Document wgXVG5j5JwX5N45jKQD2BkVGo

Enclosure 5 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 ^3058 Research Drive kState College, PA 16801, USA P A G E m ^f . 800.281.3219 lF: 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 number assigned to the project is L34910. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC /M S/M S) was requested for all samples. A total of 26 samples were received for analysis. The samples were prepared and analyzed by LC/M S/M S for the following list of fluorochemicals: T able 1: T arget Analysis Compound Name Perfluorohexanesulfonate Perfluorooctanesulfonate Perfluorooctanoic Acid Perfluorooctanesulfonvlamide Acronym C 6 Sulfonate (PFHSf C 8 Sulfonate fPFOS) C 8 Acid (PFOA) FOSA The analytical methods used were originally developed for groundwater samples and were validated by Exygen. The validation protocol and results are on file with Exygen. Only the C 8 Sulfonate, FOSA, and C 8 Acid were included in the original method validation. It should be noted that the quality control elements included in this analysis demonstrate the applicability of the method to the additional analytes. 2 Sample Receipt The samples were submitted in plastic containers. All samples were cooled to 4C from time 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 Attachment C. 3 Holding Times Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 30 days of receipt. PACE2 OF5 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/M S/M S analysis. A forty-milliliter portion of sample was used for analysis. The samples were transferred to a C i8 SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatment 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 methanol). The methanol extract was diluted to forty-milliliters 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/M S 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 fluorochemicals are observed and quantitated against standards. A Hewlett-Packard H P 1100 HPLC system coupled to a Micromass Ultima M S/M S 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/M S/M S 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 .9 8 5 (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. PAGE30F5 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. Instrument 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/M S/M S analytical methods. 5.4 Matrix Spikes Field matrix spikes were prepared at low and high levels for each sample for all compounds of interest. Single laboratory matrix 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 Attachment B. For sediment samples, recovery is calculated from the amount present in the sample extract. Please see Section 5.7 foradditional discussion of matrix 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/M S/M S 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 S W -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. 6 Data Summary Please see Attachment 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. PACE 4 OF 5 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 maintained by Exygen. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: Raw Analytical Data (Surface W ater Samples) 8.5 Attachment E: Raw Analytical Data (Sediment Samples) 9 Signatures Other Lab Mem bers Contributing to Data Karen R isha PAGESOFS SECTION A Summary of PFOA, PFHS, PFOS and FOSA in Water Samples Analyte Found (ng/mL) C8 Acid PFOA C6 Sulfonate PFHS . Sample ID_______________ Perfluorooctanolc Acid__________ Perfluorohexanesulfonate . BC2SW-04 4.21 0 .8 9 6 BC2 SW-04* 4.21 0 .8 8 2 BC2 SW-04 Dup 2 .5 4 0.571 BC2 SW-05 BC2 SW-05* BC2 SW-05 Dup 0.591 0 .6 1 6 1.56 0 .155 0 .1 5 2 0 .377 BC2-SW-06 12.1 6 .06 BC2-SW-06* 12.3 6 .3 0 BC2-SW-06 Dup 11.6 5 .8 7 Outfall to River SW-25 15.8 7 .6 6 Outfall to River SW-25' 16.0 7 .1 0 Outfall to River SW-25 Dup 14.4 6 .7 7 Equipment Blank-Pump, ND ND Equipment Blank-Dredge ND ND Field Control/Travel Blank ND ND Sample 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 Blank-Pump Equipment Blank-Dredge Field Control/Travel Blank Analyte Found (ng/mL) C8 Sulfonate PFOS FOSA Perfluorooctanesulfonate Perttuorooctanesulfonylamide 11.5 11.5 8 .2 5 1.67 1 .3 9 1 .3 7 0 .7 9 0 0 .146 T.54 4 .3 3 26.1 2 6 .7 25.1 3 1 .2 3 1 .5 3 0 .8 ND ND ND , . . 0 .150 0 .3 8 9 2 .4 3 2 .30 2 .5 7 3 .2 6 3 .1 8 3 .2 8 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 x .3058 Research Drive m s tSatatte 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 lim ite d to th e term s and c o n d itio n s stated herein, unless o th e rw is e agreed to in a fo rm a l contract. CONFIDENTIALITY-- tn)%en Research ('Exygen." "us," 01 "we") 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, the ciienl 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 oflicer. PAYMENT TERMS--Unless otherwise set forth in this Purchase Order, terms of payment are "Net 30 Days." The time 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 chaige 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 o ' 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 iri writing, via a signed statement acknowledging and accepting responsibility for payment. Exygen will assume that.the paperwork submitted with a sample describes die desired testing protocol. Any changes to the protocol must be submitted in writing. Please fax changes to Exygen marked. "URGENT11 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 wiil 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 suicharge is usually added to the list fee if rush analysis is requested. M IN IM U M FEE--The minimum fee tor commeicial services is one hundred dollars (S100). SAMPLE COLLECTION/SUBMISSION--C\rent shall be responsible for propel 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. All samples submitted must be accompanied by: purchase order, 01 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. SAM PLE 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 arrangements have been made for long-ieirn storage, Exygen shall dispose of the sainple(s). Exygen shall charge: a monthly tec for long-term storage. Samples found or suspected to contain hazardous waste, according to definitions hi state an 'or federal guidelines, will be returned to the client upon completion of tfo analysis The cost of relutning the sampleis) will be invoiced lo the client Exygen reserves the right to chaige a disposal lee 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 conditions. An internal chain-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 of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required bv applicable law. QUALITY ASSURANCE-- Exygen will perfoim services consistent with its Quality Assurance Standard Operating Procedures (SOPsi. the terms of which are expressly incorporated herein by reference; provided, however, rt 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 order for work. In the event client desires an alternative to these SOPs. such requests must be made in writing prior to sample submission and acceptance by Exygen. ETHICS POLICY-- cxygen Research strives to provide its clients with the highest, quality data in the vastest realistic turnaround time. We balance the high standards of this goal by insisting that each employee also perfoim within the guidelines ol the highest possible professional ethics. Each Exygen employee is required to sign e 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 bv 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, AN D INSURANCE--Exygen agrees to indemnify, defend, and save the client, its officeis, 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, dealh. 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 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 dient. its officers, 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, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage. WARRANTY A N D LIMITS OF LIABILITY--In accepting analytical work, Exygen guarantees the accuracy of the test results for flip sample as submitted within the tolerances set forth in the SOPs We disclaim airy other warranties, expressed or implied by law. Exygen does not accept any legal responsibility for the purposes for which dient 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 O F PURCHASE ORDER -T h is Purchase Order becomes a ,, binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement of work. Report 1Analytical ^ Summary of PFOA, PFHS, PFOS and FOSA in $<5il Samples S am p le ID B.C2 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 A n alyte Found (n g /g , as re ceived ) ^ /* C8 A cid PFO A C 6 S u lfo n ate PFHS Perfluorooctanolc Acid Perfiuorohexanesulfonate 3 .0 2 0 .5 6 6 2 .1 4 5.14 4.41 14.2 13.6 10.7 7.59 17.7 0 .4 1 3 1 .4 5 1 .7 5 2 .4 6 2.61 3 .1 9 2 .2 6 4 .9 8 S am p le 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 A nalyte Found (n g /g , as received ) C 8 S ulfo n ate PFOS Perfluorooctanesulfonate FOSA Perfluorooctanesulfonylamlde \ 14.6 , 11.9 7 .1 5 7 .8 4 2 2 .8 2 5 .0 880 7 .8 6 12.1 7 1 .4 \ 992 107 8 3 .2 2 8.0 72.1 140 2 3 .5 3 5 .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 >^L305.3058 Research Drive k SStatatte College, PA 16801, USA V,T. 814.272.1039 F: 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services p rovided by Exygen Research are lim ite d tD th e term s and co n d itio ns stated herein, unless o th e rw is e agreed to in a form al contract. CONFIDENTIALITY--Exygen Research ("Exygen," "us," or " we") maintains the strictest confidentiality in all of our client interactions. If a signed confidentiality agreement is lequired, we will provide one. If a regulatory or 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 Exygen1s 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 appioval by Exygeri's legal council and must be signed by a corporate officer. PAYMENT TERMS-- Un\tm otherwise set forth in this Purchase Order, 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 to reasonable costs of collection, including, but not limited to, attorneys' fees. . BILLING--All fees and charges ate billed directly lo the client requesting services. Exygen will riot bill a third party without prior notification m 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, "URGENT" 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 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 lee if rush analysis is requested. M IN IM U M FEE--The minimum fee for commercial services is one hundred dollars ($100!. SAMPLE COLLECT/ON/SUBMISSION-- Client 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-oi-custody upon sample receipt unless the client includes one with the sample(s). By request, Exygen will provide cliairi-nf-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 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 ol sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SAM PLE 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 arrangements have Been made for long-term storage, Exygen shall dispose of tire sample(s). Exygen shall charge a monthly lee for long-term storage. Samples found or suspected to contain hazardous waste, aceoiduig to definitions in slate an /o r federal guidelines, will be returned lo the client upon completion ol (In* analysis. The cost of returning the sample(s) will be invoiced In the client. Exygen reserves the right to charge a disposal fee *ot the disposal of any and all samples unless returned by Exygen to client. Exygen shall, unless the natuie and character ot the sample dictaies otherwise, store all samples under locked, temperature-controlled conditions. An interna! chnin-ofcustody is maintained for each lot of samples received. HAZARD COMMUNICATION-- The client has the responsibility to inform the laboratory ot any known or suspected hazardous characteristics of the sample, and to provide information ori hazard prevention and personal protection as necessary oi otherwise required 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: provided, however, it shall be the exclusive responsibility of the client to confirm that Exygw's standard practices will meet the client's needs prior to placing an order for work. In the event client desires an alternative 1n these SOPs, such requests must be made in writing prior to sample submission and acceptance by Exygen. ETHICS POLICY-- Research strives to provide its clients with the highest quality data in the fastest realistic lurnaiound 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 fo 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 lo any subpoena for documents, for testimony in a court of law, or tor any other purpose '** relating to work performed by Exygen Reseaich 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, AN D INSUR ANCE-txygen agrees to indemnify, defend, and save the client, its officers, directors, employees, agents, and representatives harmless train all losses, expenses, demands, and claims made against the client, its officers, directors, ernpioyees^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 iri 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; tiowever. such indemnification and damages shall, in the aggregate, be limited to the amount equal fo the lesser of (a) damages suffered by the client as the direct result thereof, or tb; 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 SOPs We disclaim any other warranties, expressed or implied by law. Exygen does not accept any legal responsibility tor the purposes for which client uses the test results. Exygen will not accept any purchase order or any other order far work that includes conditions that vary from these Standard Conditions. ACCEPTANCE O F PURCHASE ORDER--This Purchase Order becomes a ^ binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement o( work. Proven Resulte. 5 Summary of PFOA, PFHS, PFOS and FOSA in d fi Samples S am p le 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 A nalyte Found (n g /g , d ry w e ig h t) C 8 A cid PFO A C 6 S u lfo n ate PFHS Perfluorooctanoic Acid Perfluorohexanesulfonate 4.31 3.06 7.39 6.34 23.6 22.5 16.9 12.0 26.2 0.809 0.591 2.09 2.51 4.08 4.33 5.05 3.57 7.39 S am p le ID A n alyte Found (n g /g , d ry w e ig h t) C8 S u lfo n ate PFO S FOSA . Perfluorooctanesulfonate Perfluorooctanesulfonylamide 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 2 0 .9 , 17.0 3 2 .8 3 6 .0 . 1460 1640 169 .1 1 4 208 1 0 .2 1 1 .2 1 1 .3 1 7 .4 118 138 4 4 .3 3 7 .2 5 2 .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 J ^ 3 0.350588 Research Drive ^ r m s tSatatte College, PA 16801, USA VJ: 814.272.1039 F: 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are lim ite d to the term s and co n d itio ns stated herein, unless o th e rw ise agreed to in a form al contract. CONFIDENTIALITY-- Exygen Research ("Exygen," "us," or " we") maintains the strictest confidentiality in all of cm client interactions. It 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 legal council and must be signed by a corporate officer. PAYMENT TERMS--Unless otherwise set forth in 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 satisfaclory 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 are billed directly to the client requesting services. Exygen will not bill a third party 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. "URGENT" 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 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 amilysis is requested. M IN IM U M FEE-- The minimum fee for commercial services is one hundred dollars ($100). SAMPLE COLLECTION/SUBMISSION--C \\tn\ 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 al 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. All samples submitted must be accompanied by: purchase order, or signed quotation; sample description, including sample type, source, time and date ot 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 preservahve 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. SAM PLE 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 arrangements have been made for long-term storage. Exygen shall dispose of the samplers) Exygen shall charge a monthly fee for long-term storage. Samples found or suspected (o contain hazardous waste, according to definitions in state an /o r federal guidelines, will be returned to the client upon completion of ths* analysis. The cost of returning the samplers) will be invoiced to 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 and character of the sample dictates otherwise, store all samples under locked, temperature-controlled conditions. An internal chain-ofcustody is maintained for each lot of samples received. HAZARD COMMUNICATION--The client has the responsibility to infor in the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary oi otherwise required by applicable law. QUALITY ASSURANCE--Exygen will perfoim services consistent with its Quality Assurance Standard Operating Procedures (SOPs). the terms of which are expressly incorporated herein by reference; provided however, if shall be the exclusive responsibility of the 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 desires an alteinative to these SOPs. such requests must be made in writing prior to sample submission and 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 o f 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 statement of personal and professional integrity. SPECIAL REPORTS--McMtona\ charges may be necessary for custom report formats LITIGATION--All cosls 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 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, AN D INSURANCE--tx y g in 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, director, 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 reptesentahves 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 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, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage. WARRANTY AN D LIM ITS 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 SOEs. 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 O F PURCHASE ORDER-- This Purchase Order becomes a binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement of work. SECTION B Recovery Summary for PFOA, PFHS, PFOS and FOSA In Water ______________________ C8 Acid PTOA_________________________ C6 Sulfonate PFHS . Sample Description Amount Amt Found Amount Amount Amt Found Amount Spiked In Semple Recovered Recovery Spiked in Sample Recovered Recovery (ng/mL) (na/mL) (na/mL) <%) (ng/mL) (ncj/mL) (no/mL) (%) BC2 SW-04 Lab Spika 5 4.21 8.14 79 5 0.896 5.52 92 BC2 SW-04 Low Spike 0.1 4.21 2.76 -1450* 0.1 0.896 0.647 -249* BC2 SW-04 High Spika BC2 SW-05 Lab Spike 10 4.21 9.92 57 10 0.896 9.73 88 s 0.591 4.96 87 5 0.155 5.00 97 BC2 SW-05 LOW Spika 0.1 0.591 2.17 1579' 0.1 0.155 0.607 452 BC2 SW-05 High Spke BC2 SW-06 Lab Spike 10 0.591 s 12.1 7.21 66 10 0.155 17,8 114 5 6.06 9.58 11.8 94 115 BC2 SW-06 Low Spka 0.1 12.1 13.9 1800' 0.1 6.06 7.11 1050' BC2 SW-06 High Spke \ 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 0.1 15.8 15.0 -800' 0.1 7.66 6.64 -1020' Outfail to River SW-25 High Spke 10- 15.8 26.2 104 10 7.66 18.1 104 Field Control/Travei Blank Low Spike 0.1 ND 0.114 114 0.1 ND 0.119 119 Field Control/Travei Blank High Spike 10 ND 11.9 119 10 ND 10.8 108 Sample Description C Sulfonate PFOS_____________________________ FOSA Amount Amt Found Amount Amount Amt Found Amount Spiked In Sample Recovered Recovery Spiked In Sample Recovered Recovery (nm L) (ng/mL) (ng/mL) <%) (no/mU (ng/mL) (no/mL) (%) BCZ SW-04 Lab Spike 5 11.5 ' 17.1 112 5 1.39 5.58 84 BC2 SW-04 Low Spke 0.1 11.5 6.89 -4610' 0.1 1.39 0.672 -718' BC2 SW-04 High Spke 10 11.5 17/7 62 10 1.39 7.18 58 BC2 SW-05 LabSpke 5 1.67 5.94 85 5 0.146 4.86 94 BC2 SW-05 Low Spke 0.1 1.67 5.37 3700' 0.1 0.146 0.498 352 BC2 SW-05 High Spke 10 1.67 )za 111 10 0.146 4.14 40 BC2 SW-06 Lab Spike 25 26.1 49.8 95 5 2.43 7.10 95 BC2 SW-06 Low Spike 0.1 26.1 32.1 6000' 0.1 2.43 2.55 120* BC2 SW-06 High Spke 10 26.1 43.9 178 \ 10 2.43 8.44 60 Outfall to River SW-25 Lab Spike 50 31.2 80.9 99 5 3.26 7.97 94 Outfall to River SW-2S Low Spike 0.1 31.2 29.4 -1800' 0.1 3.26 2.66 -600* OutfaHto River SW-25 High Spke 10 31.2 41.2 100 10 3.26 9.02 58 Field Control/Travei Blank Low Spike 0.1 ND 0.109 109 0.1 \N D 0.0898 90 Field Control/Travei Blank High Spke 10 ND 11.4 114 10 NO 11.9 119 NONot DetectedReaporse between 0 and 0.025 ng/mL NGNot Q uantiflabte-Responae between 0.025 ng/mL and LOQ (0.05 ng/mL) 'Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. 3058 Research Drive ^ W s tSatalte College, PA 16801 VT: 800.281.3219 F: 814.272.1019 exygen.com USA Proven Resulte. R eco very S um m ary fo r P FO A , P FH S , PFO S an d FO S A in S o il Sample \ Description _____________________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) <%) BC2 SED-04 Lab Spik 40 3.02 41.5 96 40 0.566 42.2 104 BC2 SED-05 Lab Spike 40 5.13 43.7 96 40 1.46 44.2 107 BC2 SED-06 Lab Spike 40 14.2 49.4 88 40 2.46 44.5 105 Outfall to River SED-25 Lab Spike 40 10.7 47.1 91 4 0 3.1 9 44.5 103 Sample Description 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 Amont 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 J & 3 30055f8 Research Drive - E m s tSatalte College, PA 16801, USA YT: 800.281.3219 F: 814.272.1019 exygen.com SECTION C '/ZraceAnalyticar I Required C ileni Information; Section A m i ss3Compari/t g r + , Address CHAIN-OF-CUSTODY / Analytical Request Document The Chaln-of-Custody Is a LEGAL DOCUMENT. All relevant fields must be completed accurately. Required Client Information:______ S s C tiO H B `Report To: 17 Ff\r, J e GldfrJqe^ Copy To: Page: J of fX. Invoice To: C lient Inform ation (Check quota/contraci): Requested Due Date: TAT: 715679 To Be Completed by Pace Analytical and C lle nl Quote Reference: S e c tio n C Project Manager P.O. Turn around times less than 14 days subject to laboratory and contractual obligations and may result in i Rush Turnaround Surcharge. Profile # t-K b T E 0 '3 ~ q & ( p I pD Fax utfi------ `i r / W v te te ir 4- 5e<iliV*^>i T30?-// Turn Around Time (TAT) h calendar day. Requested Anelyels: Section D Required Client Information: S A M P L E ID One character per box. (A-Z, 0 - 9 / . - ) Sample IDs MUST BE UNIQUE ,,w V.i'. S 3l> s j! \ fH Si dr 0 -47-1 if > v *?v date COLLECTED -4Valid Matrix Codes ----- ^ MATRIX CODE aLU Preservatives MATRIX C O D E J fcv? WATER SOIL OIL WIPE AIR TISSUE OTHER P| WT SL OL WP AR TS OT rI\fL4*m-mi , J 1 5 5 S5" uLU Pd 8 hhrmm a/p ton 'cca 8 Unpreserved %Xo. zron 0X 1 zdCaO2J0ac<Z30 i m fief 7-31`03 / W ^ 7 1 m 'M 1 ti& T-JJ-63 / w r L 1 \ &/ 7 V T l V T J / / / rf//1 / / / / / / / / / / Remarks / Lab ID 2S .y.-. uteyi- yk y.{J H ' i k - t . h ? &e-- i P r ., -,y.1___ _ - 1 % H% PS (L.i t _ s m C g? - J U *"i s < c '-"1 f e a| 4 -0 D II -.V/S' y_ * : v iS r \_2 D D tei 1 His 1 ,.H .X-lj juL. tK. A it iu: If Li i 5 a i a0 V; -i <!?> !-Vi S -- a i*i'L. fis f W P* S w u It s _ iV<'r ShWr i s '.1l illi in if SL r * SHIPM ENT METHOD ^ sd r4si 8 >E\> - a * i 'i-ty'- ^ WT i^ o k 1 B i-'Hv m f -T> p l) > )Hl3 L I j __ B Tjr - m I j Sfe "1 1 it < i M 3 fcrr ? W o 3 " 1 rr (?# / o r Tl^V0*' i M 3 Arr h ii Hr M/S L L //S c L \& [< & * / L r jj I / i 8 f vr 7/*3/o? \ 8 ! Tff? UJ 7 / t i / o / ! / < t 1 S W--V _ Ibtf l / I ITEM NUMBER R E L IN Q U IS H E D BY / AFFILIATION 1 1 r DATE t |_ - s m& P I" ! $ !! _ 1 __ ji _---_----1I L J V 9 / 0 - 5 " s iyi -*7; ^ -- ^ u . 1/ L Jyvro - Y iy i ; i i L . 3 r?/<3 - / o vM- f<Lw - J V 9 /4 _ i I i l: T IM E (M 8 y>rrk L 3r H *----v----i--*------- f* i^- . // J/ / j i I n 1g 3--L------- *9/- / ___ 9 S w|if ife CV9/a ~ I 9 S >& 74 L */9/a -Z e A C C EPTED BY / AFFILIATION DATE TIM E J 5; J SAMPLE CONDITION Temp in C ,1 Received on Ice y n Sealed Cooler Samples Intact ' n Additional G ' 'X.ents: SAMPLE NOTES 0 i ( f > " // d d /# n r4 , fV tT x im o / ' S P tv ff^ 0<p tu ~57Rf7ir~i ^2S' t r O 'O f t * ) I fa l 'iv v t 0 /2 d lftr u s ts ft g r V - ^ g ik = ^ ~ /r * * c jr SA M PLER NAME AND SIGNATURE PRINT Nairn y i x h s ig n a tu r e ypLER. ) -1 / r r -- -- t- +l kr/`k/ / / > DATE Sign*,( (M M /D O /Y Y ) fA 3 /o i  f faace. Analytical" www.pacalabs.com A c q u ire d Oient Information: Section A Company 3m g 7 js j> Address (5 ) WA* OS3 CHAIN-OF-CUSTODY / Analytical Request Document The Chaln-of-Custody is a LEGAL DOCUMENT. All relevant fields must be completed accurately. R e q u ire d Client Information: TtssReport To: v ^ Copy To: Section B }Jr>'<Ue. Page: g o f 3 , Client Inform ation (Check quote/oontract): Requested Due Date: . |*TAT: 639392 To Be Completed by Pace Analytical and C lient Quote Reference: S G C tiO fl C Project Manager P.O. R * 6 w C reek. * * r a ts m e h r, f S E p ttr tm i Project Number X x fT tfm b e r 30 ? // Turn around times less than 14 days subject to laboratory and contractual obligations and may result In a Rush Turnaround Surcharge. Turn Around Time (TAT) In calendar days. Project #: 3 t t t A-b f n t f e c f f J u m t r r 7e O 3 -Q S ~ / SAMPLE CONDITION Temp in C Received on Ice Y/N Sealed Cooler Y/N Samples Intact Y/N rAdditional r nts: AIRBILL NO. SAMPLE NOTES SHIPPING DATE NO. OF; COOLERS I ITEM NUMBER RELINQUISHED BY / AFFILIATION !1 / 1 \------------------- V _i - i ______ _ _ ,. DATE TIME im ACCEPTED BY / AFFILIATION 70 ----------------------------- 7 s -- *i DATE TIME SAMPLER NAME AND SIGNATURE PRINT Name of S, 2 L \jr-u. SIGNATURE AMPLER: ______ DATE Sigr' (MM / DDCD /YY> i- J^/oy 7/ 21/2003 Project: E3-0561 3M ENVIRONMENTAL LABORATORY Preminary/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 flU K c NfTfe ft* + f t l l W a . - ' k f ' ' C x *d ('^ \o -> -fjv t y - ft'ih t Protect Results/Activitv Pace Field Sampling Event 3M Sample Number E03-0S61-49786 ' Sampled Date 7/22/2003 UB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49787 7/22/2003 LAB EXYGEN EXYGEN EXYGEN Aaalyiltal Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49788 7/22/2003 LM EXYGEN Aailytltal Method PFOS by ESMS EXYGEN EXYGEN PFHS FOSA EXYGEN PFOA 03-0561--49789 7/22/2003 LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49790 7/22/2003 LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49791 7/22/2003 LAB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA Sample Description BC2 SW-04 Componen PFOS PFHS FOSA PFOA BC2 SW-04 DUP Componen PFOS PFHS FOSA PFOA BC2 SED-04 CQtppfnfn PFOS PFHS FOSA PFOA BC2 SW-05 Coran,9nen PFOS PFHS FOSA PFOA BC2 SW-05 DUP Componen PFOS PFHS FOSA PFOA BC2 SED-05 C h w k "!? PFOS PFHS FOSA Result SL Oualifier Result EL Qualifier Result - Result SL Qualifier EL Qualiflir Risal EL Qualifier Result SL QHalill.tr 7/21/2003 3M ENVIRONMENTAL LABORATORY Prelim inary/Unauthorized Report Project: E03-0561 (cont.) 3M Sample Number E03-0561-49791 (cont.) Sampled Date 7/22/2003 Sample Description BC2 SED-05 LAB EXYGEN Analytical Method PFOA E03-0561-49792 7/22/2003 Components PFOA BC2 SW-06 Result LAB EXYGEN Analytical Method PFOS byESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49793 7/22/2003 Components PFOS PFHS FOSA PFOA BC2 SW-06 DUP BftgR LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49794 7/22/2003 Components PFOS PFHS FOSA PFOA BC2 SED-06 R m lt LAB EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49795 7/22/2003 PFOS PFHS FOSA PFOA Outfall to River SW-25 Eflflli LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Metbart PFOS by ESMS PFHS FOSA PFOA E03-0561-49796 7/22/2003 IAB. EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49797 7/22/2003 Components PFOS PFHS FOSA PFOA Outfall to River SW-25 DUP ClfllUfU1111 PFOS PFHS FOSA PFOA Outfall To River SED-25 Remit BfZfll! LM EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49813 7/22/2003 CpntP94?nte PFOS PFHS FOSA PFOA Outfall to River SED-25 DUP Snail LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA CffitflDffibfnte PFOS PFHS FOSA PFOA Remit 2 of 3 BL Oualifier EL Oualifier BL QnaUec BL Oualifier BL Oualifier BL Qualifier BL Qualifier BL Qualifier 7/ 21/2003 3M ENVIRONMENTAL LABORATORY PreHminary/Unaudiorized Report Project: E03-0561 (coni.) 3M Sample Number_______Sampled Date_______ Sample Description E03-0561-59479 Field Control/Travel Blank LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytic! Method PFOS by ESMS PFHS FOSA PFOA E03-0561-59480 Component PFOS PFHS FOSA PFOA Equipment Blank - Pump Result LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-056I -59481 C w itn tn|i PFOS PFHS FOSA PFOA Equipment Blank - Dredge Result U fi EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA Component PFOS PFHS FOSA PFOA Result 3 of 3 SL Oualifler L Qualifier EL Qualifier 3058 Research Drive State College, PA 1.6801 ' >4 Phone: 800-281-3219 Fax: 814-272-1019 */ Laboratory Sample Log-in Sheet (Environmental) Complete upon sample receipt: Client and/or Project Name ^ W r /( A A / ./ Method of Delivery Walk-in Tracking #: Pick-up D UPS If fa ff ZfFedEx. 0 Air Borne n Other (explain) Chain of Custody Temperature Preservation Custody Seals: presguM rQ intact / broken (explain) D-oCsent Thermometer ID: 2- P f Cooler ID: " / seco/ifo Cooler ID: Cooler ID: Cooler ID: Cooler temo: Cooler temo: Cooler temD: Cooler temo: , ' f *C C *C C Chain of Custody Record: .^"present 1 absent Samples Received: ^ 0 o n ice in ice melt with ice pack none Explanation Completed by Sionature: / Complete durincsamplelop-ln: " UM S Log-in # .- - Physical Condition Samples intact? Chain of Custody Samples received agree with COC record? Analysts Request Analysis request clear? Preservation Sample containers appropriate? Chemical presentation appropriate? Samples received within holding time? Sample volume/mass adequate? . . ........................ , , "Date (Time): y j ? f / r ? !* )* J Y 1 /- ' ^ p -Y e s No (explain) -E T e s No (explain) ^ Y e s No (explain) Yes No (explain) Yes No (explain) Yes No (explain) Yes No (explain) . * Explanation Completed by Slanature: / Complete followlno resolution of an v nonconformances: Client Contacted Yes Client: No Resolution . Date: ,, A *M Date (Time): ' Completed by Slanature: Lab Sx Log-in Sheet -Ex Date: 11-5-01/0  ( f # f * e e. & U S A A i r m -B f i m S S b 3 2 M 3 0 1 From B -- Sender' Name Phone 9 k y 4a Expraii Package Service ->/ \, Pcksgstup ta 150104. WMHWmT mwmou--nto*Fpayy--baMt l*aabtu mr n*i nif. TOTadEx PriorityOvernight p j 'FedEx Standard Overnight I 1 FedExFirst Overnight ^ M tan n iiM M t /\ 4 i^ 4 tv m u ilH io M A. 1-- 1 ta rik e a a * kuMnaiiMom* M m rttN lidbM ioiu i I FedEx2Day Q FedEx Express Saver S*ond Um s day Hwdbuwwntiv fadfc tn>atomrmnot.aMtaMjr*iwtftauaOo-aound ---- uompanv 4b Express FreightService1 - -------- (Mn^tanHPManciikMafgtailWt eivheiarn15a0jrlibMs. Address y n i-j K m i i n & /< *. .^uTTi /fin tf&yAMrwWnM FedEx IDay Freight* N M M m fW dir ' Ca( In Carirmatet . 5 Packaging j I fedE*2Day Freight '-- ' SacandbuMMJtdai FedEx30ay Freight Hardb u a t e t day ' OtcUMd t In* SB) City 1 Yau( Interjal Billing Referenca Recpienl' Name Lr fL ^ J u J i/q _ _ Company I Address_____________ fc 'MXp` a<fsdi tame*, printftd&idtW tai st / ( y r . z l J n M f.4 % ^ -- g. zip n FedExEnvelope* FedEx Pik* ^Other \cy.<vUita d t. Snat f a t Ft i Legi ftk . r< 4 h ilt Study fife -- " ' 'V 6 SpacialHandling lAchrda Faji A fem Socm 1 ......'[ -- 1 lURDAYDeSmy r--I HOU) Weekday i-- i JJ0U3 Satorday * fc j V I I *naj>tfaarapbPadEir<My I_i el FedExLocation Nat m alate In %[__I 4atdFaekdtEx%loiecation Fadafb*Ovn*)d F e ta Pnom Ortmglx Imi thisatupnantcontateSugarawleedrf MSMEkHW talM iiiM i ----------- - - - O tiahoateuiiiatlM cl'K d , 1T>tto n Yes r ~ l Yes (JO I-- I A s a e a ta d e d 1 I SnapariDatera* J \ SippariOadaMA M ita M .Oawgeo>ifiod>|wauda|Oivlc(crnitaYiW)padreg>aai:taga^ Dry Ice M et Cargo Aircraft Only Wfcratdafav tZ . k n orf.tt t e n 7 Payment fl/ffie: / lobtanfiecip I ----- l u . c frale Xc3.t t e a C a f t Card Ma. b a i o * . -------------------j '-- A cct No. Recipient J lT h ird Party Q Credit Card QCasWCbeck Address 3 - S~4 3 ____ b r i ^ g - (*> r> ) ___j i f a ? a_ I d / / U ^ T ^ g fty) ZIP A415 5b3fl 243C , Ho m . .... TOur a fey it fcdiyr la ^ l w j f f s y i j u t i m higlw v tW S< b>d; 1erd e ta il Rabais Signp*rjf i n abfco*' Mltea acan ti uynst*ra. L 4 4 b ]. ,. . ' i t i ' . ByaigqineyouaueiortreiMMWSnaipm<ari^^obti^aignMira ind agra* to Iftdmarly a n f l U us h a rrt horn anym ulling c la m . ' Queidon} VHItfitjr Web alte at fodiex.com orcM1R)0Ci>rOji` WX6U333e ., ftv IU!afll*rt/l:-.NilfU>lkH .tt)llK>*owml>MlUA YWSttt} *"*"-* ...-i .v v .> a i^ * 3 i 5 i ^ V ^ > - - V A \v .- - .* .:. - .......... LOGIN CHAIN OF CUSTODY REPORT (InOl) Jul 28 2003, 07:54 am Login Number: L34910 Account: 2046 3M ENVIRONMENTAL LABORATORY Laboratory Sample Number Client : Sample Number Collect 'Receive = ' Due Date Date' ;P R D a t e , L 3 4 910-1 BC2 SW-04 SAMPLES KEPT IN D0000539 21-JUL-03 25-JUL-03 L34910-2 : BC2 SW-04 L O W SPK (0.1 PPB) 21-JUL-03 25-JUL-03 'L34910-3 , BC2 SW-04 H I G H SPK (10 PPB) 21-JUL-03 25-JUL-03 L34910-4 . .- V: BC2 SW-04 DUP 21-JUL-03 25-JUL-03 L34910-5 SOIL V:;i; ; : 3C2 S E D - 04 23-JUL-03 25-JUL-03 S'PERC S O L I D ........... Hold: 01-AUG-03 d0000539 L3491 0 -6 : : : BC2 SW-05 21 -J U L - 03 25-JUL-03 L34910-7 : BC2 SW-05 LOW S P K ; ( 0 . 1 .PPB):21-JUL-03 25-JUL-03 L34910-8 . BC2 SW-05 H IGH SPK (10 PPB). .21-JUL-03: 25:-JUL-03. .. L34910-9 W' : , BC2 SW-05 DUP . 21-JUL-03 25-JUL-03 L34910-10 BC2 S E D - 05 SOIL S PERC SOLID ; . 21-JUL-03 2 5 - J U L - 0 3 ;:: H old :0 1 - A UG-03 d0000539 " .V-;:,:..-: ; L34910-11 V 3C2 S E D - 06 SOIL S PERC SOLID . 2 3 -JUL-03 25-JUL-. H o l d : 0 1 -AUG-03 d00CC539 L34 910 -12 . BC2 SW-06 23-JUL-03 25-JUL-03 L 3 4 9 1 0 - 1 3 .i; : BC2 SW-06 LOW SPK (0.1 PPB) 23-JUL-03 25-JUL-03 L34 910-14 :. BC2 SW-06 HIGH S P K (10 PPB) 2 3 -JUL-03 25-JUL-03 L34910-15 . . . BC2 SW-06 DUP 23-J U L - 0 3 ;2 5 - J U L - 03 .. /';'/it. ; L34 910-16 : . .. O U T F A L L T O ,RIVER SW-25 2 3 -JUL-03 2.5- J UL-0.3 . . L34910-17 ' ; : OUTFALL TO RIVER SW-25 23-JUL-03 25-JUL-03 C O M P L E T E ID READS OUT F A L L TO R I V E R SW-25 LOW S P K (0.1 P P B ) ....... ;: L34910-18 : : OUTFALL TO RIVER SW-25 23-JUL-03 25-JUL-03 C O M P L E T E ID READS O U T F A L L TO R I V E R SW-25 H I G H S P K (10 PPB) . L 3 4 9 1 0 - 19 : OUTFALL TO RIVER SW-25 DUP 23-JUL-C3 25-JUL- Page 1 LOGIN CHAIN OF CUSTODY REPORT (InOl) Jul 28 2003, 07:54 am Login Number: L34910 Account: 2046 3M ENVIRONMENTAL LABORATORY Laboratory Sample Number Client Sample Number Collect Date Receive Date Due PR Date L34910-20 , OUTFALL TO RIVER SED-25' 23:-JUL-03 25-JUL-03: SOIL S PERC SOLID H o l d :01-AUG-03 d0000539 L34910-21 O U T F A L L .TO RIVER, SED-25 D U P L 23-JUL-03 25-JUL-03 ;- ;-v SOIL S PERC SOLID H o l d :01- A U G - 03 d 0 0 C 0 5 3 9 ................ L34910-22 ^ F I ELD CONTR O L / T R A V E L B L A N K 2 3 - U U L - 0 3 ::25:-;iIUL-.03:.: : ; L 3 4.910 -23 ; , F I E L D CONTROL/TRAVEL: B L A N K LOVi 23 -J U L -03 2 5 -J U L - 03 - A C O M P L E T E ID READS FIE L D CONTR O L / T R A V E L B L A N K L O W SPIKE (0.1 P P B ) . L34910-24 FIELD C O N T R O L / T R A V E L B L A N K 23-JUL-03 25-JUL-03 ' i i. C O M P L E T E ID READS FIELD C O N T R OL/TRAVEL B L A N K H I G H SPIKE (10 PPB) .......... L3 4910-25 ,. E Q U I P M E N T BL A N K - P U M P .21- JUL- 03 2 5 -JUL- 03 ...i L34910-26 v :r\-;v E Q U I P M E N T B L A N K - D R E D G E .23 -JUL.-.O3 2 5 -JUL-03 Page 2 Signature : Date : SECTION D Bt 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Date: 08/26/03 Exygen Study # L34910 NOTE TO FILE NOTE: Throughout the raw data generated for study L34910 the 498 > 78 monitored transition (perfluorooctanesulfonylamide) was assigned the acronym PFOSA instead of FOSA. Any reference to PFOSA in the raw data is equivalent to FOSA. Initials: 4 Ol 2 k ) D 3 Sponsor Study No: NA V Exygen Study No: L34910 Analyte: PFOA Ions Monitored: 413->369 Site: Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ppt 15pL Water 40.0 mL 5.0 mL Set No.Analyst Instrument Type: Extraction Date: Analyzed on: 073103A Karen Risha LC/MS/MS Unit # 6 07/31/03 08/01*02/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC0725O3-4 XC072503-5 XC072503-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spk B L349UM Spk C L34910-6 Spk D L34910-12 Spk E L34910-16SpkF 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 L34910-12 L34910-12 Rep L349HM5 L34910-I3 L34910-L4 XC071503-4 L349HM6 134910-16 Rep L34910-I9 L34910-17 L34910-18 XC072503-5 L34910-25 U 4 9 10-26 L34910-22 L34910-23 U49I0-24 XC071003-6 Sponsor ID BC2SW-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 B C l SW-05 BC2 SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk - - BC2SW-06 BC2SW-06 BC2 SW-06 Dup BC2SW-06 Low Spk BC2 SW-06 High Spk - Outfall to River SW-25 Out&ll to River SW-25 Outfall to River SW-25 Dup Outfell to River SW-25 Low Spk Outfall to River SW-25 High Spk - Equipment Blank-Pump Equipment Blank-Dredge Held Control/Travel Blank Field Coottol/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 es 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-1005 073103A-I006 073103A-1007 073103A-1008 073103A-1009 073103A-1010 073103A-1Q11 073103A-1012 073103A-1013 07303A-1014 073103A-1015 073103A-1016 073103A-1017 073103A-1018 073103A-1019 073103A-1020 073103A-1021 073103A-1022 073103A-1023 073103A-1024 073103A-1025 073103A-I026 073I03A-1027 073103A-1028 073103A-1029 073103A-1030 073103A-1031 073103A-1032 073103A-1033 073103A-1034 073103A-1035 073103A-1036 073103A-1037 073103A-1038 Q731Q3A-1039 073103A-1040 073103A-1041 073103A-1042 073103A-1043 073103A -1044 073103A-1045 073103A-1046 Analyte Found (ppt) * (peak area * intercept) f slope x DF Recovery (%} * (analyte found (ppt)-analyte found in control (ppt)| x 100 amount added (ppt) Std. Cone. (PPO 0 25 50 lOO 250 500 1000 25 50 100 250 500 1000 Dilution Peak Factor Area 550 8614 16102 29438 66169 142891 264459 267 1 659 1 14411 I 132909 10 239247 10 145872 10 418651 10 ' 515606 6931 1 849301 826648 1 575640 I 605630 100 29529 13780 1 173871 1 . 181075 1 355190 1 521363 100 21596 31758 1 2471389 1 2425189 1 2527002 I 2849870 100 71294 75537 1 3072978 I 3276529 1 2758295 1 3102823 100 77205 156964 1 652 1 940 1 808 l 34004 100 35258 - 322068 Analyte Found (ppo Amount Added (ppo Recovery (%) ND 47.6 452 8140 4960 * 50 500 5000 5000 5000 95 90 79* 87 - * * 9920 591 616 * 7210 5000 100 10000 100 10000 - - . 57* 66 - 24200 100 10000 . - 121A -` - `- - - 26200 100 10000 . 104 - ND ND ND U4 11900 100 10000 114 119 - - Ctandypt Curve : Linear (I/x weighted) Intercept * 445.057 Slope 293343 Coef. O f D el - 0.986042 CS * Calibration standard LF * Lab fortified sample C Control sample FF * Field fortified sample S * Sample LCS a Laboratory Control Spike CK * Check Standard ND * Not detected a Response between 0 and 23 ppt NQ Not quantifiable * Response between 23 ppt and LOQ (50 ppt) Spreadsheet prepared by:. ASample was corrected using the data found in set 073103AR. Sample requires fiither dilution. See data set 073103AR Sponsor Study No: Exygen Study No: Analyte: loos Mooitored: Site: NA L34910 PFHS 399 -> 80 Decatur Baker's Creek RAW DATA REPORT Lindt 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: 073ICOA Karen Risha LC/MS/MS Unit # 6 07/31/03 08/01*02/03 Exygen ID XC0725Q3-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spk B L3491CM SpkC L34910-6 SpkD L34910-12SpkE L34910-16SpkF XCQ725Q3-1 L34910-1 L34910-1 Rep L34910-4 L34910-2 L34910-3 XC072503-2 L34910-6 L34910-6 Rep L34910-9 L34910-7 L34910-8 XC072503-3 L34910-12 L34910-12 Rep L34910-15 L34910-13 L349I0-14 XC072503-4 L34910-16 L349HM6 Rep L34910-19 U4910-17 L349UM8 XC072503-5 L34910-25 U 4 9 10-26 L34910-22 L34910-23 L34910-24 XC071003-6 Sponsor ID BC2 SW-04 BC2 SW-05 BC2 SW-06 Outfall to River SW-23 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 Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-2S 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 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 073103-1003 073103A-1004 073103-1005 073103A-1006 0731G3A-1007 073103-1008 073103A-1009 073103A-1010 Q731Q3A-I011 073I03A-1012 073103A-1013 073103A-1014 073103A-1015 073103A-1016 073103A-1017 073I03A-1018 073103A-1019 073103A-1020 073103A -1021 073103A-1022 073103A-1023 073103A-1024 073103A-1025 073103A-1026 073103A-1027 073103A -1028 073103A-1029 073103A-I030 073103A-I031 073103A-1032 073103A-1033 073103A-1034 073103A-1035 073103A-1036 073I03A-1037 0731Q3A-1038 073103A -1039 073103 A -1040 073103A-1041 073103A-1042 0731Q3A-1043 073103A-1044 073103A -1045 0731Q3A-1046 Analyte Found (ppt) (peak area intercept) / slope x DF Recovery (9b) = fanalyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) S ii Conc. (PPt) 0 23 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Factor 10 10 10 10 100 100 100 . 100 100 Peak Area 0 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 tax) Amount Added (PPt) Recovery <%> ND 49.7 475 5520 5000 896 882 571 647 9730 155 152 377 607 9580 * * 17400 * * 18100 ND ND ND 119 10800 50 500 5000 5000 5000 5000 - - 100 10000 - . - 100 10000 .. 100 10000 '. . . 100 10000 . 100 10000 99 95 92 97 -249+ 88 452 94 113. . 104* 119 108 -- - Starnimi P i r e : Linear (1/x weighted) Intercept * -23.5660 Slope * 53.9970 Coef. Of D el - 0.989093 CS * Calibration standard L F Lab fortified sample C Control sample FF < Held 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: In to ^Sample was corrected using the data found in set 073103AR. 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-. Exygea Study No: Analyte: loos Monitored: Site: NA L34910 pros 499 -> 99 Decatur Baker's Creek RAW DATA REPORT Limit rtf Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 30 ppt L Water 40.0 mL 5.0 mL Set No: Analyse Instrument Type: Extraction Date: Analyzed om 0731Q3A Karen Risha LOMS/MS Unit # 6 07/31/03 08/01-02/03 Exygea ID XC072503-0 XC072503-1 XC072503-2 XC0725O3-3 XC072503-4 XC072503-5 XC072503-6 Methanol Wash 0106020 Cootrol 0106020 Spk A 0106020 SpkB L34910-1 SpkC U4910-6 Spk D L349IO-12 Spk E L34910-16 Spk F XCO72S03-\ L34910-I 134910-1 Rep L349I0-4 L34910-2 L34910-3 XC072503-2 134910-6 134910-6 Rep L34910-9 L34910-7 134910-8 XC072503-3 L34910-12 L34910-I2 Rep 134910-13 134910-13 13491014 XC072503-4 134910-16 L34910-16 Rep L34910-I9 L34910-17 13491018 XCQ72503-5 13491025 13491026 L3491022 U491023 13491024 XC071003-6 Recovery (%) Sponsor ID - _. BC2SW-04 BC2SW-05 BC2SW-06 Outfall to River SW-25 -' BC2SW-04 BC2SW-04 BC2SW-04 Dup BC2 SW-04 Low Spk BC2 SW-04 High Spk * BC2SW-05 BC2 SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-05 High Spk BC2SW-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-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 LF LF LF CS S s s FF FF CS S s s FF FF es S S S FF FF es S S s FF FF es s s s FF FF CS Run No. 073103A-1001 073103A-1002 073103A-1003 073103A-1004 073103A-10G5 073103A-1006 073103A-1007 073103A-1008 073103A-1009 073103A-1010 073103A-1011 073103A-1012 073103A-1013 073103A-1014 073I03A-10I5 073HHA-1016 073103A-1017 073103A-1018 073103A-1019 073103A-1020 073103A-1021 073103A-I022 073103A-1023 073103A-1024 073103A-1025 Q73103A-1026 073103A -1027 073103A-1028 073103A-1029 073103A-1030 073103A-1031 073103A-1032 073103A-I033 073103A -1034 073103A-1035 073103A-1036 073103A -1037 073103A-1038 073103A-1039 073103A -1040 073103A-1041 073103A -1042 073103A -1043 073103A-1044 073103A-1044 073103A -1046 [analyte found (ppO-analyte found in control (ppt)l x 100 amount added (ppt) Std. Cane. (PPt> 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Analyte Dilution Peak Found Factor Area (ppt) 0 971 . 1963 . 3040 7518 17228 32298 *. 0 -0 * ' nd * 1673 50.4 13199 10 50011 445 * 10 20296 5940 10 96734 * 10 120697 954 280183 274170 211725 191631 * 100 6016 17700 1656 44922 46036 112926 149088 * * 100 4333 12800 3500 1 558236 571211 1 560118 1 667186 * 100 14981 43900 8521 i 691166 1 707270 I 636333 1 683639 * * 100 14072 41200 19341 . 1 316 ND 1 0 ND 1 0 ND 1 3691 109 100 3833 11400 - 35665 Amount Added '' 50 500 5000 5000 5000 5000 . . .' . 100 10000 . . . . 100 10000 . 100 10000 . . . . 100 10000 . . . . 100 10000 Recovery (%) 101 89 85A 62 1UA 178 100* 109 114 - S lan ted Cmvt : Linear (1/* weighted) Intercept * -56.2500 Slope - 34.2805 Cocf. Of D et 0.992844 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 23 ppt NQ Not quantifiable - Response between 23 ppt and LOQ (30 ppt) 1 Spreadsheet prenared by* ' r --' ASamplc 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 set 073103AR. 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 Volume: Final Volume: 50 ppt 15 nL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 073103A Kaien Risha LC/MS/MS Unit # 6 07/31/03 08/01-02/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072S03-4 Sponsor ID Sample Code CS CS CS CS CS Run No. 0 7 3 103A-1001 073103A-1002 073103A-1003 073103A -1004 073103A -1005 . XC072503-5 XC072503-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 SpkB L349I0-1 SpkC L34910-6 Spk D L34910-12 Spk E L34910-16 SpkF XC072503-1 L34910-1 L349I0-1 Rep L34910-4 L34910-2 L34910-3 XC072503-2 L34910-6 L34910-6 Rep L34910-9 L34910-7 L3491Q-8 XC072503-3 L34910-12 L34910-12 Rep L34910-15 L349I0-I3 L34910-14 XC072503-4 L34910-I6 L34910-16 Rep L34910-19 BC2SW-04 BC2 SW-05 BC2 SW-06 Outfall 10 River SW-25 BC2SW-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 Outfall to River SW-25 Outfall to River SW-25 Outfall to River SW-25 Dup CS 073103A -1006 CS 073103A-1007 c 073103A -1008 c 073103A -1009 LCS 073103A-101 LCS 073103A-111 LF 073103A-I012 LF 073103A-1013 LF 073103A-1014 LF 073103A-1Q15 CS 073103A-1016 s 073I03A-117 S 073I03A-1018 s 073103A-1019 FF 073103A-I020 FF 073103A-1021 es 073103A-1022 S 073103A-1023 s 073103A-1024 s 073103A-1025 FF 073103A-1026 FF 073103A-1027 CS 073103A-1028 s 073103 A-1029 s 073103A-103Q s 073103A-103I FF 073103A-1032 FF 073103A-1033 CS 073103A-1034 s 073103A-1035 S 073103A-1036 s 073103A-1037 L34910-17 L34910-18 XC072503-5 U 49I0-25 L34910-26 U 4 9 10-22 L34910-23 L 3 4 9 10-24 X C 0 7 1003-6 Outfall to River SW-25 Low Spk FF 073103A -1038 Outfall to River SW-25 High Spk FF 073103A-1039 - CS 073103A-I040 Equipment Blank-Pump s 073103A-1041 Equipment Blank-Dredge Field Control/Travel Blank s 073103A-1042 s 073103A-1043 Field Control/Travel Blank Low Spk FF 073103A-1044 Field Control/Travel Blank High Spk FF 073103A-1045 - CS 073103A-1046 Analyte Found (ppt) (peak area * intercept) / slope x DF Recovery (%) * fanalyte found (ppt)-analyte found in control (ppt)l x 100 amount added (ppt) Std. Conc. (ppt) 0 25 50 100 250 500 1000 25 - - 50 - 100 - 250 - 500 1000 Dilution Factor 10 10 10 10 100 100 100 100 100 - Peak Area 0 3440 6725 13321 31340 65687 127765 0 0 6872 62898 74954 65330 96556 107094 3545 148109 143575 106161 90364 9716 6634 19717 20175 52363 67031 5639 13989 269867 2634 II 276134 284082 11410 33866 358032 358872 369645 311246 12191 72430 0 814 0 12140 16047 139302 Analyte Found Amount Added Recovery (p p o (ppo <%> . . . . ND 50.6 468 5580 4860 7180 7970 . * 50 500 5000 5000 5000 5000 - - - -fOe>O 101 94 94 95A 94A . - 790 672 7180 146 150 389 498 4140 * * * 8440 * 9020 - 100 10000 - - - - 100 10000 . 100 10000 . . 100 10000 - -718*+ 58* - - 352 40 - 60* 58A ND ND ND 89.8 11900 . 100 10000 90 119 - - Standard Curve : Linear (1/x weighted) Intercept 78.1882 Slope * 134.313 Coef. O f D el - 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:. a 'Sample was corrected using the data found in set 073103AR *Sample requires futher dilution. See data set 073103AR. +Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. Exysen % / t / R E S E A RR C H 3058 Research Drive State Colleg_e, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number: Exygen Sample # -fc 3 * m trr -L34940-a- L34910= Hb3491Q-4 -i,3 49t 0-5 4 .3 4916-6" fc349 O-T 4 4 4910-8L34910-9U 4 9 1 0 -tftU 4910 4 *- L 3 19*8-45 L 3 4 9 104-3 NA_________ Exygen Study Number:________L34910_______ Sponsor Sample # BC2 SW-04 BC2 SW-04 Low Spk BC2 SW-04 High Spie BC2 SW-04 Dup BC2 SED-04 BC2 SW-05 BC2 SW-05 Low Spk BC2 SW-05 High Spk BC2 SW-05 Dup BC2SED-05 BC2SED-06 BC2 SW-06 BC2 SW-06 Low Spk Exygen Sample # E34940 14' L3 4943 4 5 -L 34Q40 4-7L 349 10 L349 0 19 - 444916=20- J-34910.7.1. L-349 0 -2 5 434910-2 3U4910-34- 44W L25. 1=34910-24 - Sponsor Sample # BC2SW -06 High Spk BC2 SW-06 Dup Outfall to River SW-25 Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk Outfall to River SW-25 tXip 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 Karen Risha 7/31/03 0800_______ Requested By (Printed Name/Date/Time) Samples removed from: -- Box# Box# ---- Shelf# Shelf# -- Samples transferred to the custody of Sample Custodian Initials/Date/Time Samples received from custodian; Samples moved to REF 3 7 - fcfl7l3l63 CfoO Laboratory Personnel Initials/Date/Time Samdes removed from P ~ b ^ Samples returned to CJ6 0 0 3 o / Comments: A ll S W k i l u l x/tfos M i t i Sample Custodian Initials/Date/Time December 19, 2002/6 E\yge 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: L349I0 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No, i L . , Time rfllf) ____________________________ Date 5 . _ Initials CEE- 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 EDNUMBER 0106020 Control 0106020 Spk A 0106020 Spk B L34910-1 SpkC 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 L34910-6Rep 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 SpkE L 3 4 9 t0 -1 6 S p k F - Spiking Solution Used F 0 6 1 103-2 (10 ng/raL) F 0 6 1103-1 (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) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - Initial/Date P r- /ifal r /b7N V t ftn h i 9 W L /Tfai H /0 7 )i 0 S ' itili U- All samples were measured: Time 0 Z O _______ Date (7 1i1js3i1/ o0.3 After measuring samples were returned to refrigerator No. 32- Time HOP_________ Date D l j ^ O ^ Initials Initials C h - Comments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. lnitials/Date: l Analysis Summary: Data Set:. (573>!tibh Data Set: _ i Data Set: lnitials/Date: lnitials/Date: Inidals/Date: Set extraction/analysis data verified by:, O July 26, 2001/6 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 M ATRIX: Water METHOD: " A N A LY TES: PFHS. PFOS. PFO A and PFOSA PROTOCOL NUMBER: MA Client ID na na na BC2 SW -04 BC2 SW -05 Exygen ID 0106020 Control 0106020 Spk A 0106020 Spk B L34910-1 Spk C L34910-6 Spk D STEP 1 STEP 2 D ilu tion s (m L/m L) - -Y t ,o V i.o STEP 3 DDutions (m L /m L ) _ - - (D M .o - STEP 4 Y" J/ R eagen ts/ M aterials Methanol C18 SPE Type I Water _ . L ot# 43IK ?JP > W a i B 3 NA BC2 SW -06 L34910-12 Spk E '0 -V l.O Outfall to River SW -25 BC2 SW -04 BC2 SW -04 L34910-16 Spk F L34910-1 L34910-1 Rep 'V i .O ( 0 o ,V i. * '/t.o o ,v /( .0 ,, ._ BC2 SW -04 Dup BC2 SW -04 Low Spk L 34910-4 L34910-2 In itia ls/D a te CEE cnl*tlr>*s . --- o -'/t.D \ t -------- _ BC2 SW -04 High Spk L34910-3 o y .o --- . BC2 SW -05 BC2 SW -05 BC2 SW -05 Dup BC2 SW -05 Low Spk BC2 SW -05 High Spk L34910-6 L 34910-6 Rep L34910-9 L34910-7 L34910-8 -- -- - o,,/ l 0 -V u o -'/i.t> -- \/ . _ _ _ _ BC2 SW -06 L34910-12 HPLC BC2 SW -06 BC2 SW -06 Dup L34910-12 Rep L 34910-15 - C Methanol Ammonium Acetate 4 3 0 8 7 ? > lU BC2 SW -06 L ow Spk BC2 SW -06 High Spk L 3 4910-13 L34910-14 --/ 1r Type I water \1f >1< o . t / , 0 4 -- *s NA * - -- - L /E ? Q pT i / *lnitials/Date - fa it o j/si 0 2 - <g@ > o fc fo fe W * fc' W t / V U IU U U I ^ U U U H l U I V tV *T U M 1J STEP 2: Final volum e to 5 m L collected in 15 mL polypropolene tubes STEP 3: LC/M S/M S analysis STEP 4: LC/M S/M S reanalysis. Initials and date under each step indicates the personnel that perform ed this step. I F P 4 A , TpJttxiSbj t>vumsSAM i.fiuAbF=icD. fSAM?tU^S PRSHlM blUlTb lOOH ( *ViD - ____k no VrTA set .. 3 . $$ M ethod o f A nalysis for the Determination o f Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylam ide (PFOSA), and Perfluorooctanoate (PO A A ) in Water )6 tA /o i foS COMMENTS: Final extracts stored in refrigerator/ ' ^ - Initials: / E L Date: f t l j s i l lo^> U July 19, 2001/4 EWg; e 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. ? 2 - . . Time M l D ______ Date n 'ljk>l\C S?> Initials Ce - CLIENT SAMPLE 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 Field Control/Travel Blank Low Spk Field Control/Travel Blank High Spk Equipment Blank-Pump Equipment Blank-Dredge EXYGEN ID NUMBER L34910-16 L34910-16 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 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: " A N A LY TES: PFH S. PFO S. PFOA and PROSA PROTOCOL NUMBER: N A Client ID Outfall to R iver SW -25 Outfall to R iver SW -25 Outfall to R iver SW -25 D un Outfall to River SW-25 Low Spk Outfall to River SW-25 High Spk Field Control/Travel Blank Field Control/Travel Blank Low Spk R eid Control/Travel Blank High Spk Equipment Blank-Pump Equipment Blank-D redge - *lnitiaU/Date E xygen ID L34910-16 L 349l0-16R ep L 3 4 9 1 0 -1 9 L 3 4910-17 L 34910-18 L 34910-22 L 3 4 910-23 L 3 4910-24 L 3 4 910-25 L 34910-26 - - - - STEP 1 STEP 2 _______ 1____ D ilu tio n s (m L/m L) -- o'/tO STEP 3 NY - - CE N _ . - - C&f \ -'/to . . - _ _ . - ~1 _ _ _ _ . _ _ _ . o y v lo s D ilu tion s (m L/m L) tD to (0 -- -- -- -- _ _ _ _ . _ . _ r /` oB & hb STEP 4 V/ - "V _ _ _ _ _ _ _ _ J" R eagen ts/ M aterials Methanol C l 8 SPE Type I Water L ot# te lic i a VJ NA . . . Initia ls/D a te _ cn im irfe . __ . HPL c Methanol H 5 0 8 7 3 /-( Ammonium Acetate Type I water . NA _ In itia ls/D a te STEP 2: Final volum e to 5 mL collected in 15 m L polypropolene tubes STEP 3: LC/M S/M S analysis STEP 4: LC/M S/M S reanalysis. 10DA ( J/\o ^ 0 0 |6 3 li> 3 Initials and date under each step indicates the personnel that performed this step. $$ Method o f A nalysis for the Determination o f Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylam ide (PFO SA), and Perfluorooctanoate (P O A A ) in W ater CO M M ENTS: Final extracts stored in refrigerator 3~ 2- Initials: Date: July 19, 2001/4 ^*4 M asslynx - Sam ple List Sample List: C:\MASSLYNX\Fluorochemicals.PRO\SampleDB\073103A Decatur BC.SPL l^jepik___________Printed: Fri Aug 01 08:36:23 2003 Vial File Name LIMS ID Client ID Sample Description M 1 41 073103A-1001 -- 2 42 073103A-1002 -- 3 43 073103A-1003 -- 4 44 073103A-1Q04 -- S 45 073103A-1005 -- 6 46 073103A-1006 -- 7 47 073103A-1007 -- 8 92 073103A-1008 -- 9 51 073103A-1009 -- 10 52 073103A-1010 -- 11 53 073103A-1011 -- 12 54 073103A-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 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC072503-0, 0 ng/L Standard XC072503-1, 25 ng/L Standard XC072503-2, 50 ng/L Standard XCQ72503-3,100 ng/L Standard XC072503-4, 250 ng/L Standard XC072503-5, 500 ng/L Standard XC072503-6, 1000 ng/L Standard Methanol Wash 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 XC072503-1, 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 f^kyiBOn STUDY N O . V Page 1 Page Position: (1,1) atrix 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 too 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 -w- -- 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 I ______ __________ ____ 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 C8 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 C8 ACID PFOSA 10 C6 C8 SULF C8 ACID PFOSA 11 C6 C8 SULF C8 ACID PFOSA 12 C 6C 6 SULF C8 ACID PFOSA 13 C6 CB SULF C8 ACID PFOSA 14 C6 C8 SULF C8 ACID PFOSA 15 C6 CB 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 C B SULF C8 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 C8 SULF C8 ACID PFOSA 31 C6 C B SULF C B ACID PFOSA 32 C6 CB SULF CB ACID PFOSA 33 C6 C8 SULF C8 ACID PFOSA 34 C6 CB SULF C8 ACID PFOSA 35 C6 CB SULF C8 ACID PFOSA 36 C6 CB SULF CB ACID PFOSA 37 C6 CB SULF C8 ACID PFOSA 38 C6 C8 SULF C8 ACID PFOSA 39 C6 C8 SULF C8 ACID PFOSA 40 C6 C8 SULF C8 ACID PFOSA 41 C6 C8 SULF C8 ACID PFOSA 42 C6 C B SULF CB ACID PFOSA 43 C6 CB SULF CB ACID PFOSA 44 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 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 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 . lM lo Page 2 Page Position: (2. 1) Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroc:hhqammiiccaallss.PRO\SampleDB\073103A Decatur BC.SPL Printed: Fri Aug 01 08:36:23 2003 J p 8|?i53_____________ jExygen study n o . LbWUv. 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 XC072503-6. 1000 ng/L Standard Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF -- QC -- Standard 10000 1000 0 100 01 Masslynx - Sample List Sample List: C:\MASSLYNX\Ruorochernicaallss..PPRO\SamplleDB\073103A Decatur BC.SPL Printed: Fri Aug 01 0B:36:23 2003 Btygen study n o . t a J W MS Method HPLC Method MS Tune File Inj.Volume 45 C6 C 8SULF C8 A C ID P F O S A pfbs water 46 C6 C8SULF C8 ACID PFOSA pfbs water Fluorochems 15 Fluorochems 15 K Page 4 ' Page Position: (2.2) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exveen Study No: L34910 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: 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 computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. A ll Handwritten Peak ID 's by: ,c>3 S c a n n in g M ethod R e p o rt 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 0! 0 5 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 M ethod R e p o rt Method File: Last Modified: Printed: c :\masslynx\fluorochemicals >pro\acqudb\pbs water Friday, August 01, 2003 08:27:00 Friday, August 01, 2003 08:36:39 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 90.0 100.0 100.0 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 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 (/il) Vial Number 200.0 200 0.50 20.00 15.0 69 T u n in g M ethod R e p o rt 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 lEnergy 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 12 14 16 -648 Rdbk 131.4 754.2 Q u a n tify C a lib ra tio n R ep o rt \m * S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i a h a Page 1 Calibration: Last modified: Printed: P :\D ata\L G M S M S 6 \K assly n x \F lu o ro cb em icals.P R O \C u rv eD B \0 7 3 1 0 3 A Sun Aug 03 0 7 :1 2 :4 6 2003 Sun Aug 03 0 7 :1 9 :2 6 2003 D ecatu r ti BC E x y g en R e s e a r c h , 3 058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tify C a lib ra tio n R eport S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.S a t e :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 2 C a l i b r a t i o n : P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ 7 1 u o r o c h e m i c a l s .P R O \C u r v e D B \0 7 3 1 0 3 A D e c a t u r BC L a s t m o d ifie d : Sun Aug 03 0 7 :1 2 :4 6 2003 P rin te d : Sun Aug 03 0 7 :1 9 :2 6 2003 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R ep o rt V w / S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 3 C a l i b r a t i o n : P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ F l u o r o c h e m i c a l s .P R 0 \ C u r v e D B \ 0 7 3 1 0 3 A D e c a t u r BC L a s t m o d ifie d : Sun Aug 03 0 7 :1 2 :4 6 2003 P rin te d : Sun Aug 03 0 7 :1 9 :2 6 2003 E scygan R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R ep o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 4 C a l i b r a t i o n : P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ F l u o r o c h e i o i c a l s . P R O \ C u r v e D B \ 0 7 3 1 0 3 A D e c a t u r BC L a s t m o d ifie d : Sun Aug 03 0 7 :1 2 :4 6 2003 P rin te d : Sun Aug 03 0 7 :1 9 :2 6 2003 Z x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 168 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 1 Sample List: P:\Data\LGMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochaniicals.PR0\MethDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 tJob Code: Initiais Date Printed: Sun Aug 03 07:19:29 2003 Run# 073JC&A- ioo[ m uM Name: 073103A-1001 Text: 1: C8 Acid (PFOA) W 2: C6 Sulfonate (PFHS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o. : 073103A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly st.-K .R ish a Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Flubrochemicals.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 E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tify S am ple R e p o rt \m f S t u d y N .-.L 3 4 9 1 0 , S e t N o . :0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : X . R i s h a 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\LGMSMS6\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-1002 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) B x y g en R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, AnalystsK.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRQ\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 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 5 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.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-1003 Text: 1: C8 Acid (PFOA) 'S t* 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t :lC .R ish a Page 6 Sample List: P:\Data\LCMSMS6\Kasslynx\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-1003 Text: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt Vm > S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Decatur SC 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: 1: C8 Acid (PF0A) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 8 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-1004 Text: 4: PFOSA XC072503-3,100 ng/L Standard, 0 7 3 103A -1004 Sm (M n, 2x3) 100i %- 01-Aug-2003 10:29:31 LC/MS/MS #6 M R M of 4 Channels ES- 9.89 13321 498 > 78 7.20e4 Area 0 IIrI I I ~ n Time 2.00 4 .0 0 6.00 8.00 10.00 12.00 E x y g en R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 801 Quantify Sample Report Study No.:L34910, Set No.: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: Sim 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-1005 Text: 1: C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 073103A -1005 Sm (Mn, 2x3) ' 1OOn %- 9.15 66169~| 1 01-Aug-2003 10:51:16 LC/MS/MS #6 M R M of 4 Channels ES413 >369 4.06e5 Area 1 : : : - 1 Tim e-- '' ' T ^ 1 1 1 T " 1 ' 1 1 r - T - i - r - i I - T - I - I 1 1-- r --1--i -- | - i - i ' " I 1 1 i - T - i -- r - r - r - ^ P T I 1 1--1 "1 1 i i 1 2.00 4 .0 0 6.00 8 .0 0 10.00 12.00 W 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103A -1005 Sm (Mn, 2x3) 10Ch %: 8.99 01-Aug-2003 10:51:16 LC/MS/MS #6 M RM of 4 Channels ES399 > 80 8 .1 0e4 Area 0 1 1 i i 1-1 i ' i 1 1 1 ' i ' ' 2.00 4 .0 0 3: C8 Sulfonate (PFOS) t "' 1 i~ r~ r 6.00 8.00 I I ' I ' ' I 1 1 1 1 I Tim e 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report < W Study No.:L34910, Set No.s073103A, 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\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-1005 Text: 4: PFOSA XC072503-4, 250 ng/L Standard 073103A -1005 Sm (Mn, 2x3) 10Ch %: 01-Aug-2003 10:51:16 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 1.69e5 Area 0 I ~ l ' I I | I . I T 'l I I I I " I - I I I ! 2.00 4.00 6.00 8.00 10.00 n Tim e 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report VeS Study No.:L34910, Set No.:073103A, Ext.Data:07/31/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SanpleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Secatur 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) 100n %- 9.13 142891 01-Aug-2003 11:12:56 LC/MS/MS #6 M R M of 4 Channels ES413 >369 8.51e5 Area -n ~ r- 2.00 'tar 2: C6 Sulfonate (PFHS) 4.00 6L00 Ir 8.00 t-i--T 1 I r- i r I 'I j Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h / 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 12 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\Hasslynx\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-1006 Text: 4: PFOSA w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R ia h a P age 13 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\HethDB\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) XC072503-6,1000 ng/L Standard 073103A -1007 Sm (M n, 2x3) 100n %- 01-Aug-2003 11:34:42 LC/MS/MS #6 M R M of 4 Channels ES413 >369 1.57e6 Area O ' .................... i "i- i i - ' i iii 2 .0 0 2: C6 Sulfonate (PFHS) 1i 1 4.00 6^00 '- r ............. i *1 'i * i Tim e 10.00 12.00 3: C8 Sulfonate (PFQS) E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s ts K .R is h a P age 14 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-1007 Text: 4: PFOSA w Z x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .: 1.34910, S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 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.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-1008 Text: W * 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SamgpleDB\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 : E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , 2 x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R ish a P age 17 Sample List: P:\Data\LCHSMS6\Masslynx\Fluorochexoicals.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-1009 Text: W * 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t .D a te : 0 7 /3 1 /0 3 , A n a ly s t :K .R is h a Page 18 Semple List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCHSMS6\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-1009 Text: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t H o .: 073103A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R ia h a Page 19 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-1010 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt HmS S t u d y N o . : B 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t . - K .R i s h a 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\DCMSHS6\Masslynx\Fluorochemicals.PR0\MetliDB\Decatur BC 080103 Bast modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1010 Text : 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt W ? S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t .D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 21 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\Dacatur 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) 0106020 Spk B, 500 ng/L 0731Q3A-1011 Sm (M n, 2x3) 10Ch %: 01-Aug-2003 13:01:43 LC/MS/MS #6 . M R M of 4 Channels ES- 9.15 413 >369 1329091 7.82e5 1 Area 1 (y 1 i . . . I r - T , . , . i-- i--| i - 1 i i' t --t --t ~|'*' r~ i * i i , 1 ' ' ! t " ' t ' i T - i T-i i - . .I | Tim e ___________________ ZOO____________ 4110____________ 6JD0____________8J30___________ 1 0 .0 0 ___________12.00 Ve/ 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) 0106020 Spk B, 500 ng/L 073103A-1011 Sm (Mn, 2x3) 10O ] %: 0 11 1 1 1 1 1 ' ',T " i -i ' 1 ' T ' ' r 2 .0 0 4 .0 0 1I 1111I 6.00 01-Aug-2003 13:01:43 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 8.83e4 Area *1t0.i0'0 i ' ' i1'2.i0T0ime E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\FluorochemicalS.PRQ\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslycx\Fluorochemicals.PRO\HetbDB\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: 4: PFOSA E x y g en R e s e a r c h 3058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 168 0 1 Q u a n tify S am ple R e p o rt \m 0 S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K .R i s h a S age 23 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\Hasslynx\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-1012 Text: 1: C8 Acid (PFOA) 2 : C6 Sulfonate (PFHSi L34910-1 Spk C, 5000 ng/L, DF=10 073103A-1012 Sm (Mn, 2x3) 10CH %- 8.98 30859"] I1 01-Aug-2003 13:23:31 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.84e5 Area 0- 1 i i ' i " 1r 1i"1-'... i 1..... i - t - r - r - f -i--r r - r - r . . ...... i 1 i i i i i i i i Time 2.00________ 4,00________ 6J)0________ 8^0________ 10,00 12.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N O .: 1.34910, S e t N o .: 073103A , E x t.D a te : 0 7 /3 1 / 0 3 , A n a ly s ts K .R is h a 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\LCMSMS6\Masslynx\Fluorochemicals.FRO\MethDB\Decatur BC 080103 Last modified: Sim Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1012 Text: 4: PFOSA L34910-1 Spk C, 5000 ng/L, DF=10 073103A-1012 Sm (Mn. 2x3) 100] %: 01-Aug-2003 13:23:31 LC/MS/MS #6 MRM of 4 Channels ES- 9-92 498 > 78 749541 4.01 e5 Area 0 - -- I-----1-----1---- 1---- [---- 1---- 1---- f----1---- j---- 1---- 1-----1---- 1---- [---- 1---- 1---- 1-----1-----j-----1---- 1---- 1---- !---- J---- 1---- 1-- 1---- 1 I I 2.00 4.00 6.00 Time 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 25 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\Masslyxnc\Fluorocheinicals.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) mrv-, %- 9.13 1458721 I 01-Aug-2003 13:45:17 LC/MS/MS #6 MRM of 4 Channels ES413 >369 8.79e5 Area 1 y ' n i l r^ j- i" -i r " i-- >--r r--r r -i" r t 1r~r~ r "i | r I ' l T ' f T 1 i i i { i i ii"*n " p i T T ~ r - ^ ^ P *r ' 1 i r 1 1 1 i 1 1 1 1 i Time ____________ zoo_______ 4 og_______ aoo_______ zoo_______ 10.00______ 12.00 W 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , FA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:073103A, 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 L34910-6 Spk D, 5000 ng/L, DF=10 073103A -1013 Sm (Mn, 2x3) 100i %- 01-Aug-2003 13:45:17 LC/MS/MS #6 M R M of 4 Channels ES- 9.88 6533C 498 > 78 3.48e5 Area O ' i 1-1 r , '~'r 2.00 4 .00 6.00 10.00 - n Time 12.00 W E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 168 0 1 Q u a n tify Sam ple R e p o rt 'Umt S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a Page 27 Sample List: P:\Data\LCMSMS6\Masslynx\7luorocheioicals.PRO\SasipleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\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-1014 Text: 1: C8 Acid (PFOA) L34910-12 Spk E, 5000 ng/L, DF=10 073103A-1014 Sm (Mn, 2x3) 100-] %- 9.14 4186511 01-Aug-2003 14:07:06 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.49e6 Area ___0-___' ___l___ zoio1_"_1__i_11_1_' f1koi o_1_'_1_i_1_1_1aoo_______1; "i-- r " i y i t"i f j ri- *'-~i i 1 1 * t 1 aoo_______ io.oo______ 1 * i Time 12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 28 Sample List: P:\Data\LCMSMS6\Masslymc\Fluorochemicals.PRO\SampleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicala.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-1014 Text: 4 : PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt V e / S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:X .R is h a 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\Masslyox\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: 1: C8 Acid (PFOA) L34910-16 Spk F, 5000 ng/L, DF=10 073103A -1015 Sm (Mn, 2x3) 100i . 0/o: 0-^--'--1--I--I i" 1--'--1--1--1--1--1--1--1--1--1--1--1--1--1--1--1--1--1--I--1--1--1--1--I--1--r 2.00 4.00 6.00 2: C6 Sulfonate (PFHS) 01-Aug-200314:28:57 LC/MS/MS #6 9.13 M R M of 4 Channels ES413 >369 2.96e6 Area n 8.00 \ < 1 1 I ' ' ' > I Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-16 Spk F, 5000 ng/L, DF=10 073103A -1015 Sm (Mn, 2x3) 1 0 0 -] %: 0~ I I I I I I ' I" I |-l I I I I I I I I I ' I" I l - f I I T ' ! |-T- 2 .0 0 4.00 6.00 01 Aug-2003 14:28:57 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 6.80e5 Area I I ' ' ' I 10.00 -n Tim e 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt Mmtf S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a Page 30 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-1015 Text: 4 : PFOSA L34910-16 Spk F, 5000 ng/L, DF=10 073103A-1015 Sm (Mn, 2x3) 100i %- 01-Aug-2003 14:28:57 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 107094 5.50e5 Area a 't a * 6.00 10.002.00 - i -| -i -r - r- i i i . i - i r 1 4.00 8.00 T Time 12.00 w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam pla R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 31 Sample List: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\SangpleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\71uorochemicals.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) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o. :L 34910, S e t N o .: 073103A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Pagre 32 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 Nane: 073103A-1016 Text : 4: PFOSA %m0 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt 1 ^ / S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 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.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-1017 Text: 1: C8 Acid (PFOA) L34910-1 073103A -1017 Sm (Mn, 2x3) 100i %- 01-Aug-2003 15:12:28 LC/MS/MS #6 M R M of 4 Channels ES413 >369 5.12e6 Area a 2.00 W 2: C6 Sulfonate (PFHS) L34910-1 073103A -1017 Sm (Mn, 2x3) 100i %- 4.00 -T--r-T- 6.00 t t --I . - I . -r I r I , - . I Tim e 10.00 12.00 01-Aug-2003 15:12:28 LC/MS/MS #6 8.99 M R M of 4 Channels ES399 > 80 3.04e5 Area 0 ' ' I ' 1 I I 1 I 1 I--J'-I--I r--r |-t- I T-i |--r 2.00 4 .0 0 6.00 8.00 n ' ' I ........ -t- i Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-1 073103A -1017 Sm (Mn, 2x3) 10CH %: 9.25 2801831 1 01-Aug-2003 15:12:28 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 1.61e6 Area 1 0 - I t - . I . 1 I 1 1 ' ' 1 1 1 1 1 1V I 1 ' ' 1 ^ r-i I I I 1--r 1--I- ' -r- ' i--1 T im e 2.00 4.00 6 .0 0 _________ 8 .0 0 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 168 0 1 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 34 Sample List: P:\Data\LCMSMS6\Masslyiuc\Fluorochamieals.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 Marne: 073103A-1017 Text: 4: PFOSA L34910-1 073103A -1017 Sm (Mn, 2x3) 100n %- 01-Aug-2003 15:12:28 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 7 8 1481091 7.51 e5 Area T im e 2.00 4 .0 0 6.00 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 35 Sample List: P:\Data\LCMSMS6\Masslymc\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-1018 Text: 1: C8 Acid (PFOA) L34910-1 Rep 073103A -1018 Sm (Mn, 2x3) 1 0 0 -, % 9.13 826648 01-Aug-2003 15:34:18 LC/MS/MS #6 M R M of 4 Channels ES413 >369 4.94e6 Area O -L t- i i T T ` i r--i--i i' i i i i i i i 1 i ' 1 1 1 i 1 2.00 4.00 'i1 6.00 8.00 10.00 ' i i Time 12.00 3: C8 Sulfonate (PFOS) L34910-1 Rep 073103A -1018 Sm (M n, 2x3) 100] %- 9.26 2741701 1 01-Aug-2003 15:34:18 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 "1.56 e 6 Area 0 : 1 1 1 1 i 1 1 ' 1 i 1 1 1 1 , ' ' 1 >- r 1 1 1 1 T 1 1- ! ,-r . i- ! ! i -r-T T , i i i i ' 2.00 4.00 6.00 8.00 10.00 i i i i ' ' ' 1'2i.0T0im e E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 36 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-1018 Text: 4 : PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 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-1019 Text: 1: C8 Acid (PFOA) L34910-4 073103A-1019 Sm (Mn, 2x3) mrv-, %- 9.14 575640*1 I 01-Aug-2003 15:56:09 LC/MS/MS #6 MRM of 4 Channels ES413 >369 3.34e6 Area 1 0- T ' r'1 i ' 1 r * |-i i i `I r i 'I' ' r ' 1'"111 1 I"1'1 1' T-T-r-^^T-r i i . . . .-i i T-1i-. Time ___________________ 2 ,0 0 ____________ 4/D0____________ 6 ^ 0 ____________8 ^ 0 ___________ 10.0 0 ___________12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 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 -,0 7 3 1 0 3 A -1 0 1 9 S m (M n, 2x3) 100 %: 01-Aug-2003 15:56:09 LC/MS/MS #6 9.91 M RM of Channels ES498 > 78 5.46e5 Area O - U - l - i i i ", I" i i - I - I r r < I - i i" * ' I ' r i v | - i 2 .0 0 4.00 6.00 W 8.00 10.00 i 1 * * 1 i Time 12.00 Z x y g en R e s e a r c h , 3 058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt ^ S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R ia h a P age 39 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-1020 Text: 1: C8 Acid (PFOA) L34910-2 073103A -1020 Sm (Mn, 2x3) 10Q -] %: 01-Aug-2003 16:17:55 LC/MS/MS #6 9.13 M R M of 4 Channels ES413 >369 3.49e6 Area ' O - W ' ! - ! r-1 r-T I-- r -i T I I- , - r - T T - r T ~l -. T | T - T T - I- - r - 1- 2 .0 0 4.00 6.00 2: C6 Sulfonate (PFHS) 8.00 - , - r T--, v * i 1 I r I Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) L349 10-2 0 7 3 1(33A -1020 S m (M n, 2x3) 100 %- VJ-J 2.00 9.27 1916311 01-Aug-2003 16:17:55 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 1.08e6 Area L ............. 1 1 1 i 1 1n 11 ' 11 1" 1 i" 1' r - r ' l_i 1 ' r 1 1 1 1 i ^ 4.00 6.00 8.00 10.00 12.00 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 8 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 40 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochsmicals.PR0\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) 100i %- 01-Aug-2003 16:17:55 LC/MS/MS #6 M R M of 4 Channels ES- 9.92 9036' 498 > 78 4.67e5 Area 12.004 .0 0 aoo I 11 11 I 8.00 r 10.00 T im e E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 41 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.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: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 42 Sample List: P:\Data\LCMSMS6\Hasslynx\71uorochemicals.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: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a 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.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: 1: C8 Acid (PFOA) W 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set NO.:073103A, 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.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-1022 Text: 4: PFOSA %0 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt \ tm/ S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a Page 45 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) 10Ch %- 9.14 173871 01-Aug-2003 17:23:17 LC/MS/MS #6 M R M of 4 Channels ES413 >369 1.01 e6 Area 0 ' I ~ i ' - , I ' 1 I I ' 1 1 I I 1 ' I I 1 1 1 < I " 2.00 4 .0 0 6.00 2: C6 Sulfonate (PFHS) ' r 8.00 [ I r I I I I I I I I Time 10.00 12.00 E x y g en R e s e a r c h , 3 058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Paga 46 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\HethDB\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 07 3 1 03A -1023 Sm (Mn, 2x3) 1 0 0 -1 %: 01-Aug-2003 17:23:17 LC/MS/MS #6 M R M of 4 Channels ES- 9-88 498 > 78 19717^ 1.01e5 Area 0 ' I I ' I h [ I r *i "i" I ~r~`i I I I \ r i I " I I I I i I 2.00 4.00 6.00 8.00 10.00 Tim e 12.00 W E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R ls h a Paga 47 Sample List: P:\Data\LCMSMS6\Kasslynx\Fluorochemicals.PRO\SainpleDB\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-1024 Text: 1: C8 Acid (PFOA) L34910-6 Rep 073103A-1024 Sm (Mn, 2x3) 100n %- 01-Aug-2003 17:45:07 LC/MS/MS #6 9.13 M R M of 4 Channels ES413 >369 1.07e6 Area O l i -i , i t ...............-I . . . I 2.00 Vts* 2: C6 Sulfonate (PFHS) . I- I I 4.00 6.00 8.00 -I I- 1 I----1~----I Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-6 Rep 073103A -1024 Sm (Mn, 2x3) 100n %- 0 1 ' ' 1 1 I 1 1 I I ............- 1 ' I I ' |--r 1 r- ' p- r 2.00 4 .0 0 6.00 01 -Aug-2003 17:45:07 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 2.62e5 Area -i ii''ii..... Time 10.00 12.00 S x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y H o. :Ii3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , R x t.D a te -.0 7 /3 1 /0 3 , A n a ly s ts K .R is h a Page 48 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-1024 Text: 4: PFOSA L34910-6 Rep 073103A-1024 Sm (Mn, 2x3) 100-1 % 01-Aug-2003 17:45:07 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 2 0 1 1. 01e5 Area n <" 2.00 4 .0 0 -r-1 T - i - T- I 1 1 1 1 I 1 6.00 8.00 10.00 T im e 12.00 V E x y g en R e s e a r c h , 3 058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 / S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t :K .R is h a Paga 49 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-1025 Text: 1: C8 Acid (PFOA) L34910-9 073103A-1025 Sm (Mn, 2x3) 10Ch %- 9.13 3551901 I 01-Aug-2003 18:06:53 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.13e6 . Area 1 0: ' . . I r - . . . , 2.00 -1 - 1 1- 1 [ ...i r r n - r 4.00 6.00 1 i 11 1 i 1 1 1 1 ^ f '- '- i- i ...... . r -i r r 1t - , r l1 T im e 8.00 10.00 12.00 2: C6 Sulfonate (PFHS) L34910-9 073103A-1025 Sm (Mn, 2x3) 10CH %: 8.99 210961 I 1 01-Aug-2003 18:06:53 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1.26e5 Area o - ~r l "'1 T~T" 1 ' 1 1 1 1 t- t - i- t -i--r -1 T - I - I - T r--. 7 1 - 1 - r - r - j - r t - r - r p n - i - ' i , . . . 2.00 4.00 6.00 8.00 -i-'i-' i i i-Ti -| > i--i*T--i Time 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-9 073103A-1025 Sm {Mn. 2x3) 10Ch %: 01 -Aug-2003 18:06:53 LC/MS/MS #6 9.24 MRM of 4 Channels ES499 > 99 6.60e5 Area Q l -,--r '--,--r T i ! i i i - r ' T ' i- i 2.00 4.00 TT r 6.00 T-1-i ii--ii'i'n Time 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt \ tm/ S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a P age 50 Sample List: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.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-1025 Text: 4 : PFOSA E x y g en R e s e a r c h , 3 058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 51 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-1026 Text : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-7 073103A -1026 Sm (Mn, 2x3) 100i %: CH--'--r--i--I--]--I--I--I--I--]--I--I--I--I--I--I--I--i--r--I--r 2 .0 0 4.00 w 6.00 9.26 149088 01-Aug-2003 18:28:44 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 8.38e5 Area -I7'rr II I I I I IITime 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll a g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 52 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-1026 Text: 4: PFOSA L34910-7 073103A -1026 Sm (Mn, 2x3) 100n %: 01-Aug-2003 18:28:44 LC/MS/MS #6 M R M of 4 Channels ES- 9.92 498 > 78 3.44e5 Area 0 '-I I V I I- i I I--I |--i- i r I [ I I 1-- I |--I- I I I I "'..........I I 2.00 4.00 6.00 ' 8.00 10.00 i- '- 1 r- 1 T im e 12.00 W S x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt \m f S tu d y N o. .-L 34910, S e t N o .: 073103A , E x t .D a t e : 0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P ag e 53 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-1027 Text: 1: C8 Acid (PFOA) W * 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te : 0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 54 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SompleDB\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-1027 Text: 4: PFOSA w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o. :L 34910, S e t N o .:0 7 3 1 0 3 A , E x t .D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 55 Sample List: P:\Data\LGMSMS6\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-1028 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g en R e s e a r c h , 3 058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 168 0 1 Quantify Sample Report Study No.:L34910, Set N o . :073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 56 Sample List: P:\Data\LCHSMS6\Masslynx\Fluorochemicals.PRO\SasipleDB\073103A Decatur BC Last modified: Sun Aug 03 07:08:13 2003 Method: P:\Data\LCMSMS6\Masslyux\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-1028 Text : 4: PFOSA XC072503-3,100 ng/L Standard 073103A -1028 Sm (Mn, 2x3) 100-1 %- 01-Aug-2003 19:12:20 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 1398S 7.45e4 Area I r f 1t 4.00 6.00 r J 'l I I T f T P I 8.00 I' I T 10.00 - n Time 12.00 % H0 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt 'W ' S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 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\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-1029 Text: 1: C8 Acid (PFOA) L34910-12 073103A -1029 Sm (Mn, 2x3) 100] 9.14 24713891 1 %- 1 0 "L i i - | i r i i--i i i r T r i-"| i i 2 .0 0 ___________ 4 .0 0 i i i > 1 I 1 ' ' 1 "1 6.00 ' 1 i TM 8 .0 0 ___ 2 : C6 Sulfonate (PFHS) L34910-12 073103A -1029 Sm (Mn, 2x3) 1 0 0 -] 8.99 %: 01-Aug-2003 19:34:03 LC/MS/MS #6 M RM of 4 Channels ES413 > 3 6 9 1.47e7 Area ' i 1 1-1 ~r i" 1 1 ' '"'i Tim e 10.00 12.00 01-Aug-2003 19:34:03 LC/MS/MS #6 M RM of 4 Channels ES399 > 80 1.50e6 Area 0-1- ,- , - ,.. r - T T 2.00 -r- ! -, I -, , "I I 4.00 3: C8 Sulfonate (PFOS) 6.00 8.00 --r i i ' i r i i T im e 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt Xt^0 S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a Page 58 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\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-1029 Text: 4: PFOSA % </ E x y g en R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt / S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P ag e 59 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.FRO\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-1030 Text: 1: C8 Acid (PFOA) L34910-12 Rep 073103A -1030 Sm (Mn, 2x3) 100-1 %- 9.11 2425189 01-Aug-2003 19:55:50 LC/MS/MS #6 M R M of 4 Channels ES413 >369 1 .43e7 Area 0- 2.00 W 2: C6 Sulfonate (PFHS) L349 10-12 Rep 0731 33A-1030 Sm (Mn, 2x3) 100 11i 1 4.00 %: 6.00 8.00 8.98 10.00 12.0T0im e 01-Aug-2003 19:55:50 LC/MS/MS #6 M RM of 4 Channels ES- 399 > 80 1.45e6 Area 2.00 3: C8 Sulfonate ( P F O S ) L349 10-12 Rep 0 7 3 1(3 3A -1030 S m (M n, 2x3) 100 %- 1 l 1 | ... 4.00 , ' - * ' ' ' ' ' 1 1 1 ' 1 l 1 1 l 1 7' 1 i f r" "r 6.00 8.00 10.00 ' i i 1im 12.00 ' 01-Aug-2003 19:55:50 LC/MS/MS #6 9.24 5712111 M R M of 4 Channels ES- 499 > 99 3.17e6 Area -1 i i i -r i r-i "i `if i - i - i i i i ........ 1 '"if * ' ' i r"t--* ' I"1' 1 1"'' 1' > 1--i----'----i----1 1-- i Tim e 2.00 4.00 6.00 8.00 10.00 12.00 W E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R ia h a P ag e 60 Sample List: P:\Data\LCMSMS6\Ma8slynx\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) 100n %: 01-Aug-2003 19:55:50 LC/MS/MS #6 9.90 M RM of Channels ES498 > 78 1.32e6 Area 0 ' ' ' 1 I 1 '' 1 ' T 1 2 .0 0 ' 1"' r i ' I ' ' ' i - | f r I in^r- 4 .0 0 6.00 "'I 1 8.00 10.00 T--T-- - i Tim e 12.00 W E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt W S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 61 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-1031 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS)____________________________________________________________________ L34910-15 01-Aug-2003 20:17:38 LC/MS/MS #6 073103A -1031 Sm (Mn, 2x3) M R M of 4 Channels ES- ` "" 499 > 99 3.15e6 Area r - r -r , -f i - I" -r- n T im e 2 .0 0 4 .0 0 6.00 8.00 10.00 12.00 w E ^ y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o -:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .H is h a P age 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\Masslyxuc\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 073103A-1031 Sm (Mn, 2x3) 100n %: 01-Aug-2003 20:17:38 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 2761341 1.39e6 Area 0 J ' " i I 11 ^ --r 2 .0 0 '~ i 1 r " 1 1 'T 111 ~r " v I ' I T I I -** 4 .0 0 6.00 T im e 8.00 10.00 12.00 E x y g en R e s e a r c h , 3 058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 63 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRQ\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-1032 Text: 1: C8 Acid (PFOA) L34910-13 073103A-1032 Sm (Mn, 2x3) 100-1 %- 9.11 28498701 ft 1 01-Aug-2003 20:39:25 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.69e7 Area (> j 11i" 11 i [ r i 'i i f i " T r --t-- i i i i r [' 1> i i i i i -"i t j- 1 - . - T - ! 1- 1 r r . , , . . ^ 1i 1 * "t 1 1 i--i Time _____________ 2.00__________ 4:00__________ 630__________ 830_________ 10.00_________ 12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-13 073103A-1032 Sm (Mn, 2x3) 100-1 %- O-^-r T 2.00 4.00 -r-r-f 6.00 9.24 667186 01 -Aug-2003 20:39:25 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.69e6 Area T-T 8.00 10.00 -T-i Time 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report H*/ Study No.:L34910, Set NO. :073103A, Ext .Date: 07/31/03, Analyst sK.Risha Page 64 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-1032 Text: 4: PFOSA L34910-13 073103A-1032 Sm (Mn, 2x3) 100n %: 01-Aug-2003 20:39:25 LC/MS/MS #6 9.90 M R M of Channels ES498 > 78 1.42e6 Area 0 -1 1- I 1 I I I I I . l - f I" I- I 2.00 I I I I T I I I I I -| I 4 .0 0 6.00 T 1" 8.00 10.00 -T-i Tim e 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P ag e 65 Sample List: P:\Data\LCMSMS6\Masslynx\7luorochemicals.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-1033 Text: 1: C8 Acid (PFOA) L34910-14, DF=100 073 1 03A -1033 Sm (Mn, 2x3) 10Ch %- 9.12 712941 I 1 01-Aug-2003 21:00:58 LC/MS/MS #6 M R M of 4 Channels ES413 >369 4.14e5 Area CH^-T"1 1 1-]--T"-I-1. |"l 'T-T'l |- r 1 |-| ! )--1111I T--T 1 i 1 1 1 i 1 1 1 i TM -->--i--i--i--r-i--r-r-i--i--i--| Tim e ___________________ 2 .0 0 4 .0 0 ____________ 6XJ0____________ 8J30___________ 10 .0 0 ___________12.00 W 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o. :Ii3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t :* .R is h a P age 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\Fluorochemicals.PRO\MethDB\Decatur BC 080103 hast modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-1033 Text: 4: PFOSA E x y g en R e s e a rc h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Paga 67 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-1034 Text: 1: C8 Acid (PFOA) 'ta/ 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103A -1034 Sm (Mn, 2x3) 100-1 %- 0 2.00 4.00 6.00 8.98 14198 01-Aug-2003 21:22:34 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 8.49e4 Area T im e 8.00 10.00 12.00 *0 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt Hkm* S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t s K . R i s b a P age 68 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-1034 Text: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 69 Sample List: P:\Data\LQiSMS6\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-1035 Text : 1: C8 Acid (PFOA) L 3 4 9 1 0 -1 6 073103A -1035 Sm (Mn, 2x3) m n-, %- 9.11 30729781 t 1 0 1 -A u g -2 0 0 3 21:44:25 L C /M S /M S #6 M RM of 4 Channels ES- 413 >369 1.85e7 Area Ch 1 J 1 1 1 1 1 1 1 i "r"' r 1 r "' '" 1 r" ' ' 1 1 ' "I ' T 1 T 1 1 1 1 1 1 1 1 1 i 1 1 111 1 1 1 1 1 I Tim e ______________________ Z 0 0 ______________4 0 0 ______________Z 0 0 ______________Z 0 0 _____________ 1 0 .0 0 ____________ 1 2 .0 0 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 70 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-1035 Text: 4: PFOSA E x y g en R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 71 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-1036 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) L34910-16 Rep 073103A -1036 Sm (Mn, 2x3) 100i %- 0 J"> 1 r- I I I - I I I ....... I r - r 2 .0 0 , I! 4.00 ' I1 6.00 9.25 707270 01-Aug-2003 22:06:04 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 3.94e6 Area >I 1111I 8.00 1,1 I 1 I 1 n 1 1--1 I Tim e 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 72 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-1036 Text: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a 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.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-1037 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) L34910-19 073103A-1037 Sm (Mn, 2x3) -mrw, %: 01-Aug-2003 22:27:50 LC/MS/MS #6 I8.98 2764291 M RM of 4 Channels ES399 > 80 1.67e6 Area 1 o - '"I r-i'-i "1 1 r v n - i - r - i -v i T i n - i - p i . i-| I' 1 "111 1 1 { 1 1 1 ............................ . 1 1 1 . I Tim e 2.00 4 .0 0 6.00 8 .0 0 10.00 12.00 3: C8 Sulfonate (PFOS) E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 74 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-1037 Text: 4 : PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt w S tu d y N o .'.1 .3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t .D a t e : 0 7 / 3 1 / 0 3 , A n a ly s t- .K .R is h a Page 75 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-1038 Text: 1: C8 Acid (PFOA) L34910-17 073103A -1038 Sm (Mn, 2x3) 100n %- 9.12 31028231 i 1 01-Aug-2003 22:49:40 LC/MS/MS #6 M R M of 4 Channels ES413 >369 1.85e7 Area o- i * > 1 ' J 1" r " 1 1 j ir r t-- j r i-- i-- i | i i i i j i 1--11] 1-T I v i--j T 1--r-T-p-r--j--r-- 2 .0 0 ____________ 4 .0 0 6 .0 0 ____________ 8 .0 0 t r - i 1 i-u I ' ' ' 1 Time 10.00 12.00 \* 0 2: C6 Sulfonate (PFHS) L34910-17 073103A-1038 Sm (M n, 2x3) 100n %: 8.98 2786981 1 1 01-Aug-2003 22:49:40 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 1.69e6 Area T im e 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 76 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.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-1038 Text: 4: PFOSA %0 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a 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) 'e* 2: C6 Sulfonate (PFHS) L349 10-18, DF=100 0731 D3A-1039 Sm (Mn, 2x3) 100; %- 8.96 10133"! 01-Aug-2003 23:11:32 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 6.07e4 Area U" T 1 - '! 1 I 1 1 1 I I ' 1 | " 1 2 .0 0 1- 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I I 1 ' V |-- 1-- T-- I-- 4.00 6.00 8 .0 0 I I I I I 1 I I I I 1 I I I Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) L349 10-18, DF=100 0731 33A -1039 Sm (M n, 2x3) 100] %- 9.26 14072"! 01-Aug-2003 23:11:32 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 8.21e4 Area ^T>1' T 1 1 1 1 i" 1 1 ' ' ' 1 1 ....... l-T -'-T -l-l ' ...... . 1 ' ' ' I 1 1 | , r r 1 1 1 1 2.00 4.00 6.00 8.00 IIII 10.00 I 1 1 1 1 I I irne 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly st:K .R sh a 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) 100n %: 01-Aug-2003 23:11:32 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 6.51 e4 Area 0 ,`*~r~i 'I"1 1 ' ' I ' 1-1 1 I 1 2.00 4.00 rT'1 6.00 IIIl|i 8.00 10.00 i-r-i Time 12.00 % t0 K x y g en R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 I Q u a n tify Sam ple R e p o rt S tu d y N o. :L 3 4 9 1 0 , S e t N o. -.073103A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 79 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-1040 Text: 1: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 073103A -1040 Sm (Mn, 2x3) 10CH 9.12 156964 01-Aug-2003 23:33:24 LC/MS/MS #6 M RM of 4 Channels ES413 >369 9.33e5 Area O-L-r T^ -1 1 I 1 2.00 4.00 6.00 T im e 8.00 '1o!oo 12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 073103A-1040 Sm (M n, 2x3) 100i '"I 1 2.00 I ..... I 4.00 i 1 111 11I 6.00 9.24 19341 01-Aug-2003 23:33:24 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 1.13e5 Area "I I I I I -f-n Time 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report ^ 0 Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 80 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-1040 Text : 4: PFOSA XC072503-5, 500 ng/L Standard 073103A -1040 Sm (Mn, 2x3) 100-1 %- 01-Aug-2003 23:33:24 LC/MS/MS #6 M RM of 4 Channels ES- 9.90 498 > 78 72430 I 3.86e5 Area 'i"1" r-r-i Time 2.00 4.00 6.00 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt V S S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 81 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\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-1041 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report '*a/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Riaha Page 82 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-1041 Text: E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt ^ S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P ag e 83 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-1042 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No. :L34910, Set No. :073103*., Ext.Date:07/31/03, AnalysttK.Risha Page 84 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-1042 Text: 4: PFOSA E x y g en R e s e a r c h , 3 0 5 8 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tify S asp le R eport S tu d y N o. .-L 34910, S e t N o .:0 7 3 1 0 3 A , E x t.D a te : 0 7 /3 1 / 0 3 , A n a ly s t :K .R i s h a P ag e 85 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-1043 Text: 1: C8 Acid {PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report 1,^1? 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\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-1043 Text: E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R ish a P ag e 87 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-1044 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:1,34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 88 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\Pluorochemicals.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 M R M of 4 Channels ES- 9.89 121401 498 > 78 6.45e4 Area U" ' r 'r "' I ' l - r ' Hf--r-r-i--r-- T--T--I--T--I 1 1 1 1 1 1 1 1 ' 1 1 1 1 1 1 1 ' 1 1 111 1 1 ime 2.00 4 .0 0 6.00 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 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\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: 1: C8 Acid (PFOA) 2 : C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 90 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-1045 Text: 4: PFOSA E x y g en R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a P age 91 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-1046 Text: 1: C8 Acid (PFOA) \ m f 2: C6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 073103A -1046 Sm (Mn, 2x3) 100-j %: 0 ' ' 1 ' ' I 1 1 1 I r - r - 1 r - | - ................ I -i" i i i - [ - r 2.00 4 .0 0 6.00 3: C8 Sulfonate (PFOS) 8.98 60941 02-Aug-2003 01:43: LC/MS/MS #6 M RM of 4 Channels ES399 > 80 3.71 e5 Area 8.00 -^ i ' - i ' ' i ........ i Tim e 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt *I|U^ S t u d y N o . : L 3 4 9 1 0 , S e t N O .: 0 7 3 1 0 3 A , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a P age 92 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\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-1046 Text : 4 : PFOSA XC072503-6,1000 ng/L Standard 073103A -1046 Sm (Mn, 2x3) 100i ' %- 02-Aug-2003 01:43:42 LC/MS/MS #6 M R M of 4 Channels ES- 9.89 498 >78 1393021 7.38e5 Area 2.00 4.00 i 1 1 i '. 6.00 8.00 10.00 t - i Tim e 12.00 W E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Sponsor Study No: Exygen Study No: Analyte: Ions Mooitored: Site: NA L34910 PFOA 13 -> 369 Decatur Baker's Creek R A W DATA REPORT Limit o f Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 30 ppt 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 073103AR Katen Risha LC/MS/MS Unit # 6 07/31/03 08/03*04/03 Exygen ID XC072503-0 XC072303-1 XC0725Q3-2 XCQ72503-3 XC072503-4 XC072503-5 XC072503-6 L34910-1 SpkC L349l0-12SpkE U4910-16 SpkF XC072503-1 L34910-1 L34910- Rep L34910-4 L34910-2 XC072303-2 L349I0-6 L34910-6 Rep L34910-9 L34910-7 XC072303-3 L34910-12 L34910-12Rep L34910-15 04910-13 XC07253-4 04910-16 L34910-16 Rep 04910-19 L34910-17 XC072303-5 04910-16 L34910-16 Rep 04910-19 04910-17 XC071003-6 Sponsor . ID BC2 SW-04 BC2SW-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-05 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-06 BC2SW-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 073103AR-104 073103AR-105 073103AR-106 073103AR-107 073103AR-108 073103AR-109 Q73103AR-U0 073103AR-11I 073103AR-112 073103AR-U3 073103AR-114 073103AR-115 073103AR-116 073103AR-l 17 073103AR-118 073103AR-119 073103AR-120 073103AR-121 073103AR-122 073103AR-123 073103AR-124 073103AR-125 073103AR-126 073103AR-127 073103AR-128 073103AR-129 073103AR-130 073103AR-131 073103AR-132 073103AR-133 073103AR-134 073103AR-135 073103AR-136 Std. Cone. (ppt) 0 25 50 100 250 500 1000 25 50 100 - . 250 - - 500 - - 1000 Analyte Found (ppt) * (peak area - intercept) / slope x DF Recovery (%) s {analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) 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 794 14221 27994 54680 128556 264862 516215 50564 92540 114710 14631 216041 216268 131415 142555 29284 40498 39782 81652 112700 55667 308911 315651 297735 354730 127797 82515 83658 75424 78536 271906 380900 391789 364595 362898 477931 Analyte Found (ppt) 17800 22100 4210 4210 2540 2760 ** * 1560 2170 12100 12300 11600 13900 15800 16000 14400 15000 - ** ** * Amount Added (ppt) 5000 5000 5000 100 100 .100 -- - 100 - - - 100 Recovery (%) 114 126 * -1450+ 1579*+ 1800+ -800+ - -- - Standard Curve : Linear (1/x weighted) Intercept * 2202.17 Slope * 508.394 Coef. O f D e t a 0.996211 CS * Calibration standard LF s Lab fortified sample C - Control sample FF 3 Field fortified sample S * Sample LCS 3 Laboratory Control Spike CK Check Standard ND 3 Not detected 3 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. H ie appropriate results are reported. ^Sample was corrected using the data found in set 073103A. -^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 134910 PFHS 399 -> 80 Decatur Baker's Creek RAW DATA REPORT lim it 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 oq: 073103AR Karen Risha LOMS/MS Unit # 6 07/31/03 08/03-04/03 Exygen ID XC072503-0 XC072503-1 XCQ72503-2 XC072503-3 XC072J03-4 XC072503-5 XC072503-6 134910-t SpkC L34910-12 SpkE 134910-16 SpkF XC072503-I L34910-1 L34910-1 Rep L34910-4 L34910-2 XC072503-2 L34910-6 134910-6 Rep L349I0-9 L34910-7 XC072503-3 L34910-12 L34910-12Rep L34910-15 134910-13 XC072303-4 L34910-16 134910-16 Rep L34910-19 134910-17 XC072503-5 L34910-16 L34910-16Rep 134910-19 L349HM7 XC071003-6 Sponsor ID BC2SW-04 BC2 SW-06 Out&ll to River SW-25 BC2 SW-04 BC2SW-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-23 Outfall to River SW-25 Dup Outfall to River SW-23 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 5 S FF CS s s s FF CS s S s FF CS Run No. 073103AR-101 073103AR-102 073103AR-103 073103AR-104 073103AR-105 073103AR-106 073103AR-107 073103AR-108 073103A R -109 073103AR-110 073103A R -11! 073103AR-112 073103AR-113 073I03AR-114 073103AR-115 073103AR-116 073103R-117 073103AR-U8 073103AR-119 073103AR-120 073103AR-I21 073I03AR-122 073103AR-123 073103AR-124 073103AR-125 073103AR-126 073103AR-127 073103AR-128 073103A-129 073103AR-130 Q73103AR-131 073103AR-132 073103AR-133 073103AR-134 073103AR-135 073103AR-136 Analyte Found (ppt) a (peak area intercept) / slope x DF Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Std. Cone. (PPO 0 25 50 100 250 500 1000 25 50 too 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 426 1526 1565 3729 6025 9486 26169 27209 25364 30673 21551 6872 6261 6156 6030 45496 33004 30633 29219 28660 80818 Analyte Found (ppt) Amount Added (ppt) Recovery (%) - * 11800 12200 ** a * ** 6060 6300 5870 7110 ** ** * ** 7660 7100 6770 6640 5000 5000 5000 .- 100 100 100 100 - 100 115 91 1050+ -1020+ -- - Standard Curve Linear (1/x weighted) Intercept * 218.845 Slope a 85.6521 Coef. Of Dec *0.996560 CS Calibration standard LF a Lab fortified sample C a Control sample FF a Field fortified sample S a Sample LCS = Laboratory Control Spike CK a Check Standard ND a Not detected &Response between 0 and 25 ppt NQ a Not quantifiable a 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. 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; 073103AR Karen Risha LC/MS/MS Unit # 6 07/31/03 08/03*04/03 Exygen Sponsor Sample Run ID XC072503-0 ED Code No. CS 073103AR-101 XC072503-! XC0725O3-2 XC072303-3 XC0723O3-4 XC072503-5 XC072503-6 L34910-1 SpkC L3491Q-I2 Spk E BC2 SW-04 BC2 SW-06 CS 073103AR-102 CS 073103AR-103 CS 073103AR-104 CS 073103AR-105 CS 073103AR-106 CS 073103AR-107 LF 0731Q3AR-108 LF 0731O3AR-IO9 L34910-16 Spk F XC072303-1 L349HM L34910-1 Rep L34910-4 L34910-2 XC072503-2 L34910-6 L34910-6 Rep L34910-9 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 . LF 073103AR-110 CS 073103AR-1U s 073103AR-112 s 073103AR-113 s 073103AR-114 FF 073103AR-113 CS Q73103AR-116 s 073103AR-117 s 073103AR-118 s 073103AR-119 L34910-7 BC2 SW-05 Low Spk FF 073103AR-120 XC072303-3 L34910-12 U 4910-12 Rep L34910-15 U4910-13 XCQ72503-4 L34910-16 L349I0-16 Rep L34910-19 U4910-17 XC072503-5 L34910-16 L34910-16 Rep L34910-19 L34910-17 X C 0 7 1003-6 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 - CS s s s FF CS s s s FF CS s s s FF CS 073103AR-121 073I03AR-122 073103AR-I23 073103AR-124 073103AR-125 073103AR-126 073103AR-127 073103AR-128 073103AR-129 073103AR-130 073103AR-131 073103AR-132 073103AR-133 073103AR-134 073103AR-135 073103AR-136 Analyte Found (ppt) s (peak area intercept) / slope x DF Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)l x 100 amount added (ppt) Std. Cone. <ppt) 0 23 30 100 230 500 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 too 100 20 20 20 20 - Peak Area 0 1481 2986 3100 13283 28978 33617 9428 17124 22403 1473 61301 59888 44921 37360 2882 9224 8484 23649 29284 6004 64499 64047 64656 77839 13289 17094 17264 16861 16123 28469 81862 84263 82201 79698 53137 Analyte Amount Found Added Recovery <ppt> (pp (%> - -- - -- -- - -- - -- - -- - 17100 AA AA 5000 5000 5000 112* - -*- - 8250 * - 6890 100 -4610*+ -- - 1670 - - 1540 - - 4330 - - 5370 100 3700+ - *- * 100 - - - -- 31200 - - 31500 - - 3Q80 - - 29400 100 -1800+ -- - * - - ** -` - - 100 - - Standard Curve : Linear (1/x weighted) Intercept = 152345 Slope 54.2382 Coef. O f DeL = 0.998217 CS a Calibration standard LF a Lab fortified sample C * Control sample FF a Held fortified sample S Sample LCS a Laboratory Control Spike CK a Check Standard ND Not detected a Response between 0 and 25 ppt NQ 3 Not quantifiable Response between 25 ppt and LOQ (50 ppt) -,031Spreadsheet prepared by: <nlo3 Sample was analyzed with several diludoo foetors in order to accommodate all compounds. The appropriate results are reported. ASample was corrected using the data found in set 080603 A Sample requires hither dilution. See data set 080603A **Sarapk requires a higher spikiQg level. See data set 080603A. +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 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: 073103AR Karen Risba 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 XC072503-6 L34910-1 SpkC L34910-12 SpkE L34910-16 SpkF XC072503-1 L349I0-1 L34910-1 Rep L34910-4 L34910-2 XC072503-2 L34910-6 L34910-6 Rep L34910-9 L34910-7 XC072503-3 L34910-12 L34910-12 Rep L34910-L5 L34910-13 XC072503-4 L34910-16 L34910-16 Rep L34910-19 L34910-17 XC072503-5 L34910-16 L349I0-16 Rep L34910-19 U 49I0-17 X C 0 7 1003-6 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 BC2 SW-05 BC2SW-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-I01 073I03AR-102 073103AR-103 0 7 3 103A R -104 073103AR-105 073103AR-106 073103AR-107 073103AR-108 073103AR-109 073I03AR-110 073103AR-111 073103AR-112 073103AR-113 073103AR-114 073103R-115 073103AR-116 073103AR-117 073103AR-118 073103AR-119 073103AR-120 073103AR-121 073103AR-122 073103A R -123 073103AR-124 073103AR-125 073103AR-126 073103AR-127 073103AR-128 073103AR-129 073103 AR-130 073103AR-131 073103AR-132 073103AR-133 073103AR-134 073103AR-135 073103 AR-136 Analyte Found (ppt) = (peak area intercept) / slope x DF Recovery (%) - fanalyte found (pptVanalyte 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 to 10 20 20 20 20 100 100 100 100 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 U595 21221 24495 23261 25908 25736 49195 6718 6206 6506 5831 102292 32659 31916 32869 26767 190680 Analyte Found (ppo Amount Added (ppt) Recovery (%) ----.- - - ** +* 1390 1370 ** ** ** ** * 2430 2300 2570 2550 ** ** ** ** 3260 3180 3280 2660 - 5000 5000 5000 100 100 100 100 - 100 120 -600+ -- - Linear (1/x weighted) Intercept - 611.080 Slope = 196.925 Coef. O f D e t - 0.998392 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 quantifiable35Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by: Sample was analyzed with several dilution factors m order to accommodate aU compounds. The appropriate results are reported. ^Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated. i( Masslynx - Sample List Sample List: C:tMASSLYNX\Fluorochen licals.PRO\SampleD8\073103AR Decatur BC.SPL Printed: Sun Aug 03 08:19:25 2003 |03|03 ________________ Vial File Name LIMS ID Client ID S am p le Description Mai 1 41 073103AR-101 ___ XC072503-0, 0 ng/L Standard 2 42 073103AR-102 -- -- XC072503-1, 25 ng/L Standard 3 43 073103AR-103 -- -- XC072503-2.50 ng/L Standard 4 44 073103AR-104 -- -- XC072503-3,100 ng/L Standard 5 45 073103AR-105 -- -- XC072503-4, 250 ng/L Standard 6 46 073103AR-106 -- -- XC072503-5,500 ng/L Standard 7 47 073103AR-107 -- -- XC072503-6,1000 ng/L Standard 8 51 073103AR-108 -- -- L34910-1 Spk C, 5000 ng/L. DF=100 -- 9 52 073103AR-109 -- -- L34910-12 Spk E. 5000 ng/L. DF= 100 -- 10 53 073103AR-110 -- -- L34910-16 Spk F, 5000 ng/L, DF=100 -- 11 42 0731Q3AR-111 -- -- XC072503-1.25 ng/L Standard 12 54 073103AR-112 -- -- L34910-1, DF=10 13 55 073103AR-113 -- -- L34910-1 Rep, DF=10 14 56 073103AR-114 -- -- L34910-4. DF=10 15 57 073103AR-115 -- -- L34910-2. DF=10 -- 16 43 073103AR-116 -- -- XC072503-2, 50 ng/L Standard -- 17 58 073103AR-117 -- -- L34910-6, DF=10 -- 18 59 073103AR-118 -- L34910-6 Rep, DF=10 -- 19 60 073103AR-119 -- -- L34910-9, DF=10 -- 20 61 073103AR-120 -- -- L34910-7, DF=10 -- 21 44 073103AR-121 -- -- XC072503-3,100 ng/L Standard -- 22 62 073103AR-122 -- -- L34910-12, DF=20 -- 23 63 073103AR-123 -- -- L34910-12 Rep, DF=20 -- 24 64 073103AR-124 -- -- L3491-15, DF=20 -- 25 65 073103AR-125 -- -- L34910-13, DF=20 -- 26 45 073103AR-126 -- -- XCO72503-4, 250 ng/L Standard -- 27 66 073103AR-127 -- -- L34910-16, DF=100 -- 28 67 073103AR-128 -- -- L34910-16 Rep, DF=100 -- 29 68 073103AR-129 -- -- L34910-19, DF=100 -- 30 69 073103AR-130 -- -- L34910-17, DF=100 -- 31 46 073103AR-131 -- -- XC072503-5, 500 ng/L Standard -- 32 70 073103AR-132 -- -- L34910-16, DF=20 -- 33 71 073103AR-133 -- -- L34910-16 Rep, DF=20 -- 34 72 073103AR-134 -- -- L34910-19, DF=20 -- 35 73 073103AR-135 -- -- L34910-17. DF=20 -- 36 47 073103AR-136 -- -- XC072503-6,1000 ng/L Standard Exygen STUDY NO. L3K1D 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 -- -- -- 10 100 -- -- -- 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\Fluorochemjcals.PRO\SampleDB\073103AR Decatur BC.SPL Printed: Sun Aug 03 08:19:25 2003 E f f i ^ 0 3 k 3 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 C8 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 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 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 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 ACID PFOSA 30 C6 C8 SULF C8 ACID PFOSA 31 C6 C8 SULF C8 ACID PFOSA 32 C6 C8 SULF C8 ACID PFOSA 33 C6 C8 SULF C8 ACID PFOSA 34 C6 C8 SULF C8 ACID PFOSA 35 C6 C8 SULF C8 ACID PFOSA 36 C6 C8 SULF C8 ACID PFOSA 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 waier 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 Ftuorochems 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 Exygen STUDY NO. * K Page 2 Page Position: (2, 1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS W Sponsor Protocol No: NA Exveen Study No: L34910 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: 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 (i (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 V 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 S c a n n in g M ethod R e p o rt Page 1 Method: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 C8 SULF C8 ACID PFOSA Last Modified: Thu Jul 31 16:23:50 2003 Printed: Sun Aug 03 08:20:40 2003 03 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 M ethod R ep o rt Method File: Last Modified: w P rin te d : C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQODB\pfbs water Sunday, August 03, 2003 08:06:07 Sunday, A ugust 03, 2003 0 8 :2 0 :4 5 Page 1 HPllOO 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 HPllOO 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 HP11Q0 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 Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HPllOO Autosampler Initial Conditions Draw Speed Eject Speed (/xl/min) Draw Position (mm) Stop Time (mins) Injection Volume(il) Vial Number 200.0 200 0.50 20.00 15.0 27 Tuning Method Report Method: Printed: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS Sun Aug 03 08:20:54 2003 si Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp . 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 Q u a n tify C a lib ra tio n R eport S tu d y N o. .-L 34910, S e t N o. :073103A R , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s ts K .R is h a Page 1 C a l i b r a t i o n : P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ F l u o r o c h e m i c a l s . P R O \ C u r v e D B \ 0 7 3 1 0 3 A R D e c a t u r BC L a s t m o d ifie d : Tue Aug 05 0 7 :0 3 :4 5 2003 P rin te d : Hed Aug 06 1 1 :0 3 :5 9 2003 ^cB|ot>|o3toal-4 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R ep o rt Vnd* S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A R , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a Page 2 C a l i b r a t i o n : P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ P l u o r o c h e m i c a l s . P R O \ C u r v e D B \ 0 7 3 1 0 3 A R D e c a t u r BC L a s t m o d ifie d : Tue Aug 05 0 7 :0 3 :4 5 2003 P rin te d : Wed A ug 06 1 1 :0 3 :5 9 2003 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R ep o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A R, E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 3 C a l i b r a t i o n : P :\D a t a \L C M S M S 6 \ M a s s ly n x \ F l u o r o c h e m ic a l s .P R O \ C u r v e D B \0 7 3 1 0 3 A R D e c a t u r BC L a s t m o d ifie d : Tue Aug 05 0 7 :0 3 :4 5 2003 P rin te d : Wed A ug 06 1 1 :0 3 :5 9 2003 W E x y g en R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R ep o rt W S tu d y N o. :L 3 4 9 1 0 , S e t N o. :073103A R , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t.-K .R is h a Page 4 C a l i b r a t i o n : P : \ D a t a \ I i C M S M S 6 \ M a s s l y n x \ F l u o r o c h e m i c a l s . P R O \C u r v e D B \0 7 3 1 0 3 A R D e c a t u r BC L a s t m o d ifie d : Tue Aug 05 0 7 :0 3 :4 5 2003 P rin te d : Wed A ug 06 1 1 :0 3 :5 9 2003 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A R, E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 1 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 Jab Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-101 Text: 1: C8 Acid (PFOA) * * * 2: C6 Sulfonate (PFHS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt \ |^ / S tu d y N o .:L 3 4 9 1 0 , S e t N o.:0 7 3 1 0 3 AR, E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 2 Sample List: P:\Data\LCHSHS6\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-101 Text: w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt . ^ S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A R, E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 3 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.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) x c o ; ^2503-1,25 ng/L Standard 03-Aug-2003 19:32:33 LC/MS/MS #6 0731133AR-102 Sm (Mn, 2x3) M R M of 4 Channels ES- 100] 9.13 14221^ 413 >369 8.87e4 A%- Area 0" | i i i t | 1 i 1 1 i |-- i . r i | " in ' 'TMl r 1 i 1 ' , , , . , . - r - r - n - p r - - r - i --r - j --t - i - r - i - p - i - r - i t *] lim 2.00 4.00 6.00 8.00 10.00 12.00 2 : C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No. :073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 4 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.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: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A R, E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\0731Q3AR 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) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.: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: Tue Aug 05 06:59:53 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheinicals.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: 073103AK-103 Text: 4: PFOSA XC072503-2, 50 ng/L Standard 073103AR -103 Sm (Mn, 2x3) 1 0 0 -i %- 03-Aug-2003 19:54:17 LC/MS/MS #6 M R M of 4 Channels ES- 9.89 498 > 78 103031 5.55e4 Area ~1 r -r--r r - | r - t - 2.00 I 1 - ' i ' i ' f i~ i I1' 1 I" 1 4 .0 0 6.00 ' ! ` ........ I 8 .0 0 i~t ' r - r - i- ^ ^ r -T i i | i i i i | Tim e 10.00 12.00 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tif y Sam ple R e p o rt i M ? S t u d y No . : L 3 4 9 1 0 , S e t N o .: 0 7 3 1 0 3 A R , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a Page 7 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.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-104 Text: 1: C8 Acid (PF0A) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 168 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:073103A R , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 8 Sample List: P:\Data\LCMSHS6\Masslynx\Fluorochemicals.PRO\SaiipleDB\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: 073103AK-104 Text: 4: PFOSA XC072503-3,100 ng/L Standard 073103A R -104 Sm (Mn, 2x3) 100] %: 0 --i--i " " -- I- -I--i--i--|--i--i--i--i--j--i ""I r- i--j--i--r 2 .0 0 4.00 03-Aug-2003 20:16:01 LC/MS/MS #6 M R M of 4 Channels ES- 9.89 498 > 78 1.07e5 Area 1-- I-- I-- I-- I-- r 6.00 1 ' I 1 8.00 10.00 t ' i ' I Time 12.00 E x y g en R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o.:0 7 3 1 0 3 A R , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\7luorochemicals.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 : 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103A R -105 Sm (Mn, 2x3) 100n 8.98 21488 03-Aug-2003 20:37:50 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 1 .29e5 Area 0 --r t~I '~I -< ' ' I " T - i-r-i" 2.00 3: C8 Sulfonate (PFOS) 1 I 1 1 1 1T 4.00 6.00 1T 111T I f I 8.00 1 111I 1 10.00 T im e 12.00 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A R, E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Page 10 Simple List: P:\Data\LCMSMS6\Masslynx\Fluorocheniicals.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-105 Text: 4 : PFOSA %0 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o.:073103A R , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s ts K .R is h a P age 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SanpleDB\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-106 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 073103A R -106 Sm (Mn, 2x3) 1 0 0 -, ' 'i 1 ' 1 1 i 2.00 3: C8 Sulfonate (PFOS) 4.00 r" i 1 6.00 8.98 43819 03-Aug-2003 20:59:39 LC/MS/MS #6 M RM of 4 Channels ES399 > 80 2.54e5 Area 8.00 10.00 T im e 12.00 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o.:0 7 3 1 0 3 A R , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R is h a Paga 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\Hasslynx\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-106 Text: 4 : PFOSA XC072503-5, 500 ng/L Standard 073103A R -106 Sm (Mn, 2x3) 10Ch %~ 0-* -T`' I - V | I - ` I I | I I * l I I I I | I I I I I I T I I-- | . 2.00 4 .0 0 6.00 V 03-Aug-2003 20:59:39 LC/MS/MS #6 M RM of 4 Channels ES- 9-90 _ 1040851 498 >78 5.47e5 Area 8.00 10.00 T im e 12.00 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o.:073103A R , E x t.D a te :0 7 /3 1 /0 3 , A n a ly s ts X .R is h a P age 13 Sample List: P:\Data\LCHSMS6\Hasslymc\71uorochejnicals.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 073103A R -107 Sm (Mn, 2x3) 1nru %- O1lt 1--r T --i 1 1 1 111 < 1 1 1 1 r 1 1 2.00 4 .0 0 ***? 2: C6 Sulfonate (PFHS) 9.15 5162151 1 03-Aug-2003 21:21:27 LC/MS/MS #6 M RM of 4 Channels ES413 >369 2.96e6 Area 1 1 "r"' l - r_ 1 1 1 i~' 1 '~T' 1 6.00 _____ 8 .0 0 1 >ri 1 I 1 1 1 * 1 |! 1 1 |M1 Tim e ____ 10.0 0 12.00 3: C8 Sulfonate (PFOS) XC072503-6,1000 ng/L Standard 073103A R -107 Sm (Mn, 2x3) 10Ch %: C H -- '-- i-- i-- i-- |-- r - i -- i-- i-- |-- i-- i-- i-- i-- |-- i-- i-- i-- i-- j-- i-- r 2 .0 0 4.00 61X) 9.27 53617 03-Aug-2003 21:21:27 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 3.12e5 Area 1 I 1 1 1 "I 8.00 10.00 -r-r-i Tim e 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .-.1,34910, S e t N o .:0 7 3 1 0 3 AR, E x t.D a te - .0 7 /3 1 /0 3 , A n a ly s t-.K .R is h a P age 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDBV073103AR 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-107 Text : 4: PFOSA XC072503-6,1000 ng/L Standard 073103A R -107 Sm (Mn, 2x3) 100h %- 03-Aug-2003 21:21:27 LC/MS/MS #6 M RM of 4 Channels ES498 > 78 1 .0 1 e 6 Area 0 - 1 - i i i i"i i i i > < i i i 1>- i | i 2.00 4.00 6.00 8.00 - '- I Time 12.00 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify S am ple R e p o rt V^ 0 S t u d y N o . : L 3 4 9 1 0 , S e t N o . : 0 7 3 1 0 3 A R , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a P age 15 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: 1: C8 Acid (PFOA) L34910-1 Spk C, 5000 ng/L, DF=100 073103A R -108 Sm (Mn, 2x3) 100-1 %: O -^T-l 1 -p T T I 1 I- 1 1 l-r-| "T 1 I 1 1 I T 1 1 1 T 11 1 I' 1 2.00 4.00 6.00 2: C6 Sulfonate (PFHS) 9.13 505641 1 03-Aug-2003 21:43:18 LC/MS/MS #6 M R M of 4 Channels ES413 >369 2.96e5 Area 1 i - 1" 1" 1 1 1 1 1 1 1 TM T n ? 1 I I I I 1 ....... 1 Tim e 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) Z x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 073103A R, E x t.D a te :0 7 /3 1 /0 3 , A n a ly s t:K .R iah a 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 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report %/ Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Paga 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: Wed Aug 06 11:04:02 2003 Name: 073103AR-109 Text : 1: C8 A c i d (PFOA) L34910-12 Spk E, 5000 ng/L, DF=100 073103AR-109 Sm (Mn, 2x3) 100- %- 9.13 925401 I 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES413 >369 5.53e5 Area 0- ' 1 ' 1 r'1-T' 1--r-r ''' i i ' i ' | I , , ' 1 ' 1" T '_ 2.00 4.00 6.00 i 8.00 1 1 i i 1 1 1 1 i i !i ' i Time 10.00 12.00 2: C6 S u l f o n a t e (PFHS) L34910-12 Spk E, 5000 ng/L, DF=100 073103AR-109 Sm (Mn, 2x3) 100- %- 8.98 103141 I 1 o- '~r' r 11 1 1 11111 I 2.00 r ! l--r--r 'I I I ' 1 T T-I t~| 1 -------------------------- i 4.00 6.00 8.00 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 6.00e4 Area i i t ' 1 1 i-- Ti me 10.00 12.00 3: C8 S u l f o n a t e (PFOS) L34910-12 Spk E, 5000 ng/L, DF=100 0731Q3AR-109 Sm (Mn, 2x3) 10CH % 9.25 17124 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1,03e5 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Fags 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheinicals.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-109 Text: 4: P F O S A V Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 19 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-110 Text : 1: C8 A c i d (PFOA) L34910-16 Spk F, 5000 ng/L, DF=100 073103AR-110 Sm (Mn, 2x3) 1 0 0 -] %: 03-Aug-2003 22:26:40 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 6.50e5 Area 0 '' 1 1 r 1 1 ' _l" I 1-1 '--'"T-r ' I ' 111 11 T"r 111 1T 1 2.00 4.00 6.00 W 2: C 6 S u l f o n a t e (PFHS) L34910-16 Spk F, 5000 ng/L, DF=100 073103AR-110 Sm (Mn, 2x3) 1 0 0 -1 %- 0 -^ 1I 11 f ' I ' ! 1 1 1 1t t '~ i - r - r 1 2.00 4.00 6.00 3: C8 S u l f o n a t e (PFOS) L34910-16 Spk F, 5000 ng/L, DF=100 073103AR-110 Sm (Mn, 2x3) 10CH t- t- i Time 12.00 03-Aug-2003 22:26:40 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 6.13e4 Area 1 0 .0 0 - n Time 12.00 03-Aug-2003 22:26:40 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.26e5 Area *0 0 - L r , T- ,- , ; I I I I ! I r - I - I- -| I ! I I I I i- v I - I I I - I r ' 2.00 4.00 6.00 I i-T I -r I I I I I I Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Paga 20 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-110 Text: 4 : PFOSA Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Faga 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 A c i d (PFOA) 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslyux\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: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 23 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-112 Text: 1: C8 A c i d (PFOA) ' U / 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .: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: 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-112 Text: 4 : PFOSA U h# Exygen Research, 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, 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.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-113 Text: 1: C8 A c i d (PFOA) 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/Q3, Analyst:K.Risha Page 26 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: 4: P F O S A W Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .: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 A c i d (PFOA) L34910-4, DF=1Q 073103AR-114 S m (Mn, 2x3) 10CH %: o^ 11' ' 1 1 I 1 1 ' 1 I ' 1 ' 1 1 1 2.00 4.00 2: C 6 S u l f o n a t e (PFHS) T 6.00 9.13 131415 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES413> 369 7.74e5 Area 8.00 T T " | r - 1 I 1 I I r I I ! Time 10.00 12.00 3: C8 S u l f o n a t e (PFOS) L34910-4, DF=10 073103AR-114 Sm (Mn, 2x3) 10Ch %: T7 2.00 4.00 6.00 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.59e5 Area io!oo - n Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date .07/31/03, Analyst :K.Risha Page 28 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-114 Text: 4: P F O S A w Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext-Date:07/31/03, Analyst:K.Risha Page 29 Simple 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-115 Text: 1: C8 A c i d (PFOA) 3: C8 S u l f o n a t e (PFOS) L34910-2, DF=10 073103AR-115 Sm (Mn, 2x3) 10Ch 9.27 375601 1 04-Aug-2003 00:15:30 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.19e5 Area 1% : - n -- I-- I-- ' ' p i !-- I-- r-- I-- I-- I-- I-- !-- I-- I-- I-- '-- I-- i-- !-- -- I-- I-- !-- I-- I-- r 1 " ' 1 2.00 4.00 6.00 1 1 ' 1 ' ~ r " l T - i ' -- T-- 8.00 1 1 Times - t - i - 11 > I 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Pasje 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.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: Q73103AR-115 Text: 4: P F O S A L34910-2, DF=10 073103AR-115 Sm (Mn, 2x3) 1 0 0 -1 O/ o/ . 04-Aug-2003 00:15:30 LC/MS/MS #6 MRM of 4 Channels ES- 9-90 16630 1 498 > 78 8.43e4 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 % *0 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha 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: w 2: C6 S u l f o n a t e (PFHS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report \ ^ 0 Study No.:L34910, Set No.: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.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-116 Text : 4 : PFOSA XC072503-2, 50 ng/L Standard 073103AR-116 Sm (Mn, 2x3) 1 0 0 -1 %- 04-Aug-20Q3 00:37:19 LC/MS/MS #6 MRM of 4 Channels ES- 9 .9 0 498 > 78 1089C 5.94e4 Area 0 w T --r 2.00 4.00 1 I 1 ! ri 6.00 r n" r ,|' 1 I 1 8.00 10.00 - n Time 12.00 %0 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 33 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-117 Text: 1: C8 A c i d (PFOA) 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report ''OmJ Study No.:L34910, Set N o .:073103AR, Ext .Date :07/31/03, Analyst :K.Risha * Page 34 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Decatur BC Tue Aug 05 06:59:53 2003 P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-117 Text: 4: P F O S A w Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date :07/31/03, Analyst:K.Risha Paga 35 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\MathDB\Decatur BC 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Coda: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-118 Text: 1: C8 A c i d (PFOA) % / 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sanqple Report Study No.:L34910, Sat N o .: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.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-118 Text: 4 : PFOSA %0 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report m S Study No .:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Hisha Page 37 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-119 Text: 1: C8 A c i d (PFOA) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 38 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocbemicals.PR0\SaiiqpleDB\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-119 Text : 4: P F O S A ___________________________________________________________________________________________________ |L34910-9, DF=10 ' ' '" ' 04-Aug-2003 01:42:36 LC/MS/MS #6 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No. .-L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst :K.Risha Page 39 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-120 Text: 1: C8 A c i d (PFOA) 3: C8 S u l f o n a t e (PFOS) L34910-7, DF=10 073103AR-120 Sm (Mn, 2x3) 100- %: 04-Aug-2003 02:04:23 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 j29284"! I 1.69e5 Area 0J 1 ' 1 "p - 1 1 1 1 1 1 1 1 ! ' 1 1 1 ' r_'! 1 1 1 I - r 1' 1"1 1 1 ' "i ' >--i-i-- ^ M ' I ' ' r-'"1 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report W Study No.:L34910, Set N o .:073103AR, Ext.Data:07/31/03, Analyst:K.Risha Page 40 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-120 Text: 4 : PFOSA Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 41 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-121 Text: 1: C8 A c i d (PFOA) ' W * 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report II,*/ Study No. .-L34910, Set N o .:073103AR, E x t .Date :07/31/03, Analyst:K.Risha Page 42 Sample List: Last modified: Method: Last modified: Job Code: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-121 Text: 4 : PFOSA X C 072503-3,100 ng/L Standard 073103AFM21 Sm (Mn, 2x3) 1OOn %- 04-Aug-2003 02:26:03 LC/MS/MS #6 MRM of 4 Channels ES498 > 78 1.12e5 Area 0 ` i ' ' i ' i , , n 111 ' i 1 i 1 1 1 1 i ' 2.00 4.00 6.00 W 8.00 10.00 - n Time 12.00 Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report / Study No.:L34910, Set N o .: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 Name: 073103AR-122 Text : 1: C8 A c i d (PFCA) L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) mn- %- 9.13 3089111 I 04-Aug-2003 02:47:47 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 1.81 e6 Area 1 CA I i : I I 1"l '' ' '""r'I 1 I ' 1 l'""i>| IT-- 1'' ''-"'1--" ''"I 1 1I-1'1 `! I1 .1.1.-.1.--.. ....'*-....'~..i ..' 1.' ' i 'i i'ii -ir-1i TIiIIme 2.00 4.00 6.00 8.00 10.00 12.00 2: C6 S u l f o n a t e (PFHS) L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) mrv, %- 8.98 261691 1 I 04-Aug-2003 02:47:47 LC/M S/M S #6 MRM of 4 Channels ES399 > 80 1,54e5 Area O -- - 1 'j ` 1 1 1 1 1 1 1 1 1 '1 1 1 '! 1 1 r---r-1- , T-T r--- ' ; 1 ' 1 ' ! ' ' ' TM ''i i-| ' ' ' i 2.00 4.00 6.00 8.00 10.00 ' T-| Time 12.00 3: C8 S u l f o n a t e (PFOS) L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) lOCh %: 9.25 644991 I 04-A u g -2003 02:47:471 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.81e5 Area 1 0^-~r--i'i-'- P " fi 1 r -i i i'i i i l'i r'T-i-f- i i I i' < i"'T"1^" r' 1 1mr " T"'1 2.00 4.00 6.00 8.00 -t , -r-i 10.00 i -T-r i-i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date :07/31/Q3, Analyst:K.Risha Page 44 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-122 Text: 4 : PFOSA E x y g a n R e s e a r c h 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o . :073103AR, Ext.Date:07/31/03, Analyst:K.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\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: 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) L34910-12 Rep, DF=20 073103AR-123 Sm (Mn, 2x3) 10CH %: 0--r i -i r -I : i [ I -i r-T[ r-I ! i- y ' r ' ' I '' ' ' '~r '' 2.00 4.00 6.00 04-Aug-2003 03:09:25 LC/MS/MS #6 MRM of 4 Channels ES9.25 499 > 99 3.75e5 Area 8.00 i ' 1i i i 10.00 .-i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .: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 Quantify Sample Report Study No.:L34910, Set N o .: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: 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-124 Text: 1: C8 A c i d (PFOA) 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) L34910-15, DF=20 073103AR-124 Sm (Mn, 2x3) 10Ch %: 0'1 r~r'1n"T1 1 '~r''T'` '"I 1 1 1T 1' 2.00 4.00 i11 1 1 I-- 6.00 04-Aug-2003 03:31:09 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 3.74e5 Area ' i ' "' ' i-T ' Tim e 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify San^ile Report Study No.:L34910, Sat N o .:073103AR, Ext.Data: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 L34910-15, DF=20 073103AR-124 Sm (Mn, 2x3) 100 %: (1V/ i i i i - ' 1 1 , * 1 ' -- . . . . . . . . r 7-1 ,"'1' i _r"1 r"i 2.00 4.00 6.00 04-Aug-2003 03:31:09 LC/MS/MS #6 MRM of 4 Channels ES9.90 498 > 78 1,30e5 Area 1 i ' 1 1 1 i ! 1 1 i 1 1 1 1 Time 8.00 10.00 12.00 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o . :073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 49 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaropleDB\073103AR Decatur Tue Aug 05 06:59:53 2003 P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 BC Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-125 Text: 1: C8 A c i d (PFOA) L34910-13, DF=20 073103AR-125 Sm (Mn, 2x3) 100- %- Ch _ r i 1 1 1 1 i~'- ' ~| i"1 2.00 4.00 2: C6 S u l f o n a t e (PFHS) 9.13 3547301 I 04-Aug-2003 03:52:55 LC/MS/MS #6 MRM of 4 Channels ES413> 369 2.09e6 Area [ i 1 1 ' 11 ii 1''1 1 1 ii 1 `' 1 1 ii .1.1.1..1.TM..-.r~'.' ii T~,`- 1i v'ii 1' ' ii 1 ii Tiinme 6.00 8.00 10.00 12.00 3: C8 S u l f o n a t e (PFOS) L34910-13, DF=20 073103AR-125 Sm (Mn, 2x3) 10Ch 9.25 77839 04-Aug-2003 03:52:55 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.48e5 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 E x y g e n R e s e a r c h , 30 58 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 16801 Quantify Sample Report *, f# Study No. :L34910, Set No. :073103AR, E x t .D a t e :07/31/03, Analyst :K.Risha Page 50 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: 4 : PFOSA E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report S t u d y N o .:L 3 4 9 1 0 , S e t No . :0 7 3 1 0 3 A R , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t :K.R i sha Page 51 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SanpleDB\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: 1-. C 8 A c i d (PFOA) XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) 10Ch %: 04-Aug-2003 04:14:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 7.35e5 Area 0~r 2.00 2: C 6 S u l f o n a t e (PFHS) 4.00 6.00 - n Time 8.00 io!oo 12.00 3: C8 S u l f o n a t e (PFOS) XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) 04-Aug-2003 04:14:4^ LC/MS/MS #6 MRM of 4 Channels ES ' " 499 > 99 7.65e4 Area i i ' ' ? | n r i | Time 2.00 4.00 6.00 8.00 10.00 12.00 W ------------------------------------------------------------------------------------------ Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report S t u d y No.:L34910, S e t N o .:073103AR, E x t . D a t e : 07/31/03, A n a l y s t :K.R i s h a Page 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) 100-, %: 04-Aug-2003 04:14:42 LC/MS/MS #6 MRM of Channels ES9.92 498 > 78 2.56e5 Area 0- - ' " ' ' ' I ' - ' 1 '~1 r~'"i r ' 1 1 ' 'I r 1 1 I-] -i-i-- r -i-- j-- r- 2.00 4.00 6.00 8.00 10.00 i t T- .-i.! Time 12.00 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 53 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-127 Text: 1: C8 A c i d (PFOA) 2: C6 S u l f o n a t e (PFHS) 3: C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report S t u d y No . : L 3 4 9 1 0 , S e t N o .:0 7 3 1 0 3 A R , E x t . D a t e :0 7 / 3 1 / 0 3 , A n a l y s t :K . R i s h a Page 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\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-127 Text: 4 : PFOSA M0 Exygen Research 3058 Research Drive State College, PA 16801 Quantify Sample Report i|t|< Study No.:L34910, Set N o .:073103AR, Ext .Date :07/31/03, Analyst :K.Risha Page 55 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Tue Aug 05 06:59:53 2003 P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-128 Text: 1: C8 A c i d (PFOA) L34910-16 Rep, DF=100 073103AR-128 Sm (Mn, 2x3) 10Cb %: 9-13 83658 1 1 04-Aug-2003 04:58:16 LC/MS/MS #6 MRM of 4 Channels ES413 >369 4.68e5 Area o: ' ' ' 1T"r T_T |-"l 1' 1''1' I' I1 I' 11 rr 'I' I1 1' 1i '"Ii iI--- *'----- 1- 1 i!"l1_1i 1 1 rr11 1',11 '7t 1- ' 1 1i m i- 1 Ii' II <<ir '' t 1I i-i-I Ii TIiimme , 2.00__________ 400__________ 6/30__________ 8/30__________10.00_________ 12.00 | 3: C8 S u l f o n a t e (PFOS) L34910-16 Rep, DF=100 073103AR-128 Sm (Mn, 2x3) ^nn_ %- Ch 1' 1 r~' 1 i ' --- ' i 2.00 9.27 172641 I 04-Aug-2003 04:58:16 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.56e4 Area ' ' i 1 1 1 "i r"' 1 ............................... 4.00 6.00 8.00 1 1 -| . i r 10.00 Time 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report i.B Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 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.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: 4 : PFOSA w E x y g e n R e s e a r c h 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:Q73103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 57 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-129 Text: 1: C8 A c i d (PFOA) L34910-19, DF=100 073103AR-129 Sm (Mn, 2x3) 10CH 9.13 75424 04-Aug~2Q03 05:20:01 LC/MS/MS #6 MRM of 4 Channels ES413 >369 4.39e5 Area 2.00 2: C6 S u l f o n a t e (PFHS) 4.00 6.00 8.00 10.00 Time 12.00 3: C8 S u l f o n a t e (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, E x t .D a t e :07/31/03, Analyst:K.Risha Page 58 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-129 Text: 4 : PFOSA E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set N o .:073103AR., Ext.Date:07/31/03, Analyst:K.Riaha 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 A c i d (PFOA) L34910-17, DF=100 Q73103AR-130 Sm (Mn, 2x3) 100t %: 04-Aug-2003 05:41:49 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 >369 4.61e5 Area 2.00 2: C6 S u l f o n a t e (PFHS) 4.00 6.00 8.00 - T 1 v 1 ' I -1'1r - r 1 I Time 10.00 12.00 3: C8 S u l f o n a t e (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report i^ r Study N o .:L34910, Set N o .: 073103AR, E x t . Date:07/31/03, Analyst:K.Riaha 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\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: 4 : PFOSA %H0 E x y g e n R e s e a r c h 3058 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 168 0 1 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Riaha Page 61 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-131 Text : 1: C8 A c i d (PF0A) 2: C6 S u l f o n a t e (PFHS) XC072503-5, 500 ng/L Standard 073103AR-131 Sm (Mn, 2x3) 100-1 %- 8.96 45496 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.61e5 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 S u l f o n a t e (PFOS) XC072503-5, 500 ng/L Standard 073103AR-131 Sm (Mn, 2x3) 100-1 9.27 28469 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.62e5 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 %0 Exygen Research, 3053 Research Drive, State College, PA 16801 Quantify Sample Report Study N o .:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 62 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Decatur BC Tue Aug 05 06:59:53 2003 P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-131 Text: 4: P F O S A w Exygen Research, 3058 Research Drive State College, PA 15801 Quantify Sample Report W Study No.:L34910, Set N o .:073103AR, E x t .D a t e :07/31/03, Analyst:K.Risba 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 080103 Last modified: Sun Aug 03 07:11:59 2003 Job Code: Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-132 Text : 1: C8 A c i d (PFOA) [L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) 10CH % 9.13 380900 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.20e6 Area 2.00 2: C6 S u l f o n a t e ( P F H S ) (L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) 10(h 4.00 6.00 8.00 8.96 33004 10.00 Time 12.00 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1,86e5 Area 2.00 3: C8 S u l f o n a t e (PFOS) 4.00 6.00 Time 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.-.L34910, Set N o .:073103AR, Ext .Date :07/31/03, Analyst:K.Riaha Page 64 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\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-132 Text: 4: P F O S A Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report t.--/ S t u d y No.: L 3 4 9 1 0 , S e t N o .: 0 7 3 1 0 3 A R , E x t . D a t e : 0 7 / 3 1 / 0 3 , A n a l y s t : K . R i s h a Page 65 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-133 Text: 1: C8 A c i d (PFOA) L34910-16 Rep, DF=20 073103AR-133 Sm (Mn, 2x3) mn-, %- 9.12 3917891 I 1 04-Aug-2003 06:47:22 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.26e6 Area (h _ '~"l I ' r 1 f l - i - r - r I . .--i-]--r--.-I-'-,--' I1I1,' 1-- ^I ' ! ' 'i 7| ': i I-, r , i-- i Ii TIiIIme 2.00 4.00 6.00 8.00 10.00 12.00 2: C6 S u l f o n a t e (PFHS) L34910-16 Rep, DF=20 073103AR-133 Sm (Mn. 2x3) 1007 04-Aug-2003 06:47:22 LC/MS/MS #6 MRM of 4 Channels ES8.97 399 > 80 1.81 e5 Area 0 ' 1 r-n--i ^ i 1 1 r~n i 1 1 1 1 I 2.00 4.00 3: C8 S u l f o n a t e (PFOS) L34910-16 Rep, DF=20 073103AR-133 Sm (Mn, 2x3) 10Ch %: 6.00 0 ' ' 1 1 I 1 1 1 1 I ' 1 '11 I '-1"'-| 1 1 1 I"1 -- T-1" 2.00 4.00 6.00 8.00 10.00 -r-i Time 12.00 04-Aug-2003 06:47:22 LC/MS/MS #6 MRM of 4 Channels ES9.25 499 > 99 4.80e5 Area 8.00 r 1 ' m .......... I Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 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\SampleDB\0731Q3AR 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-133 Text : 4: P F O S A w E x y g e n R e s e a r c h 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext .Date:07/31/03, Analyst :K.Risha Page 67 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-134 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-19, DF=20 073103AR-134 Sm (Mn, 2x3) 10Ch %- 9.25 822011 I 04-Aug-2003 07:09:05 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.64e5 Area 0- --'--'----'--1--'--'--1--1--1--^---- 1 1 1 1 1 1 1 1 1 1 1 1 1 1 ' ' 1 1 1 r .............. " ^ 1 .............. . 2.00 4.00 6.00 8.00 10.00 Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, E x t .Date:07/31/03, Analyst:K.Risha W Page 68 Sample List: P : \Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\San5>leDB\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 w Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.-.L34910, Set N o .:073103AR, Ext .Date:07/31/03, Analyst :K. Ri sha Page 69 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\ScimpleDB\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: 1: ca Acid (PFOA) 2: C6 Sulfonate (PFHS) L34910-17, DF=20 073103AR-135 Sm (Mn, 2x3) %- 0- ' r I -r- .-I -T ' " ' I ' 2.00 3: C8 Sulfonate (PFOS) L34910-17, DF=20 073103AR-135 Sm (Mn, 2x3) 100~i O//o_ 8.96 I286601 04-Aug-2003 07:30:42 LC/MS/MS #6 MRM of 4 Channels ES' 399 > 80 1.69e5 Area 1 1 T 1 i--r r-r 1 ' 1 1 ; 1 1]-- 1t 1 1 4.00 6.00 8.00 1 -- ' < I ' i-i i~'' ' Time 10.00 12.00 04-Aug-2003 07:30:42 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 4.44e5 Area O-1 I ' '1 1 1 1 1 ' I I I I ' I '-- 1 1 I"1 1 I 2.00 4.00 I 6.00 10.00 T -n Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o .:L34910, Set N o .:073103AR, Ext .Date:07/31/03, Analyst :K.Risha Paga 70 Sample List: P:\Data\LCMSMSS\Masslynx\Fluorochemicals.PRO\ScimpleDB\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 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst:K.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\i`luorochemicals.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-136 Text : 1: C8 Acid (PF0A) XC072503-6,1000 ng/L Standard 073103AR-136 Sm (Mn, 2x3) 100--i %-i 9.12 477931 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES 413> 369 2.78e6 Area Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOSj X C 072503-6,1000 ng/L Standard 073103AR-136 Sm (Mn, 2x3) 1nru. %- CH--T--I--r--i--I--!--i-- i--I--I--I--I--I--I--I--I--I--i--I--I--!--I--I--I--I--|--r "i w 2.00 4.00 6.00 9.24 531571 I 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 3.02e5 Area r~'i --i r i i i 8.00 1 ^ i i ' ' r i-i r- 1 T-r-i T im e 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report \ Study No. .-L34910, Set N o .:073103AR, Ext.Date:07/31/03, Analyst :K.Risha Page 72 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-136 Text : 4 : PFOSA XC072503-6,1000 ng/L Standard 073103AR-136 Sm (Mn, 2x3) 100-, %- 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 19068C 9.76e5 Area & w 2.00 4.00 6.00 8.00 T -, Time 10.00 12.00 W Exygen Research 3058 Research Drive, State College, PA 16801 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA 134910 PFOS 499 -> 99 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: FmaJ Volume: 30 ppt 15 pL Water 40.0 mL 3.0 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 Std. Analyte Amount Exygen Sponsor Sample Run Cone. Dilution Peak Found Added Recovery ID XC072503-0 ID Code No. (ppo Factor Area (ppo (ppt) (%) CS 08003A-1001 0 0 XC072503-1 CS 08063A-1002 25 1233 -- XCQ72503-2 CS Q80603A-10Q3 50 2570 -- XC072303-3 CS 080603A-1004 100 4455 -- XCQ72503-4 CS 080603A-1005 250 10551 - XC072503-5 - CS 080603A-1006 500 22336 -- XC072503- - CS 080603A-1D07 1000 43039 - 0106020 Control c 080603A-1008 0 ND - 0106020 Spk A - LGS 080603A-1009 2436 51.3 50 103 0106020 Spk B LCS 080603A-1010 21693 490 500 98 L34910-12 Spk E BC2SW-06 LF 080603A-1011 100 22031 49800 25000 95 L349I0-16 Spk F Outfall to River SW-25 LF 080603A-1012 200 18543 * 50000 w L34910-16 Spk F Outfall to River SW-25 LF 08063A-1013 100 35655 80900 50000 99 XC072503-1 CS 08063A-1014 25 1229 - XC072303-2 CS 080603A-1015 50 2338 - - XC072503-3 CS 080603A-1016 100 4928 - - L34910-1 134910-1 Rep L 3 4 9 1 0 -12 L34910-12 Rep L349I0-15 BC2 SW-04 BC2 SW-04 BC2SW-06 BC2 SW-06 BC2 SW-06 Dup S 080603A-1017 - 100 5243 11500 s 080603A-1018 100 5235 11500 s 080603A-1019 100 11612 26100 s 080603A-1020 100 11877 26700 s 080603A-1021 100 11205 25100 - L34910-13 BC2 SW-06 Low Spk FF 08003A-1022 100 14257 32100 100 6000+ XC072503-4 XC07 2503-3 - CS 080603A-1023 250 10803 - - - CS 080603A-1024 500 23323 - - - X C 0 7 1003-6 - CS 080603A-1025 1000 - 44271 - Analyte Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = (analyte found (ppt)-analyte found in control (ppt)] *. too amount added (ppt) 3dard Curve : Linear (1/x weighted) Intercept = 184.312 Slope = 43.8624 Coef. Of Del. = 0.998804 CS = Calibration standard LF = Lab fortified sample C = Coacrol sample FF = Field fortified sample S = Sample LGS - Laboratory Control Spike CK = Check Standard ND = Not delected = Response between 0 and 15 ppt NQ = Not quantifiable = Response between 23 ppt and LOQ (30 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. 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: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator N.o... 32- Time IQ 3 O ______ Date_ Q fe lD b lo ^ Initials CLIENT SAMPLE ID na na na BC2 SW-06 Outfall to River SW-25 EXYGEN ID NUMBER 0106020 Control 0106020 Spk A 0106020Spk 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 L3491Q-12 Spk E L3491Q-16 Spk F Spiking Solution Used F061103-2 (10 ngAnL) F061103-1 (100 ng/mL) F060203-1 (10000 ng/mL) F060203-1 (10000 ng/mL) Volume Used for Spiking 200 (iL (200 pL micropipet) 200 pL (200 pL micropipet) 100 pL (200 |iL micropipet) 200 pL (200 yrL micropipet) All samples were measured: Time 1 2 -4 0 Date After measuring samples were returned to refrigerator No. 3 2 Time \3C S ______ Date. Initials Initials. Comments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date , Q&jbfc)o3 Analysis Summary: w Data Set: Data Set: Data Set: Set extraetion/analysis data verified by: Initials/Date Initials/Date Initials/Date yjC/ oelbl^ -__ / Date:. z f m July 26. 2001/6 R E S E A R C El 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAM PLE EXTRACTIO N AND ANALYSIS TRACK ING SHEET EXYGEN STUDY NUMBER: L34910 MATRIX: Water METHOD: " ANALYTES: PLUS. PEPS, PFOA and PFOSA PROTOCOL NUMBER: tAA Client ID na na na BC2 SW-06 Outfall to River SW-25 - Exygen ID 0106020 Control 0106020 Spk A 0106020 Spk B L34910-12 Spk E L34910-16 Spk F - STEP 1 \/ - -- - -- - -- -- - -- - -- - -- -- -- - -- -- - -- - -- - -- - -- - -- -li/. *InitiaW D ate - STEP 1: SPE column clean-up (omittiDg 40% wash) STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC7MS/MS analysis STEP 4: LC/MS/MS reanalysis. STEP 2 / \1 - - - h- Dilutions (mUmL) -- - - STEP 3 1 Dilutions (mL/mL) - STEP 4 - -- " o $ 0 r ? AA o s A .o . - - - - _- - , __ - - -- - -- - -. - - --- - --_ - -. -_ _ - --- - -- - .-. - ._ - .._ - . -- . -- \l j : - e&ioE(o3 c e & c > - E F : 1 0 0 "t2 6 O . pct>&|Dfc|o?> U - - Reagents/ Materials Methanol CIBSPE Type I Water . . Lot # 4311^18 NA . _. ._ - Initials/D ate . . 0_ . ._ . . . _ HPLC Methanol Ammonium Acetate Type I water . ^3067314 V 3 ^i NA . . Ia Inifials/D aie o B lS S i Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination o f Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water COMMENTS: Final extracts stored in refrigerator 5 V Initials: Date: tg > l& |fr* > July 19, 2001/4 M asslynx - Sam ple List Sample List: C:\MASSLYNX\Fluorocherpicals.PRO\SampleDB\080603A Decatur BC.SPL Printed: Wed Aug 06 13:15:20 2003 d/y) - --- ------- ---------- T - Vial File Name LIMS ID C lient ID Sam ple D escription 1 41 080603A-1001 _ 2 42 080G03A-1002 -- 3 43 080603A-1003 4 44 080603A-1004 -- 5 45 080603A-1005 -- 6 46 080603A-1006 7 47 080603A-1007 -- - 8 51 080603A-1008 -- 9 52 080603A-1009 -- 10 53 080603A-1010 -- 11 54 080603A-1011 -- 12 55 080603A-1012 -- 13 56 080603A-113 -- 14 42 080603A-1014 -- 15 43 080603A-1015 -- 16 44 080603A-1016 -- 17 57 Q80603A-1017 -- 18 58 080603A-1D18 -- 19 59 080603A-1019 -- 20 60 80603A-1020 -- 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 XCO72503-1, 25 ng/L Standard XC072503-2, 50 ng/L Standard XCO72503-3, 100 ng/L Standard XC072503-4, 250 ng/L Standard XCO72503-5, 500 ng/L Standard XC072503-6, 1000 ng/L Standard 0106020 Control 0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/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 XCO72503-1, 25 ng/L Standard XC072503-2, 50 ng/L Standard XC072503-3, 100 ng/L Standard L34910-1, DF=10Q 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 Exygen STUDY NO. t - W l o Page Position: (1. 1) Matrix Sample Type Cone (ng/i -- Standard -- S tandard -- Standard -- Standard -- Standard -- Standard --- Standard -- Blank -- C -- QC -- QC -- QC ... QC ... Standard -- Standard -- Standard -- Analyte -- Analyte -- Analyte -- Analyte -- Analyte -- QC -- Standard -- Standard -- Standard 0 25 50 100 250 500 1000 -- 100 500 25000 50000 50000 25 50 100 -- -- -- -- -- 100 250 500 1000 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- f3> Cone C T est ID DF --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 1 100 200 100 1 1 1 100 100 100 100 100 100 1 1 1 * \ Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemlcals.PRO\SampleDB\080603A Decatur BC.SPL Printed: Wed Aug 06 13:15:20 2003 t f l u D )jo b jo i> ____ MS Method HPLC M ethod MS Tune File Inj.Volum e 1 C6 C8 SULF C8 ACID PFOSA 2 C6 C8 SULF C8 ACID PFOSA 3 C6 C-8 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 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 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 Fluorochem s 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 Exygen STUDYNO. (3 ^ ID Page 2 Page Position: (2, 1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen 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) : Analyst: 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: Iffb 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 C6jcb|o 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 O.CO 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 3 498.0C 78.00 0.20 4 499.00 99.00 0.20 35 10 30 40 5G 10 50 30 Method Report Page 1 Method File: Last Modified: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs water Wednesday, August 06, 2003 13:15:26 w Printed : Wednesday, August 06, 2003 13:16:00 & 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 35 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 Timetabl e 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 (/il) Vial Number 200 .0 200 0 .50 20.00 15.0 82  ^ Tuning Method Report Method: Printed C :\MAS SLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS Wed Aug 06 13:19:13 2003 Page 1 .4y-feYy***-jr $ ",r 'CtjauqRie;;. bF395.00 3I ^>{ ' b, `^ S viY *V> ^ ,, >f - ( - f J i> ^ v iif e * i i ' V t& ' v -`frr iiVb if, r H * 13* 5- l FJKa' f1e t r : s.* .; > ) !'** ,)* , r kin*. *-ft, # , i '~ siFr 'di' -:-r 'Tl T;1 U fi , , in v i l , 1. ! ri w h e : .327 3?R 329 3 30 331 3 3 2 'v 333 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 Quantify Calibration Report Study No .:Ij34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Paga 1 w Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report ^ Study No.:L34910, Set No.:080603A, E x t .D a t e :07/31 & 08/06/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\0806Q3A Decatur Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 080603 Thu Aug 07 08:11:08 2003 BC Job Code: . Printed: Thu Aug 07 12:49:56 2003 Initials._______ Date & \ q 11q Ts ____________ R u n # ^ 0 & - l t ^ | To Name: 080603A-1001 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o .:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur EC 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-1002 Text: 1: C8 Sulfonate (PFOS) W Exygen Research 3058 Research Drive, State College, PA 16801 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\Fluorochemicals.PR0\MethDB\PE0S only 080603 Last modified: Thu Aug 07 08:11:08 2003 Job Code: 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 Quantify Sample Report Study N o .:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Rage 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 12:49:56 2003 Name: 080603A-1004 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 Quantify Sample Report Study N o .:L3491Q, Set No.:080603A, Ext.Date:07/31 t 08/06/03, Analyst:K.Risha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\0806Q3A 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 %: U r [ r - ' < 1' 'r'1 !"r ' '' 1-1 2.00 4.00 06-Aug-2003 16:24:39 LC/MS/MS #6 9.35 105511 MRM of 4 Channels ES499 > 99 4.71e4 Area L,, 11 r 1 1 r ' 1 1 1TM 1 1 1 1 1 1 i_rI 1 i" 1-- Time 6.00 8.00 10.00 \0 Exygen Research 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:L34910, Sat No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 6 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\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-1006 Text: 1: C8 Sulfonate (PFOS) w Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Pago 7 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.FRO\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) 100-1 %- 9.33 4303i 06-Aug-2003 17:08:00 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.83e5 Area 0 V T 2.00 4.00 6.00 8.00 10.00 Time i %0 Exygen Research, 3058 Research Drive, State College PA 16801 Quantify Sample Report Study N o .:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Pago 8 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 Coda: 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 Quantify Sample Report Study N o .:L34910 , Set No.:080603A, Ext .Date:07/31 & 08/06/03, Analyst-.K.Risha Page 9 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-1009 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 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.PRO\SampleDB\0806Q3A 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-1010 Text: 1: C8 Sulfonate (PFOS) 0106020 Spk B, 500 ng/L 080603A-1010 Sm (Mn, 2x3) 10Ch %: 9.31 21693 06-Aug-2003 18:13:04 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 9.58e4 Area 0 ..... . !" ' I-'-r |"T , 2.00 4.00 6.00 8.00 10.00 Time 1*0 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o .:L34910, Set No.:080603A, Ext.Date :07/31 & 08/06/03, Analyst:K.Risha Page 11 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.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-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 ES499 > 99 9.36e4 Area o- "l~ ' : ----'~ r~ ' T- ' 1---- 1"1 ' "r 1 1MI1 1 1 1-111 1''"I---- r~T 1 i 1 r ' 1 )"1 ' 2.00 4.00 6.00 8.00 w i I i i i i |-- --i--i-- Time 10.00 w Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report 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.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-1012 Text: 1: C8 Sulfonate (PFOS) L34910-16 Spk F, 50000 ng/L, DF=200 080603A-1012 Sm (Mn, 2x3) 100n %: 9.32 18543 I 06-Aug-2003 18:56:25 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 7.99e4 Area 0 T 1!1i1111i1''1i1 111 i1 11i1 1i1 2.00 4.00 6.00 8.00 10.00 Time V Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o .:L34910, Set No .:080603a , Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SamplaDB\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-1013 Text: 1 : C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 14 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.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 Sulfonate (PFOS) w Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o .:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.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\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-1015 Text: 1: C8 Sulfonate (PFOS) XC072503-2, 50 ng/L Standard 080603A-1015 Sm (Mn, 2x3) 10CH %H 9-36 23381 1 06-Aug-2003 20:01:40 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1,08e4 Area CH /V I - 1 , ,-- ' I , , , I ' '.'T 1 r1' 1' >' - [-r"rr '1-"rr '' -- '-II "-'1 ' 1i 1 1 1' 1 1 i I 1 T ime 2.00 4.00 6.00 8.00 10.00 Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report u mt Study N o .:L34910, Set No.:080603A, Ext-Date:07/31 & 08/06/03, Analyst:K.Riaha 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.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-1016 Text : 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Page 17 Study No.:L34910, Set No.:080603A, Ext.Date:07/31 i 08/06/03, Analyst:K.Risha w 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-1017 Text: 1: C8 Sulfonate (PFOS) % kJ Exygan Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080603A, Ext.Date :07/31 & 08/05/03, Analyst:K.Risha Page 18 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.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: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report It*/ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Paga 19 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-1019 Text: 1: C8 Sulfonate (PFOS) w Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080603A, E x t .D a t e :07/31 & 08/06/03, Analyst:K.Risha Page 2 0 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-1020 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o .:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 21 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-1021 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report ' l l ' Study N o .:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 22 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\FTuorochemicals.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 Sulfonate (PFOS) L34910-13, DF=100 080603A-1022 Sm (Mn, 2x3) 10C h %: 0 1 1 1 1 I 1 1 I 1 1 ' I 1 1 I1 2.00 4.00 6.00 9-36 1425 7 06-Aug-2003 22:33:46 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 6.13e4 Area 8.00 10.00 Time Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report y Study No.:L34910, Set No.:080603A, Ext .Date:07/31 & 08/06/03, Analyst-.K.Risha Page 23 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SanqpleDB\080603A Decatur BC Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 080603 Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1023 Text: 1: C8 Sulfonate (PFOS) % *# Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Page 24 Study N o .:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K .Risha w Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Decatur BC Last modified: Th.u 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-1024 Text: Exygen Research 3058 Research Drive State Collage, PA 16801 Quantify Sample Report Page 25 Study N o .:L34910, Set N o . :080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha W Sample List: P:\Data\LCMSMS6\Masslynx\Fluarochemicals.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-1025 Text: 1: C8 Sulfonate (PFOS)______________________________________ ____________ __________________ X C 072503-6,1000 ng/L Standard 06-Aug-2003 23:38:52 LC/MS/MS #6 080603A-1025 Sm (Mn, 2x3) MRM of 4 Channels ES` " 499 > 99 1.91e5 Area T ' 1.1 'I ' I I r Time 2.00 4.00 6.00 8.00 10.00 w Exygen Research 3058 Research Drive, State College, PA 16801 SECTION E SponsorStudy No: Exygen Study No: Analyte: loosMonitored: Site: NA L34910 PFOA 413 ->369 DecaturBaker'sCreek R A W DATA REPORT LimitofQuantitation: InjectionVolume: Matrix: Sample Weight: Final Volume: 50ppt 15pL Soil 5.0g 5.0mL SetNo: Analyst InstrumentType: ExtractionDate: Analyzed on: 080103A Kuren RJsha LCMSMS #6 Q8A11/Q3 08702/03 Exygen ID XC072503-0 XC072503-1 XCO72503-2 XC072503-3 XC072503-4 XC072503-5 XC0725O3-6 Methanol Wash ReagentBlank ReagentSpk A ReagentSpk B Sponsor ID na na na Sample Code CS CS CS CS CS CS CS c c LCS LCS Run No. 08103A-2003 080103A-2002 0801Q3A-2003 080103A-2004 080103A-2005 080103A-2006 0S013A-2007 080103A-2008 080103A-2009 080103A-20LQ 080103A-2O11 XC072503-1 CS 080103A-2012 L34910-5 Spk C L34910-10 Spk D BC2 SED-04 BC2 SED-05 LF 080103A-2013 LF 080103A-2014 L34910-U Spk E BC2 SED-0 LF 080103A-2015 L34910-20 Spk F OutfalltoRiverSED-25 LF 080103A-2016 XC072503-2 - CS 080103A-2017 L34910-5 BC2 SED-04 S 0801Q3A-2018 L34910-5 Rep BC2 SED-04 s 080103A-2019 L349I0-10 BC2 SED-05 S 080103A-2020 L34910-10 Rep BC2 SED-05 s 080103A-2021 XC072503-3 CS 080I03A-2022 XC072503-4 L349I0-11 BC2SED-06 CS 080103A-2023 s 0801Q3A-2024 L34910-U Rep L34910-20 BC2 SED-06 OutfalltoRiverSFJ3-25 s 080J03A-2025 s 080103A-2026 L34910-20Rep OutfalltoRiverSED-25 s 080103A-2027 L34910-21 OutfalltoRiverSED-25 Dup s 080103A-202S XC072503-5 CS 080103A-2029 XC072503-6 - CS 080103A-2030 AnalyteFound (ppt)* (peakarea-intercept)/slopex DF Recovery (%)= (anaJvtefound(ppt)-aaaJytefoundincontrol(ppt)}x 100 amountadded (ppt) Std. Cone. (ppo 0 25 50 100 250 500 1000 25 - 50 100 250 - - 500 1000 Dilution Factor 10 10 10 10 1 l 1 Peak Area 333 9882 17917 34827 78794 171634 315768 525 518 18939 163063 9820 157971 166134 187666 179090 18190 115451 82762 195055 167826 33920 79282 473416 463017 404209 301201 532619 140009 273386 Analyte Found (ppt) Amount Added (ppt) Recovery (%) Analyte Found <ppt>) - -- - - - -- - ND - 55.3 50 111 - 536 500 107 - - 5190 5000 96 - 5460 5000 96 - 6180 5000 88A - 5890 5000 91A - -- 377 3.02 268 2.14 642 5-14 551 4.41 - * **- - - fttand^rrif^fve:Linear(1/x weighted) Intercept 2344.75 Slope ~ 300.076 Cocf.OfDd. 0.988097 Total Solids (%) 69,96 69.96 69.54 69.54 60.41 60.41 63.27 63.27 67.43 AnalyteFound (ppb) (analytefound(ppt)x volume extracted(0.04L)]/sample weight(5g) AnalyteFound (ppb)dry weight analytefound (ppb)x (100% /totalsolids(%)) CS * Calibrationstandard C = Control sample S * Sample LF = Lab fortifiedsample FF Field fortifiedsample LGS * Laboratory ControlSpike CK 9 CheckStandard ND * Notdetected= Responsebetween0 and25 ppt NQ 9 Notquantifiable* Responsebetween 25 pptandLOQ (50ppt) Analyte Found (ppb) Dry Weight - - 4.31 3.06 7.39 6.34 - - - 'Sample requires dilution. See data set 080I03AR. `Sample was corrected using the data found in set 080103AR. Spreadsheet prepared by: SponsorStudy No: Exygcn Srndy No: Analyte: Ions Mooiiorcd: Site: NA L34910 PFHS 399 ->80 DecaturBaker'sCreek RAW DATA REPORT Limit ofQuantitationInfectionVolume: Matrix: Sample Weight: Final Volume: 50 ppt 15 pL Soil 5.0 g 5.0mL SetNo: Analyst: InstrumentType: Extraction Date: Analyzed on: 080103A Karen Risha LCMSMS #6 08/01/03 08/02/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 Methanol Wash Reagent Blank ReagentSpk A ReagentSpk B XC072503-1 L34910-5Spk C L34910-10Spk D L34910-I1 Spk E L34910-20 Spk F XC072503-2 L34910-5 L34910-5 Rep L34910-10 L34910-10 Rep XC072503-3 XC072503-4 L349I0-I l L34910-U Rep L34910-20 L34910-2Q Rep L34910-21 XC072503-5 XC072503-6 Sponsor ID - - - - na na na BC2SED-04 BC2SED-05 BC2 SED-06 OutfalltoRiverSED-25 BC2 SED-04 BC2 SED-04 BC2 SED-05 BC2 SED-05 - BC2 SED-06 BC2 SED-06 O.utfalltoRiverSED-25 OutfalltoRiverSED-25 OutfalltoRiverSED-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. 080103A-2001 080103A-2002 080103A-2003 080103A-2004 080103A-2005 080103A-2006 080103A-2Q07 080103A-2Q08 080103A-2009 Q80103A-210 080103A-2011 080103A-2012 080103A-2Q13 080103A-2014 080103A-2015 080103A-2016 080I03A-2017 080103A-201S 080103A-2019 080I03A-2020 080I03A-2021 08013A-2022 080103A-2023 080103A-2024 080103A-2025 080I03A-2026 080103A-2027 080103A-2028 08Q1Q3A-2Q29 080103A-2030 AnalyteFound (ppt) {peakarea-intercept)/slopexDF Recovery (%) * [analytefound(ppt)-analytefound incontrol(ppt)Jx 100 amountadded (ppt) Std. Cone. (ppt) 0 25 50 100 250 500 1000 25 50 100 250 - 500 1000 Dilution Factor - - I 10 10 10 10 1 1 1 1 1 1 1 1 l Peak Area 0 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 (pp Amount Added (ppt) Recovery (%) Analyte Found (PPb) . - - -- - -- - ND 52.0 50 533 500 104 107 - 5280 5530 5560 5560 5000 5000 5000 5000 104 107 105 103 - 70.8 0.57 51.7 0.41 182 1.45 218 1.75 - 308 327 399 282 623 -- - 2.46 2.61 3.19 - 2.26 4.98 Standard Curve:Linear(l/xweighted) Intercept = 476.906 Slope * 573138 Coef.OfDeL = 0.995587 Total Solids (%) - - - - - - 69.96 69.96 69.54 69.54 - 60.41 60.41 63.27 63.27 67.43 - - Analyte Found (ppb) (analytefound(ppt)x volume extracted(0.04L)|/sample weight(5g) AnalyteFound (ppb)dry weight analytefound (ppb)x (100% /totalsolids(%)) CS = Calibrationstandard C Control sample S s Sample LF = Lab Fortifiedsample FP 3 Field fortifiedsample LCS = Laboratory ControlSpike CK = Check Standard ND Notdetected* Response between0 and25 ppt NQ * Notquantifiable= Responsebetween25 pptandLOQ (50ppt) Spreadsheet prepared by:. ,oe|oib Analyte Found (ppb) Dry Weight - - - - - 0.809 0.591 2.09 2.51 4.08 4.33 5.05 3.57 7.39 - SponsorStudy No; Exygen Study No: Analyte: loos Monitored: Site: NA L34910 PFOS 499 ->99 DecaturBaker'sCreek R A W DATA REPORT LimitofQuantitation: InjectionVolume: Matrix: Sample Weight: Final Volume: 50 ppt 154SoU 5.0 g 5.0mL SetNo: Analyst: InstrumentType: ExtractionDate: Analyzed on: 8013A Karen Risha LCMSMS #6 08/01/03 08/02/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 Methanol Wash ReagentBlank ReagentSpk A ReagentSpk B XC072503-1 L34910-5 Spk C L34910-10 Spk D L34910-11 Spk E L34910-20Spk F XC072503-2 L34910-5 L349IO-5 Rep L34910-10 L34910-10 Rep XC072503-3 XC0725Q3-4 L34910-11 L 3 4 9 1 0 - 1 1R e p L34910-20 L34910-20 Rep L34910-21 XCO72503-5 XC072503-6 Sponsor ID - na na na BC2 SED-04 BC2 SED-05 BC2 SED-06 Outfall toRiver5ED-25 BC2 SED-04 BC2 SED-04 BC2 SED-05 BC2 SED-05 - BC2 SED-06 BC2 SED-06 OutfalltaRiverSED-15 Outfall to RiverSED-25 OutfalltoRiverSED-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. 080103A-2001 080103A-2002 080103A-2003 080103A-2004 080103A-2005 080103A-2006 080103A-2007 080103A-2008 080103A-2009 080103A-20IO 080103A-20U 080103A-212 080103A-2013 080103A-2014 080103A-2015 08Q103A-2016 080103A-2017 080103A-2018 080103A-2019 080103A-2020 080103A-2021 080103A-2022 080103A-2023 080103A-2024 080103A-2025 08Q103A-2026 080103A-2027 080103A-2028 080103A-2029 080103A-2030 Std. Cone. (ppt) 0 25 50* ' 100 250 500 1000 25 50 100 250 500 1000 Dilution Peak Factor Area . 0 1018 2072 3701 9370 19171 37079 0 0 2011 17583 938 10 22878 10 26935 10 336383 10 72248 2233 60613 51074 93844 1 106350 3634 8965 1 2354673 1 1794353 1 418516 l 287933 1 409821 17108 - 32192 Recovery (%) = [analytefound (ppt)-analytcfoundincontrol(ppt)]x 100 amount added (ppt) AnalyteFound (ppb) [analyte found(ppt)x volume extracted (0.04L)]/sampleweight (5g) AnalyteFound (ppb)dry weight* analytefound (ppb)x (100% /totalsolids(%)) Analyte Found (ppO Amount Added (PPO Recovery (%) Analyte Found ND . 51.4 50 496 500 103 99 . _ 6470 5000 7620 5000 5000 5000 93* 95* * . _ . . _ . - .. - .- -- - :Linear(1/xweighted) Intercept 208.543 Slope 35.0593 Coef. Of Det.= 0.990916 Total Solids . . . , ,, . . ,, 69.96 69.96 69.54 69..54 ,, 60.41 60.41 63.27 63.27 67.43 _ - CS * Calibrationstandard C Control sample S a Sample LF 3 Lab fortifiedsample FF * Fieldfortifiedsample LCS = Laboratory ControlSpike CK * Check Standard ND a Notdetected* Response between0 and25 ppt NQ Not quantifiable* Response between 25pptandLOQ (50ppt) Analyte Found(ppb) . - Sample requires dilution. See data set 080103AR. ASamplc was corrected using the data found in set 080103AR. Spreadsheet prepared by: Sponsor Study No: Exygcn Study No; Analyte: IonsMonitored: Site: NA L34910 FOSA 493 -> 78 Decatur Baker'sCreek RAW DATA REPORT LimitofQuantitation: InjectionVolume: Matrix: Sample Weight: FinalVolume; 50 ppt 15 pL Soil 5.0 g 5.0 ml. SetNo; Analyst: Instrument Type: Extraction Date; Analyzed on: 080103A Karen Risha LCMSMS #6 08/01/03 08/02/03 Exygen ID XC072503-0 XC072503-S XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-O Methanol Wash Reagent Blank ReagentSpk A Reagent Spk B XC072503-1 L34910-5 Spk C L34910-10 Spk D L34910-11Spk L34910-20Spk F / XC072503-2 L34910-5 L34910-5 R ep L34910-10 L34910-10 Rep XC072503-3 XC072503-4 L349I0-1 1 L34910-11 Rep L34910-20 L34910-20 Rep L34910-21 XC072503-5 XC072503-6 Sponsor ID - - na na na BC2SED-04 BC2 SED-05 BC2SED-06 OutfalltoRiver 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 OutfalltoRiverSED-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. 080103A-2001 080103A-2002 080103A-2003 080103A-204 080103A-2005 080103A-2006 080103A-2007 Q8Q103A-2008 08G103A-2009 Q80103A-2010 Q80103A-2011 080103A-2012 08Q103A-20I3 080103A-2014 080103A-2015 080103A-2016 080103A-2017 080103A-2018 080103A-2019 080103A-2020 080103A-2021 080103A-2022 080103A-2023 080103A-2024 080103A-2025 080103A-2026 080103A-2027 080I03A-2028 080103A-2029 080103A-2030 Analyte Found (ppt)-- (peakarea-intercept)/slopex DF Recovery {%) - [analytefound (ppp-analyte found incontrol(ppt)1x 100 amount added (ppt) Std. Couc. (pp 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Factor 1 1 1 10 10 10 10 1 1 l 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 121882 133583 133763 191201 14698 34282 1215533 929771 412369 346884 357273 67231 129118 Analyte Found (ppt) Amount Added (ppt) Recovery (%) Analyte Found ip p b ) - - - ND 43.6 50 477 500 87 95 5810 6010 7370 5000 5000 5000 5000 98 101 77A 894 981 982 -- 7.15 7.84 7.36 - * - '- StandardCurve :Linear(1/x weighted) intercept - 849.062 Slope = 135.358 Coef. Of 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) AnalyteFound (ppb)dryweight= analytefound(ppb) x (100% /totalsolids(%)) CS 3 Calibrationstandard C = Control sample S " Sample LF = Lab fortifiedsample FF = Fieldfortifiedsample LCS = LaboratoryControl Spike CK =Check Standard ND * Not detected= Response between 0 and 25 ppt NQ =sNot quantifiable= Responsebetween 25 ppt andLOQ (50ppt) Analyte Found (ppb) Drv Weight - - - - - - 10.2 11.2 11.3 - - 'Sample requires dilution. See data set 080103AR. 'Sam ple was corrected using the data found in set 080103AR. Spreadsheetpreparedby: Analyst: V H % Work Group" 'VG46121 Analysis: S olidi Title: Send Date Prepared: 29-vt '003 ' ID Result Product Matrix DF MDLxDF CRDLxDF Flags Time Collect L34905-21 100 PERC SOLID SOLID 1 0.01 0 08-Jul-03 00:00 L34905-22 100 PERC SOLID, SOLID 1 0.01 0 OS-Jul-03 00:00 L34905-23 100 PERC SOLID SOLID 1 0.01 0 08-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 08-Ju!-03 00:00 L34905-26 100 PERC SOLID SOLID 1 0.01 0 08-Jul-D3 00:00 L34905-27 100 PERC SOLID SOLID 1 0.01 0 OS-Jul-03 00:00 L34905-28 100 PERC SOLID SOLID 1 0.01 0 08-Ju!-03 00:00 L34905-29 100 PERC SOLID SOLID 1 0.01 0 08-Jul-03 00:00 L34905-30 100 PERC SOLID SOLID 1 0.01 0 08-Jul-03 00:00 L34910-5 69.96 PERC SOLID SOLID 1 0.01 0 23-Jul-03 14:50 L34910-10 69.54 PERC SOLID SOUD 1 0.01 0 21 -Jul-03 14:15 L34910-11 60.41 PERC SOLID SOLID 1 0.01 0 23-Jul-03 15:25 L34910-2Q 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 B 1.19 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-JUI-D3 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 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-Jul-03 15:34 29-Jul-03 15:34 Client ID 200874 X3323B-32-21 200875X33238-32-22 200876 X33238-32-23 200877 X33238-32-24 200878 X33238-32-25 200879 X33238-32-26 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 Print Date: 30-Jul-03 Page 1 of 1 4 *% W o rk G ro u p :^ 46121 Analysis: Solids Title: Data KDate Prepared: 29- >03 Analyst Initials Date and Time Data Aquired (ctrl+t) AJH 29-Jul-03 15:34 AJH 29-Jul-03 16 06 AJH 30-Jul-03 08 34 C A L (D C LIE N T ID M A T R IX PAN ID PAN W E IG H T (g( S A M P L E + P A N (g) W G46121-1 W G46121-2 L3495-21 L34905-22 L34905-23 L34905-24 L34905-25 L34905-26 L34 905-27 L349U5-28 L.34905 -2 9 L3405-30 L34910-S L3491-1 L34910-11 134910-20 L34910-21 L34921-1 MB P E R C SOLID I SOLIO UP; L34910-I: PER C SO LID I SOLID 74 X33238-3 ! PER C SOLID (S O LID 75 X 3 3 238-3 :P E R C SOLID (S O LID 76 X 33238-3 P E R C S O L ID ! SOLID 77 X3323B-3 ' PER C SOLID I SOLID 78 X33238-3 PERC SOLID (S O LID 7 9 X 3 3 2 3 8 -3 ! PER C S O LID I SOLID 8 0 X 3 3 2 3 8 -3 1PER C SOLID (S O LID 61 X 3 3 2 3 6 -3 ; P E R C S O L ID t S O LID 82 X 33238-3 ' P E R C SOLID (S O LID 63 X 33236-3 PER C SOLID S O LID BC 2 SED -04 PER C SO LID 1SOLID BC2 SED -05 PER C SOLID [S O LID B C 2 SED -06 P E R C SOLID I SOLID L TO RIVER P ER C SOLID (S O LID TO R IV E R SE P E R C S O L ID ( S O L ID B A 5R 7-23 PER C SOLID ( SOLID 1 2 3 4 5 6 7 fi 9 10 11 12 13 14 15 16 l7 16 1 .2 5 7 8 1 2521 1 1 1 1 1 1.2512 1 2517 1 2578 1 2574 1.2638 1.2556 1 .2 5 7 6 4 3 .5 1 5 9 2 2 2 2 2 2 2 2 2 2 39.8338 286584 3 4 .2 0 7 3 2 3 .9 6 1 6 20 0233 4 .2 0 2 2 DRIED SAM PLE IG N ITE D S A M P LE + PAN (g) +PA N (g) % S olids o r "A T V S or % Ash 1.257B 319212 2 2 2 2 2 2 2 2 2 2 28 245 2Q .3l2t 21.1653 15.6246 13.9150 36481 0 72.56 100 100 100 100 100 10 100 100 100 1 69.96 69.54 60.41 63.27 67.43 81.19 Print Date: 06-Aug-03 Page 1 of 1 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: Soil Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. C cajo-jo*, Time /V?30 m - Initials PE- CLIENT SAMPLE ID EXYGEN ID NUMBER W EIGHT (g) FORTIFICATION (ng) 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 Reagent Blank Reagent Spk A Reagent Spk B L34910-5 Spk C L34910-10 Spk D L34910-11 Spk E L34910-20 Spk F L34910-5 L34910-5 Rep L34910-10 . . 5.0 5.0 5.0 5.0 5.0 5.0 5.0 _ 2.0 20.0 200.0 200.0 200.0 200.0 . . . BC2 SED-05 L34910-10 Rep 5.0 _ BC2 SED-06 L34910-11 5.0 . BC2 SED-06 L34910-11 Rep 5.0 - Outfall to River SED-25 Outfall to River SED-25 L34910-20 L34910-20 Rep 5.0 5.0 . _ Outfall to River SED-25 Dup L34910-21 5.0 - _ .- _ - - -- Reagent Spk A Spiking Solution Used F 06U 03-2 (10 ng/mL) Reagent Spk B F061103-1 (100 ng/mL) L34910-5 Spk C ' L34910-10 Spk D F060203-2 (1000 ng/mL) F060203-2 (1000 ng/mL) L34910-11 Spk E F060203-2 (1000 ng/mL) L34910-20 Spk F F060203-2 (1000 ng/mL) -- All samples were weighed on balance No. 2D Time _______ Date filniln 3_____ After weighing samples were returned to refrigerator No. 3 2 Time /3 O 0 _______ Date CR/Otfo^ V olum e Used for S piking 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) . Initlal/D ate /<&o i k l t - /o8|oil; ' /60bi f a t f a /Ojoljo | $ L /0 oik - Initials / 'F3 Initials /feZE C o m m e n ts : 200 pL of 230 mg/mL sodium thiosulfate was added to all samples before spildng. Initiats/Date: P F F ". I w A nalysis S um m ary: D ata Set: Inirials/D ate: ^ Data Set: A 8 6 l0 5 M 2" Data S et:_____~ _______ Inirials/Date:. ' Initials/Date: og. p4 k^> /__ - Set extraction/analysis data verified b y :. Date: m i Iuly 26, 2001/1 { KV 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 SAM PLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L34910 MATRIX: Soil METHOD: ExM-023-014 " ANALYTES: j PROTOCOL NUMBER: NA Client ID na na na BC2 SED-04 BC2 SED-OS 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 (a RiverSED-25 Dup ExygenID Reagent Blank Reagent Snk 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 L34910-10 Rep L34910-11 L34910-11 Rep L34910-20 L34910-20 Rep L34910-21 . STEP 1 STEP STEP STEP 234 __ 1___ STEP 5 >V \ 1/ > -. - sy s f - - -- - - - . - -- - - - . - ---- - *Initials/Date C&J % ceipiffi cdloloi oqoifoz tf/al/5 STEP I: Add 5mL of methanol and shake by hand for -1 minute STEP 2: Bring up to 40 mL with hypercarb filtered type I water STEP 3: Centrifuge for 10 minutes at -3000 rptn 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?: LC/MS/MS analysis STEP 8: LC/MS/MS reanalysis. STEP 6 - o b Dilutions (mL/mL) -- -- -- V |.B -V t,o f'/i.o -- -- -- -- -- -- -- -- -- - - - - STEP 7 Dilutions (mL/mL) -- -- - - STEP 8 -- -- - Reagents/ Materials Methanol Cl* SPE TypeI Water Glass acrodisc . Lot# 4 3 M 3 i6 U/3I1ZBI NA - . OAA o _ 0 X 6 -. O 'Y u D -v h 0 )*^fanikVho <> - In itia ls/D a te . - C & z cs/otlib !r - . \Z _ t - - - <9 - / L_i - - - if" . HPLC Methanol AmmoniumAcetate Type I water - - NA 1" C6lot lo b c e $ F |a cfcl3?tfc> In itia ls/D a te t>6)?i(b lU^cf lU c f|L -t> 6 ^ f c 3 /o a > SHciAhpNV. 'M.O)0 V ,.O h F - l O o ^ . O O y ^ o l k 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 3 2 - Initials: Date: M m m July 19, 2001/4 <( Masslynx - Sample List Sam ple List: C:\MASSLYNX\Fluorochesmiiccaals.HPKRUO\\tS>arm pleD 8\080103A Decatur B C.SPL Printed: Fri Aug 01 15:28:30 2003 P^Qlollo^ vial File Name LIMS ID Client ID Sample Descnption Matrix 1 41 080103A-2001 -- 2 42 080103A-2002 -- 3 43 080103A-2003 -- 4 44 080103A-2004 -- 5 45 080103A-2005 6 46 080103A-2006 -- 7 47 080103A-2007 -- 8 92 080103A-2008 -- 9 1 080103A-2009 -- 10 2 080103A-2010 -- 11 3 080103A-2011 -- 12 42 080103A-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 080103A-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 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC 072503-0, 0 ng/L Standard XC07253-1, 25 ng/L Standard XC 072503-2, 50 ng/L Standard XC072503-3, 100 ng/L Standard XC072503-4, 250 ng/L Standard XC072503-5, 500 ng/L Standard X C 0 7 2 5 0 3 -6 ,1000 ng/L Standard Methanol Wash Reagent Blank Reagent Spk A , 50 ng/L Reagent Spk B, 500 ng/L X C 0 7 2 5 0 3 -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 X C 0 7 2 5 0 3 -2 .5 0 ng/L Standard L34910-5 L34910-5 Rep L34910-1Q L34910-10 Rep X C 0 7 2 5 0 3 -3 ,100 ng/L Standard XC072503-4, 250 ng/L Standard L34910-11. L34910-11 Rep L34910-20 L34910-20 Rep L34910-21 XC072503-5, 500 ng/L Standard X C 0 7 2 5 0 3 -6 ,1000 ng/L Standard t Exygen study n o . L-Wto K 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 __0 1 ----0 1 ----0 1 -- --0 1 -- --0 1 ----0 1 ----0 1 ---- 0 1 -- -- 0 1 ----0 1 -- --0 ----0 ----0 ----0 ----0 ----0 ----0 ---- 0 ----0 ----0 1 1 10 10 10 10 1 1 1 1 -- -- 01 -- -- 01 -- -- 01 -- -- 01 -- -- 01 ---- 0 ---- 0 ---- 0 ----0 1 1 1 1 -- -- 01 <( Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemicals.PRO\SampleDB\080103A Decatur BC.SPL Printed: Fri Aug 01 15:28:30 2003 10 3 ______________________________ MS Method HPLC Method MS Tune Fite 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 C8 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 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 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 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 ACID 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 Exygen study n o . L^ . l Page 2 Page Position: (2 .1 ) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exygen Study No: L34910 Instrument: Computer: Software: HPLC Equipment: HPLC Column: Mobile Phase (A) : Mobile Phase (B) : Analyst: 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 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 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 , 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 ( 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 M ethod R e p o rt Method Filet Last Modified Printed: c:\masslynx\fluorochemicals.pro\acgudb\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(aC) 0.300 20.0 0 400 35.0 35.0 HP11Q0 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 Contactl Off Off Off On Off Off Off Off 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 (/il) Vial Number 200.0 200 0.50 20.00 15.0 69 <_ f Tuning Method Report Method: Printed: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\FLUOROCHEMS Fri Aug 01 15:29:30 2003 Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source 3iock 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 Rdbk 14.0 14.0 1.0 -2 15 2 14.0 14 .0 2.0 650 36 19 40 -648 Rdbk 131.8 751.3 Q u a n tify C a lib ra tio n R ep o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , Z x t.D a te :0 8 /0 1 /0 3 , A n a ly s ts K .R is h a Page 1 C a l i b r a t i o n : P : \ D a t a \ L C H S M S 6 \ M a s s l y n x \ F l u o r o c h e m i c a l s . P R O \ C u r v e D B \ 0 8 0 1 0 3 A D e c a t u r BC L a s t m o d ifie d : Sun Aug 03 0 7 :2 6 :0 3 2003 P rin te d : Sun Aug 03 0 7 :3 2 :2 2 2003 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R eport t ^ S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Paga 2 C a l i b r a t i o n : P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ F l u o r o c h e m i c a l s . P R 0 \ C u r v e D B \ 0 8 0 1 0 3 A D e c a t u r BC L a s t m o d ifie d : Sun Aug 03 0 7 :2 6 :0 3 2003 P rin te d : Sun Aug 03 0 7 :3 2 :2 2 2003 E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 801 Q u a n tify C a lib ra tio n R ep o rt S tu d y N o. :L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 3 C a l i b r a t i o n : P :\ D a t a \ L C M S M S 6 \ K a s s l y n x \ F l u o r o c h e m i c a l s .P R 0 \ C u r v e D B \ 0 8 0 1 0 3 A D e c a t u r BC L a s t m o d ifie d : Sun Aug 03 0 7 :2 6 :0 3 2003 P rin te d : Sun Aug 03 0 7 :3 2 :2 2 2003 E x y g en R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tify C a lib ra tio n R eport S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is b a Page 4 C a l i b r a t i o n : P : \ D a t a \ L C H S M S 6 \ M a s s l y n x \ F l u o r o c h e m i c a l s . P R O \ C u r v e D B \ 0 8 0 1 0 3 A D e c a t u r BC L a s t m o d ifie d : Sun Aug 03 0 7 :2 6 :0 3 2003 P rin te d : Sun Aug 03 0 7 :3 2 :2 2 2003 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report ^ Study No.:L34910, Set No. :080103A, Ext.Date:08/01/03, Analyst-.K.Risha Page 1 Sample List: F:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaBqpleDB\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 Initials --- oaoltftABate ce|oblo5> Run# -2 6 0 \ To O g o io A - ift Name: 080103A-2001 Text: 1: C8 Acid (PF0A) H*/ 2: C6 Sulfonate (PFHS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 2 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-2001 Text: W E x y g e n R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDBV080103A 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 (PF0A) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt . ^ S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 4 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-2002 Text: 4: PFOSA w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 5 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 Marne: 080103A-2003 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t;K .R ish a Page 6 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-2003 Text: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o. -.1,34910, S e t N o .:0 8 0 1 0 3 A , E x t .D a t e : 0 8 / 0 1 / 0 3 , A n a ly s t :K .R i s h a 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 (PF0A) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 16801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 080103A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ish a Rage 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) 100-5 %- 02-Aug-2003 03:32:27 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 150821 7.93e4 Area i i-- r-p--r r-r-T-'p-r..T r-- >| i -j , ( ,<| i i-"i i [ i r i t i i i - i | 2.00 4 .0 0 6.00 1-1 T l~'~ I 1 1 1 M 1 1 8.00 10.00 Tim e 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Rage 9 Sample List: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.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-2005 Text : 1: C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 0 8 0 1 03A -2005 Sm (Mn, 2x3) 100-1 %- 9.13 787941 I 1 02-Aug-2003 03:54:13 LC/MS/MS #6 M R M of 4 Channels ES413 >369 4.78e5 Area 0 - 1 f O ' ' 1 T 1 1 - 1 r f - 1 - i - i - |-| 1 I " . [ - 1 I - I - I 1" 1 1 1 ' I-1 1 1 1 I -1 r - r - r - ^ P r^i-T f--1 r 1 1 1 1 1 1 1 1 T im e 2.00 4 .0 0 6.00 8.00 10.00 12.00 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 080103A -2005 Sm (Mn, 2x3) 100- %- 8.98 157701 02-Aug-2003 03:54:13 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 9.57e4 Area 0 - 1 ' 1 ' I ............. ... , . 1 , ` I , . 1 1 1 . , , ! . . . 1 1 r"| ri - i - r i- i 1 i tt- > i - i 1I i t i - r i-i 1 r 1 Tim e 2.00 4.00 6 .0 0 ____________ & 0 0 ___________ 1 0 .0 0 ___________12.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 080103A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Rage 10 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-2005 Text : 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a W Page 11 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\Fluorocheiaicals.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) 100-1 %- 9.12 171634 02-Aug-2003 04:15:54 LC/MS/MS #6 M R M of 4 Channels ES413 >369 1.01e6 Area 2.00 4.00 2: C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 080103A -2006 Sm (Mn, 2x3) 100i %- 6.00 8.00 8.98 31281 r",~r r 10.00 Tim e 12.00 02-Aug-2003 04:15:54 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 1.90e5 Area 0 1 ''' 2.00 'I 1-r 1 4.00 3: C8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 080103A -2006 Sm (Mn, 2x3) 100n 6.00 8.00 10.00 t - i Time 12.00 9.24 19171 02-Aug-2003 04:15:54 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 1 .1 1e5 Area Vi r ;r r \ i I I T r . I I I i r | 2.00 4 .0 0 6.00 1I1111r 8.00 10.00 i Time 12.00 E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o. :L 34910, S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P ag e 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SainpleDB\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-2006 Text: 4: PFOSA XC072503-5, 500 ng/L Standard 080103A -2006 Sm (Mn, 2x3) 10(H %: 02-Aug-2003 04:15:54 LC/MS/MS #6 M R M of 4 Channels ES- 9.92 498 > 78 3.82e5 Area O ' ' 11I 1 11I ' 2 .0 0 ' T ' T-1 -T- | -V 4.00 W ' I-1' 6.00 1I11 8.00 t-- I-- 10.00 I Time 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt W S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 080103A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P ag e 13 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\Masslymc\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-2007 Text: 1: C8 Acid (PFOA) XC072503-6,1000 ng/L Standard 080103A -2007 Sm (Mn, 2x3) 100i %- 9.13 3157681 I i 02-Aug-2003 04:37:34 LC/MS/MS #6 M R M of 4 Channels ES413 >369 . 1.84e6 Area 0 - ' ' ' ' I , _ l ' I ' 1 ' ' 1 ............. T ! 2.00 4.00 1' 1' 11 1-l 1 ' i - it- 1 1 ' 1 - r ' T - , - n T im e 6 .0 0 __________80___________ 10 .0 0 ___________12.00 W 2: C6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 080103A-2007 Sm (Mn, 2x3) m r\_ %: 8.98 583081 1 [ 02-Aug-2003 04:37:34 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 3.49e5 Area o - 'r 1 *"I I I I ' 1--1--1--1--1--1--n --i-- i-- i----r"i--1----1--r 1 - t 1--11 I ' I" "1 - . . - 1 ' ' ' ' 1 ' '' 1 Tim e 2.00 4 .0 0 _________6 ,00____________ 8X30___________ 10 ,0 0 ___________12.00 3: C8 Sulfonate ( P F OS) XC072503-6,1000 ng/L Standard 080103A -2007 Sm (Mn, 2x3) 100-1 %- 02-Aug-2003 04:37:34 LC/MS/MS #6 9.25 M R M of 4 Channels ES499 > 99 2 .1 2e5 Area 0"--n -- I-- I-- I-- I--i--i-- I-- I-- r 2.00 %0 "r I 1 1 ' I ' ' 1 1 7 1 4 .0 0 6.00 8.00 10.00 T i- i Time 12.00 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 Quantify Sample Report . , Study No. :L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 14 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-2007 Text: 4: PFOSA XC072503-6,1000 ng/L Standard 080103A -2007 Sm {Mn, 2x3) 100-, %- 02-Aug-2003 04:37:34 LC/MS/MS #6 M RM of 4 Channels ES- 9.92 498 > 78 137821 7.22e5 Area a 2.00 4 .0 0 6.00 10.00 T im e 12.00 B x y g en R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3491Q , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ia h a P age 15 Sample List: P:\Data\LCMSMS6\Masslynx\7luorochemicals.PRO\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 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 07:32:25 2003 Name: 080103A-2008 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R iB h a Rage 16 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\Hasslynx\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: w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P ag e 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SainpleDB\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) Vw/ 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) B x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sem ole R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P ag e 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\Fluorochemieals.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: E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 19 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-2010 Text: 1: C8 Acid (PF0A) Reagent Spk A, 50 ng/L 080103A -2010 Sm (Mn, 2x3) 10Ch %~ 9.13 02-Aug-2003 05:42:42 LC/MS/MS #6 M R M of 4 Channels ES413 >369 1.12e5 Area 0~ T*i i i i-r I-|' i i i i ) r"i i i-- |--t I-- I I"I It"t r I It 2.00 4 .0 0 6.00 2: C6 Sulfonate (PFHS) 8.00 -r-r-T -r-r-T -r Time 10.00 12.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o. :I>34910, S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P age 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\SampleDB\Q80103A 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-2010 Text: 4: PFOSA %0 E x y g en R e s e a rc h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 lWUMl4.ll Q u a n tif y S am ple R e p o rt ^ S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SamgpleDB\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: 1: C8 Acid (PFOA) Reagent Spk B, 500 ng/L 080103A-2011 Sm (Mn, 2x3) 100i %- 02-Aug-2003 06:04:23 LC/MS/MS #6 M R M of 4 Channels ES- 9.15 413 >369 1630631 9.90e5 11 Area 0- ^ m --. . C . r i r-r i i i i 1i i i i t | r i r i i i i r 1 1t "1 r i 1 " 1 F 1 1 i 1 1 r 'i - i - i t , i--! Tim e ___________________ ZOO____________ 4 0____________ Q M ____________ Z 0 0 ___________ 10.00___________ 12.00 2: C6 Sulfonate (PFHS)_________________________________________________________________ Reagent Spk B, 500 ng/L 02-Aug-2003 06:04:23 LC/MS/MS #6 0 80103A -2011 Sm (Mn, 2x3) m n-. %: M R M of 4 Channels ES- 8.99 11310001 399 > 80 1 .8 3 e 5 Area o -L | ~'"' , I 'i-T- l-T-l-T1"1 l-'l 1~1 |-r |-| 11' IT-1 -- 1 1 1 ' ' ' 1 1 1 ' ' ' 1 2.00 4 .0 0 6.00 8.00 *--1 t i ' ...... i i-' r~1 i T im e ___1 0 .0 0 _________ 12.00 3: C8 Sulfonate (PFOS) Reagent Spk B, 500 ng/L 080103A-2011 Sm (Mn, 2x3) 100n %: 02-Aug-2003 06:04:23 LC/MS/MS #6 9.25 M R M of 4 Channels ES499 > 99 1.05e5 Area 0 |' 1 ' I 1 IT " I -r i t- i |- | i ' 1 1 I 1 2 .0 0 4.00 T " 16.00 8.00 r ' "'--r' n Tim e 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A f E x t,D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a 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.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: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S a t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Faga 23 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.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 (PF0A) 3: C8 Sulfonate (PFOS) E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 24 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-2012 Text : 4: PFOSA E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.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-2013 Text: 1: C8 Acid (PF0A) 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 M RM of 4 Channels ES413 >369 9.32e5 Area 0 I I | I l"l I | I I I ! | II 2.00 4.00 2: C6 Sulfonate (PFHS) L34910-5 Spk C, 5000 ng/L, DF=10 080103A -2013 Sm (Mn, 2x3) 10(h %- 6.00 " I T-1' T~7'" 8.00 8.98 30746 10.00 Tim e 12.00 02-Aug-2003 06:47:56 LC/MS/MS #6 M RM of 4 Channels ES399 > 80 1.76e5 Area 2.00 3: C8 Sulfonate (PFOS) '1 1 i 1 4 .0 0 6.00 1 Time 8.00 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report . ^ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Faga 26 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.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: 060103A-2013 Text : 4: PFOSA L34910-5 Spk C, 5000 ng/L, DF=10 080103A -2013 Sm (Mn, 2x3) 1 0 0 -] %: 1 1 ' 1 ' ' 1' T - r '1-- 1 -1 1 i 1 1 i 1 1 1 1 2 .0 0 4.00 02-Aug-2003 06:47:56 LC/MS/MS #6 M RM of 4 Channels ES- 9.90 498 > 78 795171 4.18e5 ,,A1 1-1 ........................ [-- l-- T-- T-- T - T - r -- i-- r 6 .0 0 8 .0 0 1 0 .0 0 Area t -| Time 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 27 Sample List: P:\Data\LCMSMS6\Hasslynx\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-2014 Text: 1: C8 Acid (PFOA) L34910-10 Spk D, 5000 ng/L, DF=10 080103A -2014 Sm (Mn, 2x3) 100-1 %- 02-Aug-2003 07:09:35 LC/MS/MS #6 M RM of 4 Channels ES413 >369 9.88e5 Area 2.00 1I111 4.00 2: C6 Sulfonate (PFHS) L34910-1Q Spk D, 5000 ng/L, DF=10 080103A -2014 Sm (Mn, 2x3) 100n %- 6.00 io!oo -T-i Tim e 12.00 8.98 321921 02-Aug-2003 07:09:35 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 1.89e5 Area 0 - ' ' ' * i ' ' ' ' 1 ' ' 1 1 1 1 ' 1 ' 1"T" '1 ' ' 1 1 | 1 ' ............. i ' ' 1 -r-i i r i i i" i | -. , , . , Tim e 2.00_________ 4^00_________ 6^00_________ 8.00_________ 10,00 ________12.00 3: C8 Sulfonate (PFOS) 1 i 1 E x y g en R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 8 0 1 Quantify Sample Report Jl* Study No.:L34910, Set No.:080103A, Ext .Date: 08/01/03, Analyst:K.Risha Page 28 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\0B0103A Decatur BC Last modified: Sun Ang 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-2014 Text: 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 801 Q u a n tify Sam ple R e p o rt % m l0 S t u d y N o . .-1 ,3 4 9 1 0 , S e t N o . : 0 8 0 1 0 3 A , E x t . D a t e : 0 8 / 0 1 / 0 3 , A n a l y s t : K . R i s h a R age 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.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 : 1: C8 Acid (PFOA) L34910-11 Spk E, 5000 ng/L, DF=10 080103A -2015 Sm (Mn, 2x3) lOOn %: 9.13 1876661 02-Aug-2003 07:31:17 LC/MS/MS #6 M R M of 4 Channels ES413 >369 1.11 e6 Area o- ' ' ' T 1" 1 1 T 1 2 .0 0 1 1 !' 1 l-l 1T 1 1 1 1 i 1 1 1 1 i 1 1 1 1 TM 1-- i i i ' T - t -- r - |- r i i T ' T im e 4 .0 0 6 .0 0 8.00 10.00___________ 12.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt , ^ S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P ag e 30 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur -BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCUSMS6\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 M R M of 4 Channels ES- 9.88 15509C 498 > 78 7.93e5 Area 0 V 2.00 4.00 T--T--'--'r - T - f- f 6.00 r 1 1 ' 1 I ............ r - | 8.00 1 10.00 -r-i Time 12.00 w E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ia h a Page 31 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-2016 Text: 1: C8 Acid (PF0A) L34910-20 Spk F, 5000 ng/L, DF=10 080103A -2016 Sm (Mn, 2x3) 100n %: 02-Aug-2003 07:52:54 LC/MS/MS #6 9.13 M R M of 4 Channels ES413 >369 1.02e6 Area O ' . . . T ' 1' -1' 1 T 1 1 ' I 1 1 1 I 1 ' r~ i t~' ...... . r1 2.00 4 .0 0 6.00 2: C6 Sulfonate (PFHS) T 8.00 ' I ............... .. ) Tim e 10.00 12.00 J i 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report 1*/ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 32 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SainpleDB\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: 4: PFOSA L34910-20 Spk F, 5000 ng/L, DF=10 080103A -2016 Sm (Mn, 2x3) 100n %- 02-Aug-2003 07:52:54 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 >78 100640^ 5.19e5 Area T im e 2.00 4.00 6.00 8.00 10.00 12.00 %0 E x y g en R e s e a rc h . 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No. :L34910, Set No.:080103A, Ext .Date: 08/01/03, Analyst:K.Risha Paga 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 Code: Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2017 Text: 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report '>*/ Study No.:L34910, Set No.:080103A, Bxt.Date:08/01/03, Analyst:X.Risha Page 34 Saiaple 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-2017 Text : 4: PFOSA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 16801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P age 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-2Q18 Sm (Mn, 2x3) 10CH %- 02-Aug-2003 08:36:27 LC/MS/MS #6 M R M of 4 Channels ES- 499 > 99 3.58e5 Area O' '1-- r_1-- 1-- I-- -- I-- I-- I-- I-- I-- I-- I-- I-- '-- i-- I-- I-- 1-- r 2.00 4.00 6.00 8 jOO 10.I00I ' I I I I I1I2-1.0T0ime E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report )._Study No. :L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 36 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheinicals.PR0\SainpleDB\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-2018 Text: 4: PFOSA L34910-5 080103A-2018 Sm (Mn, 2x3) 1 0 0 -j %: 02-Aug-2003 08:36:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 121882 1 498 > 78 6.28e5 Area 0 ................................ I T - | -- 2.00 - i - l - T " | - i " i - r - i - r ' 1- 1- n - | - I - 4.00 6.00 8.00 10.00 Time 12.00 E x y g en R e s e a rc h , 3058 R e s e a rc h D riv e , S ta t e C o lle g e , PA 1 6 801 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s ts K .R is h a P ag e 37 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-2019 Text: 1: C8 Acid (PFOA) L34910-5 Rep 080103A-2019 Sm (Mn, 2x3) 100-] /<r 9.13 827621 1 [ 02-Aug-2003 08:58:12 LC/MS/MS #6 MRM of 4 Channels ES413 >369 4.81e5 Area CH 11 "i iMpr,ir,ii i i t,mTt t -i 'r ti i i i r i 11r"r m . | >i i i 1--iT"i1r p' "i " r r ^ .....................i"' 1 1 1 i Time 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-5 Rep 080103A-2019 Sm (Mn, 2x3) HA A _ %- 0- 2.00 4.00 02-Aug-2003 08:58:12 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 I510741 1 3.06e5 Area 1 i 1 1 1 '"1 11 i ' ^ < 1 i 1 1 1 1 i ' i ' ' i Time 6.00__________ 8^00_________ 10.00_________ 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:08Q103A, Ext.Date:08/01/03, Analyst:K.Risha w Page 38 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\MethD3\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 L34910-5 Rep -,0 8 0 1 0 3 A -2 0 1 9 Sm (Mn, 2x3) 100 %- 02>Aug-2003 08:58:12 LC/MS/MS #6 M R M of Channels ES- 9.88 498 > 78 6.93e5 Area Q -l-, , r..r n r . r - , 2.00 ... 4.00 6.00 8.00 10.00 i ' ' i Time 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 39 Sample List: P:\Oata\LCHSMS6\Masslynx\Fluorochemicals.PR0\SanqpleSB\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: 1: C8 Acid (PF0A) L34910-10 080103A -2020 Sm (Mn, 2x3) 100-] %- 02-Aug-2003 09:19:59 LC/MS/MS #6 I9.13 1950551 M R M of 4 Channels ES413 >369 1.13e6 Area 1 Ch 1 1 1 1 I ' 1 ' ' r .............! 1 1 1 1 1 ' ' 1 I"1 1 ..... I"'1' ~l" ' 1 . ^ 2.00 4 .0 0 6.00 8.00 I ' r . |-i i - . 'i -| T im e 10.00 12.00 2: C6 Sulfonate (PFHS) L34910-10 080103A -2020 Sm (Mn, 2x3) 100n %- 8.97 108961 I 02-Aug-2003 09:19:59 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 6.71 e4 Area 0- 1 l '' 1 1 1 I 1 1 1 1 I .......... I I - ! L-l-l-1- ' 11 ........ ' r r 1 11 1 1 '"i -i-i r - iT 1--1 1 1 1 1 1 1 1 T im e 2.00 4.00 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o.:L 3491Q , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s tK .R is h a P age 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 %: 02-Aug-2003 09:19:59 LC/MS/MS #6 M RM of 4 Channels ES- 9.91 498 > 78 1337631 6.89e5 Area A- ' ' ' I . . . . , I 1 1 I 2.00 4.00 --1--'--'--'--1------'-->--1 6.00 8.00 1 1 1--1 1 1 1 1 1 1 1 1 1 Time 10.00 12.00 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 5 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o. :L 34910, S e t N o. : 080103A , E x t .D a te :0 8 /0 1 /0 3 , A n a ly st.-K .R ish a Page 41 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-2021 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) L34910-10 Rep 080103A-2021 Sm (Mn, 2x3) 10O i %1 8.98 12999 02-Aug-2003 09:41:47 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 7.94e4 Area o 2.00 3: C8 Sulfonate (PFOS) L34910-10 Rep 080103A-2021 Sm (Mn, 2x3) 100; %- 4.00 I ~,~ i 6.00 8.00 1 T . , i..| i-.| , I 10.00 12.0T0im e 9.24 1063501 1 1 02-Aug-2003 09:41:47 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 6.22e5 Area 0 - , 1 r"TMr'1 11 1 1 --T"' 1r 1 -r-i -i--r i T" i r i > [ i i"T 1---IT -! r-| 1-1 1~I" 1 ' 1 ' ' 2.00 4.00 6.00 8.00 10.00' 'I ' ' ' t 1' - f '-T"! Tim e 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Pape 42 Sample List: P:\Data\LCMSMS6\Masslynx\71uorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: F:\Data\LCMSMS6\Masslynx\FluorochemicalSiPR0\MethDB\Decatur BC 0S0103 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 02-Aug-2003 09:41:47 LC/MS/MS #6 080103A-2021 Sm (Mn, 2x3) 100] M R M of 4 Channels ES- 9 .9 0 498 > 78 1912011 9 .9 2 e 5 A rea %' nL r ................... .... 1-1 T 2 .0 0 1 1 --T- V 1 ---1--J - T - I T T ] 1 1 1 1 I 1 1 1 1 4 .0 0 6 .0 0 1 r ~1 1 i 1 1 8 .0 0 11 1 1 1 ' 1 ' I r-| h 1 0 .0 0 ^ 1 1 I im e 1 2 .0 0 E x y g a n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o. : 080103A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a w R age 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: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) E x y g en R e s e a r c h , 3 058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 16801 Quantify Sample Report w Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Rage 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) 1 0 0 -1 %- 02-Aug-2003 10:03:27 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 1469 7.86e4 Area 0 -l r 1 I I I I I l~ 1 T I "I T I 1 I p i " I ________ 2.00 4.00 ; i i i r T --i - r r p 6.00 8r .0n 0 < t .......... 10.00 "n Time 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ish a Page 45 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-2023 Text: 1: C8 Acid (PF0A) 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 080103A -2023 Sm {Mn, 2x3) 10CH %- . CH r 1 ~I 1 1,1 1 r~i~ --1i "1 1 1 r 1 `~r"' 1 2 .0 0 __________ 4 .0 0 6 .0 0 3: C8 Sulfonate (PFOS) 8.98 [148011 I 02-Aug-2003 10:25:10 LC/MS/MS #6 M RM of 4 Channels ES399 > 80 9.02e4 Area 1`"1 1 T' ` I- 1 8.00 ~r" 1 . I . . I I I ) Tim e 10.00 _____ 12.00 E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 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 E x y g e n R e s e a rc h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 080103A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P age 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\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-2024 Text: 1: C8 Acid (PFOA) L34910-11 080103A -2024 Sm (Mn, 2x3) 100- %- 9.12 4734161 1 1 02-Aug-2003 10:47:05 LC/MS/MS #6 M RM of 4 Channels ES413 >369 2 .8 8 e 6 Area o - 1 1 1 1 I 1 ................ ...-- r r 1 1 ' 1 1 1' 1 -, , T- , r-, ,-r , , r " I 1 r 1 r 1 ' 1 Time ___________________ 2 ,0 0 ____________ 4 0 0 ____________ a 0 0 ____________ 8 jOO___________ 1 0 .0 0 ___________12.00 2: C6 Sulfonate (PFHS)_____________________________________________________________________ L34910-11 02-Aug-2003 10:47:05 LC/MS/MS #6 080103A -2024 Sm (Mn, 2x3) 100- 8.96 181331 I M R M of 4 Channels ES399 > 80 1.03e5 Area %- 0 - ^ ' 1 1 ............................................................ ...... . 1 1 1 1 - J - - I -I-- 1 T-- I i-- r 1 1 1 1 1 1 1 ' 1 1 ' 1 1 1 1 '' 2.00 4 .0 0 6.00 8.00 3: C8 Sulfonate (PFOS) I I I I 'I I-' ' ' I Tim e 10.00 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:Ii34910, Set No.:080103A, Ext.Date:08/01/03, AnalystsK.Risha Pape 48 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-2024 Text: 4: PFOSA L34910-11 080103A -2024 Sm (Mn, 2x3) 10C H %- 02-Aug-2003 10:47:05 LC/MS/MS #6 M RM of 4 Channels ES- 9.90 498 > 78 1215533 I 6.18e6 Area \^ 0 0 1 ' I ^ 'l T 1 T l ' ' I ............... I 1 2 .0 0 4.00 6.00 8.00 10.00 Tim e 12.00 w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o. :L 34910, S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a 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\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-2025 Text: 1: C8 Acid (PFOA) L34910-11 Rep 080103A-2025 Sm (Mn, 2x3) -mn-, %- 02-Aug-2003 11:08:44 LC/MS/MS #6 I9.12 4630171 M R M of 4 Channels ES413 >369 2.77e6 Area 1 O1 .................................................................... ........ "1 1 |M i n - T - f -- i n r i r T1 I [ 1 I 1 i 1 r -1 2.00 4.00 6.00 r - r r r""!-- r . . ^ 8.00 `I ' ' ' I ' ' j - 1 1 10.00 ' ' 1 Time 12.00 i m * 2: C6 Sulfonate (PFHS) L34910-11 Rep 080103A-2025 Sm (Mn, 2x3) 100- %: 8.96 192031 1 1 02-Aug-2003 11:08:44 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 1.09e5 Area 0 - 1 1 ' 1 1 ........... 2 .0 0 4 .0 0 6.00 8 .0 0 - 1 1 - 1 r . i T T - p . ....... -I Tim e 10.00 12.00 3: C8 Sulfonate (PFOS)_______________ ^_________________________________________________________ L34910-11 Rep 02-Aug-2003 11:08:44 LC/MS/MS #6 080103A -2025 Sm (Mn, 2x3) M RM of 4 Channels ES- ` " 499 > 99 1.00e7 Area T-i11 ~' ' ' ' I ' ' -i T im e 2 .0 0 4.00 6.00 8.00 10.00 12.00 % r ----------------------------------------------------------------------------------------------- E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:Q8/01/03, Analyst:K.Risha v Rage 50 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-2025 Text : 4: PFOSA B x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study NO.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 51 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Decatur BC Last modified: Sun Aug 03 07:25:44 2003 Method: P:\Data\LCHSMS6\Masslymc\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-2026 Text: 1: C8 Acid (PFOA) L 34910-20 080103A -2026 Sm (Mn, 2x3) m ru %- 9.12 4042091 0 2 -A u g -2 0 0 3 11:30:26 L C /M S /M S #6 M R M of 4 Channels ES- 413 >369 2.37e6 Area 0- L~l" r 1 1T~' 1 1 1 1 ' ' T 1 '" j '1 1 '' ' 1 ~l r rT - ' 1 '* r~l ' T " 1 1-1 1 1 1 11 1 TM "f-1 i | i i i i | i j i | Tim e 2.00 4 .0 0 6.00 8.00 10.00 12.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) L34910-20 080103A-2026 Sm (Mn, 2x3) 100i %: 0 " 1 1 i" ' 1 1 11 i~ ,i" 1 ' 1 r ' 1 .... . i " 1" 2.00 4.00 6J30 9.25 418516 02-Aug-2003 11:30:26 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 2.35e6 Area 1r 8.00 10.00 - n Time 12.00 Z x y g en R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tif y Sam ple R e p o rt Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:X.Risha R age 52 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-2026 Text: 4 : PFOSA L34910-20 080103A -2026 Sm (Mn, 2x3) 100-1 %- 02-Aug-2003 11:30:26 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 412369 2.10e6 Area & T ' - r " 1" < V 1 10.002.00 4.00 6.00 8.00 ' - I Time 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P ag e 53 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: Sim Aug 03 07:32:25 2003 Name: 080103A-2027 Text: 1: C8 Acid 1PF0A) L34910-20 Rep 080103A -2027 Sm (Mn, 2x3) m n-. %- 9.13 3012011 1 [ 02-Aug-2003 11:52:11 LC/MS/MS #6 M RM of 4 Channels ES413 >369 1,76e6 Area 0-L"1` 1 1 1 1 1 ' 1 1 ' i 1 ' i ' T"1 r~i' r~T" 1~r' r i-r-r-r r i | 'i 'i r" i- i 2.00 4 .0 0 6.00 8 .0 0 `r i i ' ' I - 1 ...... - i Tim e 10.00 12.00 2: C6 Sulfonate (PFHS) L34910-20 Rep 080103A -2027 Sm (Mn, 2x3) m n -, % 8.97 166491 1 1 02-Aug-2003 11:52:11 LC/MS/MS #6 M RM of 4 Channels ES399 > 80 9.68e4 Area "r">o - r - r ' i - ' i- i i ) i i i i 1 j ................... i - i i -| 1 i -i i i - 1 r i i t t r i r i I i' t t ^ T "y- i- i -'i i t- t--i 1 i--r i -r i T im e 2 .0 0 4 .0 0 6.00 8.00 10.00 12.00 3: C8 Sulfonate (PFOS) L34910-20 Rep 080103A -2027 Sm (Mn, 2x3) 1 0 0 -] /c r 02-Aug-2003 11:52:11 LC/MS/MS #6 9.25 M RM of 4 Channels ES499 > 99 1 .6 8 e 6 Area 0 - i > ' i 2.00 r 1 ' 1 i 1 4.00 1 'I 1 T 6.00 T "'l T 8.00 10i.00 > I I I I 1r2I.0T0ime E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 1 6 801 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 54 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-2027 Text: 4: PFOSA E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ia h a Page 55 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 Marne: 080103A-2028 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) L34910-21 080103A -2028 Sm (Mn, 2x3) 100- %: 8.98 361721 02-Aug-2003 12:13:52 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 2.11e5 Area 0^ 1 i i 1 i i 1 1 1 r"1 1 V I J . - i . 2.00 4 .0 0 6.00 | . 1 1 . | . i ^ P l --1i~|` i 8.00 10.00 -, Tim e 12.00 3: C8 Sulfonate (PFOS) L34910-21 08 0 1 03A -2028 Sm (Mn, 2x3) 10Ch %1 9.25 4098211 1 02-Aug-2003 12:13:52 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 2.39e6 Area 1 Ch--r 1-1-I r"< 1 1 1 T' 1 t 1 1 1-r 1 11 r--[--1--1r - r - 'i r - r i f i i t i i i i t i | 2.00 4 .0 0 6.00 8.00 i t -, 10.00 i ----I Tim e 12.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.-.L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 56 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-2028 Text: 4: PFOSA w E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P ag e 57 Sample List: F:\Data\LCMSMS6\Masslynx\FluorocheraicalS.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) 1 nru %: 9.13 140009"! 1 1 02-Aug-2003 12:35:39 LC/MS/MS #6 M RM of 4 Channels ES413 >369 8.49e5 Area cy 1 1 ' I I ' ' ' ' I 1 1 1 1"i-1' M| 1 1 1 1 1 1 l~ r~1 r T 11,1 1 ' T 2.00 4 .0 0 6.00 8.00 f "" ' I ' 1 I ' 1 ' ' I 1 1 Tim e 10.00 12.00 2: C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 080103A -2029 Sm (Mn, 2x3) lO O n % -j 8.98 02-Aug-2003 12:35: LC/MS/MS #6 M R M of 4 Channels ES399 > 80 1.72e5 Area 0 1 'I r-- r-r-- r-- |-- r-- i-- i-- i-- |-- i-- i-- i-- i-- |-- r- 2.00 4 .0 0 3: C8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 080103A -2029 Sm (Mn, 2x3) 100n %- 6.00 T 8.00 1'0.I00 I I I I I ' ' 1' 2.I0T0im e 02-Aug-2003 12:35:39 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 1.02e5 Area 0 ^t n < ~ T I ' I ' I I I I I IMi I ; t 2.00 I I-- i - 4.00 T " ' r ~i' 1 6.00 10.i"0T0T - T i- i I I ' 1I21.I0T0ime E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha V Page 58 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-2029 Text : 4: PFOSA XC072503-5, 500 ng/L Standard 080103A -2029 Sm (Mn, 2x3) 100i %- 02-Aug-2003 12:35:39 LC/MS/MS #6 M R M of 4 Channels ES- 9.88 67231 498 > 78 3.54e5 Area 0- 1 I 1" ' 1 r- I I i , I I I , - I T 10.00 12.002.00 4.00 6.00 8.00 -T-i Tim e %0 E x y g e n R e s e a r c h 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P age 59 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-2030 Text: 1: C8 Acid (PFOA) imi* 2; C6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 0 80103A -2030 Sm {Mn, 2x3) 100] %- 8.98 541981 I 1 02-Aug-2003 12:57:26 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 3.29e5 Area 0 - 1 1 ' I 1 * ' 1 I * 1 I 1 ! -- r-T-- r- I--r 1 1 ' ' [ 1 ' 1 - f 1-- r--T--r - 1--1- r --r -r-- . - 2.00 4.00 6.00 8.00 - ' I ' ' ' I > ' ' ' I Tim e 10.00 12.00 3: C8 Sulfonate (PFOS) E x y g en R e s e a r c h , 3058 R e s e a rc h D r iv e , S t a t e C o lle g e , PA 16801 Q u a n tify S am ple R e p o rt V S tu d y N O .:L 3 4 9 1 0 , S e t N o .:0 8 0 1 0 3 A , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Rage 60 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: 4: PFOSA w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Sponsor Study No: Exygen Study No: Analyte: loos Mooitored: Site: NA L34910 PFOA 413->369 Decatur Baker1! 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: 080103AR Karen Risha LCMSMS #6 08/01/03 08/04/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 L349I0-II SplcE L34910-11 Spk E L34910-20 Spk F L34910-5 L34910-5 Rep L34910-10 L349UM0 Rep XC072503-1 XC072503-2 L34910-11 L34910-11 Rep U 49lO .ll L349I0.11 Rep L34910-20 U 4910-20 Rep XC072303-3 XC072503-4 L34910-20 U 49I0-20 Rep L349L0-21 L34910-21 XC072503-5 XC072503-6 Sponsor ID BC2SED-06 BC2 SED-06 Outfall to River SED-25 BC2SED-04 BC2 SED-04 BC2 SED-03 BC2 SED-05 . BC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 SED-06 Outfall to River SED-23 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 5 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 080103AR-306 080103AR-307 080103AR-308 0S0I03AR-309 080103AR-310 080103AR-311 080103AR-312 080103AR-313 080103AR-314 080103AR-315 080103AR-316 080103AR-317 080103AR-318 080103AR-319 080103AR-320 080103AR-321 0801Q3AR-322 080103AR-323 080103AR-324 080103AR-325 080103AR-326 080103AR-327 080103AR-328 080103AR-329 080103AR-330 Analyte Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)l x 100 amount added (ppt) Std. Cone. (ppo 0 25 30 100 250 500 1000 25 50 too 250 500 1000 Dilution Factor - - 1000 100 100 10 10 10 10 100 100 10 10 100 100 10 10 100 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 Amount Added (ppo Recovery (%) Analyte Found (ppb) ** 5000 * 5000 5000 * * ** * 1780 1700 * * 1340 949 2210 - 14.24 13.60 - 10.72 7.39 - 17.68 Standard Curve: Linear (1/x weighted) Intercept * 2443.00 Slope = 438.457 Coef. Of D et 0.990236 Total Solida (%) - - - 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 (S 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) Dry Weight . - - 23.6 22.5 16.9 12.0 - 26.2 - 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. Sponsor Study No: Exygen Study No: Analyte: loos Monitored: Site: NA L34910 PFOS 499 -> 99 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 15 pL Soil 5.Q g 5.0 mL Set No: Analyst Instrument Type: Extraction Date: Analyzed on: 080103AR Karen Risha LCMSMS #6 08/01/03 08/04/03 % 0 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 L349IO-11 Spk E L34910-U SpkE L34910-20 Spk F L349I0-5 L34910-5 Rep L34910-10 L34910-10 Rep XC072503-1 XC072503-2 L3490-11 L34910-I1 Rep L34910-11 L34910-11 Rep L34910-20 L34910-20 Rep XC072503-3 XC072503-4 L34910.20 L34910-2Q Rep L34910-21 L34910-2I XCQ72503-S XC072503-6 Sponsor ID BC2 SED-06 BC2 SED-06 Outfall to River SED-25 BC2 SED-04 BC2SED-04 BC2SED-05 BC2SED-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 RiverSED-25 Dup - Sample Code CS CS CS CS CS CS CS LF LF LF s s s s CS CS s 5 s s s 5 CS CS s s s s CS CS Run No. 080103AR-301 080103AR-302 0B0103AR-303 080103AR-304 080103AR-305 O801O3AR-3O6 080103AR-307 080103AR-308 080103AR-309 080103AR-310 080103AR-3I1 080103AK-312 080103A.R-313 080103AR-314 08013AR-315 080103AR-316 080103AR-317 080103AR-318 080103AR-319 080103AR-320 080103AR-321 08103AR-322 080103AR-323 080103AR-324 080103AR-325 080103AR-326 080103AR-327 080103AR-328 080103AR*329 080103AR-330 Analyte Found (ppt) * (peak area - intercept) / slope x DF Recovery (%) * [analyte found (ppQ-anaiytc found in control (ppt)} x 100 amount added (ppt) Sed. Cone. (p p o 0 25 50 100 250 500 1000 25 so 100 250 500 1000 Dilution Factor 1000 100 100 10 10 10 10 - 100 100 10 10 100 100 10 10 100 10 - Peak Area 0 1442 3003 5613 11976 25896 31730 5387 51842 9506 9121 7449 14012 15401 1301 2860 66379 48518 526238 390663 6714 4609 4445 11649 65108 45122 8701 80003 24473 44784 Analyte Found tppQ Amount Added (p p q Recovery w Analyte Found (PPB) AA 19100 1830 1490 2850 3130 5000 5000 5000 * ' * 114 14.64 11.92 22.80 25.04 - -- - A* AA ** M 13400 9010 107.20 72.08 * ** ** 17500 ** - 140.00 - -- Standard Curve : Linear (1/x weighted) Intercept * 254.789 Slope = 48.3413 Coef. Of D ec* 0.991571 Total Solids w 69.96 69.96 69.54 69.54 * 60.41 60.41 60.41 60.41 63.27 6317 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 a Calibration standard C Control sample S Sample LF MLab fortified sample FF * Field fortified sample LCS * Laboratory Control Spike CK = Check Standard ND a Not detected * Response between 0 and 25 ppt NQ * Not quantifiable a 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 accommodate all compounds. The appropriate results are reported. ^S am ple requires reextraction. See data set 080603B. md3 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 yiL Soil 5.0 g 5.0 mL Set No: Analyst; Instrument Type: Extraction Date-. Analyzed on: 080103AR (taren Ristia LCMSMS M 08/01/03 08/04/03 Exygen ID XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 L349I0-II SpkE L34910-11 SpkE L34910-20 Spk F L34910-5 L34910-5 Rep L349I0-10 L34910-10 Rep XC072503-1 XC072503-2 L34910-11 U4910-11 Rep L34910-11 L34910-11 Rep U 4 9 10-20 L34910-20 Rep XC072503-3 XC072503-4 L34910-20 L34910-20 Rep L34910-21 L34910-21 X C 0 72503-5 XC072503-6 Sponsor ID - - - - - - - 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. 0S0103AR-301 080103AR-302 080103AR-303 080103AR-304 080103AR-305 080103AR-306 080103AR-307 080103AR-308 080103AR-309 080103AR-310 080103A R -311 080103AR-312 080103AR-3J3 080103AR-314 080103AR-315 080103AR-316 080103AR-3I7 080103AR-318 080103AR-319 080103AR-320 080103AR-321 080103AR-322 080103AR-323 080103AR-324 080103AR-325 080103AR-326 080103AR-327 080103AR-328 080103AR-329 080103AR-330 Analyte Found (ppt) * (peak area - intercept) / slope x DF Recovery (%) * [analyte found (ppt)-analvte found in control (ppt)] x 100 amount added (ppt) Std. Conc. >P'> 0 25 50 100 250 500 1000 25 50 L00 250 - 500 1000 Dilution FactOT 1000 100 100 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 (pp o Recovery (%) Analyte Found (PPb> -- -- - - - ** AA ** ** ** 1510 5000 5000 5000 - ---- - - 12.08 -- AA AA * * ** -- - -- - 3500 2940 4460 - 28.00 23.52 - 35.68 -- -- - - - Standard Curve : Linear ( l / x wetphtedl Intercept 610.451 Slope * 174.067 C o e f .O f D e t- 0.996985 Total Solids (%> - - 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)J / 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 Weiht - - - 17.4 - 44.3 37.2 - 52.9 - - Spreadsheet prepared by: H w u o i p n u ? "S am 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. (( Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemiicals.PHRKO)\SampleDB\080103AR Decatur BC.SPL Printed: Mon Aug 04 07:47:05 2003 l o ^ ___________________________ Vial Fite Name LIMS ID Client ID Sample Description Mai 1 41 080103AR-301 2 42 080103AR-302 -- 3 43 080103AR-303 -- 4 44 080103AR-304 -- 5 45 080103AR-305 -- 6 46 080103AR-306 -- 7 47 080103AR-307 -- 8 1 080103AR-308 -- 9 2 080103AR-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 080103AR-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 08013AR-324 -- 25 14 080103AR-325 -- 26 15 080103AR-326 -- 27 16 080103AR-327 -- 28 17 080103AR-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 -- L34910-20 Spk F, 5000 ng/L, DF=100 -- L34910-5, DF=10 -- L34910-5 Rep, DF=10 -- L34910-10, DF=10 -- L3491O-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=10 -- 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 L3491O-20, DF=10 L3491O-20 Rep. DF=10 L34910-21. DF=100 L34910-21, DF=10 XCO72503-5, 500 ng/L Standard XCO72503-6, 1000 ng/L Standard 1 Exygen study n o . L ^ i 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 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 50 100 250 500 1000 5000 5000 5000 -- -- -- -- 25 50 -- -- -- -- -- -- 100 250 -- -- -- -- 500 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 1 1 1 1 1 1 1 1000 100 100 10 10 10 10 1 1 100 100 10 10 100 100 1 1 10 10 100 10 1 1 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC.SPL Printed: Mon Aug 04 07:47:05 2003 ^ \o3> MS Method HPLC Method MS Tune File Inj.Volume 1 C 6 C8 SULF CS ACID PFOSA pfbs water 2 C 6 C8 SULF C8 ACID PFOSA pfbs water 3 C 6 C8 SULF C8 ACID PFOSA pfbs water 4 C 6 C B SU LF C8 A C ID PFOSA pfbs water 5 C6 C8 SULF C8 ACID PFOSA pfbs water 6 C 6 C8 SULF C8 ACID PFOSA pfbs water 7 C6 C8 SULF C8 ACID PFOSA pfbs water 8 C 6 C8 SULF C8 ACID PFOSA pfbs water 9 C 6 C 8 SULF C8 ACID PFOSA pfbs water 10 C 6 C8 SU LF C8 A C ID PFOSA pfbs water 11 C 6 C 8 SULF C8 A C ID PFOSA pfbs water 12 C6 C8 SULF C8 A C ID PFOSA pfbs water 13 CB C8 SULF C8 A C ID PFOSA pfbs water 14 C 6 C8 SULF C8 A C ID PFOSA pfbs water 15 C6 C8 SULF C8 ACID PFOSA pfbs water 16 C 6 C8 SU L F C8 A C ID PFOSA pfbs water 17 C 6 C 8 SULF C8 A C ID PFOSA pfbs water 18 C 6 C8 SU LF C8 ACID PFOSA pfbs water 19 C 6 CB SULF C8 ACID PFOSA pfbs water 20 C 6 C 8 SULF C8 A C ID PFOSA pfbs water 21 C 6 C 8 SULF C8 ACID PFOSA pfbs water 22 C 6 C8 SU L F C8 A C ID PFOSA pfbs water 23 C 6 C 8 SULF C8 ACID PFOSA pfbs water 24 C 6 C8 SU LF C8 A C ID PFOSA pfbs water 25 C 6 C8 SULF C8 ACID PFOSA pfbs water 26 C 6 C8 SULF C8 A C ID PFOSA pfbs water 27 C 6 C8 SULF C8 ACID PFOSA pfbs water 28 C6 C B SU L F C8 A C ID PFOSA pfbs water 29 C6 C8 SULF C8 ACID PFOSA pfbs water 30 C 6 C 8 SU LF C8 A C ID 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 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 . l ^ 10 Page 2 Page Position: (2,1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA ExVsen Study No: L34910 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: MassLynx 3.4 Build 004 HPLC Equipment: H ewlett 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 computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by:. C b /O P ^<m l? 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: Mon Aug 04 07:47:13 2003 o3 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 Method Report Method Files Last Modified: Printed: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfha 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) 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 Contactl Off Off Off On Off Off Off Off 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 (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume (pi) Vial Number 200.0 200 0.50 20.00 15.0 27 Tuning Method Report Method: C :\ M A S S L Y N X \ F L U O R O C H E M I C A L S .P R O \ A C Q U D B \ F L U O R O C H E M S 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 Flows 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 Q u a n tify C a lib ra tio n R eport S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 080103AR E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 1 Calibration: P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ F l u o r o c h e m i c a l s . P R O \ C u r v e D B \ 0 8 0 1 0 3 A R D e c a t u r BC Last modified: T u e A u g 0 5 0 7 : 3 0 : 0 0 2 0 0 3 Printed: Tue Aug 05 0 7 :3 1 :5 8 2003 Pft&tema ( W B x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R eport S tu d y N o. :L 3 4 9 1 0 , S e t N o. :080103A R , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a W Page 2 C a l i b r a t i o n : P :\ D a t a \L C M S M S 6 \ M a s s ly n x \ F l u o r o c h e m ic a l s .P R O \ C u r v e D B \0 8 0 1 0 3 A R D e c a t u r BC L a s t m o d ifie d : Tue Aug 05 0 7 :3 0 :0 0 2003 P rin te d : Tue Aug 05 0 7 :3 1 :5 8 2003 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R eport S tu d y N o .:L 3 4 9 1 0 , S e t N o. s080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st-.K .R ish a Page 3 C a l i b r a t i o n : P : \ D a t a \L C M S M S 6 \ M a s s ly n x \ F l u o r o c h e m ic a l s .P R 0 \C u r v e D B \ 0 8 0 1 0 3 A R D e c a t u r BC L a s t m o d ifie d : Tue Aug 05 0 7 :3 0 :0 0 2003 P rin te d : Tue Aug 05 0 7 :3 1 :5 8 2003 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify C a lib ra tio n R eport S tu d y N o .:L 3 4 9 1 0 , S e t N o .:080103A R , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 4 C a l i b r a t i o n : P : \ D a t a \ L C M S M S 6 \ M a s s l y n x \ F l u o r o c h e i n i c a l s . P R O \ C u r v e D B \ 0 8 0 1 0 3 A R D e c a t u r BC b a s t m o d ifie d : Tue Aug 05 0 7 :3 0 :0 0 2003 P rin te d : Tue Aug 05 0 7 :3 1 :5 8 2003 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o ll e g e , PA 168 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R iah a Page 1 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: Initials_ _ _ _ _ Data o8|ts(ty_______________________ Printed: Tue Aug 05 07:32:01 2003 Run# C&>I 3 A E i Tb cftta3At- Name: 080103AR-301 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Riaha Page 2 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-301 Text: E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaxnpleDB\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-302 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study N o .:L34910, Set No.s080103AR, Ext.Date:08/01/03, Analyst:K.Risha Ve/ Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaiipleDB\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 E x y g e n R e s e a r c h , 3058 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report 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) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.;080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 6 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-303 Text : 4: PFOSA XC072503-2, 50 ng/L Standard 080103A R -303 Sm (Mn, 2x3) 100i %- 04-Aug-2003 09:19:12 LC/MS/MS #6 M R M of 4 Channels ES- 9.90 498 > 78 1026 5.34e4 Area O-J-r w 2.00 I I-- I I I I `I I I I I C* l I I I I I I I I 4 .0 0 6.00 8.00 ..' I I 10.00 ' ' Time E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4910, S e t N o. : 080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ish a Page 7 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: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o lle g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt W S tu d y N o .:L 3 4 9 1 0 , S e t N o.:080103A R , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page B 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 080103A R -304 Sm (Mn, 2x3) 10CH %: 04-Aug-2003 09:41:00 LC/MS/MS #6 M RM of 4 Channels ES- 9-92 498 > 78 196841 1.03e5 Area 0 '`" I T- I I -[--I I I I | T I I I | I I I I | I 2.00 4.00 ' " I -r 6.00 8.00 10.00 T im e E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y No. :L 34910, S e t N o .: 080103AR, E x t.D a te .-0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 9 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-305 Text: 1: C8 Acid (PFOA) x c o : P2503-4, 250 ng/L Standard 0 8 0 1(33A R -305 Sm (Mn, 2x3) 10CH %- 9.15 1137981 04-Aug-2003 10:02:40 LC/MS/MS #6 M RM of 4 Channels ES413 >369 6.66e5 Area Lr '' ........................... I t i -i i 1 1 ' ,|" r ' ; r"1 2.00 4.00 6.00 \ 0 i 2: C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 080103A R -305 Sm (Mn, 2x3) 100-1 8.00 ^ i i ] 1 ' 1 i i r f ' * Tim 10.00 8.98 20947 04-Aug-2003 10:02:40 LC/MS/MS #6 M RM of 4 Channels ES399 > 80 1.20e5 Area 2.00 4 .0 0 3: C8 Sulfonate (PFOS) XC0-/2503-4, 250 ng/L Standard 0801 33AR-305 Sm (Mn, 2x3) 100-3 %1 6.00 8.00 10.00 T im e 9.25 119761 04-Aug-2003 10:02:40 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 6.98e4 Area ^ i - r i - p P n - i | i i i i "| i i i i | i T- i i - | 1 1 1 r "i 1 - i 1 1 1 ' ' ! 1 1 1 1 1 2.00 4.00 6.00 8.00 " i | i 1 iiTM i i " i 10.00 i ime E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 S 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o. : 080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ish a P age 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.PR0\HethDB\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 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt V S tu d y N o .:L 3 4 9 1 0 , S e t N o .: 080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 11 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\MathDB\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: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Q u a n tif y S am ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o.:080103A R , E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ia h a P ag e 12 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-306 Text: 4: PFOSA Z x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r iv e , S t a t e C o ll e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 13 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-307 Text: 1: C8 Acid (PFOA) XC072503-6,1000 ng/L Standard 080103A R -307 Sm (Mn, 2x3) 10CR %: 9.13 4699941 04-Aug-2003 10:46:08 LC/MS/MS #6 M R M of 4 Channels ES413 >369 2.69e6 Area o -U - ' - i -i p m i ! - r T - T - r - r -- i--r--t -r T- i - r - i - i | - r -r i- i - | - ' 1' '* T r 1" '" 1 2.00 4.00 6.00 8.00 ' V '"i 10.00 -! Tim e 3: C8 Sulfonate (PFOS) XC072503-6, 1000 ng/L Standard 080103A R -307 Sm (Mn, 2x3) 100n %: 0 J - '" ` ' ' | I- I 1-1 -> r r r i - i T T T - j - T - T 2 .0 0 4.00 T 6.00 04-Aug-2003 10:46:08 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 2.90e5 Area 10.00 T im e E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt Study N o .:L3491Q, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Riaha P ag e 14 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: 080103AK-307 Text : 4: PFOSA XC072503-6,1000 ng/L Standard 080 1 03A R -307 Sm (Mn, 2x3) 10Ch %- 04-Aug-2003 10:46:08 LC/MS/MS #6 M RM of 4 Channels ES9.91 4 9 8 > 78 9.27e5 Area & T- Time 2.00 4.00 6.00 8.00 10.00 E x y g e n R e s e a r c h / 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 5 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o. : 080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a Page 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaunpleDB\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-308 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt S tu d y N o. :Ii34910, S e t N o. : 080103A R, E x t .D a te : 0 8 /0 1 /0 3 , A n a ly s t :K .R is h a Page 16 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-308 Text: 4 : PFOSA X& E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o. : 080103A R, E x t.D a te : 0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P ag e 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.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-309 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report . Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 18 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-309 Text : 4: PFOSA L34910-11 Spk E, 5000 ng/L, DF=100 080103A R -309 Sm (Mn, 2x3) 100-1 %- 04-Aug-2003 11:29:36 LC/MS/MS #6 M R M of 4 Channels ES- 9.87 498 > 78 21870 1.12e5 Area 0 - ^ - - T . - [.. ' T '' 2.00 W 4.00 6.00 8.00 10.00 -r- Time E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tif y Sam ple R e p o rt v S tu d y N o .:L 3 4 9 1 0 , S e t N o. : 080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ish a P age 19 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 030103 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)_________________________________________________________________________ L34910-20 Spk F, 5000 ng/L, DF=100 04-Aug-2003 11:51:14 LC/MS/MS #6 0 8 0 1 03A R -310 Sm (Mn, 2x3) M R M of 4 Channels ES~ " 413 >369 1.66e5 Area ' jt i 1 I 1-- ] 1 - r 2.00 j ' ' ' ~ TimeT -T V- r - 1 j 1 - 1 1 1 1 1 1 1- [ 1 1 1 1 I 1 1 1 ' 1 1 1 1 > 1 I 111I 4.00 6.00 8.00 10.0 0 __________________ 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) B x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R e p o rt S tu d y N o .:L 3 4 9 1 0 , S e t N o. : 080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P age 20 Sample List: P:\Data\LCMSHS6\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__________________________________________________________________________________ L34910-20 Spk F, 5000 ng/L, DF=100 04-Aug-2003 11:51:14 LC/MS/MS #6 080103A R -310 Sm (Mn, 2x3) 100] %- M R M of 4 Channels ES- 9.90 498 > 78 [135241 6.94e4 Area " 1-'1 1 T"I1- r~l I'"1-T" 1 -I~l 1 1 1 1 1 1 r 1 1 1 f 1 1 ' 1 1 ' 2.00 4.00 6.00 8.00 1-| 1 1-1 1 1 1 rri 1 1 10.00 Tim E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 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\Fruorochemicals.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) W 2: C6 Sulfonate (PFHS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\7luorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\7luorochemicals.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 04-Aug-2003 12:12:52 LC/MS/MS #6 Q801Q3AR-311 Sm (Mn, 2x3) 10Ch M R M of 4 Channels ES- 9.90 498 > 78 166801 8.67e4 Area %: 1 Q~^y rM' r r 1 T 1 1-1 '~i 1 1 1 1 'i 1 1~n 1 ' 1 1 i 1 1 1 1 1 i ] 1 r 1 r 1 1 1 1 1 1 1 1 1 1 1 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 23 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SainpleDB\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: 030103AR-312 Text : 1: C8 Acid (PFQA) L34910-5 Rep, DF=10 0801 33AR-312 Sm (Mn, 2x3) 10Ch %- 9.12 14512^ 04-Aug-2003 12:34:39 LC/MS/MS #6 M RM of 4 Channels ES413 >369 8.59e4 Area 0*L -r-r I f - i 1 ) 1- I r 1 I I ' " ~ ' " i 1 1 i _ r n ~ 2 .0 0 4.00 11 1 6.00 " , 1' r r ' , 1 '' r r-T - T T -, ,-V T"~I-- , --T1^ n m e 8.00 10.00 3: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 24 Sample List: P:\Data\LCMSMS6\Mas3lynx\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-312 Text: 4: PFOSA L34910-5 Rep, DF=10 0801 D3AR-312 Sm (Mn, 2x3) loth %: 04-Aug-2003 12:34:39 LC/MS/MS #6 MRM of 4 Channels ES- 9.87 498 > 78 181891 9.40e4 1 Area o-I-, !-! T-ITT| . r I T' I-, -r-r-rri 1 '-f" 2.00 4.00 6.00 "*"*"1--r r--i 1 J r 1 i i i"i i > |ime 8.00 10.00 w Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sang?la Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 25 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-313 Text: 1: C8 Acid (PFOA) 2: CS Sulfonate (PFHS) 3: C8 Sulfonate (PFOS)____________________________________________________________________ L34910-10, DF=10 04-Aug-2003 12:56:21 LC/MS/MS #6 080103A R -313 Sm (Mn, 2x3) M RM of 4 Channels ES ' 499 > 99 8.15e4 Area em___________________ 2,00____________4 joo_________ i ' n ......t - '" '~r~r" Time _________ 8.oo_________ io.oo_______________ w Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, AnalystsK.Risha Page 26 Sample List: P:\Data\LCMSMS6\Masslynx\5,luorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.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 : 4: PFOSA L34910-10, DF=10 080103A R -313 Sm (Mn, 2x3) 100-1 %- 04-Aug-2003 12:56:21 LC/MS/MS #6 M RM of 4 Channels ES- 9.90 1950C 498 > 78 1.01e5 Area 0 W T 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Q u a n tify Sample R ep o rt SS tt uuddyy Noo..:: LL34991100,, SS eett Noo.. :: 00 8800110033AARR,, Exxtt .. DDaatt ee:: 0088// 0011 // 003,, Annaallyysstt :: KK.. R ii ss hhaa w Page 27 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.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 (PF0A) L34910-10 Rep, DF=10 080103A R -314 Sm (Mn, 2x3) 10CH %- 9.13 310621 1 1 04-Aug-2003 13:18:10 LC/MS/MS #6 M RM of 4 Channels ES413 >369 1 .85e5 Area o2 T1 j 1 j ; 1 -r1~j1--r~"'if'mr i"" 1I 1I 1I ) 1I "Ii '1I r I1 i 1|' r i1 r1---1i pr 1t rI"1i ri--m\i rni ^t tr f--i--i--i--i--|--i--i--i--i--]---,i--=^=-T=r-'f-F ` 2.00 4.00 6.00 8.00 10.00 h- Tim e 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) V E x y g e n R e s e a r c h , 3058 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 16801 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S e t No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a Rage 28 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\Masslyax\Fluorocheiaicals.PRjO\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 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S et N o .: 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a Page 29 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\Masslyzuc\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-315 Text: 1: C8 Acid (PFOA) XCOi^2503-1, 25 ng/L Standard 0801 D 3A R -315S m (M n ,2x3) 100 %- 9.13 12807^ 04-Aug-2003 13:39:58 LC/MS/MS #6 M RM of 4 Channels ES413 >369 8.23e4 Area . 0~ A < r ' .............................. , . . , . 2 .0 0 4.00 - r 1 , 7- [-1 -- 1 , 1 r--,r"' T r~' r' 1 6.00 8.00 2: C6 Sulfonate (PFHS) XCOI^2503-1, 25 ng/L Standard 0801 D3AR-315 Sm (Mn, 2x3) 100-1 8.98 2099^ %: 10.00 I ' ' ' ' ^ I im e 04-Aug-2003 13:39:58 LC/MS/MS #6 M RM of 4 Channels ES399 > 80 1.27e4 Area 0 L,,,", j r , -,-r-T-T-1 -- 2.00 ^T T-r-r-r- 1 ' ' ' l ' 1 ` ' 1 1 4.00 6.00 3: C8 Sulfonate (PFOS) X C 0 `f2 503-1, 25 ng/L S tandard 0801 D3AR-315 Sm (Mn, 2x3) 10Ch A "r ' 1--' T' r-r-r -i--'!~T"T--T*1 T' 8.00 10.00 JUTl 9.24 13011 04-Aug-2003 13:39:58 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 8.29e3 Area CH 1 ' ' ' i ' 1 1 ' I ' 1 1 1 I ' ' ' ' I ' ' ' ' 2.00 4.00 |-T I"- I---- 11 6.00 ______ A _ .. .. M ^ --'------ 1 J 'I , ,-| IT - . - . ' T ' j - r - t r-|--r- I r 1 '1 1 ' 1 1r 11 8.00 10.00 -j-. IITIG E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R eport S tu d y N o.:L 34910, S et No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n aly stsK .R ish a P age 30 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\0801Q3AR 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 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u an tify Sanale R eport S tu d y N o.:L 34910, S e t N o.:080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R iaha Page 31 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-316 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tudy N o.:L 34910, S e t No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a P age 32 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-316 Text: 4 : PFOSA E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set N o .:0801Q3AR, Ext.Date:08/01/03, Analyst:K.Risha Paffe 33 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: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S e t N o.:080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a W Page 34 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SeunpleDB\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 080103A R -317 Sm (Mn, 2x3) 1OOn %- u~ ' 1--| ! 1 ' T ~r"1"1- i - i r i ! -i--i--,--1--)--1--1--1--1--!--'--1--1--'--1 i i 2.00 4.00 6.00 04-Aug-2003 14:23:27 LC/MS/MS #6 M R M of 4 Channels ES- 9.89 498 > 78 219881 1.09e5 Area 1 i-y r r r 1 1 1 1 111 1 . . . . | 8.00 10.00 W E x y g e n R e s e a r c h 305 8 R e s e a r c h D r i v e S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S et No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a 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.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: 030103AR-318 Text: 1: C8 Acid (PFOA) 3: C8 Sulfonate (PFOS)____________________________________________________________________ L34910-11 Rep, DF=100 04-Aug-2003 14:45:17 LC/MS/MS #6 0 8 0 1 03A R -318 Sm (Mn, 2x3) M RM of 4 Channels ES` " 499 > 99 2.82e5 Area 2.00 4.00 6 .0 0 t i r 1 1 t T im e 8 .00___________ 10.00___________________ E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R ep o rt ( S tudy N o.:L 34910, S et No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a P age 36 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-318 Text : 4: PFOSA w E x y g e n R e s e a r c h 3058 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 168 0 1 Q u a n tify Sam ple R ep o rt S tu d y N o.:L 34910, S e t No. :080103A R, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R is h a P age 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) L34910-11, DF=10 080103A R -319 Sm (Mn, 2x3) 100- %: o:'_r-' 1 ' T 1'1 > 1 1 1 '"1 ' T i"1 2.00 4 .0 0 9.11 804731 I 04-Aug-2003 15:07:04 LC/MS/MS #6 M RM of 4 Channels ES413 > 3 6 9 4.67e5 Area 1 n "r" 1 1 "1 111 1 ' 1 1 1 i ' TM r-. T' !--! r-1 r pi t i"i Time 6.00 8.00 10.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 30 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 3 0 1 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Riaha Page 38 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-319 Text : 4 : PFOSA L34910-11, DF=10 0801Q3AR-319 Sm (Mn, 2x3) 100-1 %- 04-Aug-2003 15:07:04 LC/MS/MS #6 9.87 20029; M RM of 4 Channels ES498 > 78 10.00e5 Area O ri r T im e 2.00 4 .00 6.00 8.00 10.00 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R ep o rt S tu d y N o. :L34910, S et N o. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R isha VW P age 39 Sample List: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\FTuorochemicals.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: C8 Acid (PFOA) L34910-11 Rep, DF=10 080103A R -320 Sm (Mn, 2x3) 100- %- 9.13 768401 1 1 04-Aug-2003 15:28:46 LC/MS/MS #6 M RM of 4 Channels ES4 1 3 > 369 4.58e5 Area 0J 1 1 1 1 1 ' ' 1 1I 1 ' 1 'r I1 '' 11-1 T r"-11-! -1'T"-I1-- Tr-' 1-1' t'V rr IT r _1 n1 1 1-]1r 1i i 11 ' 1 * I 2.00 4 .0 0 6.00 8.00 r-1i 1i Ii ' i i t i - r i -i -r-r Tim e 10.00 3: C8 Sulfonate (PFOS) L34910-11 Rep, DF=10 080103A R -320 Sm (Mn, 2x3) 100i %: 0 J - r - r - r - ^ T ~ r ~ r ~ r - r - p - 1-- r - i -- r-- J-- r-- i-- r-- r-- |-- r - r - r - r - r r - T - r T l - r 2.00 4 .0 0 6.00 w 9.25 390663 04-Aug-2003 15:28:46 LC/MS/MS #6 M RM of 4 Channels ES499 > 99 2.30e6 Area 8.00 10.00 i 1 111 ' T im e E x y g e n R e s e a r c h , 3058 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 801 Q u a n tify Sample R ep o rt Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 40 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\ScwqpleDB\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-320 Text : 4 : PFOSA L34910-11 Rep, DF=10 080103A R -320 Sm (Mn, 2x3) 100-1 %- 04-Aug-2003 15:28:46 LC/MS/MS #6 M RM of 4 Channels ES- 9.87 498 > 78 15038-! 7.59e5 Area 0- Tim e 2.00 4.00 6.00 8.00 10.00 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S et N o .: 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a W Page 41 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Hetbod: P:\Data\LCMSMS6\Masslynx\Eluorochemicals.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) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 42 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-321 Text: 4: PFOSA E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R ep o rt S tu d y N o.:L 34910, S et No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a P age 43 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-322 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R ep o rt S tu d y N o.:L 34910, S e t N o.:080103A R, E x t.D a te :0 8 /0 1 /0 3 r A n a ly s t:K .R is h a Page 44 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-322 Text: 4 : PF0SA E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sam ple R ep o rt S tu d y N o.:L 34910, S et N o .: 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a Page 45 Sample Lists P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SajnpleDB\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) w E x y g e n R e s e a r c h , 30 58 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 16801 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S et No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A nalyst-.K .R isha Page 46 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-323 Text: 4 : PFOSA XC072503-3,100 ng/L Standard 080103A R -323 Sm (Mn, 2x3) 10Ch %: O ' 1 1 1 t ' ' 1 ' 1 1 1 r 1 I v 1 1" I 1T "1 1 - 1 - r - i | - r - 2.00 4.00 6.00 W 04-Aug-2003 16:33:50 LC/MS/MS #6 M R M of 4 Channels ES- 9.89 498 > 78 176281 9.31 e4 Area 8.00 10.00 T im e w S x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y No. : L34910, S e t N o .: 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a P ag e 47 Sample List: P:\Data\LCMSMS6\Masslynx\Fluarochemicals.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: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS1____________________________________________________________________ XC072503-4, 250 ng/L Standard 04-Aug-2003 16:55:35 LC/MS/MS #6 080103A R -324 Sm (Mn, 2x3) M RM of 4 Channels ES " ' 399 > 80 1.05e5 Area 2.00 3: C8 Sulfonate (PFOS) 4.00 6.00 8.00 ' '-n ' 10.00 ' I ' ' 1 ' Time E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Page 48 Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha W . Sample List: P:\Data\LCMSMS6\Masslynx\Fluorocheuiicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorocheraicals.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 080103A R -324 Sm (Mn, 2x3) 100-1 %- 04-Aug-2003 16:55:35 LC/MS/MS #6 M R M of 4 Channels ES- 9.89 40102 498 > 78 2.14e5 Area 0- 2.00 4 .00 6.00 8.00 T im e E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:CLI3R4S9I1O0, Set Noo.. :080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 49 Sample List: P:\Data\LCMSMS6\Masslynx\FTuorochemicals.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-325 Text: 1: C8 Acid (PFOA) 2: C6 Sulfonate (PFHS) W 3: C8 Sulfonate (PFOS) L34910-20, DF=10 080103AR-325 S m (Mn, 2x3) 100-; % -i 9.24 651081 1 04-Aug-2003 17:17:20 LC/MS/MS #6 M R M of4 Channels ES499 > 99 3.76e5 Area 1 w 0- I 1 Time--r--r - r - T 1T 111r--I!'1 r fr-t----i----fr r- i ir ----ri----p7---i1----ri--r--rr --r--r - r -tT----'f--r --pr--r -r --i --t--r"r -ii - np--r r- -r r- --T T---t--t--pt-<t -tt-it --i r -^ r ^l ^l k1 r <r j .-I T - r r - r - T t r - 2.00 4.00 6.00 8.00 ________ 10.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S et NO.: 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ish a P ag e 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\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-325 Text: 4 : PFOSA w V E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 168 0 1 Quantify Sample Report Study N o .:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 51 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\Pluorochemicals.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-326 Text: 1: C8 Acid (PFOA) L34910-20 Rep, DF=10 080103A R -326 Sm (Mn, 2x3) 100-j %: 9.12 44037 04-Aug-2003 17:39:07 LC/MS/MS #6 M R M of 4 Channels ES4 1 3 > 369 2.64e5 Area 0 r 11 1T 111Tl -r-1 11 T'1T~' '"I T' 2.00 4.00 2: C6 Sulfonate (PFHS) 6.00 P1 T I ""T I " T T " 8.00 ~ i ' ' i ' i ~ i Time 10.00 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 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\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-326 Text: 4 : PFOSA Mm* w E x y g e n R e s e a r c h , 305 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S et No. : 080103AR, E x t.D ate : 0 8 /0 1 /0 3 , A n a ly st:X .R ish a P ag e S3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: F:\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-327 Text : 1: C8 Acid (PFOA) L34910-21, DF=100 0 80103A R -327 Sm (Mn, 2x3) 10CH /<H 9.13 101691 1 04-Aug-2003 18:00:47 LC/MS/MS #6 M R M of 4 Channels ES413 >369 6.21e4 Area o: t i - i < . i-- i r t -- r r r i-- , - r r -- i - i -- i - i 2.00 4.00 i - r - i -- r~ i ' 1 ' ' ~r ' 1 f " " 6.00 1-- ' T ~ ' T ~ I 8.00 1 - 1" f-- 1" T -. - , 10.00 .-i-T-r-r-r^ Time 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 30 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S e t No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .R ish a P ag e 54 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\Fluorocheroicals.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: 4: PFOSA w E x y g e n R e s e a r c h 305 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 55 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SaunpleDB\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-328 Text: 1: C8 Acid (PFOA) L34910-21, DF=10 080103AR-328 Sm (Mn, 2x3) 100-] %- 9.16 992401 1 04-Aug-2003 18:22:28 LC/MS/MS #6 MRM of 4 Channels ES413 >369 5.73e5 Area 1 O ' 1 ` i~ ' 1 ' ' I " 1 r ` 1 --r [ ~~1 1 1 ' 1 - p - r T T ' i - i - r T -- 1-- r - r - i i 1 1 I 1 " I 1 r r - n - T ^ 2.00 4.00 6.00 8.00 ' T - ' r r I 1 I ! ! . Time 10.00 2: C6 Sulfonate (PFHS) 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 30 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set N o .:080103AR, Ext.Date:08/01/03, Analyst:K.Riska Page 56 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-328 Text : 4: PFOSA w E x y g e n R e s e a r c h 305 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tudy N o.:L34910, S et No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a Page 57 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\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-329 Text: 1: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 080103AR-329 Sm (Mn, 2x3) 100- %- 0J 2.00 4.00 9.15 2150481 I 04-Aug-2003 18:44:11 LC/MS/MS #6 MRM of 4 Channels ES413 >369 1.26e6 Area 1 .............................. -.... 6.00 8.00 t-M-i r -r- Timer - T - r - n -- -- r - T - 10.00 2: C6 Sulfonate (PFHS) w XCQ72503-5, 500 ng/L Standard 080103AR-329 S m (Mn, 2x3) in r u %- 8.99 371831 I 04-Aug-2003 18:44:11 LC/MS/MS #6 M R M of 4 Channels ES399 > 80 2.23e5 Area 1 0 - L -- 1-- I-- 1-- I-- 1-- i-- i-- 1-- I-- 1-- 1-- 1-- r - l -- 1-- 1-- 1-- 1-- I-- 1-- 1-- 1-- 1-- I-- 1-- 1-- 1-- 1-- -- i -- r -- r T r - r - r - l ............................. -r TimeI- ' * - < t t - i- 2.00 4.00 6.00 8.00__________10.00 3: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu dy N o.:L 34910, S e t No. : 080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly st:K .R ish a Page 58 Sample List: P:\Data\LCMSMSS\Masslynx\Fluorochemicals.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-329 Text: 4: PFOSA XC072503-5, 500 ng/L Standard 080103AR-329 Sm (Mn, 2x3) 10Ch %- 04-Aug-2003 18:44:11 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 86063 498 > 78 4.48e5 Area 0- Time 2.00 4.00 6.00 8.00 10.00 W E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Page 59 Sample List: P:\Data\LCMSMSS\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Decatur BC Last modified: Tue Aug 05 07:24:43 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRQ\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 %: 9.15 4062541 1 1 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES413 >369 2.39e6 Area 2.00 4.00 6.00 8.00 10.00 Time 2: C6 Sulfonate (PFHS) XC072503-6,1000 ng/L Standard 080103AR-330 Sm (Mn, 2x3) 1QQ~i %- 8.99 71521 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 4.19e5 Area 0 Time 2.00 4.00 6.00 8.00 10.00 3: C8 Sulfonate (PFOS) XC072503-6,1000 ng/L Standard 080103AR-330 Sm (Mn, 2x3) 1 0 0 -1 9.27 44784 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.57e5 Area W 2.00 r i T " i " I- r - r - T - , T 4,00 6.00 1 rr 8.00 " T r 1-1 10.00 Time E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 S 8 0 1 Q u a n tify Sam ple R ep o rt S tu d y N o.:L 34910, S e t No. s080103AR, E x t.D a te :0 8 /0 1 /0 3 , A n a ly s t:K .H is h a Paga 60 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-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) MRM of 4 Channels ES- ` " 498 > 78 8.67e5 Area iT T - p - n - ,- Time 2.00 4.00 6.00 8.00 ______ 10.00 _____ w E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 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 Weight: Final Volume: 50 ppt 15 Soil 5.0 g SflmL . . Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 081203A Karen Risha LCMSMS #6 08/123 08/13/03 Exygen Sponsor Sample Run ID ID Code No. XCQ811Q3-G XC08II03-1 - CS 081203A-3001 cs Q812Q3A-3002 XC081103-2 - CS 081203A-3003 XC081103-3 - cs 0SI23A-3004 XC08U03-4 - cs 0S1203A-3005 XC081103-5 cs 081203A-3006 XC081103-6 - cs Q812Q3A-3QQ7 Methanol Wash c 081203A-3008 ReagentBlank na c 081203A-3009 ReagentSpk A na LCS 081203A-3010 ReagentSpk B na LCS 081203A-3011 L34910-1 Spk E BC2SED-6 LF 081203A-3012 L34910-U SpkE BC2SED-6 LF 0812Q3A-3013 XC081103-1 - CS 081203A-3014 XC081103-2 XC081103-3 L34910-U L34910-U Rep L3491Q-11 L34910-1I Rep XC081103-4 XC081103-5 XC081103-6 - - BC2 SED-06 BC2 SED-06 B G SED-06 BC2 SED-06 - - - CS 081203A-3015 cs 081203A-3016 s 081203A-3017 s 081203A-3018 s 08I203A-3019 s 081203A-3020 cs 081203A-3021 cs 081203A-3022 cs 081203A-3023 Analyte Found (ppQ = (peak area - intercept) / slope x DF Recovery (%) = (analyte found (pptVanaiyte found in control (ppt)} x 100 amount added (ppt) Std. Cone. (PPO 0 25 50 100 250 500 1000 Dilutioa Factor 1000 too 25 50 100 - 1000 1000 - 100 - 100 250 500 1000 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 Amount Analyte Found Added Recovery Found (PPO (pp0 <%) (ppb) - - - - - - - - ND - 49.2 50 98 - 533 215000 500 100000 100000 107 105 - - -- - 110000 880.00 124000 * 992.00 - *- -- -- - - Standard Curve: Linear (1/x weighted) Intercept a 10.4732 Slope a 39.6727 Coef. OfDet. = 0.998540 Total Solids (%) 60.41 60.41 60.41 60.41 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 solid* (%)) CS = Calibration standard C = Control sample S a Sample LF a Lab fortified sample FF = Field fortified sample LCS > Lalxiratofy 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 - 1460 1640 - Dilution was for PFOSA. jty-/Spreadsheet prepared by:. celieltft SponsorStudy No: Exygen StudyNo: Analyte: IonsMonitored: Site: NA L34910 FOSA 498 -> 78 DecaturBaker'sCreek RAW DATA REPORT Limit ofQuantitation: InjectionVolume: Matrix: Sample Weight: FinalVolume: 50 ppt 15 Soil 5.0 g 5.0mL SetNo: Analyst: InstrumentType: Extraction Date: Analyzed on: 081203A Karen Risha LCMSMS #6 08/12/03 08/13/03 Exygen ID XC081103-0 XC081103-1 XC081103-2 XC081103-3 XC081103-4 XC08U03-5 XC081103-6 Methanol Wash ReagentBlank ReagentSpk A ReagentSpk B L34910-11Spk E . L34910-11Spk E ~ XC081103-1 XCQ81103-2 XC081103-3 L349I0-J? L34910-11Rep L34910-I1 L34910-1I Rep XC081103-4 XC0R1103-5 XC081103-d Sponsor ID - - - na na na BC2 SED-06 BC2 SED-06 BC2 S E D - 0 6 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. 08J203A-3001 081203A-3002 081203A-3003 081203A-3004 081203A-3005 081203A-3006 08I203A-30Q7 081203A-3008 08J203A-3009 081203A-3010 081203A-30U 081203A-30I2 081203A-3013 081203A-3014 081203A-3015 081203A-3016 081203A-3017 081203A-3018 081203A-3019 081203A-3020 081203A-3021 0812Q3A-3022 081203A-3023 AnalyteFound(ppt)* (peakarea-intercept)/slopex DF Recovery(%) (analytefound(ppQ-analytcfound incontrol(ppt)lx 100 amount added (ppt) Std. Cone. (pp<) 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Factor 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 Analyte Found (pp() Amount Added (pp() Recovery (%i Analyte Found (ppfa) ND 45.5 481 81200 - 50 500 100000 100000 91 96 72 8930 10400 - 71.44 83.20 - StandardCurve :Linear(l/xweighted) Intercept * 434.4SS Slope = 150.037 Coefi OfDet. = 0.998129 Total Solids (%) * - 60.41 60.41 60.41 60.41 AnalyteFound (ppb)= [analytefound(ppt)x volume extracted(0.04L)]/sampleweight(5 g) AnalyteFound (ppb)dryweight* analytefound(ppb)x (100% /totalsolids(%)) CS - Calibrationstandard C Control sample S = Sample LF - Lab fortifiedsample FF * Fieldfortifiedsample LCS = LaboratoryControlSpike CK = Check Standard ND * Not detected- Response between 0 and 25 ppt NQ = Not quantifiable= Response between 25 pptand LOQ (50ppt) Analyte Found (ppb) Dry Weight - - * 118 138 * ` Dilution was for PFOS Spreadsheetpreparedby. 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number: NA Exygen Study Number. L34910 Exygen Sample # L34910-11 _ - Sponsor Sample # BC2 SED-06 _ - Exygen Sample # _ _ - Sponsor Sample # _ _ - --- - - -- - -- -- _- W -- Karen Risha 08/11/03 1400 Requested By (Printed Name/Date/Time) - - Samples removed from: cz& o Samples removed from: P _______ Box#_____ ^ _________Shelf# Box# '-- Shelf# Samples transferred to the custody of Samples received from custodian; Samples moved to / i t - `Z'/Z-rt /? J o Sample Custodian Initials/Date/Time jL ofe|n\Q 3 i Laboratory Personnel Initials/Date/Time Samples removed from A S - Samples returned to__ Sample Custodian Initials/Date/Time Exysen %/ 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 L 3 4 9 10 Matrix: Soil Sponsor Study/Protocol No: HA The samples listed below were removed from refrigerator No. Time ______ Date Initials, CEB 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 L349I0-11 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 Spk E _ . . Spiking Solution Used F061103-2 (10 ng/mL) F061103-1 (100 ng/mL) F060203-1 (10000 ng/mL) . . _ -- All samples were weighed on balance No. 2 C ) Time A Q 7 - 0 Date Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 400 pL (200 pL micropipet) - Initial/Date !L - /c e lu fo=, f /e>t>j ._ .- - Initials C'f-b-. After weighing samples were returned to refrigerator No. Time I H 7 - 0 ______ Date O &jlt-ji(R ____ Initials Comments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: C E ,j Q f j f a o Z Analysis Summary: Data Set: o & ii o s A Data Set:. Data Set:. Initials/Date: / Initials/DateK: JO. /__ z __ Initials/Date: Set extraction/analysis data verified by: Date: 1 L ' July 26, 2001/1 c( * 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 MATRIX: Soil METHOD: ExM-023-014 n ANALYTES: PPHS. PFOS. PFOA and PFOSA PROTOCOL NUMBER: NA C lien t ID na na na B C 2 SE D -06 B C 2 SE D -06 B C 2 SED -06 - - . - - *ln itia is /D a le E xygenID R eag en t B lank Reagent Spk A Reagent Spk B L 34910-11 Spk E L 34910-11 L 34910-11 R ep - - - - STEP 1 STEP 2 STEP 3 STEP 4 V vj/ \ -- - -- - -- - --- - - ----- - -- - -- - -- -- - - S fa C C0Z f a ll t fa lfa . V/ - - - - - STEP 5 STEP 6 D ilutions (m L /m L ) -- -- -- C A \ *Vm r \ If \ L i . -- . -- - -- - .- - -- . -- . -- --- - -- - -- - -- -- - - C ef c d lif a Q & lifa STEP 7 \1 - - - - D ilutions (m L /m L ) -- -- -- - - - - - - - ' -- STEP 8 -- -- - - - -- R eag en ts/ M aterials M ethanol C l 8 SPE Type I Water Glass acrodisc . _ . . In itia ls /D a te - L o t ft U m it> W *O J o Ia / A ! ( o T & 2 _ NA _ _ . P E E - C & jl2 J n *> _- ._ . HPLC M ethanol Ammonium Acetate 4 A 8 rr3 N Type I water NA - 1' In itia ls /D a te O & lf e STEP 2: Bring up to 40 mL with hypercarb filtered type I 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. = io o i o o fee 'Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctanesulfonate (PFOS) and Pentadecafluorooctanoic Acid (PFOA) in Soil COMMENTS: Final extracts stored in refrigerator ^>2- Initials: P E F l Date: July 19, 2001/4 RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Protocol No.: None Method No.: $$ Exygen Study No.: NA Analytes: PFBS. PFHS. PFOS. PFOA Matrix: Type I Water* Sample Vol: 40 mL Sponsor Sample ID NA NA NA NA NA Exygen Sample ID 0106020 0106020 0106020 0106020 0106020 Sample Description t U /r.t w \ J p s / X Ult/1 Type I Water'1 Type I Water7' Type I Water7' Type I WaterA Fort Solution ID - F 0 6 1103-2 F 0 6 1 103-2 F 0 6 1103-2 F 0 6 1103-1 and PFOSA Fort. Fort- Soin. Cone. Volume (ne/mL) (mL) 10 100 10 200 10 400 100 100 Micropipet used (ML). 200 200 200 200 Fort Level (P P t) 25 50 100 250 Final Solution ID #** 11 1V / ^ r v o A C -U O no n X C 0 8 1 103-1 X C 0 8 1103-2 XC081103-3 X C 0 8 1103-4 Reagents/ Materials viciiii C l8 SPE Type I Water _ Lot # t tO 14 NA . NA 0106020 Type I Water71 F061103-1 100 200 200 500 XC081103-5 NA 0106020 Type I WaterA F061103-1 100 400 200 1000 XC081103-6 . _ -- - - -- - Vertical arrows in a column indicate identical values. - - _- - --- c - Initials/Date: o e j i i 1o 3 *This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3. etc. Samples removed frogTTefngerator / freezer It ^?2- Time: CROP In irials /D ate - /fifJ h jn * . 40 mL of each sample measured using a Initials/Date After measuring, samples returned tt^rgfngeragfr ! freezer # 3 2 - Time: ifS Z O Initials/Date Samples fortified: Initials/Date / c e fu [03 SPE clean-up (omitting 40% Wash): Initials/Date Final volume adjusted to 5 mL: Initials/Date Extracts placed in refrigerator # -^2- Initials/Date STANDARD EXPIRATION DATE: 8/25/03 Comments: AThis type I water has been filtered through a hypercarb filter $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamidc (PFOSA), and Perfluorooctanoate (POAA) in Water July 10,2001/0 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochen iicals.PRO\SampleD8\081203A Decatur BC.SPL Printed: Wed Aug 13 09:36:59 2003 U 4 M b \ & _____________________________ Vial File Name LIMS ID Client ID Sample Description Mai 1 1 081203A-3001 _,, 2 2 081203A-3002 -- 3 3 081203A-3003 -- 4 4 081203A-3004 5 5 081203A-3005 -- 6 6 081203A-3006 -- 7 7 081203A-3007 -- 8 92 081203A-3008 -- 9 11 081203A-3009 -- 10 12 fu\ Qu i1 OL Au Qv na ' oo ur wI nu -- 11 13 081203A-3011 -- 12 14 081203A-3012 -- 13 15 081203A-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 SpK 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 L34910-11 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 study n o J ( Page 1 Page Positjon. ^ ^ Sample Type Standard Standard Standard Standard Standard Standard Standard Blank Blank QC QC QC QC Standard Standard Standard Analyte Analyte Analyte Analyte Standard Standard Standard Cone (ng/L) 0 25 50 100 250 500 1000 -- -- 50 500 100000 10000 25 50 100 -- -- -- -- 250 500 1000 Cone B ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- Cone C _ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- Test ID 0 0 0 0 0 0 0 0 0 \AJ 0 0 0 0 0 0 0 0 0 0 0 0 0 DF 1 1 1 1 1 1 1 1 1 A1 1 1000 100 1 1 1 1000 1000 100 100 1 1 1 c( Masslynx - Sample List Sample List: C3MASSLYNX\Fluorochei iicals.PRO\SampleDB\081203A Decatur BC.SPL Printed: Wed Aug 13 09:36:59 2003 i PbB l l3|i> ^ ______________________________ 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 C8 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 C8 ACID PFOSA 10 C6 Co SULF Co 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 C8 ACID PFOSA 21 C6 C8 SULF C8 ACID PFOSA 22 C6 C8 SULF C8 ACID PFOSA 23 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 Fluorochems Fluornchems 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 Exygen STUDY NO.' LffihP Page 2 Page Position: (2, 1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS 1*/ 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: Hewlett Packard (HP) Series 1100 HP B in Pump HP V acuum 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 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 Scanning Method Report Page 1 Method: C:\MASSLYNX\FLU0R0CHEMICALS.PR0\ACQUDB\C6 C8 SULF C8 ACID PFOSA Last Modified: Thu Jul 31 18:23:50 2003 Printed: Wed Aug 13 00:37:33 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 V w Method Report Method File: Last Modified: Printed: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\p fbs w a te r Wednesday, August 13, 2003 09:25:46 Wednesday, August 13, 2003 09:37:56 Page 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 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 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(/il) 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 Tuning Method Report Method C :\MAS SLYNX\S'LUOROCHEMICALS .PRO\ACQUDB\FLUOROCHEMS Printed: Wed Aug 13 09:37:50 2003 Odi 303 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 Q uantify C a lib ra tio n R eport S tu d y N o.:L 34910, S a t N o.:081203A , E x t.D a te :0 8 /1 2 /0 3 , A n a ly s t:K .R isha 'W Page 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\081203A Decatur BC Last modified: Mon Aug 18 10:47:18 2003 , P rin ted : Mon Aug 18 1 0 :5 0 :2 4 2003 ,00 18 03 1'2- E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u an tify C a lib ra tio n R eport S tu d y N o.:L 34910, S et No. s081203A, E x t.D a te :0 8 /1 2 /0 3 , A n a ly st:K .R isb a 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 E x y g e n R e s e a r c h , 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 168 0 1 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 1 w 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\,P F* 0wSw and PFOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 IDniattieal_s.2Siimsuxmai---------- . --- - R u n # ~ y & L To.CflIiC fih ~ 3ftit? Name: 081203A-3001 Text: 1: C8 Sulfonate (PFOS) 2: PFOSA W E x y g e n R e s e a r c h 305 8 R e s e a r c h D r i v e S t a t e C o l l e g e , PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Riaha Page 2 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-3002 Text: 1: C8 Sulfonate (PFOS) 2: PFOSA E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e S t a t e C o l l e g e PA 1 6 8 0 1 Quantify Sanle Report Study No.:L34910, Set N o .:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 3 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-3003 Text : 1: C8 Sulfonate (PFOS) V E x y g e n R e s e a r c h 3058 R e s e a r c h D r i v e , S t a t e C o l l e g e PA 16801 Q u an tify Sandle R aport S tu d y N o.:L 34910, S e t N o.:081203A , E x t.D a te :0 8 /1 2 /0 3 , A n a ly st:K .R ish a Page 4 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 PPOSA 081103 Last modified: Mon Aug 11 09:49:08 2003 Job Code: Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3004 Text: w E x y g a n R e s e a r c h 3058 R e s e a r c h D r i v e S t a t e C o l l e g e PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu dy No. : L34910, S et N o.:081203A , E x t.D a te :0 8 /1 2 /0 3 , A n a ly st:K .R ish a Rape 5 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\Fluorochemical9.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-3005 Text: 1: C8 Sulfonate (PFOS) 2 : PFOSA W XC081103-4, 250 ng/L Standard 081203A-3005 S m (Mn, 2x3) 10CH 13-Aug-2003 16:10:15 LC/MS/MS #6 MRM of 4 Channels ES- 9-95 498 > 78 39080 4 1 ,88e5 Area 0 L, I , I - , -, , , , , I , i 2.00 4.00 6.00 8.00 10.00 Time W E x y g e n R e s e a r c h 305 8 R e s e a r c h D r i v e , S t a t e C o l l e g e PA 1 6 8 0 1 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 6 W Sample List: P:\Data\LCMSMS6\Masslynx\Fruorochemicals.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-3006 Text: 1: C8 Sulfonate (PFOS) XC081103-5, 500 ng/L Standard 081203A-3006 Sm (Mn, 2x3) 100-1 9.33 19165 13-Aug-2003 16:32:00 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.06e5 Area 2: PFOSA 2.00 I ' 1 1 I ' ' m 1 4.00 6.00 8.00 10.00 Time E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S et N o .: 081203A, E x t.D a te :0 8 /1 2 /0 3 , A n a ly st:K .R ish a Page 7 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-3007 Text : 1: C8 Sulfonate (PFOS) XC081103-6,1000 ng/L Standard 081203A-3007 Sm (Mn, 2x3) 10O i 9.33 39020 13-Aug-2003 16:53:41 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 2.06e5 Area 2.00 4.00 6.00 8.00 10.00 Time 2 : PFOSA W XC081103-6,1000 ng/L Standard 081203A-3007 Sm (Mn, 2x3) 100-1 13-Aug-2003 16:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 1450231 498 >78 6.91e5 Area 2.00 4.00 6.00 8.00 10.00 Time % 10 E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e , PA 1 6 8 0 1 Q u a n tify Sample R ep o rt S tu d y N o.:L 34910, S e t N o.:081203A , E x t.D a te :0 8 /1 2 /0 3 , A n a ly st:K .R ish a Page 8 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-3008 Text: 1: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h 3 0 5 8 R e s e a r c h D r i v e , S t a t e C o l l e g e PA 1 6 8 0 1 Q u a n tif y Sample R ep o rt S tu d y N o.:L 34910, S et N o.:081203A , E x t.D a te :0 8 /1 2 /0 3 , A n a ly s t:K .R isba Page 9 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.PRO\MethDB\PFOS and PFOSA 081103 Last modified: Hon Aug 11 09:49:08 2003 Job Code: Printed: Hon Aug 18 10:50:26 2003 Name: 081203A-3009 Text: 1: C8 Sulfonate (PFOS) E x y g e n R e s e a r c h 305 8 R e s e a r c h D r i v e , S t a t e C o l l e g e PA 1 6 8 0 1 Quantify Santis Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 10 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-3010 Text: Exygen Research 3058 Research Drive, State College PA 16801 Xmif Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 11 - 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\Ma3slynx\E,luorochemicals-PRO\MethDB\PFOS and PPOSA 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) 2 : PFOSA W Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 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 Quantify Sample Report Study N o .:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 13 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: 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 %: O ' ' I ' I ' ' T r T . - r I I | . " i I ................ 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 %- 13-Aug-2003 19:03:40 LC/MS/MS #6 MRM of 4 Channels ES9.36 499 > 99 4.77e5 Area -r r r-r i ' .-i Time 8.00 10.00 13-Aug-2003 19:03:40 LC/MS/MS #6 MRM of 4 Channels ES- 9-98 498 >78 122331 | 5.76e5 Area 0 " 1 1 1 i 1 1 1 ' i 1 ' ' ' --i--r 2.00 ` 'i ' 4.00 1 i 1 1 ' 1 i~ r 6.00 8.00 10.00 Time W Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 14 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.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: 1: C8 Sulfonate (PFOS) 2 : PFOSA w XC081103-1, 25 ng/L Standard 081203A-3014 Sm (Mn, 2x3) 10C^ %- 13-Aug-2003 19:25:25 LC/MS/MS #6 . MRM of 4 Channels ES- 9-96 42301 498 >78 2.10e4 1 Area 0: ' ' ' I ' ' ' 1 I ' ' ` ' I ' 1 ' 1 I 1 ' ' 1 I ' ' ' ' I 1 ' 1 1 1 r 1 1 . 1 . 1 ' 1 1 1 1 1 1 1 1 i ' ' Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 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.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-3015 Text: 2: PFOSA Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analysts. Ri sha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\FTuorochemicals.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-3016 Text: 1^ 2 : PFOSA X C 081103-3,100 ng/L Standard 081203A-3016 Sm (Mn, 2x3) 10Ch /o: 0 '- 1 1 1 I 1 1 ' T - | " r ' 1 ' I T ' ' 1 I .................... | I 2.00 4.00 II 6.00 13-Aug-2003 20:08:51 LC/MS/MS #6 M RM of 4 Channels ES- 9-96 498 > 78 162481 7.75e4 Area 8.00 10.00 Time Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 17 Sample List: P:\Data\LCHSMS6\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: Mon Aug 18 10:50:26 2003 Name: Q81203A-3017 Text: 1: C8 Sulfonate (PFOS) 2 : PFOSA Exygen Research 3058 Research Drive, State College PA 16801 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\San9leLB\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: Q81203A-3018 Text : 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risba Page 19 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-3019 Text: L34910-11, DF=100 081203A -3019 Sm (Mn, 2x3) 10O-] %- CM-t- 2.00 4.00 11i 6.00 13-Aug-2003 21:13:55 LC/MS/MS #6 M RM of 4 Channels ES- 9.96 498 > 78 138341 6.48e4 Area 8.00 10.00 T im e Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 20 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.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) 1 0 0 -i %- 9-36 483561 1 13-Aug-2003 21:35:42 LC/MS/MS #6 M RM of 4 Channels ES499 ? 99 2 .5 1e5 Area i i i0 - ' ' ' ' 1 l " ' " 1 11 I1 ' 1 ' ' I| 1 1 1 T'"- |'I 1'----- ----- I - r - I .iT-I i" -' i' - r [I tt Ii Fr---ii I| Ii ii T - i [i -iI Ii I-T----I i iI 1 ................1........... '1 i 2.00 4.00 6.00 8.00 10.00 ' i Time 2: PFOSA w L34910-11 Rep, DF-100 081203A -3020 Sm (Mn, 2x3) 100n %: 13-Aug-2003 21:35:42 LC/MS/MS #6 M RM of 4 Channels ES498 > 78 7.31 e4 Area 0'L| 1 1 1 : 1 1' 1 I 1 1 1 1 I 1 1 1 ' i > 2.00 4.00 & oo 8.00 T im e Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Rage 21 Sample List: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Decatur SC 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-3021 Text: 1: C8 Sulfonate (PFOS) 2: PFOSA Exygen Research 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risila 'll-- / Page 22 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-3022 Text: 1: C8 Sulfonate (PFOS) X C 0 8 1 1 0 3 -5 , 5 0 0 n g/L S ta n d a rd 081203A-3022 Sm (Mn, 2x3) 100- %: 9-35 206681 1 1 3 -A u g -2 0 0 3 22:19:08 L C /M S/M S # 6 MRM of 4 Channels ES499 > 99 1 09e5 Area r-| r r-T -o - I p n - T - i - i 11 ' 1 1 1 r 1 T r - [ . r i - l f i i - t- i f - r i --1-- 1-- - | - 1 i i i 1 6.00 10.002.00 4.00 8.00 f1*1 1 1 1 i 11 r - 1 Time 2: PFOSA 'W X C 0 8 1 1 0 3 -5 , 5 0 0 n g/L S ta n d a rd 10O] %: U" ~r --I r - . f . - r r- | i h t- j n' rr i | -i , 11 111, ' 1' ` 1' ' ' 1 2.00 4.00 6.00 13 -A u g -2 0 0 3 22:19:08 L C /M S/M S # 6 MRM of 4 Channels ES- 9.96 788481 498 > 78 3.74e5 Area 1 -r- i 1 ' ' 8.00 10.00 Time % >0 Exygen Research 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No. .-L34910, Set Noo..:081203A, Ext .Daattee:08/12/03, Analyst :K.Risha Page 23 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\MaBslynx\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-3023 Text : 1: C8 Sulfonate (PFOS) XC081103-6,1000 ng/L Standard 081203A -3023 Sm (Mn, 2x3) 10Ch %- 9.36 39291 13-Aug-2003 22:40:47 LC/MS/MS #6 M R M of 4 Channels ES499 > 99 2.13e5 Area ~i r_ 2.00 4.00 6.00 8.00 10.00 T im e 2: PFOSA XC081103-6,1000 ng/L Standard 081203A -3023 Sm (Mn, 2x3) 100-1 %- 13-Aug-2003 22:40:47 LC/MS/MS #6 M RM of 4 Channels ES- 9.96 498 > 78 1494431 7.03e5 Area 0 -'n -,-r , 2.00 4.00 6.00 8.00 10.00 Time Exygen Research 3058 Research Drive, State Collage PA 16801 9/19/2003 Project: E03-0561 3M ENVIRONMENTAL LABORATORY Final 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: 9/2/2003 Project Lead: Jess S. Eldridge Phone Number: 651-778-5233 Email Address: jseldridge@mmm.com 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 E rw st Rssubs/Astm tt Pace Field Sampling Event - Complete 3M Sample Number_______ Sampled Date_______ Sam ple Description E03-0S61-49786 7/21/2003 BC2 SW-04 MS EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49787 9/21/2003 Cumpuncnts PFOS PFHS FOSA PFOA BC2 SW-04 DUP LAB EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49788 7/23/2003 C om ponents PFOS PFHS FOSA PFOA BC2 SED-04 ME EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49789 7/21/2003 Components PFOS PFHS FOSA PFOA BC2 SW-05 MB 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 EL Qualifier 0.05 0.05 0.05 0.05 EL Qualifier 0.05 0.05 0.05 0.05 EL Qualifier 0.4 0.4 0.4 0.4 EL Qualifier 0.05 0.05 9/19/2003 3M ENVIRONMENTAL LABORATORY Final Report Project: E03-0561 (cont) 3M Sample Number______ Sampled Date E03-0561-49789 (cont.) 7/21/2003 Sample Description BC2 SYV-05 LAE EXYGEN Analytic! Method FOSA EXYGEN 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 LAB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49792 7/23/2003 Components 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 Components 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 PFHS EXYGEN FOSA EXYGEN PFOA E03-0561-49794 7/23/2003 Component} PFOS PFHS FOSA PFOA BC2 SED-06 Result 25.1 ng/mL 5.87 ng/mL 2.57 ng/mL 11.6 ng/mL LAE EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49795 7/23/2003 Components PFOS PFHS FOSA PFOA Outfall to River SW-2S Result 880 ng/g 2.46 ng/g 71.4 ng/g 14.2 ng/g LAE EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA 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 LAE EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA Com ponents PFOS PFHS FOSA Result 30.8 ng/mL 6.77 ng/mL 3.28 ng/mL 2 of 3 E L Qualifier 0.05 0.05 EL 0.05 Q u alifier 0.05 0.05 0.05 E L Qualifier 0.4 0.4 0.4 0.4 E L Qualifier 0.05 0.05 0.05 0.05 E L Qualifier 0.05 0.05 0.05 0.05 E L Qualifier 0.4 0.4 0.4 0.4 EL 0.05 Q ualifier 0.05 0.05 0.05 EL 0.05 Q ualifier 0.05 0.05 9/19/2003 3M ENVIRONMENTAL LABORATORY Final Report Project: E03-0561 (cont.) 3M Sample Number_______Sam pled Date_______ Sam ple Description________ E03-0561-49796 (cont.) 7/23/2003 Outfall to River SW-25 DUP LM 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 Method PFOS byESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-49813 7/23/2003 Components PFOS PFHS FOSA PFOA Outfall to River SED-25 DUP E sault 107 ng/g 3.19 ng/g 28.0 ng/g 10.7 ng/g LAB EXYGEN Analytical Method PFOS by ESMS EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA E03-0561-59479 7/21/2003 Components PFOS PFHS FOSA PFOA Field Control/Travel Blank Result 140 ng/g 4.98 ng/g 35.7 ng/g 17.7 ng/g LAE EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-59480 7/21/2003 Components PFOS PFHS FOSA PFOA Equipment Blank - Pump Result ND ng/mL ND ng/mL ND ng/mL ND ng/mL LAE EXYGEN Analytical Method PFOS by ESMS EXYGEN PFHS EXYGEN FOSA EXYGEN PFOA E03-0561-59481 7/21/2003 Components PFOS PFHS FOSA PFOA Equipment Blank - Dredge B e a u 11 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 0.05 Q u alifier B L Qualifier 0.4 0.4 0.4 0.4 B L Qualifier 0.4 0.4 0.4 0.4 B L Qualifier 0.05 0.05 0.05 0.05 B L Qualifier 0.05 0.05 0.05 0.05 B L Qualifier 0.05 0.05 0.05 0.05 Project Lead Review: H ale V / / g