix: Soil Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. ^ 2 - Time t y i /A 1 Date, Initials CE^ CLIENT SAMPLE ID na na na BC2 SED-06 BC2 SED-06 BC2 SED-06 EXYGEN ID NUMBER Reagent Blank Reagent Spk A Reagent Spk B L34910-11 Spk E L34910-11 L34910-11 Rep . W EIGHT (g) . _ _ 5.0 5.0 5.0 FORTIFICATION (ng) 2.0 20.0 4000.0 . -_ . - __ - ._ __ - _ -_ _ -_ -- - .. -- - - -- Reagent Spk A Reagent Spk B L34910-11 SpkE . . . Spiking Solution Used F061103-2 (10 ng/mL) F061103-1 (100 ng/mL) F060203-1 (10000 ng/mL) . , Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 400 pL (200 pL micropipet) _ Initial/Date /r e lu .o = , /o&llzfv. I V b lJ! ._ -- All samples were weighed on balance No. 2 & T im e. C fiZ Q .______ Date 0 & jlZ :jG 3 . Initials - - After wceignhiinnjg samples were returned to refrigerator No. Time M 2 Date IIU Initials. Comments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: P P T ij Analysis Summary: Data Sec 0 6 . 1 2 . 0 3 A Data Set:. Data S et:. Initials/Date: Initials/Date:: Z 2 X Initials/Date: J. '/o 3 Set extraction/analysis data verified by: Date: W /& July 2 6 . 2 0 0 1 / 1 0 0 0 4 ^ 6 (i 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34910 MATRDC: Sail METHOD: ExM-023-014 M ANALYTES: PFHS. PPOS. PFOA and PFOSA PROTOCOL NUMBER: NA Client ID na na na BC2 SED-06 BC2 SED 06 BC2 SED-06 -' *lnitiah/Dale ExygenID Reagent Blank Reagent Spk A Reagent Spk B L34910-11 Spk E L34910-11 L34910-11 Rep - - - - - - STEP 1 STEP 2 STEP 3 STEP 4 STEP 5 STEP 6 Dilutions (mL/mL) w -- STEP 7 Dilutions (mL/mL) -- -- --- \' * -- \> / -- C I'd nA0 Vio-Mr 51/ \ 'T-VyafMv \ -- -- -- - . -- - - - - _ -- - - - - - `- - -- - - - - - - - -- - - . - -- -' - - - - - _. -- - - . . . . -- - - - - - - - - - - _- - - - - -' -- - - - - -' - - -- - - - - - . -' - -- - --- - -.- .- - - -- - - - - -' O f, c e r & (Xf c m jl2p S L jz s M a oefafa `-- STEP 2: Bring up to 40 mL with hypercarb filtered type 1water STEP 3: Centrifuge for 10 minutes a t-3000 rpm STEP 4: Filter through glass acrodisc STEP 5: SPE column clean up (omitting 40% wash) STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 7: LC/MS/MS analysis STEP g: LC/MS/MS reanalysis. f f i t i - IOO l 0 0 STEP g *-- -- - - _ _ _ - - - -- Reagents/ Materials Methanol 0 8 SPE Type I Wna Class acrodisc _ . Lot# IfaHtf&OJi, NA - Initiais/Dute _ . _ . _ _ - _ _ HPLC Methanol AmmoniumAcetate Type I water . NA ]' oInitials/Daie 81 5 Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctanesulfonate (PFOS) and Pentadecafluorooctanoic Acid (PFOA) in Soil COMMENTS: Final extracts stored in refrigerator .''2- Initials: C'EF. Date: July 19, 2001/4 000427 Exygen m/ t S LARC H 3058 Research Drive State C ollege, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 preparation of extracted calibration standards Protocol No.: None Method No.: Sponsor Sample ID NA NA NA NA NA NA NA Exygen Sample ID mU1/UwUvU>S.n 0106020 0106020 0106020 0106020 0106020 0106020 Sample Description 1J f J/C A *VUtt/1 Type I WaierA Type I Water* Type I Water* Type I Water* Type I Water* Type I Water* Exygen Study No.: tiA Analytes: PFBS. PFHS. PFOS. PFOA Fort. Solution ID and PFOSA Fort Fort Soin. Cone. Volume (ne/mU (ML) Micropipet used (uL) - --- F 0 6 1 103-2 10 100 200 F 0 6 1 103-2 10 200 200 F 0 6 1103-2 10 400 200 F 0 6 1 103-1 100 100 200 F061103-1 100 200 200 F061103-1 100 400 200 Fort Level (ppt) - 25 50 100 250 500 1000 Matrix: Type I Water* Sample Vol: 40 mL Final Solution ID #** V i'in o i irirt a AV-UOilU J-U XC081103-1 X C 0 8 1 103-2 XC081103-3 XC081103-4 XC081103-5 XC081103-6 Reagents/ Materials --------------------------------------1 Lot# Methanol 0 8 SPE Type I Water W 3llrTBZ NA - _ - -- - - . _- - - - - - .- - Vertical arrows inacolumnindicate identical values. **Thismust be a uniquenumber. Use this system: ExtractedCalibrationSolnID#: XCMMDDYY0,1,2,3. etc. - Initials/Date: Samples removed froprTelflgerator / freezer tt f?2- Time: fflC O Initials/Date (,ET l & jtlfa 40 mL o f each sample measured using a *^5 mT. graduated cylinder. Inidals/Date After measuring, samples returned uyreTngeratpT/ freezer # P X . Time: l S 3 Q Initials/Date Samples fortified: Initials/Date: / tB h ll0 3 SPE clean-up (omitting 40% Wash): Initials/Date: C E X Fmal volume adjusted to 5 mL: Initials/Date: /V k . h Extracts placed in refrigerator # Z- Initials/Date: PfPL I6M jiijr x STANDARD EXPIRATION DATE: 1O 0 |l/1 0 3 1 8/25/03 Comments: *This type I water has been filtered through a hypercarb filter J$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water July 10,2001/0 cc Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochesnailiccaallss.PROI\SarmpleD8\081203A Decatur BC.SPL Printed: Wed Aiug 13 09:36:59 2003 E jf.te liilo a Vial File Name LIMS ID Client ID Sample Description Ma 1 1 081203A-3001 _ _ 2 2 081203A-3002 3 3 081203A-3003 -- 4 4 081203A-3004 -- 5 5 081203A-3Q05 -- 6 6 081203A-3006 -- 7 7 081203A-3007 -- 8 92 081203A-3008 -- 9 11 081203A-3009 -- 10 12 Au Qu 4i Ot uA uI nA ' no nu i f1 ut -- 11 13 081203A-3011 -- 12 14 081203A-3012 -- 13 15 81203A-3013 - 14 2 081203A-3014 -- 15 3 081203A-3015 -- 16 4 081203A-3016 -- 17 16 081203A-3017 -- 18 17 081203A-3018 -- 19 18 081203A-3019 -- 20 19 081203A-3020 -- 21 5 081203A-3021 -- 22 6 081203A-3022 -- 23 7 081203A-3023 __ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC081103-0,0 ng/L Standard XC081103-1,25 ng/L Standard XC081103-2,50 ng/L Standard XC081103-3.100 ng/L Standard XC081103-4,250 ng/L Standard XC081103-5.500 ng/L Standard XC081103-6,1000 ng/L Standard Methanol Wash Reagent Blank Reagent SpR A, 50 ng/L Reagent Spk B, 500 ng/L L34910-11 Spk E, 100000 ng/L, DF=1000 L34910-11 Spk E. 100000 ng/L, DF=100 XC081103-1, 25 ng/L Standard XC081103-2, 50 ng/L Standard XC081103-3,100 ng/L Standard L34910-11, DF=1000 L3491-11 Rep, DF=1000 L34910-11, DF=100 L34910-11 Rep, DF=100 XC081103-4,250 ng/L Standard XC081103-5, 500 ng/L Standard XC081103-6,1000 ng/L Standard __ ... -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- Exygen STUDYNO* J jlf l i Page 1 Page Position: (1.1) Sample Type Standard Standard Standard Standard Standard Standard Standard Blank Blank QC QC C QC Standard Standard Standard Analyte Analyte Analyte Analyte Standard Standard Standard Cone (ng/L) 0 25 50 100 250 500 1000 -- -- 50 500 100000 100000 25 50 100 -- -- -- -- 250 500 1000 Cone B ___ -- -- -- ------- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- Cone C __ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- Test ID 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 DF 1 1 1 1 1 1 1 1 1 1 1 1000 100 1 1 1 1000 1000 100 100 1 1 1 c( Massiynx Sample List Sample List: C:\MASSLYNX\Fluorochei ilcals.PRO\Samp!eDB\081203A Decatur BC.SPL Printed: Wed Aug 13 09:36:59 2003 L M e IoS _____________________ MS Method HPLC Method MS Fune File Inj.Volume 1 C6 C8 SULF C8 ACID PFOSA pfbs water 2 C6 C8 SULF C8 ACID PFOSA pfbs water 3 C6 C8 SULF C8 ACID PFOSA pfbs water 4 C6 C8 SULF C8 ACID PFOSA pfbs water 5 C6 C8 SULF C8 ACID PFOSA pfbs water 6 C6 C8 SULF CS ACID PFOSA pfbs water 7 C6 C8 SULF C8 ACID PFOSA pfbs water 8 C6 C8 SULF C8 ACID PFOSA pfbs water 9 C6 C8 SULF C8 ACID PFOSA pfbs water 10 CO C8 SULF Co ACID PFOSA pfbs water 11 C6 C8 SULF C8 ACID PFOSA pfbs water 12 C6C8 SULF C8 ACID PFOSA pfbs water 13 C6 C8 SULF C8 ACID PFOSA pfbs water 14 C6 C8 SULF C8 ACID PFOSA pfbs water 15 C6 C8 SULF C8 ACID PFOSA pfbs water 16 C6 C8 SULF C8 ACID PFOSA pfbs water 17 C6 C8 SULF C8 ACID PFOSA pfbs water 18 C6 C8 SULF C8 ACID PFOSA pfbs water 19 C6 C8 SULF C8 ACID PFOSA pfbs water 20 C6 C8 SULF C8 ACID PFOSA pfbs water 21 C6 C8 SULF C8 ACID PFOSA pfbs water 22 C6 C8 SULF C8 ACID PFOSA pfbs water 23 C6 C8 SULF C8 ACID PFOSA pfbs water Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems Fluorochems 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 000430 Exygen study NO; t ( Page 2 Page Position: (2, 1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L3491Q Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: M assLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin 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: 74A ) (JONESCHROMATOGRAPHY: Part N o. FK5962E) Mobile Phase (A) : Mobile Phase (B) : 2 mM Ammonium Acetate in Type I Water Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are com puter generated printouts from the m asslynx software program . The pages contain the instrum ent settings used for the analysis of this data set. All Handwritten Peak ED's by: 03> w 000431 Scanning Method Report Page 1 Method: C:\MASSLYNX\IXU0R0CHEMICALS.PR0\ACQUDB\C6 C8 SULF C8 ACID PFOSA Last Modified: Thu Jul 31 16:23:50 2003 Printed: Wed Aug 13 09:37:33 2003 t>3 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay { Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone 1 399.00 80.00 0.20 2 413.00 369.00 0.20 3 498.00 78.00 0.20 4 499.00 99.00 0.20 35 10 30 40 50 10 50 30 V w 000432 Method Report Method File: Last Modified: Printed: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs water Wednesday, August 13, 2003 09:25:45 Wednesday, August 13, 2003 09:37:56 Page 1 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 10.0 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 20.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time 0.00 2.00 5.00 9.00 9.50 14.00 14.50 20.00 A% 90.0 90.0 10.0 10.0 0.0 0.0 90.0 90.0 10.0 10.0 90.0 90.0 100.0 100.0 10.0 10.0 C% 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 Flow 0.300 0.300 0.300 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Contactl Off Off Off On Off Off Off Off Off Off Off Off Contact2 Off Off Off On Off Off HP110Q Autosampler Initial Conditions Draw Speed Eject Speed (/il/min) Draw Position (mm) Stop Time (mins) Injection Volume(^1) Vial Number 200.0 200 0.50 20.00 15.0 47 Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off 000433 Tuning Method Report Vue*/ Method: C :\MASSLYNX\E'LUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS Printed: Wed Aug 13 09:37:50 2003 & Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -42 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.5e- 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 15 2 14.0 14.0 2.0 650 26 38 29 -648 Rdbk 132.1 755.7 000434 Quantify Calibration Report Study No.:L34910, Set No.:081203a , Ext.Date:08/12/03, Analyst:K.Risha Exygen Research, 3058 Research Drive, State College, PA 16801 000435 Quantify Calibration Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 2 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\CurveDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:18 2003 Printed: Mon Aug 18 10:50:24 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 000436 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Riaha Page 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PrFar Ov Su and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Initials._ Date_sa L ur hMTfpc..F .=..-......... . i y ii-ijF Run# i^Q,lTo CfiltfrYr ani f ? Name: 081203A-3001 Text: 2: PFOSA % t0 Exygen Research, 3058 Research Drive, State College, PA 16801 000437 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 2 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3002 Text: 1: C8 Sulfonate (PFOS) 2 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000438 Quantify Sample Report Study No.-.L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst-.X.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Hon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3003 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College PA 16801 000439 Quantify Sample Report Study N o .:L34910, Set No.:081203A, Ext.Date:08/12/03, AnalystrK.Risha Page 4 W Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SamplsDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3004 Text : 1: C8 Sulfonate (PFOS) 2: PFOSA W Exygen Research, 3058 Research Drive, State College, PA 16801 000440 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, AnalystsK.Risha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3005 Text : 1: C8 Sulfonate (PFOS) 2: PFOSA XC081103-4, 250 ng/L Standard 081203A-3005 Sm (Mn, 2x3) 10O i %- 2.00 4,00 13-Aug-2003 16:10:15 LC/MS/MS #6 MRM of 4 Channels ES- 9-95 390801 498 > 78 aae5 Area 6.00 8.00 10.00 Time V Exygen Research, 3058 Research Drive, State College, PA 16801 000441 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SanpleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Kluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3006 Text: 1: C8 Sulfonate (PFOS) XC081103-5, 500 ng/L Standard 081203A-3006 Sm (Mn, 2x3) 1 0 0 -1 9.33 19165 13-Aug-2003 16:32:00 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.06e5 Area TT 2.00 4.00 2 : PFOSA XC081103-5, 500 ng/L Standard 081203A-3006 Sm (Mn, 2x3) 1 0 0 -1 %- 2.00 4.00 I : - r - i - r T i r i r | 6.00 '1 I 1 1 1 8.00 10.00 Time 13-Aug-2003 16:32:00 LC/MS/MS #6 MRM of 4 Channels ES- 9.95 498 > 78 739051 3.53e5 Area 6.00 8.00 10.00 T im e Exygen Research, 3Q58 Research Drive, State College, PA 16801 000442 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha W Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SarapleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3007 Text: 1: C8 Sulfonate (PFOS) XC081103-6,1000 ng/L Standard 081203A-3007 Sm (Mn, 2x3) 10Ch - %: 9.33 39020 13-Aug-2003 16:53:41 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.06e5 Area 0 ......................... ' ' i 1 > 1 1 i 1 ' t t ' - t- , 2.00 4.00 2 : PFOSA XC081103-6,1000 ng/L Standard n i t ' > r ' 6.00 081203A-3007 Sm (Mn, 2x3) 100n ' %- O - - 1 ' 1 .......... [ 1 1 T i.... ' 2.00 r ' ' 1 'T 1 4.00 6TK3 8.00 10.00 Time 13-Aug-2003 16:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 145023 6.91 e5 Area L00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 000443 Quantify Sample Report Study No.JL34910, Set No.;081203A, Ext.Date:08/12/Q3, Analyst;K.Risila Page 8 Sandle List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SainpleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3008 Text : Exygen Research, 3058 Research Drive, State College, PA 16801 000444 Quantify Sample Report Study No-:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemcals.PRQ\SampleDB\0812Q3A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Last modified: Mon Aug 11 09:49:08 2003 PFOSA 081103 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 0S1203A-3009 Text: 1: C8 Sulfonate (PFOS) % *0 Exygen Research, 3058 Research Drive, State College, PA 16801 000445 Quantify Sample Report Study No.:L34910, Set N o .:Q81203A, Ext.Data:08/12/03, AnalystsK.Risha Page 10 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicala.PRO\SampleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3010 Text: 1: C8 Sulfonate (PFOS) 2: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000446 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 11 Sample List: P :\Data\LCMSMS6VMasslynx\Fluorochemiaals.PRO\SampleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3011 Text: 1: C8 Sulfonate (PFOS) H0 Exygen Research 3058 Research Drive, State College, PA 16801 000447 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Pape 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3012 Text: 1: C8 Sulfonate (PFOS) 2 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 0004^8 Quantify Sample Report Study No.:L34910, Sat No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha W Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Kluorocheniicals.PRO\SainpleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3013 Text: 1: C8 Sulfonate (PFOS) L34910-11 Spk E, 100000 ng/L, DF=100 081203A-3013 Sm (Mn, 2x3) 10CH %: 13-Aug-2003 19:03:40 LC/MS/MS #6 MRM of 4 Channels ES9.36 499 > 99 4.77e5 Area 0 ' ' ' I I 1 ' i ' " i - i r I i - i i' i I ' ' i r - | --r 2.00 4.00 6.00 2 : PFOSA w L34910-11 Spk E, 100000 ng/L, DF=100 081203A-3013 Sm (Mn, 2x3) 100-1 %- -r p-r-T-, , -r i..-, -, - Time a i o 10.00 13-Aug-2003 19:03:40 LC/MS/MS #6 MRM of 4 Channels ES- 9.98 498 >78 1223311 5.76e5 Area 0 J--1 1 i 1 1 ' ' 1~i 1 1 r | - r ~ T' 1' " 1 1 ' i ' - i - i - r - i-T ' >- "'- r- r - 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 000449 Quantify Sample Report Study No.:L34910, Set N o .:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslyxuc\Fluorochemicals.PR0\SampleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslymc\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3014 Text: 2: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000450 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\Q81203A Decatur BC Last modified: Hon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3015 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State Collage PA 16801 000451 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, AnalystsK.Risha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Hon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 0812Q3A-3016 Text: 2: PFOSA w XC081103-3,100 ng/L Standard 081203A-3016 Sm (Mn, 2x3) 10Ch 13-Aug-2003 20:08:51 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 162481 7.75e4 Area 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, FA 16801 000452 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 17 Simple List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Hon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug IS 10:50:26 2003 Name: 081203A-3017 Text: 1: C8 Sulfonate (PFOS) 2: PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 000453 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\081203A Decatur BC Last modified: Hon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3018 Text: 1: C8 Sulfonate (PFOS) 2: PFOSA L34S 10-11 Rep, DF=1000 0812 D3A-3018 Sm (Mn, 2x3) 100; %- 13-Aug-2003 20:52:12 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 1737 8.70e3 1 Area 0 - L-i' r i T 1 . , p-T , , r , r 1 1 1 ; 1-i r -1--..,-'"1 ' I 1 r r 2.00 4.00 6.00 8.00 ..1 1 ' ' 1 ' ' ............... .. Time 10.00 Exygen Research 3058 Research Drive, State College, PA 16801 000454 Quantify Sample Report Study No.:L3491Q, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Hon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Hon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3019 Text: 2 : PFOSA L34910-11, DF=100 081203A-3019 Sm (Mn, 2x3) 100^ %- lr~ 1 1 ' 1 ! 1 ...... 1 ' " ..r" 1 1 1 , , , , 1 1 . . , 2.00 4.00 6.00 13-Aug-2003 21:13:55 LC/MS/MS #6 . MRM of 4 Channels ES- 9.96 498 > 78 .1138341 6.48e4 Area ........... .. 1 1 1 1 1 1 1 1 1 ! . . . 1 8.00 10.00 Exygen Research, 3058 Research Drive State College, PA 16801 000455 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Rage 20 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3020 Text: 1: C8 Sulfonate (PFOS) L34910-11 Rep, DF=100 081203A-3020 Sm (Mn, 2x3) 100-1 %- 9-36 _ 483561 1 13-Aug-2003 21:35:42 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.51 e5 Area 0- ' 1 1 ' ' 1 1 1 ' 1.... '1 ' 1'1 ' 1 1 Tn 1 1 ..... i i r- 1 i- 1 |T i-- r T T - r ^ , i ' i ' ' ' ' - Time 2.00 4.00 6.00____ 8.00 10.00 2 : PFOSA L34910-11 Rep, DF=;100 081203A-3020 Sm (Mn, 2x3) 100"] %- 13-Aug-2003 21:35:42 LC/MS/MS #6 MRM of Channels ES9.98 498 > 78 7.31e4 Area 0 - 1- ' ' I T > ' ' I ' 1 ' ' I I'- r r -r-T r i r 2.00 4.00 , i , --i--i ! i- 6.00 r -r 8.00 10.00 r' Time w Exygen Research 3058 Research Drive, State College, PA 16801 000456 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Ri.sha Page 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\081203A Decatur BC Last modified: Hon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocbemicals.PR0\MethDB\PF0S and PPOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3021 Text: 2 : PFOSA Exygen Research, 3058 Research Drive, State College PA 16801 000457 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Dates08/12/03, AnalystsK.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur BC Last modified: Hon Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Hon Aug 18 10:50:26 2003 Name: 081203A-3022 Text: 1: C8 Sulfonate (PFOS) XC081103-5, 500 ng/L Standard 081203A-3022 Sm (Mn, 2x3) 10CH %: 9.35 20668 , 13-Aug -2003 22:19:08 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 ' 1.09e5 Area 0 -- i-- i-- i-- i-- |-- i-- i-- !-- i-- |-- i-- i-- r-- i-- |-- r -- i-- i i j-- i-- r 2.00 4.00 2: PFOSA w XC081103-5, 500 ng/L Standard 081203A-3022 Sm (Mn, 2x3) 1Q0-] %: r" "i I-- I-- r - T 6.00 ~T",li 1 r~' "'1 8.00 T ' ' H --'..... Time 10.00 13-Aug-2003 22:19:08 LC/MS/MS #6 MRM of Channels ES9.96 498 > 78 3.74e5 Area 0 1'. ' 1 I ' 1T "' 1 1 I '! 1 | 1 1 I '' 2.00 4.00 6.00 aoo 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 000458 Quantify Sample Report Study No.:L34910, Set No.:0B1203A, Ext.Date:08/12/03, Analyst:K.Risha W Pape 23 Sample List: F:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\081203A Decatur BC Last modified: Non Aug 18 10:47:09 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S and PFOSA 081103 Last modified: Mon Au? 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3023 Text: 1: C8 Sulfonate (PFOS) XC081103-6,1000 ng/L Standard 081203A-3023 Sm (Mn, 2x3) 100- %- 9-36 392911 1 13-Aug-2003 22:40:47 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.13e5 Area Ch ` 1 i 1 1 i 1 1 1 1 i 1 ' 1 i ' 11 i 1 i 1 1 1 i 1 1 r--^--.............. 2.00 4.00 6.00 8.00 i | i i i i | i i i i Time 10.00 2: PFOSA XC0S1103-6,1000 ng/L Standard 081203A-3023 Sm (Mn, 2x3) 10Ch %: 13-Aug-2003 22:40: LC/MS/MS #6 MRM of Channels ES9.96 498 > 78 7.03e5 Area O' - 1"1 ' '' I1-1 1 I'' 1 .... 'I '"T-T-r-1 "r ' I ' 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 0004F9 9/19/2003 Project: E03-0561 3M ENVIRONMENTAL LABORATORY fin a l Report 1 of 3 Requester: Schnobrich, Dana M(223-1N-08) Completion Date: 9/2/2003 Department: 530711 Project Lead: Jess S. Eldridge Project Number: 0022674449 Phone Number: 651-778-5233 Date Received: 6/26/2003 Email Address: jseldridge@mmm.com Project Description: Decatur Bakers Creek #2 Surface Water and Sediment Comments: Statement of Accuracy: Based on results of field spikes, laboratory spikes, field blank spikes, and laboratory control spikes, the analytical accuracy for all compounds is 30%. Exceptions for the water samples are as follows: BC2 SW-04 high spike (PFOA 57%, PFOS- 62%, FOSA- 58%), BC2 SW-05 high spike (PFOA - 66%, FOSA - 40%), BC2 SW-06 high spike (FOSA - 60%), Outfall to River SW-25 (FOSA - 58%). Also, several low spike samples showed unacceptable recoveries in cases where the spiking concentration was comparable or below the inherent sample concentration. However, all laboratory control spikes, laboratory matrix spikes, and all other field spikes showed recoveries between 70%and 130%for all compounds. The accuracy for the sediment samples is based upon laboratory spike recoveries, all of which were between 70% and 130%for all compounds. Sediment sample results are reported as received. Results reported as dry weight are available in the Exygen report. REVISED REPORT: Due to schedule changes, the original sample dates entered were revised to relect the actual collection dates. BGJ-Pace-9/19/03 Project Results/Activitv Pace Field Sampling Event - Complete 3MSample Number______ Sampled Date______ Sample Description E03-0561-49786 7/21/2003 BC2 SW-04 LAS EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49787 9/21/2003 Components PFOS PFHS FOSA PFOA BC2 SW-04 DUP LAS EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49788 7/23/2003 Components PFOS PFHS FOSA PFOA BC2 SED-04 LAB EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E 0 3-0561-49789 7/21/2003 C&mpcMPta PFOS PFHS FOSA PFOA BC2 SW-05 LAS EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS Components PFOS PFHS Result 11.5 ng/mL 0,896 ng/mL 1.39 ng/mL 4.21 ng/mL Result 8.25 ng/mL 0.571 ng/mL 0.790 ng/mL 2.54 ng/mL Result 14.6 ng/g 0.566 ng/g 7.15 ng/g 3.02 ng/g Result 1.67 ng/mL 0.155 ng/mL BL 0.05 0.05 0.05 0.05 Q ualifier BL Q ualifier 0.05 0.05 0.05 0.05 BL Q ualifier 0.4 0.4 0.4 0.4 BL Q ualifier 0.05 0.05 000460 9/19/2003 3M ENVIRONMENTAL LABORATORY Final Report Project: E03-0561 (cont.) 3M Sample Number_______Sampled Date_______ Sample Description E03-0561-49789 (cont.) 7/21/2003 BC2 SW-05 LAB EXYGEN EXYGEN Analytical Method FOSA PFOA E03-0561-49790 7/21/2003 Components FOSA PFOA BC2 SW-05 DUP Result 0.146 ng/mL 0.591 ng/mL LAB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49791 7/21/2003 Components PFOS PFHS FOSA PFOA BC2 SED-05 Result 4.33 ng/mL 0.377 ng/mL 0.389 ng/mL 1.56 ng/mL IAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49792 7/23/2003 C um ponenti PFOS PFHS FOSA PFOA BC2 SW-06 Result 22.8 ng/g 1.45 ng/g 7.86 ng/g 5.14 ng/g LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49793 7/23/2003 ilttmmmenla PFOS PFHS FOSA PFOA BC2 SW-06 DUP Result 26.1 ng/mL 6.06 ng/mL 2.43 ng/mL 12.1 ng/mL LAB EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN PFHS FOSA EXYGEN PFOA E03-0561-49794 7/23/2003 Components PFOS PFHS FOSA PFOA BC2 SED-06 Result 25.1 ng/mL 5.87 ng/mL 2.57 ng/mL 11.6 ng/mL LAB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E3-0561-49795 7/23/2003 Components PFOS PFHS FOSA PFOA Outfall to River SW-25 Result 880 ng/g 2.46 ng/g 71.4 ng/g 14.2 ng/g LAB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49796 7/23/2003 Components PFOS PFHS FOSA PFOA Outfall to River SW-25 DUP Result 31.2 ng/mL 7.66 ng/mL 3.26 ng/mL 15.8 ng/mL lab EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA CumPMvsnti PFOS PFHS FOSA Result 30.8 ng/mL 6.77 ng/mL 3.28 ng/mL 2 of 3 L 0.05 0.05 BL 0.05 0.05 0.05 0.05 BL 0.4 0.4 0.4 0.4 BL 0.05 0.05 0.05 0.05 BL 0.05 0.05 0.05 0.05 BL 0.4 0.4 0.4 0.4 BL 0.05 0.05 0.05 0.05 BL 0.05 0.05 0.05 Qualifier Q ualifier Qualifier Q ualifier Qualifier Qualifier Q ualifier Qualifier 000461 9/19/2003 3M ENVIRONMENTAL LABORATORY Final Report Project: E03-0561 (cont.) 3M Sample Number_______Sampled Date_______ Sample Description________ E03-Q561-49796 (cont.) 7/23/2003 Outfall to River SW-25 DUP LAB EXYGEN Analytical Method PFOA E03-0561-49797 7/23/2003 Components PFOA Outfall To River SED-25 Result 14.4 ng/mL LAB EXYGEN Analytical M ethttd PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49813 7/23/2003 Components PFOS PFHS FOSA PFOA Outfall to River SED-25 DUP Result 107 ng/g 3.19 ng/g 28.0 ng/g 10.7 ng/g LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-59479 7/21/2003 Components PFOS PFHS FOSA PFOA Field Control/T ravel Blank Result 140 ng/g 4.98 ng/g 35.7 ng/g 17.7 ng/g LAB EXYGEN Analytical. M ethod PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-59480 7/21/2003 C nnuancntj PFOS PFHS FOSA PFOA Equipment Blank - Pump Result ND ng/mL ND ng/mL ND ng/mL ND ng/mL LAB EXYGEN A nalytical M ethod PFOS by ESMS EXYGEN EXYGEN PFHS FOSA EXYGEN PFOA E03-0561-59481 7/21/2003 Components PFOS PFHS FOSA PFOA Equipment Blank - Dredge Result ND ng/mL ND ng/mL ND ng/mL ND ng/mL LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA Components PFOS PFHS FOSA PFOA Result ND ng/mL ND ng/mL ND ng/mL ND ng/mL 3 of 3 BL Q ualifier 0.05 BL Qualifier 0.4 0.4 0.4 0.4 BL QM.wtlfl.ee 0.4 0.4 0.4 0.4 BL Qualifier 0.05 0.05 0.05 0.05 BL Q ualifier 0.05 0.05 0.05 0.05 BL Q ualifier 0.05 0.05 0.05 0.05 Project Lead Review: Date: 000462