Document QXMqvVMMkowwxZnydbZjv2MV6

Proven Results. AR &&.&- 1 7 0 0 Analytical Report f- jH Fluorochemical Characterization of Soil Samples if ] Daikin America Well Installation Exygen Research Laboratory Report No. L0001278A Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester John Simmons E. Robert Alley and Associates 210 N. Atlanta Avenue Sheffield, AL 35660 (256) 383-1552 h I_Ii. 4, W 3058 Research Drive State College, PA 16801, USA PAGE I: 800.281.3219 F: 814.272.1019 exygen.com h3 Results are reported for the analysis of soil samples received by Exygen Research (Exygen) from E. Roberts Alley and Associates. The Exygen study number assigned to the project is L0001278A. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 32 samples were received for analysis. T he samples were prepared and analyzed by LC/M S/M S for the following list of fluorochemicais: T able 1: T arget Analysis Compound Name Perfluorooctane Sulfonate Acronym C8 Sulfonate fPFOS) 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. The methods were adapted for soil samples. Soil sample methods have not been fully validated at this time. The samples were submitted in amber glass 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 between 11/3/03 and 11/5/03. Chainof-custody information is presented in Attachment C. Field and laboratory spikes of these fluorochemicais have shown stability for periods greater than 90 days. Samples were analyzed within 60 days of receipt. 4 Methods - Analytical and Preparatory f1 k- i Soil samples were extracted into methanol (5 grams of soil to 5 mL of methanol). The methanol extract was diluted to 40 mL with water. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. The diluted extracts were transferred to a C18 SPE cartridge. T h e cartridge was eluted with 5 mL of 100% methanol. This treatment resulted in an eight-fold concentration of the diluted samples prior to analysis. 4.1.2 Sam ple 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 H PLC 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 | 1 known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard H P 1 100 HPLC system coupled to a Micromass Ultima M S/M S was used to i " i analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted between 12/18/03 and 12/22/03. Samples were analyzed between 12/19/03 and 12/25/03. Raw analytical data is provided in Attachment D. fi 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, H t3 500, and 1000 ng/L (ppt) for LC/MS/MS analysis. The instrument response versus the k ; 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). f Calibration standards are prepared using the same SPE procedure used for samples. n Calibration check standards were analyzed periodically (every three to five sample injections) ?- i throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. k All calibration criteria were met for this analysis. 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. t. i- 4 . Instrument blanks in the form of clean methanol solvent were also analyzed after every high- level 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 Matrix spikes were prepared for four samples. Matrix spike recoveries are given in Attachment B. Recovery is calculated from the amount present in the sample extract. PAGE 3 OF5 0233 p 1.1 n f 5.5 Duplicates Laboratory duplicates were performed for four samples. The duplicate results are included with 0 the sample results in Attachment A. f**, 5.6 L abo ratory C ontrol Sam ples i ; 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 f*"* along with the raw data in Attachment D. |1 6 Data Summary . . > . . . . . . . ; . . . . . nik - Please see Attachment A for a detailed listing of the analytical results. Results are reported in parts per billion (ppb) (ng/g). Results are reported on a dry-weight basis. i 7 Data/Sample Retention ' r..,. I*--i 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 i \; folders maintained by Exygen. fft*"* 8 Attachments ....... 8.1 Attachment A: Results *f$*0^-i fi 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody n H 8.4 Attachment D: R aw Analytical Data n fi- nf . nfe<A r' ti te ! fe. ; PAGE 4 OF 5 9 Signatures Other Lab Members Contributing to Data Karen Risha I/ PAGE5 OF5 0 0 0 2 ?5 : Tr* ; li j i** !M ip :^ H - 1i 1 p fi ,j r f- -t , r t . 41 Ji :P 4. n 4j p1^ t 1 1 Proven Results. S um m ary of PFOS in Soil Sam ples Sam ple ID Analyte Found (ng/g) PFOSA M W -2 (0-2) MW-2 (0-2)* M W -2 (3-5) M W -2 (8-1,0) MW-2 (13-15), 1900 1590 2370 1980 107 MW -2 (18-20) , MW-2 (23-25) \ MW -2 (28-30) \ MW -2 (33-35) \ MW -5 (0-2) , MW -5 (3-5) \ 133 116 303 106 3410 425 MW -5 (8-10) MW-5 (13-f5) MW -5 (18-20) \ 1800 338 399 MW -5 (23-25) MW -5 (23-25)* 430, 413 , ` Laboratory Duplicate ADry-weight basis Total Solids _ (%) 84.67 84.67 81.95 90.42 79.15 80.22 78.89 79.09 76.81 . 86.68 86.58 86.34 79.45 75.93 74.05 74.05 000296 ) ^3058 Research Drive LS tate College, PA 16801, USA 814.272.1039 * F : 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDENTIALITY-- Exygen Research {"Exygen," "us," or "w e"} maintains the strictest confidentiality in ail o f our client interactions, if a signed confidentiality agreement is required, 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 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 Order, terms o f payment are "N et 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 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 o f 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 for hold times that are missed due to such changes. RUSH SERVICE--Exygen routinely offers expedited turnaround times on critical analyses. Rush analysis services are contingent upon availability and prearrangement with an authorized Exygen representative. A surcharge is usually added to the list fee if rush analysis is requested. M IN IM U M FEE--The minimum fee for commercial services is one hundred dollars ($100). SAMPLE COLLECTION/SUBMISSION--Client shall be responsible fo r 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 clieht prior to acceptance by an Exygen sample custodian. Exygen w ill 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 o f 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 o f the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery o f sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SAMPLE DISPOSAL--Exygen retains samples for one month after reporting results, then disposes o f or returns the sample. Unless the client 0 requests that the sample(s) be returned, or prior arrangements have been made for long-term storage, Exygen shall dispose of the sample. Exygen shall charge a monthly fee for long-term storage. Samples found or 1suspected to contain hazardous waste, according to definitions in state and /o r federal guidelines, will be returned to the client upon completion of the analysis. The cost o f returning the sample will be invoiced to the client. Exygen reserves the right to charge a disposal fee 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 interna! chain-of- custody 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 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 i" 1 shall be the exclusive responsibility of the client to confirm that Exygen's ; j standard practices will meet the client's needs prior to placing an order fo r - 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 ~j 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 o f the highest possible professional ethics. Each Exygen employee is required to sign a statement of persona! and professional integrity. ___ i ;J SPECIAL REPORTS--Additional charges may be necessary for custom report formats. " LITIGATION--AM costs associated with compliance to any subpoena for documents, for testimony in a court of law, or for any other purpose relating to work performed by Exygen Research shall be invoiced by Exygen and paid by client. These costs shall include, but are not limited to, hourly charges for the persons involved, travel, mileage, and accommodations, and fo r any and all other expenses associated with said litigation. ___ . r_ INDEMNIFICATION, LIABILITY, A N D INSURANCE--Exygen agrees to indemnify, defend, and save the client, its officers, directors, employees, agents, and representatives harmless from all losses, expenses, demands,. -- and claims made against the client, its officers, directors, employees, agents and representatives because o f any personal injuries, death, or property damage to the extent caused by the negligence or willful misconduct of Exygen, its employees, agents, or representatives in connection with the " performance of services under this agreement, except to the extent such losses, expenses, demands, or claims, occur as a result o f the negligent or willful acts or omissions o f the client, its officers, directors, employees, agents, and representatives; however, such indemnification and damages ~ shaii, 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 o f insurance from its carrier - evidencing appropriate insurance coverage. , WARRANTY A N D LIM ITS O F 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 SORs. We disclaim any ' other warranties, expressed or implied by law. Exygen does not accept any ' legal responsibility fo r 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 o f work. < 1 i* - |H : Cl ! ' frU - , 5P 4; : 'fH i* j; 'p S um m ary o f PFO S in Soil S am ples Sam ple ID Analyte Found (ng/g) PFOSA \ M W -4 (0-2) IVW-4 (3-5) MW-4. (8-10) M W -4 (13-15) MW -4 (13-15)* MW -4 (18-20) \ MW-4 (28-30) \ MW-3 (4-6) . MW-3 (9-11) \ MW -3 (14-16) , MW-3 (19-21) \ 333 5130 350 129 128 99.1 57.9 2230 155 53.4 16.9 ` Laboratory Duplicate ADry-weight basis Total Solids (% ) 88.07 83.17 80.21 80.32 80.32 77.80 68.10 83.49 84.75 74.92 81.95 7 -r. \ 000237 r* ^ ^ 3 0 5 8 Research Drive M m u ta te College, PA 16801, USA 814.272.1039 m F : 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDENTIALITY-- Exygen Research ("Exygen," " us," or "w e" ) maintains the strictest confidentiality in all o f our'dieht interactions, if a signed confidentiality agreement is required, 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 Exygen's reputation or business. Approval must be obtained, in writing, before Exygen's name can be published in any way. CONTRACTS--N il contracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer. . PAYMENT TERMS--Unless otherwise set forth in this Purchase Order, terms o f 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 o f 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 wifi not be responsible for hold times that are missed due to such changes. ' RUSH SERVICE--Exygen routinely offers expedited turnaround times on critical analyses. Rush analysis services are contingent upon availability and prearrangement with an authorized Exygen representative. A surcharge is usually added to the list fee if rush analysis is requested. M IN IM U M REF--The minimum fee for commercial services is one hundred dollars ($100). SAMPLE C O LLE C rtO N /S U B M S S S IO N -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 o f 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 samp!e(s). By request, Exygen will provide chain-of-custody forms for client's use. . All samples submitted must be accompanied by: purchase order, or signed quotation; sample description, including sample type, source, time and date of collection; specific analyses requested; estimated concentration levels; requested report date; current billing address; and 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 ail appropriate safely precautions. Clients requesting oyernight delivery of sample containers will be invoiced for freight., Exygen reserves the right to charge a fee for sample containers. SAMPLE DISPOSAL-- Exygen retains samples for one month after reporting results, then disposes of or returns the sample. Unless the client requests that the sample(s) be returned, or prior arrangements have been made for long-term storage, Exygen shall dispose of the sample(s). Exygen shall charge a monthly fee for long-term storage. Samples found or suspected to contain hazardous waste, according to definitions in state and /o r federal guidelines, will be returned to the client upon completion of the analysis. The cost of returning the sample(s) will be invoiced to the client. Exygen reserves the right to charge a disposal fee for the disposal o f 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 o f samples received. HAZARD COMMUNICATION--The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law. QUALITY ASSURANCE--Exygen will 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 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--Exygen Research strives to provide its clients with the highest quality data in the fastest realistic turnaround time. We balance the high standards of this goal by insisting that each employee also perform within the guidelines of the highest possible professional ethics. Each Exygen employee is required to sign a statement o f 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 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 fo r any and all other expenses associated with said litigation. INDEMNIFICATION, LIABILITY, AN D INSURANCE--Exygen agrees to indemnify, defend, and save the client, its officers, directors, employees, agents, and representatives harmless from ail losses, expenses, demands, and claims made against the client, its officers, directors, employees, agents arid representatives because o f any personal injuries, death, or property damage to the extent caused by the negligence or willful misconduct of Exygen, its employees, agents, or representatives in connection with the performance of services under this agreement, except to the extent such losses, expenses, demands, or claims, occur as a result o f 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 o f (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 o f insurance from Its carrier evidencing appropriate insurance coverage. WARRANTY A N D LIM ITS OF LIABILITY-- In accepting analytical work; Exygen guarantees the accuracy o f the test results for the sample as submitted within the tolerances set forth in the SOPs. We disclaim any other warranties, expressed or implied by law. Exygen does not accept any legal responsibility for the purposes for which client uses the 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 o f work. Report 1-- Analytical ^ 'fr* h Xfc -H j( ""k ' r r- i; S um m ary of PFO S in Soil Sam ples Sam ple ID Analyte Found (ng/g) PFOSA \ MW-1 (0-2) MVy-1 (8-10) M W -6 (0-2) M W -6 (4-6) M W -6 (9-1 i ) MW -6 (9-11)* MW -6 (14-16) \ MW -6 (19-21) \ MW -6 (24-26) \ 1700 394 1970 4850 1970 1980 3450 1430 372 ` Laboratory Duplicate ADry-weight basis Total Solids (% ) 85.85 80.12 94.85 82.13 84.66, 84.66 84.86 80.88 78.28 0 lH tj MV h \ 000298 r ^ ^ 3 0 5 8 Research Drive M m S ta te College/ PA 16801, USA r 814.272.1039 F : 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDENTIALITY---Exygen Research ("Exygen," "us," or "w e ") maintains the strictest confidentiality in all of our client interactions. If a signed confidentiality agreement is required, we will provide one. If a regulatory or legal body subpoenas information, 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---M ess otherwise set forth in this Purchase Order, terms of payment are "Net 30 Days." The time allowable fo r payment shall begin after both: (a) client's receipt o f Exygen's invoice; and (b) the satisfactory performance o f 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 o f 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 for hold . times that are missed due to such changes, RUSH SERVICE-- Exygen routinely offers expedited turnaround times on critical analyses. Rush analysis services are contingent upon availability and prearrangement with an authorized Exygen representative. A surcharge is usually added to the list fee if rush analysis is requested. M IN IM U M FEE--The minimum fee for commercial services is one hundred dollars ($100). SAMPLE COLLECTION/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 w ith 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 o f 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 o f sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SAMPLE DISPOSAL--Exygen retains samples fo r one month after reporting results, then disposes of or returns the sample. Unless the client n requests that the samplefe) be returned, or prior arrangements have been made for long-term storage, Exygen shall dispose of the sample(s). Exygen shall charge a monthly fee for long-term storage. Samples found or , suspected to contain hazardous waste, according to definitions in state and /o r federal guidelines, will be returned to the client upon completion o f the analysis. The cost of returning the sample(s) will be invoiced to the client. Exygen reserves the right to charge a disposal fee for the disposal o f any nand all samples unless returned by Exygen to client. Exygen shall, unless the nature and character o f 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 n the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law. QUALITY ASSURANCE--Exygen will 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 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 --1 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 of this goal by insisting that each employee also perform within the guidelines of the highest possible professional ethics. Each Exygen employee is required to sign a 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 fo r _ documents, for testimony in a court o f 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, A N D INSUR ANCE-Exygen agrees to 1 indemnify, defend, and save the client, its officers, directors, employees, agents, and representatives harmless from all losses, expenses, demands, ~ and claims made against the client, its officers, directors, employees, agents and representatives because o f any personal injuries, death, or property damage to the extent caused' by the negligence or willful misconduct of Exygen, its employees, agents, or representatives in connection with the |performance o f 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 o f 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 o f (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 o f insurance front its carrier evidencing appropriate insurance coverage. WARRANTY A N 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 SOPs. We disclaim any other warranties, expressed or implied by law. Exygen does not accept any legal responsibility for the purposes fo r which client uses the test results. Exygen will not accept any purchase order or any other order for work that includes conditions that vary from these Standard Conditions. ACCEPTANCE OF PURCHASE ORDER--This Purchase Order becomes a binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement o f work. ' Proven Results. R ecovery S um m ary fo r PFO S in Soil Sam ple Description MW-2 (0-2) 50 ng/mL Spike MW-5 (23-25) 50 ng/mL Spike MW -4 (13-15) 25 ng/m L Spike M W -6 (9-11 ) 250 ng/mL Spike Amount Spiked (ng /m L ) Amt Found Amount in S a m p le R ec o ve red R ec o ve ry (ng/m L) (ng/m L) (% ) 250 201 516 126 50 39.8 78.8 78 25 13.0 34.1 84 250 209 512 121 / 000299 J & 3 03505*8 Research Drive State College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com Composite Number of Containers 000300' CHAIN O F CUSTODY/ANALYSIS REQUEST FORM RESEARCH PROJECT INFORMATION Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.cLm Page I of ^ ANALYSES REQUESTED Client (name & address): A v, r?A !Cx?rT< il u <7 2 L \0 A l ctLuAU. , A \~ 3 5 1 e k O Phone: / Z M o \ 3 B 3 ~ / A 5 2 - Fax: r z a g y . * * 3 - Samoler: Vm now MS . Project Manager (Name & E-mail Address): ... ____ ( k Project Name: ev/.-C qsk\---------------7 ,. . JS/iL.'ildr'n A m enV cc. U ^ e ll Xn$ulm<rn ro. #: 7 rx ^ ~ ru o ^ 7 .k -tc ,-z . Quotation # : Please fill out this form completely to ensure correct analysis and proper handling of your samples. o $4 <35 ao>-< T Si k - SAMPLE ANALYSIS .a ExyLIMS# Client Sample Identification Collection Collection Date Time o2 M liV Z (O -Z ^ ` ''v-/- JAk \ - 2 t 3 - S \ ... , M \ A ~ Z II 15! iD TTO" I.V2 1 15,'30 Y A W ' Z r io ts ') X Z / /S?-7/>') M uV 2 rtZ-Z") A \ "2 / iv. m / Xtb'.os x JWS M V & -Z __N Ilf 3 5 ----- Specify Matrix Comments \/ - -< c> 24o. t/ l7 1/ . j/ / -- -- -- -- --- - | CHAIN OF CUSTODY Relinomsbld by Date lim- Time / `.CO OTHER INFORMATION Cruder ID # { H fe Cooler Temp. (Q % <j Received by: Date , //A A ",r ' -'v-^-V'0 - . ' Time tHU LAB USE ONLY v PROJECT REQUIREMENTS Results Deadline: ,*5 W L > rd Laboratory Report Options: Q Sample results only A dd'case narrative Add quality control summary 0 Add calibration summary ' 0 Add raw data 0 O ther__________ I I,I 1 L { l ( L i i l i ! L I I I I /.3-ot D00301 CHAIN O F CUSTODY/ANALYSIS REQUEST FORM Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 * exygenresearch.dom Fae Z f /.... PROJECT INFORMATION ANALYSES REQUESTED Client (name & address); . Project Manager (Name & E-mail Address): kv\ _______________ Project Name: Phone Fax: ----------- Sampler: iQ v - -- RO. # : & >> Z c g > 3 ~ 0 (c S 2 A Quotation # : '______________________ / Please fill out this form completelyto ensure correct analysis and proper handling of your samples. *1 sta Jd? V) Q <5r SAMPLE ANALYSIS ExyLIMS# Client Sample Identification jA ^ ~ 5 lQ r Z AUS-.S 3-5 a v a - 5 . rs -/o . MV-S /J3-/.3 A ltV f/ g - 3 9 . AV>- / 3 -Z 5 . EAv Ei>~24 TT- 1 3 /3-5S LAB USE ONLY Collection Collection Date Time ESfc a m u # y i a > JJ2&. l L ir .z o UM >5:60 3/ 3 "o S2 MoCL E ai.E fcJSc o 3O u Z U Specify Matrix 351 vr Comments CHAIN OF CUSTODY Relioaui^ed by ^ --Z sy Z r O ` CL-> Date Time u/bjt>3 iUeo Cooler ID # Received by A * Cooler Temp. (C) ^ / Date " / Time nh'Thi /Ho 'a* OTHER INFORMATION % LAB USE ONLY ItI ii Li JoS 1 v V 3 3 PROJECT REQUIREMENTS Results Deadline: . ____l^ n c /d ru - ______ Laboratory Report Options: 0 Sample results only 0 Add1cate narrative 0 Add quality control summary 0 Add calibration summary 0 Add raw data 0 Other ___________ l l JV. 3- L Composite Number of Containers 000302 CHAIN O F CUSTODY/ANALYSIS REQUEST FORM RESEARCH Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA T: 8 1 4.231.8032 F: 8 1 4.231.1580 exygenresearch.com 5? ( jd "age _ ^ 2 L - t-- I-- PROJECT INFORMATION Client (name & address): , AWey g k< 5\ Project Manager (Name & E-mail Address): ____ ~7>h hiY\ S i m ------------------- ANALYSES REQUESTED 3 * ' '- -- -- - ' I ... ......... - Phone: . - Fax: Sampler: >- .. : . H - ............... I. - Proiect Name: .........- ................ . P.O. # : Quotation # : -- .................................... ; 1 t- f Please fill out this form completely to ensure correct analysis and proper handling of your samples. u SAMPLE ANALYSIS ExyLIMS# Client Sample Identification U \ ~ 4' ' . ( 1 3 - / 5 ) W w M f z% -3 o y /A -/.S 'V" ' M -H \ AVN-^ /iM -IU S Collection Collection Date Time i i f f h H :o5 rfw s H :z$ > S. W3 w o^U 5 f,2 5 J3 o2 * i X h V Y i A D I IC C r > M I V w . n, Specify JVlatrix Comments \/ I V si %/ V !1 -- 1 PROJECT REQUIREMENTS Results Deadline: ____ __ Laboratory Report Options: Sample results only Add case 'narrative Add quality control summary Add calibration summary Add raw data Other_________ -l l I L I r-02 l .... Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L1278 PFOS 499 -> 99 NA R A W DATA REPORT Limit of 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: 121803A Karen Risha LC/MS/MS Unit #6 12/18/03 12/19/03 Exygen ID XC121603-0 XC121603-1 XC121603-2 XC121603-3 XC121603-4 XC121603-5 XC121603-6 Methanol Wash Reagent Blank Reagent Spk A Reagent Spk B L1278-1 SpkC L1278-14 Spk D XC121603-1 XC121603-2 L1278-1 L1278-1 Rep L1278-2 L1278-3 L1278-4 L1278-5 XC121603-3 L1278-6 L1278-7 L1278-8 L1278-9 L1278-10 XC121603-4 L1278-11 L1278-12 L1278-13 L1278-14 L1278-14 Rep XC121603-5 XC121603-6 Sponsor Sample ID Code -c - CS - CS - CS - CS - CS - -` NA CS c c NA LCS NA LCS MW-2 (0-2) LF MW-5 (23-25) LF - CS - MW-2 (0-2) MW-2 (0-2) MW-2 (3-5) MW-2 (8-10) MW-2 (13-15) MW-2 (18-20) CS s s s s s s MW-2 (23-25) MW-2 (28-30), MW-2 (33-35) MW-5 (0-2) MW-5 (3-5) CS s s s s s MW-5 (8-10) MW-5 (13-15) MW-5 (18-20) CS s s s MW-5 (23-25) MW-5 (23-25) S s - CS - CS Run No. 121803A-101 121803A-102 121803A-103 121803A-104 121803A-105 121803A-106 121803A-107 121803A-108 121803A-109 121803A-110 121803A-111 121803A-112 121803A-113 121803A-114 121803A-115 121803A-116 121803A-117 121803A-118 121803A-119 121803A-120 121803A-121 121803A-122 121803A-123 121803A-124 121803A-125 121803A-126 121803A-127 121803A-128 121803A-129 121803A-130 121803A-131 121803A-132 121803A-133 121803A-134 121803A-135 Analyte Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Std. Cone. (ppo 0 25 50 100 250 500 1000 - - - - - - 25 50 100 - 250 - - - - 500 1000 Dilution Factor - - - - - - - - 1 1 1 1 1 - - 1 1 1 1 1 1 - 1 1 1 1 1 1 1 I 1 1 - - Peak Area 0 647 1445 2887 7007 15370 26924 0 0 1616 15247 2141016 712081 743 1294 2881959 2507088 3209743 3213363 259017 300173 2621 281116 629941 260205 4503248 892672 7168 2949395 685468 788833 790001 811878 14318 26663 Analyte Found (ppo - - - - Amount Added (ppo - - Recovery (%) . - - - - Analyte Found (ppb) - - - - - -- -- ND 57.8 50 548 500 A 500 A 500 --******- -- ***** -***- *- *- - - - 116 110 - - - - - - - - - - - - - - - - - - -- - - -- -- Standard Curve: Linear (1/x weighted) Intercept = 11.5876 Slope =27.7786 Coef. OfDet. = 0.995722 Total Solids m . - - - - - - - - - - - 84.67 84.67 81.95 90.42 79.15 80.22 - 78.89 79.09 76.81 86.68 86.58 86.34 79.45 75.93 74.05 74.05 - - Analyte Found (ppb) = [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight = analyte found (ppb) x (100% / total solids (%)) CS = Calibration standard C = Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike CK = Check Standard ND - Not detected = Response between 0 and 25 ppt NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) ASample requires higher spiking level. See data set 122203A Sample requires dilution. See data set 122203A. Spreadsheet prepared by: Oh Analyte Found (ppb) Dry Weight _ - - - - - - - - - n RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internai Chain of Custody/Fortification Sheet Exygen Study Number: L1278 Matrix: Soil Spo_n__so__r _S_t_u_d,,y_/P__ro__to_c_o_l No.: NA T he samples listed below w ere removed from refrigerator No. 3 7 - Date_ CLIENT SAMPLE ID EXYGEN ID NUMBER W EIG H T (g) FO R TIFIC A TIO N (ng) na na na MW-4 (13-15) MW -6 (9-11) M W -4 (0-2) M W -4 (3-5) M W -4 (8-10) MW-4 (13-15) MW -4 (13-15) MW -4 (18-20) MW-4 (28-30) M W -3 (4-6) MW-3 (9-11) MW-3 (14-16) MW-3 (19-21) M W -1 (0-2) MW-1 (8-10) M W -6 (0-2) M W -6 (4-6) M W -6 (9-11) MW -6 (9-11) MW-6 (14-16) MW-6 (19-21) MW -6 (24-26) Reagent Spk A Reagent Spk B L1278-18 SpkC L1278-29 SpkD Reagent Blank Reagent Spk A Reagent Spk B L1278-18 Spk C L1278-29 SpkD L1278-15 L1278-16 L1278-17 L1278-18 L1278-18 Rep L1278-19 L I278-20 L1278-21 L1278-22 L I 278-23 L1278-24 L I 278-25 L I278-26 L I 278-27 L I 278-28 L1278-29 L I278-29 Rep L1278-30 L1278-31 L I278-32 Spiking Solution Used F061703-10 (lOng/mL) F061703-9 (100 ng/mL) F061703-9 (100 ng/mL) F061703-9 (100 ng/mL) - - _ 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - 2.0 20.0 20.0 20.0 - Initiai/Date /e to ls A All samples w ere weighed on balance No. T im e Date 1 2 - jiQ jo S Initials. A fter weighing samples w ere returned to>remfrisgeerraattor No. 32- Tim e ( 2 7 1 0 ________ Date /X- Initials C om m ents: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: C ) 2- j Analysis Sum m ary: Data Set: \24 2 D ata S e t:. 122 Data S et:. Set extraction/analysis data verified by: -^ Initials/D ate:-.----| j j ~ ! In itials/D ate:. In itials/D ate:. D ate:. p-lsp/ts 0 0 0 3 0 5 1 11 11 3058 Research Drive Phone: 814-272-1039 !'RES A RC H State College, PA 16801 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L1278 MATRIX: Soil METHOD: 01M-008-046 Rev 1 (Modified) ANALYTES: PFOS PROTOCOL NUMBER: NA Client ID na na na MW-4 (13-15) MW-6 (9-11) MW-4 (0-2) MW-4 (3-5) MW-4 (8-10) MW-4 (13-15) MW-4 (13-15) MW-4 (18-20) MW-4 (28-30) MW-3 (4-6) MW-3 (9-11) MW-3 (14-16) MW-3 (19-21) MW-1 (0-2) MW-1 (8-10) MW-6 (0-2) MW-6 (4-6) MW-6 (9-11) MW-6 (9-11) MW-6 (14-16) MW-6 (19-21) MW-6 (24-26) *Initials/Date Exygen ID Reagent Blank Reagent Spk A Reagent Spk B L1278-18 Spk C L1278-29 Spk D L1278-15 L1278-16 L1278-17 L1278-18 L1278-18 Rep L1278-19 L1278-20 L1278-21 L1278-22 L I278-23 L I278-24 L I278-25 L I278-26 L1278-27 L1278-28 L1278-29 L I278-29 Rep L1278-30 L1278-31 L1278-32 STEP STEP 12 \ STEP 3 STEP 4 l STEP 5 STEP 6 Dilutions (mL/mL) - -- - -- -- -- -- -- $f C& CkS CBS y\A 5 'ik ik r L V Ces /\ CBS tzjitijt -- -- -- -- STEP 7 Dilutions (mL/mL) -- -- - -- <- 'V\0 STEP 8 - -- -- -- - '/t 0 y io o-Ko O,0V \.O V .o # y p . w/ . o o o -V t.o 7>0-'Ao-Xc 'Vto 6VX. #V7.x> rePVio^Yi.o Y i 1/ Reagents/ Materials Methanol C18 SPE L o t# 433o h m s Type I Water , . - Initials/Date _ _ _ . . . - NA - - C e r o J(r t l 1 S _ . _ _ - '' _ _ _ - HPLC Methanol Ammonium Acetate Type I water - NA , L- 1 s k > lnitials/Date : |ii s 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 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. 0 32- 0&C jFinal extracts stored in refrigerator Initials: Date: {2. Initials and date under each step indicates the personnel that performed this step. July 19, 2001/4 Ev en RESEARCH s 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Exygen s t u d y NO, j-feTb Protocol No.: None Method No.: M Sponsor Sample BD NA NA NA NA NA Exygen Sample ID 0106020 0106020 0106020 0106020 0106020 Sample Description Type I WaterA Type I WaterA Type I W ater'' Type I WaterA Type I Water* Exygen Study No.: NA Analytes: C4.C5.C6.C7 and C8 Acids: C4. C6 & C8 Sulfonates Fort. Solution ID Fort. Soin. Cone. (ng/mL) Fort. Volume (ML) Micropipet used (ml) Fort. Level (ppt) -- F061703-10 10 100 200 . 25 F061703-10 10 200 200 50 F061703-10 10 400 200 100 F061703-9 100 100 200 250 Matrix: Type I WaterA Sample Vol: 40 mL Final Solution ED#** X C121603-0 XC121603-1 X C 121603-2 XC121603-3 -XC121603-4 Reagents/ Materials Methanol C18 SPE Type I Water - - L o t# NA - NA 0106020 Type I Water* F061703-9 100 200 200 500 XC121603-5 NA 0106020 Type I Water* F 061703-9 100 400 200 1000 XC121603-6 - - -- - - - - -- - c& . - - - - - - - - - Initials/Date: I3.|M 0 3 Vertical arrows in a column indicate identical values. **This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3. etc. Samples removed from pefrigerato^ / freezer # 3 2 - Time: O l ^ D Initials/Date: f'E E / iT-ljitjcZ 40 mL of each sample measured using a S O mL graduated cylinder. Initials/Date: CCE /iz-junln^ T H IS IS AN EXACT C O PY O F After measuring, samples returned tOjfeffigeragir / freezer # 3 2 Time: 1'2-bo Samples fortified: Initials/Date: CJct. /izjiLfjo'i Initials/Date: C'E ! i z j t b j c R T H E ORIGINAL DOCUM ENT* H V . h At P 12.^2240 3 SPE clean-up (omitting 40% Wash): Initials/Date: CEE /vzjupicz " Final volume adjusted to 5 mL: Initials/Date: C.EE Extracts placed in refrigerator # 3 2 Initials/Date: i STANDARD EXPIRATION DATE: 12/30/03 Comments: AThis type I water has been filtered through a hypercarb filter $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water July 10, 2001/0 1 1I 1 1I 1) ] Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochei iicals.PRO\SampleDB\121803A Soil.SPL Printed: Thu Dec 18 14:49:09 2003 12-iie^os Vial File Name LIMS ID Client ID Sample Description 1 1 121803A-101 -- 2 2 121803A-102 -- 3 3 121803A-103 -- 4 4 121803A-104 -- 5 5 121803A-105 -- 6 6 121803A-106 -- 7 7 121803A-107 -- 8 92 121803A-108 -- 9 51 121803A-109 -- 10 52 121803A-110 -- 11 53 121803A-111 -- 12 54 121803A-112 -- 13 55 121803A-113 -- 14 2 121803A-114 -- 15 3 121803A-115 -- 16 56 121803A-116 -- 17 57 121803A-117 -- 18 58 121803A-118 -- 19 59 121803A-119 -- 20 60 121803A-120 -- 21 61 121803A-121 -- 22 4 121803A-122 -- 23 62 121803A-123 -- 24 63 121803A-124 -- 25 64 121803A-125 -- 26 65 121803A-126 -- 27 66 121803A-127 -- 28 5 121803A-128 -- 29 67 121803A-129 -- 30 68 121803A-130 -- 31 69 121803A-131 -- 32 70 121803A-132 -- 33 71 121803A-133 -- 34 6 121803A-134 -- 35 7 121803A-135 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC121603-0, 0 ng/L standard XC121603-1,25 ng/L standard XC121603-2, 50 ng/L standard XC121603-3,100 ng/L standard XC121603-4, 250 ng/L standard XC121603-5, 500 ng/L standard XC121603-6,1000 ng/L standard Methanol Wash Reagent Blank Reagent Spk A, 50 ng/L Reagent Spk B, 500 ng/L L1278-1 S pkC , 500 ng/L L1278-14 Spk D, 500 ng/L XC121603-1,25 ng/L standard XC121603-2, 50 ng/L standard L1278-1 L1278-1 Rep L1278-2 L1278-3 L1278-4 L1278-5 XC121603-3,100 ng/L standard L1278-6 L1278-7 L1278-8 L1278-9 L1278-10 XC121603-4, 250 ng/L standard L1278-11 L1278-12 L1278-13 L1278-14 L1278-14 Rep XC121603-5, 500 ng/L standard XC121603-6,1000 ng/L standard 000308 111I 1 Exygen STUDY N O . -- 1 1 ill Page 1 1 1Page Position: ( , ) Matrix Sample Type Cone (ng/L) Cone B ConcC Test ID DF MS Method ___ Blank 0 -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 -- Blank -- -- Blank -- -- QC 50 -- QC 500 -- QC 500 -- QC 500 -- Standard 25 -- Standard 50 -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Standard 100 -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Standard 250 -- Analyte ~ Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Standard 500 -- Standard 1000 0___ ___ ---- 0 ---- 0 ----0 ----0 ----0 ---- 0 ---- 0 ----0 ----0 ----0 ----0 ----0 ---- 0 ----0 --0 ---- 0 ----0 ----0 ----0 ----0 ----0 ----0 ----0 ---- 0 ----0 ----0 ----0 ----0 ---- 0 ---- 0 ----0 ---- 0 ----0 ----0 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 PFOS 1 ] I ] 1] ] I 1 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemiqals.PRO\SampleDB\121803A Soil.SPL Printed: Thu Dec 18 14:49:09 2003 Db HPLC Method MS Tune File Inj.Volume 1 PFOSand PFOA Fluorochems 15 2 PFOSand PFOA Fluorochems 15 3 PFOSand PFOA Fluorochems 15 4 PFOSand PFOA Fluorochems 15 5 PFOSand PFOA Fluorochems 15 6 PFOSand PFOA Fluorochems 15 7 PFOSand PFOA Fluorochems 15 8 PFOSand PFOA Fluorochems 15 9 PFOSand PFOA Fluorochems 15 10 PFOSand PFOA Fluorochems 15 11 PFOSand PFOA Fluorochems 15 12 PFOSand PFOA Fluorochems 15 13 PFOSand PFOA Fluorochems 15 14 PFOSand PFOA Fluorochems 15 15 PFOSand PFOA Fluorochems 15 16 PFOSand PFOA Fluorochems 15 17 PFOSand PFOA Fluorochems 15 18 PFOSand PFOA Fluorochems 15 19 PFOSand PFOA Fluorochems 15 20 PFOSand PFOA Fluorochems 15 21 PFOSand PFOA Fluorochems 15 22 PFOSand PFOA Fluorochems 15 23 PFOSand PFOA Fluorochems 15 24 PFOSand PFOA Fluorochems 15 25 PFOSand PFOA Fluorochems 15 26 PFOSand PFOA Fluorochems 15 27 PFOSand PFOA Fluorochems 15 28 PFOSand PFOA Fluorochems 15 29 PFOSand PFOA Fluorochems 15 30 PFOSand PFOA Fluorochems 15 31 PFOSand PFOA Fluorochems 15 32 PFOSand PFOA Fluorochems 15 33 PFOSand PFOA Fluorochems 15 34 PFOSand PFOA Fluorochems 15 35 PFOSand PFOA Fluorochems 15 oo W O 1 ]1 1 ] Exygen STUDY N O . U 3 7 ] ]]i Page 2 Page Position: (2,1 ) l LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L1278 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 E): 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: & 000310 Scanning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\PFOS Last Modified: Thu Dec 18 14:43:11 2003 Printed: Thu Dec 18 14:45:23 2003 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 M R M of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone 1 499.00 99.00 0.20 40 30 Page 1 Method Report Page 1 Method File: Last Modified: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\PFOSand PFOA Thursday, December 18, 2003 14s43:32 Printed: Thursday, December 18, 2003 14:45:33 p |l8 (o b HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60..0 40.,0 0 ..0 0 ..0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 9 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 C% D% Flow Pressure 0.0 0.0 0.300 400 0.0 0.0 0.300 400 0.0 0.0 0.300 400 0.0 0.0 0.300 400 0.0 0.0 0.300 400 0.0 0.0 0.400 400 0.0 0.0 0.400 400 0.0 0.0 0.400 400 0.0 "0.0 0.300 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 7.95 8.00 Column Switch Contact1 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 (1/min) Draw Position (mm) Stop Time (mins) Injection Volume (/il) Vial Number 200.0 200 0.50 14.00 15.0 7 Tuning Method Report Method: C: \MASSLYNX\FLUOROCHEMICALS. PRO\ACQUDB\FLUOROCHEMS Printed: Thu Dec 18 14:46:01 2003 Page 1 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 -46 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3. le- 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 Rdb 14.0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650 26 33 30 -64 Rdbk 130.7 752.7 000313 Quantify Calibration Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\CurveDB\121803A Soil Last modified: Mon Dec 22 07:52:52 2003 Printed: Mon Dec 22 07:54:15 2003 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121803A# Ext.Date:12/18/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Mon Dec 22 07:45:59 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Mon Dec 22 07:47:40 2003 i, Mon Dec 22 07:54:17 2003 Initials Date U-I73J&: Run#J2L ib S E ^ Name: 121803A-101 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Saiqple Report Study No.:I>1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Non Dec 22 07:45:59 2003 Method: P:\Data\LCNSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Non Dec 22 07:47:40 2003 Job Code: Printed: Non Dec 22 07:54:17 2003 Name: 121803A-102 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 000316 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Rage 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-103 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000317 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-104 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 000318 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-105 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 0003j 3 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Rage 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-106 Text: 1: C8 Sulfonate (PFOS) XC121603-5, 500 ng/L standard 121803A-106 Sm (Mn, 2x3) 100-1 %- 19-Dec-2003 04:43:56 LC/MS/MS #6 5.49 MRM of 1 Channel ES499 > 99 8.60e4 Area 0 1 ' p -1 T"i I-I-1-I 1 I.r i I T 'l I m I H T I p 1.00 2.00 3.00 r-r-p n 4.00 5.00 6.00 rnr","i'~r""i ' n 7 .0 0 i~n'1 I Tim e 8.00 Exygen Research, 3058 Research Drive, State College PA 16801 Quantify Sample Report Study No.:L1278, Set N o . :121803A, Ext.Date:12/18/03, AnalysttK.Risha Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-107 Text: 1: C8 Sulfonate (PFOS) XC121603-6,1000 ng/L standard 121803A -107 Sm (Mn, 2x3) 100n %- 19-Dec-2003 04:59:43 LC/MS/MS #6 5.50 M RM of 1 Channel ES499 > 99 1 .5 5 e 5 Area 0 ' ' I 1 ' ' I I 1 1 H ' f'T'V I T I T""] 1T"1""1T "1 1 1.00 2.00 3.00 4.00 5.00 6.00 ,r ,, r -p - r T-.'i-T-T'i-, I T im e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000321 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 8 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-108 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set N o . :121803A, Ext.Date:12/18/03, AnalysttK.Risha Page 9 S a m p l e List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-109 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Q0033 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 10 Sample List: Ps\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-110 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 y /K Quantify Sample Report Study Ho.:L1278, Set Ho.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 11 . Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Harne: 121803A-111 Text : 1: C8 Sulfonate (PFOS) Reagent Spk B, 500 ng /L 121803A -111 Sm (Mn, 2x3) 100n %- 5.49 1524' 19-Dec-2003 06:02:28 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 9.21 e4 Area 3.00 4.00 1 I 1 1 1 1 ! ' 1 1~ I ` 1 1 -p--r i r | I t I I "I"<I -TI t T im e 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive State College PA 16801 0 0325 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-112 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 ooos^e Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Harne: 121803A-113 Text: 1: C8 Sulfonate (PFOS) L1278-14 Spk D, 500 ng/L 121803A-113 Sm (Mn, 2x3) 100i %: 19-Dec-2003 06:33:55 LC/MS/MS #6 5.48 M RM of 1 Channel ES499 > 99 3.91 e6 Area O'-'t-i1 <~t r T "'~` 1 I 1 '1 '' I 1.00 I I I I I I I >-i r-|-in 2.00 3.00 4.00 5 .0 0 6.00 "I ' ' .' h 7 .0 0 Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 O e Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 14 Sample Lists P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-114 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0Q 0328 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-115 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:L1278, Set N o . :121803A, Ext.Bate:12/18/03, Analyst:K.Risha Page 16 Sample List: P:\Bata\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleBB\121803A Soil Last modified: Mon Bee 22 07:45:59 2003 Method: P:\Bata\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethBB\PFOS only 121803 Last modified: Mon Bee 22 07:47:40 2003 Job Code: Printed: Mon Bee 22 07:54:17 2003 Name: 121803A-116 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Brive, State College PA 16801 000330 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, AnalystsK.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-117 Text: 1: C8 Sulfonate (PFOS) L1278-1 Rep 121803A -117 S m (Mn, 2x3) 10Ch %: 5.50 19-Dec-2003 07:36:43 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 1.29e7 Area 0 |-I I I I r-1 I T -1 I - r - j , I I , I I I I I I . n , | - r . , - r - | r - r - i r ' | - r 1.00 2.00 3.00 4.00 5 .0 0 6.00 7.00 T im e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-118 Text: 1: C8 Sulfonate (PFOS) L1278-2 121803A-118 Sm (Mn, 2x3) 10O i 5.49 3209743 19-Dec-2003 07:52:38 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 1.57e7 Area 1.00 2.00 3.00 4.00 5.00 6.00 7.00 T~n T im e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000332 > Quantify Sample Report v Study No.:L1278, Set No.:121803A, Ext-Dates12/18/03, Analyst:K.Risha Page 19 r- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil ; Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 ^ Job Code: - Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-119 Text: 3* Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date12/18/03, AnalystK.Risha Page 20 Sandle List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-120 Text: 1: C8 Sulfonate (PFOS) L1278-4 121803A -120 Sm (Mn, 2x3) 100i %- 5.49 2590 19-Dec-2003 08:24:20 LC/MS/MS #6 M R M of 1 Channel ES499 > 99 1.40e6 Area 2.00 3.00 4.00 5.00 6 .0 0 7.00 Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:Ll278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-121 Text: 1 : C8 Sulfonate (PFOS) L1278-5 121803A-121 Sm (Mn, 2x3) 100-] %: I5.49 300173"! 1 19-Dec-2003 08:40:09 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 1.65e6 Area o1*-r-1--r~f"[ i i ` i i' 1I""fi~~ii i' r'~lI--i1i' i1 i111I--i1--i1-- i1--r1nI--i1--r1--i1--iH--]--iI---Ii--rI ,I TI",I iI rI--iIII I I I I I I I"t I I I I I I I I I I !I I 'I iI 'I 'I HI I 'I 'I ir''|h-f iI-Ii iI iI iI iI 'I 'I iI TI im e 1.00 2 .0 0 3 .0 0 4 .0 0 ________ 5 T )0 ________ 6 ,0 0 ________ 7X)0________ 8 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 77C Quantify Sample Report Study Ho.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil : Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 P" Job Code: Printed: Mon Dec 22 07:54:17 2003 Z"6'** Harne: 121803A-122 Text : Exygen Research, 3058 Research Drive, State College, PA 16801 ooo3-?e Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Rage 23 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-123 Text: 1: C8 Sulfonate (PFOS) L1278-6 121803A-123 Sm (Mn, 2x3) 100n %: 0 *I -1--I 11--p i i l I I I I i l I T I I "I I.r I.i- | I I I I I I I I I I1I I I" I p I 1.00 2 .0 0 3.00 4.00 5.49 5.00 19-Dec-2003 09:11:31 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 1.51e6 Area 6 .0 0 1r> 1 p 1 1 1 ' ' ' ' I T im e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Rage 24 /'**' Sample List: P:\Data\LCMSMS6\Masslynx\Pluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 ^ Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-124 Text: 1: C8 Sulfonate (PFOS) L1278-7 s 121803A -124 Sm (Mn, 2x3) 10CH %: 0 i t I " H r - r - i - r | i i i i | . i i . | ' i i r i | t i i...., 1.00 2 .0 0 3.00 19-Dec-2003 09:27:16 LC/MS/MS #6 5.49 M RM of 1 Channel ES499 > 99 3.46e6 Area 4 .0 0 T--T 5.00 6.00 f ' '-I [ n '.r I I t | T im e 7.00 8.00 r Exygen Research, 3058 Research Drive, State College, PA 16801 000338 , Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil / Last modified: Mon Dec 22 07:45:59 2003 , Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-125 Text: 1: C8 Sulfonate (PFOS) L1278-8 121803A-125 Sm (Mn, 2x3) 100n %: . Q I r r .., !-j.,, i-r i j'-i i-ri j "T-i r i [ i I i- r -j r i r-T j >-- t 1.00 2.00 3.00 4.00 19-Dec-2003 09:43:03 LC/MS/MS #6 5.49 M R M of 1 C hannel E S - 499 > 99 1.42e6 Area 1 i 1 1 l T l 11 1 1 i 1 1 r , -1T"r'-'"h I i `"'i T im e 5.00 6.00 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000330 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 26 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil , Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 ^ Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-126 Text: 1: C8 Sulfonate (PFOS) L1278-9 121803A -126 Sm (Mn, 2x3) 100i iCN %- 19-Dec-2003 09:58:50 LC/MS/MS #6 5.49 M RM of 1 Channel ES499 > 99 2.35e7 Area 0 1 1 1 I I `-I < I > 1 I 1 1 1 1 n 1 1.00 2.00 1-T-r-T 3.00 4.00 5.00 6.00 .T ' ` 11`T ' ` -'-I I T im e 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000340 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 27 f~. Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 f*'' Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-127 Text: 1: C8 Sulfonate (PFOS) 1*0 Z ** I Exygen Research, 3058 Research Drive, State College, PA 16801 000341 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, AnalystsK.Risha Page 28 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-128 Text: 1: C8 Sulfonate (PFOS) XC121603-4, 250 ng/L standard 121803A-128 Sm (Mn, 2x3) 100-1 %- 5.48 7168 19-Dec-2003 10:30:23 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 4 .2 8 e 4 Area 0-H Tim e 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000342 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Bate:12/18/03, Analyst:K.Risha Page 29 Sample List: P:\Bata\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleBB\121803A Soil Last modified: Mon Bee 22 07:45:59 2003 Method: P:\Bata\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethBB\PFOS only 121803 Last modified: Mon Bee 22 07:47:40 2003 Job Code: Printed: Mon Bee 22 07:54:17 2003 Name: 121803A-129 Text: Exygen Research, 3058 Research Brive, State College, PA 16801 O - &-i Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 30 f" Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil ' Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 ^ Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-130 Text: 1: C8 Sulfonate (PFOS) / Exygen Research, 3058 Research Drive, State College, PA 16801 000344 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K. Ri sha Rage 31 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-131 Text: 1: C8 Sulfonate (PFOS) L1278-13 121803A-131 Sm (Mn, 2x3) 10CH 5.47 788833 19-Dec-2003 11:17:34 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 4 .1 5 e 6 Area 1.00 2.00 3.00 4.00 --I 1 1 * 5.00 6.00 7.00 Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 /* t-*' Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K .Risha Page 32 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-132 Text : 1 : C8 Sulfonate (PFOS) L1278-14 121803A -132 Sm (Mn, 2x3) 1 0 (h %- 5.46 79000 19-Dec-2003 11:33:26 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 3.87e6 Area 0 1 I 1 1 1 1 I "r ' '...H 1 1 ` 1 I 1 1 I '' 1.00 2.00 3.00 4.00 5.00 6.00 T im e Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Dates12/18/03, AnalystsK.Risha Page 33 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Mon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-133 Text : 1: C8 Sulfonate (PFOS) L1278-14 Rep 121803A-133 Sm (Mn, 2x3) 10Ch %- 5.46 811878 19-Dec-2003 11:49:17 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 3.99e6 Area 1.00 2.00 3.00 4.00 T 5.00 6.00 ' "H ' r 7.00 I i "i i i T im e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 3 4 .7 Quantify Sample Report Study No.:Iil278, Set No.:121803A, Ext.Dates12/18/03, Analyst:K.Risha Page 34 S a m p l e L i s t : F:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Hon Dec 22 07:45:59 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-134 Text: 1: C8 Sulfonate (PFOS) XC121603-5, 500 ng/L standard 121803A -134 Sm (Mn, 2x3) 100] %: 19-Dec-2003 12:04:54 LC/MS/MS #6 5.46 M RM of 1 Channel ES499 > 99 8 .0 3 e 4 Area 0 I t-|- i -n -r-p I r11 1 I T"T"T' '.T-| 'in' |-I~| -TT I T~| T im e 1.00 2 .0 0 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 348 Quantify Sample Report Study No.:L1278, Set No.:121803A, Ext.Date:12/18/03, Analyst:K.Risha Page 35 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121803A Soil Last modified: Hon Dec 22 07:45:59 2003 . Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 07:54:17 2003 Name: 121803A-135 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000349 /"-- Sponsor Study No: ! Exygen Study No: Analyte: Ions Monitored: Site: NA L1278 PFOS 499 -> 99 NA R A W DATA REPORT Limit of 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: 121903A Karen Risha LC/MS/MS Unit #6 12/19/03 12/19-20/03 Exygen ID XC121603-0 XCI21603-1 XC121603-2 XC121603-3 XC121603-4 XC121603-5 XC121603-6 Methanol Wash Reagent Blank 1 Reagent Spk A Reagent Spk B '----- L1278-18 Spk C L1278-29 Spk D XC121603-1 L1278-15 L1278-16 L1278-17 L1278-18 L1278-18 Rep XC121603-2 L I278-19 L1278-20 L1278-21 L1278-22 L1278-23 XC121603-3 L1278-24 L1278-25 L1278-26 : J L I278-27 L1278-28 XC121603-4 L1278-29 L1278-29 Rep L1278-30 L1278-31 L1278-32 XC121603-S XC121603-6 Sponsor ID NA NA NA MW-4 (13-15) MW-6 (9-11) MW-4 (0-2) MW-4 (3-5) MW-4 (8-10) MW-4 (13-15) MW-4 (13-15) MW-4 (18-20) MW-4 (28-30) MW-3 (4-6) MW-3 (9-11) MW-3 (14-16) MW-3 (19-21) MW-1 (0-2) MW-1 (8-10) MW-6 (0-2) MW-6 (4-6) - MW-6 (9-11) MW-6 (9-11) MW-6 (14-16) MW-6 (19-21) MW-6 (24-26) - - Sample Code C CS CS CS CS CS CS c c LCS LCS LF LF CS s S s s s CS s s s s s CS s s s s s CS s s s s s CS CS Run No. 121903A-201 121903A-202 121903A-203 121903A-204 121903A-205 121903A-206 121903A-207 121903A-208 121903A-209 121903A-210 121903A-2U 121903A-212 121903A-213 121903A-214 121903A-215 121903A-216 121903A-217 121903A-218 121903A-219 121903A-220 121903A-221 121903A-222 121903A-223 121903A-224 121903A-225 121903A-226 121903A-227 121903A-228 121903A-229 121903A-230 121903A-231 121903A-232 121903A-233 121903A-234 121903A-235 121903A-236 121903A-237 121903A-238 121903A-239 Std. Cone. (ppt) 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Factor 1 1 1 1 1 1 1 1 1 1 1 1 l 1 1 1 1 1 1 1 1 1 1 1 1 - - Analyte Found (ppt) ss (peak area - intercept) / slope x DF ' Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Peak Area 0 629 1247 2383 7139 14059 25223 0 0 1429 14623 290097 2987439 1006 707243 5722416 658171 279838 409937 221760 1249 120111 3175225 341491 115544 41509 2423 2551765 756989 3208199 5338240 7366 2787671 2732608 4574666 2250395 697285 13797 24862 Analyte Found Amount Added Recovery Analyte Found (ppt) ND 51.2 558 A A * * * * * * * * * * ___ <EE2___ 50 500 500 500 ' ' - - -' *****- -** * **- -- <%) 102 112 - i p p ^ ___ - Standard Curve : Linear (1/x weighted) Intercept = 96.2077 Slope - 26.0335 Coef. Of Det. = 0.994530 Total Solids (%) 88.07 83.17 80.21 80.32 80.32 77.80 68.10 83.49 84.75 74.92 81.95 85.85 80.12 94.85 82.13 ' 84.66 84.66 84.86 80.88 78.28 - Analyte Found (ppb) = [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight = analyte found (ppb) x (100% / total solids (%)) CS = Calibration standard C = Control sample S = Sample LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike CK ss Check Standard ND as Not detected = Response between 0 and 25 ppt NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) ASample requires higher spiking level. See data set 122203A. Sample requires dilution. See data set 121903AR. Spreadsheet prepared by: Analyte Found (ppb) Dry Weight * '* * 000350 RESEARCH 3058 Research Drive State Colleg-e, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internai Chain of Custody/Fortification Sheet Exygen Study Number: L1278 Matrix: Soil Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. M - Time ________ Date / Z l i a i S Initials CLIENT SAM PLE ID na na na M W -2 (0-2) MW-5 (23-25) M W -2 (0-2) MW-2 (0-2) MW -2 (3-5) MW -2 (8-10) MW-2 (13-15) MW-2 (18-20) MW-2 (23-25) MW-2 (28-30) MW-2 (33-35) MW-5 (0-2) MW-5 (3-5) MW-5 (8-10) MW-5 (13-15) MW-5 (18-20) MW-5 (23-25) MW-5 (23-25) EXYGEN ID NUMBER Reagent Blank Reagent Spk A Reagent Spk B L1278-1 Spk C L1278-14 Spk D L1278-1 L1278-1 Rep L1278-2 L1278-3 L1278-4 L1278-5 L1278-6 L1278-7 L 1278-8 L I 278-9 L1278-10 L1278-11 L1278-12 L1278-13 L1278-14 L1278-14 Rep W E IG H T (g) _ _ _ 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 FO R TIFIC A TIO N (ng) _ 2.0 20.0 20.0 20.0 _ _ _ _ _ _ _ _ _ _ _ _ _ _ - Reagent Spk A Reagent Spk B L1278-1 SpkC L1278-14 SpkD Spiking Solution Used F061703-10 (10 ng/mL) F061703-9 (100 ng/mL) F061703-9 (100 ng/mL) F061703-9 (100 ng/mL) -- All samples were weighed on balance No.. 2 o Time m S O Date / 2 - j l t i / o S Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) - Initial/Date ( - /U lie to /te lia te Initials After w eighing samples were returnedl to refrigera tor No. Time 2 - 0 0 ________ Date /2 -1 1 8 /0 3 , Initials _Z 7A?T Com m ents: 200 (iL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initiais/Date: Analysis Summary: D ata Set: \2-)ftog>A In itials/D ate:. D ata Set: 1 2 1 ^ 6 ^ ^ - In itials/D ate:. D ata S e t:______ <-- In itials/D ate:. ( 2-J te > io 3 / P -lS / ^ j Set extraction/analysis data verified by: Date: &kjt& July 26, : 17 RE SE A RC H 1 "i i ' ) -i .... i 3058 Research Drive Phone:814-272-1039 State College, PA 16801 Fax: 814-231-1580 i SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: U 2 78 METHOD: OlM-008-046 Rev 1 (Modified) P R O T n rn r Knnumrm. *t* I * In itia ls/D a te STEP 1: 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 rpm STEP 4: Filter through glass acrodisc STEP 5: SPE column clean up 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. in itials and date under each step indicates the personnel that performed this step COMMENTS: ` _l: iru u cu s/u a ie kknotma uwuniffa,,uiajoS i f M O ~ Final extracts stored in refrigerator 3 2 - Initials: CE Date: /z fm j6* July 19, 2001/4 1 ]iiI 1 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorocti 5micals.PRO\SampleDB\121903A Soil.SPL Printed: Fri Dec 19 10:00:10 2003 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 o 39 o o CO :n CO Vial File Name LIMS ID Client ID Sample Description 1 121903A-201 2 121903A-202 3 121903A-203 4 121903A-204 5 121903A-205 6 121903A-206 7 1219Q3A-207 92 121903A-208 72 121903A-209 73 121903A-210 74 121903A-211 75 121903A-212 76 121903A-213 2 121903A-214 77 121903A-215 78 121903A-216 79 121903A-217 80 121903A-218 81 121903A-219 82 121903A-220 3 121903A-221 83 121903A-222 84 121903A-223 85 121903A-224 86 121903A-225 87 121903A-226 4 121903A-227 88 121903A-228 89 121903A-229 90 121903A-230 46 121903A-231 5 121903A-232 47 121903A-233 48 121903A-234 49 121903A-235 50 121903A-236 10 121903A-237 6 121903A-238 7 121903A-239 XC121603-0,0 ng/L standard XC121603-1,25 ng/L standard XC121603-2, 50 ng/L standard XC121603-3,100 ng/L standard XC121603-4, 250 ng/L standard XC121603-5, 500 ng/L standard XC121603-6,1000 ng/L standard Methanol Wash Reagent Blank Reagent Spk A, 50 ng/L Reagent Spk B, 500 ng/L L1278-18 Spk C, 500 ng/L L1278-29 Spk D, 500 ng/L XC121603-1, 25 ng/L standard L1278-15 L1278-16 L1278-17 L1278-18 L1278-18 Rep L1278-19 XC121603-2, 50 ng/L standard L1278-20 L1278-21 L1278-22 L1278-23 L1278-24 XC121603-3,100 ng/L standard L1278-25 L1278-26 L1278-27 L1278-28 XC121603-4,250 ng/L standard L1278-29 L1278-29 Rep L1278-30 L1278-31 L1278-32 XC121603-5, 500 ng/L standard XC121603-6,1000 ng/L standard ) 1 I 1' I Exygen STUDY N O . !1I I Page 1 Page Position: (1,1) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF MS Method _____ Blank -- Standard -- Standard Standard -- Standard -- Standard -- Standard -- Blank -- Blank -- QC -- QC -- QC -- QC -- Standard -- Analyte -- Analyte -- Analyte -- Analyte -- Analyte -- Analyte -- Standard -- Analyte -- Analyte Analyte -- Analyte -- Analyte -- Standard -- Analyte -- Analyte -- Analyte -- Analyte -- Standard -- Analyte -- Analyte Analyte -- Analyte -- Analyte -- Standard -- Standard 0 25 50 100 250 500 1000 -- -- 50 500 500 500 25 -- -- -- -- -- -- 50 -- -- ... -- -- 100 -- -- -- -- 250 ... -- -- -- -- 500 1000 _____ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 0 1 PFOS 1 1)I1 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroche iicals.PRO\SampleDB\121903A Soil.SPL Printed: Fri Dec 19 10:00:10 2003 HPLC Method MS Tune File Inj.Volum e 1 PFOSand PFOA Fluorochems 15 2 PFOSand PFOA Fluorochems 15 3 PFOSand PFOA Fluorochems 15 4 PFOSand PFOA Fluorochems 15 5 PFOSand PFOA Fluorochems 15 6 PFOSand PFOA Fluorochems 15 7 PFOSand PFOA Fluorochems 15 8 PFOSand PFOA Fluorochems 15 9 PFOSand PFOA Fluorochems 15 10 PFOSand PFOA Fluorochems 15 11 PFOSand PFOA Fluorochems 15 12 PFOSand PFOA Fluorochems 15 13 PFOSand PFOA Fluorochems 15 14 PFOSand PFOA Fluorochems 15 15 PFOSand PFOA Fluorochems 15 16 PFOSand PFOA Fluorochems 15 17 PFOSand PFOA Fluorochems 15 18 PFOSand PFOA Fluorochems 15 19 PFOSand PFOA Fluorochems 15 20 PFOSand PFOA Fluorochems 15 21 PFOSand PFOA Fluorochems 15 22 PFOSand PFOA Fluorochems 15 23 PFOSand PFOA Fluorochems 15 24 PFOSand PFOA Fluorochems 15 25 PFOSand PFOA Fluorochems 15 26 PFOSand PFOA Fluorochems 15 27 PFOSand PFOA Fluorochems 15 28 PFOSand PFOA Fluorochems 15 29 PFOSand PFOA Fluorochems 15 30 PFOSand PFOA Fluorochems 15 31 PFOSand PFOA Fluorochems 15 32 PFOSand PFOA Fluorochems 15 33 PFOSand PFOA Fluorochems 15 34 PFOSand PFOA Fluorochems 15 35 PFOSand PFOA Fluorochems 15 36 PFOSand PFOA Fluorochems 15 37 PFOSand PFOA Fluorochems 15 38 PFOSand PFOA Fluorochems 15 39 PFOSand PFOA Fluorochems 15 Q o CO 7l ) 1 "'] ! J 1 1 1 ) u mExygen STUDY NO Page 2 Page Position: (2,1 ) 1 LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L1278 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 Methano1 Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 My 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 I D 's bv: Scanning Method Report Method: C :\MA.SSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\ PFOS Last Modified: Thu Dec 18 14:43:11 2003 Printed: Fri Dec 19 10:00:17 2003 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 499.00 99.00 0.20 40 30 Page 1 000356 Method Report Method File: Last Modified Printed: Page 1 c :\masslynx\fluorochemicals.pro\acqudb\pfosand pfoa Friday, December 19, 2003 09:49:13 Friday, December 19, 2003 10:00:24 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 9 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 Pressure 400 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 7.95 8.00 Column Switch Contact1 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 (/1/min) Draw Position (mm) Stop Time (mins) Injection Volume ( i l ) Vial Number 200.0 200 0.50 14.00 15.0 64 000357 Tuning Method Report Method : C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\FLUOROCHEMS Printed: Fri Dec 19 10:00:44 2003 Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -31 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 2 . 9e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650 37 39 41 -648 Rdbk 130.3 752.7 Quantify Calibration Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Calibration: P :\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\121903A Soil Last modified: Mon Dec 22 08:12:36 2003 Printed: Mon Dec 22 08:13:21 2003 Rage 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000359 Quantify Sample Report Study No.:I>1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P :\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Initials_ Jfc:--------------------- DateJ E Run# J iZ m -3ol To 12iqo^A-2.^i Name: 121903A-201 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 3 GO Quantify Sample Report Study N o.:1.1278, Set No.:121903A, Ext.Bate:12/19/03, Analyst:K.Risha Page 2 Sample List: P:\Bata\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleBB\121903A Soil Last modified: Mon Bee 22 08:08:13 2003 Method: P:\Bata\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethBB\PF0S only 121803 Last modified: Mon Bee 22 07:47:40 2003 Job Code: Printed: Mon Bee 22 08:13:24 2003 Name: 121903A-202 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Brive, State College, PA 16801 Jfc- Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-203 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000332 Quantify Sample Report Study NO.:L1278, Set No.s121903A, Ext.Date:12/19/03, AnalystsK.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-204 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 003G2 Quantify Sample Report Study No. :L1278, Set No.:121903A, Ext .Date:12/19/03, Analyst :K. Ri sha Page 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-205 Text: 1: C8 Sulfonate (PFOS) XC121603-4, 250 ng/L standard 121903A-205 Sm (Mn, 2x3) 10Ch . %: 5.47 19-Dec-2003 15:28:49 LC/MS/MS #6 M R M of 1 Channel ES499 > 99 3.92e4 Area 0 n - I I I '* I I I r-r- r - r - p r - r ,'T j n | i" i 7 l i"r i T" P"' 1.00 2.00 3.00 4.00 5.00 6 .0 0 ~~^ .^ r r -^-r 7.00 Tim e 8.00 Exygen Research 3058 Research Drive, State College, PA 16801 334 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-206 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903a . Ext.Date:12/19/03, Analyst:K.Risha Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-207 Text: 1: C8 Sulfonate (PFOS) XC121603-6,1000 ng/L standard 121903A -207 S m (Mn, 2x3) 10Ch %- 5.46 25223 19-Dec-2003 16:00:13 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 1.38e5 Area 0 "T T -- I-- I-- I-- I-- r ~ l -- I-- 1-- !-- I "I" j 1 P 1 r 1 I"T'I1r-r I I 1.00 2.00 3.00 4.00 " 1I 1` ' ' I ' 111 I ' 1 1 ' I 1' ' ` I Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive State College PA 16801 oooac^e Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Dates 12/19/03, AnalystsK.Risha Rage 8 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-208 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0003^7 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-209 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0003G8 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Dates 12/19/03, AnalysttK.Risha Page 10 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-210 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 *7fcOf Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-211 Text : 1: C8 Sulfonate (PFOS) Reagent Spk B, 500 ng/L 121903A -211 Sm (Mn, 2x3) 10CH %- 5.46 14623 19-Dec-2003 17:02:50 LC/MS/MS #6 M R M of 1 Channel ES499 > 99 7.77e4 Area 1.00 2.00 3.00 4.00 'i 11 >I 1111I ` 5 .0 0 6.00 7 .0 0 m i Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000370 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Non Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-212 Text: 1: C8 Sulfonate (PFOS) L1278-18 Spk C, 500 ng/L 121903A-212 Sm (Mn, 2x3) 10CH %- 5.45 29009 19-Dec-2003 17:18:38 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 1.45e6 Area & 1 T " I ! I <-TT'; I T--1 i Time 5 .0 0 6.00 7.00 8.00 Exygen Research 3058 Research Drive State College, PA 16801 O -f -i- Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Rage 13 -- ' Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 ^ Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-213 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000372 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-214 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Rage 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil , Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 r, Last modified: Mon Dec 22 07:47:40 2003 ^ Job Code: \ Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-215 Text: 1: C8 Sulfonate (PFOS) /* r* Exygen Research, 3058 Research Drive, State College, PA 16801 0003^4 Quantify Sample Report Study NO.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-216 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-217 Text: 1: C8 Sulfonate (PFOS) L1278-17 121903A-217 Sm (Mn, 2x3) 100n %: 5.46 6581711 I i 0: r~r I--r-r-r-i"r i i i i i i i' r r r i i i--m "T i 1i i 1i--i--i--m--f--1--n --1--1--I--1--1--i--1--I--1 11 1I--1-- 1.00 2.00 3 .0 0 4.00 5.00 19-Dec-2003 18:37:31 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 3.36e6 Area 1 1 1""I""1 1 1 1 1 1 11 1 1 r-r j-T'T-i j T im e 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000370 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 18 *** Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil [ Last modified: Non Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code : Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-218 Text: 1: C8 Sulfonate (PFOS) L1278-18 121903A -218 Sm (Mn, 2x3) 10O] %: 19-Dec-2003 18:53:16 LC/MS/MS #6 5.46 M RM of 1 Channel ES499 > 99 1.44e6 Area 0 1ri-- i-- I-- ]-- I-- :-- :-- I-- I-- i-- i-- I-- r]~r-i-- I-- :-- I-- r~ 1.00 2.00 3.00 ]-- 1-- 1-- I-- I-- j-- !-- I-- r 4.00 5.00 6 .0 0 11i"' 1 " i " ` 1 i 11 1 Tim e 7.00 8.00 / <r~ Exygen Research, 3058 Research Drive, State College, PA 16801 000377 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-219 Text: 1: C8 Sulfonate (PFOS) L1278-18 Rep 121903A -219 Sm (Mn, 2x3) 100n %- 5.46 40993' 19-Dec-2003 19:09:07 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 2.13e6 Area 6.00 7.00 - n Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000378 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-220 Text: 1: C8 Sulfonate (PFOS) L1278-19 121903A-220 Sm (Mn, 2x3) 10Ch - %: 5.46 221760"! 1 i 19-Dec-2003 19:24:37 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 1.17e6 Area cy I" " I " " " 11 I 1.00 . . . p . , 1 , 1 , 1 1 r r ' i .. r n ... i " i " i ... r " i " i | i i i i j i " i i " t | i i T im ei i " i 1 1 i i i i i 1 1 | i 1 1 ' | i i ! 1 1 2.00 3.00 4.00 5 .0 0 ________ 6 ^ 0 ________ 7^00________8 .0 0 /*S Exygen Research, 3058 Research Drive, State College, PA 16801 0003^9 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, AnalysttK.Risha Page 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-221 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College PA 16801 000380 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Sate:12/19/03, Analyst:K.Risha Page 22 Sample List: P:\Bata\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleBB\121903A Soil Last modified: Mon Bee 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethBB\PFOS only 121803 Last modified: Mon Bee 22 07:47:40 2003 Job Code: Printed: Mon Bee 22 08:13:24 2003 Name: 121903A-222 Text: 1: C8 Sulfonate (PFOS) L1278-20 121903A-222 Sm (Mn, 2x3) 10Ch - %: 5.47 120111"! 1 1 19-Dec-2003 19:55:46 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 6.44e5 Area o : 11 1 N |-f- T-|*'i~i-- T'"i I I 1 I . T im eI 1 1 r r11 ',I)"|"r,.--TT-Tr "' 1I ~Tr TI TI I......1.....I.....I......I.....1.....I.....I.....1......I.....I.....I1 I` ' - --T--r[--- i - i I 1 I 1 11--11--11--Ir ~ 1m 1--1i--1!--I!--1'1--1 I I I I 1 1 1 1 I 1 1 1 1 I 1 11 11--11--I 11 11 11 11 II 11 ;1 11 11 II I 1.00 2.00 3-00________ 4 ,0 0 ________5 ^ 0 ________ 6 0________7XK)________8J00 Exygen Research, 3058 Research Brive, State College, PA 16801 000381 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 23 r~ Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903A Soil ; Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 ^ Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-223 Text : Exygen Research, 3058 Research Drive, State College, PA 16801 000382 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, AnalystK.Risha Page 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SarnpleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-224 Text: 1: C8 Sulfonate (PFOS) L1278-22 121903A-224 Sm (Mn, 2x3) 100- %: 5.47 341491"1 1 19-Dec-2003 20:26:54 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 1.87e6 Area n * 111i 1*'1'"1'" Ii_" 1_111'11II 1' *` 11 ' iI_1' 1' 1' 1` I1 '111 111'' 1I' '1j1 11 '11P ~m7."m "1 1I1"11"1 1I11111'1^ 111Mi 1 M111" 1"1 1I11111"1 I1`1"''i'1 I1 I111 !1I1T1* 1 1 ime 1-00________ 2 m ________ 3 ,0 0 ________4k00________ 50________ 6 .0 0 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 < Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 25 r"' Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Non Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 ~T Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-225 Text: 1: C8 Sulfonate (PFOS) L1278-23 121903A-225 Sm (Mn, 2x3) 100n %: 19-Dec-2003 20:42:29 LC/MS/MS #6 5.47 MRM of 1 Channel ES499 > 99 6.32e5 Area 0 ~ J I .I I I I I I I I I I I I I |-i.I I I I I I I I I I I I I I I I I I I I I I I 1 1 1 .0 0 ................2 .0 0 3.00 4.00 5.00 6.00 I ' 1 I 1 I I tt"iT I Tim e 7.00 8.00 i Exygen Research, 3058 Research Drive, State College, PA 16801 000384 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 26 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochexnicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-226 Text: 1: C8 Sulfonate (PFOS) L1278-24 121903A-226 Sm (Mn, 2x3) 10Ch %: 19-Dec-2003 20:58:13 LC/MS/MS #6 5.46 M RM of 1 Channel ES499 > 99 2.26e5 Area 0 '-( i i r i i . i i i 1.00 2.00 3.00 1--I--i I I I I I 4.00 5.00 6.00 i ' i.'' r"i--i~n ft i T im e 7.00 8.00 Exygen Research, 3058 Research Drive State College, PA 16801 000385 Quantify Sample Report Study N o .:Iil278, Set No.:121903A, Ext.Date:12/19/03, Analyst :K.Risha Page 27 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-227 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000386 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 28 -r* Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 r4 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-228 Text: 1: C8 Sulfonate (PFOS) ' L1278-25 )l~"1 1 2 1 9 0 3 A -2 2 8 S m (M n , 2x3) 100] r- %: 5.47 2551765~1 Ift 19-Dec-2003 21:29:29 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 1.34e7 Area 0: I TT-I J-T-I 1 1 I l I 1 TI I 1.1 1 |- 11 1 r 1, , | , , t--r~|--i--i--i--i--|--i--i--i--i--|----i--i--r~|--i--i-- 1.00 2.00 3.00 4.00 5.00 t1 6 .0 0 i "t' 1 1t'"i f 'i"1"1 ft 1 1,r.>' i Tim 7.00 8.00 r~ Exygen Research, 3058 Research Drive, State College, PA 16801 000387 Quantify Sample Report ' Study N o . :L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 29 -- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code : Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-229 Text: r* Exygen Research 3058 Research Drive, State College, PA 16801 000388 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 30 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-230 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive, State College, PA 16801 000389 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 31 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-231 Text: 1: C8 Sulfonate (PFOS) L1278-28 121903A-231 Sm (Mn, 2x3) 10<h %- 5.48 S 19-Dec-2003 22:16:46 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 2.70e7 Area 0 " 1"r * > T T -IT 1.00 I1 '1`1I11 5 .0 0 6.00 - n Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 32 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Marne: 121903A-232 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000391 Quantify Sample Report Study No.:Ij1278/ Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 33 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Harne: 121903A-233 Text: 1: C8 Sulfonate (PF0S) L1278-29 121903A-233 Sm (Mn, 2x3) 100~i %- 5.48 2787671 19-Dec-2003 22:48:14 LC/MS/MS #6 M R M of 1 Channel ES499 > 99 1.45e7 Area 1.00 2 .0 0 3.00 4 .0 0 5.00 6.00 T Tim e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study Ho. :L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risila Page 34 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Harne: 121903A-234 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000393 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 35 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Mame: 121903A-235 Text: 1: C8 Sulfonate (PFOS) L1278-30 121903A-235 Sm (Mn, 2x3) ^OA_ 1 \J \J - 5.48 4574666~1 1 19-Dec-2003 23:19:46 LC/MS/MS #6 M RM of 1 Channel ESC a n c e l'x 2 .3 1 e 7 Area %: 1 1 11 1 1o - `'T-r i i' "|-T" i - h T ' r" 1 i i I i1 i i...i H i n - i i . , . i r , i~ i i -r i 7 " i T--i t--i" i ~ r -- r T T - r m ^ ^ f f h 1 it ' 1 p i_r ,_ r -t--i T im e 1.00 2.00 3.00 4.00 5.00 6 .0 0 7 .0 0 ________ 8 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No-:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 36 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Marne: 121903A-236 Text: 1: C8 Sulfonate (PFOS) L1278-31 121903A-236 Sm (Mn, 2x3) 1i \AJA\J_ %: 5.48 2 2 5 0 3 9 5 ~k 1 1 19-Dec-2003 23:35:27 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 1.16e7 Area 0 - *""r i -i--i--i-i i~~i"i --i--i--i--i--|--i--i--i--i--r"i r'i i t i--r r r r r r i i I-r i -i--r-p"TTr \ ci i""i \ T '- ' I "' 1 1 i 1 ' 1 r i i Tim e 1.00 2.00 3.00 4 .0 0 ________ 5XK)________ 6^00________ 7 \0 0 ________ 8 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 35*5 Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 37 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-237 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0003? Quantify Sample Report Study No.:L1278, Set No.:121903A, Ext.Date:12/19/03, Analyst:K.Risha Page 38 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-238 Text: 1: C8 Sulfonate (PFQS) XC121603-5, 500 ng/L standard 121903A-238 Sm (Mn, 2x3) 100i % 5.47 1379 20-Dec-2003 00:07:05 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 8.08e4 Area 6.00 7.00 T im e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set N o . :121903A, Ext.Date:12/19/03, AnalystsK.Risha Rage 39 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903A Soil Last modified: Mon Dec 22 08:08:13 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Mon Dec 22 07:47:40 2003 Job Code: Printed: Mon Dec 22 08:13:24 2003 Name: 121903A-239 Text: 1: C8 Sulfonate (PFOS) XC121603-6,1000 ng/L standard 121903A -239 Sm (Mn, 2x3) 100n %- 5.47 24862 20-Dec-2003 00:22:52 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 1.40e5 Area 0 r -r- i-i y I I 1.00 t i pT i - i...t - p - i--v -i i "" p ' i r ' T I I"' I I T I p r 2.00 3.00 4.00 5.00 6.00 7.00 - h Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA LI 278 PFOS 499 -> 99 NA R A W DATA REPORT Limit of 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: 122203A Karen Risha LC/MS/MS Unit #6 12/19 & 22/03 12/24-25/03 Exygen ID XC121603-0 XC121603-1 XC121603-2 XC121603-3 XC121603-4 XC121603-5 XC121603-6 Methanol Wash Reagent Blank Reagent Spk A Reagent Spk B L1278-1 Spk C L1278-14 Spk D L1278-18 Spk C L1278-29 SpkD XC121603-1 XC121603-2 L1278-1 L1278-1 Rep L1278-2 L1278-3 L1278-4 L1278-5 XC121603-3 L I278-6 L1278-7 L1278-8 L1278-9 L1278-10 XC121603-4 L1278-11 L1278-12 L1278-13 L1278-14 L1278-14Rep XC121603-5 XC121603-6 Sponsor ID - '- NA NA NA MW-2 (0-2) MW-5 (23-25) MW-4 (13-15) MW-6 (9-11) MW-2 (0-2) MW-2 (0-2) MW-2 (3-5) MW-2 (8-10) MW-2 (13-15) MW-2 (18-20) MW-2 (23-25) MW-2 (28-30) MW-2 (33-35) MW-5 (0-2) MW-5 (3-5) MW-5 (8-10) MW-5 (13-15) MW-5 (18-20) MW-5 (23-25) MW-5 (23-25) - - Sample Code C CS CS CS CS CS CS C c LCS LCS LF LF LF LF CS CS S s s s s s CS s s s s s CS s s s s s CS CS Run No. 122203A-501 122203A-502 122203A-503 122203A-504 122203A-505 122203A-506 122203A-507 122203A-508 122203A-509 122203A-S10 122203A-511 122203A-512 122203A-513 122203A-514 122203A-515 122203A-516 122203A-517 122203A-518 122203A-519 122203A-520 122203A-521 122203A-522 122203A-523 122203A-524 122203A-525 122203A-526 122203A-527 122203A-528 122203A-529 122203A-530 122203A-531 122203A-532 122203A-533 122203A-534 122203A-535 122203A-536 122203A-537 Analyte Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = [analyte found (ppt>analyte found in control (ppt)j x 100 amount added (ppt) Std. Cone. (ppo 0 25 50 100 250 500 1000 25 50 100 250 500 1000 Dilution Factor 1 1 1 1000 1000 100 1000 1000 1000 1000 1000 100 100 100 100 100 1000 100 1000 100 100 100 100 - - Peak Area 0 614 1233 2324 5927 12317 22881 0 0 1331 12547 11849 1824 7835 11743 563 1053 4636 3876 5583 5142 2452 3072 2237 2626 6899 2368 8476 10552 5902 4476 7723 8704 9136 8767 11325 22082 Analyte Found Amount Added Recovery Analyte Found (ppo ND 57.2 547 516000 78800 34100 512000 201000 168000 243000 224000 10600 13300 11400 30000 10200 369000 46000 194000 33600 37900 39800 38200 - (ppo . 50 500 250000 50000 25000 250000 -- m - 114 109 126 78 84* 121* - - - (PPb) - 1610 1340 1940 1790 84.8 106 91.2 240 81.6 2950 368 1550 269 303 318 306 - -- -- Standard Curve : Linear (1/x weighted) Intercept - 19.3902 Slope = 22.9155 Coef. O fD e t = 0.997870 Total Solids (%> - - 84.67 84.67 81.95 90.42 79.15 80.22 78.89 79.09 76.81 86.68 86.58 86.34 79.45 75.93 74.05 74.05 - - 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 (%)) C S - 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) '"Sample was corrected using die data found in set 121903AR. Spreadsheet prepared by:. Analyte Found (ppb) Dry Weight _ 1900 1590 2370 1980 107 133 116 303 106 3410 425 1800 338 399 430 413 - - 0003?9 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: L1278 Matrix: Soil Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. 3*^* moTime _ Date_ V {72 \ ob ______ . Initials_ CLIENT SAM PLE ID EXYGEN ID NUMBER W E IG H T (g) F O R T IF IC A T IO N (ng) na na na M W -2 (0-2) MW -5 (23-25) M W -4 (13-15) M W -6 (9-11) _ _ _ _ _ _ _ _ Reagent Blank Reagent Spk A Reagent Spk B L1278-1 Spk C L1278-14 SpkD L1278-18 Spk C L1278-29 Spk D _ - _ _ _ - -. - 2.0 _ 20.0 5.0 10000.0 5.0 2000.0 5.0 1000.0 5.0 10000.0 __-_ -__-_- -- _ _ _- _ _ _.- - - - Reagent Spk A Reagent Spk B L1278-1 SpkC L1278-14 SpkD Spiking Solution Used F061703-10 (10 ng/mL) F061703-9 (100 ng/mL) F061703-6 (100000 ng/mL) F061703-7 (10000 ng/mL) L1278-18 Spk C L1278-29 Spk D F061703-7 (10000 ng/mL) F061703-6 (100000 ng/mL) All samples were weighed on balance No. Time 1*5 Date \> \22\b3> Volum e Used fo r Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) Initial/D ate L /liiz b * & / \z\a\oi 100 pL (200 pL micropipet) - = - ^ 22k> 200 pL (200 pL micropipet) 100 pL (200 pL micropipet) 100 pL (200 pL micropipet) t C " /12)221/5: Initials After weighing samples were returned to refrigerator N o .. 32- Time ) 3 3 Q D ate _ M 22\C& > Initials. C o m m en ts: 200 pL of 250 mg/mL sodium ttosulfatewasadded to i samples before spiking. Initials/Date: Analysis Sum m ary: D ata Set: D ata Set: D ata Set: **________ ~_______ Initials/Date: Initials/Date: In itials/D ate:__ n . ite Set extraction/analysis data verified by: m JL "d Date: p h /p 3 July 26, 2001/1 1 11 1 l i 1 1 \ 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L1278 METHOD: 01M-008-046 Rev 1 (Modified) PROTOCOL NUMBER: NA MATRIX: Soil ANALYTES: PPOS Client ID na na na MW-2 (0-2) MW-5 (23-25) MW-4 (13-15) MW-6 (9-11) - - . Exygen ID Reagent Blank Reagent Spk A Reagent Spk B L1278-1 Spk C L1278-14 SpkD L1278-18 SpkC L1278-29 Spk D - - - STEP STEP 12 s ----- STEP 3 >J - - - STEP 4 I \t - - - STEP 5 t 1 1 I 1 'w - - - STEP 6 Dilutions (mL/mL) - - STEP 7 )V.;'M.o O-'/tO \! \' -- -- - -- - -- - Dilutions (mL/mL) -- V. - - - - STEP 8 __ - -- -- - - - Reagents/ Materials Methanol C18 SPE Type I Water - - - - _ Initials/Date - L o t# 4330flS H NA - - - -- -- - -- - - -- - - - - - - - - - - .- - - - - - - - --- - -- - - -- - - - - --- - - - - - -- HPLC - - -- - - - - - - - - Methanol - - - - - - - - - - - - AmmoniumAcetate .\>2l5fl - - --- - - - - - - - Type I water NA - *Initials/Date - -- - - - - U- - - CBS CBB CB - ililzJoS 2}z2jo3 jjzzjc tzzzli M 3 P io o a Initials/Date STEP 1: 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 rpm STEP 4: Filter through glass acrodisc STEP 5: SPE column clean up STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 7: LC/MS/MS analysis O STEP 8: LC/MS/MS reanalysis. Final extracts stored in r e f r i g e r a t o r I n i t i a l s : Q P K Date: ^ Initials and date under each step indicates the personnel that performed this step. COMMENTS: O H* July 19, 2001/4  ] 1 )J 11 1 11 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorocheirrjuccaalsls..PPRKOO\\SSaamr pleDB\122203A Soil.SPL Printed: Wed Dec 24 09:53:11 2003 Vial File Name LIMS ID Client ID Sample Description 1 1 122203A-501 -- -- XC121603-0, 0 ng/L standard 2 2 122203A-502 -- -- XC121603-1,25 ng/L standard 3 3 122203A-503 -- -- XC121603-2,50 ng/L standard 4 4 122203A-504 -- -- X C 121603-3,100 ng/L standard 5 5 122203A-505 -- -- XC1216Q3-4,250 ng/L standard 6 6 122203A-506 -- -- XC121603-5, 500 ng/L standard 7 7 122203A-507 -- -- XC121603-6,1000 ng/L standard 8 92 122203A-508 -- -- Methanol Wash 9 71 122203A-509 -- -- Reagent Blank 10 72 122203A-510 -- -- Reagent Spk A, 50 ng/L 11 73 122203A-511 -- -- Reagent Spk B, 500 ng/L 12 74 122203A-512 -- -- L1278-1 Spk C, 250000 ng/L, DF=1000 13 75 122203A-513 -- -- L1278-14 Spk D, 50000 ng/L, DF=1000 14 76 122203A-514 -- 15 77 122203A-515 -- -- -- L1278-18 Spk C, 25000 ng/L, DF=100 L1278-29 Spk D, 250000 ng/L, DF=1000 16 2 122203A-516 -- -- XC121603-1,25 ng/L standard 17 3 122203A-517 -- -- XC121603-2,50 ng/L standard 18 78 122203A-518 -- -- L1278-1, DF=1000 19 79 122203A-519 -- -- L1278-1 Rep, DF=1000 20 80 122203A-520 -- -- L1278-2, DF=1000 21 81 122203A-521 -- -- L1278-3, DF=1000 22 82 122203A-522 -- -- L1278-4, DF=100 23 83 122203A-523 -- -- L1278-5, DF=100 24 4 122203A-524 -- -- X C 121603-3,100 ng/L standard 25 84 122203A-525 -- -- L1278-6, DF=100 26 85 122203A-526 -- -- L1278-7, DF=100 27 86 122203A-527. -- -- L1278-8, DF=100 28 87 122203A-528 -- -- L1278-9, DF=1000 29 88 122203A-529 -- -- L1278-10, DF=100 30 5 122203A-530 -- -- XC121603-4,250 ng/L standard 31 89 122203A-531 -- -- L1278-11, DF=1000 32 90 122203A-532 -- 33 8 122203A-533 -- -- -- L1278-12, DF=100 L1278-13, DF=100 34 9 122203A-534 -- -- L1278-14, DF=100 35 10 122203A-535 -- -- L1278-14 Rep, DF=100 36 6 122203A-536 -- -- XC121603-5, 500 ng/L standard 37 7 122203A-537 -- - - XC121603-6,1000 ng/L standard o oo W }1 )1 Exygen study n o . l |278> 11 Page 1 Page Position: (1 ,1 ) ) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF MS Method . Blank 0 ____ Standard 25 0. . . ____ --0 ____ Standard 50 ----0 ____ Standard 100 ---- 0 _____ Standard 250 ____ Standard 500 ---- 0 0-- ---- ____ Standard 1000 ----0 ____ Blank -- ----0 ____ Blank . . . QC ____ QC ____ QC -- ----0 50 -- -- 0 500 ---- 0 250000 -- -- 0 ____ QC 50000 -- -- 0 ____ QC 25000 -- -- 0 ____ QC 250000 -- -- 0 -- Standard 25 ----0 -- Standard 50 ---- 0 -- Analyte -- ... -- 0 -- Analyte -- ... -- 0 . . . Analyte -- -- 0 ____ Analyte -- ---- 0 ____ Analyte -- ---- 0 -- Analyte -- ---- 0 -- Standard 100 ---- 0 -- Analyte -- ----0 -- Analyte -- ---- 0 -- Analyte -- ----0 ____ Analyte -- ----0 -- Analyte -- ---- 0 -- Standard 250 ----0 ____ Analyte -- ----0 ____ Analyte ____ Analyte -- -- ---- 0 ---- 0 -- Analyte -- ----0 -- Analyte -- ----0 -- Standard 500 ----0 -- Standard 1000 -- 0 1 1 1 1 1 1 1 1 1 1 1 1000 1000 100 1000 1 1 1000 1000 1000 1000 100 100 1 100 100 100 1000 100 1 1000 100 100 100 100 1 1 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS ] 1 11 1 1 1 1 l Masslynx Sample List Sample List: C:\MASSLYNX\Fluorochemmiipcaailss.P.PKROOV\SaammtpleDB\122203A Soil.SPL Printed: Wed Dec 24 09:53:11 2003 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 O O o HPLC Method MS Tune File Inj.Volume PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA PFOSand PFOA 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 o Cv foygen study n o . Page 2 Page Position: (2,1 ) UWt>_____________________ LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exvsen Study No: L1278 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 ED: 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 000404 Scanning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\PFOS Last Modified: Thu Dec 18 14:43:11 2003 Printed: Wed Dec 24 09:53:55 2003 03 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 499.00 99.00 0.20 40 30 Page 1 Method Report Method File: Last Modified: Printed Page 1 c:\masslynx\fluorochemicals.pro\acqudb\pfosand pfoa Wednesday, December 24, 2003 09:54:01 Wednesday, December 24, 2003 09:54:05 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 9 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 Pressure 400 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 7.95 8.00 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 (/xl) Vial Number 200.0 200 0.50 14.00 15.0 7 000406 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\FLUOROCHEMS Printed: W e d Dec 24 09:54:20 2003 Page 1 Dau 499.00 SOURCE ( ESP- ) CapillaryCone 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 -51 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3 . 0e-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 28 29 31 -648 Rdbk 132.1 760.1 Quantify Calibration Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Calibration: P: \Data\LCMSMS6\Masslynx\Fluorochemicals .PRO\CurveDB\122203A Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K-Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Tue Dec 30 07:56:47 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Tue Dec 23 16:00:17 2003 J, Tue Dec 30 08:09:48 2003 In itials. D ate__ VxlSoloB Run# j .-To \72103h~^n Name: 122203A-501 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o . :1(1278/ Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed.: Tue Dec 30 08:09:48 2003 Name: 122203A-502 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date :12/19&22/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-503 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, AnalystsK.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-504 Text : 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0004 o Quantify Sample Report Study No.: 1.1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Rage 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-505 Text : 1: C8 Sulfonate (PFOS) XCt 21603-4, 250 ng/L standard 122203A -505 S m (Mn, 2x3) 10Oi %- 5.25 5927 24-Dec-2003 20:44:41 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 3.45e4 Area 0 rT"r1 1.00 2.00 ........... 3.00 4.00 7 .0 0 Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst .-K.Risha E Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-506 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date :12/19&22/03, Analyst:K.Risha Page 7 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-507 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203a , Ext.Date:12/19&22/03, Analyst:K.Risha Page 8 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-508 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive State College, PA 16801 000416 Quantify Sample Report Study Ho.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-509 Text : 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000417 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date :12/19&22/03, Analyst:K.Risha Rage 10 Sanale List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code : Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-510 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 00043.8 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-511 Text: 1: C8 Sulfonate (PFOS) Reagent Spk B, 500 ng/L 1 2 2 2 0 3 A -5 11 S m (M n , 2x3) 100n %: 24-Dec-2003 22:18:51 LC/MS/MS #6 5.24 M R M of 1 Channel ES499 > 99 6.97e4 Area 0 oi I'T y r - p - t - p - r - p 1.00 TIMI 2.00 3.00 4.00 5.00 T ' l ' T i n - i ' i l T i rr | Tim e 6.00 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 00049 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-512 Text: 1: C8 Sulfonate (PFOS) L1278-1 Spk C, 250000 ng/L, DF=1000 122203A -512 Sm (M n, 2x3) 10CH %: 0 "i".IIT1''!IIII1f-rn r, Ir-i ,I.I,II.I 1 .0 0 2 .00 3 .0 0 4.00 5.00 24-Dec-2003 22:34:27 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 5.79e4 Area 6.00 I I I I I 1 I I ' I I r'i I I T im e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, E x t .Date:12/19&22/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Mama: 122203A-513 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College PA 16801 000421 Quantify Sample Report Study No. :L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst :K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-514 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000422 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Rage 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Pec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-515 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 0004 70 Quantify Sample Report Study No.:L1278, Set N o . :122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-516 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000424 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-517 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-518 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 _ I Quantify Sample Report Study No.:L1278, Set No.:122203A, E x t .Date:12/19&22/03, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-519 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000427 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-520 Text : 1: C8 Sulfonate (PFOS) U 278-2, DF=1000 122203A-520 Sm (Mn, 2x3) 10CH %: 25-Dec-2003 00:40:37 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 2.67e4 Area O-^-rr iT i-rrrtyiT-i-r-iT i'i ii~rT~i"i p n i | ii r ip h'q'Tn 1.00 2.00 3.00 4.00 i T' r i r 1< i i"i r i T"i -| Time 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000478 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 21 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-521 Text: 1: C8 Sulfonate (PFOS) L1278-3, DF=1000 122203A-521 Sm (Mn, 2x3) 100n %: 5.24 25-Dec-2003 00:56:24 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 2.54e4 Area 0 -% = !- | ' = I - I I T I ] ~ i I j I I I I J I I I ! p i I i I I I r-i I r 1.00 2.00 3.00 4.00 5 .0 0 6.00 frpF, I I . 7.00 T im e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Sec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-522 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000430 Quantify Sample Report Study No.:L1278, Set No.:122203A, E x t .Date:12/19&22/03, Analyst:K.Risha Page 23 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-523 Text: 1: C8 Sulfonate (PFOS) ff* Exygen Research, 3058 Research Drive, State College, PA 16801 000431 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Rage 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-524 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha pa Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-525 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000433 Quantify Sample Report Study No.:L1278, Set No.:122203a , Ext.Date:12/19&22/03, Analyst:K.Risha Page 26 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-526 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000434 Quantify Sample Report Study Ho. :L1278, Set No.:122203A, Ext .Date: 12/19&22/03, Analyst:K.Risha Page 27 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-527 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0004^5 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Pate:12/19&22/03, Analyst:K.Risha Page 28 Sample List: P:\Pata\LCMSMS6\Masslynx\Fluorochemicals.PRO\SamplePB\122203A Soil Last modified: Tue Pec 30 07:56:47 2003 Method: P:\Pata\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethPB\PFOS only 1218 Last modified: Tue Pec 23 16:00:17 2003 Job Code: Printed: Tue Pec 30 08:09:48 2003 Marne: 122203A-528 Text: 1: C8 Sulfonate (PFOS) L1278-9, DF=1000 122203A-528 S m (Mn, 2x3) 100i %- 5.25 25-Dec-2003 02:45:47 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 Cancel Area 3.00 4.00 5.00 6.00 ` 1 I 1 1 ` ' I T"1 ITIim e 7.00 8 .0 0 Exygen Research, 3058 Research Prive, State College, PA 16801 Quantify Sample Report Study N o .:L1278, Set N o . :122203A, Ext .Date:12/19&22/03, Analyst :K.Risha Page 29 Sample List: P: \Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-529 Text: 1: C8 Sulfonate (PFOS) L1278-10, DF=100 122203A-529 Sm (Mn, 2x3) 100-1 %- 25-Dec-2003 03:01:22 LC/MS/MS #6 5.26 M R M of 1 Channel ES499 > 99 5 .3 4 e 4 Area 0 1.00 6.00 -I- r ''T 'T-i n T im e 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K. Ri sha Page 30 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-530 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 TO Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 31 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-531 Text: 1: C8 Sulfonate (PFOS) L1278-11, DF=1000 122203A-531 Sm (M n, 2x3) 100-, %- 5.26 44' 25-Dec-2003 03:32:49 LC/MS/MS #6 M R M of 1 Channel ES499 > 99 2 .2 8 e 4 Area 7.00 Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000499 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Rage 32 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\122203A Soil i Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 f* Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-532 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 000440 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, AnalystsK.Risha Page 33 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 1218 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-533 Text: 1: C8 Sulfonate (PFOS) L1278-13, DF=100 122203A -533 Sm (Mn, 2x3) 100-1 %- 5.29 8704 25-Dec-2003 04:04:28 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 4 .1 7 e4 Area 0 1.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study Mb.:Ll278, Set Mo.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risba Page 34 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil , Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 <-* Job Code : Printed: Tue Dec 30 08:09:48 2003 Marne: 122203A-534 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 00044*2 Quantify Sample Report Study N6.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 35 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 1218 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Name: 122203A-535 Text: 1: C8 Sulfonate (PFOS) Lt 278-14 Rep, DF=100 122203A-535 Sm (Mn, 2x3) 100~i %- 25-Dec-2003 04:36:00 LC/MS/MS #6 5.28 MRM of 1 Channel ES499 > 99 4.07e4 Area 0T 1.00 2.00 3.00 4.00 T im e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 36 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Tue Dec 30 08:09:48 2003 Harne: 122203A-536 Text: 1: C8 Sulfonate (PFOS) XC121603-5, 500 ng/L standard 122203A-536 Sm (Mn, 2x3) 10CH %: 25-Dec-2003 04:51:46 LC/MS/MS #6 5.28 MRM of 1 Channel ES499 > 99 6.26e4 Area 0 iI'II | i i i I | i T i r | 1.00 I ' r 1 1 t I ~i I ] I I I i r [ i ~ f ' i 2.00 3.00 rr"i~1 4.00 5.00 6.00 i f T f i , r i i~i TT r | T im e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000444 Quantify Sample Report Study No.:L1278, Set Mo.:122203A, Ext.Date:12/19&22/03, Analyst:K.Risha Page 37 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\122203A Soil Last modified: Tue Dec 30 07:56:47 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 <Tob Code: Printed: Tue Dec 30 08:09:48 2003 Marne: 122203A-537 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0004'* 5 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L1278 PFOS 499 -> 99 NA RA W DATA REPORT Limit of 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: 121903AR Karen Risha LC/MS/MS Unit #6 12/19/03 12/23/03 Exygen ID XC121603-0 XC121603-1 XC121603-2 XC121603-3 XC121603-4 XC121603-5 XC121603-6 L1278-15 L1278-16 L1278-17 L1278-18 H 278-18 Rep L1278-19 XC121603-1 XC121603-2 L1278-20 L1278-21 L1278-22 L1278-23 L1278-24 XC121603-3 L 1278-25 L1278-26 L I278-27 L1278-28 XC121603-4 L1278-29 LI 278-29 Rep L1278-30 L1278-31 L1278-32 XC121603-5 XC121603-6 Sponsor ID - - - - - - - MW-4 (0-2) MW-4 (3-5) MW-4 (8-10) MW-4 (13-15) MW-4 (13-15) MW-4 (18-20) - - MW-4 (28-30) MW-3 (4-6) MW-3 (9-11) MW-3 (14-16) MW-3 (19-21) - MW-1 (0-2) MW-l (8-10) MW-6 (0-2) MW-6 (4-6) - MW-6 (9-11) MW-6 (9-11) MW-6 (14-16) MW-6 (19-21) MW-6 (24-26) - - Sample Code c CS CS CS CS CS CS S S s s s s CS CS s s s s s CS s s s s CS s s s s s CS CS Run No. 121903AR-301 121903AR-302 121903AR-303 121903AR-304 121903AR-305 121903AR-306 121903AR-307 121903AR-308 121903AR-309 121903AR-310 121903AR-311 121903AR-312 121903AR-313 12903AR-314 12903AR-315 121903AR-316 121903AR-317 121903AR-318 121903AR-319 121903AR-320 121903AR-321 121903AR-322 121903AR-323 121903AR-324 121903AR-325 121903AR-326 121903AR-327 121903AR-328 121903AR-329 121903AR-330 121903AR-331 121903AR-332 121903AR-333 Analyte Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = [analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Std. Cone. (ppt) 0 25 50 100 250 500 1000 - - - 25 50 - 100 - - 250 - - - 500 1000 Dilution Factor - - - - - - - 100 1000 100 100 100 20 - - 10 1000 100 10 10 - 1000 100 1000 1000 - 1000 1000 1000 1000 100 - - Peak Area 0 706 1297 2453 6688 14252 26090 9458 13739 9062 3381 3338 12417 707 1188 12685 5987 4241 12878 4489 2597 4725 10179 6036 12816 6508 5411 5439 9444 3750 9376 12856 23975 Analyte Found <ppt) - Amount Added (ppo Recovery - (%> . Analyte Found (ppb) - -- -- -- -- -- -- -- -- -- - - - 36700 534000 35100 13000 12900 9640 - -- - 294 - 4270 - 281 - 104 - 103 - 77.1 - '4930 232000 16400 5000 1730 - - -- -- - 39.4 - 1860 - 131 - 40.0 - 13.8 - 183000 39500 234000 498000 - -- - 1460 - 316 - 1870 - 3980 - 209000 210000 366000 145000 36400 - -- - 1670 - 1680 - 2930 - 1160 - 291 - -- -- -- Standard Curve: Linear (1/x weighted) Intercept = 36.4562 Slope = 25.6834 Coef. Of Det. = 0.994297 Total Solids (%) - - - - - - - 88.07 83.17 80.21 80.32 80.32 77.80 - - 6S.10 83.49 84.75 74.92 81.95 - 85.85 80.12 94.85 82.13 - 84.66 84.66 84.86 80.88 78.28 - - Analyte Found (ppb) = [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Analyte Found (ppb) dry weight = analyte found (ppb) x (100% / total solids (%)) CS = Calibration standard C = Control sample S - Sample LF - Lab fortified sample FF =s 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 arid LOQ (50 ppt) Analyte Found (ppb) Dry Weight . - - - - - - 333 5130 350 129 128 99.1 - - 57.9 2230 155 53.4 16.9 - 1700 394 1970 4850 - 1970 1980 3450 1430 372 - - Spreadsheet prepared by: 1 ) J I 11 1 11 M asslynx - Sample L ist Sample List: C:\MASSLYNX\Fluorochemicalis.PRKO(j\\bSaamm[pleDB\121903AR Soil.SPL Printed: Mon Diec 22 13:32:43 2003 Vial File Name LIMS ID Client ID Sample Description Mat 1 1 121903AR-301 _____ 2 2 121903AR-302 -- 3 3 121903AR-303 -- 4 4 121903AR-304 -- 5 5 121903AR-305 -- 6 6 121903AR-306 -- 7 7 121903AR-307 -- 8 51 121903AR-308 -- 9 52 121903AR-309 -- 10 53 121903AR-310 -- 11 54 121903AR-311 -- 12 55 121903AR-312 -- 13 56 121903AR-313 -- 14 2 121903AR-314 -- 15 3 121903AR-315 -- 16 57 121903AR-316 -- 17 58 121903AR-317 -- 18 59 121903AR-318 -- 19 60 121903AR-319 -- 20 61 121903AR-320 -- 21 4 121903AR-321 -- 22 62 121903AR-322 -- 23 63 121903AR-323 -- 24 64 121903AR-324 -- 25 65 121903AR-325 -- 26 5 121903AR-326 -- 27 66 121903AR-327 -- 28 67 121903AR-328 -- 29 68 121903AR-329 -- 30 69 121903AR-330 -- 31 70 121903AR-331 -- 32 6 121903AR-332 -- 33 7 121903AR-333 _____ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC121603-0, 0 ng/L standard XC121603-1, 25 ng/L standard XC121603-2, 50 ng/L standard XC121603-3,100 ng/L standard XC121603-4, 250 ng/L standard XC121603-5, 500 ng/L standard XC121603-6,1000 ng/L standard L1278-15, DF=100 L1278-16, DF=1000 L1278-17, DF=100 L1278-18, DF=100 L1278-18 Rep, DF=100 L1278-19, DF=20 XC121603-1, 25 ng/L standard XC121603-2, 50 ng/L standard L1278-20, DF=10 L1278-21, DF=1000 L1278-22, DF=100 L1278-23, DF=10 L1278-24, DF=10 XC121603-3,100 ng/L standard L1278-25, DF=1000 L1278-26, DF=100 L1278-27, DF=1000 L1278-28, DF=1000 XC121603-4, 250 ng/L standard L1278-29, DF=1000 L1278-29 Rep, DF=1000 L1278-30, DF=1000 L1278-31, DF=1000 L1278-32, DF=100 XC121603-5, 500 ng/L standard XC121603-6, 1000 ng/L standard --- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- o o A ; Exygen STUDY N O . lut& _ } Page 1 Page Position: (1 ,1 ) Sample Type Cone (ng/L) Cone B C on cC Test ID DF MS Method Blank Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Standard Standard Analyte Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Standard Analyte Analyte Analyte Analyte Analyte Standard Standard 0 25 50 100 250 500 1000 -- -- -- -- -- -- 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 ---- 0 ---- 0 ---- 0 1 1 1 1 1 1 1 100 1000 100 100 100 20 1 1 10 1000 100 10 10 1 1000 100 1000 1000 1 1000 1000 1000 1000 100 1 1 PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS PFOS ii } i ii i ii Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemicals.PRO\SampleDB\121903AR Soil.SPL Printed: Mon Dec 22 13:32:43 2003 , o \-r> 1 HPLC Method MS Tune File Inj.Volume 1 PFOSand PFOA Fluorochems 15 2 PFOSand PFOA Fluorochems 15 3 PFOSand PFOA Fluorochems 15 4 PFOSand PFOA Fluorochems 15 5 PFOSand PFOA Fluorochems 15 6 PFOSand PFOA Fluorochems 15 7 PFOSand PFOA Fluorochems 15 8 PFOSand PFOA Fluorochems 15 9 PFOSand PFOA Fluorochems 15 10 PFOSand PFOA Fluorochems 15 11 PFOSand PFOA Fluorochems 15 12 PFOSand PFOA Fluorochems 15 13 PFOSand PFOA Fluorochems 15 14 PFOSand PFOA Fluorochems 15 15 PFOSand PFOA Fluorochems 15 16 PFOSand PFOA Fluorochems 15 17 PFOSand PFOA Fluorochems 15 18 PFOSand PFOA Fluorochems 15 19 PFOSand PFOA Fluorochems 15 20 PFOSand PFOA Fluorochems 15 21 PFOSand PFOA Fluorochems 15 22 PFOSand PFOA Fluorochems 15 23 PFOSand PFOA Fluorochems 15 24 PFOSand PFOA Fluorochems 15 25 PFOSand PFOA Fluorochems 15 26 PFOSand PFOA Fluorochems 15 27 PFOSand PFOA Fluorochems 15 28 PFOSand PFOA Fluorochems 15 29 PFOSand PFOA Fluorochems 15 30 PFOSand PFOA Fluorochems 15 31 PFOSand PFOA Fluorochems 15 32 PFOSand PFOA Fluorochems 15 33 PFOSand PFOA Fluorochems 15 vom QO 1 '] 1 ] Exygen STUDY NO. U 27ft 1 1J1 Page 2 Page Position: (2,1 ) ] LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A Exvgen Study No: L1278 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: Software: COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 p (Exygen ID: 74A ) (JONESCHROMATOGRAPHY: Part 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 0 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: ogr 3 O Scanning Method Report Method: C :\MASSLYNX\ FLUOROCHEMICALS ,PRO\ACQUDB\PFOS Last Modified: Thu Dec 18 14:43:11 2003 Printed: Mon Dec 22 13:32:50 2003 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 M R M of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 499.00 99.00 0.20 40 30 Page 1 00045 Method Report Method File: Last Modified: Printed: c:\masslynx\fluorochemicals.pro\acqudb\pfosand pfoa Monday, December 22, 2003 13:23:46 Monday, December 22, 2003 13:32:58 Page 1 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 9 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 Pressure 400 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 6 entr ies which are : Time Initial 0.00 0.05 0.10 7.95 8.00 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 14.00 15.0 7 Tuning Method Report Method : C :\MA.SSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\FLUOROCHEMS 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 -46 100 299 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3. 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 Rd 14.0 14.0 1-.0 -2 15 2 14.0 14.0 2.0 650 26 33 30 -6 Rdbk 131.0 752.7 Quantify Calibration Report Study N o .:L1278, Set No.:121903AR, Ext.Dates 12/19/03, AnalystsK.Risha Calibration: P :\Data\LCMSMS6 \Masslynx\Fluorochemicals. PRO\CurveDB\ 121903AR Last modified: Wed Dec 24 07:37:47 2003 Printed: Wed Dec 24 08:37:57 2003 Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 r* *> Quantify Sample Report Study No.:L1278, Set No. :121903AR, Ext.Date:12/19/03, AnalystsK.Risha Rage 1 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Name: 121903AR-301 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000454 Quantify Sample Report Study No.:L1278, Set N o . :121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-302 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000455 Quantify Sample Report Study No.:L1278, Set N o . :121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 3 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-303 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 4 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-304 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 rr'-'l i Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Rage 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-305 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive State College, PA 16801 000458 ' Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 6 -- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Ned Dec 24 08:37:58 2003 Name: 121903AR-306 Text: H'--I> 1: C8 Sulfonate (PFOS) XC121603-5, 500 ng/L standard 121903AR-306 Sm (Mn, 2x3) 10Ch %: 0 ` I * i l ' - T T 1 I1 I I ' n MT I j ! r I I I ! '! ! I I I ; I I 1 I I j I I j ' I I I I I I 1.00 2.00 3.00 4.00 23-Dec-2003 08:10:36 LC/MS/MS #6 5.40 MRM of 1 Channel ES499 > 99 7.87e4 Area 'i1l W i 11I1 5 .0 0 6.00 -1[-t--i i | 11111 i i i i | Tim e 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0004^9 Quantify Sample Report Study N o . :1.1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 7 -- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903AR Soil ; Last modified: Vue Dec 23 15:57:03 2003 ; Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only121803 Last modified: Vue Dec 23 16:00:17 2003 p Job Code: Printed: Ned Dec 24 08:37:58 2003 Name: 121903AR-307 Text: /P 1: C8 Sulfonate (PFOS) XC121603-6,1000 ng/L standard 1 2 1 9(D3AR -307 S m (M n, 2 x 3 ) 10Ch %: 5.39 2 6 0 9 0 '! 23-Dec-2003 08:26:26 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 1.50e5 Area 1.00 2.00 3.00 I I I I I I I I I I 1111I 11 4.00 5.00 ^I I I I I r I I I I r I1I I -|--t-i-t -i j-11i i r | T|iImme 6 .0 0 7.00 8 .0 0 kS3 i**\ Exygen Research, 3058 Research Drive, State College, PA 16801 ft* 000480 Quantify Sample Report Study No.:Iil278, Set N o . :121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 8 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-308 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, AnalystsK.Risha Page 9 j-* Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: < Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-309 ' Text : 1: C8 Sulfonate (PFOS) L1278-16, DF=1000 121903A R -309 Sm (Mn, 2x3) [ 100- %- 5.37 13739"! 1 23-Dec-2003 08:57:57 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 6.97e4 Area U" * 1.00 2.00 3.00 1 r-r -r-i -T-, -r r 1 1 1 11 1 1 4.00 5.00 n rq 6.00 1iy i 111111M 1Time 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000462 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 10 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-310 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0004^3 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 12180 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-311 Text: 1: C8 Sulfonate (PFOS) L1278-18, DF=100 121903A R -311 Sm (Mn, 2x3) 100n %- 5.37 3381 23-Dec-2003 09:29:34 LC/MS/MS #6 M RM of 1 Channel ES499 > 99 1.66e4 Area 0 I | I T-J" 1 I '-> 1 1 r 1.00 2.00 3.00 4.00 "rpr- . 6 .0 0 . i i TT~fT~rrr'| T im e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, AnalysttK.Risha Page 12 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 i~a Job Code: Printed: Wed Dec 24 08:37:58 2003 I Name: 121903AR-312 Text: Exygen Research, 3058 Research Drive, State College, PA 16801 s Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 12180 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-313 Text: 1: C8 Sulfonate (PFOS) L1278-19, DF=20 121903A R -313 Sm (Mn, 2x3) 10CH %- 5.39 124 23-Dec-2003 10:01:08 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 5.92e4 Area 1.00 2.00 3.00 1' 1I11`1I1111I1 5.00 6.00 7.00 Tim e 8.00 Exygen Research, 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:L1278, Set N o . :121903AR, Ext.Date:12/19/03, Analyst:K.Risha Rage 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-314 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 00046 7 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Rage 15 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-315 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set N o . :121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-316 Text: 1: C8 Sulfonate (PFOS) L1278-20, DF=10 121903A R -316 Sm (Mn, 2x3) 100- %: o: ~ ' 1 1 11 '' 1 ! 1 1 1 1 1 1 1 1 1 11 11 1.00 2.00 11111 1111 1 1 1 1 1 1 1 1 3.00 4.00 5.37 126851 1 23-Dec-2003 10:48:27 LC/MS/MS #6 MRM of 1 Channel ES499 > 99 6 .1 0 e 4 Area 1 1 1m 1 * 1 1 1 1 1 1 1 1 ` I 1 I ' "v i"1 1 1 ' T im e 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000469 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst :K.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Ned Dec 24 08:37:58 2003 Name: 121903AR-317 Text: 1: C8 Sulfonate (PFOS) Exygen Research 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:11127s, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Rage 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-318 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive State College, PA 16801 /N * Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Rage 19 Santple List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 12180 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-319 Text: 1: C8 Sulfonate (PFOS) L1278-23, DF=10 121903A R -319 Sm (Mn, 2x3) 1 0 0 --j %- 5.30 12878 23-D ec-2003 11:35:49 LC/M S/M S #6 M RM of 1 Channel ES499 > 99 6 .8 2 e 4 Area 0 r I I I I I r i ] I r " i r y i~nT r I ] I I I i" j r I I I |' , ! 1! |T r r r f r i ft 1Time 1.00 2.00 3.00 4.00 5.00 So 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000472 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, AnalystrK.Risha Page 20 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-320 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 0004^3 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 21 Sample List: F:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: F:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-321 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-322 Text: 1: C8 Sulfonate (PFOS) L1278-25, DF=1000 121903AR-322 Sm (Mn, 2x3) 100i %: 5.22 23-Dec-2003 12:23:02 LC/M S/M S #6 MRM of 1 Channel ES499 > 99 2.36e4 Area .--rrj-,-r-r ,,n n- 1.00 2.00 3.00 4.00 -rit-Irrrr, i ' ' ` | ' 5 .0 0 6.00 f - r-r-T I 7.00 T im e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 00047S Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 23 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-323 Text: 1: C8 Sulfonate (PFOS) L1278-26, DF=100 121903A R -323 Sm (Mn, 2x3) 100i 5.24 10179 23-D ec-2003 12:38:47 LC /M S/M S #6 M R M of 1 Channel ES499 > 99 4 .9 0 e 4 Area 1.00 1 1 ' 'I 1 ,VT r T 2.00 3.00 4 .0 0 5.00 6.00 7.00 Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000476 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 24 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-324 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College, PA 16801 000477 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 25 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Ned Dec 24 08:37:58 2003 Name: 121903AR-325 Text: 1: C8 Sulfonate (PFOS) L1278-28, DF=1000 121903AR-325 Sm (Mn, 2x3) 10 0 n %- 5.22 23-D ec-2003 13:10: LC /M S/M S #6 M RM of 1 Channel ES499 > 99 6.40e4 Area Q -- r~i i I | M I i Tlj~ I I T~'i | ' 1.00 "l i | i I i --r*' ! r ~ r LV i ^ ' i 2.00 3.00 4.00 5.00 6.00 T '-' ' i i i-r^ T ty-t i i T im e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000478 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 26 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-326 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive, State College PA 16801 0004^9 Quantify Sample Report Study No.:L1278, Set No. :121903AR, Ext.Bate:12/19/03, Analyst:K.Risha Page 27 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Bee 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 12180 Last modified: Tue Bee 23 16:00:17 2003 Job Code: Printed: Wed Bee 24 08:37:58 2003 Name: 121903AR-327 Text : 1: C8 Sulfonate (PFOS) L1278-29, DF=1000 121903AR-327 Sm (Mn, 2x3) 100n %- 5.20 5411 23-Dec-2003 13:41:58 LC/M S/M S #6 MRM of 1 Channel ES499 > 99 2.83e4 Area 0-j-- _ _ 3.00 r | T l T l T r T T 1--1~I-T-1 ( I'! 6 .0 0 7.00 :?=f=n Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000480 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 28 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-328 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive State College, PA 16801 000481 Quantify Sample Report Study No. :L1278, Set No. :121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 29 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-329 Text: 1: C8 Sulfonate (PFOS) L1278-30, DF=1000 121903A R -329 Sm (Mn, 2x3) 1 0 0 -n %- 5.23 9444 4 A 23-D ec-2003 14:13:29 LC /M S/M S #6 M R M of 1 Channel ES499 > 99 4 .8 8 e 4 Area 1.00 2.00 t"t 1 i _ i I r"` 1'"I 1 1 rr I ' 1 3.00 4.00 5.00 1 1 1 I 1 11 1 I~i ' I 1 1 1' I T im e 6.00 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 30 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-330 Text : Exygen Research, 3058 Research Drive, State College, PA .16801 00048 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 31 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 12180 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-331 Text: 1: C8 Sulfonate (PFOS) L1278-32, DF=100 121903AR-331 Sm (Mn, 2x3) 10Ch %- 5.22 9376 23-D ec-2003 14:45:06 LC /M S/M S #6 M RM of 1 Channel ES499 > 99 4.58e4 Area 1 1 I'i-|'r1 rI1 ' 6.00 7.00 i=n Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No. :121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 32 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOS only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-332 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive State College, PA 16801 000485 Quantify Sample Report Study No.:L1278, Set No.:121903AR, Ext.Date:12/19/03, Analyst:K.Risha Page 33 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\121903AR Soil Last modified: Tue Dec 23 15:57:03 2003 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0S only 121803 Last modified: Tue Dec 23 16:00:17 2003 Job Code: Printed: Wed Dec 24 08:37:58 2003 Name: 121903AR-333 Text: 1: C8 Sulfonate (PFOS) Exygen Research, 3058 Research Drive State College, PA 16801 000486