Document YEdxbMzdayOOpLbyaMXkrqOV

Proven Results. ri Lit *u n Analytical Report r 1 Fluorochem ical Characterization of Water and Sludge Sam ples Daikin America Well Installation n u Exygen R esearch Laboratory Report No. L0001278 J Testing Laboratory pi Exygen Research [_' 3058 Research Drive State College, PA 16801 n n Requester Ii ; J John Simmons n E. Robert Alley and Associates I I 210 N. Atlainta Avenue * Sheffield, AL 35660 n (256) 383-1552 t fi IPP f- !! '0 0 0 0 3 9 fi B Hi I 3058 Research Drive JT:State College, PA 16801, USA PAGE 800.281.3219 F: 814.272.1019 exygen.com 1 Introduction 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 L0001278. Specific fluorochemical characterization by liquid chromatography / tandem m ass spectrometry (LC/MS/MS) was requested for all sam ples. A total of 32 sam ples were received for analysis. The sam ples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: T able 1: T arget Analysis Comoound Name Perfluorooctanoic Acid Acronym C8 Acid (PFO A) The analytical methods used were originally developed for groundwater sam ples and were ' validated by Exygen. The validation protocol and results are on file with Exygen. The methods were adapted for soil samples. Soil sample methods have not been fully validated at this time. The sam ples were submitted in amber glass containers. All sam ples were cooled to 4C from time of collection to receipt at Exygen Research. Sam ples 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. f: & f $ o M fj% Times Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Sam ples were analyzed within 30 days of receipt. 4 Methods - Analytical and Preparatory r ' 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Soil samples were extracted into methanol (5 grams of soil to 5 mL of methanol). The methanol extract was diluted to 40 m L with water. Solid phase extraction (S P E ) was used to prepare the sam ples for LC/MS/MS analysis. The diluted extracts were transferred to a C 18 S P E cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatment resulted in an eight-fold concentration of the diluted samples prior to analysis. PAGE2 O F 5 r' ***** 4.1.2 Sample Analysis by LC/MS/MS fir In H PLC, 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 m eans for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively n mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. l; A Hewlett-Packard H P1100 H PLC system coupled to a Micromass Ultima MS/MS w as used to Vrr* analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM ). Sam ples were extracted on 11/10/03. Sam ples were analyzed on 11/10/03 and 11/11/03. Raw analytical data is provided in Attachment D. ir*. u *tr",i 5.1 Calibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/MS/MS analysis. The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. n A calibration curve is acceptable if r >.0.985 (r2 > 0.970). f! Calibration standards are prepared using the sam e S P E procedure used for sam ples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. n *&< All calibration criteria were met for this analysis. 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of sam ples. The extraction blanks should not have any target analytes present at or above the concentration of H the low-level calibration standard. For these sam ples, the extraction blanks were compliant. Instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level sam ples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical methods. e : 5.4 Matrix Spikes Matrix spikes were prepared for four sam ples. Matrix spike recoveries are given in Attachment B . Recovery is calculated from the amount present in the sam ple extract. i?""* PAGE3 OF5 O O O iO l 5.5 Duplicates Laboratory duplicates were performed for four sam ples. The duplicate results are included with the sample results in Attachment A. 5.6 Laboratory Control Sam ples For LC/MS/MS analyses, Milliq water w as spiked with all compounds with each extraction set. All recoveries for all compounds were between 70-130% in each LC S. Results are given along with the raw data in Attachment D. 6 Data Summary 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. 7 Data/Sample Retention Sam ples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C : Chain of Custody 8.4 Attachment D: R aw Analytical Data PAGE 4 O F 5 000102 5.5 Duplicates i ; Laboratory duplicates were performed for four sample. The duplicate results are included with the sample results in Attachment A. fr * { 5.6 Laboratory Control Sam ples For LC/MS/MS analyses, Milliq water was spiked with all compounds with each extraction set. All recoveries for all compounds were between 70-130% in each L C S . Results are given f*. along with the raw data in Attachment D. * ;.11 6 Data Summary Please see Attachment A for a detailed listing of the analytical results. Results are reported in parts per million (ppm) (ug/g). Results are reported on a dry-weight basis. 11 7 Data/Sample Retention iH' :' Sam ples 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 t i folders maintained by Exygen. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C : Chain of Custody j. 8.4 Attachment D: Raw Analytical Data >jrf*-t.; 'r : t li t- iJ PAGE4 OF5 000103 i * i r! r< i u, fi Other Lab Members Contributing to Data Karen Risha n ?? t3 i n r- Ii a*. r i, . t' t! PAGE5 OF 5 000104 --Analytical ^ L . Report ^ Sum m ary of P FO A in Soil Sam p les \ Sample ID IVW-2 (0-2) MW-2. (0-2)* MW-2 (3.-5) MW-2 (8-1), 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)* ` Laboratory Duplicate ADry-weight basis Analyte Found (ng/g) PFOAA 1300 1030 3200 6 0 .8 4 7 .8 50.1 79.1 \ 76.4 \ 25.1 \ 48.9 \ 7.69 \ 205 88.4 259. 140 \ 136 \ , \ Total Solids (% ) 8 4 .6 7 8 4 .6 7 8 1 .9 5 90.42 7 9 .1 5 80.22 78.89 79.09 76.81 86.68 86.58 8 6 .3 4 79.45 75.93 74.05 7 4 .0 5 000105 v ^ ^ k3 0 5 8 Research Drive ^ ^ State College, PA 16801, USA ^ L r : 814.272.1039 W F : 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are lim ited to the term s and conditions stated herein, unless otherw ise agred 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 contrais are subject to review and approval by Exygen's legal council and must be signed by a corporate officer. PAYMENT TERMS--\Snless otherwise set forth in this Purchase Order, terms of payment are "Net BO 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 tor 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 wifi 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, "URGEN T" 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 UM FEE--The minimum fee for commercial services is one hundred dollars ($100). SAM PLE COLLECT/ON/SUBMISSLON--Client shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law and good commercial practice. Title and risk of loss with respect to submitted samples shall at all times remain with client prior to acceptance by an Exygen sample custodian. Exygen w ill initiate a chain-of-custody upon sample receipt unless-the client includes one with the sam ple(s). By request, Exygen will provide chain-of-custody forms for client's use. A il 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 inform ation. . Upon request, Exygen will provide and ship appropriate sample containers to clients. These containers w ill include the appropriate preservative if particular analyses require one. it is the responsibility of the client to handle these preserved containers safeiy, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers w ill be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SA M PLE DISPOSAL--Exygen retains samples for one month after reporting results, then disposes of or returns the sample. Unless the client requests that the sample(s) be returned, or prior arrangements have been made for long-term storage, Exygen shall dispose of the sam ple(s), Exygen shall charge a monthly fee fo r long-term storage. Samples found or suspected to contain hazardous waste, according to definitions in state and /or federal guidelines, w ill be returned to the client upon completion of the analysis. The cost of returning the sample(s) w ill 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 internal chain-ofcustody is maintained for each lot of samples received. HAZARD COMMUNICATION--The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law. QUALITY ASSURANCE--Oxygen will perform services consistent with its Quality Assurance Standard Operating Procedures (SO Ps), 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 of personal and professional integrity. SPECIAL REPORTS--Additional charges may be necessary for custom report formats. . LITIGATION--All costs associated with compliance to any subpoena for documents, for testimony in a court of law, or for any other purpose relating to work performed by Exygen Research shall 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 for any and all other expenses associated with said litigation. INDEMNIFICATION LIABILITY, AND INSURANCE--Exygen agrees to indemnify, defend, and save the client, its officers, directors, employees, agents, and representatives harmless from all losses, expenses, demands, and claims made against the client, its officers, directors, employees, agents and representatives because of any personal injuries, death, or property damage to the extent caused by the negligence dr w illful misconduct of Exygen, its employees, agents, or representatives in connection with the performance of services under this agreement, except to the extent such losses, expenses,, demands, or claims, occur as a result of the negligent or w illful 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 w ill, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage. - WARRANTY AND 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 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 of work. 7 P O /0 S A - _ Analytical ^ Report 1 Sum m ary of P FO A in Soil Sam p les Sample ID MW-4 (0-2) Analyte Found (ng/g) PFOAA 2 2 .7 - M VM (3-5) 7 3 .8 MW-4 (8-10) 770 MW-4 (13-15) 377 MW-4 (13-15)* 455 MW-4 (18-20) . 121 MW-4 (28-30) \ 49.0 MW-3 (4-6) \ 416 MW-3 (9-11) MW-3 (14-16) \ 41.8 \ 39.3 MW-3 (19-21) 30.3 ` Laboratory Duplicate ADry-weight basis , . Total Solids (%> 8 8 .0 7 8 3 .1 7 80.21 8 0 .3 2 80.32 7 7 .8 0 6 8 .1 0 83.49 84.75 74.92 8 1 .9 5 000106 3058 Research Drive X o # m sStatatte College, PA 16801, USA J: 814.272.1039 V F: 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are lim ited to th e term s and conditions stated herein, unless otherw ise 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--AWcontracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer. PAYMENT TERMS--Unless otherwise sef forth in this Purchase Order, terms of payment are " Net 30 Days." The lime allowable lor payment shall begin after both: (a) client's receipt of Exygen's invoice: and (b) the satisfactory performance of the services contemplated hereunder. A 1.5% monthly service charge shall be added to all past due balances. Notwithstanding any payment terms to the contrary set forth in this Purchase Order, Exygen, in its sole discretion, reserves the right to request payment in advance from client. In the event of default in payment for services rendered. Exygen shall be entitled to reasonable costs of collection, Including, but not limited to, attorneys' fees. BILUNG--All fees and charges are billed directly to the client requesting services. Exygen w ill not bill a-third party without prior notification in writing, via a signed statement acknowledging and accepting responsibility for payment. .Exygen w ill assume that the paperwork submitted with a sample describes the desired testing protocol. Any changes to the protocol must be submitted in w riting. Please fax changes to Exygen marked, "URGEN T'' 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 UM FEE--The minimum fee for commercial services is one hundred dollars ($100). ' , SAM PLE COLLECTION/SUBMISSION--CWeht shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law and good commercial practice. Title and risk of loss with respect to submitted samples shall at all times remain with client prior to acceptance by an Exygen sample custodian. Exygen w ill initiate a chain-of-custody upon sample receipt unless the client includes one with the sam ple(s). By request, Exygen w ill 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 inform ation. Upon request, Exygen w ill provide and ship appropriate sample containers to clients. These containers will include the appropriate preservative if particular analyses require one. It is the responsibility of the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SAM PLE DISPOSAL-- Exygen retains samples for one month after reporting resuits, 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 /or 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 of any and all samples unless returned by Exygen to client. Exygen shall, unless the nature and character of the sample dictates otherwise, store all samples under locked, temperature-controlled conditions. An internal chain-ofcustody is maintained for each lot of samples received. HAZARD COMMUNICATION--The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law. Q UALITY 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 of personal and professional integrity. SPECIAL REPORTS--Additional charges may be neefesary 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 for any and all other expenses associated-with said litigation. . INDEMNIFICATION, LIABILITY, AN D IN SU RA N CE-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 of any personal injuries, death, or property damage to the extent caused by the negligence or w illful misconduct of Exygen, its employees, agents, or representatives in connection with the performance of services under this agreement, except to the extent such losses, expenses, demands, or claims, occur as a result of the negligent or willful, acts or omissions of the client, its officers, directors, employees, agents, and representatives; however, such indemnification and damages shall, in the aggregate, .be limited to the amount equal to the lesser of (a) damages suffered by the client as the direct result thereof, or (b) the total amount paid to Exygen for the work herein covered. Exygen w ill, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage. WARRANTY AND 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 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--YHs Purchase Order becomes a binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement of work. P / v se n k.f R E S E A R C H Precise Research. \ Proven Results. 1k -- Analytical Report 1 Sum m ary of P FO A in Soil Sam ples Sample ID Analyte Found (ng/g) PFOAA (%)Total Solids 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) , 530 111 52.2 163 954 954 596 183 86.4 85.85 80.12 94.85 . 82.13 84.66 84.66 84.86 80.88 78.28 ` Laboratory Duplicate AQry-weight basis 000107 M_^ ^ 3 0 5 8 Research Drive m u t a t e College, PA 16801, USA 814.272.1039 m R 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are lim ited to th e term s and conditions stated herein, unless otherw ise agreed to in a form al contract; CONFIDENTIALITY-- Exygen Research ("Exygen,'' "us," or "w e") maintains the strictest confidentiality in ail of our ciient 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--Ail contracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer. PAYMENT TERMS--iM ess otherwise set forth in this Purchase Order, temis of payment are "Net 30 Days." The time allowable for payment shall begin after both: (a) client's receipt of Exygen's invoice; and (b) the satisfactory performance of the services contemplated hereunder. A 1.5% monthly service 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 w ill 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, "URGEN T" 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 w ill 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 UM ASF--The minimum fee for commercial services is one hundred dollars <5100). SAM PLE COLLECTION/SUBMISS/ON--Client shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law and good commercial practice. Title and risk of loss with respect to submitted samples shall at all times remain with client prior to acceptance by an Exygen sample custodian. Exygen w ill initiate a chain-of-custody upon sample receipt unless the client includes one with the sam ple(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 inform ation. Upon request, Exygen will provide and ship appropriate sample containers to clients. These containers w ill include the appropriate preservative if particular analyses require one. It is the responsibility of the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SAM PLE DISPOSAL-- Exygen retains samples fo r 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. /or 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 of any and all samples unless returned by Exygen to client. Exygen shall, unless the nature and character of the sample dictates otherwise, store all samples under locked, temperature-controlled conditions. An internal chain-ofcustody is maintained for each lot of samples received. HAZARD COMMUNICATION--The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law. QUALITY ASSURANCE--Exygen will perform services consistent with its Quality Assurance Standard Operating Procedures (SOPs), the terms of which arc 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 of persona! 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, AND IN SU RA N CE-txygen 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 w illful misconduct of Exygen, its employees, agents, or representatives in connection with the performance of services under this agreement, .except to the extent such losses, expenses, demands, or claims, occur as a result of the negligent or w illful 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 w ill, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage. WARRANTY AN D LIM ITS O F LIABILITY--An accepting analytical work, Exygen guarantees the accuracy of the test results for the sample as submitted within the tolerances set forth in the SOPs. We disclaim any other warranties, expressed or implied by law. Exygen does not accept any legal responsibility for the purposes for which client uses the test results. Exygen w ill not accept any purchase order or any other order for work that includes conditions that vary from these Standard Conditions. ACCEPTANCE O F PURCHASE ORDER-- This Purchase Order becomes a binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement of work. 0 0 0 /7 /r Proven Results. Recovery Sum m ary for P FO A in Soil fm i. Sample Description MW-2 (0-2) 50 ng/mL Spike PFOA Amount Amt Found Amount Spiked in Sample Recovered Recovery (ng/mL) (ng/mL) (ng/mL) (%) 50 138 192 108 MW-5 (23-25) 25 ng/mL. Spike 25 13.0 45.3 129 MW-4 (13-15) 100 ng/mL Spike 100 37.9 158 120 MW-6 (9 - it ) 100 ng/mL Spike 100 101 230 129 r p 000108 3058 Research Drive State College, PA 16801, USA T: 800.281.3219 m F: 814.272.1019 exygen.com 3058 Research Drive State College, PA 16801 Phone:814-272-1039 Fax: 814-231-1580 Login #: L0001278 > 1,388 P ro je c t: P0000440 Project Title/Type: p f o a in Soil / R O U TIN E Project Storage: Refrigerated Submitted B y: John Sim mons P Status: U n re ce ive d ; Login Type: Started: ,, D a te Start: ; Due Date: Immediate Receipt of Sam ples T 11/7/2003 2:54:38PM 11/21/2003 Received Date: 11/07/2003 Received B y: AMMERMAN, M ARK '" 'Spread Sam ple: 1 Label: Login Notes: P" Conform Notes: Conform C O C Sam ple: Conform C O C : Conform Sam ple: Conform Request: True True True True ^"Package >4(0001843 Carton Packages / Containers Mail Date / Condition Shipper / IP Temp. Control / Temperai 11/7/2003 10:40:42PM Package & Contents Uncompromised FEDEX 8425212510620215 W ETiCE Direction / Handled By RECEIVED AMMERMAN, MARK i Container # C0013455 ,,C0013456 : C0013458 ! C0013459 C 0013460 r*C0013461 i C 0013462 1 C0013463 C0013464 r " C0013465 ! C 0013466 C0013467 ^ C0013468 ; C0013469 ! C0013470 C0013471 r * C0013472 ; C0013473 C0013474 C0013475 f C0013476 C0013477 C0013478 ^ C 0013483 ! C0013484 i COO13487 COO13493 -- CO013496 > C0013499 G ro ss Weight P Container Type 294.4 g 120 ml Amber G lass 290.3 g 120 ml Amber Glass 293.8 g 120 ml Amber G lass 278.2 g 120 ml Amber G lass 298.2 g 120 ml Amber G lass 277.4 g 120 ml Amber Glass 285.6 g 120 ml Amber Glass 296.0 g 120 ml Amber Glass 287.2 g 120 ml Amber G lass 265.4 g 120 ml Amber G lass 292.8 g 120 ml Amber Glass 294.1 g 120 ml Amber Glass 281.3 g 120 ml Amber Glass 288.9 g 120 ml Amber G lass 255.1 g 120 ml Amber Glass 261.1 g 120 ml Amber Glass 281.3 g 120 ml Amber Glass 261.0 g 120 ml Amber Glass 283.2 g 120 ml Amber Glass 285.0 g 120 ml Amber G lass 316.1 g 120 ml Amber Glass 271.3 g 120 ml Amber Glass 290.3 g 120 ml Amber Glass 281.2 g 120 ml Amber G lass 260.1 g 120 ml Amber G lass 241.6 g 120 ml Amber Glass 278.2 g 120 ml Amber Glass 250.8 g 120 ml Amber Glass 298.9 g 120 ml Amber Glass Preservative NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE r i 1/10/2003 I Login.rpt Report Version: Oct 23 2003 9:55AM Page 1 of 6 Mfg. Lot 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 2106010 Instance: Mfg. ID 676116 676117 676119 676120 676121 676122 676123 676124 676125 676126 676127 676128 676129 676130 676131 676132 . 676133 676134 676135 676136 676137 676138 676139 675784 675785 675788 675794 675797 000167058900 R0072108 R0072108 _ Login #: L0001278 > 1,388 ! Project: P0000440 Project Title/Type: P FO A in Soil / RO U TIN E Project Storage: Refrigerated r * Submitted By: John Sim mons ! Status: U n re ce ive d P Login Type: ^ Started: Date Start: Immediate Receipt of Sam ples T 11/7/2003 2:54:38PM ! Due Date: 11/21/2003 Received Date: 11/07/2003 --Received B y: AMMERMAN, MARK Spread Sam ple: L a b e l: P Login Notes: Conform Notes: Conform C O C Sam ple: Conform C O C : Conform Sam ple: Conform Request: True True True True Package C0013502 C 0018680 Carton 311.6 g 284.3 g Packages / Containers Mail Date / Condition 120 ml Amber G lass 120 ml Amber G lass Shipper MD NONE NONE Temp. Control / Temperat 2106010 Direction I Handled By 675803 M iscellaneous j-- Item K e y None Description IC O C r - 11/10/2003 Login.rpt ReDort Version: O ct 23 2003 9:55AM Page 2 of 6 O O O llO ' Instance: R0072108 R0072108 Sample ID .0001278-0001 L0001278-0002 r--L.0001278-0003 .0001278-0004 -0001278-0005 L0001278-0006 ^ .0001278-0007 .0001278-0008 L0001278-0009 JL 0 0 0 1 278-0010 .0001278-0011 .0001278-0012 L0001278-0013 ^1.0001278-0014 .0001278-0015 -0001278-0016 L0001278-0017 .0001278-0018 .0001278-0019 L0001278-0020 _L0001278-0021 .0001278-0022 .0001278-0023 L0001278-0024 -L0 001278-0025 .0001278-0026 -0001278-0027 L0001278-0028 "1.0001278-0029 L0001278-0030 L0001278-0031 L0001278-0032 Matrix SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID SOLID Fraction Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Soil Sample MW2 (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-4 (0-2) MW-4 (3-5) MW-4 (8-10) 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 (14-16) MW-6 (19-21) MW-6 (24-26) Sam ples Date Sampled Date Received 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 11/07/2003 Date Due 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 11/21/2003 - 11/10/2003 .ogin.rpt Report Version: Oct 23 2003 9:55AM Page 3 of 6 Instance: R0072108 R0072108 (MMX | 3001278-0001 fm C o n ta in e r C0013466 /120 ml Amber G lass / NONE | 1.0001278-0002 r Container C0013459 /120 ml Amber G lass / NONE W)001278-0003 C ontainer C0013472 / 120 ml Amber G lass / NONE 3001278-0004 ,, Container C0013478 /120 ml Amber G lass / NONE L0001278-0005 C ontainer C0013465 /120 ml Amber G lass / NONE r-" ; 0001278-0006 C o n ta in e r r - C0013471 /120 ml Amber G lass / NONE L.0001278-0007 P" C ontainer 1 C0013477 / 120 ml Amber G lass / NONE >001278-0008 C ontainer 00013476 /120 ml Amber G lass / NONE 0001278-0009 _ Container ; C0013470 /120 ml Amber G lass / NONE L0001278-0010 C ontainer C0013464 /120 ml Amber G lass / NONE fo o o i 278-0011 C ontainer r * CO013458 /120 ml Amber G lass / NONE L0001278-0012 C ontainer H 1/10/2003 ' .ogin.rpt Bottles M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod M ethod Report Version: Oct 23 2003 9:55AM Page 4 of 6 000x12 Instance: R0072108 R0072...1..0...8........ C0013475 /1 2 0 ml Amber Glass / NONE H>001278-0013 1 Container C0013469 /120 ml Amber G lass / NONE _D001278-0014 -- Container i. a C0013463 /120 ml Amber G lass / NONE L0001278-0015 r-1 Container C0018682 /120 ml Amber G la ss / NONE 0001278-0016 Container ["" CO013474 /120 ml Amber G la ss / NONE L0001278-0017 Container ' C0013468 /120 ml Amber G lass / NONE P0001278-0018 Container ^ C0013462 /120 ml Amber G lass / NONE -0001278-0019 r - Container C0013473 /120 ml Amber G lass / NONE J.0001278-0020 Container CO013456 /120 ml Amber G lass / NONE \ 0001278-0021 !Container " " C0013467 120 ml Amber G lass / NONE L0001278-0022 Container 1 C 0013 460 /120 ml Amber G la ss/N O N E P 0 0 0 1 278-0023 Container _ C0013461 /120 ml Amber G la ss / n o n e -0001278-0024 Container i C 0013 455 /120 ml Amber G la ss/N O N E -- 11/10/2003 Login.rpt Method Method Method Method Method Method Method Method Method Method Method Method Report Version: Oct 23 2003 9:55AM Page 5 of 6 000113 Instance: R0072108 R0072108 L0001278-0025 Container C0013483 /120 ml Amber G lass / NONE ^0001278-0026 Container Aw C0013484 /120 ml Amber G lass / NONE L.0001278-0027 Container . C0013496 /120 ml Amber G lass / NONE ^001278-0028 Container C0013502 /120 ml Amber G lass / NONE [ 0001278-0029 Container C0018680 /120 ml Amber G lass / NONE JL0001278-0030 | Container C0013487 /120 ml Amber G lass / NONE 0001278-0031 1Container f"" CO013493 120 ml Amber G lass / NONE L0001278-0032 **" Container i C0013499 /120 ml Amber G lass / NONE PMl Method Method Method Method Method Method Method Method 11/10/2003 Login.rpt Report Version: O ct 23 2003 9:55AM Page 6 of 6 000114 Instance: R0072108 R0072108 RESEARCH CHAIN O F CUSTODY/ANALYSIS REQUEST FORM Exygen Research Sample Receiving 3117 Research Drive State College, PA 16801, USA . 1 T: 814.231.8032 F: 814.231.1580 exygenresearch.com PaSe -- I-- ' _ J _ PRO JECT IN FORM ATIO N ANALYSES REQUESTED Client (name & address): Project Manager (Name & E-mail Address): `X o k n s 5 2 T i n t i n g : ______________________ i vAV-....3 5 6 1 ^ ___________ Phone: / Z 5 t o \ 3 S ' 3 ~ 5 2 - Fax: ( Z 0 \ E Z Z - y Z W Sampler: '\*> V m nnm < ry?S Project Name: / , ,, _ y//( J \ a -iiA 'o A w v sricA . k !)e ll iim RO. # : /o -K ' ^ o 3 - 0 * S 2 A - & 0 ~ Z . Quotation # : Please fill out this form completelyto ensure correct analysis and proper handling of your samples. .9 S$ Sra? < o c,, rl H SAMPLE ANALYSIS ExyLIMS# Client Sample Identification .q Collection Collection Date Time o M I -Z (D-Z^> b 3 /5 :io T A M - 2 3 ~ S '> i \ 3 l / 5 2 'V M \A -Z * /5/JO X y Specify Matrix Comments ^ > i _____ Li AABn Ui irS-tE"O<-NifcnL\Y/ M t -Z M \^ 2 A \o -2 \ -a / Iff-Z o S / 7 3 -2 3 ) / z ir - t ) (* k -? S r~ X /i>5 X /^ I5 X 7 " / 3 S 4 - .. --MP-- / CHAIN OF CUSTODY ReliQftui^bd by Date mm Time I/*',GO Cooler ID # { J fa Received by A ------------- --- _______ Cooler Temp. (C) Date . Time f i l l h i i&*tU OTHER INFORMATION LAB USE ONLY i i t , .. 1 i ( . I ( . A .... ?.. I i .... l I ' I Composite Number of Containers -< Q: JLf-- Q- / l/ 1/ \<J/, / ______ PROJECT REQUIREMENTS Results Deadline: S k M ' c W d __________________ Laboratory Report Options: Q ] Sample results only Add case narrative Q Add quality control summary C l Add calibration summary Add raw data Other______________________ i .. I f .,EV. 3-1. Composite Number of Containers 000116 F CHAIN O F CUSTODY/ANALYSIS REQUEST FORM RESEARCH Exygen Research Sample Receiving *3117 Research Drive State College, PA 16801, USA T: 814.231.8032 F: 814.231.1580 exygenresearch.com . Page Z, of J 2 PROJECT INFORMATION ANALYSES REQUESTED Client (name & address): --S L --A \W Q Project Manager (Name & E-mail Address): ___ V dIwa. Phone: Fax: Sampler: s? S ' _ Project Name: vK*-. Quotation # : AZ ct> 3 - 0 1 * 8 2 .- / a . Please fill out this form completelyto ensure correct analysis and proper handling of your samples. isS 5? 45? o- pQ Si SAMPLE ANALYSIS ExyLIMS# Client Sample Identification A l -( 'Z ') Collection Collection Date Time HEM .a0(}0. AM-S /J-5 5 ii:ao 8-10) am A\~5 i 13-15\ D;iz /Vvw- n% -z i l \zt> A \ "5 IS-ZB 'i 11:30 t3 :$ o KVi-M / 3 - 5 \ LAB USE ONLY / l 3 i 2 L -- 1.... Specify Matrix Comments 'A>i ( J__ jQ S t 3 cu "7 1/ T A "7 ir PROJECT REQUIREMENTS Results Deadline: , t'--' I ......... . ( ......... l . _ C . .. . I l l Laboratory Report Options: 0 Sample results only CD Add case narrative Q Add quality control summary [H Add calibration summary 1 I Add raw data Other____________________ i I 4....... RESEARCH CHAIN O F CUSTODY/ANALYSIS REQUEST FORM Exygen Research Sample Receiving *3117 Research Drive State College, PA 16801, USA ~ ,j T: 814.231.8032 F: 814.231.1580 exygenresearch.com Page of PROJECT INFORMATION Client (name & address): _____E r k a * A lie v / . Phone: Sampler: ^r-> r---?--I, __________ Project Manager (Name & E-mail Address): A A Kv-\ <r>nS Project Name: RO. # : Quotation # : ANALYSES REQUESTED Si ft & 1845 I c r* V 'i H Oo o Please fill out this form completelyto ensure correct analysis and proper handling of your samples. SAMPLE ANALYSIS O ExyLIMS# Client Sample Identification Collection Collection xi im CL Eo Date Time O u fISzm - l 5 ) K \ 0 " ^( - im b H :d5 ms tH'.zS iC M !H5 MV-.3 i m W M . m ia . J 5 _ ms M Vy-S / LAB USE ONLY W Specify Aflatrix L Comments L , . C_ i I J. IJ 8 & 3- / v '/ V V V/ z PROJECT REQUIREMENTS Results Deadline: - S k y ySt f i'ir p ______________ Laboratory Report Options: Sample results only IG Add case narrative CD Add quality control summary CDCD Add calibration summary Add raw data Other______________________ l--- I----- -.,*V. 3-(L - Fvppn 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.com Page L < * . ANALYSES REQUESTED Client (name & address): . ____ B . Kph& fiz A lle y $ tfs s d c Project Manager (Name & E-mail Address): ______ ---------------------------------------------------------------------------------------------------------------------- Phone: Fax: Sam p ler^ ^ ^ ^ T Project Name: RO. # : Quotation # : Please fill out this form completelyto ensure correct analysis and proper handling of your samples. Composite Number of Containers SAMPLE ANALYSIS Si ExyLIMS# Client Sample Identification Collection Collection 2 Date Time Specify Matrix Comments AW-I O-Z) k \o - \ 7k - i \ M W to ff)~ Zf) M s~ (o K\b"in C9~lls) MUV-io JiA-ll i AR 1ICC n M I V lilslo X\Z\D S>F l______ i$30 y (5135 i( ____ V Z J '.SO Y ! If`10 y Nr Ik'M J f _ _ ___ ;> CHAIN OF CUSTODY Cooler ID # / ti f c Cooler Temp. (C) o iS 5 -w oss>e Ja C s?-t> 2-s J <3^ >- -oc 2- X X X X t X X ____ J L ----i 11 PROJECT REQUIREMENTS Results Deadline: ___ <rd------------------------ Laboratory Report Options: n Sample results only Q Add case narrative Add quality control summary Add calibration summary I I Add raw data CD Other____________________ _ i i ..., I i %.. . i ( * ; u ... i < . c....- t L 1 3- L 000119 BEST COPY AVAILABLE USAAirbill ,j AMES E1E5 IDLE canberemovedto Recipient'sraconter--- / ) 3 _______________FedEx Trackin g Num ber 4 a E xp re ss P a i [X /f Fed Ex P rio rity M V N*lburines*momi W atrr\ 3 Phone P 5 f c . m T - l S S P * Com pany E Iz- . R O B ER TS A LLEY fc r ^ A d d ress 2 1 0 N A T L A N T A U utct City SHEFFIELD AVE A SSO C I MC STE 210 Dept/RootfSutai/Roofli State A L Z IP 3 5 & 0 ~ " 3 0 0 4 2 y * 1" " Z l9 -* > - / c 'A Z - c x r z , i To R ecip iente N am e V j\,'n ' ) -i m ry V . r- < < -v, y r \ \ / Phone I Z ' l ~ 5 iA ? Company 1 - Y y r P i K fe r Va * 7 -) t \ J LA ddress I n i To'HQtD" atFodExestnn,phntFedExaddress. i~r < "7 ( V /-- V~i \\i L L WecantadefvertoP.0,boxaorP.0.2P coda. [ 3 FedEx 2Day ( j FedEx Exp ress S aver . -- Secondbusineaday -- TMrdbusinessday M ----- fiatBtEnveloperatsnotevatobte-ffaBnumehanwOne-poundrate ----- -- 4 b E x p r e s s F re ig h t S e r v ic e DeSverycommiPtmaenctmkaaygbeeslaotevrienrsoImXaalrbeass.. F e d E x! D ay Freight* N tribusinessasy * CelforConfirmation:. 5 P a c k a g in g I 1 FedEx 2D ay Freig h t I-- I Secondbusinessday I I FedEx 3D ay Freight I-- I Thirdbusinessosy *Ddw ivb.lW tSSXI F e d ^ ty e lo p e * FedEx Pak* M o th e r InduA i FedExSmalPak, FedEx ~A tergePak,andFedExSturdyPak_____________ __________ a! m SATURDAYDeSwry i__J AveiabtowfyforFedExPriority includeFedEx iddream Section 3. p-, HOU)Weekday ,--i HOLDSaturdaiy I___I a tFed Ex Locador L J a t FedEx Location OvernightandFetOExffley Notaveteblefor AvaWrieonlyfor tosafectaPeoda Fexfirst Overnight Fex PriorityOvernight Doosthis shipmentcontaindangoroosgoods? endFedEx2D>yto selectlocation* ----------- Oneboxmustbecheeked ----------- (st/ I No Lwr*ij n Yes n Yes I___i Asperattached 1___ ) Shipper'sDeclaration Shfcper'sDeclaration notreqtrimd DBrySlete*,9-,UN1845- DangerousGoods{ndudrg DryIce)cannotbeshippedinFerSExpackaging. mito:P a ym e n t EnterFedExA cci No.orCreditCardNo.bi Cargo A irc ra ft O nly Sender R ecip ient AcetNo.inSection 1-- 1 Iw i babied. Th ird P arty C red it C ard 1-- 1 1 1 --1 1--1 Cash/Check L.1 L l._ I 'L. 1 A..~v i t :S I ._ * \v-\V3Date:11-12-03 I ) ije c t ____iPOOt t) Analyst Initials Date and Time Data Aquired (ctrl+t) shz shz 12-NOV-03 13:291 12-Nov-03 14:16 shz 13-NOV-03 16:27 Exygen ID L1278-1 L1278-2 L1278-3 L1278-4 L1278-5 L1278-6 L1278-7 L1278-8 L1278-9 L1278-10 L1278-11 L1278-12 L1278-13 L1278-14 L1278-15 L1278-16 L1278-17 L1278-18 L1278-19 L1278-20 CLIENT ID _ _ _ _ _ _ _ _ MATRIX PAN ID PAN W EIGHT (g) SA M PLE +PAN (g) MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 1.2711 1.2621 1.2679 1.266 1.2842 1.266 1.2711 1.2635 1.2685 1.2666 1.2666 1.2658 1.2723 1.2769 1.2651 1.267 1.2708 1.268 1.2758 1.2701 20.0909 20.1943 21.2097 22.4221 18.6859 19.4742 23.6772 21.6385 21.9363 21.1609 22.2035 21.8966 22.206 21.1285 21.0171 21.3326 21.1877 21.4419 21.4876 21.0179 DRIED SAM PLE + PAN (g) 17.2059 16.7779 19.3 18.0111 15.2446 15.6306 18.9927 16.9143 19.1842 18.4906 19.3428 17.6562 17.1678 15.9771 18.6610 17.9561 17.2464 17.4707 17.0013 14.7179 % Solids 84.6704 81.9546 90.4236 79.1502 80.2243 78.8908 79.0927 76.8137 86.6841 86.5776 86.3366 79.4463 75.9326 74.0505 88.0716 83.1727 80.2113 80.3152 77.8036 68.0977 _ _ _ --- ------ \V - < ] O l 000120 Data WorkGroup: %solid L278 a Page 1 1 l v~t: S ' " '* Date: 11-12-03 1 ) Xyyfen K^SfcftRch J 1 1 1 ` ect Y<xx p i Item S a m P|e amP^e Sample Sample Comment About 20 g of each sample was weighed in aluminum weighing dishes using balance 9 (IN0000288) .shz 11-12-03 Samples were placed into oven 2 (IN0000062) at 104C for over night time in 1430 temp in 104*0 .shz 11-12-03 Samples were removed from oven time out 1600 temp out 104*0 and cool in desiccator 6 (IN160) .shz 11-13-03 weighed samples using balance 9 (IN0000288).shz 11-13-03 o o Comments WorkGroup: %solid L278 a Page 1 i A :::;jf c s C i Date: 11-12-03 $ \\-u \V -O ~ o 3 i 1) Analyst Initials Date and Time Data Aquired (ctrl+t) xvufen K S E A h fo h 1 \ 1 " ~ iject 'p o o f J> shz 12-NOV-03 14:36 shz 12-NOV-0314:36 shz 13-NOV-0316:39 Exygen ID L1278-21 L1278-22 L1278-23 L 1 278-24 L1278-25 L1278-26 L 1278-27 L1278-28 U 278-29 L1278-30 L1278-31 L1278-32 CLIENT ID _ _ MATRIX PAN ID PAN W EIGHT (a) SA M PLE +PAN (g) MOISTURE l SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID MOISTURE | SOLID 41 42 43 44 45 46 47 48 49 50 51 52 1.278 1.2722 1.2706 1:266 1.2676 1.2668 1.2717 1.2663 1.2596 1.2617 1.2638 1.2697 21.0433 21.5448 21.2328 21.5623 22.7791 21.5705 21.504 21.5362 22.7564 22.3696 22.2768 21.1445 DRIED SAMPLE + PAN (g) 17.7797 18.4537 16.2271 17.8986 19.7348 17.5345 18.4379 17.9131 19.4596 19.1736 18.259 16.8281 % Solids 83.4882 84.7523 74.9241 81.9489 85.8480 80.1218 84.8455 82.1257 84.6638 84.8587 80.8795 78.2820 1 __________ _ .'y..... t3 \ if V -- 3^ 3 0001 Data WorkGroup: %solid L278 b Page 1 * )Ai 1 J i t : SK Date: 11-12-03 ! 1 1 1 Xyyfen SfcMfbh...1 ' 1 ect yc r 1 Item Sample Sample Sample Sample Comment About 20 g of each sample was weighed in aluminum weighing dishes using balance 9 (IN0000288) .shz 11-12-03 1113.03Samples were placed into oven 2 (IN0000062) at 104C for over niaht time in 1430 temp in 104*C .shz 11-12-03 Samples were removed from oven time out 1600 terrmout 104C and cool in d e sicca to r fi (iN-mn) h? . weighed samples using balance 9 (IN0000288).shz 11-13-03 000123 Comments WorkGroup: %solid L278 b Page 1 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: She: NA L1278 PFOA 413->369 NA RAW DATA REPORT lim it of Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 15 pL Soil 5.0 g 5.0 niL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: H1003A Karen Risha LC/MS/MS Unit #7 11/10/03 11/10-11/03 Exygen ID XC111003-0 X C 1 1 1003-1 XC111003-2 X C 1 11003-3 XC111003-4 XC111003-5 XC11100-6 XC111003-7 Methanol Wash Reagent Blank Reagent Spk A ReagentSpk B L1273-1 SpkC L1278-l4SpkD L1278-18SpkC L1278-29 Spk D X C 1 11003-1 L1278-1 L1278-1 Rep L1278-2 L1278-2 L1278-3 L1278-4 L1278-5 L1278-6 L1278-7 X C 1 11003-2 L1278-8 L1278-9 L1278-10 L1278-U L1278-12 L1278-13 L1278-14 L1278-14Rep X Ci 11003-3 L1278-15 L1278-16 L1278-17 L1278-18 L1278-18Rep LI278-19 L1278-20 X C ll 1003-4 L1278-21 L1278-22 L1278-23 L1278-24 L I278-25 L1278-26 L1278-27 X C ll 1003-5 L1278-28 L1278-29 L1278-29 Rep L127S-30 U278-31 L1278-32 XC111003-6 Sponsor ID - NA NA NA MW-2 (0-2) MW-5 (23-25) MW-4 (13-15) MW -6(9-ll) MW-2 (0-2) MW-2 (0-2) MW-2 (3-5) 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) 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 CS c c LCS LCS LF LF LF LF CS s s s s s s s s s CS s s s s s s s s CS s s s s s s s CS s s s s s s s CS s s S s. s s CS Run No. 111203A-801 U1203A-802 U1203A-803 111203A-804 111203A-805 111203A-806 111203A-87 111203A-808 I112Q3A-809 111203A-810 1I1203A-811 111203A-812 1I1203A-813 111203A-814 IU203A-815 111203A-816 111203A-817 111203A-818 1U203A-819 111203A-820 UI203A-821 111203A-822 111203A-823 111203A-824 111203A-825 111203A-826 111203A-827 1U203A-828 111203A-829 111203A-830 111203A-831 111203A-832 111203A-833 111203A-834 111203A-835 1I203A-836 111203A-837 111203A-838 1I1203A-839 1U203A-840 111203A-84I I11203A-842 11I203A-843 111203A-844 111203A-845 111203A-846 U1203A-847 111203A-848 111203A-849 U1203A-850 111203A-851 111203A-852 111203A-853 111203A-854 111203A-855 ' U1203A-856 1.1203A-857 111203A-858 U12Q3A-859 Analyte Found (ppt) = (peak aiea - intercept) / slope x DF . Recovery (%) - [analyte found (ppt)-aaalyte found in control (ppt)] x 100 amount added (ppt) Std. Cone. Dilution (ppp 0 Factor - 25 50 - 100 - 250 - 500 - 1000 - 250 -- -1 -1 -1 1000 100 1000 - 1000 25 - - 1000 - 1000 10000 - 1000 - 100 - 100 - 100 - 100 100 50 . - 10 100 - 10 - 100 - 100 100 - 100 - 100 100 - - 10 100 - 1000 100 100 - 100 20 250 - 100 - 20 - 10 - 10 - 200 - 100 - 100 500 - - 100 - 1000 - 1000 - 200 - 100 - 100 1000 Peak Area 0 4273 9041 17266 41590 80055 163829 40821 0 251 8689 80411 29710 69465 24663 35465 4219 21558 17156 5175 50352 11037 7784 8233 12453 12077 7832 37145 8646 13243 34099 13942 38008 20303 19740 14503 38499 12252 12334 58174 70077 18584 32297 36469 66541 34223 56502 47617 43828 17442 10007 71742 25925 15983 15965 48618 28663 13442 141105 Analyte Found (ppt) - - - ND 53.2 526 192000 45300 158000 230000 138000 109000 * 328000 6870 4730 5020 7800 7550 2410 5300 832 22100 8780 24600 13000 12600 2500 7670 77200 37900 45700 11800 4170 Amount Added (ppt) . . 50 500 50000 25000 100000 100000 - - - - - - - - Recovery (%> . _ . . . . . . 106 105 108 129 120 129 . - - - - Analyte Found (ppb) . . . . - - 1100 872 2620 55.0 37.8 40.2 62.4 60.4 . 19.3 42.4 6.66 177 70.2 197 104 101 20.0 61.4 618 303 366 94.4 33.4 43400 4430 3680 3100 56900 11100 6190 - 16700 101000 101000 63200 18500 8450 - - - -- - 347 - 35.4 - 29.4 - 24.8 455 - 88.8 - 49.5 - - 134 - 808 - 808 - 506 - 148 - 67.6 - - -- Standard Curve: Linear (1/x weighted) Intercept = 605.783 Slope = 151.858 Coef. Of Det. = 0.990509 Total Solids (%) . . . . . . . . . . 84.67 84.67 81.95 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 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 R und (ppb) Dry Weight . . . . . . . . . . . . . 1300 1030 3200 60.8 47.8 50.1 79.1 76.4 25.1 48.9 7.69 205 88.4 259 140 136 22.7 73.8 770 377 455 121 49.0 416 41.8 39.3 30.3 530 111 52.2 163 954 954 596 183 86.4 - 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 Samplewas analyzed at several different dilution levels. The appropriate results are reported. CK = Check Standard ND = Not detected = Response between 0 and 25 ppt NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by:^. a 4 o l o : 000124 il RESEARCH 3058 Research D rive State Colleg- e, 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 samplesJisted below were removed from refrigerator No. Tim e___tk O Date Initials CLIENT SAMPLE ED na na na MW-2 (0-2) MW-5 (23-25) MW-4 (13-15) MW-6 (9-11) EXYGEN ID NUMBER Reagent Blank Reagent Spk A Reagent Spk B L1278-1 SpkC L1278-14 SpkD L1278-18 Spk C L1278-29 Spk D WEIGHT (g) _ _ 5.0 5.0 5.0 5.0 FORTIFICATION (ng) _ 2.0 20.0 2000.0 1000.0 4000.0 4000.0 - _ __ - - __ -- - _ __ _- _ - _ __ - __ - __ _- - -_ - _ __ - - __ - - -- Reagent Spk A Reagent Spk B L1278-1 SpkC LI278-14 SpkD L1278-18 SpkC L1278-29 SpkD Spiking Solution Used F092203-5 (10 ng/mL) F092203-4 (100 ng/mL) F092203-2 (10000 ng/mL) F092203-2 (10000 ng/mL) F092203-2 (10000 ng/mL) F092203-2 (10000 ng/mL) Volume Used for Spiking 200 |oL(200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 100 pL (200 pL micropipet) 400 pL (200 pL micropipet) 400 pL (200 pL micropipet) jlnitial/Date iL lU l( n\ii2J z jL / I p k f it /wllzjf L /i]ltzfo Time t H x Date il [n iC Initials After weighing samples were returned to refrigerator N o .. Time fe>3t) Date Initials. Comments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: Analysis Summary: Data Set: maafr Data Set: ~ ________ Data Set: Initials/Date: Initials/Date: Initials/Date: LSet extraction/analysis data verified by:. I-- \ Date:. ALJul0y 206,200011/21 5 } 11 11 I 1 1) ]1 I ] 5I ) RSEA RC H 3058 Research D rive Phone: 814-272-1039 State College, P A 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: PFOA Client ID na na na MW-2 (0-2) MW-5 (23-25) MW-4 (13-15) MW-6(9-ll) - Exygen ID Reagent Blank Reagent Spk A Reagent Spk B L1278-1 SpkC L1278-14SpkD L1278-18 SpkC LI278-29 Spk D - - STEP STEP STEP STEP STEP STEP Dilutions STEP Dilutions STEP 1 2 3 4 5 6 (mL/mL) 7 (mlVmL) 8 --A -- -- /--s - -_ "Md -- 1 - 1 - \1 - \ - / \ 1 \ 0 0`Mo,aM.o >/ -- - - -- -- -- ------ - - - - ------ - - - - - - - - - - - -- --- - - - - - -- - - --- - - - - - -- - - --- - - - - - -- - - -- - - - - - - -- - - --- - - - - - -- - - --- - - - - - -- - - --- - - - - - -- - - --- - -- *Initials/Date - n |i2 $ u 4r h SSSSSTTTTTEEEEEPPPPP 24351::::: CAFBSiPredlintEdnetrgr5citomufhulpurLgomteouonfgf4ohmc0rlgeem1lat0ahnLsmasunwiaponiclturhatonehdsdyisapsctehr-a3cka0er0bb0yfirlhptaemrneddftoyrp~e1Imwiantuerte 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. Initials and date under each step indicates the personnel that performed this step COMMENTS: -- - -- 5 J '. i l a i n 1i0z0iOa'-b lKPpjlzjD -- - - - Final extracts stored in refrigerator Initials: Reagents/ Materials Methanol C18SPE Type I Water _ Lot# 43230 \n1326H B 2. NA _ . _ - Initials/Date _ B ill 12-03 _ __ _ _ HPLC Methanol * f3 1 ta 3 2 4 AmmoniumAcetate Type I water NA -- Initials/Date Date: July 19,2001/4 32:1000  M asslynx - Sam ple List Sample List: C:\MASSLYNX\008 APFi >.PRO\SampleDB\111203A.spl Printed: Fri Nov 14 12:36:20 2003 l "1 Exygen STUDYNO. UT7< ) Page 1 Page Position: (1,1) Vial File Name LIM S ID C lien t ID S a m p le D escription Matrix Sam p le Type C o n e (ng/L) C o n e B C o n e C T e st ID D F 1 21 111203A-801 2 22 111203A-802 __ 3 23 111203A-803 ... 4 24 111203A-804 __ 5 25 111203A-805 __ 6 26 111203A-806 ... 7 27 111203A-807 __ 8 28 111203A-808 __ 9 92 111203A-809 __ 10 31 111203A-810 __ 11 32 111203A-811 -- 12 33 111203A-812 __ 13 34 111203A-813 __ 14 35 111203A-814 15 36 111203A-815 __ 16 37 111203A-816 __ 17 22 111203A-817 __ 18 38 111203A-818 __ 19 39 111203A-819 __ 20 40 111203A-820 __ 21 41 111203A-821 __ 22 42 111203A-822 __ 23 43 111203A-823 __ 24 25 44 45 111203A-824 111203A-825 ... __ 26 46 111203A-826 . . . 27 23 111203A-827 . . . 28 47 111203A-828 -- 29 48 111203A-829 . . . 30 49 111203A-830 __ 31 50 111203A-831 __ 32 51 111203A-832 . . . 33 52 111203A-833 . . . 34 53 111203A-834 . .. 35 54 111203A-835 . . . 36 24 111203A-836 37 55 111203A-837 __ 38 56 111203A-838 __ 39 57 111203A-839 . .. 40 58 111203A-840 . . . 41 59 111203A-841 __ 42 60 111203A-842 . . . 43 61 111203A-843 -- 44 25 111203A-844 -- __ -- -- __ __ -- -- __ __ -- -- -- ... __ __ __ -- __ -- ... __ __ -- -- __ __ -- -- -- ... ... -- -- -- __ __ -- -- __ -- -- -- -- -- X C 1 11003-0,0 ng/L standard -- Blank 0 ----0 X C 1 11003-1,25 ng/L standard -- Standard 25 ----0 X C 1 11003-2,50 ng/L standard -- Standard 50 ... 0 X C 1 11003-3,100 ng/L standard -- Standard 100 ----0 X C 1 11003-4, 250 ng/L standard -- Standard 250 ----0 X C 1 11003-5, 500 ng/L standard -- Standard 500 ----0 X C 1 11003-6,1000 ng/L standard -- Standard 1000 -- 0 X C 1 11003-7,250 ng/L check standard -- QC 250 -- -- 0 Methanol W ash -- Blank -- -- ... 0 Reagent Blank -- Blank -- ----0 Reagent Spk A, 50 ng/L -- QC 50 -- -- 0 Reagent Spk B, 500 ng/L -- QC 500 ... ... 0 L1278-1 Spk C , 50000 ng/L, DF=1000 -- QC 50000 ----0 L1278-14 Spk D, 25000 ng/L, DF=100 -- QC 25000 ^ -- -- 0 L1278-18 Spk C, 5eeee-ng/L, DF=1000 -- QC 50000 CD -- -- 0 L1278-29 Spk D, 100000 ng/L, DF=1000 -- QC 100000 -- 0 X C 1 11003-1,25 ng/L standard -- Standard 25 -- 0 L1278-1, DF=1000 -- Analyte -- -- ... 0 L1278-1 Rep, DF=1000 -- Analyte -- ... -- 0 L1278-2, DF=10000 -- Analyte -- ----0 L1278-2, DF=1000 -- Analyte -- ----0 L1278-3, DF=100 -- Analyte -- ----0 L1278-4, DF=100 -- Analyte -- ... -- 0 L1278-5, DF=100 -- Analyte -- ... ... 0 L1278-6, DF=100 L1278-7, DF=100 -- Analyte -- Analyte -- -- ----0 ----0 X C 1 11003-2, 50 ng/L standard -- Standard 50 ----0 L1278-8, DF=10 -- Analyte -- -- ... 0 L1278-9, DF=100 -- Analyte -- ----0 L1278-10, DF=10 -- Analyte -- ... ... 0 L1278-11, DF=100 -- Analyte -- ----0 L1278-12, DF=100 -- Analyte -- ----0 L1278-13, DF=100 -- Analyte -- ----0 L1278-14, DF=100 -- Analyte -- ----0 L1278-14 Rep, DF=100 -- Analyte -- ----0 X C 1 11003-3,100 ng/L standard -- Standard 100 ----0 L1278-15, DF=10 -- Analyte -- ----0 L1278-16, DF=100 -- Analyte -- ... ... 0 L1278-17, DF=1000 -- Analyte -- ----0 L1278-18, DF=100 -- Analyte -- ----0 L1278-18 Rep, DF=100 -- Analyte -- ----0 L1278-19, DF=100 -- Analyte -- ---- 0 L1278-20, DF=20 -- Analyte -- ---- 0 X C 1 11003-4, 250 ng/L standard -- Standard 250 ... -- 0 1 1 1 1 1 1 1 1 1 1 1 1 1000 100 1000 1000 1 1000 1000 10000 1000 100 100 100 100 100 1 10 100 10 100 100 100 100 100 1 10 100 1000 100 100 100 20 1 O 1 0 0 ,0 0 0 ( & TOGO 1} 1 1 1 1 ]) Masslynx - Sample List Sample List: C:\M ASSLYNX\008APFO.PRO\Sam pleDB\111203A.spl Printed: Fri Nov 14 12:36:20 2003 1/,/) 1) ____________________ MS Method H P LC Method MS Tune File Inj Volum e (pL) 1 008 PFO A 2 008 PFOA 3 008 PFO A 4 008 PFO A 5 008 PFOA 6 008 PFO A 7 008 PFO A 8 008 PFO A 9 008 PFOA 10 008 P F O A 11 008 P FO A 12 008 P FO A 13 008 P FO A 14 008 P FO A 15 008 P FO A 16 008 P FO A 17 008 P FO A 18 008 P FO A 19 - 008 P FO A 20 008 PFO A 21 008 P F O A 22 008 PFO A 23 008 PFO A 24 008 PFO A 25 008 PFO A 26 008 PFO A 27 008 PFO A 28 008 PFO A 29 008 PFO A 30 008 P F O A 31 008 P F O A 32 008 PFO A 33 008 PFO A 34 008 PFO A 35 008 PFO A 36 008 PFO A 37 008 PFO A 38 008 PFO A 39 008 PFO A 40 008 PFO A 41 008 P F O A 42 008 PFO A 43 008 PFO A 44 008 PFO A water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water PFOA Tune PFOA Tune PFO A Tune PFO A Tune PFOA Tune PFOA Tune PFO A Tune PFO A Tune PFOA Tune PFO A Tune PFOA Tune PFOA Tune PFO A Tune PFOA Tune PFO A Tune PFOA Tune PFOA Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFOA Tune PFOA Tune PFO A Tune PFOA Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFOA Tune PFO A Tune PFO A Tune PFOA Tune PFO A Tune PFOA Tune PFO A Tune 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 .15 15 15 15 15 15 15 15 15 15 15 15 OOOiS'S 11 1 } Exygen STUDY NO. t-II/fi Page 2 Pag e Position: (2,1 ) I ! I I 11i 1 Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO,PRO\Sam pleDB\111203A.spl Printed: Fri Nov 14 12:36:20 2003 1 Vial File Name LIM S ID C lien t ID S a m p le D escriptio n 45 62 111203A-845 -- 46 63 111203A-846 -- 47 64 111203A-847 -- 48 65 111203A-848 -- 49 66 111203A-849 -- 50 67 111203A-850 -- 51 68 111203A-851 -- 52 26 111203A-852 -- 53 69 111203A-853 -- 54 70 111203A-854 -- 55 71 111203A-855 -- 56 72 111203A-856 -- 57 73 111203A-857 -- 58 74 111203A-858 -- 59 27 111203A-859 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- L1278-21, DF=100 L1278-22, DF=20 L1278-23, DF=10 L1278-24, DF=10 L1278-25, DF=200 L1278-26, DF=100 L1278-27, DF=100 X C 1 11003-5,500 ng/L standard L1278-28, DF=100 L1278-29, DF=1000 L1278-29 Rep, DF=1000 L1278-30, DF=200 L1278-31, DF=100 L1278-32, DF=100 X C 1 11003-6,1000 ng/L standard *1 0 0 0 Exygen study n o . M2-70 Page 3 Page Position: (1, 2) Matrix Sa m p le T y p e C o n e (ng/L) C o n e B C o n e C T e st ID D F -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Standard 500 -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Standard 1000 -- __ 0 100 -- -- 0 20 -- -- 0 10 -- -- 0 10 -- -- 0 200 -- -- 0 100 -- -- 0 100 -- -- 01 -- -- 0 100 -- -- 0 1000 ---- 0 1000 -- -- 0 200 -- -- 0 100 -- -- 0 100 -- -- 01 l l l 1 1 .) .1 1 Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO.PRO\Sam pleDB\111203A.spl Printed: Fri Nov 14 12:36:20 2003 l A # L ______________________ 11 MS Method H P L C Method MS T u n e File Inj V olum e (mL) 45 008 PFO A 46 008 PFO A 47 008 PFO A 48 008 PFO A 49 008 PFO A 50 008 P FO A 51 008 P F O A 52 008 P FO A 53 008 P FO A 54 008 PFO A 55 008 PFO A 56 008 PFO A 57 008 P F O A 58 008 P FO A 59 008 P FO A water water water water water water water water water water water water water water water PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune PFO A Tune 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 000130 ) i 1 1 Exygen STUDY N O . .I2L :1 i Page 4 22Page Position: ( , ) i LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exvsen Study No: L1278 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381 : Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Quat 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:MA10464) (JONESCHROMATOGRAPHY: Part No. FK5962EJ) Mobile Phase (A) Mobile Phase (B) M2 metMhanAoml monium Acetate in Type I Water Analyst: Karen Risha Exygen Research P30h5o8neR: e(s8e1a4r)ch27D2r-1iv0e3,9StFatAeXC:o(ll8e1g4e), 2P3A1-115688001 NOTE: Titnhhseetrmnueamxssteln3ytnpsxaegsttoeisfntawgrsaeurcesoepdmrfopogurrtaethrmeg.eannTeahrleyaspteiasdgoepfsrtichnoitsnodtuaatistnafrtshoeemt. A ll Handwritten Peak ID's by: Scanning Method Report Method: C:\MASSLYNX\008 APFO. PRO\ACQUDB\008 PFOA Last Modified: Wed Mar 20 15:07:50 2002 Printed: Fri Nov 14 12:36:26 2003 Solvent Delay { mins ) : 0.00 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 ) 1 413.00 369.00 0.20 10 10 Page 1 000132 Method Report Method File: Last Modified Printed: C :\MASSLYNX\008 APFO.PRO\ACQUDB\water Friday, November 14, 2003 07:58:46 Friday, November 14, 2003 12:36:32 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Contactl Off Off Off On Off Off Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/zl/min) Draw Position (mm) Stop Time (mins) Injection Volume (/zl) Vial Number 200.0 200 0.10 15.00 15.0 7 Page 1 Pressure 400 400 400 400 400 400 400 400 400 400 Tuning Method Report Method: C:\MASSLYNX\008 A P F O .PRO\ACQUDB\PFOA TUNE Printed: Fri Nov 14 12:36:38 2003 Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 99 300 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 Rdbk 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 '9 11 -696 Rdbk 98.8 704.4 000134 Quantify Calibration Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03/ Analyst:K.Risha Calibration: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\CurveDB\111203A Last modified: Sun Nov 16 06:27:38 2003 Printed: Sun Nov 16 06:49:36 2003 11 03 Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 3 .3 5 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Sun Nov 16 06:27:21 2003 P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Fri Nov 14 10:37:34 2003 Sun Nov 16 06:49:38 2003 . fcNtiafs Date M ilk ie r Run# J1 iESSO a^L-ToJ iia b j Name: 111203A-801 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000136 Quantify Sample Report Study No.:L1278, Set No.:111203a , Ext.Date:ll/12/03, Analyst :K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 A PFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-802 Text: 1 : PFOA Page 2 Exygen Research, 3058 Research Drive, State College, PA 16801 000137 Quantify Sample Report Study No.:Xj1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-803 Text: 1 : PFOA Page 3 Exygen Research, 3058 Research Drive, State College, PA 16801 000138 Quantify Sample Report Study N o . :L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PF< Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Page 4 Name: 111203A-804 Text: 1 : PFOA X C 1 11003-3,100 ng/L standard -,111203A-804 Sm (Mn, 2x2) 100 %- 157.22666 14-NOV-2003 14:44:43 LC/MS/MS #7 MRM of 1 Channel ES413 >369 2.68e5 Area 5.00 Time7T V | I I n T H T |T T r T p m T , 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000133 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Page 5 Name: 111203A-805 Text: 1: PFOA X C 111003-4, 250 ng/L standard 111203A-805 S m (Mn, 2 x2 ) 100- %: 5.26 415901 14-Nov-2003 15:01:35 LC/MS/MS #7 MRM of 1 Channel ES413 >369 6.33e5 Area (y 'T-'r-n e'!--I--I--I--j'i I I f"| I T' 1 "i"r'ri r r 1} i i t t j t n"i \*r r \ ryt 1v )' I i"i 11'( 1.00_________ 2X)0_________ O 00_________ 4.00 5.00 "i r -1 ' it i 1 r i 1 I 1 1 T i t i j 1 "1 I Tim e 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000140 Quantify Sample Report Study No.:L1278, Set N o . :111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APF0.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Page 6 Name: 111203A-806 Text: 1 : PFOA X C 1 11003-5,500 ng/L standard 111203A-806 Sm (Mn, 2x2) 100n %: 0 I I I I I I 1 I I I ` 1 1 ` f 1 1 I I I I I I """I I I I I I I 1 I 1.00 2.00 3.00 4.00 5.27 5.00 14-NOV-2003 15:18:24 LC/MS/MS #7 MRM of 1 Channel E S 413 >369 1.30e6 Area i~H '.1 IT T 'I 1r -r- r '|' I I I I I I I I I I T im e 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst :K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PF< Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Page 7 Name: 111203A-807 Text: 1 : PFOA X C111003-6,1000 ng/L standard 111203A-807 Sm (Mn, 2x2) 100i %- 5.29 163829 14-NOV-2003 15:35:06 LC/MS/MS #7 MRM of 1 Channel E S 413 >369 2.60e6 Area a 1.00 2.00 3.00 4.00 5.00 I ' I 'I I I I ' I ' I ' ' ' ' I Tim e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000142 : Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha i Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslyax\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 r * Job Code: j ' Printed: Sun Nov 16 06:49:38 2003 Rage 8 Name: 111203A-808 Text: I s PFOA X C 1 11003-7,250 ng/L ch eck standard 111203A-808 Sm (Mn, 2x2) 10Ch 450.82291 %: 0 I I I I [ IT T I ( 1"1 I I (.I I I I I I I I I I 1I I I j I I I I i i i ) I" r i 1.00 2.00 3.00 4.00 i 'i I pr" 5.00 14-NOV-2003 15:51:49 LC/MS/MS #7 MRM of 1 Channel ES413 >369 6.57e5 Area ''i >i `i I r i i | n I i |'I i i i |Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-809 Text: Page 9 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K. Ri sha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-810 Text: 1: PFOA Page 10 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst :K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-811 Text: 1 : PFOA Page 11 Exygen Research, 3058 Research Drive, State College, PA 16801 000146 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PF< Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Page 12 Name: 111203A-812 Text : 1: PFOA Reagent Spk B, 500 ng/L 111203A-812Sm (Mn, 2x2) 100i %- 5.32 80411 14-NOV-2003 16:59:00 LC/MS/MS #7 M RM of 1 Channel E S 413 > 369 1.35e6 Area 6.00 7.00 T-n Time 8.00 Exygen Research, 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha f - Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A 1 Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 r" Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-813 Text: Page 13 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-814 Text: 1 : PFOA Rage 14 Exygen Research, 3058 Research Drive, State College, PA 16801 000149 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-815 Tent: 1 : PFOA Page 15 Exygen Research, 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No. :L1278, Set No.:111203A, Ext .Bate: 11/12/03, Analyst :K.Ri sha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-816 Text: 1 : PFOA Page 16 Exygen Research, 3058 Research Prive, State College, PA 16801 000151 Quantify Sample Report Study No.:L1278, Set No.:111203A# Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-817 Text: 1 : PFOA Page 17 Exygen Research, 3058 Research Drive, State College, PA 16801 000152 Quantify Sample Report Study N o .sL1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-818 Text: 1 : PFOA Rage 18 Exygen Research, 3058 Research Drive, State College, PA 16801 3 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-819 Text: 1: PFOA Page 19 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:Iil278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-820 Text: 1: PFOA Page 20 Exygen Research, 3058 Research Drive, State College, PA 16801 000155 Quantify Sample Report Study No. :L1278, Set No.:111203A, Ext.Date: 11/12/03, AnalystsK.Risha /-** Sample Lists P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A ; Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 A PFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 r-' Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-821 Text: 1 : PFOA Page 21 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\Sani>leDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-822 Text: 1 : PFOA Page 22 Exygen Research, 3058 Research Drive, State College, PA 16801 000157 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-823 Text: 1 : PFOA Page 23 Exygen Research 3058 Research Drive, State College, PA 16801 000158 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SarapleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-824 Text: 1 : PFOA Page 24 Exygen Research, 3058 Research Drive, State College, PA 16801 00015-3 Quantify Sample Report Study No.:L1278/ Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample Lists P:\Data\LCMSMS7\Masslynx\008 ABFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-825 Text: 1 : PFOA Page 25 Exygen Research, 3058 Research Prive, State College, PA 16801 000160 Quantify Sample Report Study Mo.:L1278, Set No.:111203A, Ext.Bate:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\ 111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-826 Text: 1 : PFOA Page 26 Exygen Research, 3058 Research Drive, State College, PA 16801 000161 Quantify Sample Report Study No.:L1278/ Set No.:111203A, Ext.Pate:11/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Sun Nov 16 06:27:21 2003 P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethPB\111203 PFOA Fri Nov 14 10:37:34 2003 Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-827 Text: 1 : PFOA Page 27 Exygen Research, 3058 Research Drive, State College, PA 16801 000162 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\Sanq?leDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-828 Text: 1 : PFOA Page 28 Exygen Research, 3058 Research Drive, State College, PA 16801 ^ rf? '> Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, AnalystrK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-829 Text: 1 : PFOA Page 29 Exygen Research, 3058 Research Drive, State College, PA 16801 000X84 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-830 Text: 1 : PFOA Page 30 Exygen Research, 3058 Research Drive, State College, PA 16801 165 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date-.il/12/03, Analyst :K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APPO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PPOA Last modified: Pri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-831 Text: 1: PFOA Page 31 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-832 Text: 1: PFOA Page 32 Exygen Research, 3058 Research Drive, State College, PA 16801 000167 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha r* Sample List: P:\Data\LCMSMS7VMasslynx\008 APFO.PRO\SampleDB\111203A . Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 T"4 Job Code: ' Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-833 Text: < 1 : PFOA Page 33 ..N ' Exygen Research, 3058 Research Drive, State College, PA 16801 0001SS Quantify Sample Report Study NO.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha r"* Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A ! Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 v" Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-834 Text: 1 : PFOA Page 34 A Exygen Research, 3058 Research Drive, State College, PA 16801 000163 Quantify Sample Report Study No. :L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst :K.Ri sha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-835 Text: 1: PFOA Page 35 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date: 11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SamgpleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Page 36 Name: 111203A-836 Text: 1 : P F O A ___________________________________________________________________________________________________________________________________________________ XC111003-3,100 ng/L standard 14-NOV-2003 23:41:22 111203A-836 Sm (Mn, 2x2) LC/MS/MS #7 MRM of 1 Channel ES413 >369 2.41 e5 Area 1.00 2.00 3.00 4.00 T*r >i '"'"I r-'1' '' r 1T~1I I I I1 1 1I 11,"1I Time 5.00 6.00 7.00 8.00 Exygen Research 3058 Research Drive State College, PA 16801 000171 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.FRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-837 Text: 1: PFOA Page 37 Exygen Research, 3058 Research Drive, State College, PA 16801 2 Quantify Sample Report Study No.:L1278f Set No.:111203a , Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-839 Text: 1 : PFOA Rage 39 Exygen Research, 3058 Research Drive, State College, PA 16801 000173 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-840 Text: 1: PFOA Page 40 Exygen Research, 3058 Research Drive, State College, PA 16801 000174 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-841 Text: 1: PFOA Page 41 Exygen Research, 3058 Research Drive, State College, PA 16801 000175 Quantify Sample Report Study No.:L1278, Set No.:111203a , Ext.Date:ll/12/03, AnalysttK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-842 Text: 1 : PFOA Page 42 Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 1 '? G Quantify Sample Report Study No.:L1278, Set N o . :111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-843 Text: 1 : PFOA Page 43 Exygen Research, 3058 Research Drive, State College, PA 16801 000177 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Bate:11/12/03, Analyst:K.Risha Sample Bist: P:\Data\BCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Bast modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\BCMSMS7\Masslynx\008 APFO.PRO\MethBB\111203 PF< Bast modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Page 44 Name: 111203A-844 Text: 1 : PFOA X C 1 11003-4, 250 ng/L standard 111203A-844 Sm (Mn, 2x2) 10(h %- 5.35 36469 15-Nov-2003 01:55:29 LC/MS/MS #7 MRM of 1 Channel ES413 >369 6 .1 1e5 Area 6.00 T im eT - T- p r - l--I - r - ] - T T - T-T--I 7.00 8.00 ExFOen Research, 3058 Research Drive, State College, PA 16801 0001^8 Quantify Sample Report Study N.:L1278, Set N o . :111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 ARFO.RRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-845 Text: 1 : PFOA Rage 45 Exygen Research, 3058 Research Drive, State College, PA 16801 0001*79 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: F:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-846 Text: 1 : PFOA Page 46 Exygen Research, 3058 Research Drive, State College, PA 16801 000180 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Sun Nov 16 06:27:21 2003 P:\Data\LCMSMS7\Masslynx\008 A P F O .PRO\MethDB\ 111203 PFOA Fri Nov 14 10:37:34 2003 Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-847 Text: 1: PFOA Page 47 Exygen Research, 3058 Research Drive, State College, PA 16801 000181 Quantify Sample Report Study No. :L1278, Set No.:111203A, Ext.Date:ll/12/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-848 Text: 1 : PFOA Page 48 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, AnalystsK. Ri sha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-849 Text: 1: PFOA Page 49 Exygen Research, 3058 Research Drive, State College, PA 16801 000183 Quantify Sample Report Study No.:Ll278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-850 Text: 1: PFOA Page 50 Exygen Research, 3058 Research Drive State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, AnalystsK.Risha Sample List: P:\Data\LOMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-851 Text: 1 : PFOA Page 51 Exygen Research, 3058 Research Drive State College, PA 16801 000,185 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Rage 52 Name: 111203A-852 Text: 1 : PFOA X C 1 11003-5, 500 ng/L standard 111203A-852 Sm (Mn, 2x2) 15-Nov-2003 04:09:43 LC/MS/MS #7 MRM of 1 Channel ES 413 >369 1.23e6 Area 1.00 2.00 3.00 4.00 I I ' ' T""i""r ' ' t'1'111T 1' 1I Tim e 5 .0 0 __________6 M ________ 7 0 0 __________8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000186 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-853 Text: 1 : PFOA Page 53 Exygen Research, 3058 Research Drive State College, PA 16801 000187 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:11/12/03, AnalysttK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-854 Text: 1 : PFOA Page 54 Exygen Research, 3058 Research Drive, State College, PA 16801 000188 Quantify Sample Report Study No.:L1278/ Set No.:111203A, Ext.Date:11/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-855 Text: 1: PFOA Page 55 Exygen Research, 3058 Research Drive, State College, PA 16801 000189 Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sim Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-856 Text: 1 : PFOA Page 56 Exygen Research/ 3058 Research Drive State College, PA 16801 000190 Quantify Sample Report Study NO.:L1278, Set No.:111203A, Ext.Date:11/12/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-857 Text: 1: PFOA Page 57 Exygen Research, 3058 Research Drive, State College, PA 16801 AJ L. Q. -y fJ Quantify Sample Report Study No.:I>1278, Set No.:111203A, Ext.Date:ll/12/03, AnalystK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Name: 111203A-858 Text: 1: PFOA Page 58 Exygen Research, 3058 Research Drive, State College, PA 16801 ; Quantify Sample Report Study No.:L1278, Set No.:111203A, Ext.Date:ll/12/03, Analyst:K.Risha --' Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111203A Last modified: Sun Nov 16 06:27:21 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Sun Nov 16 06:49:38 2003 Page 59 I Name: 111203A-859 Text: 1 : PFOA X C 111003-6,1000 ng/L standard 111203A-859 Sm (Mn, 2x2) 15-Nov-2003 06:07:20 LC/MS/MS #7 MRM of 1 Channel ES413 >369 2.41 e6 Area 1 .0 0 2 .0 0 3 .0 0 4 .0 0 5 .0 0 T " i" n - r | I T -i-r | I i-i r | i n"i | i i t t | T lT ie 6 .0 0 7 .0 0 8 .0 0 t Exygen Research, 3058 Research Drive, State College, PA 16801 Sponsor Study No: NA Exygen Study No: L1278 Analyte: PFOA r Ions Monitored: Site: 413->369 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: 111003A Karen Risha LC/MS/MS Unit #7 11/10/03 11/10-11/03 pm* Exygen Sponsor Sample Run 1 ID XCl 11003-0 ID Code No. - c 111003A-501 XC111003-1 - CS 111003A-502 XCl 11003-2 - CS 111003A-503 c 1 XCl 11003-3 XCl 11003-4 - CS 111003A-504 - CS 111003A-505 nm , XCl 11003-5 : XCl 11003-6 XCl 11003-7 Methanol Wash 4*"* Reagent Blank Reagent Spk A - CS 111003A-506 - CS 111003A-507 - CS 111003A-508 - c 111003A-509 NA c 1U003A-510 NA LCS 111003A-511 ' ' Reagent Spk B NA LCS 111003A-512 L1278-1 SpkC MW-2 (0-2) LF 111003A-513 L1278-14 SpkD MW-S (23-25) LF 111003A-514 XCl 11003-1 XCl 11003-2 L1278-1 L1278-1 Rep mm L1278-2 - MW-2 (0-2) MW-2 (0-2) MW-2 (3-5) CS 111003A-515 CS 111003A-516 s 111003A-517 s U1003A-518 s 111003A-519 L1278-3 L1278-4 L1278-5 M XCI11003-3 MW-2 (8-10) MW-2 (13-15) MW-2 (18-20) - s 111003A-520 s 111003A-521 s 111003A-522 CS 111003A-523 LI278-6 L1278-7 L1278-8 L 1278-9 MW-2 (23-25) MW-2 (28-30) MW-2 (33-35) MW-5 (0-2) s 111003A-524 s 111003A-525 s 111003A-526 s 111003A-527 r L1278-10 i XCl 11003-4 MW-5 (3-5) - s 111003A-528 CS 111003A-529 L1278-11 L1278-12 p L1278-13 MW-5 (8-10) MW-5 (13-15) MW-5 (18-20) sss U1003A-530 111003A-531 111003A-532 V L1278-14 L1278-14Rep MW-5 (23-25) MW-5 (23-25) ss 111003A-533 111003A-534 XCl 11003-5 - CS 111003A-535 t. - XCl 11003-6 - Analyte Found (ppt) = (peak area - intercept) / slope x DF CS 111003A-536 Recovery (% ) = [analyte found (ppt)-analyte found in control (ppt)] x 100 amount added (ppt) Std. Cone. Dilution Peak (ppt) Factor Area 0- 0 25 - 3650 50 - 7486 100 - 13815 250 - 35372 500 - 68963 1000 - 141260 250 - 35658 -- 0 -1 0 - 1 7457 - 1 68809 - 1 19066772 - 1 3146206 25 - 4736 50 - 7629 - i 24077158 - 1 20982604 - 1 37079996 - 1 1696077 - 1 1230678 - 1 1280725 100 - 14554 - 1 1679077 - 1 1855369 - 1 544238 - 1 1312797 - 1 176840 250 - 34857 - i 4833649 - i 2130617 - 1 5738712 - 1 2729042 - 1 2926074 500 - 69161 1000 - 138471 Analyte Amount Analyte Found Added Recovery Found (ppo (ppo (%) (PPb) - -- - - -- - -- - -- . - -- - - -- -- -- ND 49.3 50 493 500 A 500 A 500 -- -**- ***- -*****- - - 99 99 - - -- - *- - *- - *- - *- - - *- - -- -- -- - - Standard Curve: Linear (1/x weighted) Intercept = 646.174 Slope = 138.233 Coef. Of Det.= 0.999707 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) Dry Weight . . - - 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 111203A. Sample requires dilution. See data set 111203A. Spreadsheet prepared by: \_ 000194 n 3058 Research Drive R E S E A R C H State College, 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. 3 % Time QQCsO________ Date llftnlfi?, Initials CLIENT SAMPLE ID na na na MW-2 (0-2) MW-5 (23-25) 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) EXYGEN ID NUMBER Reagent Blank Reagent Spk A Reagent Spk B L1278-1 SpkC L1278-14 SpkD L1278-1 L1278-1 Rep L1278-2 L1278-3 L1278-4 L1278-5 L1278-6 L1278-7 L1278-8 L1278-9 L1278-10 L1278-11 L1278-12 L1278-13 L1278-14 L1278-14Rep WEIGHT (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 FORTIFICATION (ng) _ 2.0 20.0 20.0 20.0 _ - _ _ _ _ _ _ _ _ _ _ _ - Reagent Spk A Reagent Spk B L1278-1 SpkC L1278-14 SpkD - Spiking Solution Used F092203-5 (10 ng/mL) F092203-4 (100 ng/mL) F092203-4 (100 ng/mL) F092203-4 (100 ng/mL) - All samples were weighed on balance No 2 - 0 _____ Time <0930 Date ll/joja=? Volume Used for Spiking Initial/Date 200 pL (200 pLmicropipet) p h n \ t \ & 200 pL (200 pL micropipet) P j f / \ \ \ b \ t 200 pL (200 pLmicropipet) A\dIq3 200 pL (200 pLmicropipet) /l\^o|2> - y -'' Initials.....Cm . After weighing samples were returned to refrigerator No. 3 2 Time JDSO_______ Date i i j i o j ^ ______ Initials (lP~. iJ/ti/n-KComments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: /V y / Analysis Summary: Data Set: i u d q s a Data Set: 1\ 1 2 .0 3 A Data Set:_______ Initials/Date:. Initials/Date:. Initials/Date:. /JlM|5 / n \J.4l.05 Set extraction/analysis data verified by: m f Date:. JIM IU*y2 C W 0 1 9 5 1 ) j} " l t : ) .i "T'"> i i >1 11 3058 Research D rive 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: PFOA Client ID Exygen BD STEP STEP STEP STEP STEP STEP Dilutions STEP Dilutions STEP 1 2 3 4 5 6 (mL/mL) 7 (mL/mL) 8 Reagents/ Materials Lot# na na na MW-2 (0-2) MW-5 (23-25) MW-2 (0-2) Reagent Blank Reagent Spk A 1 ___ Reagent Spk B L1278-1 SpkC L1278-14 Spk D L1278-1 \___ L - ----- Methanol C18 SPE -- -- - TypeIWater NA --- - - --- -- - mm* -- MW-2 (0-2) MW-2 (3-5) MW-2 (8-10) L1278-1 Rep L1278-2 L1278-3 --- & M e_ - - - - - MW-2 (13-15) L1278-4 y> Initials/Date /!K ii|io |o s. MW-2 (18-20) L1278-5 - -V\D - MW-2 (23-25) MW-2 (28-30) MW-2 (33-35) L1278-6 L1278-7 L1278-8 - -'/io -- VlD -- M ,o -- -- -- MW-5 (0-2) MW-5 (3-5) L1278-9 L1278-10 - M o -- -Vu0 -- -- MW-5 (8-10) L1278-11 - o-Yio HPLC MW-5 (13-15) MW-5 (18-20) L1278-12 L1278-13 - 6 ,Vto Methanol M 3 lt 3 2 4 - 0-v/|D AmmoniumAcetate MW-5 (23-25) MW-5 (23-25) L1278-14 L1278-14 Rep 1 1/ \ ! 11/ i ( - J-- -v/i0 ....1 . ! \ Type I water - NA *Initials/Date _ CE C&. cm , i l k k i . * 2 3 . j i h m If/t/tlS, 1 <0 f\ nhfoe Initials/Date h ife > SSSSSTTTTTEEEEEPPPPP42351::::: FCABSiPredlitnEdnetrgr5ciotmufhlupurLgomteouonfgf4ohmc0rlgeem1lta0ahLnsmasuwniaponictlurhatoenhdsdyisapsctehr-ac3ka0er0bb0yfirlhpteamrneddftoyrp~e1Imwiantuerte ^ }m )O M -\o fo o 2 STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP7: LC/MS/MS analysis STEP 8: LC/MS/MS reanalysis. Final extracts stored in refrigerator ,^2- Initials: f e Date: ^Initials and date under each step indicates the personnel that performed this step. COMMENTS: July 19, 2001/4 96X000 1 I r~ < -\ .7/ ~ ~ i > i :.. > > 1 s T 'D 1 :1 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Protocol No.: None Method No.: 01M-008-046* Exygen Study No.: NA Analytes: PFOA Matrix: Type I Water* BXygQfl STUDY N O . 2-/^3 Sample Vol: 40 mL ` Sponsor Sample ID Exygen Sample ID Sample Description Fort Fort. Fort. Micropipet Fort Solution Soin. Cone. Volume used Level ID fne/mL) (ML) (uL) (ppt) Final Solution ID#** Reagents/ Materials Lot# NA 0106020 Type I WaterA - - - XC111003-0 Methanol 4 3 2 3 8 3 3 5 NA 0106020 Type I Water7' F092203-5 10 100 200 25 XC111003-1 C18 SPE \ 4 5 2 0 H B I NA 0106020 Type I Water7' F092203-5 10 200 200 50 XC111003-2 Type I Water NA NA 0106020 Type I Water71 F092203-5 10 400 200 100 XC111003-3 - NA 0106020 Type I WaterA F092203-4 100 100 200 250 XC111003-4 _ - NA 0106020 Type I Water7' F092203-4 100 200 200 500 XC111003-5 - - NA 0106020 Type I WaterA F092203-4 100 400 200 1000 XC111003-6 - - NA 0106020 Type I Water7' F102703-2 100 -- - - - 100 - 200 - 250 XC111003-7 -- Initials/Date: |i f|(0 {, o Vertical arrows in a column indicate identical values. **This m ust be a unique number. Use this system : E xtracted Calibration Soln ID #: XCM M DDYY-0,1,2,3. etc. Samples 40 mL o freeamcohvseadmfrpolemmpesafsnugreerdautosi^nfgreaezeSr O# *$2- mL Time: C f iCiD graduated cylinder. Initials/Date: i'E S /J /j/o jn -? Initials/Date: P E E After measuring, samples returned to tSfngeratorAfreezer # 32- TivosrJOSQ.. Initials/Date: /lE E liijlo f o < Samples fortified: Initials/Date: THIS IS AN EXACT COPY OF THEORIGINAL DOCUMENT.* B Y ^ .,,^ DAtE il(lb[03 SPE clean-up: Initials/Date: /jEE /iljinjo-T. Final volume adjusted to 5 mL: Initials/Date: B E Extracts placed in refrigerator # S 2 - Initials/Date: C E E lu jio jn * STANDARD EXPIRATION DATE: 11/24/03 Oo o Comments: AThis type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of AmmoniumPerfluorooctanoate (APFO) in Water. '0 July 10, 2001/0 ! A. Masslynx - Sample List \A[JSample List: C:\MASSLYNX\008 A P F0 .P R 0 \S a m p le D B \1 11003A.spl Printed: Mon Nov 10 15:38:31 2003 _______________ Vial File Name LIM S ID C lie n t ID Sample Description 1 21 111003A-501 _____ 2 22 111003A-502 -- 3 23 111003A-503 -- 4 24 111003A-504 -- 5 25 111003A-505 -- 6 26 111003A-506 -- 7 27 111003A-507 -- 8 28 111003A-508 -- 9 92 111003A-509 -- 10 31 111003A-510 -- 11 32 111003A-511 -- 12 33 111003A-512 -- 13 34 111003A-513 -- 14 35 111003A-514 -- 15 22 111003A-515 -- 16 23 111003A-516 -- 17 36 111003A-517 -- 18 37 111003A-518 -- 19 38 111003A-519 -- 20 39 111003A-520 -- 21 40 111003A-521 -- 22 41 111Q03A-522 -- 23 24 111003A-523 -- 24 42 111003A-524 -- 25 43 111003A-525 mmm 26 44 111003A-526 -- - 27 45 111003A-527 -- 28 46 111003A-528 -- 29 25 111003A-529 -- 30 47 111003A-530 -- 31 48 111003A-531 -- 32 49 111003A-532 -- 33 50 111003A-533 -- 34 51 111003A-534 -- 35 26 111003A-535 -- 36 27 111003A-536 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- ---- -- -- -- -- -- -- -- -- -- -- -- -- X C 1 11003-0,0 ng/L standard ng/L standardX C 1 11003-1,25 ng/L standard X C 1 11003-2, 50 X C 1 11003-3,100 ng/L standard X C 1 11003-4,250 ng/L standard X C 1 11003-5,500 ng/L standard X C 1 11003-6,1000 ng/L standard X C 1 11003-7,250 ng/L check standard Methanol W ash Reagent Blank Reagent Spk A, 50 ng/L ng/LReagent Spk B, 500 ng/L L1278-1 Spk C, 500 L1278-14 Spk D, 500 ng/L X C 1 11003-1,25 ng/L standard X C 1 11003-2, 50 ng/L standard L1278-1 L1278-1 Rep L1278-2 L1278-3 L1278-4 L1278-5 X C 1 11003-3, 100 ng/L standard L1278-6 L1278-7 L 1278-8 L1278-9 L1278-10 X C 1 11003-4,250 ng/L standard L1278-11 L1278-12 L1278-13 L1278-14 L1278-14 Rep X C 1 11003-5, 500 ng/L standard X C 1 11003-6,1000 ng/L standard '* .1 ' ^ ' T ..1 Exygenstudyno. JJZ2& li Page 1 Page Position: (1 ,1 ) Matrix Sam ple Type C o n e (ng/L) C o n e B C o n e C T e st ID D F _____ Blank 0 -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 Standard-- 500 -- Standard 1000 -- QC 250 -- Blank -- -- Blank -- -- QC -- QC -- QC 50 550000 -- 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 -- Standard 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 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 M S Method 008 PFOA 008 PFO A 008 PFOA 008 PFO A 000088 PPFFOOAA 008 PFOA 008 PFOA 008 PFO A 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFO A 008 PFOA 008 PFOA 008 PFOA 008 PFO A 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFOA 008 PFO A 008 PFOA 008 PFOA \1 '...... p ` ~ ' v ) ...3 Masslynx - Sample List Sample List: C:\MASSLYNX\008 A P FO .f 0\Sam pleDB\111003A.spl Printed: Mon Nov 10 15:38:31 2003 n||blo3>__________ 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 oo o fQ PO H P L C Method MS T u n e File Inj V o lu m e (|j L) water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water PFOATune PFO A Tune PFOATune P FO A Tune PFOATune PFOATune PFOATune PFOATune PFOATune PFOA Tune PFO A Tune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOA Tune PFOATune PFOATune PFOATune PFOATune PFOATune PFOA Tune PFOATune PFO A Tune PFOATune PFOATune PFO A Tune PFOATune PFO A Tune PFOATune 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 li "'"'t "' > Exygenstudyno. J2IH 1 \ ' ~ i> - " i : ..i Page 2 Page Position: (2 ,1 ) 1 LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L1278 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: HewHlPetQt PuaactkPaurmdp(HP) Series 1100HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C -8,5 cm x 2.1 mm i.d. x 4 ja (Exygen ID:MA10327) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : 2 tnM Ammonium Acetate in Type I Water Mobile Phase (B) : Methanol \\W 0^ Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: Titnhhseetrmnueamxssteln3ytnpsxaegsttoeisfntawgrsaeurcesoepmdrfopogurrteathrmeg.aenTneahrleyaspteiasdgoepfsrtichnoitsnodtuaatistnaftrshoeemt. All Handwritten Peak ID's by: II 11o 3 I 000200 Scanning Method Report Method: C:\MASSLYNX\008 APFO.PRO\ACQUDB\008 PFOA Last Modified: Wed Mar 20 15:07:50 2002 Printed: Mon Nov 10 15:42:52 2003 Solvent Delay ( mins ) : 0.00 Function : 1 MRM of 1 Mass Pair ( ESP- i Inter Channel Delay ( Secs ) : 0.03 Span ( Daltons ) : 0.00 Start Time ( Mins ) : 0.00 End Time ( Mins ) : 8.00 Repeats : 1 Channel Parent Daughter Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 413.00 369.00 0.20 10 10 Page 1 000201 "SS M ethod R e p o rt Method File: Last Modified: Printed: C:\MASSLYNX\008 APFO.PRO\ACQUDB\water Monday, November 10, 2003 15:39:51 Monday, November 10, 2003 15:43:01 i HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Contactl Off Off Off On Off Off Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/zl/min) Draw Position (mm) Stop Time (mins) Injection Volume(^1) Vial Number 200.0 200 0.10 15.00 15.0 7 Page 1 Pressure 400 400 400 400 400 400 400 400 400 400 000202 Tuning Method Report Method: Printed: C:\MASSLYNX\008 APFO.PRO\ACQUDB\PFOA TUNE Mon Nov 10 15:43:08 2003 ID o3 Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 101 300 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.4e- 3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rd] 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -6 Rdbk 102.5 711.7 000203 Quantify Calibration Report Study No.:L1278/ Set No.:111003A, Ext.Date:11/10/03/ Analyst:K.Risha Calibration: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\CurveDB\111003A Last modified: Tue Nov 11 09:32:17 2003 Printed: Tue Nov 11 09:33:14 2003 Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000204 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Rage 1 Sanale List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS7\Masslynx\008 Tue Nov 11 09:28:10 2003 P:\Data\LCMSMS7\Masslynx\008 Thu Oct 30 07:08:49 2003 Tue Nov 11 09:33:15 2003 APFO.PRO\SampleDB\111003A APFO.PRO\MethDB\102703 PFOA Initials__ D ate it NIH: 4- Run#Il ^ - ^ l _ Tb .1U.0O3A-SV, Name: 111003A-501 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000205 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Datesll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-502 Text: 1: PFOA Page 2 Exygen Research, 3058 Research Drive, State College, PA 16801 | Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Pate:11/10/03, Analyst:K.Risha -- Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 r" job Code: ' Printed: Tue Nov 11 09:33:15 2003 f"' Name: 111003A-503 Text : Page 3 Exygen Research, 3058 Research Drive, State College, PA 16801 000207 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:ll/10/03, Analyst:K.Hisha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 4 Name: 111003A-504 Text: 1: PFOA X C t 11003-3,100 ng/L standard 111003A-504 Sm (M n, 2x2) 100i %: 10-NOV-2003 21:41:34 LC/MS/MS #7 MRM of 1 Channel ES5.07 413 > 369 1 .1 5 e 5 A re a 1.00 2.000 iri i y i1^ riT II f"i IIIIrI'p I J j 1' I l 1 'I I' T1"i l r J 1 "T I I I ! T I I I I I 3 .0 0 4 .0 0 5 .0 0 i~ t - | ~ r --'r - r - 1 I t I I j I T -i r " | r - i r - i - - | T i m e 6 .0 0 7 .0 0 8 .00 Exysen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Sate:11/10/03, Analyst:K.Risha Sample List: P:\Bata\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Bata\LCMSMS7\Masslynx\008 APFO.PRO\MethBB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-505 Text: 1: PFOA Page 5 Eiqrgen Research, 3058 Research Srive, State College, PA 16801 000209 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, AnalystrK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynac\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-506 Text: 1: PFOA Page 6 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:1.1278, Set No.:111003A, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PF( Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Rage 7 Name: 111003A-507 Text: 1: PFOA X C111003-6,1000 ng/L standard 111003A-507 Sm (Mn, 2 x2 ) 100-1 %- 5.08 141260 10-NOV-2003 22:31:53 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1 .2 0 e 6 A re a 6.00T -T -r-p r 3 .0 0 4 .0 0 I" " Ir 5 .0 0 7 .00 Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000211 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Tue Nov 11 09:28:10 2003 P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Thu Oct 30 07:08:49 2003 Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-508 Text: 1 : PFOA Page 8 Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 2 1 .2 Quantify Sample Report Study No.:L1278, Set No.:111003a , Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslymx\008 APFO.PRO\SanqpleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-509 Text: Page 9 Exygen Research, 3058 Research Drive, State College, PA 16801 'y Quantify Sample Report Study No.:I<1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.R i sha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-510 Text: 1 : PFOA Rage 10 Exygen Research, 3058 Research Drive, State College, PA 16801 21.4 Quantify Sample Report Study No.:L1278, Set No . :111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-511 Text: 1: PFOA Page 11 Exygen Research, 3058 Research Drive, State College, PA 16801 00021.5 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PF< Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 12 Name: 111003A-512 Text: 1: PFOA Reagent Spk B, 500 ng/L 111003A-512 Sm (Mn, 2x2) 100n %- 5.07 68809 IO-Nov-2003 23:55:52 LC/MS/MS #7 MRM of 1 Channel ES 413 >369 5 .9 6 e 5 A re a 4 .0 0 5 .0 0 6 .0 0 '.' I I ' I IT i-T i-i I Tim e 7 .0 0 8 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 00021.6 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 13 Name: 111003A-513 Text: 1: PFOA L1278-1 Spk C , 500 ng/L 111003A-513 S m (Mn, 2 x2) 10O - %: U - , - r - |--r p - i - . t T r - r " i - r I--r 11--r - r - |- T - i --I - I - I 1 ' 1 1 T" ` T - r 1 .0 0 2 .0 0 3 .0 0 5 .0 6 190667721 11-Nov-2003 00:12:38 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1 .2 9 e 8 A re a 1 iiiIIIIIIi' 'I"IT lT Tim e 4 . 0 0 5 . 0 0 6.00 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 00021.7 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APPO.PRO\MethOB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 14 Name: 111003A-514 Text: 1: PFOA L1278-14 Spk D, 500 ng/L 111003A-514 Sm (M n, 2x2) 101 %: t r 1* 1 T--pi 1 1* 1 1 t~t--T JT r n I 1 n i i 1 .0 0 2 .0 0 3 .0 0 5 .0 6 31462061 4 .0 0 1 5 .0 0 11-Nov-2003 00:29:18 LC/MS/MS #7 MRM of 1 Channel ES413 >369 2 .3 0 e 7 A re a i. T I- 1 I |-, p it p T-i T 'p T i-r1] Tim e 6 .00 7 .0 0 8 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-515 Text: 1: PFOA Page 15 Exygen Research, 3058 Research Drive, State College, PA 16801 A ffcffcM Q Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-516 Text: 1: PFOA Page 16 Exygen Research, 3058 Research Drive, State College, PA 16801 c .N \ Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K .Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PF< Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 17 Name: 111003A-517 Text: 1: PFOA L1278-1 111003A-517 Sm (Mn, 2x2) 100i %- 5.07 24077158 11-Nov-2003 01:19:34 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.31e8 Area a TTJTTT I.' r I r I I I I 1 1 I I I I 1 1- 1 T-r-| Time 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000221 Quantify Sample Report Study No.:L1278# Set NC.s111003A, Ext.Date:ll/10/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 18 Name: 111003A-518 Text: 1 : PFOA L1278-1 Rep 111003A-518 Sm (M n, 2x2) 10O- 5.05 209826041 11-Nov-2003 01:36:24 LC/MS/MS #7 MRM of 1 Channel E S 413 > 369 1 .2 0 e 8 A rea v - -' r 1r -r r 1 r - r - r - r - H 1.00 r I r 1 T-r-|- 1T 1r ( T'l TT! 2 .0 0 3 .00 4 .0 0 J 5 .0 0 T f-r i-TTf r 'I T I -| I T I -I' I -I 1 -I I "I Tim e 6 .00 7 .00 8 .0 0 Exygen Research/ 3058 Research Drive# State College# PA 16801 000222 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext .Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Rage 19 Name: 111003A-519 Text: 1: PFOA L1278-2 111003A-519 Sm (Mn, 2 x2) 10Ch %: 11-Nov-2003 01:53:15 LC/MS/MS #7 MRM of 1 Channel E S 413 >369 1 .3 4 e 8 A re a Q-1,,-- 1" , I--r,,,-r r-|.-i-r I--I j-i ,-| .f-| .I--.| 1.00 2.00 I I I I i - r -T - p r i i -T p r ' i 3 .0 0 4 .0 0 r r r - n - p .rr r-r r-r i-r ! T i m e 7 .0 0 8 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 000223 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha r-- Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A , Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFQA Last modified: Thu Oct 30 07:08:49 2003 -< Job Code: Printed: Tue Nov 11 09:33:15 2003 ; Name: 111003A-520 Text: ^ 1 : PF0A Rage 20 Exygen Research, 3058 Research Drive, State College, PA 16801 ) *''jL Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PF< Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 21 Name: 111003A-521 Text: 1 : PFOA L 1 278-4 111003A-521 Sm (Mn, 2x2) 10CH %- 5.06 1230677881 11-Nov-2003 02:26:52 LC/MS/MS #7 MRM of 1 Channel ES413 >369 7.67e6 Area 5 .0 0 1"` f 1-r-<-r I-T..I n f i n 6 .00 7 .0 0 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report : Study No.:L1278, Set No.:111003A, Ext.Date:ll/10/03, Analyst:K.Risha -- < Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A j Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 A Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A- 522 Text: 1 : PFOA Page 22 \ ! Exygen Research, 3058 Research Drive, State College, PA 16801 ; 000226 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Pate:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 23 Name: 111003A-523 Text: 1 : PFOA X C 1 11003-3,100 ng/L standard 111003A-523 Sm (Mn, 2x2) * tr\ n _ %: 5.05 145541 11-Nov-2003 03:00:28 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.04e5 Area o: n - n " i - t~ I-- i i r ; i **i n 1 r r 1.00 1 r ~ r ~ T ~ 1-- r r r r r i 2.00 Timer t r r " T | - t - t 1 1-- 1 1 -1 1 I-- r r r i t ~ i r r i ...r - i v-i v - i 1 1 1 1 1 1 1 I 1 ' 1 1 1 I 1 1' 1 1 -I 1 -1 i T 1 3.00 4.00_________5^0_________ 60_________ 7\00_________ 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003a , Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PF< Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 24 Name: 111003A-524 Text: 1 : PFOA L1 278-6 1 1 1003A-524 Sm (M n, 2 x2 ) 10Ch %- 5.05 V 11-Nov-2003 03:17:19 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.03e7 A re a a 1 .0 0 2 .00 3 .0 0 4 .00 5 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 000228 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample Dist: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PF( Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 25 Name: 111003A-525 Text: 1 : PFOA L 1 278-7 111003A-525 Sm (M n, 2 x2 ) 10Ch %- 5.06 1 11-Nov-2003 03:34:01 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1 .1 2 e 7 A rea 0T 1.00 2 .0 0 I' I I "I H 'JT T'T 1 3 .0 0 I | I I' I 4 .0 0 5 .0 0 6.00 I r i i-i q-n-r-q Tim e 7 .0 0 8 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 000299 : Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha f Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 P> Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-526 Text: 1 : PFOA Page 26 Exygen Research, 3058 Research Drive, State College, PA 16801 000230 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SajnpleDB\111003A | Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: i Printed: Tue Nov 11 09:33:15 2003 Page 27 Name: 111003A-527 Text: 1 : PFOA L 1 278-9 111003A-527 Sm (M n, 2x2) 100n f0 %: 1.00 2.00O ' i i i --|--i r i I j--I--i--i--r j r i I--i--[--i--I--r 3 .0 0 5.05 4 .00 5 .0 0 11-Nov-2003 04:07:51 LC/MS/MS #7 MRM of 1 Channel ES413 >369 7 .9 1 e 6 A re a 11I 1 111 I ' 1*"r'i" I-r-v-j-r r r i-| Tim e 6 .00 7 .0 0 8 .00 r ; n Exygen Research, 3058 Research Drive, State College, PA 16801 000231 Quantify Sample Report Study No. :L1278, Set No. :111003A, Ext .Date: 11/10/03, Analyst :K.Risha Sample List: P:\Data\LCHSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PF< Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 28 Name: 111003A>528 Text: 1: PFOA L t 278-10 111003A-528 Sm (M n, 2x2) 10Ch %- 5.05 1 11-Nov-2003 04:24:32 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1 .1 6e6 A re a 0T Tim e 1 .0 0 2 .0 0 3 .0 0 4 .0 0 5 .0 0 6.00 7 .0 0 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000232 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:ll/10/03, Analyst:K.Risha f Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A : Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 f~ Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-529 Text: Page 29 Exygen Research, 3058 Research Drive, State College, PA 16801 0001273 Quantify Sample Report Study No.:L1278, Set No.:111003a . Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: F:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-530 Text: 1 : PFOA Rage 30 & Exygen Research, 3058 Research Drive, State College, PA 16801 000234 ! Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, AnalysttK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 r * Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 31 Name: 111003A-531 Text: 1 : PFOA L 1 278-12 111003A-531 Sm (M n, 2x2) 100q %~ 0" I' I-"1' r"'i ' I I-r I r-| ' ' ' ' ! ' ! 1.00 2.00 3.00 5.06 4.00 5.00 11-Nov-2003 05:15:02 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.35e7 Area r-i-p T-i-i 1 1 1 1 I I i-i-i h "I i-i-i I Tim e 6.00 7.00 8.00 Exygen Research 3058 Research Drive State College PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:ll/10/03, Analyst :K.Risha Sandle List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-532 Text: 1 : PFOA Rage 32 Exygen Research, 3058 Research Prive State College, PA 16801 00023G i Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A ' Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 T Name: 111003A-533 Text: Page 33 Exygen Research, 3058 Research Drive, State College, PA 16801 000237  Quantify Sample Report Study No. :L1278, Set No.:111003A, Ext .Date: 11/10/03, Analyst :K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 -- Job Code: Printed: Tue Nov 11 09:33:15.2003 Name: 111003A-534 Text:i 1: PFOA Rage 34 i Exygen Research, 3058 Research Drive, State College, PA 16801 0 0 0 2 .2 8 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Page 35 Name: 111003A-535 Text: 1 : P F O A ________________________ ___________________________________________________________________________________________________________________________________ X C 1 11003-5, 500 ng/L standard 11-Nov-2003 06:22:18 LC/MS/MS #7 111003A-535 Sm (M n, 2 x2 ) 100- 5.05 691611 MRM of 1 Channel ES413 >369 4 .6 8 e 5 A re a % f\ "1 1 1 1 I 1 1 I 1 |-r 1T'i 1r-r 1T- 1 1 t 1r n T T r i T r y m r i T-|"irj-rrrj"r f-JTMn r T=i==r*n Tim e 1 .0 0 2 .0 0 3 .0 0 4 .0 0 5 .0 0 6 .0 0 7 .0 0 8 .0 0 / Exygen Research, 3058 Research Drive, State College, PA 16801 )0 2 ?9 Quantify Sample Report Study No.:L1278, Set No.:111003A, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003A Last modified: Tue Nov 11 09:28:10 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Tue Nov 11 09:33:15 2003 Name: 111003A-536 Text: 1 : PFOA X C 1 11003-6,1000 ng/L standard 111003A-536 Sm (M n, 2 x2) 100; 5.04 1384711 %- 0- ' I ' r"1' 1I"'1"111 ~r" ' 1111' ' 1 11 i 1111 11 1| 1111| 1 .0 0 2 .0 0 3 .00 4 .0 0 J 5 .0 0 11-Nov-2003 06:39:12 LC/MS/MS #7 MRM of 1 Channel ES 413 >369 9 .3 7 e 5 A re a 6.00 7 .0 0 Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000240 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L1278 PFOA 413->369 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: 111003B Katen Risha LC/MS/MS Unit #7 11/10/03 11/11/03 Exygen ID XC111003-0 XC111003-1 XC111003-2 XC111003-3 XCU1003-4 XCl 11003-5 XC111003-6 XC111003-7 Methanol Wash ReagentBlank Reagent Spk A Reagent Spk B L1278-I8 Spk C L1278-29 Spk D XCl 11003-1 U278-15 L1278-I6 L1278-17 L1278-18 L1278-18 Rep XCl 11003-2 L1278-19 L1278-20 L1278-21 L1278-22 L1278-23 XCl 11003-3 L1278-24 L1278-25 LI 278-26 U278-27 L1278-28 XCl 11003-4 L1278-29 L1278-29 Rep L1278-30 L1278-31 L1278-32 XCl 11003-5 XCU 1003-6 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-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 Run Code No. c 111003B-601 CS 111003B-602 CS 111003B-603 CS 111003B-604 CS 111003B-605 CS 111003B-606 CS 111003B-607 CS 111003B-608 c 111003B-609 c 111003B-610 LCS 111003B-611 LCS 111003B-612 LF 111003B-613 LF 111003B-614 CS 111003B-615 s 111003B-616 s 111003B-617 s 111003B-618 s 111003B-619 s 111003B-620 CS 111003B-621 s 111003B-622 s 111003B-623 s 111003B-624 s 111003B-625 s 111003B-626 CS 111003B-627 s U1003B-628 s 111003B-629 sss 1U003B-630 111003B-631 1U003B-632 CsssssS 111003B-633 111003B-634 111003B-635 111003B-636 111003B-637 111003B-638 CS 111003B-639 CS 111003B-640 Analyte Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = [analyte found (ppt>analyte found in control (ppt)l x 100 amount added (ppt) Std. Cone. Dilution Peak (PPt) Factor Area 0- 0 25 - 3131 50 - 6631 100 - 12800 250 - 32252 500 - 64456 1000 - 133574 250 - 32963 -- 0 -1 0 - 1 6415 - 1 62544 - l 7464335 - 1 19982676 25 - 6325 - 1 497314 - I 1739249 - 1 14567455 - 1 7587623 - 1 9075131 50 - 7580 - 1 2529208 - 1 974634 - 1 8541184 - 1 949420 100 1- 723288 14073 - 1 664568 - 1 12242205 - 1 2601276 - 1 1508137 - 1 3853684 250 - 34815 - 1 18733028 - 1 18311804 -- 500 1 11776531 1 4047390 l- 1971910 65699 1000 - 132996 Analyte Amount Analyte Found Added Recovery Found (ppo (ppo (%) (ppb) .- .. ._ -- -- -- -- -- -- -- -- -- -- -- -- -- ND 41.1 50 472 500 A 500 A 500 - - 82 94 - - - -- - - *- - - *- -- *- -- *- *- --- -* * * - -* * - - - - - - --* * * - - - - -- *- -- *- -- -- -- *- -- *- -- *** -- - --- - --- - --- Standard Curve: Linear (1/x weighted) Intercept = 1056.74 Slope = 130.299 Coef. OfDet = 0.999101 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)] / sampleweight (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 111203A. ^Sample requires dilution. See data set 111203A. Spreadsheet prepared by: Analyte Found (ppb) Dry Weight . . . . - - -- - --- il RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fa x: 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. 2 7 ~ Time f f l O Date_ Initials /!ET CLIENT SAMPLE ID EXYGEN ID NUMBER WEIGHT (g) FORTIFICATION (ng) na Reagent Blank _ _ na Reagent Spk A _ 2.0 na Reagent Spk B 20.0 MW-4 (13-15) L1278-18 SpkC 5.0 20.0 MW-6 (9-11) L1278-29 SpkD 5.0 20.0 MW-4 (0-2) L1278-15 5.0 _ MW-4 (3-5) L1278-16 5.0 - MW-4 (8-10) L1278-17 5.0 - MW-4 (13-15) L1278-18 5.0 _ MW-4 (13-15) L1278-18 Rep 5.0 _ MW-4 (18-20) L1278-19 5.0 MW-4 (28-30) L1278-20 5.0 _ MW-3 (4-6) L1278-21 5.0 _ MW-3 (9-11) L1278-22 5.0 _ MW-3 (14-16) L1278-23 5.0 _ MW-3 (19-21) L1278-24 5.0 - MW-1 (0-2) L1278-25 5.0 _ MW-1 (8-10) L1278-26 5.0 _ MW-6 (0-2) LI278-27 5.0 - MW-6 (4-6) L1278-28 5.0 _ MW-6 (9-11) L1278-29 5.0 _ MW-6 (9-11) L1278-29 Rep 5.0 - MW-6 (14-16) L1278-30 5.0 - MW-6 (19-21) L1278-31 5.0 _ MW-6 (24-26) L1278-32 5.0 - Spiking Solution Used Volume Used for Spiking Initial/Date Reagent Spk A F092203-5 (10 ng/mL) 200 uL (200 pL micropipet) iP L /llici^> Reagent Spk B F092203-4 (100 ng/mL) 200 uL (200 pLmicropipet) L1278-18 SpkC LI278-29 Spk D F092203-4 (100 ng/mL) F092203-4 (100 ng/mL) 200 pL (200 pL micropipet) /n'toi)2 . 200 pL (200 pL micropipet) iffi- /n'liD){g> Time 0 Q 3 O Date / Initials After weighing samples were returned to refrigerator No. J22- Time I Q 5 D Date t t j l b j o S_____ Initials . Comments: EJJl^ij200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: 3 Analysis Summary: Data Set: i| 1003> Data Set: \T02? A Data Set: -- Initials/Date:__hg-J__/_ ii Initials/Date:. Initials/Date:. Set extraction/analysis data verified by: O/S r> Date:. / 1 ]) ]] 1 RESEARCH 3058 Research D rive Phone: 814-272-1039 State College, P A 16801 Fa x: 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: PFOA Client ID na na na MW-4 (13-15) MW-6 (9-11) Exygen ID Reagent Blank Reagent Spk A Reagent Spk B L1278-18 Spk C L1278-29 Spk D STEP STEP STEP STEP STEP STEP Dilutions STEP Dilutions STEP 1 2 3 4 5 6 (mL/mL) - 7 (mL/mL) - 8 - -- - --- -- *- Reagents/ Materials Methanol C18 SPE Type I Water . - Lot# 43Z -3S33S 1aI3Z ^TB2- NA _ - 000 po n: b MW-4 (0-2) L1278-15 - -- MW-4 (3-5) L1278-16 ;ox - -_ MW-4 (8-10) L1278-17 - -- MW-4 (13-15) L1278-18 -V i -- MW-4 (13-15) L1278-18 Rep o - Initials/Date lE B ll|/n joA MW-4 (18-20) L1278-19 'Vv0 - MW-4 (28-30) L1278-20 - O.o5/t>o _- MW-3 (4-6) MW-3 (9-11) MW-3 (14-16) L1278-21 L1278-22 L1278-23 ___ -- -- 0.054,0 --* Xo -_ -- MW-3 (19-21) L1278-24 Vu> -_ MW-1 (0-2) L1278-25 0,0V to -- MW-1 (8-10) L1278-26 -- -- 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) C*ITnDitDia1ls./DAaAtAe LI278-27 L1278-28 L1278-29 !___ L1278-29 Rep L1278-30 L1278-31 L1278-32 <T 5T ~ Ce r CEB \onol rtnrl choho h\r Vton/4 frlr J.1 mi M &. [I T~ T~ T~ COS CPE liM i. -- -M o --- -- -- Kof-M.o L_ HPLC Methanol Ammonium Acetate LVSfciSfl ___ V iO ;)/p 1 ^r ~ Type I water - -- - NA )J u\lofo3 1 5 1 >1 _Initials/Date 1 2 SSSSTTTTEEEEPPPP 4352:::: CBFSPirelintEnetrgrciotufhlupurgomteounfg4ohcr0lge1mla0anLsmsuwiapnicturhtoehdsyisapcter-3ca0r0b0firlptemred type I water , j* STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes Q STEP 7: LC/MS/MS analysis STEP 8: LC/MS/MS reanalysis. OUTW ..i.ros^upi_ 010\\\\o\t>b Burbs 03W0T.V Final extracts stored in refrigerator3 2 - Initials: Date: Initials and date under each step indicates the personnel that performed this step. July 19,2001/4 ) 5 1 1 1 1 1 "1 Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO .I >RO\SampleDB\111003B.spl Printed: Mon Nov 10 15:42:43 2003 il|lo |o 3 _________ 1) 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 40 Vial File Name LIM S ID Client 10 Sample Description 21 111003B-601 __ 22 111003B-602 23 111003B-603 -- 24 111003B-604 -- 25 111003B-605 -- 26 111003B-606 -- 27 111003B-607 -- 28 111G03B-608 -- 92 111003B-609 -- 61 111003B-610 -- 62 111Q03B-611 -- 63 111003B-612 -- 64 111003B-613 -- 65 111003B-614 -- 22 111003B-615 -- 66 111003B-616 -- 67 111003B-617 -- 68 111003B-618 -- 69 111003B-619 -- 70 111003B-620 -- 23 111003B-621 -- 71 111003B-622 -- 72 111003B-623 -- 73 111003B-624 -- 74 111003B-625 -- 75 111003B-626 -- 24 111003B-627 -- 76 111003B-628 -- 77 111003B-629 -- 78 111003B-630 -- 79 111003B-631 -- 80 111003B-632 -- 25 111003B-633 -- 81 111003B-634 -- 82 111003B-635 -- 83 111003B-636 -- 84 111003B-637 -- 85 111003B-638 -- 26 111003B-639 -- 27 111003B-640 -- -- -- X C 1 11003-0, 0 ng/L standard X C 1 11003-1, 25 ng/L standard X C 111003-2,50 ng/L standard X C 1 11003-3,100 ng/L standard X C 1 11003-4,250 ng/L standard X C 1 11003-5,500 ng/L standard standardXC111003-6,1000 ng/L standard X C 111003-7, 250 ng/L check Methanol W ash 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 X C 1 11003-1,25 ng/L standard L1278-15 L1278-16 L1278-17 L1278-18 L1278-18 Rep X C 111003-2,50 ng/L standard L1278-19 L1278-20 L1278-21 L1278-22 L1278-23 X C 1 11003-3,100 ng/L standard L1278-24 L1278-25 L1278-26 L1278-27 L1278-28 X C 1 11003-4, 250 ng/L standard L1278-29 L1278-29 Rep L 1278-30 L1278-31 L1278-32 X C 111003-5, 500 ng/L standard X C 1 11003-6,1000 ng/L standard 1 ) 1 1 Exygen STUDY N O . L21& Page 1 P ag e Position: (1 ,1 ) 1 (ng/L)Matrix Sam ple Type C one C o n e B C o n e C T e s t ID D F M S M ethod Blank 0 -- Standard 25 -- Standard 50 -- Standard 100 -- Standard 250 -- Standard 500 -- Standard 1000 -- QC 250 -- Blank -- -- Blank -- -- QC -- QC 50 500 -- QC 500 -- QC 500 -- Standard 25 -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Analyte -- -- Standard 50 -- 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 0 0 0 0 0 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFOA 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFOA 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFOA 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A 1 008 PFO A } 1 I11)1 Masslynx - Sample List Sample List: C:\M ASSLYNX\008 A P F 0 .P R 0 \S a m p le D B \1 11003B.spl Printed: Mon Nov 10 15:42:43 2003 |d [o ^ 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 O 37 O '"i 3398 40 H P LC Method MS Tune File Inj Volum e (pL) water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water water PFOATune PFOATune PFO A Tune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFO A Tune PFOATune PFO A Tune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFO A Tune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 15 in 1 11 Exygen STUDY NO . l i n ' d 111 1 Page 2 Page Position: (2,1 ) 1 LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L1278 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Quat 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:MA10327) (JONESCHROMATOGRAPHY: Part No. FK5962E) M obile Phase (A) : 2 mM Ammonium Acetate in Type I Water M obile Phase (B) : Methanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: Titnhhseetrmnueamxstseln3ytnpsxaegstteoisfntagwrsaeurcseoepdmrfopogurrtaethrmeg.aenTneahrleyaspteiasdgoepfsrtichnoitsnotduaatistnaftrshoeemt. A ll Handwritten Peak ID 's by:_ Il|izjq3 Scanning Method Report Method: C:\MASSLYNX\008 APFO.PRO\ACQUDB\008 PFOA Last Modified: W e d Mar 20 15:07:50 2002 Printed: Mon Nov 10 15:42:52 2003 Solvent Delay ( mins ) : 0.00 Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 413.00 369.00 0.20 10 10 Page 1 000247 M ethod R e p o rt Method File: Last Modified: Printed C:\MASSLYNX\008 APFO.PRO\ACQUDB\water Monday, November 10, 2003 15:39:51 Monday, November 10, 2003 15:43:01 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 Page 1 II IQ Pressure 400 400 400 400 400 400 400 400 400 400 HP1100 L Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Contactl Off Off Off On Off Off Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/zl/min) Draw Position (mm) Stop Time (mins) Injection Volume(/Lil) Vial Number 200.0 200 0.10 15.00 15.0 7 000248 Tuning Method Report Method: C:\MASSLYNX\008 APFO.PRO\ACQUDB\PFOA TUNE Printed: Mon Nov 10 15:43:08 2003 m Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 101 300 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3.4e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -695 Rdbk 102.5 711.7 Quantify Calibration Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Hisha Calibration: P:\Data\LCMSMS7\Masslynx\008 A P F O .PRO\CurveDB\111003B Last modified: Wed Nov 12 07:22:06 2003 Printed: Wed Nov 12 07:23:27 2003 Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000250 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P :\Data\LCMSMS7\Mas slynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Initials. Date. Printed: Wed Nov 12 07:23:28 2003 Run# . Page 1 - UK> Name: 111003B-601 Text: 1 : PFOA X C 1 11003-0,0 ng/L standard 111003B-601 Sm (Mn, 2x2) 100-1 11-Nov-2003 07:12:49 LC/MS/MS #7 MRM of 1 Channel ES- 6.29 6.52 6 7 9 7 .7 3 413 > 369 5.99. \ . (I ft f Y . 5.66e3 1 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-602 Text: 1 : PFOA Page 2 Exygen Research, 3058 Research Drive, State College, PA 16801 000252 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-603 Text: 1: PFOA Page 3 Exygen Research, 3058 Research Drive, State College, PA 16801 000253 Quantify Sample Report Study N o .:L12 78, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-604 Text: 1 : PFOA Page 4 Exygen Research 3058 Research Drive, State College PA 16801 254 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst tK.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Wed Nov 12 07:17:06 2003 P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Thu Oct 30 07:08:49 2003 Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-605 Text: 1: PFOA Page 5 Exygen Research 3058 Research Drive State College PA 16801 o r - cr Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-606 Text: 1: PFOA Page 6 Exygen Research, 3058 Research Drive State College, PA 16801 Q0025G Quantify Sample Report Study No.:L1278, Set No.s111003B, Ext.Date:11/10/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APF0.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-607 Text: 1 : PFOA Page 7 Exygen Research 3058 Research Drive State College PA 16801 i V Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 f3S Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-608 Text : 1: PFOA Rage 8 /V '/ pm i Exygen Research 3058 Research Drive State College PA 16801 000258 Quantify Sample Report Study N o . :1.1278/ Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-609 Text: Page 9 /f** Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-610 Text: 1 : PFOA Page 10 Exygen Research, 3058 Research Drive, State College, PA 16801 000260 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-611 Text: 1 : PFOA Page 11 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 AFFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Page 12 Name: 111003B-612 Text: 1 : PFOA Reagent Spk B, 500 ng/L 111003B-612 Sm (Mn, 2x2) 100- %: 1.00 2 .0 0 3.001 1 1 1/LVr r_ r"r ' I "'-1 ' 1 1 111111111 111111 1 11 '41.01 0 Ai652.504441 5 .0 0 1 ' ' '...* 1 ' 11-Nov-2003 10:17:24 LC/MS/MS #7 MRM of 1 Channel ES413 >369 4.15e5 Area 6.00 7.00 T-i Time 8.00 fS Exygen Research, 3058 Research Drive, State College, PA 16801 0002G2 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-613 Text: 1 : PFOA Page 13 Exygen Research, 3058 Research Drive, State College, PA 16801 000263 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-614 Text: ^ 1 : PFOA Rage 14 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study N o . :1*1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PROXMethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-615 Text: 1 : PFOA Page 15 Exygen Research, 3058 Research Drive State College, PA 16801 e-.o Quantify Sainple Report Study No.:L1278, Set No.:111003b , Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-616 Text: 1 : PFOA Page 16 Exygen Research, 3058 Research Drive, State College, PA 16801 000266 Quantify Sample Report Study No.:Ll278, Set No.:111003B, Ext.Date:ll/10/03, AnalystrK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Page 17 Name: 111003B-617 Text: 1 : PFOA L1278-16 111003B-617 Sm (Mn, 2x2) -4 1 AU UA __ - 5.03 17392491 I 11-Nov-2003 11:41:25 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.08e7 Area J y( *-r--r I-- 1-- |-- n - r ri | | rI--- rr ii -Tr" I\ ri~" iI lr--i11 |\ Ti" ii iI ii {{ ii tr i r -rr yy i 1 1i 1i 1i ) 1 i 1- r1 i1' q ( " ti 1i i i`-- 1-- ^ 1.00 2.00 3.00 4.00 r r T im ei----ir vi --|j > 1t i' tM | r1 i1 r1 - i1 p[ i111i-` i1 i1 j i1 n 1i*"T"{" n1 i1 r |1 | 5.00 6.00 7 .0 0 _________ a 0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 000267 Quantify Sample Report Study No.:I>1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample Lists P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-618 Text: 1: PFOA Page 18 Exygen Research, 3058 Research Drive, State College, PA 16801 000268 Quantify Sample Report Study No.:L1278, Set No.:111003b , Ext.Date:ll/10/03, Analyst:K.Risha Sample Lists P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-619 Text: 1: PFOA Page 19 Exygen Research, 3058 Research Drive, State College, PA 16801 000269 Quantify Sample Report Study Mo.:L1278, Set No.:111003B, Ext.Date:11/10/03/ AnalystrK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-620 Text: 1: PFOA Page 20 Exygen Research/ 3058 Research Drive/ State College, PA 16801 000270 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Ned Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-621 Text: 1: PFOA Rage 21 Exygen Research, 3058 Research Drive, State College, PA 16801 000271 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-622 Text: 1 : PFOA Rage 22 Exygen Research, 3058 Research Drive, State College, PA 16801 000272 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Page 23 Name: 111003B-623 Text: / 1 : PFOA L 1 278-20 111003B-623 S m (Mn, 2x2) 10Ch f-- ' %: U~t- 1 1 - 1 rr r - ' - 1 1 1 1 1 1 ( r ' I1 1 1 <* 1.0 0 2 .0 0 3.00 5.02 9746341 11-Nov-2003 13:22:23 LC/MS/MS #7 MRM of 1 Channel ES413 >369 5.51 e6 Area 1 1 ] 1 1 1 1 4.00 ' .I 1 H , - r lT l ' r 5.00 6 .0 0 T im e | 'T~i " r-r" I-- r-'i-- r~i -[~t ~i-- r i-- [ 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000273 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Dates11/10/03/ Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-624 Text: 1 : PFOA Rage 24 Exygen Research, 3058 Research Drive, State College, PA 16801 000274 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Page 25 Name: 111003B-625 Text: 1 : PFOA L 1 278-22 111003B-625 Sm (Mn, 2x2) 100n %: 5.02 11-Nov-2003 13:56:07 LC/MS/MS #7 MRM of 1 Channel ES413 >369 5.47e6 Area 0 ' 1 1 1 i ' 1 1 1 i 1 1 111 i 1 1 '' 1 i 1.00 2.00 3.00 4.00 5.00 - n i--- H -' 1 ' I 1 1 1 1 I Tim e 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-626 Text: 1 : PFOA Page 26 Exygen Research, 3058 Research Drive State College PA 16801 000276 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst :K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003*1 Page 27 Name: 111003B-627 Text: 1 : PFOA X C 1 11003-3,100 ng/L standard 111003B-627 S m (Mn, 2 x2 ) 100i %: 11-Nov-2003 14:29:48 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.13e5 Area 0 r . - i I I r ~ T j y " i~ i i- | -- r-1 ! [ I 1.00 2.00 T - | - v r T =r p r i 3.00 1 T 1 r,i| I I 1 1 1 I 1 1 1 1 I ' 1 1 1 I Tim e 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 277 Quantify Sample Report Study No.:L1278, Set No.:111003b , Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SanleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-628 Text: 1 : PFOA Rage 28 Exygen Research, 3058 Research Drive, State College, PA 16801 000278 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sanle List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-629 Text: 1 : PFOA Page 29 Exygen Research, 3058 Research Drive, State College, PA 16801 000279 Quantify Sample Report Study N o .:L1278, Set No.:111003B, Ext.Date:ll/10/03, AnalystsK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003*1 Page 30 Name: 111003B-630 Text: 1 : PFOA L1 278-26 1 1 1003B-630 S m (Mn, 2x2) 100i %' 5.03 26012761 11-Nov-2003 15:20:24 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.67e7 Area 0" 1 1 1 ' I " 1 1 I rr-i I p I M I 1.00 2.00 3.00 ' 4.00 11 1 1 1 5.00 ' 6 .0 0 7.00 1 1 1 1 ` 1 Tinie 8 .0 0 Exygen Research, 3058 Research Drive, State College, PA 16801 000280 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Page 31 Name: 111003B-631 Text: 1 : PFOA L 1 278-27 111003B-631 Sm (Mn, 2x2) 10Ch 5.04 15081371 %: CH"11 ' T~l 1"1| 1 I 1 T J 1" 1 11i 1[--n 1i 1.00 2.00 3.00 j ' 111i 1111i 1111 11 4.00 5.00 11-Nov-2003 15:37:21 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.04e7 Area ,| 6.00 | T~i r~I j I I I I | i I I -r11 Tim e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext .Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-632 Text: 1 : PFOA Page 32 Exygen Research, 3058 Research Drive, State College, PA 16801 000282 Quantify Sample Report Study No.:L1278, Set No.:111003b , Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Rage 33 Name: 111003B-633 Text: 1: PFOA X C 111003-4, 250 ng/L standard 111003B-633 Sm (Mn, 2x2) 100i %: 5.02 348151 11-Nov-2003 16:10:52 LC/MS/MS #7 MRM of 1 Channel ES413 >369 2.88e5 Area (J- f'rri }T-l-l "l-p-T-TT-11 r I-- 'rT-f r r r "T*l~| T-I H' l~l"'~rlI'1`'`T'"' 1' 11' 1 1.00 2 .0 0 3.00 4.00 5.00 11111 11 , , , , , , , , , I 111t 1 Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000283 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:ll/10/03, Analyst:K.Risha Sample Lists P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Rage 34 Name: 111003B-634 Text: 1: PFOA L 1 278-29 111003B-634 Sm (Mn, 2x2) 100n %: 1.00 2.00Q -i I I I , j -- ,-- j-- i-- I-- I I j i - i -- I-- I-- j-- i-- 3.00 5.02 4.00 5.00 11-Nov-2003 16:27:41 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.21e8 Area - it '1T-T-pi-r n - 1 I I I I I I I I I I Time 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000284 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Page 35 Name: 111003B-635 Text: 1: PFOA L1278-29 Rep 111003B-635 Sm (Mn, 2x2) 10 0 n %~ 5.01 i183118041 u~^ 111r 5 11111--1 1 1 rl I'1 1 11'1 1 ''I H" >' ' 1>' 1.0 0 2 .0 0 3.00 4.00 5.00 11-Nov-2003 16:44:30 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1 .2 0 e 8 Area ' "I 1 *' I t"i 7.1 p'i h ' i j i t i t ] Tim e 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000285 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Mov 12 07:23:28 2003 Page 36 Name: 111003B-636 Text: 1: PFOA L1278-30 111003B-636 Sm (Mn, 2x2) 10 0 - %: i5.00 117765311 -) i'-T-- n -- r 1 1 1 1 1 1 1 1 1.0 0 'r - n - i " , - ! ... | T T i 1 1T ,_r'" 2 .0 0 3.00 4.00 5.00 11-Nov-2003 17:01:22 LC/MS/MS #7 MRM of 1 Channel E S 413 >369 7.73e7 Area , ri. 6.00 r-i j--r IT 1 7 -! T-i"n Tim e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000286 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03/ Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Ned Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PF< Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Page 37 Name: 111003B-637 Text : 1: PFOA U 278-31 111003B-637 Sm (Mn, 2x2) 100-1 %- 4.99 4047390 11-Nov-2003 17:18:13 LC/MS/MS #7 MRM of 1 Channel ES413 >369 2.78e7 Area 2.00 6.00 n r"i r I I Tim e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000287 Quantify Sample Report Study No.:L1278, Set No.:111003b / Ext.Date:ll/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFi Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003*1 Page 38 Name: 111003B-638 Text : 1 : PFOA U 278-32 111003B-638 Sm (Mn, 2 x 2 ) 1OOn 5.00 1971$ 11-Nov-2003 17:34:55 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.46e7 Area 5.00 6.00 7.00 r-n Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000288 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Name: 111003B-639 Text: 1: PFOA Page 39 Exygen Research, 3058 Research Drive, State College, PA 16801 000289 Quantify Sample Report Study No.:L1278, Set No.:111003B, Ext.Date:11/10/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111003B Last modified: Wed Nov 12 07:17:06 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\102703 PFOA Last modified: Thu Oct 30 07:08:49 2003 Job Code: Printed: Wed Nov 12 07:23:28 2003 Rage 40 Name: 111003B-640 Text: 1 : PFOA X C 1 11003-6,1000 ng/L standard 111003B-640 Sm (Mn, 2x2) 1 00n %: jI4.98 1329961 11-Nov-2003 18:08:41 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.17e6 Area o: ' ' I'l I ' ' i M '.. I T .. ' ' ' ' - " "| \I " i \ T"r~r r v ' \' ' ` I ' Ty \ I in'i Tim e1 1 i I 1 I 11 1 j I I....i1-11i I1 I t ~i 1 I1 I I I I1 I1 r- ' r n h) I-- r 7i i 1 i1 i1 i1 i1 j1 i1 i l l i i i iy t t i m| i i1 t c )1 i i t i i1 t1 1 t1 | i1 i1 t t ') | 1.00 2.00 3.00 4.00_________ 5 ^ 0 _________ & 00_________ 7,00_________ 8X30 Exygen Research, 3058 Research Drive, State College, PA 16801 000290